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#\#CIF_1.0 ################################################################################ # # # This CIF is a part of the B-IncStrDB # # (Bilbao Incommensurate Structures Database) # # http://www.cryst.ehu.eus/bincstrdb/ # # # # Please note that the structure of the CIF file may differ from the one # # deposited, as it may have been modified to comply with the standard. The # # file has been validated against official dictionaries as well as local # # dictionaries including non-standard data names used by SHELXL (Sheldrick, # # G. M. (2008). Acta Cryst. A 64, 112-122) and JANA (Petricek, V., Dusek, M. # # and Palatinus, L. (2014), Z. Kristallogr. 229, 345-352). # # # # For comments and/or criticisms, please e-mail to administrador-bcs@ehu.es # # # ################################################################################ data_global _publcif_datablock.id '{8155da1e-8a83-443a-bcc9-ed40a73704dc}' _audit_update_record ;2015-08-21 # Formatted by IUCr publCIF system ; _database_code_depnum_ccdc_archive 'CCDC 927469' #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic 2015-02-24 _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code YC5004 _journal_coeditor_notes ; ? ; _journal_paper_category FA _journal_techeditor_code ? _iucr_compatibility_tag ACTA95 _journal_coden_ASTM ? _journal_name_full 'IUCrJ' _journal_year 2015 _journal_volume 2 _journal_issue ? _journal_page_first 584 _journal_page_last 600 _journal_paper_doi http://dx.doi.org/10.1107/S2052252515011665 _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _publ_contact_author_name 'Stoger, Berthold' _publ_contact_author_address ;Institute of Chemical Technologies and Analytics Vienna University of Technology Vienna Austria ; _publ_contact_author_email bstoeger@mail.tuwien.ac.at _publ_section_title ;Crystal chemistry of layered structures formed by linear rigid silyl-capped molecules ; loop_ _publ_author_name _publ_author_address 'Lumpi, Daniel' ;Institute of Applied Synthetic Chemistry Vienna University of Technology Vienna Austria ; 'Kautny, Paul' ;Institute of Applied Synthetic Chemistry Vienna University of Technology Vienna Austria ; 'Stoger, Berthold' ;Institute of Chemical Technologies and Analytics Vienna University of Technology Vienna Austria ; 'Frohlich, Johannes' ;Institute of Chemical Technologies and Analytics Vienna University of Technology Vienna Austria ; #============================================================================== data_ASYM #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C13 H22 S1 Si2' _chemical_formula_weight 266.6 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 7.2016(4) _cell_length_b 9.7603(4) _cell_length_c 12.2829(4) _cell_angle_alpha 95.4952(16) _cell_angle_beta 92.510(2) _cell_angle_gamma 101.346(2) _cell_volume 840.86(6) loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.8378(11) 1 0 0 0 1 0 0 0 1 2 0.1622(11) -1 0.5333 0.1494 0 1 0 0 0 1 _cell_formula_units_Z 2 _cell_measurement_reflns_used 8516 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 30.1 _cell_measurement_temperature 100 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 1.0524 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 288 _exptl_absorpt_coefficient_mu 0.313 _exptl_crystal_description block _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.61 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_colour 'clear colourless' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.94 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\w- and \f-scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 21588 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 30.15 _diffrn_reflns_theta_full 29.04 _diffrn_measured_fraction_theta_max 0.96 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 4622 _reflns_number_gt 3651 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_gt 0.0532 _refine_ls_R_factor_all 0.0762 _refine_ls_wR_factor_ref 0.0549 _refine_ls_goodness_of_fit_ref 2.27 _refine_ls_goodness_of_fit_gt 2.49 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 4622 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_number_constraints 88 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0102 _refine_ls_shift/su_mean 0.0011 _refine_diff_density_max 0.61 _refine_diff_density_min -0.39 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.86915(9) 0.88589(6) 0.65955(4) Uani 0.02025(19) 2 1 d . . . Si2 Si 0.70091(8) 0.30001(6) -0.04248(4) Uani 0.01583(17) 2 1 d . . . S1 S 0.72090(10) 0.39931(6) 0.38295(4) Uani 0.02794(19) 2 1 d . . . C1 C 0.7757(3) 0.5774(2) 0.35942(15) Uani 0.0154(6) 2 1 d . . . C2 C 0.8091(3) 0.6819(2) 0.45166(15) Uani 0.0168(6) 2 1 d . . . C3 C 0.8371(3) 0.7643(2) 0.53256(16) Uani 0.0204(7) 2 1 d . . . C4 C 0.7861(3) 0.6114(2) 0.25543(15) Uani 0.0209(7) 2 1 d . . . C5 C 0.7553(3) 0.5109(2) 0.16171(16) Uani 0.0203(7) 2 1 d . . . C6 C 0.7310(3) 0.4267(2) 0.08120(16) Uani 0.0204(7) 2 1 d . . . C7 C 0.7327(4) 1.0237(3) 0.6368(2) Uani 0.0398(10) 2 1 d . . . C8 C 1.1260(3) 0.9638(2) 0.68819(17) Uani 0.0288(8) 2 1 d . . . C9 C 0.7807(4) 0.7832(3) 0.77261(18) Uani 0.0387(9) 2 1 d . . . C10 C 0.8896(3) 0.1956(3) -0.03317(18) Uani 0.0250(8) 2 1 d . . . C11 C 0.4620(3) 0.1839(3) -0.04603(19) Uani 0.0268(8) 2 1 d . . . C12 C 0.7230(3) 0.4002(2) -0.16385(16) Uani 0.0251(7) 2 1 d . . . C13 C 0.7202(4) 0.4061(2) 0.52981(16) Uani 0.0263(7) 2 1 d . . . H4 H 0.815937 0.709181 0.244356 Uiso 0.025 2 1 d . . . H71 H 0.745287 1.088845 0.701696 Uiso 0.0478 2 1 d . . . H72 H 0.780703 1.072711 0.57652 Uiso 0.0478 2 1 d . . . H73 H 0.601278 0.981128 0.62038 Uiso 0.0478 2 1 d . . . H81 H 1.144251 1.02231 0.756769 Uiso 0.0346 2 1 d . . . H82 H 1.19586 0.889965 0.691999 Uiso 0.0346 2 1 d . . . H83 H 1.170417 1.019307 0.630586 Uiso 0.0346 2 1 d . . . H91 H 0.796553 0.844206 0.839921 Uiso 0.0465 2 1 d . . . H92 H 0.648659 0.742054 0.75704 Uiso 0.0465 2 1 d . . . H93 H 0.851126 0.710239 0.779451 Uiso 0.0465 2 1 d . . . H101 H 0.886881 0.136275 -0.100482 Uiso 0.0299 2 1 d . . . H102 H 1.011193 0.257987 -0.020558 Uiso 0.0299 2 1 d . . . H103 H 0.868292 0.138585 0.026337 Uiso 0.0299 2 1 d . . . H131 H 0.684179 0.312584 0.550388 Uiso 0.0316 2 1 d . . . H132 H 0.844828 0.448186 0.561784 Uiso 0.0316 2 1 d . . . H133 H 0.63121 0.461264 0.555624 Uiso 0.0316 2 1 d . . . H111 H 0.448178 0.112484 -0.106965 Uiso 0.0322 2 1 d . . . H112 H 0.448567 0.140468 0.020879 Uiso 0.0322 2 1 d . . . H113 H 0.366182 0.238678 -0.053835 Uiso 0.0322 2 1 d . . . H121 H 0.702722 0.335862 -0.229451 Uiso 0.0302 2 1 d . . . H122 H 0.630085 0.458479 -0.163632 Uiso 0.0302 2 1 d . . . H123 H 0.847798 0.458071 -0.161256 Uiso 0.0302 2 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Si1 Si 0.0271(3) 0.0191(3) 0.0123(3) 0.0030(3) -0.0023(3) -0.0042(2) Si2 Si 0.0135(3) 0.0203(3) 0.0122(2) 0.0027(3) -0.0005(2) -0.0034(2) S1 S 0.0432(4) 0.0181(3) 0.0203(3) 0.0044(3) -0.0039(3) -0.0024(2) C1 C 0.0106(10) 0.0175(10) 0.0172(9) 0.0043(9) -0.0019(8) -0.0040(8) C2 C 0.0156(10) 0.0182(10) 0.0166(9) 0.0037(9) -0.0010(9) 0.0018(8) C3 C 0.0237(11) 0.0193(11) 0.0175(9) 0.0034(10) -0.0005(9) 0.0012(8) C4 C 0.0238(11) 0.0183(11) 0.0180(10) -0.0001(10) 0.0005(9) -0.0016(8) C5 C 0.0190(11) 0.0233(11) 0.0178(9) 0.0034(10) -0.0004(9) 0.0009(8) C6 C 0.0145(10) 0.0269(12) 0.0186(10) 0.0031(10) 0.0002(9) -0.0012(9) C7 C 0.0490(18) 0.0457(18) 0.0272(14) 0.0253(15) -0.0066(13) -0.0125(12) C8 C 0.0333(13) 0.0221(12) 0.0272(12) 0.0002(11) -0.0041(11) -0.0036(10) C9 C 0.0467(16) 0.0424(16) 0.0178(11) -0.0116(14) -0.0010(12) 0.0008(11) C10 C 0.0226(12) 0.0310(14) 0.0230(12) 0.0120(11) -0.0009(10) -0.0011(10) C11 C 0.0180(12) 0.0317(14) 0.0278(12) -0.0006(10) -0.0006(10) 0.0006(10) C12 C 0.0263(13) 0.0304(13) 0.0208(10) 0.0099(11) 0.0038(10) 0.0033(9) C13 C 0.0327(14) 0.0265(12) 0.0218(10) 0.0092(12) 0.0002(11) 0.0066(9) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Si1 C3 . . 1.844(2) ? Si1 C7 . . 1.850(3) ? Si1 C8 . . 1.861(2) ? Si1 C9 . . 1.852(3) ? Si2 C6 . . 1.841(2) ? Si2 C10 . . 1.858(3) ? Si2 C11 . . 1.861(2) ? Si2 C12 . . 1.855(2) ? S1 C1 . . 1.760(2) ? C1 C2 . . 1.428(3) ? C1 C4 . . 1.352(3) ? C2 C3 . . 1.201(3) ? C4 C5 . . 1.419(3) ? C4 H4 . . 0.96 ? C5 C6 . . 1.207(3) ? C7 H71 . . 0.96 ? C7 H72 . . 0.96 ? C7 H73 . . 0.96 ? C8 H81 . . 0.96 ? C8 H82 . . 0.96 ? C8 H83 . . 0.96 ? C9 H91 . . 0.96 ? C9 H92 . . 0.96 ? C9 H93 . . 0.96 ? C10 H101 . . 0.96 ? C10 H102 . . 0.96 ? C10 H103 . . 0.96 ? C11 H111 . . 0.96 ? C11 H112 . . 0.96 ? C11 H113 . . 0.96 ? C12 H121 . . 0.96 ? C12 H122 . . 0.96 ? C12 H123 . . 0.96 ? C13 H131 . . 0.96 ? C13 H132 . . 0.96 ? C13 H133 . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C3 Si1 C7 . . . 107.10(11) ? C3 Si1 C8 . . . 109.19(10) ? C3 Si1 C9 . . . 107.83(10) ? C7 Si1 C8 . . . 110.81(12) ? C7 Si1 C9 . . . 112.10(13) ? C8 Si1 C9 . . . 109.70(11) ? C6 Si2 C10 . . . 107.63(10) ? C6 Si2 C11 . . . 108.53(10) ? C6 Si2 C12 . . . 108.15(10) ? C10 Si2 C11 . . . 110.48(11) ? C10 Si2 C12 . . . 111.22(11) ? C11 Si2 C12 . . . 110.71(11) ? S1 C1 C2 . . . 118.56(15) ? S1 C1 C4 . . . 119.45(15) ? C2 C1 C4 . . . 121.99(19) ? C1 C2 C3 . . . 176.7(2) ? Si1 C3 C2 . . . 177.07(19) ? C1 C4 C5 . . . 123.7(2) ? C1 C4 H4 . . . 118.15 ? C5 C4 H4 . . . 118.14 ? C4 C5 C6 . . . 179.0(2) ? Si2 C6 C5 . . . 178.36(19) ? Si1 C7 H71 . . . 109.47 ? Si1 C7 H72 . . . 109.47 ? Si1 C7 H73 . . . 109.47 ? H71 C7 H72 . . . 109.47 ? H71 C7 H73 . . . 109.47 ? H72 C7 H73 . . . 109.47 ? Si1 C8 H81 . . . 109.47 ? Si1 C8 H82 . . . 109.47 ? Si1 C8 H83 . . . 109.47 ? H81 C8 H82 . . . 109.47 ? H81 C8 H83 . . . 109.47 ? H82 C8 H83 . . . 109.47 ? Si1 C9 H91 . . . 109.47 ? Si1 C9 H92 . . . 109.47 ? Si1 C9 H93 . . . 109.47 ? H91 C9 H92 . . . 109.47 ? H91 C9 H93 . . . 109.47 ? H92 C9 H93 . . . 109.47 ? Si2 C10 H101 . . . 109.47 ? Si2 C10 H102 . . . 109.47 ? Si2 C10 H103 . . . 109.47 ? H101 C10 H102 . . . 109.47 ? H101 C10 H103 . . . 109.47 ? H102 C10 H103 . . . 109.47 ? Si2 C11 H111 . . . 109.47 ? Si2 C11 H112 . . . 109.47 ? Si2 C11 H113 . . . 109.47 ? H111 C11 H112 . . . 109.47 ? H111 C11 H113 . . . 109.47 ? H112 C11 H113 . . . 109.47 ? Si2 C12 H121 . . . 109.47 ? Si2 C12 H122 . . . 109.47 ? Si2 C12 H123 . . . 109.47 ? H121 C12 H122 . . . 109.47 ? H121 C12 H123 . . . 109.47 ? H122 C12 H123 . . . 109.47 ? H131 C13 H132 . . . 109.47 ? H131 C13 H133 . . . 109.47 ? H132 C13 H133 . . . 109.47 ? # start Validation Reply Form #_vrf_PLAT924_ASYM #; #PROBLEM: The Reported and Calculated Rho(min) Differ by . 3.80 eA-3 #RESPONSE: Structure is twinned and therefore intensities are misinterpreted #by CHECKCIF. #; #_vrf_PLAT925_ASYM #; #PROBLEM: The Reported and Calculated Rho(max) Differ by . 3.31 eA-3 #RESPONSE: Structure is twinned and therefore intensities are misinterpreted #by CHECKCIF. #; #_vrf_PLAT902_ASYM #; #PROBLEM: No (Interpretable) Reflections found in FCF .... Please Check #RESPONSE: This structure was refined from HKLF5 style reflection data #which CHECKCIF cannot parse correctly #; #======================================================================= data_BSEM _publcif_datablock.id '{4740eb5d-65a9-4075-bc68-4cd2da624df7}' _database_code_depnum_ccdc_archive 'CCDC 927472' #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_sum 'C22 H30 S2 Si2' _chemical_formula_weight 414.8 _chemical_absolute_configuration ? _chemical_compound_source ? _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' _space_group_IT_number 15 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y,-z+1/2 3 -x,-y,-z 4 x,-y,z+1/2 5 x+1/2,y+1/2,z 6 -x+1/2,y+1/2,-z+1/2 7 -x+1/2,-y+1/2,-z 8 x+1/2,-y+1/2,z+1/2 _cell_length_a 34.148(6) _cell_length_b 6.8690(12) _cell_length_c 10.3442(18) _cell_angle_alpha 90 _cell_angle_beta 98.343(8) _cell_angle_gamma 90 _cell_volume 2400.7(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 18955 _cell_measurement_temperature 100 _cell_measurement_theta_max 34.9 _cell_measurement_theta_min 2.4 _exptl_crystal_type_of_structure cryst _exptl_absorpt_coefficient_mu 0.326 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour 'clear yellow' _exptl_crystal_density_diffrn 1.1472 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'plate' _exptl_crystal_F_000 888 _exptl_crystal_size_max 0.77 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_size_rad ? #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_unetI/netI 0.0228 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 38270 _diffrn_reflns_reduction_process ? _diffrn_reflns_theta_full 35 _diffrn_reflns_theta_max 35 _diffrn_reflns_theta_min 1.21 _diffrn_ambient_temperature 100 _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_measurement_method '\w- and \f-scans' _diffrn_measurement_specimen_support ? _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source_current ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 4193 _reflns_number_total 5255 _reflns_threshold_expression 'I>3\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics ? _computing_publication_material ? _computing_structure_refinement ? _computing_structure_solution ? _refine_diff_density_max 0.43 _refine_diff_density_min -0.22 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? _refine_ls_extinction_coef ? _refine_ls_extinction_method 'none' _refine_ls_goodness_of_fit_gt 2.41 _refine_ls_goodness_of_fit_ref 2.19 _refine_ls_hydrogen_treatment 'constr' _refine_ls_number_constraints 60 _refine_ls_number_parameters 118 _refine_ls_number_reflns 5255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0307 _refine_ls_restrained_S_all ? _refine_ls_restrained_S_gt ? _refine_ls_shift/su_max 0.0035 _refine_ls_shift/su_mean 0.0006 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0442 #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group S S 0.419611(6) 0.11777(3) 0.11095(2) Uani 0.01837(6) 8 1 d . . . Si Si 0.321272(7) 0.35715(3) 0.43975(2) Uani 0.01769(7) 8 1 d . . . C1 C 0.46995(2) 0.42787(11) 0.06768(8) Uani 0.01359(19) 8 1 d . . . C2 C 0.49845(2) 0.30281(11) 0.02820(8) Uani 0.0156(2) 8 1 d . . . C3 C 0.47204(2) 0.62626(11) 0.03738(8) Uani 0.0155(2) 8 1 d . . . C4 C 0.43845(2) 0.35546(11) 0.13903(8) Uani 0.0140(2) 8 1 d . . . C5 C 0.42532(2) 0.46355(12) 0.23315(8) Uani 0.0165(2) 8 1 d . . . C6 C 0.39321(2) 0.41453(12) 0.30064(8) Uani 0.0171(2) 8 1 d . . . C7 C 0.36568(3) 0.38581(12) 0.35998(9) Uani 0.0185(2) 8 1 d . . . C8 C 0.30424(3) 0.60690(14) 0.47498(11) Uani 0.0328(3) 8 1 d . . . C9 C 0.33321(3) 0.21502(14) 0.59275(9) Uani 0.0254(3) 8 1 d . . . C10 C 0.28334(3) 0.22535(19) 0.32517(11) Uani 0.0366(3) 8 1 d . . . C11 C 0.41142(3) 0.09948(12) -0.06499(9) Uani 0.0220(2) 8 1 d . . . H2 H 0.497455 0.166172 0.046963 Uiso 0.0187 8 1 d . . . H3 H 0.452654 0.714258 0.06259 Uiso 0.0186 8 1 d . . . H5 H 0.438836 0.583836 0.256514 Uiso 0.0198 8 1 d . . . H81 H 0.27977 0.598682 0.51013 Uiso 0.0394 8 1 d . . . H82 H 0.323867 0.669084 0.537266 Uiso 0.0394 8 1 d . . . H83 H 0.300301 0.681531 0.395692 Uiso 0.0394 8 1 d . . . H91 H 0.31118 0.219313 0.640727 Uiso 0.0305 8 1 d . . . H92 H 0.338531 0.082339 0.571889 Uiso 0.0305 8 1 d . . . H93 H 0.356114 0.269829 0.644875 Uiso 0.0305 8 1 d . . . H101 H 0.261133 0.194452 0.368688 Uiso 0.044 8 1 d . . . H102 H 0.274733 0.306195 0.25075 Uiso 0.044 8 1 d . . . H103 H 0.294552 0.107359 0.2969 Uiso 0.044 8 1 d . . . H111 H 0.397377 -0.018702 -0.090426 Uiso 0.0264 8 1 d . . . H112 H 0.396098 0.208936 -0.101064 Uiso 0.0264 8 1 d . . . H113 H 0.436429 0.098479 -0.097055 Uiso 0.0264 8 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S S 0.02379(11) 0.01330(10) 0.01955(11) -0.00388(7) 0.00835(8) -0.00053(7) Si Si 0.01397(11) 0.02170(12) 0.01876(12) 0.00170(8) 0.00695(9) 0.00076(9) C1 C 0.0128(3) 0.0140(3) 0.0144(3) -0.0003(2) 0.0034(3) -0.0015(3) C2 C 0.0162(3) 0.0125(3) 0.0188(4) 0.0005(3) 0.0050(3) -0.0004(3) C3 C 0.0146(3) 0.0139(3) 0.0188(4) 0.0018(3) 0.0057(3) -0.0022(3) C4 C 0.0129(3) 0.0136(3) 0.0160(3) -0.0006(2) 0.0033(3) -0.0003(3) C5 C 0.0154(3) 0.0168(4) 0.0184(4) -0.0019(3) 0.0062(3) -0.0018(3) C6 C 0.0180(4) 0.0154(3) 0.0186(4) 0.0003(3) 0.0051(3) -0.0019(3) C7 C 0.0180(4) 0.0172(4) 0.0213(4) 0.0011(3) 0.0058(3) -0.0007(3) C8 C 0.0359(6) 0.0303(5) 0.0355(6) 0.0140(4) 0.0166(5) 0.0052(4) C9 C 0.0240(4) 0.0279(5) 0.0258(5) 0.0029(3) 0.0089(4) 0.0055(4) C10 C 0.0225(5) 0.0585(7) 0.0293(5) -0.0116(5) 0.0054(4) -0.0055(5) C11 C 0.0278(4) 0.0176(4) 0.0207(4) -0.0054(3) 0.0038(3) -0.0039(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S C4 . . 1.7634(9) ? Si C7 . . 1.8391(11) ? Si C8 . . 1.8644(12) ? Si C9 . . 1.8539(11) ? Si C10 . . 1.8593(12) ? C1 C2 . . 1.4025(12) ? C1 C3 . . 1.4024(12) ? C1 C4 . . 1.4765(12) ? C2 C3 . 3_665 1.3826(12) ? C2 H2 . . 0.96 ? C3 H3 . . 0.96 ? C4 C5 . . 1.3516(12) ? C5 C6 . . 1.4232(13) ? C5 H5 . . 0.96 ? C6 C7 . . 1.2112(13) ? C8 H81 . . 0.96 ? C8 H82 . . 0.96 ? C8 H83 . . 0.96 ? C9 H91 . . 0.96 ? C9 H92 . . 0.96 ? C9 H93 . . 0.96 ? C10 H101 . . 0.96 ? C10 H102 . . 0.96 ? C10 H103 . . 0.96 ? C11 H111 . . 0.96 ? C11 H112 . . 0.96 ? C11 H113 . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C7 Si C8 . . . 106.87(5) ? C7 Si C9 . . . 110.24(4) ? C7 Si C10 . . . 108.04(5) ? C8 Si C9 . . . 110.72(5) ? C8 Si C10 . . . 111.37(5) ? C9 Si C10 . . . 109.54(5) ? C2 C1 C3 . . . 118.05(7) ? C2 C1 C4 . . . 121.73(7) ? C3 C1 C4 . . . 120.22(7) ? C1 C2 C3 . . 3_665 120.86(7) ? C1 C2 H2 . . . 119.57 ? C3 C2 H2 3_665 . . 119.57 ? C1 C3 C2 . . 3_665 121.09(7) ? C1 C3 H3 . . . 119.46 ? C2 C3 H3 3_665 . . 119.46 ? S C4 C1 . . . 120.29(6) ? S C4 C5 . . . 118.43(6) ? C1 C4 C5 . . . 121.12(7) ? C4 C5 C6 . . . 125.66(8) ? C4 C5 H5 . . . 117.17 ? C6 C5 H5 . . . 117.17 ? C5 C6 C7 . . . 175.65(9) ? Si C7 C6 . . . 174.87(7) ? Si C8 H81 . . . 109.47 ? Si C8 H82 . . . 109.47 ? Si C8 H83 . . . 109.47 ? H81 C8 H82 . . . 109.47 ? H81 C8 H83 . . . 109.47 ? H82 C8 H83 . . . 109.47 ? Si C9 H91 . . . 109.47 ? Si C9 H92 . . . 109.47 ? Si C9 H93 . . . 109.47 ? H91 C9 H92 . . . 109.47 ? H91 C9 H93 . . . 109.47 ? H92 C9 H93 . . . 109.47 ? Si C10 H101 . . . 109.47 ? Si C10 H102 . . . 109.47 ? Si C10 H103 . . . 109.47 ? H101 C10 H102 . . . 109.47 ? H101 C10 H103 . . . 109.47 ? H102 C10 H103 . . . 109.47 ? H111 C11 H112 . . . 109.47 ? H111 C11 H113 . . . 109.47 ? H112 C11 H113 . . . 109.47 ? #======================================================================= data_BSEMOX1 _publcif_datablock.id '{fb1d8f59-01f8-4c16-90b1-7499f77f1e79}' _database_code_depnum_ccdc_archive 'CCDC 928106' #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C22 H30 O4 S2 Si2' _chemical_formula_weight 478.8 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 6.8197(3) _cell_length_b 12.1073(5) _cell_length_c 16.1123(7) _cell_angle_alpha 92.3607(19) _cell_angle_beta 93.9781(19) _cell_angle_gamma 98.3425(19) _cell_volume 1311.34(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9974 _cell_measurement_temperature 150 _cell_measurement_theta_max 34.9 _cell_measurement_theta_min 3.1 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 1.2121 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 0.318 _exptl_crystal_colour 'clear colourless' _exptl_crystal_description plate _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.97 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 150 _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_measurement_method '\w- and \f-scans' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_specimen_support ? _diffrn_reflns_number 57779 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 35.06 _diffrn_reflns_theta_full 35.06 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_unetI/netI 0.0227 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 11485 _reflns_number_gt 8331 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_gt 0.0436 _refine_ls_R_factor_all 0.0512 _refine_ls_wR_factor_ref 0.0443 _refine_ls_goodness_of_fit_ref 2.15 _refine_ls_goodness_of_fit_gt 2.50 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 11485 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_number_constraints 120 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0013 _refine_ls_shift/su_mean 0.0001 _refine_diff_density_max 0.44 _refine_diff_density_min -0.39 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.21273(5) 0.10115(3) 0.383099(19) Uani 0.03221(10) 2 1 d . . . S S 0.09772(3) 0.261886(18) 0.087388(15) Uani 0.01803(7) 2 1 d . . . O1 O 0.03695(10) 0.29046(6) 0.00453(4) Uani 0.0281(2) 2 1 d . . . O2 O -0.03105(11) 0.27970(6) 0.15188(5) Uani 0.0301(2) 2 1 d . . . C1 C 0.42030(13) 0.42138(7) 0.05499(6) Uani 0.0179(3) 2 1 d . . . C2 C 0.30773(14) 0.50002(7) 0.02378(6) Uani 0.0197(3) 2 1 d . . . C3 C 0.61308(14) 0.42241(7) 0.03067(6) Uani 0.0200(3) 2 1 d . . . C4 C 0.34126(14) 0.33876(7) 0.11406(6) Uani 0.0203(3) 2 1 d . . . C5 C 0.44536(17) 0.31828(9) 0.18362(7) Uani 0.0317(3) 2 1 d . . . C6 C 0.37894(18) 0.24393(10) 0.24546(7) Uani 0.0357(4) 2 1 d . . . C7 C 0.32224(19) 0.18517(10) 0.30006(7) Uani 0.0381(4) 2 1 d . . . C8 C 0.2319(2) -0.04684(10) 0.35776(9) Uani 0.0480(5) 2 1 d . . . C9 C 0.3553(3) 0.15520(13) 0.48198(8) Uani 0.0586(6) 2 1 d . . . C10 C -0.0514(2) 0.12119(13) 0.38208(9) Uani 0.0542(5) 2 1 d . . . C11 C 0.13139(14) 0.12060(8) 0.08265(7) Uani 0.0237(3) 2 1 d . . . Si' Si 0.14044(5) 0.56394(2) 0.354503(17) Uani 0.02587(9) 2 1 d . . . S' S 0.69783(3) 0.830984(19) 0.194600(15) Uani 0.01936(7) 2 1 d . . . O1' O 0.67601(12) 0.84820(7) 0.28160(5) Uani 0.0354(3) 2 1 d . . . O2' O 0.86046(10) 0.89621(6) 0.15839(5) Uani 0.0307(2) 2 1 d . . . C1' C 0.49096(12) 0.92932(7) 0.06724(6) Uani 0.0145(2) 2 1 d . . . C2' C 0.59696(13) 1.03736(7) 0.07734(6) Uani 0.0159(2) 2 1 d . . . C3' C 0.60477(12) 1.10686(7) 0.01088(6) Uani 0.0160(2) 2 1 d . . . C4' C 0.47361(13) 0.85264(7) 0.13667(6) Uani 0.0158(2) 2 1 d . . . C5' C 0.29722(14) 0.79691(8) 0.15367(6) Uani 0.0196(3) 2 1 d . . . C6' C 0.25949(14) 0.71875(8) 0.21631(6) Uani 0.0210(3) 2 1 d . . . C7' C 0.21260(15) 0.65324(8) 0.26845(6) Uani 0.0239(3) 2 1 d . . . C8' C 0.0676(3) 0.65591(11) 0.43712(8) Uani 0.0625(6) 2 1 d . . . C9' C -0.0732(2) 0.45820(10) 0.31548(8) Uani 0.0413(4) 2 1 d . . . C10' C 0.3590(2) 0.49934(13) 0.39039(10) Uani 0.0619(6) 2 1 d . . . C11' C 0.71327(15) 0.68927(8) 0.17262(7) Uani 0.0274(3) 2 1 d . . . H2 H 0.17503 0.500515 0.039994 Uiso 0.0236 2 1 d . . . H3 H 0.691979 0.368788 0.05186 Uiso 0.024 2 1 d . . . H5 H 0.578317 0.357665 0.192817 Uiso 0.038 2 1 d . . . H111 H 0.218118 0.108183 0.039861 Uiso 0.0284 2 1 d . . . H112 H 0.189286 0.102084 0.135334 Uiso 0.0284 2 1 d . . . H113 H 0.005155 0.074386 0.070168 Uiso 0.0284 2 1 d . . . H2' H 0.66448 1.063553 0.130298 Uiso 0.0191 2 1 d . . . H3' H 0.677173 1.181145 0.018639 Uiso 0.0192 2 1 d . . . H5' H 0.183503 0.811471 0.119646 Uiso 0.0235 2 1 d . . . H111' H 0.717696 0.676051 0.113671 Uiso 0.0329 2 1 d . . . H112' H 0.831565 0.670526 0.200977 Uiso 0.0329 2 1 d . . . H113' H 0.598979 0.643814 0.191213 Uiso 0.0329 2 1 d . . . H81 H 0.179929 -0.091938 0.401125 Uiso 0.0576 2 1 d . . . H82 H 0.156978 -0.07068 0.305862 Uiso 0.0576 2 1 d . . . H83 H 0.36877 -0.054855 0.353113 Uiso 0.0576 2 1 d . . . H101 H -0.114106 0.078675 0.424545 Uiso 0.0651 2 1 d . . . H102 H -0.059452 0.198977 0.392527 Uiso 0.0651 2 1 d . . . H103 H -0.117673 0.096294 0.328635 Uiso 0.0651 2 1 d . . . H91 H 0.302317 0.114177 0.527176 Uiso 0.0703 2 1 d . . . H92 H 0.492287 0.146523 0.478792 Uiso 0.0703 2 1 d . . . H93 H 0.345111 0.232932 0.491257 Uiso 0.0703 2 1 d . . . H81' H 0.013715 0.611465 0.480467 Uiso 0.075 2 1 d . . . H82' H 0.182006 0.706625 0.45972 Uiso 0.075 2 1 d . . . H83' H -0.03095 0.697607 0.414249 Uiso 0.075 2 1 d . . . H91' H -0.115408 0.4123 0.360015 Uiso 0.0496 2 1 d . . . H92' H -0.180751 0.495113 0.294855 Uiso 0.0496 2 1 d . . . H93' H -0.034345 0.412303 0.271318 Uiso 0.0496 2 1 d . . . H101' H 0.328104 0.456103 0.437656 Uiso 0.0742 2 1 d . . . H102' H 0.392839 0.451549 0.346249 Uiso 0.0742 2 1 d . . . H103' H 0.46938 0.556864 0.405874 Uiso 0.0742 2 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Si Si 0.0474(2) 0.02372(15) 0.02452(16) 0.00038(13) 0.00266(14) 0.00738(12) S S 0.01440(10) 0.01724(10) 0.02198(12) -0.00026(8) 0.00287(9) 0.00215(8) O1 O 0.0212(4) 0.0321(4) 0.0275(4) -0.0065(3) -0.0058(3) 0.0089(3) O2 O 0.0268(4) 0.0286(4) 0.0365(4) 0.0048(3) 0.0138(3) -0.0012(3) C1 C 0.0179(4) 0.0145(4) 0.0196(5) -0.0021(3) -0.0016(3) 0.0022(3) C2 C 0.0149(4) 0.0173(4) 0.0264(5) 0.0007(3) 0.0021(4) 0.0017(4) C3 C 0.0170(4) 0.0149(4) 0.0275(5) 0.0018(3) -0.0028(4) 0.0048(4) C4 C 0.0200(4) 0.0172(4) 0.0215(5) -0.0037(3) -0.0004(4) 0.0030(3) C5 C 0.0318(6) 0.0302(5) 0.0273(6) -0.0117(4) -0.0083(5) 0.0092(4) C6 C 0.0398(7) 0.0344(6) 0.0272(6) -0.0098(5) -0.0109(5) 0.0102(5) C7 C 0.0465(7) 0.0346(6) 0.0289(6) -0.0053(5) -0.0078(5) 0.0083(5) C8 C 0.0614(9) 0.0314(6) 0.0534(9) 0.0095(6) 0.0109(7) 0.0069(6) C9 C 0.0840(12) 0.0576(9) 0.0297(7) -0.0020(8) -0.0048(7) 0.0087(6) C10 C 0.0599(10) 0.0463(8) 0.0582(10) 0.0099(7) 0.0142(8) -0.0004(7) C11 C 0.0175(4) 0.0184(4) 0.0347(6) 0.0006(3) 0.0045(4) -0.0013(4) Si' Si 0.03791(17) 0.02103(13) 0.01707(14) -0.00308(12) 0.00359(12) 0.00579(10) S' S 0.01356(10) 0.02294(11) 0.02119(12) 0.00154(8) -0.00222(9) 0.00671(9) O1' O 0.0328(4) 0.0513(5) 0.0204(4) 0.0055(4) -0.0067(3) -0.0013(3) O2' O 0.0133(3) 0.0325(4) 0.0463(5) -0.0002(3) 0.0003(3) 0.0186(3) C1' C 0.0098(4) 0.0165(4) 0.0182(4) 0.0029(3) 0.0027(3) 0.0052(3) C2' C 0.0131(4) 0.0176(4) 0.0170(4) 0.0022(3) 0.0005(3) 0.0017(3) C3' C 0.0117(4) 0.0151(4) 0.0212(5) 0.0010(3) 0.0018(3) 0.0030(3) C4' C 0.0127(4) 0.0182(4) 0.0168(4) 0.0023(3) 0.0012(3) 0.0047(3) C5' C 0.0144(4) 0.0238(4) 0.0211(5) 0.0021(3) 0.0014(3) 0.0086(4) C6' C 0.0141(4) 0.0269(5) 0.0217(5) 0.0010(3) 0.0015(4) 0.0063(4) C7' C 0.0206(5) 0.0272(5) 0.0236(5) 0.0009(4) 0.0028(4) 0.0061(4) C8' C 0.1141(14) 0.0335(7) 0.0380(8) -0.0100(8) 0.0372(9) -0.0008(6) C9' C 0.0487(8) 0.0344(6) 0.0361(7) -0.0131(5) 0.0096(6) 0.0031(5) C10' C 0.0665(10) 0.0594(10) 0.0596(10) 0.0121(8) -0.0159(8) 0.0275(8) C11' C 0.0214(5) 0.0264(5) 0.0365(6) 0.0081(4) 0.0021(4) 0.0104(4) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Si C7 . . 1.8474(13) ? Si C8 . . 1.8465(13) ? Si C9 . . 1.8510(14) ? Si C10 . . 1.8512(17) ? S O1 . . 1.4410(8) ? S O2 . . 1.4354(8) ? S C11 . . 1.7579(10) ? C1 C2 . . 1.3953(13) ? C1 C3 . . 1.3962(14) ? C1 C4 . . 1.4798(13) ? C2 C3 . 2_665 1.3892(13) ? C2 H2 . . 0.96 ? C3 H3 . . 0.96 ? C4 C5 . . 1.3361(14) ? C5 C6 . . 1.4236(16) ? C5 H5 . . 0.96 ? C6 C7 . . 1.2035(17) ? C8 H81 . . 0.96 ? C8 H82 . . 0.96 ? C8 H83 . . 0.96 ? C9 H91 . . 0.96 ? C9 H92 . . 0.96 ? C9 H93 . . 0.96 ? C10 H101 . . 0.96 ? C10 H102 . . 0.96 ? C10 H103 . . 0.96 ? C11 H111 . . 0.96 ? C11 H112 . . 0.96 ? C11 H113 . . 0.96 ? Si' C7' . . 1.8431(11) ? Si' C8' . . 1.8409(15) ? Si' C9' . . 1.8501(12) ? Si' C10' . . 1.8501(18) ? S' O1' . . 1.4298(8) ? S' O2' . . 1.4380(8) ? S' C11' . . 1.7572(11) ? C1' C2' . . 1.3971(11) ? C1' C3' . 2_675 1.4001(12) ? C1' C4' . . 1.4830(13) ? C2' C3' . . 1.3880(13) ? C2' H2' . . 0.96 ? C3' H3' . . 0.96 ? C4' C5' . . 1.3426(12) ? C5' C6' . . 1.4229(14) ? C5' H5' . . 0.96 ? C6' C7' . . 1.2066(14) ? C8' H81' . . 0.96 ? C8' H82' . . 0.96 ? C8' H83' . . 0.96 ? C9' H91' . . 0.96 ? C9' H92' . . 0.96 ? C9' H93' . . 0.96 ? C10' H101' . . 0.96 ? C10' H102' . . 0.96 ? C10' H103' . . 0.96 ? C11' H111' . . 0.96 ? C11' H112' . . 0.96 ? C11' H113' . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C7 Si C8 . . . 107.97(6) ? C7 Si C9 . . . 106.61(6) ? C7 Si C10 . . . 106.81(7) ? C8 Si C9 . . . 112.61(7) ? C8 Si C10 . . . 110.27(7) ? C9 Si C10 . . . 112.24(7) ? O1 S O2 . . . 117.21(5) ? O1 S C11 . . . 107.78(5) ? O2 S C11 . . . 109.02(5) ? C2 C1 C3 . . . 118.85(8) ? C2 C1 C4 . . . 121.55(9) ? C3 C1 C4 . . . 119.60(8) ? C1 C2 C3 . . 2_665 120.27(9) ? C1 C2 H2 . . . 119.87 ? C3 C2 H2 2_665 . . 119.87 ? C1 C3 C2 . . 2_665 120.89(9) ? C1 C3 H3 . . . 119.56 ? C2 C3 H3 2_665 . . 119.56 ? C1 C4 C5 . . . 122.64(8) ? C4 C5 C6 . . . 126.55(10) ? C4 C5 H5 . . . 116.72 ? C6 C5 H5 . . . 116.72 ? C5 C6 C7 . . . 177.07(12) ? Si C7 C6 . . . 174.42(12) ? Si C8 H81 . . . 109.47 ? Si C8 H82 . . . 109.47 ? Si C8 H83 . . . 109.47 ? H81 C8 H82 . . . 109.47 ? H81 C8 H83 . . . 109.47 ? H82 C8 H83 . . . 109.47 ? Si C9 H91 . . . 109.47 ? Si C9 H92 . . . 109.47 ? Si C9 H93 . . . 109.47 ? H91 C9 H92 . . . 109.47 ? H91 C9 H93 . . . 109.47 ? H92 C9 H93 . . . 109.47 ? Si C10 H101 . . . 109.47 ? Si C10 H102 . . . 109.47 ? Si C10 H103 . . . 109.47 ? H101 C10 H102 . . . 109.47 ? H101 C10 H103 . . . 109.47 ? H102 C10 H103 . . . 109.47 ? S C11 H111 . . . 109.47 ? S C11 H112 . . . 109.47 ? S C11 H113 . . . 109.47 ? H111 C11 H112 . . . 109.47 ? H111 C11 H113 . . . 109.47 ? H112 C11 H113 . . . 109.47 ? C7' Si' C8' . . . 106.73(6) ? C7' Si' C9' . . . 108.35(5) ? C7' Si' C10' . . . 107.73(6) ? C8' Si' C9' . . . 110.34(7) ? C8' Si' C10' . . . 111.35(7) ? C9' Si' C10' . . . 112.11(6) ? O1' S' O2' . . . 118.76(5) ? O1' S' C11' . . . 109.09(5) ? O2' S' C11' . . . 107.64(5) ? C2' C1' C3' . . 2_675 118.67(8) ? C2' C1' C4' . . . 122.30(8) ? C3' C1' C4' 2_675 . . 119.02(7) ? C1' C2' C3' . . . 120.08(8) ? C1' C2' H2' . . . 119.96 ? C3' C2' H2' . . . 119.96 ? C1' C3' C2' 2_675 . . 121.24(7) ? C1' C3' H3' 2_675 . . 119.38 ? C2' C3' H3' . . . 119.38 ? C1' C4' C5' . . . 121.44(8) ? C4' C5' C6' . . . 127.46(9) ? C4' C5' H5' . . . 116.27 ? C6' C5' H5' . . . 116.27 ? C5' C6' C7' . . . 175.09(10) ? Si' C7' C6' . . . 174.91(9) ? Si' C8' H81' . . . 109.47 ? Si' C8' H82' . . . 109.47 ? Si' C8' H83' . . . 109.47 ? H81' C8' H82' . . . 109.47 ? H81' C8' H83' . . . 109.47 ? H82' C8' H83' . . . 109.47 ? Si' C9' H91' . . . 109.47 ? Si' C9' H92' . . . 109.47 ? Si' C9' H93' . . . 109.47 ? H91' C9' H92' . . . 109.47 ? H91' C9' H93' . . . 109.47 ? H92' C9' H93' . . . 109.47 ? Si' C10' H101' . . . 109.47 ? Si' C10' H102' . . . 109.47 ? Si' C10' H103' . . . 109.47 ? H101' C10' H102' . . . 109.47 ? H101' C10' H103' . . . 109.47 ? H102' C10' H103' . . . 109.47 ? S' C11' H111' . . . 109.47 ? S' C11' H112' . . . 109.47 ? S' C11' H113' . . . 109.47 ? H111' C11' H112' . . . 109.47 ? H111' C11' H113' . . . 109.47 ? H112' C11' H113' . . . 109.47 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C11 H112 C6 . . . 0.96 2.56 3.2082(15) 124.92 ? C5' H5' O1 . . 2_565 0.96 2.57 3.3290(11) 135.63 ? C9' H93' O2 . . . 0.96 2.46 3.3938(15) 164.69 ? # start Validation Reply Form #_vrf_PLAT230_BSEMOX1 #; #PROBLEM: Hirshfeld Test Diff for Si -- C9 .. 7.7 su #RESPONSE: Hirshfeld tests are not really relevant for atoms heavier than O. #The affected TMS group is slightly disordered and features enlarged ADPs, #but nothing out of the norm. #; # end Validation Reply Form #======================================================================= data_BSEMOX2 _publcif_datablock.id '{3421d942-ae4a-47e8-bc97-5d77493da92e}' _database_code_depnum_ccdc_archive 'CCDC 928107' #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C22 H30 O4 S2 Si2' _chemical_formula_weight 478.8 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 7.3096(2) _cell_length_b 11.3935(3) _cell_length_c 18.7425(6) _cell_angle_alpha 73.167(2) _cell_angle_beta 105.319(2) _cell_angle_gamma 118.926(2) _cell_volume 1293.21(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9931 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 29.9 _cell_measurement_temperature 100 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 1.2291 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 0.323 _exptl_crystal_description plate _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.10 _exptl_crystal_size_rad ? _exptl_crystal_colour 'clear colourless' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_correction_T_min 0.81 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\w- and \f-scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 40880 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 30.15 _diffrn_reflns_theta_full 30.15 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_unetI/netI 0.0563 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 7541 _reflns_number_gt 5106 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_gt 0.0911 _refine_ls_R_factor_all 0.1083 _refine_ls_wR_factor_ref 0.0925 _refine_ls_goodness_of_fit_ref 3.05 _refine_ls_goodness_of_fit_gt 3.68 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 7541 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_number_constraints 120 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0059 _refine_ls_shift/su_mean 0.0004 _refine_diff_density_max 1.17 _refine_diff_density_min -0.70 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group S S 0.05875(11) 0.58519(9) 0.84239(5) Uani 0.0137(3) 2 1 d . . . Si Si 0.34677(17) 1.07380(11) 0.63991(6) Uani 0.0231(5) 2 1 d . . . O1 O -0.0402(3) 0.4555(2) 0.89127(13) Uani 0.0171(10) 2 1 d . . . O2 O -0.0238(3) 0.6831(3) 0.82836(14) Uani 0.0206(11) 2 1 d . . . C1 C 0.4163(4) 0.5774(3) 0.94119(17) Uani 0.0113(13) 2 1 d . . . C2 C 0.6701(4) 0.4845(3) 0.99142(17) Uani 0.0128(13) 2 1 d . . . C3 C 0.5868(4) 0.5601(3) 0.93318(18) Uani 0.0123(13) 2 1 d . . . C4 C 0.3333(5) 0.6614(3) 0.87911(18) Uani 0.0134(14) 2 1 d . . . C5 C 0.4597(5) 0.7892(3) 0.84719(18) Uani 0.0160(14) 2 1 d . . . C6 C 0.4023(5) 0.8768(4) 0.7835(2) Uani 0.0187(15) 2 1 d . . . C7 C 0.3701(6) 0.9539(4) 0.7281(2) Uani 0.0233(17) 2 1 d . . . C8 C 0.2741(7) 0.9833(5) 0.5612(2) Uani 0.039(2) 2 1 d . . . C9 C 0.6075(7) 1.2230(4) 0.6347(2) Uani 0.035(2) 2 1 d . . . C10 C 0.1367(6) 1.1221(4) 0.6386(2) Uani 0.0286(18) 2 1 d . . . C11 C 0.0579(5) 0.5521(4) 0.75641(18) Uani 0.0188(15) 2 1 d . . . S' S 1.09914(12) 1.14700(9) 0.86315(5) Uani 0.0158(4) 2 1 d . . . Si' Si 1.50574(15) 1.60457(11) 0.63339(6) Uani 0.0202(4) 2 1 d . . . O1' O 1.0614(3) 1.2400(3) 0.79758(13) Uani 0.0231(12) 2 1 d . . . O2' O 0.9548(3) 1.0041(3) 0.87028(15) Uani 0.0244(11) 2 1 d . . . C1' C 1.4276(4) 1.0780(3) 0.93697(18) Uani 0.0126(14) 2 1 d . . . C2' C 1.3188(5) 0.9351(3) 0.95048(18) Uani 0.0143(14) 2 1 d . . . C3' C 1.3920(5) 0.8588(3) 1.01280(18) Uani 0.0139(14) 2 1 d . . . C4' C 1.3610(4) 1.1657(3) 0.87148(18) Uani 0.0118(13) 2 1 d . . . C5' C 1.4969(5) 1.2632(3) 0.82560(18) Uani 0.0154(14) 2 1 d . . . C6' C 1.4746(5) 1.3676(4) 0.76498(19) Uani 0.0188(15) 2 1 d . . . C7' C 1.4862(5) 1.4606(4) 0.7130(2) Uani 0.0210(16) 2 1 d . . . C8' C 1.6173(6) 1.7619(4) 0.6715(2) Uani 0.033(2) 2 1 d . . . C9' C 1.2360(6) 1.5639(5) 0.5788(2) Uani 0.033(2) 2 1 d . . . C10' C 1.6873(6) 1.6204(5) 0.5738(2) Uani 0.032(2) 2 1 d . . . C11' C 1.1138(5) 1.2016(4) 0.94391(19) Uani 0.0218(17) 2 1 d . . . H2 H 0.788055 0.474287 0.985616 Uiso 0.0153 2 1 d . . . H3 H 0.646088 0.600945 0.88705 Uiso 0.0147 2 1 d . . . H5 H 0.605389 0.82566 0.869832 Uiso 0.0193 2 1 d . . . H81 H 0.270082 1.044763 0.513949 Uiso 0.0472 2 1 d . . . H82 H 0.377132 0.951948 0.564554 Uiso 0.0472 2 1 d . . . H83 H 0.137507 0.906594 0.564396 Uiso 0.0472 2 1 d . . . H91 H 0.604537 1.283444 0.587005 Uiso 0.0418 2 1 d . . . H92 H 0.640576 1.27022 0.674662 Uiso 0.0418 2 1 d . . . H93 H 0.713139 1.192893 0.639684 Uiso 0.0418 2 1 d . . . H101 H 0.105561 1.169144 0.58903 Uiso 0.0343 2 1 d . . . H102 H 0.011481 1.041179 0.652106 Uiso 0.0343 2 1 d . . . H103 H 0.184341 1.180776 0.674151 Uiso 0.0343 2 1 d . . . H111 H 0.120822 0.491063 0.765705 Uiso 0.0226 2 1 d . . . H112 H -0.084951 0.510848 0.731709 Uiso 0.0226 2 1 d . . . H113 H 0.137461 0.636208 0.724813 Uiso 0.0226 2 1 d . . . H2' H 1.1942 0.889906 0.916885 Uiso 0.0172 2 1 d . . . H3' H 1.317263 0.760925 1.021542 Uiso 0.0166 2 1 d . . . H5' H 1.63238 1.262986 0.83506 Uiso 0.0185 2 1 d . . . H81' H 1.64584 1.839397 0.630763 Uiso 0.0397 2 1 d . . . H82' H 1.517826 1.756454 0.698495 Uiso 0.0397 2 1 d . . . H83' H 1.746211 1.77159 0.705004 Uiso 0.0397 2 1 d . . . H91' H 1.239708 1.640788 0.539683 Uiso 0.0392 2 1 d . . . H92' H 1.189144 1.485903 0.556756 Uiso 0.0392 2 1 d . . . H93' H 1.140157 1.544048 0.611915 Uiso 0.0392 2 1 d . . . H101' H 1.674858 1.679182 0.526259 Uiso 0.0387 2 1 d . . . H102' H 1.830199 1.658436 0.598964 Uiso 0.0387 2 1 d . . . H103' H 1.65023 1.531745 0.565552 Uiso 0.0387 2 1 d . . . H111' H 1.13093 1.137093 0.988028 Uiso 0.0261 2 1 d . . . H112' H 1.232391 1.289552 0.946012 Uiso 0.0261 2 1 d . . . H113' H 0.986229 1.207961 0.941841 Uiso 0.0261 2 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S S 0.0086(3) 0.0072(4) 0.0247(4) 0.0029(3) 0.0040(3) -0.0019(3) Si Si 0.0300(5) 0.0123(6) 0.0257(5) 0.0111(4) 0.0040(4) 0.0013(4) O1 O 0.0088(10) 0.0088(14) 0.0300(13) 0.0010(9) 0.0074(9) 0.0002(10) O2 O 0.0098(10) 0.0112(14) 0.0443(15) 0.0079(10) 0.0049(10) -0.0034(11) C1 C 0.0078(12) 0.0024(17) 0.0221(16) 0.0007(11) 0.0020(12) -0.0030(12) C2 C 0.0055(12) 0.0074(18) 0.0254(17) 0.0005(11) 0.0062(12) -0.0039(13) C3 C 0.0106(13) 0.0046(17) 0.0207(16) 0.0012(12) 0.0057(12) -0.0020(13) C4 C 0.0136(14) 0.0080(18) 0.0219(17) 0.0060(13) 0.0044(12) -0.0037(13) C5 C 0.0147(14) 0.0078(19) 0.0223(17) 0.0024(13) 0.0025(13) -0.0031(13) C6 C 0.0152(15) 0.0092(19) 0.0278(19) 0.0012(13) 0.0055(13) -0.0035(14) C7 C 0.0252(18) 0.016(2) 0.0271(19) 0.0077(15) 0.0035(15) -0.0039(16) C8 C 0.058(3) 0.034(3) 0.031(2) 0.028(2) -0.004(2) -0.008(2) C9 C 0.042(2) 0.023(3) 0.038(2) 0.0170(19) 0.0097(19) 0.0056(18) C10 C 0.0240(18) 0.017(2) 0.039(2) 0.0080(16) 0.0028(16) -0.0019(17) C11 C 0.0141(15) 0.016(2) 0.0253(18) 0.0049(14) 0.0030(13) -0.0056(15) S' S 0.0087(3) 0.0083(5) 0.0290(5) 0.0037(3) 0.0036(3) -0.0010(3) Si' Si 0.0202(5) 0.0150(6) 0.0253(5) 0.0099(4) 0.0057(4) 0.0023(4) O1' O 0.0144(11) 0.0189(16) 0.0333(14) 0.0096(10) 0.0035(10) 0.0031(11) O2' O 0.0084(10) 0.0076(14) 0.0500(17) -0.0015(9) 0.0042(10) -0.0048(11) C1' C 0.0085(13) 0.0088(18) 0.0231(17) 0.0049(12) 0.0060(12) -0.0013(13) C2' C 0.0121(14) 0.0082(18) 0.0236(17) 0.0041(12) 0.0037(12) -0.0042(13) C3' C 0.0120(14) 0.0038(18) 0.0273(18) 0.0031(12) 0.0057(13) -0.0034(13) C4' C 0.0060(12) 0.0029(17) 0.0245(17) -0.0011(11) 0.0047(12) -0.0032(13) C5' C 0.0076(13) 0.0083(19) 0.0273(18) 0.0008(12) 0.0042(12) -0.0027(14) C6' C 0.0174(15) 0.015(2) 0.0237(18) 0.0063(14) 0.0047(13) -0.0029(15) C7' C 0.0206(16) 0.015(2) 0.0262(19) 0.0064(15) 0.0050(14) -0.0033(15) C8' C 0.035(2) 0.016(2) 0.043(3) 0.0102(18) 0.0093(19) 0.0006(18) C9' C 0.0269(19) 0.039(3) 0.034(2) 0.0172(19) 0.0058(17) -0.0029(19) C10' C 0.029(2) 0.033(3) 0.037(2) 0.0188(19) 0.0155(18) 0.0093(19) C11' C 0.0203(16) 0.017(2) 0.034(2) 0.0107(15) 0.0090(15) -0.0044(16) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S O1 . . 1.441(2) ? S O2 . . 1.440(3) ? S C4 . . 1.785(3) ? S C11 . . 1.756(4) ? Si C7 . . 1.843(4) ? Si C8 . . 1.860(5) ? Si C9 . . 1.844(4) ? Si C10 . . 1.858(6) ? C1 C2 . 2_667 1.402(4) ? C1 C3 . . 1.404(6) ? C1 C4 . . 1.476(5) ? C2 C3 . . 1.384(5) ? C2 H2 . . 0.96 ? C3 H3 . . 0.96 ? C4 C5 . . 1.348(4) ? C5 C6 . . 1.431(5) ? C5 H5 . . 0.96 ? C6 C7 . . 1.204(5) ? C8 H81 . . 0.96 ? C8 H82 . . 0.96 ? C8 H83 . . 0.96 ? C9 H91 . . 0.96 ? C9 H92 . . 0.96 ? C9 H93 . . 0.96 ? C10 H101 . . 0.96 ? C10 H102 . . 0.96 ? C10 H103 . . 0.96 ? C11 H111 . . 0.96 ? C11 H112 . . 0.96 ? C11 H113 . . 0.96 ? S' O1' . . 1.435(3) ? S' O2' . . 1.438(2) ? S' C4' . . 1.789(4) ? S' C11' . . 1.756(5) ? Si' C7' . . 1.845(4) ? Si' C8' . . 1.846(5) ? Si' C9' . . 1.864(4) ? Si' C10' . . 1.864(5) ? C1' C2' . . 1.401(5) ? C1' C3' . 2_877 1.401(4) ? C1' C4' . . 1.479(5) ? C2' C3' . . 1.392(5) ? C2' H2' . . 0.96 ? C3' H3' . . 0.96 ? C4' C5' . . 1.338(4) ? C5' C6' . . 1.428(5) ? C5' H5' . . 0.96 ? C6' C7' . . 1.199(5) ? C8' H81' . . 0.96 ? C8' H82' . . 0.96 ? C8' H83' . . 0.96 ? C9' H91' . . 0.96 ? C9' H92' . . 0.96 ? C9' H93' . . 0.96 ? C10' H101' . . 0.96 ? C10' H102' . . 0.96 ? C10' H103' . . 0.96 ? C11' H111' . . 0.96 ? C11' H112' . . 0.96 ? C11' H113' . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 S O2 . . . 118.43(17) ? O1 S C4 . . . 107.75(14) ? O1 S C11 . . . 107.67(17) ? O2 S C4 . . . 109.27(17) ? O2 S C11 . . . 109.62(18) ? C4 S C11 . . . 102.99(18) ? C7 Si C8 . . . 106.9(2) ? C7 Si C9 . . . 107.39(17) ? C7 Si C10 . . . 110.0(2) ? C8 Si C9 . . . 110.5(2) ? C8 Si C10 . . . 109.8(2) ? C9 Si C10 . . . 112.1(2) ? C2 C1 C3 2_667 . . 119.0(3) ? C2 C1 C4 2_667 . . 121.4(4) ? C3 C1 C4 . . . 119.5(3) ? C1 C2 C3 2_667 . . 120.6(4) ? C1 C2 H2 2_667 . . 119.72 ? C3 C2 H2 . . . 119.72 ? C1 C3 C2 . . . 120.4(3) ? C1 C3 H3 . . . 119.8 ? C2 C3 H3 . . . 119.8 ? S C4 C1 . . . 118.0(2) ? S C4 C5 . . . 119.8(3) ? C1 C4 C5 . . . 122.2(3) ? C4 C5 C6 . . . 127.6(3) ? C4 C5 H5 . . . 116.19 ? C6 C5 H5 . . . 116.19 ? C5 C6 C7 . . . 174.4(4) ? Si C7 C6 . . . 173.6(4) ? Si C8 H81 . . . 109.47 ? Si C8 H82 . . . 109.47 ? Si C8 H83 . . . 109.47 ? H81 C8 H82 . . . 109.47 ? H81 C8 H83 . . . 109.47 ? H82 C8 H83 . . . 109.47 ? Si C9 H91 . . . 109.47 ? Si C9 H92 . . . 109.47 ? Si C9 H93 . . . 109.47 ? H91 C9 H92 . . . 109.47 ? H91 C9 H93 . . . 109.47 ? H92 C9 H93 . . . 109.47 ? Si C10 H101 . . . 109.47 ? Si C10 H102 . . . 109.47 ? Si C10 H103 . . . 109.47 ? H101 C10 H102 . . . 109.47 ? H101 C10 H103 . . . 109.47 ? H102 C10 H103 . . . 109.47 ? S C11 H111 . . . 109.47 ? S C11 H112 . . . 109.47 ? S C11 H113 . . . 109.47 ? H111 C11 H112 . . . 109.47 ? H111 C11 H113 . . . 109.47 ? H112 C11 H113 . . . 109.47 ? O1' S' O2' . . . 118.59(14) ? O1' S' C4' . . . 109.15(15) ? O1' S' C11' . . . 108.9(2) ? O2' S' C4' . . . 108.57(18) ? O2' S' C11' . . . 108.30(17) ? C4' S' C11' . . . 102.14(17) ? C7' Si' C8' . . . 108.49(18) ? C7' Si' C9' . . . 107.88(16) ? C7' Si' C10' . . . 107.6(2) ? C8' Si' C9' . . . 112.4(3) ? C8' Si' C10' . . . 109.8(2) ? C9' Si' C10' . . . 110.5(2) ? C2' C1' C3' . . 2_877 118.9(3) ? C2' C1' C4' . . . 122.8(3) ? C3' C1' C4' 2_877 . . 118.3(3) ? C1' C2' C3' . . . 119.7(3) ? C1' C2' H2' . . . 120.14 ? C3' C2' H2' . . . 120.14 ? C1' C3' C2' 2_877 . . 121.4(3) ? C1' C3' H3' 2_877 . . 119.32 ? C2' C3' H3' . . . 119.32 ? S' C4' C1' . . . 116.4(2) ? S' C4' C5' . . . 121.9(3) ? C1' C4' C5' . . . 121.4(3) ? C4' C5' C6' . . . 130.9(4) ? C4' C5' H5' . . . 114.53 ? C6' C5' H5' . . . 114.53 ? C5' C6' C7' . . . 170.2(4) ? Si' C7' C6' . . . 179.6(3) ? Si' C8' H81' . . . 109.47 ? Si' C8' H82' . . . 109.47 ? Si' C8' H83' . . . 109.47 ? H81' C8' H82' . . . 109.47 ? H81' C8' H83' . . . 109.47 ? H82' C8' H83' . . . 109.47 ? Si' C9' H91' . . . 109.47 ? Si' C9' H92' . . . 109.47 ? Si' C9' H93' . . . 109.47 ? H91' C9' H92' . . . 109.47 ? H91' C9' H93' . . . 109.47 ? H92' C9' H93' . . . 109.47 ? Si' C10' H101' . . . 109.47 ? Si' C10' H102' . . . 109.47 ? Si' C10' H103' . . . 109.47 ? H101' C10' H102' . . . 109.47 ? H101' C10' H103' . . . 109.47 ? H102' C10' H103' . . . 109.47 ? S' C11' H111' . . . 109.47 ? S' C11' H112' . . . 109.47 ? S' C11' H113' . . . 109.47 ? H111' C11' H112' . . . 109.47 ? H111' C11' H113' . . . 109.47 ? H112' C11' H113' . . . 109.47 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C5 C4 C1 C2 . . . . -50.2(7) ? C5' C4' C1' C2' . . . . -128.5(4) ? C5 C4 S C11 . . . . 71.8(4) ? C5' C4' S' C11' . . . . -109.1(4) ? C9 Si C5 C4 . . . . -176.7(5) ? C9' Si' C5' C4' . . . . -29.9(5) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C5 H5 O2' . . . 0.96 2.37 3.239(3) 149.82 ? # start Validation Reply Form #_vrf_PLAT213_BSEMOX2 #; #PROBLEM: Atom O2 has ADP max/min Ratio ..... 3.6 prola #RESPONSE: The crystal structure was refined from a terrible data set of #a crystal that burst into many small fragments after a reconstructive #phase transition. #; #======================================================================= data_BSEMOX3 _publcif_datablock.id '{b87663d1-9ceb-45f2-9a7e-76ba56bdd648}' _database_code_depnum_ccdc_archive 'CCDC 927473' #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C22 H30 O4 S2 Si2' _chemical_formula_weight 478.8 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 5.7300(3) _cell_length_b 10.2961(5) _cell_length_c 10.9801(6) _cell_angle_alpha 85.9433(17) _cell_angle_beta 79.7181(16) _cell_angle_gamma 80.1150(15) _cell_volume 627.39(6) _cell_formula_units_Z 1 _cell_measurement_reflns_used 8294 _cell_measurement_theta_min 3.8 _cell_measurement_theta_max 25.5 _cell_measurement_temperature 100 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 1.2668 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 254 _exptl_absorpt_coefficient_mu 0.332 _exptl_crystal_description 'plate' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_size_rad ? _exptl_crystal_colour 'clear colourless' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.98 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\w- and \f-scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 16087 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 27.63 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_unetI/netI 0.0192 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 2909 _reflns_number_gt 2371 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_gt 0.0386 _refine_ls_R_factor_all 0.0417 _refine_ls_wR_factor_ref 0.0393 _refine_ls_goodness_of_fit_ref 2.19 _refine_ls_goodness_of_fit_gt 2.39 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 2909 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_number_constraints 60 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0154 _refine_ls_shift/su_mean 0.0021 _refine_diff_density_max 0.31 _refine_diff_density_min -0.26 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si -0.53335(7) 0.61622(4) 0.26340(4) Uani 0.01652(14) 2 1 d . . . S1 S 0.00389(7) 0.10973(3) 0.30445(4) Uani 0.01720(12) 2 1 d . . . O1 O 0.0623(2) -0.03183(10) 0.30608(11) Uani 0.0327(4) 2 1 d . . . O2 O -0.24475(19) 0.16738(12) 0.33388(11) Uani 0.0309(4) 2 1 d . . . C1 C 0.3167(2) 0.07921(13) 0.07667(13) Uani 0.0133(4) 2 1 d . . . C2 C 0.5302(2) 0.02428(13) 0.11879(14) Uani 0.0165(5) 2 1 d . . . C3 C 0.2893(3) 0.05341(13) -0.04189(13) Uani 0.0161(4) 2 1 d . . . C4 C 0.1243(2) 0.16934(13) 0.15372(13) Uani 0.0148(4) 2 1 d . . . C5 C 0.0409(3) 0.29002(14) 0.10936(15) Uani 0.0208(5) 2 1 d . . . C6 C -0.1427(3) 0.39013(15) 0.16678(15) Uani 0.0234(5) 2 1 d . . . C7 C -0.2910(3) 0.48169(15) 0.20419(16) Uani 0.0256(5) 2 1 d . . . C8 C -0.7504(3) 0.54336(18) 0.38231(19) Uani 0.0375(7) 2 1 d . . . C9 C -0.3979(3) 0.73712(15) 0.33371(16) Uani 0.0277(6) 2 1 d . . . C10 C -0.6838(3) 0.68750(15) 0.13195(16) Uani 0.0266(6) 2 1 d . . . C11 C 0.1590(3) 0.17006(18) 0.40562(15) Uani 0.0290(6) 2 1 d . . . H81 H -0.85684 0.612453 0.427929 Uiso 0.045 2 1 d . . . H82 H -0.841896 0.494259 0.342845 Uiso 0.045 2 1 d . . . H83 H -0.665055 0.485508 0.437918 Uiso 0.045 2 1 d . . . H91 H -0.5212 0.807923 0.365168 Uiso 0.0332 2 1 d . . . H92 H -0.321634 0.694388 0.400299 Uiso 0.0332 2 1 d . . . H93 H -0.280639 0.771715 0.272118 Uiso 0.0332 2 1 d . . . H101 H -0.807579 0.759634 0.15968 Uiso 0.0319 2 1 d . . . H102 H -0.567884 0.718767 0.067262 Uiso 0.0319 2 1 d . . . H103 H -0.753644 0.620997 0.100878 Uiso 0.0319 2 1 d . . . H111 H 0.327147 0.135155 0.385869 Uiso 0.0348 2 1 d . . . H112 H 0.136853 0.264631 0.397352 Uiso 0.0348 2 1 d . . . H113 H 0.098422 0.143559 0.489252 Uiso 0.0348 2 1 d . . . H2 H 0.551711 0.040378 0.200823 Uiso 0.0198 2 1 d . . . H3 H 0.142736 0.09003 -0.071188 Uiso 0.0193 2 1 d . . . H5 H 0.115514 0.312503 0.026929 Uiso 0.025 2 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Si1 Si 0.0148(2) 0.0146(2) 0.0183(2) 0.00228(15) -0.00179(17) -0.00127(16) S1 S 0.0150(2) 0.01967(19) 0.0162(2) -0.00398(14) 0.00180(15) -0.00414(14) O1 O 0.0459(8) 0.0183(6) 0.0282(7) -0.0075(5) 0.0119(6) -0.0026(5) O2 O 0.0139(6) 0.0483(7) 0.0265(7) -0.0003(5) 0.0043(5) -0.0060(5) C1 C 0.0118(7) 0.0119(6) 0.0146(8) -0.0009(5) 0.0009(6) 0.0006(5) C2 C 0.0155(7) 0.0203(7) 0.0130(8) -0.0007(6) -0.0018(6) -0.0024(6) C3 C 0.0121(7) 0.0176(7) 0.0173(8) 0.0011(5) -0.0029(6) 0.0008(6) C4 C 0.0114(7) 0.0189(7) 0.0134(7) -0.0011(5) -0.0007(6) -0.0038(6) C5 C 0.0187(8) 0.0231(8) 0.0179(8) 0.0048(6) -0.0025(7) -0.0041(6) C6 C 0.0231(8) 0.0231(8) 0.0220(9) 0.0045(6) -0.0058(7) -0.0025(6) C7 C 0.0245(9) 0.0252(8) 0.0260(9) 0.0034(7) -0.0078(7) -0.0039(7) C8 C 0.0315(10) 0.0414(10) 0.0380(12) -0.0099(8) -0.0014(8) 0.0074(8) C9 C 0.0323(10) 0.0224(8) 0.0304(10) -0.0037(7) -0.0122(8) 0.0008(7) C10 C 0.0255(9) 0.0256(8) 0.0294(10) -0.0006(7) -0.0104(7) 0.0008(7) C11 C 0.0290(9) 0.0445(10) 0.0162(9) -0.0151(8) -0.0012(7) -0.0040(7) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Si1 C7 . . 1.8478(15) ? Si1 C8 . . 1.8482(19) ? Si1 C9 . . 1.8519(19) ? Si1 C10 . . 1.8552(18) ? S1 O1 . . 1.4380(11) ? S1 O2 . . 1.4349(11) ? S1 C4 . . 1.7848(14) ? S1 C11 . . 1.746(2) ? C1 C2 . . 1.399(2) ? C1 C3 . . 1.388(2) ? C1 C4 . . 1.4898(18) ? C2 C3 . 2_655 1.3864(18) ? C2 H2 . . 0.96 ? C3 H3 . . 0.96 ? C4 C5 . . 1.3427(19) ? C5 C6 . . 1.432(2) ? C5 H5 . . 0.96 ? C6 C7 . . 1.198(2) ? C8 H81 . . 0.96 ? C8 H82 . . 0.96 ? C8 H83 . . 0.96 ? C9 H91 . . 0.96 ? C9 H92 . . 0.96 ? C9 H93 . . 0.96 ? C10 H101 . . 0.96 ? C10 H102 . . 0.96 ? C10 H103 . . 0.96 ? C11 H111 . . 0.96 ? C11 H112 . . 0.96 ? C11 H113 . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C7 Si1 C8 . . . 107.82(8) ? C7 Si1 C9 . . . 108.19(8) ? C7 Si1 C10 . . . 107.75(7) ? C8 Si1 C9 . . . 110.05(9) ? C8 Si1 C10 . . . 109.51(8) ? C9 Si1 C10 . . . 113.35(8) ? O1 S1 O2 . . . 117.83(7) ? O1 S1 C4 . . . 107.13(7) ? O1 S1 C11 . . . 109.04(8) ? O2 S1 C4 . . . 108.86(7) ? O2 S1 C11 . . . 107.91(8) ? C4 S1 C11 . . . 105.39(8) ? C2 C1 C3 . . . 118.89(12) ? C2 C1 C4 . . . 121.53(13) ? C3 C1 C4 . . . 119.51(13) ? C1 C2 C3 . . 2_655 119.90(14) ? C1 C2 H2 . . . 120.05 ? C3 C2 H2 2_655 . . 120.05 ? C1 C3 C2 . . 2_655 121.20(13) ? C1 C3 H3 . . . 119.4 ? C2 C3 H3 2_655 . . 119.4 ? S1 C4 C1 . . . 117.79(10) ? S1 C4 C5 . . . 121.46(10) ? C1 C4 C5 . . . 120.73(13) ? C4 C5 C6 . . . 129.57(14) ? C4 C5 H5 . . . 115.21 ? C6 C5 H5 . . . 115.21 ? C5 C6 C7 . . . 173.37(17) ? Si1 C7 C6 . . . 176.58(16) ? Si1 C8 H81 . . . 109.47 ? Si1 C8 H82 . . . 109.47 ? Si1 C8 H83 . . . 109.47 ? H81 C8 H82 . . . 109.47 ? H81 C8 H83 . . . 109.47 ? H82 C8 H83 . . . 109.47 ? Si1 C9 H91 . . . 109.47 ? Si1 C9 H92 . . . 109.47 ? Si1 C9 H93 . . . 109.47 ? H91 C9 H92 . . . 109.47 ? H91 C9 H93 . . . 109.47 ? H92 C9 H93 . . . 109.47 ? Si1 C10 H101 . . . 109.47 ? Si1 C10 H102 . . . 109.47 ? Si1 C10 H103 . . . 109.47 ? H101 C10 H102 . . . 109.47 ? H101 C10 H103 . . . 109.47 ? H102 C10 H103 . . . 109.47 ? S1 C11 H111 . . . 109.47 ? S1 C11 H112 . . . 109.47 ? S1 C11 H113 . . . 109.47 ? H111 C11 H112 . . . 109.47 ? H111 C11 H113 . . . 109.47 ? H112 C11 H113 . . . 109.47 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C11 H111 O2 . . 1_655 0.96 2.49 3.362(2) 150.78 ? #======================================================================= data_DSEM1 _publcif_datablock.id '{d6b6d973-fc2a-4196-8550-5f6f0e7a4ba6}' _database_code_depnum_ccdc_archive 'CCDC 1407074' #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C22 H32 O2 S3 Si2' _chemical_formula_weight 480.8 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' _space_group_IT_number 15 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y,-z+1/2 3 -x,-y,-z 4 x,-y,z+1/2 5 x+1/2,y+1/2,z 6 -x+1/2,y+1/2,-z+1/2 7 -x+1/2,-y+1/2,-z 8 x+1/2,-y+1/2,z+1/2 _cell_length_a 34.344(2) _cell_length_b 8.1665(5) _cell_length_c 20.0791(12) _cell_angle_alpha 90 _cell_angle_beta 100.532(2) _cell_angle_gamma 90 _cell_volume 5536.7(6) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9911 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 100 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 1.1533 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.369 _exptl_crystal_description 'rhombic prism' _exptl_crystal_size_max 0.87 _exptl_crystal_size_mid 0.66 _exptl_crystal_size_min 0.03 _exptl_crystal_size_rad ? _exptl_crystal_colour 'clear yellow' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.99 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\w- and \f-scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 77428 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.61 _diffrn_reflns_theta_full 27.61 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_unetI/netI 0.0185 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 6397 _reflns_number_gt 4903 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_gt 0.0580 _refine_ls_R_factor_all 0.0691 _refine_ls_wR_factor_ref 0.0588 _refine_ls_goodness_of_fit_ref 3.02 _refine_ls_goodness_of_fit_gt 3.43 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 6397 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_number_constraints 128 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0303 _refine_ls_shift/su_mean 0.0010 _refine_diff_density_max 0.87 _refine_diff_density_min -0.75 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.762685(15) -0.33644(6) 0.15507(3) Uani 0.02279(16) 8 1 d . . . S2 S 0.847992(18) -0.37717(8) 0.11586(3) Uani 0.0353(2) 8 1 d . . . S3 S 0.700129(18) -0.47388(6) 0.23712(3) Uani 0.02868(18) 8 1 d . . . Si1 Si 0.93168(2) -0.24524(14) -0.06764(4) Uani 0.0623(4) 8 1 d . . . Si2 Si 0.576085(19) -0.28110(10) 0.35009(3) Uani 0.0365(2) 8 1 d . . . O1 O 0.75965(4) 0.06737(17) 0.05109(7) Uani 0.0245(5) 8 1 d . . . O2 O 0.69334(4) 0.04163(17) 0.12397(7) Uani 0.0230(5) 8 1 d . . . C1 C 0.77861(6) -0.1981(2) 0.09999(10) Uani 0.0208(6) 8 1 d . . . C2 C 0.75376(6) -0.0650(2) 0.08999(9) Uani 0.0192(6) 8 1 d . . . C3 C 0.72162(6) -0.0764(2) 0.12477(10) Uani 0.0189(6) 8 1 d . . . C4 C 0.72227(6) -0.2160(2) 0.16354(10) Uani 0.0190(6) 8 1 d . . . C5 C 0.81443(6) -0.2305(3) 0.07343(10) Uani 0.0232(6) 8 1 d . . . C6 C 0.82130(6) -0.1636(3) 0.01512(11) Uani 0.0304(7) 8 1 d . . . C7 C 0.85643(7) -0.1883(3) -0.01190(12) Uani 0.0388(9) 8 1 d . . . C8 C 0.88601(8) -0.2089(4) -0.03517(13) Uani 0.0498(10) 8 1 d . . . C9 C 0.69553(6) -0.2693(2) 0.20742(10) Uani 0.0206(6) 8 1 d . . . C10 C 0.66931(6) -0.1683(3) 0.22935(11) Uani 0.0271(7) 8 1 d . . . C11 C 0.64076(6) -0.2167(3) 0.26906(11) Uani 0.0291(7) 8 1 d . . . C12 C 0.61537(7) -0.2474(3) 0.30132(12) Uani 0.0334(8) 8 1 d . . . C13 C 0.92858(8) -0.4492(5) -0.10887(16) Uani 0.0694(13) 8 1 d . . . C14 C 0.97377(9) -0.2385(6) 0.00601(18) Uani 0.113(2) 8 1 d . . . C15 C 0.93686(10) -0.0800(5) -0.12833(17) Uani 0.0798(15) 8 1 d . . . C16 C 0.55161(11) -0.4795(5) 0.3267(2) Uani 0.109(2) 8 1 d . . . C17 C 0.59717(11) -0.2798(5) 0.44071(15) Uani 0.0865(16) 8 1 d . . . C18 C 0.54202(12) -0.1076(6) 0.3313(3) Uani 0.141(3) 8 1 d . . . C19 C 0.86345(7) -0.2835(3) 0.19798(12) Uani 0.0383(8) 8 1 d . . . C20 C 0.67977(9) -0.5825(3) 0.16113(13) Uani 0.0438(9) 8 1 d . . . C21 C 0.77523(7) 0.2073(3) 0.09102(11) Uani 0.0314(7) 8 1 d . . . C22 C 0.67373(7) 0.0962(3) 0.05813(11) Uani 0.0364(8) 8 1 d . . . H6 H 0.80111 -0.094723 -0.009835 Uiso 0.0365 8 1 d . . . H10 H 0.66994 -0.054804 0.217203 Uiso 0.0326 8 1 d . . . H131 H 0.95267 -0.470648 -0.125182 Uiso 0.0833 8 1 d . . . H132 H 0.924798 -0.531753 -0.076613 Uiso 0.0833 8 1 d . . . H133 H 0.906657 -0.450798 -0.146167 Uiso 0.0833 8 1 d . . . H141 H 0.998379 -0.246254 -0.010028 Uiso 0.1353 8 1 d . . . H142 H 0.972955 -0.137344 0.030044 Uiso 0.1353 8 1 d . . . H143 H 0.971574 -0.328613 0.035831 Uiso 0.1353 8 1 d . . . H151 H 0.961386 -0.093158 -0.144236 Uiso 0.0958 8 1 d . . . H152 H 0.915203 -0.085166 -0.166012 Uiso 0.0958 8 1 d . . . H153 H 0.936668 0.024229 -0.106262 Uiso 0.0958 8 1 d . . . H161 H 0.527972 -0.486943 0.345649 Uiso 0.1314 8 1 d . . . H162 H 0.54488 -0.487632 0.278223 Uiso 0.1314 8 1 d . . . H163 H 0.569264 -0.566984 0.343922 Uiso 0.1314 8 1 d . . . H171 H 0.577799 -0.3191 0.465791 Uiso 0.1038 8 1 d . . . H172 H 0.620051 -0.349537 0.449095 Uiso 0.1038 8 1 d . . . H173 H 0.604711 -0.170179 0.454735 Uiso 0.1038 8 1 d . . . H181 H 0.524557 -0.104784 0.363546 Uiso 0.1688 8 1 d . . . H182 H 0.556903 -0.007503 0.334015 Uiso 0.1688 8 1 d . . . H183 H 0.526759 -0.119462 0.286476 Uiso 0.1688 8 1 d . . . H191 H 0.885998 -0.341055 0.222371 Uiso 0.0459 8 1 d . . . H192 H 0.870413 -0.171204 0.192268 Uiso 0.0459 8 1 d . . . H193 H 0.842154 -0.288535 0.222935 Uiso 0.0459 8 1 d . . . H201 H 0.682899 -0.698138 0.168924 Uiso 0.0526 8 1 d . . . H202 H 0.652125 -0.55696 0.148318 Uiso 0.0526 8 1 d . . . H203 H 0.69337 -0.550594 0.125458 Uiso 0.0526 8 1 d . . . H211 H 0.775242 0.300712 0.061981 Uiso 0.0377 8 1 d . . . H212 H 0.758994 0.229827 0.124117 Uiso 0.0377 8 1 d . . . H213 H 0.801812 0.184658 0.113548 Uiso 0.0377 8 1 d . . . H221 H 0.650937 0.160286 0.062714 Uiso 0.0437 8 1 d . . . H222 H 0.691634 0.161728 0.037863 Uiso 0.0437 8 1 d . . . H223 H 0.66555 0.002922 0.029926 Uiso 0.0437 8 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 S 0.0233(3) 0.0181(3) 0.0288(3) 0.0029(2) 0.0096(2) 0.0019(2) S2 S 0.0358(3) 0.0429(4) 0.0284(3) 0.0181(3) 0.0084(3) -0.0026(3) S3 S 0.0403(3) 0.0202(3) 0.0270(3) -0.0011(2) 0.0098(2) 0.0029(2) Si1 Si 0.0251(4) 0.1274(9) 0.0379(4) -0.0045(4) 0.0155(3) -0.0179(5) Si2 Si 0.0225(3) 0.0631(5) 0.0256(3) -0.0034(3) 0.0087(3) 0.0024(3) O1 O 0.0343(9) 0.0214(8) 0.0185(7) -0.0011(6) 0.0065(6) 0.0015(6) O2 O 0.0272(8) 0.0221(7) 0.0199(7) 0.0080(6) 0.0050(6) 0.0005(6) C1 C 0.0236(11) 0.0210(10) 0.0188(10) -0.0023(8) 0.0065(8) -0.0018(8) C2 C 0.0230(10) 0.0187(10) 0.0158(9) -0.0017(8) 0.0036(8) -0.0008(7) C3 C 0.0209(10) 0.0167(10) 0.0187(10) 0.0028(8) 0.0029(8) -0.0040(7) C4 C 0.0198(10) 0.0157(9) 0.0219(10) 0.0013(8) 0.0053(8) -0.0023(8) C5 C 0.0215(10) 0.0260(11) 0.0222(10) 0.0021(8) 0.0048(8) -0.0048(8) C6 C 0.0233(11) 0.0416(14) 0.0277(12) 0.0035(10) 0.0085(9) 0.0025(10) C7 C 0.0333(13) 0.0565(17) 0.0287(12) 0.0014(12) 0.0114(11) 0.0018(11) C8 C 0.0328(14) 0.087(2) 0.0324(14) 0.0036(14) 0.0133(12) 0.0011(14) C9 C 0.0219(10) 0.0182(10) 0.0220(10) -0.0037(8) 0.0044(8) -0.0019(8) C10 C 0.0263(11) 0.0240(11) 0.0334(12) -0.0017(9) 0.0113(10) -0.0004(9) C11 C 0.0233(11) 0.0330(12) 0.0316(12) -0.0022(9) 0.0064(10) -0.0033(10) C12 C 0.0257(12) 0.0442(14) 0.0315(12) -0.0034(10) 0.0083(10) -0.0037(10) C13 C 0.0343(16) 0.121(3) 0.056(2) 0.0095(18) 0.0157(15) -0.010(2) C14 C 0.0346(18) 0.230(6) 0.070(3) 0.016(3) -0.0005(18) -0.052(3) C15 C 0.063(2) 0.120(3) 0.068(2) -0.037(2) 0.0413(19) -0.026(2) C16 C 0.092(3) 0.161(4) 0.095(3) -0.092(3) 0.070(3) -0.069(3) C17 C 0.082(3) 0.142(4) 0.0323(16) -0.064(2) 0.0018(16) 0.014(2) C18 C 0.072(3) 0.183(5) 0.194(5) 0.073(3) 0.094(3) 0.114(4) C19 C 0.0388(14) 0.0396(14) 0.0339(13) -0.0006(11) -0.0002(11) -0.0007(11) C20 C 0.0666(19) 0.0259(13) 0.0400(15) -0.0086(13) 0.0129(13) -0.0067(11) C21 C 0.0432(14) 0.0250(12) 0.0254(11) -0.0099(10) 0.0047(10) 0.0032(9) C22 C 0.0367(14) 0.0426(14) 0.0267(12) 0.0163(11) -0.0026(10) -0.0031(11) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 C1 . . 1.738(2) ? S1 C4 . . 1.735(2) ? S2 C5 . . 1.769(2) ? S3 C9 . . 1.771(2) ? Si1 C8 . . 1.830(3) ? Si1 C13 . . 1.854(4) ? Si1 C14 . . 1.870(3) ? Si1 C15 . . 1.849(4) ? Si2 C12 . . 1.827(3) ? Si2 C16 . . 1.846(4) ? Si2 C17 . . 1.831(3) ? Si2 C18 . . 1.833(5) ? O1 C2 . . 1.370(2) ? O1 C21 . . 1.442(2) ? O2 C3 . . 1.366(2) ? O2 C22 . . 1.440(2) ? C1 C2 . . 1.373(3) ? C1 C5 . . 1.452(3) ? C2 C3 . . 1.413(3) ? C3 C4 . . 1.379(3) ? C4 C9 . . 1.451(3) ? C5 C6 . . 1.351(3) ? C6 C7 . . 1.424(4) ? C6 H6 . . 0.96 ? C7 C8 . . 1.205(4) ? C9 C10 . . 1.353(3) ? C10 C11 . . 1.428(3) ? C10 H10 . . 0.96 ? C11 C12 . . 1.204(4) ? C13 H131 . . 0.96 ? C13 H132 . . 0.96 ? C13 H133 . . 0.96 ? C14 H141 . . 0.96 ? C14 H142 . . 0.96 ? C14 H143 . . 0.96 ? C15 H151 . . 0.96 ? C15 H152 . . 0.96 ? C15 H153 . . 0.96 ? C16 H161 . . 0.96 ? C16 H162 . . 0.96 ? C16 H163 . . 0.96 ? C17 H171 . . 0.96 ? C17 H172 . . 0.96 ? C17 H173 . . 0.96 ? C18 H181 . . 0.96 ? C18 H182 . . 0.96 ? C18 H183 . . 0.96 ? C19 H191 . . 0.96 ? C19 H192 . . 0.96 ? C19 H193 . . 0.96 ? C20 H201 . . 0.96 ? C20 H202 . . 0.96 ? C20 H203 . . 0.96 ? C21 H211 . . 0.96 ? C21 H212 . . 0.96 ? C21 H213 . . 0.96 ? C22 H221 . . 0.96 ? C22 H222 . . 0.96 ? C22 H223 . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 S1 C4 . . . 92.54(10) ? C8 Si1 C13 . . . 108.78(14) ? C8 Si1 C14 . . . 107.60(15) ? C8 Si1 C15 . . . 107.96(16) ? C13 Si1 C14 . . . 110.63(19) ? C13 Si1 C15 . . . 111.47(16) ? C14 Si1 C15 . . . 110.27(18) ? C12 Si2 C16 . . . 110.01(16) ? C12 Si2 C17 . . . 109.58(14) ? C12 Si2 C18 . . . 106.21(18) ? C16 Si2 C17 . . . 109.70(18) ? C16 Si2 C18 . . . 112.49(18) ? C17 Si2 C18 . . . 108.8(2) ? C2 O1 C21 . . . 112.76(15) ? C3 O2 C22 . . . 116.18(16) ? S1 C1 C2 . . . 110.37(16) ? S1 C1 C5 . . . 120.10(15) ? C2 C1 C5 . . . 129.51(19) ? O1 C2 C1 . . . 123.71(19) ? O1 C2 C3 . . . 122.93(17) ? C1 C2 C3 . . . 113.35(18) ? O2 C3 C2 . . . 124.45(17) ? O2 C3 C4 . . . 121.89(19) ? C2 C3 C4 . . . 113.57(18) ? S1 C4 C3 . . . 110.14(16) ? S1 C4 C9 . . . 119.76(14) ? C3 C4 C9 . . . 130.10(18) ? S2 C5 C1 . . . 117.89(15) ? S2 C5 C6 . . . 119.30(17) ? C1 C5 C6 . . . 122.58(18) ? C5 C6 C7 . . . 124.5(2) ? C5 C6 H6 . . . 117.73 ? C7 C6 H6 . . . 117.72 ? C6 C7 C8 . . . 179.6(2) ? Si1 C8 C7 . . . 177.8(2) ? S3 C9 C4 . . . 117.38(15) ? S3 C9 C10 . . . 119.28(17) ? C4 C9 C10 . . . 123.23(18) ? C9 C10 C11 . . . 125.4(2) ? C9 C10 H10 . . . 117.3 ? C11 C10 H10 . . . 117.3 ? C10 C11 C12 . . . 175.5(2) ? Si2 C12 C11 . . . 176.6(2) ? Si1 C13 H131 . . . 109.47 ? Si1 C13 H132 . . . 109.47 ? Si1 C13 H133 . . . 109.47 ? H131 C13 H132 . . . 109.47 ? H131 C13 H133 . . . 109.47 ? H132 C13 H133 . . . 109.47 ? Si1 C14 H141 . . . 109.47 ? Si1 C14 H142 . . . 109.47 ? Si1 C14 H143 . . . 109.47 ? H141 C14 H142 . . . 109.47 ? H141 C14 H143 . . . 109.47 ? H142 C14 H143 . . . 109.47 ? Si1 C15 H151 . . . 109.47 ? Si1 C15 H152 . . . 109.47 ? Si1 C15 H153 . . . 109.47 ? H151 C15 H152 . . . 109.47 ? H151 C15 H153 . . . 109.47 ? H152 C15 H153 . . . 109.47 ? Si2 C16 H161 . . . 109.47 ? Si2 C16 H162 . . . 109.47 ? Si2 C16 H163 . . . 109.47 ? H161 C16 H162 . . . 109.47 ? H161 C16 H163 . . . 109.47 ? H162 C16 H163 . . . 109.47 ? Si2 C17 H171 . . . 109.47 ? Si2 C17 H172 . . . 109.47 ? Si2 C17 H173 . . . 109.47 ? H171 C17 H172 . . . 109.47 ? H171 C17 H173 . . . 109.47 ? H172 C17 H173 . . . 109.47 ? Si2 C18 H181 . . . 109.47 ? Si2 C18 H182 . . . 109.47 ? Si2 C18 H183 . . . 109.47 ? H181 C18 H182 . . . 109.47 ? H181 C18 H183 . . . 109.47 ? H182 C18 H183 . . . 109.47 ? H191 C19 H192 . . . 109.47 ? H191 C19 H193 . . . 109.47 ? H192 C19 H193 . . . 109.47 ? H201 C20 H202 . . . 109.47 ? H201 C20 H203 . . . 109.47 ? H202 C20 H203 . . . 109.47 ? O1 C21 H211 . . . 109.47 ? O1 C21 H212 . . . 109.47 ? O1 C21 H213 . . . 109.47 ? H211 C21 H212 . . . 109.47 ? H211 C21 H213 . . . 109.47 ? H212 C21 H213 . . . 109.47 ? O2 C22 H221 . . . 109.47 ? O2 C22 H222 . . . 109.47 ? O2 C22 H223 . . . 109.47 ? H221 C22 H222 . . . 109.47 ? H221 C22 H223 . . . 109.47 ? H222 C22 H223 . . . 109.47 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C6 H6 O1 . . . 0.96 2.43 3.020(3) 119.35 ? C10 H10 O2 . . . 0.96 2.31 2.956(3) 124.29 ? C20 H201 O2 . . 1_545 0.96 2.36 3.213(3) 147.47 ? C22 H222 O1 . . . 0.96 2.43 2.989(3) 117.04 ? # start Validation Reply Form #_vrf_PLAT220_DSEM1 #; #PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) Range 7.5 Ratio #RESPONSE: The TMS groups are disordered and therefore feature large ADPs. #Refinement as two positions did not lead to a convincing model, since ##the electron density is "smeared out". #; #_vrf_PLAT242_DSEM1 #; #PROBLEM: Low Ueq as Compared to Neighbors for ..... Si2 Check #RESPONSE: The TMS groups are disordered and therefore feature large ADPs. #Refinement as two positions did not lead to a convincing model, since #the electron density is "smeared out". #; # end Validation Reply Form #======================================================================= data_DSEM2 _publcif_datablock.id '{a2613522-21c0-4ad1-b1f4-e52d4ca08d07}' _database_code_depnum_ccdc_archive 'CCDC 1407075' #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C22 H32 O2 S3 Si2' _chemical_formula_weight 480.8 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P c c n' _space_group_name_Hall '-P -2xac;-2ybc;-2zab' _space_group_IT_number 56 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,-y+1/2,z 3 -x,y+1/2,-z+1/2 4 x+1/2,-y,-z+1/2 5 -x,-y,-z 6 x+1/2,y+1/2,-z 7 x,-y+1/2,z+1/2 8 -x+1/2,y,z+1/2 _cell_length_a 33.630(10) _cell_length_b 8.271(2) _cell_length_c 19.717(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5484(3) _cell_formula_units_Z 8 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 100 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 1.1644 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 0.373 _exptl_crystal_description 'plate' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.01 _exptl_crystal_size_rad ? _exptl_crystal_colour 'clear yellow' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 1.00 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\w- and \f-scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 48785 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.09 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_max 0.95 _diffrn_measured_fraction_theta_full 0.95 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_unetI/netI 0.0584 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 4671 _reflns_number_gt 3185 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0869 _refine_ls_wR_factor_gt 0.0816 _refine_ls_R_factor_all 0.1288 _refine_ls_wR_factor_ref 0.0848 _refine_ls_goodness_of_fit_ref 3.22 _refine_ls_goodness_of_fit_gt 3.80 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 4671 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_number_constraints 128 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0333 _refine_ls_shift/su_mean 0.0024 _refine_diff_density_max 0.75 _refine_diff_density_min -0.74 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.48577(4) 0.09321(15) 0.14925(7) Uani 0.0273(5) 8 1 d . . . S2 S 0.39846(4) 0.12563(17) 0.08590(7) Uani 0.0339(5) 8 1 d . . . S3 S 0.54950(4) 0.23657(16) 0.24996(7) Uani 0.0324(5) 8 1 d . . . Si1 Si 0.31451(5) -0.0096(2) -0.12916(9) Uani 0.0483(7) 8 1 d . . . Si2 Si 0.67503(5) 0.05745(19) 0.40475(8) Uani 0.0338(6) 8 1 d . . . O1 O 0.48893(10) -0.3104(4) 0.04701(16) Uani 0.0250(12) 8 1 d . . . O2 O 0.55614(10) -0.2785(4) 0.14069(17) Uani 0.0252(12) 8 1 d . . . C1 C 0.46915(15) -0.0466(6) 0.0899(2) Uani 0.0244(18) 8 1 d . . . C2 C 0.49443(15) -0.1789(6) 0.0886(3) Uani 0.0231(19) 8 1 d . . . C3 C 0.52739(15) -0.1644(6) 0.1323(3) Uani 0.0210(19) 8 1 d . . . C4 C 0.52700(14) -0.0247(6) 0.1699(3) Uani 0.0211(18) 8 1 d . . . C5 C 0.43223(15) -0.0187(6) 0.0531(3) Uani 0.0226(18) 8 1 d . . . C6 C 0.42494(15) -0.0889(6) -0.0068(3) Uani 0.029(2) 8 1 d . . . C7 C 0.38874(18) -0.0660(6) -0.0455(3) Uani 0.033(2) 8 1 d . . . C8 C 0.35965(17) -0.0468(7) -0.0796(3) Uani 0.041(2) 8 1 d . . . C9 C 0.55396(15) 0.0329(6) 0.2232(3) Uani 0.0253(18) 8 1 d . . . C10 C 0.58022(15) -0.0638(6) 0.2547(2) Uani 0.0252(18) 8 1 d . . . C11 C 0.60874(17) -0.0138(6) 0.3044(3) Uani 0.028(2) 8 1 d . . . C12 C 0.63440(17) 0.0188(6) 0.3452(3) Uani 0.030(2) 8 1 d . . . C13 C 0.31924(16) 0.1882(8) -0.1722(3) Uani 0.057(3) 8 1 d . . . C14 C 0.27160(19) -0.0042(10) -0.0700(3) Uani 0.081(3) 8 1 d . . . C15 C 0.3085(2) -0.1777(9) -0.1915(3) Uani 0.071(3) 8 1 d . . . C16 C 0.69045(17) 0.2734(6) 0.4004(3) Uani 0.043(2) 8 1 d . . . C17 C 0.6576(2) 0.0090(7) 0.4913(3) Uani 0.057(3) 8 1 d . . . C18 C 0.71605(17) -0.0785(7) 0.3798(3) Uani 0.053(2) 8 1 d . . . C19 C 0.38635(16) 0.0445(6) 0.1687(3) Uani 0.037(2) 8 1 d . . . C20 C 0.56987(18) 0.3393(6) 0.1773(3) Uani 0.041(2) 8 1 d . . . C21 C 0.47467(16) -0.4503(6) 0.0834(3) Uani 0.036(2) 8 1 d . . . C22 C 0.57674(17) -0.3269(6) 0.0804(3) Uani 0.038(2) 8 1 d . . . H6 H 0.444962 -0.158871 -0.025243 Uiso 0.0352 8 1 d . . . H131 H 0.29571 0.208815 -0.19842 Uiso 0.0687 8 1 d . . . H132 H 0.322489 0.271836 -0.138951 Uiso 0.0687 8 1 d . . . H133 H 0.341961 0.186495 -0.201697 Uiso 0.0687 8 1 d . . . H141 H 0.268806 -0.10753 -0.048402 Uiso 0.0977 8 1 d . . . H142 H 0.275989 0.077494 -0.036251 Uiso 0.0977 8 1 d . . . H143 H 0.247792 0.020379 -0.094857 Uiso 0.0977 8 1 d . . . H151 H 0.309192 -0.279434 -0.168071 Uiso 0.0856 8 1 d . . . H152 H 0.283513 -0.166428 -0.214506 Uiso 0.0856 8 1 d . . . H153 H 0.329762 -0.173744 -0.223974 Uiso 0.0856 8 1 d . . . H161 H 0.695035 0.302993 0.35394 Uiso 0.0514 8 1 d . . . H162 H 0.669803 0.340267 0.418941 Uiso 0.0514 8 1 d . . . H163 H 0.714449 0.28839 0.425965 Uiso 0.0514 8 1 d . . . H171 H 0.651302 -0.103932 0.494065 Uiso 0.0684 8 1 d . . . H172 H 0.678226 0.034117 0.523378 Uiso 0.0684 8 1 d . . . H173 H 0.634383 0.0718 0.501474 Uiso 0.0684 8 1 d . . . H181 H 0.707294 -0.188755 0.382646 Uiso 0.0635 8 1 d . . . H182 H 0.723928 -0.054939 0.334007 Uiso 0.0635 8 1 d . . . H183 H 0.738255 -0.062471 0.409602 Uiso 0.0635 8 1 d . . . H191 H 0.361686 0.089953 0.184054 Uiso 0.0448 8 1 d . . . H192 H 0.383856 -0.07095 0.165723 Uiso 0.0448 8 1 d . . . H193 H 0.407105 0.071353 0.200161 Uiso 0.0448 8 1 d . . . H201 H 0.567032 0.453949 0.183172 Uiso 0.0497 8 1 d . . . H202 H 0.597534 0.312722 0.172904 Uiso 0.0497 8 1 d . . . H203 H 0.5559 0.305982 0.137253 Uiso 0.0497 8 1 d . . . H211 H 0.477335 -0.544569 0.055337 Uiso 0.043 8 1 d . . . H212 H 0.490003 -0.464345 0.124056 Uiso 0.043 8 1 d . . . H213 H 0.447206 -0.435164 0.095017 Uiso 0.043 8 1 d . . . H221 H 0.597893 -0.399644 0.092121 Uiso 0.0456 8 1 d . . . H222 H 0.558545 -0.380215 0.050274 Uiso 0.0456 8 1 d . . . H223 H 0.587583 -0.233208 0.058386 Uiso 0.0456 8 1 d . . . H10 H 0.579831 -0.17635 0.242934 Uiso 0.0302 8 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 S 0.0298(8) 0.0185(8) 0.0336(9) 0.0032(7) -0.0037(7) -0.0017(7) S2 S 0.0384(9) 0.0304(9) 0.0330(10) 0.0111(7) -0.0003(8) 0.0023(8) S3 S 0.0471(9) 0.0185(8) 0.0317(9) 0.0002(7) 0.0002(8) -0.0018(7) Si1 Si 0.0301(10) 0.0838(14) 0.0309(11) 0.0011(10) -0.0020(8) 0.0117(11) Si2 Si 0.0290(9) 0.0364(10) 0.0359(11) -0.0023(8) -0.0040(8) -0.0022(8) O1 O 0.041(2) 0.017(2) 0.017(2) 0.0019(18) -0.0016(18) -0.0042(19) O2 O 0.033(2) 0.016(2) 0.027(2) 0.0061(17) 0.0010(18) -0.0045(17) C1 C 0.030(3) 0.026(3) 0.017(3) 0.001(3) 0.000(3) 0.000(3) C2 C 0.030(3) 0.022(3) 0.018(3) -0.002(3) -0.001(3) -0.004(3) C3 C 0.030(3) 0.012(3) 0.022(3) 0.002(3) 0.003(3) 0.000(3) C4 C 0.023(3) 0.019(3) 0.021(3) 0.002(2) -0.001(2) 0.002(3) C5 C 0.032(3) 0.016(3) 0.020(3) 0.004(3) 0.001(3) -0.007(3) C6 C 0.030(3) 0.031(3) 0.027(4) 0.007(3) -0.002(3) 0.005(3) C7 C 0.044(4) 0.034(4) 0.020(4) 0.003(3) 0.002(3) -0.006(3) C8 C 0.029(4) 0.055(4) 0.039(4) 0.005(3) -0.003(3) -0.003(3) C9 C 0.030(3) 0.019(3) 0.027(3) 0.001(3) -0.001(3) -0.001(3) C10 C 0.036(3) 0.022(3) 0.018(3) -0.002(3) -0.002(3) -0.006(3) C11 C 0.036(4) 0.021(3) 0.026(4) -0.002(3) 0.003(3) -0.003(3) C12 C 0.033(3) 0.027(3) 0.031(4) -0.001(3) 0.000(3) 0.002(3) C13 C 0.036(4) 0.089(5) 0.047(5) 0.017(4) -0.001(3) -0.001(4) C14 C 0.044(4) 0.145(8) 0.056(5) 0.012(5) 0.009(4) 0.017(5) C15 C 0.058(5) 0.101(6) 0.054(5) -0.027(5) -0.015(4) 0.011(4) C16 C 0.033(4) 0.052(4) 0.043(4) -0.007(3) -0.004(3) 0.002(3) C17 C 0.059(5) 0.059(4) 0.054(4) -0.019(4) -0.018(4) 0.003(4) C18 C 0.047(4) 0.051(4) 0.061(5) 0.013(4) -0.014(4) -0.011(4) C19 C 0.040(4) 0.035(4) 0.037(4) 0.002(3) 0.001(3) -0.006(3) C20 C 0.059(4) 0.029(3) 0.036(4) -0.002(3) -0.003(3) -0.001(3) C21 C 0.039(4) 0.039(4) 0.029(4) -0.012(3) 0.006(3) -0.011(3) C22 C 0.039(4) 0.037(4) 0.038(4) 0.011(3) 0.006(3) 0.001(3) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 C1 . . 1.742(5) ? S1 C4 . . 1.747(5) ? S2 C5 . . 1.774(5) ? S3 C9 . . 1.777(5) ? Si1 C8 . . 1.835(6) ? Si1 C13 . . 1.855(7) ? Si1 C14 . . 1.860(7) ? Si1 C15 . . 1.870(7) ? Si2 C12 . . 1.834(6) ? Si2 C16 . . 1.867(6) ? Si2 C17 . . 1.852(6) ? Si2 C18 . . 1.852(6) ? O1 C2 . . 1.378(6) ? O1 C21 . . 1.447(6) ? O2 C3 . . 1.364(6) ? O2 C22 . . 1.435(6) ? C1 C2 . . 1.390(7) ? C1 C5 . . 1.460(7) ? C2 C3 . . 1.412(7) ? C3 C4 . . 1.375(7) ? C4 C9 . . 1.470(7) ? C5 C6 . . 1.341(7) ? C6 C7 . . 1.452(8) ? C6 H6 . . 0.96 ? C7 C8 . . 1.200(8) ? C9 C10 . . 1.347(7) ? C10 C11 . . 1.435(7) ? C10 H10 . . 0.96 ? C11 C12 . . 1.212(8) ? C13 H131 . . 0.96 ? C13 H132 . . 0.96 ? C13 H133 . . 0.96 ? C14 H141 . . 0.96 ? C14 H142 . . 0.96 ? C14 H143 . . 0.96 ? C15 H151 . . 0.96 ? C15 H152 . . 0.96 ? C15 H153 . . 0.96 ? C16 H161 . . 0.96 ? C16 H162 . . 0.96 ? C16 H163 . . 0.96 ? C17 H171 . . 0.96 ? C17 H172 . . 0.96 ? C17 H173 . . 0.96 ? C18 H181 . . 0.96 ? C18 H182 . . 0.96 ? C18 H183 . . 0.96 ? C19 H191 . . 0.96 ? C19 H192 . . 0.96 ? C19 H193 . . 0.96 ? C20 H201 . . 0.96 ? C20 H202 . . 0.96 ? C20 H203 . . 0.96 ? C21 H211 . . 0.96 ? C21 H212 . . 0.96 ? C21 H213 . . 0.96 ? C22 H221 . . 0.96 ? C22 H222 . . 0.96 ? C22 H223 . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 S1 C4 . . . 92.3(2) ? C8 Si1 C13 . . . 108.8(3) ? C8 Si1 C14 . . . 108.3(3) ? C8 Si1 C15 . . . 108.4(3) ? C13 Si1 C14 . . . 109.4(3) ? C13 Si1 C15 . . . 111.5(3) ? C14 Si1 C15 . . . 110.5(3) ? C12 Si2 C16 . . . 110.2(2) ? C12 Si2 C17 . . . 108.6(3) ? C12 Si2 C18 . . . 106.3(3) ? C16 Si2 C17 . . . 109.9(3) ? C16 Si2 C18 . . . 111.4(3) ? C17 Si2 C18 . . . 110.5(3) ? C2 O1 C21 . . . 112.5(4) ? C3 O2 C22 . . . 115.9(4) ? S1 C1 C2 . . . 109.9(4) ? S1 C1 C5 . . . 120.2(4) ? C2 C1 C5 . . . 129.8(5) ? O1 C2 C1 . . . 123.5(4) ? O1 C2 C3 . . . 122.5(4) ? C1 C2 C3 . . . 113.9(5) ? O2 C3 C2 . . . 125.0(4) ? O2 C3 C4 . . . 121.7(4) ? C2 C3 C4 . . . 113.2(4) ? S1 C4 C3 . . . 110.7(4) ? S1 C4 C9 . . . 118.5(4) ? C3 C4 C9 . . . 130.8(5) ? S2 C5 C1 . . . 118.2(4) ? S2 C5 C6 . . . 119.8(4) ? C1 C5 C6 . . . 121.8(5) ? C5 C6 C7 . . . 124.2(5) ? C5 C6 H6 . . . 117.92 ? C7 C6 H6 . . . 117.91 ? C6 C7 C8 . . . 177.6(6) ? Si1 C8 C7 . . . 177.4(5) ? S3 C9 C4 . . . 118.0(4) ? S3 C9 C10 . . . 118.9(4) ? C4 C9 C10 . . . 123.0(4) ? C9 C10 C11 . . . 125.8(5) ? C9 C10 H10 . . . 117.09 ? C11 C10 H10 . . . 117.1 ? C10 C11 C12 . . . 175.3(6) ? Si2 C12 C11 . . . 176.4(5) ? Si1 C13 H131 . . . 109.47 ? Si1 C13 H132 . . . 109.47 ? Si1 C13 H133 . . . 109.47 ? H131 C13 H132 . . . 109.47 ? H131 C13 H133 . . . 109.47 ? H132 C13 H133 . . . 109.47 ? Si1 C14 H141 . . . 109.47 ? Si1 C14 H142 . . . 109.47 ? Si1 C14 H143 . . . 109.47 ? H141 C14 H142 . . . 109.47 ? H141 C14 H143 . . . 109.47 ? H142 C14 H143 . . . 109.47 ? Si1 C15 H151 . . . 109.47 ? Si1 C15 H152 . . . 109.47 ? Si1 C15 H153 . . . 109.47 ? H151 C15 H152 . . . 109.47 ? H151 C15 H153 . . . 109.47 ? H152 C15 H153 . . . 109.47 ? Si2 C16 H161 . . . 109.47 ? Si2 C16 H162 . . . 109.47 ? Si2 C16 H163 . . . 109.47 ? H161 C16 H162 . . . 109.47 ? H161 C16 H163 . . . 109.47 ? H162 C16 H163 . . . 109.47 ? Si2 C17 H171 . . . 109.47 ? Si2 C17 H172 . . . 109.47 ? Si2 C17 H173 . . . 109.47 ? H171 C17 H172 . . . 109.47 ? H171 C17 H173 . . . 109.47 ? H172 C17 H173 . . . 109.47 ? Si2 C18 H181 . . . 109.47 ? Si2 C18 H182 . . . 109.47 ? Si2 C18 H183 . . . 109.47 ? H181 C18 H182 . . . 109.47 ? H181 C18 H183 . . . 109.47 ? H182 C18 H183 . . . 109.47 ? H191 C19 H192 . . . 109.47 ? H191 C19 H193 . . . 109.47 ? H192 C19 H193 . . . 109.47 ? H201 C20 H202 . . . 109.47 ? H201 C20 H203 . . . 109.47 ? H202 C20 H203 . . . 109.47 ? O1 C21 H211 . . . 109.47 ? O1 C21 H212 . . . 109.47 ? O1 C21 H213 . . . 109.47 ? H211 C21 H212 . . . 109.47 ? H211 C21 H213 . . . 109.47 ? H212 C21 H213 . . . 109.47 ? O2 C22 H221 . . . 109.47 ? O2 C22 H222 . . . 109.47 ? O2 C22 H223 . . . 109.47 ? H221 C22 H222 . . . 109.47 ? H221 C22 H223 . . . 109.47 ? H222 C22 H223 . . . 109.47 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C5 C1 S1 . . . . 157.1(4) ? C10 C9 C4 S1 . . . . 162.7(4) ? C6 C5 C9 C10 . . . . -51.4(7) ? C16 Si2 C10 C9 . . . . -22.1(5) ? C15 Si1 C6 C5 . . . . -160.8(4) ? C10 C9 S3 C20 . . . . 111.2(5) ? C6 C5 S2 C19 . . . . 124.7(4) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C6 H6 O1 . . . 0.96 2.41 3.026(6) 121.42 ? C20 H201 O2 . . 1_565 0.96 2.40 3.283(6) 152.38 ? C22 H222 O1 . . . 0.96 2.42 3.035(7) 121.43 ? C10 H10 O2 . . . 0.96 2.33 2.983(6) 124.64 ? # start Validation Reply Form #_vrf_PLAT029_DSEM2 #; #PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.950 Note #RESPONSE: The diffraction data was collected from a very badly diffracting #crystal with severe arking of reflections. 95% up to 2theta=50 is #unfortunately the best we could achieve. #; # end Validation Reply Form #======================================================================= data_ESEM _publcif_datablock.id '{d2cdb962-33e0-412d-984c-7ec7759e844c}' _database_code_depnum_ccdc_archive 'CCDC 1407076' #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C22 H30 O2 S3 Si2' _chemical_formula_weight 478.8 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_ssg_name 'C2/c(0\b0)s0' loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2,-x3+1/2,x4+1/2 3 -x1,-x2,-x3,-x4 4 x1,-x2,x3+1/2,-x4+1/2 5 x1+1/2,x2+1/2,x3,x4 6 -x1+1/2,x2+1/2,-x3+1/2,x4+1/2 7 -x1+1/2,-x2+1/2,-x3,-x4 8 x1+1/2,-x2+1/2,x3+1/2,-x4+1/2 _cell_length_a 31.8766(8) _cell_length_b 8.4003(5) _cell_length_c 10.0737(3) _cell_angle_alpha 90 _cell_angle_beta 95.684(2) _cell_angle_gamma 90 _cell_volume 2684.20(19) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.000000 0.6223(1) 0.000000 _cell_formula_units_Z 4 _cell_measurement_reflns_used 9719 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 100 _exptl_crystal_type_of_structure mod _exptl_crystal_density_diffrn 1.1845 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.38 _exptl_crystal_description plate _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.02 _exptl_crystal_size_rad ? _exptl_crystal_colour 'translucent colourless' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.99 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\w- and \f-scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 55245 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 1 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_unetI/netI 0.0421 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_index_m_1_min -2 _diffrn_reflns_limit_index_m_1_max 2 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 15382 _reflns_number_gt 9184 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_gt 0.0639 _refine_ls_R_factor_all 0.1097 _refine_ls_wR_factor_ref 0.0669 _refine_ls_goodness_of_fit_ref 2.36 _refine_ls_goodness_of_fit_gt 2.95 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 15382 _refine_ls_number_parameters 510 _refine_ls_number_restraints 0 _refine_ls_number_constraints 240 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0381 _refine_ls_shift/su_mean 0.0029 _refine_diff_density_max ? _refine_diff_density_min ? _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _reflns_class_code _reflns_class_description _reflns_class_number_total _reflns_class_number_gt _reflns_class_R_factor_gt _reflns_class_wR_factor_all Main 'Main reflections' 3080 2307 0.0587 0.0647 Sat1 '1st-order satellites' 6156 4248 0.0478 0.0491 Sat2 '2nd-order satellites' 6146 2629 0.1135 0.1271 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0 0.26212(6) 0.25 Uani 0.01692(15) 4 1 d . . . S2 S -0.079300(12) 0.15970(5) 0.04835(4) Uani 0.02685(13) 8 1 d . . . Si1 Si -0.178225(14) 0.34532(7) -0.36777(4) Uani 0.0400(2) 8 1 d . . . O1 O -0.03133(3) 0.68766(10) 0.13596(9) Uani 0.0225(3) 8 1 d . . . C1 C -0.01556(4) 0.55252(15) 0.19492(13) Uani 0.0159(4) 8 1 d . . . C2 C -0.02805(4) 0.40346(15) 0.15338(13) Uani 0.0154(4) 8 1 d . . . C3 C -0.06011(4) 0.35709(16) 0.04821(13) Uani 0.0175(4) 8 1 d . . . C4 C -0.07411(4) 0.45644(17) -0.05240(13) Uani 0.0206(4) 8 1 d . . . C5 C -0.10659(4) 0.41709(17) -0.15475(13) Uani 0.0230(5) 8 1 d . . . C6 C -0.13386(5) 0.38950(18) -0.24273(14) Uani 0.0291(5) 8 1 d . . . C7 C -0.20045(5) 0.5371(2) -0.43255(17) Uani 0.0568(7) 8 1 d . . . C8 C -0.15937(5) 0.2264(2) -0.50418(16) Uani 0.0416(6) 8 1 d . . . C9 C -0.21754(6) 0.2311(3) -0.28318(18) Uani 0.0725(9) 8 1 d . . . C10 C -0.10471(5) 0.15544(18) 0.20176(15) Uani 0.0361(6) 8 1 d . . . C11 C -0.02212(5) 0.82448(17) 0.22074(13) Uani 0.0297(6) 8 1 d . . . H41 H -0.061396 0.559597 -0.055019 Uiso 0.0247 8 1 d . . . H71 H -0.223724 0.516942 -0.498125 Uiso 0.0681 8 1 d . . . H72 H -0.20993 0.597485 -0.360628 Uiso 0.0681 8 1 d . . . H73 H -0.179162 0.595831 -0.472347 Uiso 0.0681 8 1 d . . . H81 H -0.18251 0.203239 -0.569385 Uiso 0.0499 8 1 d . . . H82 H -0.138361 0.285344 -0.545007 Uiso 0.0499 8 1 d . . . H83 H -0.147471 0.128905 -0.468841 Uiso 0.0499 8 1 d . . . H91 H -0.241198 0.206115 -0.345991 Uiso 0.087 8 1 d . . . H92 H -0.204992 0.134626 -0.247784 Uiso 0.087 8 1 d . . . H93 H -0.226776 0.293559 -0.21198 Uiso 0.087 8 1 d . . . H101 H -0.116554 0.052132 0.212829 Uiso 0.0434 8 1 d . . . H102 H -0.08439 0.178181 0.275932 Uiso 0.0434 8 1 d . . . H103 H -0.126624 0.233744 0.197577 Uiso 0.0434 8 1 d . . . H111 H -0.040197 0.824805 0.29104 Uiso 0.0357 8 1 d . . . H112 H -0.02767 0.919093 0.169459 Uiso 0.0357 8 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 S 0.0241(3) 0.0083(2) 0.0167(2) 0 -0.00617(19) 0 S2 S 0.0371(2) 0.0242(2) 0.01787(18) -0.01195(18) -0.00438(16) 0.00017(16) Si1 Si 0.0195(2) 0.0817(5) 0.0177(2) -0.0028(3) -0.00384(17) 0.0027(3) O1 O 0.0367(6) 0.0095(5) 0.0202(5) 0.0052(4) -0.0019(4) 0.0022(4) C1 C 0.0221(7) 0.0097(7) 0.0163(7) 0.0039(5) 0.0029(5) 0.0027(6) C2 C 0.0184(7) 0.0135(7) 0.0138(6) 0.0019(5) -0.0004(5) 0.0034(5) C3 C 0.0192(7) 0.0168(7) 0.0162(7) 0.0001(6) 0.0000(5) 0.0004(5) C4 C 0.0188(7) 0.0227(8) 0.0196(7) -0.0010(6) -0.0016(6) 0.0037(6) C5 C 0.0222(8) 0.0287(9) 0.0179(7) 0.0000(6) 0.0014(6) 0.0065(6) C6 C 0.0229(8) 0.0435(11) 0.0205(8) -0.0023(7) -0.0003(6) 0.0074(7) C7 C 0.0401(11) 0.0927(16) 0.0353(10) 0.0268(11) -0.0078(8) -0.0109(10) C8 C 0.0378(11) 0.0533(12) 0.0325(9) -0.0025(9) -0.0030(8) -0.0013(8) C9 C 0.0449(12) 0.137(2) 0.0352(11) -0.0458(13) 0.0010(9) -0.0069(12) C10 C 0.0402(10) 0.0370(10) 0.0316(9) -0.0152(8) 0.0056(7) 0.0030(7) C11 C 0.0556(12) 0.0091(8) 0.0238(8) 0.0060(7) 0.0002(7) -0.0001(6) loop_ _atom_site_Fourier_wave_vector_seq_id _jana_atom_site_Fourier_wave_vector_q1_coeff 1 1 2 2 loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id S1x1 S1 x 1 S1y1 S1 y 1 S1z1 S1 z 1 S1x2 S1 x 2 S1y2 S1 y 2 S1z2 S1 z 2 S2x1 S2 x 1 S2y1 S2 y 1 S2z1 S2 z 1 S2x2 S2 x 2 S2y2 S2 y 2 S2z2 S2 z 2 Si1x1 Si1 x 1 Si1y1 Si1 y 1 Si1z1 Si1 z 1 Si1x2 Si1 x 2 Si1y2 Si1 y 2 Si1z2 Si1 z 2 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O1x2 O1 x 2 O1y2 O1 y 2 O1z2 O1 z 2 C1x1 C1 x 1 C1y1 C1 y 1 C1z1 C1 z 1 C1x2 C1 x 2 C1y2 C1 y 2 C1z2 C1 z 2 C2x1 C2 x 1 C2y1 C2 y 1 C2z1 C2 z 1 C2x2 C2 x 2 C2y2 C2 y 2 C2z2 C2 z 2 C3x1 C3 x 1 C3y1 C3 y 1 C3z1 C3 z 1 C3x2 C3 x 2 C3y2 C3 y 2 C3z2 C3 z 2 C4x1 C4 x 1 C4y1 C4 y 1 C4z1 C4 z 1 C4x2 C4 x 2 C4y2 C4 y 2 C4z2 C4 z 2 C5x1 C5 x 1 C5y1 C5 y 1 C5z1 C5 z 1 C5x2 C5 x 2 C5y2 C5 y 2 C5z2 C5 z 2 C6x1 C6 x 1 C6y1 C6 y 1 C6z1 C6 z 1 C6x2 C6 x 2 C6y2 C6 y 2 C6z2 C6 z 2 C7x1 C7 x 1 C7y1 C7 y 1 C7z1 C7 z 1 C7x2 C7 x 2 C7y2 C7 y 2 C7z2 C7 z 2 C8x1 C8 x 1 C8y1 C8 y 1 C8z1 C8 z 1 C8x2 C8 x 2 C8y2 C8 y 2 C8z2 C8 z 2 C9x1 C9 x 1 C9y1 C9 y 1 C9z1 C9 z 1 C9x2 C9 x 2 C9y2 C9 y 2 C9z2 C9 z 2 C10x1 C10 x 1 C10y1 C10 y 1 C10z1 C10 z 1 C10x2 C10 x 2 C10y2 C10 y 2 C10z2 C10 z 2 C11x1 C11 x 1 C11y1 C11 y 1 C11z1 C11 z 1 C11x2 C11 x 2 C11y2 C11 y 2 C11z2 C11 z 2 H41x1 H41 x 1 H41y1 H41 y 1 H41z1 H41 z 1 H41x2 H41 x 2 H41y2 H41 y 2 H41z2 H41 z 2 H71x1 H71 x 1 H71y1 H71 y 1 H71z1 H71 z 1 H71x2 H71 x 2 H71y2 H71 y 2 H71z2 H71 z 2 H72x1 H72 x 1 H72y1 H72 y 1 H72z1 H72 z 1 H72x2 H72 x 2 H72y2 H72 y 2 H72z2 H72 z 2 H73x1 H73 x 1 H73y1 H73 y 1 H73z1 H73 z 1 H73x2 H73 x 2 H73y2 H73 y 2 H73z2 H73 z 2 H81x1 H81 x 1 H81y1 H81 y 1 H81z1 H81 z 1 H81x2 H81 x 2 H81y2 H81 y 2 H81z2 H81 z 2 H82x1 H82 x 1 H82y1 H82 y 1 H82z1 H82 z 1 H82x2 H82 x 2 H82y2 H82 y 2 H82z2 H82 z 2 H83x1 H83 x 1 H83y1 H83 y 1 H83z1 H83 z 1 H83x2 H83 x 2 H83y2 H83 y 2 H83z2 H83 z 2 H91x1 H91 x 1 H91y1 H91 y 1 H91z1 H91 z 1 H91x2 H91 x 2 H91y2 H91 y 2 H91z2 H91 z 2 H92x1 H92 x 1 H92y1 H92 y 1 H92z1 H92 z 1 H92x2 H92 x 2 H92y2 H92 y 2 H92z2 H92 z 2 H93x1 H93 x 1 H93y1 H93 y 1 H93z1 H93 z 1 H93x2 H93 x 2 H93y2 H93 y 2 H93z2 H93 z 2 H101x1 H101 x 1 H101y1 H101 y 1 H101z1 H101 z 1 H101x2 H101 x 2 H101y2 H101 y 2 H101z2 H101 z 2 H102x1 H102 x 1 H102y1 H102 y 1 H102z1 H102 z 1 H102x2 H102 x 2 H102y2 H102 y 2 H102z2 H102 z 2 H103x1 H103 x 1 H103y1 H103 y 1 H103z1 H103 z 1 H103x2 H103 x 2 H103y2 H103 y 2 H103z2 H103 z 2 H111x1 H111 x 1 H111y1 H111 y 1 H111z1 H111 z 1 H111x2 H111 x 2 H111y2 H111 y 2 H111z2 H111 z 2 H112x1 H112 x 1 H112y1 H112 y 1 H112z1 H112 z 1 H112x2 H112 x 2 H112y2 H112 y 2 H112z2 H112 z 2 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin S1x1 -0.00965(2) -0.00043(2) S1y1 0 0 S1z1 0.00596(6) -0.00628(6) S1x2 0 0 S1y2 0.00020(8) -0.00126(8) S1z2 0 0 S2x1 -0.008793(18) 0.004593(17) S2y1 0.01063(6) -0.03842(6) S2z1 -0.00063(5) -0.00333(5) S2x2 -0.00045(2) -0.00056(2) S2y2 -0.00006(7) -0.00004(7) S2z2 -0.00010(7) 0.00006(7) Si1x1 -0.002610(19) -0.004628(19) Si1y1 0.04816(10) -0.05186(10) Si1z1 0.00531(6) -0.00467(6) Si1x2 -0.00038(2) -0.00027(2) Si1y2 0.00594(10) 0.00008(12) Si1z2 0.00057(8) -0.00094(8) O1x1 0.01419(4) 0.00257(4) O1y1 0.01347(13) 0.01255(13) O1z1 0.00949(12) 0.01018(11) O1x2 0.00003(5) 0.00022(5) O1y2 -0.00030(15) -0.00073(15) O1z2 0.00027(16) -0.00001(17) C1x1 0.00795(6) -0.00613(6) C1y1 0.00898(19) 0.00188(19) C1z1 0.01183(17) 0.00360(16) C1x2 0.00006(7) 0.00021(7) C1y2 0.0000(2) 0.0008(2) C1z2 -0.0005(2) 0.0002(2) C2x1 -0.00255(5) -0.00726(5) C2y1 0.01543(19) -0.00525(18) C2z1 0.00984(16) -0.00272(15) C2x2 0.00021(7) 0.00003(6) C2y2 0.0006(2) 0.0003(2) C2z2 -0.0009(2) 0.0002(2) C3x1 -0.00522(5) -0.00562(5) C3y1 0.0292(2) -0.0168(2) C3z1 0.00859(16) -0.00493(16) C3x2 0.00033(5) -0.00025(5) C3y2 0.00056(19) -0.0003(2) C3z2 0.0000(2) -0.0003(2) C4x1 -0.00075(5) -0.00752(6) C4y1 0.0438(2) -0.0049(2) C4z1 0.01441(16) -0.00164(16) C4x2 0.00019(7) -0.00028(7) C4y2 -0.0005(3) 0.0019(3) C4z2 -0.0009(2) 0.0007(3) C5x1 -0.00268(6) -0.00690(6) C5y1 0.0562(3) -0.0160(2) C5z1 0.01319(18) -0.00409(18) C5x2 0.00048(7) -0.00057(7) C5y2 0.0012(3) 0.0014(3) C5z2 0.0007(3) 0.0004(3) C6x1 -0.00337(6) -0.00575(6) C6y1 0.0612(3) -0.0290(3) C6z1 0.01143(19) -0.00516(19) C6x2 -0.00016(5) -0.00023(5) C6y2 0.0061(2) 0.0010(2) C6z2 0.00087(18) -0.00092(18) C7x1 0.00465(7) -0.00715(7) C7y1 0.0705(3) -0.0115(3) C7z1 -0.0032(2) -0.0112(2) C7x2 0.00047(7) 0.00026(7) C7y2 0.0002(2) 0.0066(2) C7z2 0.0011(2) -0.0005(2) C8x1 -0.00064(6) -0.00274(7) C8y1 0.0116(3) -0.0571(3) C8z1 0.0137(2) -0.0129(2) C8x2 -0.00035(6) 0.00050(6) C8y2 0.0029(2) -0.0026(2) C8z2 0.0014(2) -0.0010(2) C9x1 -0.00465(7) 0.00014(7) C9y1 0.0255(4) -0.0792(4) C9z1 0.0027(2) -0.0043(2) C9x2 -0.00104(7) 0.00028(7) C9y2 0.0043(3) -0.0059(3) C9z2 -0.0010(2) 0.0001(2) C10x1 -0.01032(7) 0.00696(7) C10y1 0.0125(2) -0.0474(3) C10z1 -0.00396(19) 0.00019(19) C10x2 -0.00043(6) -0.00036(5) C10y2 -0.0005(2) -0.0007(3) C10z2 0.0000(3) 0.0008(2) C11x1 0.01311(8) 0.01591(8) C11y1 0.0041(2) 0.0136(2) C11z1 0.00359(19) 0.01431(19) C11x2 -0.00012(2) 0.00007(2) C11y2 0.00155(18) -0.00147(18) C11z2 0.00006(8) -0.00002(8) H41x1 0.0044 -0.0068 H41y1 0.0387 0.0122 H41z1 0.018 0.006 H41x2 0.0005 -0.0002 H41y2 -0.0023 0.0011 H41z2 -0.0021 0 H71x1 0.0048 -0.0068 H71y1 0.0694 -0.0248 H71z1 -0.0067 -0.0117 H71x2 0.0005 0.0001 H71y2 0.0014 0.007 H71z2 0.0008 -0.0005 H72x1 0.0061 -0.0073 H72y1 0.0766 0.0097 H72z1 -0.0036 -0.0164 H72x2 0.0003 0.0006 H72y2 -0.0031 0.007 H72z2 0.0014 -0.0004 H73x1 0.0077 -0.0059 H73y1 0.0646 0.004 H73z1 0.0009 -0.0121 H73x2 0.0003 0.0007 H73y2 -0.0025 0.0048 H73z2 0.0015 0.0001 H81x1 0.0004 -0.0032 H81y1 -0.0014 -0.0612 H81z1 0.01 -0.0113 H81x2 -0.0001 0.0007 H81y2 0.0025 -0.003 H81z2 0.001 -0.0016 H82x1 0.0008 -0.0045 H82y1 0.0217 -0.0457 H82z1 0.0177 -0.011 H82x2 -0.0003 0.0004 H82y2 0.0028 -0.0006 H82z2 0.0016 0.0001 H83x1 -0.0005 -0.0003 H83y1 -0.006 -0.057 H83z1 0.0134 -0.0234 H83x2 0 0.0009 H83y2 0.0002 -0.0038 H83z2 0.0007 -0.0024 H91x1 -0.0037 0.0004 H91y1 0.011 -0.0851 H91z1 0.0009 -0.0026 H91x2 -0.001 0.0004 H91y2 0.004 -0.0067 H91z2 -0.0011 0.0007 H92x1 -0.0034 0.0036 H92y1 -0.0014 -0.0822 H92z1 0.0062 -0.0097 H92x2 -0.0007 0.0012 H92y2 -0.0012 -0.0069 H92z2 -0.001 0.0004 H93x1 -0.0058 -0.0017 H93y1 0.0495 -0.0737 H93z1 -0.0015 -0.0028 H93x2 -0.0011 -0.0002 H93y2 0.0069 -0.0035 H93z2 -0.0013 0 H101x1 -0.0063 0.0134 H101y1 -0.0079 -0.0528 H101z1 -0.0037 0.0047 H101x2 -0.0007 0.0001 H101y2 -0.001 0 H101z2 0.0004 0.0006 H102x1 -0.0115 0.0062 H102y1 0.0145 -0.0385 H102z1 -0.0019 -0.0025 H102x2 -0.0003 -0.0002 H102y2 -0.0007 -0.0015 H102z2 -0.0001 0.0006 H103x1 -0.0109 0.0018 H103y1 0.0304 -0.0485 H103z1 -0.0065 0.0002 H103x2 -0.0002 -0.0005 H103y2 0.0001 -0.0004 H103z2 -0.0006 0.0012 H111x1 0.0131 0.0159 H111y1 0.0086 0.0271 H111z1 0.0036 0.0143 H111x2 -0.0002 0.0002 H111y2 0.0016 -0.0014 H111z2 0.0001 0 H112x1 0.0061 0.0239 H112y1 -0.0011 0.0172 H112z1 -0.0016 0.0152 H112x2 -0.0002 0 H112y2 0.0029 0 H112z2 0.0001 -0.0001 loop_ _atom_site_U_Fourier_id _atom_site_U_Fourier_atom_site_label _atom_site_U_Fourier_tens_elem _atom_site_U_Fourier_wave_vector_seq_id S1U111 S1 U11 1 S1U221 S1 U22 1 S1U331 S1 U33 1 S1U121 S1 U12 1 S1U131 S1 U13 1 S1U231 S1 U23 1 S1U112 S1 U11 2 S1U222 S1 U22 2 S1U332 S1 U33 2 S1U122 S1 U12 2 S1U132 S1 U13 2 S1U232 S1 U23 2 S2U111 S2 U11 1 S2U221 S2 U22 1 S2U331 S2 U33 1 S2U121 S2 U12 1 S2U131 S2 U13 1 S2U231 S2 U23 1 S2U112 S2 U11 2 S2U222 S2 U22 2 S2U332 S2 U33 2 S2U122 S2 U12 2 S2U132 S2 U13 2 S2U232 S2 U23 2 Si1U111 Si1 U11 1 Si1U221 Si1 U22 1 Si1U331 Si1 U33 1 Si1U121 Si1 U12 1 Si1U131 Si1 U13 1 Si1U231 Si1 U23 1 Si1U112 Si1 U11 2 Si1U222 Si1 U22 2 Si1U332 Si1 U33 2 Si1U122 Si1 U12 2 Si1U132 Si1 U13 2 Si1U232 Si1 U23 2 O1U111 O1 U11 1 O1U221 O1 U22 1 O1U331 O1 U33 1 O1U121 O1 U12 1 O1U131 O1 U13 1 O1U231 O1 U23 1 C1U111 C1 U11 1 C1U221 C1 U22 1 C1U331 C1 U33 1 C1U121 C1 U12 1 C1U131 C1 U13 1 C1U231 C1 U23 1 C2U111 C2 U11 1 C2U221 C2 U22 1 C2U331 C2 U33 1 C2U121 C2 U12 1 C2U131 C2 U13 1 C2U231 C2 U23 1 C3U111 C3 U11 1 C3U221 C3 U22 1 C3U331 C3 U33 1 C3U121 C3 U12 1 C3U131 C3 U13 1 C3U231 C3 U23 1 C4U111 C4 U11 1 C4U221 C4 U22 1 C4U331 C4 U33 1 C4U121 C4 U12 1 C4U131 C4 U13 1 C4U231 C4 U23 1 C5U111 C5 U11 1 C5U221 C5 U22 1 C5U331 C5 U33 1 C5U121 C5 U12 1 C5U131 C5 U13 1 C5U231 C5 U23 1 C6U111 C6 U11 1 C6U221 C6 U22 1 C6U331 C6 U33 1 C6U121 C6 U12 1 C6U131 C6 U13 1 C6U231 C6 U23 1 C7U111 C7 U11 1 C7U221 C7 U22 1 C7U331 C7 U33 1 C7U121 C7 U12 1 C7U131 C7 U13 1 C7U231 C7 U23 1 C8U111 C8 U11 1 C8U221 C8 U22 1 C8U331 C8 U33 1 C8U121 C8 U12 1 C8U131 C8 U13 1 C8U231 C8 U23 1 C9U111 C9 U11 1 C9U221 C9 U22 1 C9U331 C9 U33 1 C9U121 C9 U12 1 C9U131 C9 U13 1 C9U231 C9 U23 1 C10U111 C10 U11 1 C10U221 C10 U22 1 C10U331 C10 U33 1 C10U121 C10 U12 1 C10U131 C10 U13 1 C10U231 C10 U23 1 C11U111 C11 U11 1 C11U221 C11 U22 1 C11U331 C11 U33 1 C11U121 C11 U12 1 C11U131 C11 U13 1 C11U231 C11 U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin S1U111 0 0 S1U221 0 0 S1U331 0 0 S1U121 -0.0006(3) -0.0013(3) S1U131 0 0 S1U231 0.0013(2) -0.0010(2) S1U112 0.0019(5) 0.0000(5) S1U222 0.0002(4) 0.0014(4) S1U332 0.0028(5) -0.0006(5) S1U122 0 0 S1U132 -0.0035(4) 0.0036(3) S1U232 0 0 S2U111 0.0035(3) -0.0012(3) S2U221 0.0066(3) -0.0004(3) S2U331 0.0019(2) -0.0018(2) S2U121 -0.0015(3) -0.0012(2) S2U131 -0.0009(2) 0.0021(2) S2U231 0.0003(2) -0.0008(2) S2U112 -0.0007(4) 0.0056(4) S2U222 0.0111(4) 0.0093(4) S2U332 0.0008(4) -0.0013(4) S2U122 -0.0027(3) -0.0104(3) S2U132 0.0001(3) 0.0056(3) S2U232 0.0033(3) -0.0055(3) Si1U111 0.0037(3) 0.0008(3) Si1U221 0.0328(6) 0.0247(6) Si1U331 0.0029(3) 0.0021(3) Si1U121 -0.0063(4) -0.0032(4) Si1U131 -0.0018(2) -0.0005(2) Si1U231 0.0014(4) -0.0013(4) Si1U112 0.0021(4) -0.0010(4) Si1U222 -0.0041(7) 0.0445(8) Si1U332 0.0008(5) 0.0018(5) Si1U122 0.0021(4) -0.0013(4) Si1U132 -0.0014(3) 0.0023(3) Si1U232 0.0108(4) 0.0112(5) O1U111 0.0007(9) 0.0021(10) O1U221 -0.0019(6) 0.0005(6) O1U331 -0.0002(7) 0.0004(7) O1U121 -0.0008(6) 0.0017(6) O1U131 -0.0006(7) -0.0008(7) O1U231 -0.0005(5) 0.0008(5) C1U111 0.0037(11) 0.0020(11) C1U221 -0.0022(9) 0.0000(9) C1U331 0.0013(9) -0.0003(9) C1U121 0.0003(8) 0.0007(8) C1U131 0.0013(8) -0.0003(8) C1U231 0.0000(7) 0.0003(7) C2U111 0.0017(10) 0.0006(11) C2U221 -0.0002(9) 0.0024(9) C2U331 0.0003(9) 0.0004(9) C2U121 0.0019(7) -0.0021(8) C2U131 0.0004(7) 0.0008(8) C2U231 0.0007(7) 0.0006(7) C3U111 0.0029(11) 0.0008(11) C3U221 0.0036(11) 0.0030(10) C3U331 0.0000(9) 0.0010(9) C3U121 0.0006(8) -0.0010(8) C3U131 -0.0009(8) -0.0007(8) C3U231 -0.0008(8) 0.0000(8) C4U111 0.0014(11) 0.0032(11) C4U221 0.0030(12) 0.0017(12) C4U331 0.0004(10) -0.0001(10) C4U121 0.0009(9) -0.0002(9) C4U131 -0.0009(8) 0.0017(8) C4U231 0.0010(9) 0.0004(9) C5U111 0.0021(11) 0.0007(12) C5U221 0.0015(13) 0.0046(15) C5U331 0.0007(10) 0.0016(11) C5U121 -0.0007(10) -0.0025(10) C5U131 -0.0021(9) -0.0018(9) C5U231 0.0000(10) 0.0003(10) C6U111 0.0040(12) 0.0026(12) C6U221 0.0035(15) 0.0074(17) C6U331 0.0035(11) 0.0012(11) C6U121 -0.0024(11) -0.0076(11) C6U131 -0.0033(9) -0.0023(9) C6U231 -0.0003(11) 0.0016(11) C7U111 -0.0053(15) 0.0111(16) C7U221 0.007(2) 0.037(2) C7U331 -0.0053(15) 0.0093(14) C7U121 -0.0039(16) 0.0171(16) C7U131 0.0025(12) -0.0035(12) C7U231 0.0151(15) -0.0072(15) C8U111 0.0068(13) -0.0014(14) C8U221 0.0117(18) -0.0055(18) C8U331 0.0117(14) -0.0049(13) C8U121 -0.0095(12) 0.0037(12) C8U131 -0.0026(10) -0.0010(11) C8U231 -0.0023(12) 0.0000(12) C9U111 0.0191(17) 0.0015(16) C9U221 0.058(3) 0.030(3) C9U331 0.0085(15) 0.0040(15) C9U121 -0.0316(19) -0.0115(19) C9U131 -0.0018(12) -0.0010(12) C9U231 -0.0019(19) 0.0006(18) C10U111 0.0073(15) -0.0003(15) C10U221 0.0081(15) -0.0019(15) C10U331 0.0091(12) -0.0091(12) C10U121 -0.0055(12) -0.0001(12) C10U131 0.0040(11) -0.0030(11) C10U231 -0.0036(11) 0.0006(11) C11U111 0.0047(19) 0.0045(18) C11U221 -0.0030(11) -0.0024(10) C11U331 0.0016(11) 0.0010(11) C11U121 -0.0037(12) -0.0019(11) C11U131 0.0007(13) 0.0002(12) C11U231 -0.0016(8) -0.0003(8) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_ssg_symmetry_1 _geom_bond_site_ssg_symmetry_2 _geom_bond_distance_av _geom_bond_distance_min _geom_bond_distance_max _geom_bond_publ_flag S1 C1 . . 2.554(4) 2.544(4) 2.563(4) ? S1 C1 . 2_5555 2.554(4) 2.544(4) 2.563(4) ? S1 C2 . . 1.735(4) 1.730(4) 1.741(4) ? S1 C2 . 2_5555 1.735(4) 1.730(4) 1.741(4) ? S1 C3 . . 2.778(4) 2.769(4) 2.784(4) ? S1 C3 . 2_5555 2.778(4) 2.769(4) 2.784(4) ? S1 H102 . . 3(6) 3(6) 3(6) ? S1 H102 . 2_5555 3(6) 3(6) 3(6) ? S1 H112 . 1_5455 3(2) 2.8(18) 3(3) ? S1 H112 . 2_5455 3(2) 2.8(18) 3(3) ? S2 C2 . . 2.772(4) 2.765(4) 2.777(4) ? S2 C3 . . 1.772(4) 1.764(4) 1.781(4) ? S2 C4 . . 2.708(5) 2.692(5) 2.726(5) ? S2 C10 . . 1.817(5) 1.813(5) 1.824(5) ? S2 H101 . . 2(4) 2(4) 2(4) ? S2 H102 . . 2(2) 2(2) 2(2) ? S2 H103 . . 2(5) 2(5) 2(5) ? S2 H111 . 4_5645 3(4) 3(3) 3(4) ? S2 H112 . 1_5455 3(4) 3(4) 3(5) ? Si1 C6 . . 1.839(4) 1.832(4) 1.847(4) ? Si1 C7 . . 1.858(5) 1.841(5) 1.873(5) ? Si1 C8 . . 1.853(5) 1.840(5) 1.868(5) ? Si1 C9 . . 1.854(6) 1.839(6) 1.879(6) ? Si1 H71 . . 2(4) 2(4) 2(4) ? Si1 H72 . . 2(3) 2(3) 2(3) ? Si1 H73 . . 2.4(18) 2.3(18) 2.4(18) ? Si1 H81 . . 2(2) 2.3(19) 2.4(19) ? Si1 H82 . . 2(4) 2(4) 2(4) ? Si1 H83 . . 2(3) 2(3) 2(3) ? Si1 H91 . . 2(6) 2(5) 2(6) ? Si1 H92 . . 2(3) 2(3) 2(3) ? Si1 H93 . . 2(5) 2(5) 2(5) ? O1 O1 . 2_5555 2.899(4) 2.895(4) 2.904(4) ? O1 C1 . . 1.362(5) 1.357(5) 1.366(5) ? O1 C1 . 2_5555 2.442(5) 2.436(5) 2.449(5) ? O1 C2 . . 2.410(4) 2.399(4) 2.420(4) ? O1 C4 . . 2.969(5) 2.934(5) 2.998(5) ? O1 C11 . . 1.453(4) 1.441(4) 1.460(4) ? O1 C11 . 2_5555 2.425(4) 2.407(4) 2.441(4) ? O1 H41 . . 2(3) 2(3) 2(2) ? O1 H111 . . 2(2) 2(3) 2(2) ? O1 H111 . 2_5555 3(5) 3(5) 3(6) ? O1 H112 . . 2.0(19) 2.0(18) 2.0(19) ? C1 C1 . 2_5555 1.418(6) 1.405(6) 1.430(6) ? C1 C2 . . 1.374(5) 1.358(5) 1.387(5) ? C1 C2 . 2_5555 2.336(5) 2.322(5) 2.352(6) ? C1 C3 . . 2.556(5) 2.543(5) 2.566(5) ? C1 C11 . . 2.329(5) 2.321(5) 2.335(5) ? C1 C11 . 2_5555 2.698(5) 2.689(5) 2.712(5) ? C1 H41 . . 3(3) 3(3) 3(3) ? C1 H111 . . 3(3) 3(3) 3(2) ? C1 H111 . 2_5555 3(4) 3(5) 3(4) ? C2 C2 . 2_5555 2.517(5) 2.504(5) 2.530(5) ? C2 C3 . . 1.455(5) 1.444(5) 1.464(5) ? C2 C4 . . 2.465(6) 2.459(6) 2.473(6) ? C2 H41 . . 3(3) 3(3) 3(3) ? C2 H102 . . 3(4) 3(4) 3(5) ? C3 C4 . . 1.356(6) 1.347(6) 1.369(6) ? C3 C5 . . 2.460(6) 2.450(6) 2.466(6) ? C3 C10 . . 2.786(6) 2.773(6) 2.797(6) ? C3 H41 . . 2.0(18) 2.0(18) 2.0(18) ? C3 H102 . . 3(3) 3(3) 3(3) ? C3 H103 . . 3(5) 3(5) 3(5) ? C4 C5 . . 1.429(6) 1.405(6) 1.448(6) ? C4 C6 . . 2.631(6) 2.612(5) 2.653(5) ? C4 H41 . . 1(3) 1(3) 1(3) ? C4 H82 . 4_5655 3(5) 3(4) 3(5) ? C5 C6 . . 1.203(6) 1.192(6) 1.209(6) ? C5 H41 . . 2(4) 2(5) 2(4) ? C5 H82 . 4_5655 3(3) 3(3) 3(3) ? C5 H111 . 4_5645 3(5) 3(4) 3(5) ? C6 C7 . . 2.990(6) 2.965(6) 3.015(6) ? C6 C8 . . 3.014(6) 2.979(6) 3.049(6) ? C6 C9 . . 2.976(6) 2.954(7) 3.001(6) ? C6 H101 . 4_5545 4(2) 3(3) 4.8(17) ? C7 H71 . . 1(5) 1(5) 1(5) ? C7 H72 . . 1(3) 1(3) 1(3) ? C7 H73 . . 1(5) 1(5) 1(5) ? C8 H81 . . 1(5) 1(5) 1(4) ? C8 H82 . . 1(5) 1(5) 1(5) ? C8 H83 . . 1(3) 1(2) 1(3) ? C9 H72 . 6_4445 3(5) 3(5) 3(6) ? C9 H91 . . 1(5) 1(5) 1(5) ? C9 H92 . . 1(3) 1(3) 1(3) ? C9 H93 . . 1(3) 1(3) 1(3) ? C10 H82 . 1_5565 3(3) 3(3) 3(4) ? C10 H101 . . 1(3) 1(3) 1(3) ? C10 H102 . . 1(4) 1(4) 1(4) ? C10 H103 . . 1(5) 1(5) 1(5) ? C11 C11 . 2_5555 1.483(5) 1.481(5) 1.485(5) ? C11 H111 . . 1(5) 1(5) 1(5) ? C11 H111 . 2_5555 2(6) 2(6) 2(6) ? C11 H112 . . 1(2) 1.0(18) 1.0(18) ? C11 H112 . 2_5555 2(5) 2(5) 2(5) ? H41 H82 . 4_5655 2.8035 2.6414 3.0371 ? H41 H102 . 4_5645 2.8443 2.7612 2.9236 ? H71 H72 . . 1.5677 1.5676 1.5677 ? H71 H73 . . 1.5677 1.567 1.5683 ? H71 H91 . 7_4545 2.645 2.5594 2.7911 ? H71 H93 . 4_5645 2.689 2.5373 2.886 ? H72 H73 . . 1.5677 1.5668 1.5685 ? H72 H91 . 6_4545 2.9347 2.7266 3.1049 ? H72 H92 . 6_4545 3.0988 2.8089 3.4242 ? H72 H93 . 6_4545 2.8424 2.6068 3.1513 ? H72 H103 . 4_5645 3.0231 2.876 3.1317 ? H73 H93 . 4_5645 2.8883 2.8072 2.9751 ? H73 H103 . 4_5645 2.6896 2.5493 2.8225 ? H81 H82 . . 1.5677 1.5674 1.568 ? H81 H83 . . 1.5676 1.567 1.5683 ? H81 H91 . 7_4545 2.6201 2.417 2.8587 ? H81 H92 . 4_5545 3.4145 2.6698 4.3469 ? H82 H83 . . 1.5677 1.5666 1.5687 ? H82 H102 . 1_5545 2.7836 2.6281 3.0182 ? H82 H103 . 1_5545 2.7104 2.5795 2.8997 ? H83 H101 . 4_5545 2.5982 2.4697 2.8256 ? H91 H92 . . 1.5677 1.5668 1.5686 ? H91 H93 . . 1.5677 1.5674 1.568 ? H92 H93 . . 1.5677 1.5669 1.5685 ? H101 H102 . . 1.5677 1.5672 1.5681 ? H101 H103 . . 1.5677 1.5673 1.568 ? H101 H111 . 1_5455 3.1659 2.971 3.4335 ? H102 H103 . . 1.5677 1.5673 1.568 ? H102 H111 . 1_5455 3.3031 2.9634 3.723 ? H111 H111 . 2_5555 2.7901 2.7886 2.7917 ? H111 H112 . . 1.5485 1.5424 1.5554 ? H111 H112 . 2_5555 2.3192 2.3142 2.325 ? H112 H112 . 2_5555 2.2847 2.2824 2.2871 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_ssg_symmetry_1 _geom_angle_site_ssg_symmetry_2 _geom_angle_site_ssg_symmetry_3 _geom_angle_av _geom_angle_min _geom_angle_max _geom_angle_publ_flag C1 S1 C1 . . 2_5555 32.22(13) 31.94(13) 32.50(13) ? C1 S1 C2 . . . 30.39(15) 30.02(15) 30.67(15) ? C1 S1 C2 . . 2_5555 62.61(16) 62.29(16) 63.01(16) ? C1 S1 C3 . . . 57.10(12) 56.72(12) 57.39(12) ? C1 S1 C3 . . 2_5555 89.31(12) 89.00(12) 89.69(12) ? C1 S1 H102 . . . 95.36 94.28 96.52 ? C1 S1 H102 . . 2_5555 112.9 111.3 114.48 ? C1 S1 H112 . . 1_5455 142.78 140.84 145.32 ? C1 S1 H112 . . 2_5455 174.52 172.92 176.02 ? C1 S1 C2 2_5555 . . 62.61(16) 62.29(16) 63.01(16) ? C1 S1 C2 2_5555 . 2_5555 30.39(15) 30.02(15) 30.67(15) ? C1 S1 C3 2_5555 . . 89.31(12) 89.00(12) 89.69(12) ? C1 S1 C3 2_5555 . 2_5555 57.10(12) 56.72(12) 57.39(12) ? C1 S1 H102 2_5555 . . 112.89 111.3 114.48 ? C1 S1 H102 2_5555 . 2_5555 95.37 94.28 96.52 ? C1 S1 H112 2_5555 . 1_5455 174.5 172.92 176.02 ? C1 S1 H112 2_5555 . 2_5455 142.8 140.84 145.32 ? C2 S1 C2 . . 2_5555 93.00(18) 92.67(18) 93.33(18) ? C2 S1 C3 . . . 26.71(15) 26.41(15) 26.98(15) ? C2 S1 C3 . . 2_5555 119.70(15) 119.43(15) 119.98(15) ? C2 S1 H102 . . . 77.17 76.49 77.59 ? C2 S1 H102 . . 2_5555 124.59 122.64 126.32 ? C2 S1 H112 . . 1_5455 112.41 110.74 114.83 ? C2 S1 H112 . . 2_5455 154.49 151.95 156.57 ? C2 S1 C3 2_5555 . . 119.70(15) 119.43(15) 119.98(15) ? C2 S1 C3 2_5555 . 2_5555 26.71(15) 26.41(15) 26.98(15) ? C2 S1 H102 2_5555 . . 124.59 122.64 126.32 ? C2 S1 H102 2_5555 . 2_5555 77.18 76.49 77.59 ? C2 S1 H112 2_5555 . 1_5455 154.51 151.95 156.57 ? C2 S1 H112 2_5555 . 2_5455 112.43 110.74 114.83 ? C3 S1 C3 . . 2_5555 146.40(11) 146.38(11) 146.43(11) ? C3 S1 H102 . . . 62.67 61.96 63.37 ? C3 S1 H102 . . 2_5555 127.17 125.46 128.98 ? C3 S1 H112 . . 1_5455 85.7 83.77 88.28 ? C3 S1 H112 . . 2_5455 127.85 125.27 129.82 ? C3 S1 H102 2_5555 . . 127.18 125.46 128.98 ? C3 S1 H102 2_5555 . 2_5555 62.68 61.96 63.37 ? C3 S1 H112 2_5555 . 1_5455 127.87 125.27 129.82 ? C3 S1 H112 2_5555 . 2_5455 85.72 83.77 88.28 ? H102 S1 H102 . . 2_5555 150.84 150.66 151.02 ? H102 S1 H112 . . 1_5455 62.97 61.73 64.72 ? H102 S1 H112 . . 2_5455 89.17 87.69 90.26 ? H102 S1 H112 2_5555 . 1_5455 89.16 87.69 90.26 ? H102 S1 H112 2_5555 . 2_5455 62.96 61.73 64.72 ? H112 S1 H112 1_5455 . 2_5455 42.27 40.96 43.57 ? C2 S2 C3 . . . 27.58(15) 27.33(15) 27.77(15) ? C2 S2 C4 . . . 53.44(12) 53.28(12) 53.60(12) ? C2 S2 C10 . . . 89.36(17) 88.44(17) 90.61(17) ? C2 S2 H101 . . . 110.11 109.4 111.15 ? C2 S2 H102 . . . 70.81 70.11 71.81 ? C2 S2 H103 . . . 87.35 86.12 88.91 ? C2 S2 H111 . . 4_5645 91.33 85.59 97.52 ? C2 S2 H112 . . 1_5455 93.96 87.05 102.5 ? C3 S2 C4 . . . 25.89(15) 25.57(15) 26.24(15) ? C3 S2 C10 . . . 101.8(2) 100.8(2) 102.5(2) ? C3 S2 H101 . . . 124.79 123.76 125.5 ? C3 S2 H102 . . . 89.88 88.97 90.55 ? C3 S2 H103 . . . 89.88 88.96 90.54 ? C3 S2 H111 . . 4_5645 78.01 74.77 82.11 ? C3 S2 H112 . . 1_5455 119.21 111.74 128.27 ? C4 S2 C10 . . . 112.84(18) 109.95(18) 115.23(18) ? C4 S2 H101 . . . 133.17 130.2 135.63 ? C4 S2 H102 . . . 108.87 106.52 110.9 ? C4 S2 H103 . . . 93.7 90.73 96.07 ? C4 S2 H111 . . 4_5645 66.25 65.48 67.53 ? C4 S2 H112 . . 1_5455 140.52 133.17 149.75 ? C10 S2 H101 . . . 22.95 22.89 23 ? C10 S2 H102 . . . 22.95 22.89 23 ? C10 S2 H103 . . . 22.95 22.89 23 ? C10 S2 H111 . . 4_5645 172.94 166.57 179.3 ? C10 S2 H112 . . 1_5455 84.72 83.1 86.37 ? H101 S2 H102 . . . 39.48 39.38 39.56 ? H101 S2 H103 . . . 39.48 39.37 39.56 ? H101 S2 H111 . . 4_5645 156.16 151.37 158.77 ? H101 S2 H112 . . 1_5455 74.3 71.87 76.49 ? H102 S2 H103 . . . 39.48 39.37 39.56 ? H102 S2 H111 . . 4_5645 158.48 148.51 169.02 ? H102 S2 H112 . . 1_5455 73.43 69.6 77.99 ? H103 S2 H111 . . 4_5645 154.59 145.91 161.36 ? H103 S2 H112 . . 1_5455 107.54 105.88 109.27 ? H111 S2 H112 4_5645 . 1_5455 96.59 89.29 103.42 ? C6 Si1 C7 . . . 108.0(2) 106.8(2) 108.5(2) ? C6 Si1 C8 . . . 109.4(2) 107.9(2) 111.0(2) ? C6 Si1 C9 . . . 107.4(2) 106.7(2) 108.2(2) ? C6 Si1 H71 . . . 130.53 129.41 131.26 ? C6 Si1 H72 . . . 95.87 94.81 96.49 ? C6 Si1 H73 . . . 95.87 94.82 96.49 ? C6 Si1 H81 . . . 132.06 130.56 133.48 ? C6 Si1 H82 . . . 97.24 95.71 98.76 ? C6 Si1 H83 . . . 97.24 95.7 98.75 ? C6 Si1 H91 . . . 129.98 129.14 130.72 ? C6 Si1 H92 . . . 95.3 94.68 96.06 ? C6 Si1 H93 . . . 95.3 94.68 96.06 ? C7 Si1 C8 . . . 110.5(2) 109.6(2) 111.0(2) ? C7 Si1 C9 . . . 111.1(2) 110.7(2) 111.4(2) ? C7 Si1 H71 . . . 22.56 22.43 22.72 ? C7 Si1 H72 . . . 22.57 22.42 22.72 ? C7 Si1 H73 . . . 22.57 22.42 22.71 ? C7 Si1 H81 . . . 98.63 98.16 99.09 ? C7 Si1 H82 . . . 97.86 96.82 98.48 ? C7 Si1 H83 . . . 133.12 132.1 133.65 ? C7 Si1 H91 . . . 99.49 99.04 100.01 ? C7 Si1 H92 . . . 133.68 133.09 134.08 ? C7 Si1 H93 . . . 98.14 97.91 98.52 ? C8 Si1 C9 . . . 110.3(2) 109.4(2) 111.5(2) ? C8 Si1 H71 . . . 98.37 97.4 99.28 ? C8 Si1 H72 . . . 133.07 132.17 133.6 ? C8 Si1 H73 . . . 98.17 97.45 98.68 ? C8 Si1 H81 . . . 22.62 22.48 22.74 ? C8 Si1 H82 . . . 22.62 22.47 22.74 ? C8 Si1 H83 . . . 22.62 22.48 22.75 ? C8 Si1 H91 . . . 98.34 97.02 99.56 ? C8 Si1 H92 . . . 97.85 97.3 98.86 ? C8 Si1 H93 . . . 132.93 131.86 134.16 ? C9 Si1 H71 . . . 99.62 99.22 100 ? C9 Si1 H72 . . . 98.05 97.56 98.43 ? C9 Si1 H73 . . . 133.64 133.23 134.05 ? C9 Si1 H81 . . . 98.73 97.49 99.79 ? C9 Si1 H82 . . . 132.93 131.99 134.11 ? C9 Si1 H83 . . . 97.44 96.73 98.5 ? C9 Si1 H91 . . . 22.6 22.38 22.75 ? C9 Si1 H92 . . . 22.6 22.38 22.75 ? C9 Si1 H93 . . . 22.6 22.37 22.75 ? H71 Si1 H72 . . . 38.82 38.58 39.09 ? H71 Si1 H73 . . . 38.82 38.58 39.08 ? H71 Si1 H81 . . . 81.36 80.8 82.15 ? H71 Si1 H82 . . . 93.35 92.05 94.23 ? H71 Si1 H83 . . . 119.69 118.75 120.63 ? H71 Si1 H91 . . . 82.67 82.28 83.15 ? H71 Si1 H92 . . . 120.97 120.35 121.59 ? H71 Si1 H93 . . . 94.35 94 94.74 ? H72 Si1 H73 . . . 38.82 38.57 39.07 ? H72 Si1 H81 . . . 119.73 119.18 120.26 ? H72 Si1 H82 . . . 118.95 118 119.76 ? H72 Si1 H83 . . . 155.67 154.64 156.32 ? H72 Si1 H91 . . . 94.09 93.58 94.71 ? H72 Si1 H92 . . . 118.95 118.3 119.46 ? H72 Si1 H93 . . . 80.37 80.1 80.78 ? H73 Si1 H81 . . . 94.02 93.6 94.32 ? H73 Si1 H82 . . . 80.58 79.77 81.17 ? H73 Si1 H83 . . . 119.15 118.21 119.88 ? H73 Si1 H91 . . . 120.85 120.25 121.32 ? H73 Si1 H92 . . . 156.16 155.68 156.63 ? H73 Si1 H93 . . . 118.93 118.53 119.35 ? H81 Si1 H82 . . . 38.91 38.65 39.11 ? H81 Si1 H83 . . . 38.9 38.68 39.12 ? H81 Si1 H91 . . . 81.5 80.05 82.6 ? H81 Si1 H92 . . . 94 93.23 94.95 ? H81 Si1 H93 . . . 119.91 118.46 121.11 ? H82 Si1 H83 . . . 38.9 38.67 39.13 ? H82 Si1 H91 . . . 119.75 118.26 121.04 ? H82 Si1 H92 . . . 118.71 118.06 119.69 ? H82 Si1 H93 . . . 155.5 154.5 156.77 ? H83 Si1 H91 . . . 93.05 92.12 94.18 ? H83 Si1 H92 . . . 80.09 79.51 81.12 ? H83 Si1 H93 . . . 118.54 117.66 119.76 ? H91 Si1 H92 . . . 38.88 38.5 39.14 ? H91 Si1 H93 . . . 38.88 38.49 39.13 ? H92 Si1 H93 . . . 38.88 38.5 39.14 ? O1 O1 C1 2_5555 . . 57.0(2) 56.6(2) 57.5(2) ? O1 O1 C1 2_5555 . 2_5555 27.89(11) 27.78(10) 28.01(11) ? O1 O1 C2 2_5555 . . 85.43(13) 85.22(13) 85.72(13) ? O1 O1 C4 2_5555 . . 138.34(13) 137.84(13) 138.96(13) ? O1 O1 C11 2_5555 . . 56.62(17) 56.04(17) 57.33(17) ? O1 O1 C11 2_5555 . 2_5555 30.02(10) 29.80(10) 30.22(10) ? O1 O1 H41 2_5555 . . 148.21 145.32 150.84 ? O1 O1 H111 2_5555 . . 61.36 60.94 61.92 ? O1 O1 H111 2_5555 . 2_5555 41.93 41.66 42.2 ? O1 O1 H112 2_5555 . . 80.87 80.31 81.58 ? C1 O1 C1 . . 2_5555 29.2(2) 28.8(2) 29.5(2) ? C1 O1 C2 . . . 28.4(2) 28.0(2) 28.8(2) ? C1 O1 C4 . . . 81.6(2) 81.0(2) 82.4(2) ? C1 O1 C11 . . . 111.6(3) 111.0(3) 112.3(3) ? C1 O1 C11 . . 2_5555 86.1(2) 85.5(2) 86.7(2) ? C1 O1 H41 . . . 94.16 92.41 95.97 ? C1 O1 H111 . . . 102.92 102.14 103.72 ? C1 O1 H111 . . 2_5555 88.41 87.45 89.42 ? C1 O1 H112 . . . 137.67 137.11 138.58 ? C1 O1 C2 2_5555 . . 57.55(14) 57.31(14) 57.86(14) ? C1 O1 C4 2_5555 . . 110.56(15) 110.19(15) 111.16(15) ? C1 O1 C11 2_5555 . . 83.6(2) 83.1(2) 84.1(2) ? C1 O1 C11 2_5555 . 2_5555 57.16(14) 56.81(14) 57.48(14) ? C1 O1 H41 2_5555 . . 122.11 120.07 124.09 ? C1 O1 H111 2_5555 . . 81.51 81.2 81.78 ? C1 O1 H111 2_5555 . 2_5555 63.14 62.51 63.74 ? C1 O1 H112 2_5555 . . 108.71 108.17 109.39 ? C2 O1 C4 . . . 53.33(14) 52.91(14) 53.94(14) ? C2 O1 C11 . . . 138.4(2) 138.0(2) 138.8(2) ? C2 O1 C11 . . 2_5555 114.20(17) 113.96(16) 114.67(17) ? C2 O1 H41 . . . 66.8 65.73 67.94 ? C2 O1 H111 . . . 122.23 121.2 123.55 ? C2 O1 H111 . . 2_5555 113.07 112.18 114.1 ? C2 O1 H112 . . . 165.38 164.95 165.62 ? C4 O1 C11 . . . 163.1(2) 162.5(2) 163.6(2) ? C4 O1 C11 . . 2_5555 162.07(17) 161.51(18) 162.80(17) ? C4 O1 H41 . . . 15.82 15.31 16.26 ? C4 O1 H111 . . . 142.53 142.05 142.79 ? C4 O1 H111 . . 2_5555 144.23 143.53 144.93 ? C4 O1 H112 . . . 140.73 140.15 141.31 ? C11 O1 C11 . . 2_5555 34.73(18) 34.35(18) 35.24(18) ? C11 O1 H41 . . . 154.16 152.54 155.57 ? C11 O1 H111 . . . 27.04 26.95 27.2 ? C11 O1 H111 . . 2_5555 50.09 49.71 50.58 ? C11 O1 H112 . . . 27.05 26.95 27.2 ? C11 O1 H41 2_5555 . . 157.58 154.62 160.61 ? C11 O1 H111 2_5555 . . 53.28 52.98 53.73 ? C11 O1 H111 2_5555 . 2_5555 21.54 21.42 21.67 ? C11 O1 H112 2_5555 . . 53.28 52.98 53.74 ? H41 O1 H111 . . . 147 143.9 149.93 ? H41 O1 H111 . . 2_5555 136.08 133.09 139.15 ? H41 O1 H112 . . . 127.76 126.57 128.69 ? H111 O1 H111 . . 2_5555 73.18 72.8 73.71 ? H111 O1 H112 . . . 45.78 45.43 46.25 ? H111 O1 H112 2_5555 . . 58.63 58.42 58.92 ? S1 C1 O1 . . . 163.1(3) 162.6(3) 163.7(3) ? S1 C1 O1 . . 2_5555 101.78(15) 101.59(15) 101.98(15) ? S1 C1 C1 . . 2_5555 73.9(2) 73.6(2) 74.1(2) ? S1 C1 C2 . . . 39.68(19) 39.5(2) 39.83(19) ? S1 C1 C2 . . 2_5555 41.25(11) 41.16(11) 41.34(11) ? S1 C1 C3 . . . 65.86(12) 65.36(12) 66.26(12) ? S1 C1 C11 . . . 160.6(2) 160.3(2) 161.0(2) ? S1 C1 C11 . . 2_5555 132.79(18) 131.92(17) 133.34(18) ? S1 C1 H41 . . . 106.71 105.24 107.86 ? S1 C1 H111 . . . 144.57 143.63 145.17 ? S1 C1 H111 . . 2_5555 130.04 128.78 131.1 ? O1 C1 O1 . . 2_5555 95.1(2) 94.6(2) 95.5(2) ? O1 C1 C1 . . 2_5555 122.9(3) 122.6(3) 123.4(3) ? O1 C1 C2 . . . 123.5(4) 122.8(4) 124.1(4) ? O1 C1 C2 . . 2_5555 155.5(3) 155.0(3) 156.1(3) ? O1 C1 C3 . . . 97.3(2) 96.8(2) 98.2(3) ? O1 C1 C11 . . . 35.46(17) 34.95(17) 35.76(17) ? O1 C1 C11 . . 2_5555 63.7(2) 63.00(19) 64.3(2) ? O1 C1 H41 . . . 56.74 54.96 58.61 ? O1 C1 H111 . . . 47.04 46.64 47.51 ? O1 C1 H111 . . 2_5555 63.74 62.81 64.66 ? O1 C1 C1 2_5555 . 2_5555 27.90(18) 27.81(18) 28.04(18) ? O1 C1 C2 2_5555 . . 141.4(3) 141.3(3) 141.7(3) ? O1 C1 C2 2_5555 . 2_5555 60.54(15) 60.41(15) 60.66(15) ? O1 C1 C3 2_5555 . . 167.4(2) 166.8(2) 168.0(2) ? O1 C1 C11 2_5555 . . 61.06(14) 60.37(13) 61.58(14) ? O1 C1 C11 2_5555 . 2_5555 32.35(10) 31.93(10) 32.61(10) ? O1 C1 H41 2_5555 . . 148.73 147.83 149.65 ? O1 C1 H111 2_5555 . . 61.61 60.89 62.21 ? O1 C1 H111 2_5555 . 2_5555 42.51 42.19 42.68 ? C1 C1 C2 2_5555 . . 113.6(3) 113.3(3) 113.9(3) ? C1 C1 C2 2_5555 . 2_5555 32.64(19) 32.39(19) 32.8(2) ? C1 C1 C3 2_5555 . . 139.7(3) 139.2(3) 140.2(3) ? C1 C1 C11 2_5555 . . 88.7(2) 88.1(2) 89.1(2) ? C1 C1 C11 2_5555 . 2_5555 59.6(2) 59.1(2) 59.9(2) ? C1 C1 H41 2_5555 . . 167.13 164.19 170.59 ? C1 C1 H111 2_5555 . . 85.82 85.25 86.16 ? C1 C1 H111 2_5555 . 2_5555 65.16 64.6 65.63 ? C2 C1 C2 . . 2_5555 80.9(3) 80.7(3) 81.1(3) ? C2 C1 C3 . . . 26.2(2) 25.6(2) 26.7(2) ? C2 C1 C11 . . . 155.9(3) 155.1(3) 157.0(3) ? C2 C1 C11 . . 2_5555 170.3(3) 169.3(3) 171.2(3) ? C2 C1 H41 . . . 68.28 67.38 69.14 ? C2 C1 H111 . . . 145 143.73 146.18 ? C2 C1 H111 . . 2_5555 154.01 152.9 155.21 ? C2 C1 C3 2_5555 . . 107.11(18) 106.52(18) 107.54(18) ? C2 C1 C11 2_5555 . . 121.0(2) 120.3(2) 121.4(2) ? C2 C1 C11 2_5555 . 2_5555 91.91(17) 91.19(17) 92.39(17) ? C2 C1 H41 2_5555 . . 145.94 143.65 147.73 ? C2 C1 H111 2_5555 . . 114.29 114.02 114.6 ? C2 C1 H111 2_5555 . 2_5555 93.97 93 94.78 ? C3 C1 C11 . . . 130.7(2) 129.9(2) 131.9(2) ? C3 C1 C11 . . 2_5555 160.1(2) 159.5(2) 161.0(2) ? C3 C1 H41 . . . 43.54 43.26 43.95 ? C3 C1 H111 . . . 127.05 125.95 128.28 ? C3 C1 H111 . . 2_5555 147.63 146.98 148.02 ? C11 C1 C11 . . 2_5555 33.30(12) 33.12(12) 33.46(12) ? C11 C1 H41 . . . 92.18 90.52 93.73 ? C11 C1 H111 . . . 20.96 20.77 21.14 ? C11 C1 H111 . . 2_5555 43.51 43.36 43.73 ? C11 C1 H41 2_5555 . . 116.7 115.57 117.67 ? C11 C1 H111 2_5555 . . 44.3 44.06 44.56 ? C11 C1 H111 2_5555 . 2_5555 19.2 19.13 19.31 ? H41 C1 H111 . . . 99.45 97.15 101.97 ? H41 C1 H111 . . 2_5555 107.29 106 109.16 ? H111 C1 H111 . . 2_5555 59.96 59.73 60.16 ? S1 C2 S2 . . . 87.65(15) 86.23(15) 88.74(15) ? S1 C2 O1 . . . 138.0(2) 137.4(2) 138.6(2) ? S1 C2 C1 . . . 109.9(3) 109.5(3) 110.4(3) ? S1 C2 C1 . . 2_5555 76.14(17) 75.80(17) 76.39(17) ? S1 C2 C2 . . 2_5555 43.50(12) 43.29(12) 43.67(12) ? S1 C2 C3 . . . 120.9(3) 120.3(3) 121.4(3) ? S1 C2 C4 . . . 146.1(2) 145.3(2) 146.8(2) ? S1 C2 H41 . . . 160.79 157.57 163.86 ? S1 C2 H102 . . . 68.15 67.55 68.88 ? S2 C2 O1 . . . 133.64(17) 132.23(17) 135.84(17) ? S2 C2 C1 . . . 159.8(3) 157.8(3) 162.4(3) ? S2 C2 C1 . . 2_5555 160.4(2) 159.8(2) 161.2(2) ? S2 C2 C2 . . 2_5555 130.24(17) 129.00(17) 131.07(17) ? S2 C2 C3 . . . 34.33(17) 34.02(17) 34.80(18) ? S2 C2 C4 . . . 61.95(14) 61.52(14) 62.35(14) ? S2 C2 H41 . . . 83.42 82.98 83.73 ? S2 C2 H102 . . . 47.49 47.18 47.67 ? O1 C2 C1 . . . 28.1(2) 27.7(2) 28.5(2) ? O1 C2 C1 . . 2_5555 61.91(15) 61.57(15) 62.27(15) ? O1 C2 C2 . . 2_5555 94.54(17) 94.08(17) 94.95(17) ? O1 C2 C3 . . . 101.1(2) 100.5(2) 102.0(2) ? O1 C2 C4 . . . 75.01(17) 74.19(17) 75.63(17) ? O1 C2 H41 . . . 55.32 54.05 56.84 ? O1 C2 H102 . . . 130.15 128.81 131.6 ? C1 C2 C1 . . 2_5555 33.8(2) 33.4(2) 34.2(2) ? C1 C2 C2 . . 2_5555 66.4(2) 66.2(2) 66.9(2) ? C1 C2 C3 . . . 129.2(4) 128.4(4) 130.0(4) ? C1 C2 C4 . . . 102.9(3) 102.4(3) 103.3(3) ? C1 C2 H41 . . . 82.5 81.8 83.37 ? C1 C2 H102 . . . 129.12 127.31 130.65 ? C1 C2 C2 2_5555 . 2_5555 32.64(13) 32.34(13) 32.80(14) ? C1 C2 C3 2_5555 . . 162.9(3) 162.3(3) 163.4(3) ? C1 C2 C4 2_5555 . . 136.4(2) 135.9(2) 136.9(2) ? C1 C2 H41 2_5555 . . 115.26 114.65 115.74 ? C1 C2 H102 2_5555 . . 114.96 113.16 116.39 ? C2 C2 C3 2_5555 . . 164.3(3) 163.7(3) 164.7(3) ? C2 C2 C4 2_5555 . . 166.9(2) 165.9(2) 168.2(2) ? C2 C2 H41 2_5555 . . 145.69 144.82 147 ? C2 C2 H102 2_5555 . . 95.44 93.94 96.6 ? C3 C2 C4 . . . 27.7(2) 27.4(2) 28.0(2) ? C3 C2 H41 . . . 49.17 48.82 49.45 ? C3 C2 H102 . . . 73.55 71.81 74.86 ? C4 C2 H41 . . . 21.52 21.4 21.6 ? C4 C2 H102 . . . 97.32 94.86 99.31 ? H41 C2 H102 . . . 115.97 112.71 118.72 ? S1 C3 S2 . . . 86.75(14) 85.38(14) 87.76(14) ? S1 C3 C1 . . . 57.04(12) 56.83(11) 57.28(11) ? S1 C3 C2 . . . 32.41(17) 32.18(17) 32.82(17) ? S1 C3 C4 . . . 151.6(3) 150.3(3) 153.9(3) ? S1 C3 C5 . . . 170.6(2) 169.4(2) 172.0(2) ? S1 C3 C10 . . . 76.85(13) 76.14(13) 77.59(13) ? S1 C3 H41 . . . 127.31 126.07 129.45 ? S1 C3 H102 . . . 59.55 58.61 60.58 ? S1 C3 H103 . . . 90.38 89.12 91.8 ? S2 C3 C1 . . . 141.1(2) 140.8(2) 141.3(2) ? S2 C3 C2 . . . 118.1(3) 117.6(3) 118.5(3) ? S2 C3 C4 . . . 119.3(3) 118.5(3) 120.0(3) ? S2 C3 C5 . . . 90.71(19) 90.36(19) 91.07(19) ? S2 C3 C10 . . . 39.67(13) 39.29(13) 40.09(13) ? S2 C3 H41 . . . 144.3 143.5 144.95 ? S2 C3 H102 . . . 52.71 52.3 53.18 ? S2 C3 H103 . . . 52.71 52.3 53.18 ? C1 C3 C2 . . . 24.63(19) 24.30(18) 25.01(19) ? C1 C3 C4 . . . 99.2(3) 98.4(3) 99.9(3) ? C1 C3 C5 . . . 127.3(2) 126.7(2) 127.8(2) ? C1 C3 C10 . . . 111.1(2) 109.2(2) 113.8(2) ? C1 C3 H41 . . . 74.53 73.9 75.3 ? C1 C3 H102 . . . 93.26 91.77 95.31 ? C1 C3 H103 . . . 109.05 106.1 112.87 ? C2 C3 C4 . . . 122.5(3) 121.8(3) 123.3(3) ? C2 C3 C5 . . . 151.2(3) 150.5(3) 151.7(3) ? C2 C3 C10 . . . 97.1(3) 95.7(3) 99.2(3) ? C2 C3 H41 . . . 97.36 96.8 98.17 ? C2 C3 H102 . . . 77.87 76.59 79.92 ? C2 C3 H103 . . . 102.61 100.39 105.91 ? C4 C3 C5 . . . 28.8(2) 27.9(2) 29.5(2) ? C4 C3 C10 . . . 130.0(3) 126.7(3) 132.2(3) ? C4 C3 H41 . . . 25.14 24.87 25.38 ? C4 C3 H102 . . . 144.47 140.46 147.69 ? C4 C3 H103 . . . 113.72 109.79 116.73 ? C5 C3 C10 . . . 106.65(19) 104.29(19) 108.73(19) ? C5 C3 H41 . . . 53.9 53.28 54.5 ? C5 C3 H102 . . . 125.06 122.39 127.34 ? C5 C3 H103 . . . 95.2 91.85 97.97 ? C10 C3 H41 . . . 145.68 142.11 149.05 ? C10 C3 H102 . . . 19.2 19.1 19.32 ? C10 C3 H103 . . . 19.2 19.11 19.32 ? H41 C3 H102 . . . 149.25 145.52 153.17 ? H41 C3 H103 . . . 126.55 122.81 130.07 ? H102 C3 H103 . . . 31.18 31.01 31.37 ? S2 C4 O1 . . . 114.10(15) 113.04(15) 114.68(16) ? S2 C4 C2 . . . 64.60(14) 64.13(14) 64.93(14) ? S2 C4 C3 . . . 34.8(2) 34.3(2) 35.3(2) ? S2 C4 C5 . . . 89.4(3) 88.7(3) 90.4(3) ? S2 C4 C6 . . . 90.53(16) 88.86(16) 92.69(17) ? S2 C4 H41 . . . 152.41 151.92 152.7 ? S2 C4 H82 . . 4_5655 125.88 122.13 129.53 ? O1 C4 C2 . . . 51.66(13) 51.42(13) 51.90(13) ? O1 C4 C3 . . . 80.2(2) 79.0(2) 81.1(2) ? O1 C4 C5 . . . 150.6(3) 147.9(3) 152.9(3) ? O1 C4 C6 . . . 149.7(2) 145.5(2) 152.2(2) ? O1 C4 H41 . . . 41.67 39.9 44.38 ? O1 C4 H82 . . 4_5655 77.12 63.48 90.53 ? C2 C4 C3 . . . 29.9(2) 29.2(2) 30.3(2) ? C2 C4 C5 . . . 153.9(4) 153.2(4) 154.8(4) ? C2 C4 C6 . . . 154.9(2) 153.6(2) 156.9(2) ? C2 C4 H41 . . . 88.12 87.77 88.52 ? C2 C4 H82 . . 4_5655 117.43 105.73 128.01 ? C3 C4 C5 . . . 124.1(4) 122.9(4) 125.4(4) ? C3 C4 C6 . . . 125.2(3) 123.2(3) 127.4(3) ? C3 C4 H41 . . . 117.96 117.32 118.53 ? C3 C4 H82 . . 4_5655 126.79 118.42 133.96 ? C5 C4 C6 . . . 1.3(2) 0.3(2) 2.6(2) ? C5 C4 H41 . . . 117.96 117.33 118.53 ? C5 C4 H82 . . 4_5655 74.8 64.08 85.3 ? C6 C4 H41 . . . 116.88 115.16 118.27 ? C6 C4 H82 . . 4_5655 74.13 63.43 84.39 ? H41 C4 H82 . . 4_5655 68.9 63.65 76.05 ? C3 C5 C4 . . . 27.2(2) 26.7(2) 27.7(2) ? C3 C5 C6 . . . 155.1(4) 152.9(4) 158.1(4) ? C3 C5 H41 . . . 51.46 51.15 51.98 ? C3 C5 H82 . . 4_5655 93.75 83.43 104.52 ? C3 C5 H111 . . 4_5645 68.78 63.98 74.46 ? C4 C5 C6 . . . 177.2(5) 174.2(5) 179.3(5) ? C4 C5 H41 . . . 24.29 23.89 24.68 ? C4 C5 H82 . . 4_5655 77.74 67.97 89.12 ? C4 C5 H111 . . 4_5645 79.58 72.42 87.14 ? C6 C5 H41 . . . 153.32 150.23 155.75 ? C6 C5 H82 . . 4_5655 100.79 89.41 111.38 ? C6 C5 H111 . . 4_5645 101.59 94.31 111.91 ? H41 C5 H82 . . 4_5655 65.04 56.86 75.52 ? H41 C5 H111 . . 4_5645 90.95 83.2 99.25 ? H82 C5 H111 4_5655 . 4_5645 155.5 139.84 172.79 ? Si1 C6 C4 . . . 174.6(2) 171.9(2) 178.1(2) ? Si1 C6 C5 . . . 174.5(4) 173.0(4) 177.6(4) ? Si1 C6 C7 . . . 36.23(14) 35.76(13) 36.86(14) ? Si1 C6 C8 . . . 35.43(12) 34.82(12) 36.08(13) ? Si1 C6 C9 . . . 36.48(13) 36.13(13) 37.01(13) ? Si1 C6 H101 . . 4_5545 81.19 74.01 89.88 ? C4 C6 C5 . . . 1.5(3) 0.4(3) 3.1(3) ? C4 C6 C7 . . . 142.8(2) 137.6(2) 149.4(2) ? C4 C6 C8 . . . 148.0(2) 141.6(2) 152.9(2) ? C4 C6 C9 . . . 140.5(2) 139.5(2) 141.3(2) ? C4 C6 H101 . . 4_5545 100.34 96 103.91 ? C5 C6 C7 . . . 144.0(4) 140.0(4) 150.7(4) ? C5 C6 C8 . . . 147.7(4) 141.1(4) 151.9(4) ? C5 C6 C9 . . . 139.6(4) 138.2(4) 140.8(4) ? C5 C6 H101 . . 4_5545 99.22 93.11 103.29 ? C7 C6 C8 . . . 61.03(15) 60.83(15) 61.41(15) ? C7 C6 C9 . . . 61.73(16) 61.48(16) 62.05(16) ? C7 C6 H101 . . 4_5545 116.55 109.18 125.4 ? C8 C6 C9 . . . 61.06(15) 60.36(15) 61.67(15) ? C8 C6 H101 . . 4_5545 59.25 52.37 66.55 ? C9 C6 H101 . . 4_5545 72.49 66.75 80.63 ? Si1 C7 C6 . . . 35.80(13) 35.37(13) 36.31(13) ? Si1 C7 H71 . . . 109.47 109.46 109.48 ? Si1 C7 H72 . . . 109.47 109.46 109.48 ? Si1 C7 H73 . . . 109.47 109.46 109.48 ? C6 C7 H71 . . . 145.27 144.83 145.78 ? C6 C7 H72 . . . 89.69 89.38 89.93 ? C6 C7 H73 . . . 89.69 89.4 89.93 ? H71 C7 H72 . . . 109.47 109.44 109.51 ? H71 C7 H73 . . . 109.47 109.44 109.5 ? H72 C7 H73 . . . 109.47 109.45 109.49 ? Si1 C8 C6 . . . 35.13(12) 34.17(12) 36.05(12) ? Si1 C8 H81 . . . 109.47 109.46 109.48 ? Si1 C8 H82 . . . 109.47 109.45 109.49 ? Si1 C8 H83 . . . 109.47 109.46 109.49 ? C6 C8 H81 . . . 144.6 143.64 145.52 ? C6 C8 H82 . . . 90.08 89.55 90.65 ? C6 C8 H83 . . . 90.08 89.54 90.63 ? H81 C8 H82 . . . 109.47 109.43 109.51 ? H81 C8 H83 . . . 109.47 109.44 109.5 ? H82 C8 H83 . . . 109.47 109.45 109.49 ? Si1 C9 C6 . . . 36.14(13) 35.63(13) 36.44(13) ? Si1 C9 H72 . . 6_4445 165.17 153.06 179.56 ? Si1 C9 H91 . . . 109.47 109.46 109.48 ? Si1 C9 H92 . . . 109.47 109.47 109.48 ? Si1 C9 H93 . . . 109.47 109.46 109.48 ? C6 C9 H72 . . 6_4445 142.38 137.88 145.73 ? C6 C9 H91 . . . 145.61 145.12 145.92 ? C6 C9 H92 . . . 89.5 89.32 89.79 ? C6 C9 H93 . . . 89.5 89.31 89.78 ? H72 C9 H91 6_4445 . . 69.53 65.1 75.6 ? H72 C9 H92 6_4445 . . 79.78 58.49 96.83 ? H72 C9 H93 6_4445 . . 63.84 53.88 78.54 ? H91 C9 H92 . . . 109.47 109.45 109.49 ? H91 C9 H93 . . . 109.47 109.45 109.5 ? H92 C9 H93 . . . 109.47 109.47 109.48 ? S2 C10 C3 . . . 38.50(13) 38.10(12) 39.08(13) ? S2 C10 H82 . . 1_5565 155.98 153.7 158.59 ? S2 C10 H101 . . . 109.47 109.46 109.48 ? S2 C10 H102 . . . 109.47 109.46 109.48 ? S2 C10 H103 . . . 109.47 109.47 109.47 ? C3 C10 H82 . . 1_5565 118.4 117.16 120.35 ? C3 C10 H101 . . . 147.97 147.58 148.56 ? C3 C10 H102 . . . 88.13 87.81 88.37 ? C3 C10 H103 . . . 88.13 87.8 88.36 ? H82 C10 H101 1_5565 . . 93.31 91.8 94.06 ? H82 C10 H102 1_5565 . . 62.95 52.84 72.62 ? H82 C10 H103 1_5565 . . 58.45 48.71 68.2 ? H101 C10 H102 . . . 109.47 109.46 109.49 ? H101 C10 H103 . . . 109.47 109.46 109.48 ? H102 C10 H103 . . . 109.47 109.47 109.48 ? O1 C11 O1 . . 2_5555 93.4(2) 92.9(2) 93.8(2) ? O1 C11 C1 . . . 32.94(17) 32.72(17) 33.22(17) ? O1 C11 C1 . . 2_5555 64.07(19) 63.87(19) 64.28(19) ? O1 C11 C11 . . 2_5555 111.4(3) 110.7(3) 111.9(3) ? O1 C11 H111 . . . 109.47 109.47 109.48 ? O1 C11 H111 . . 2_5555 96.39 95.95 96.81 ? O1 C11 H112 . . . 109.47 109.47 109.47 ? O1 C11 H112 . . 2_5555 137.95 137.27 138.53 ? O1 C11 C1 2_5555 . . 61.79(14) 61.58(14) 62.16(15) ? O1 C11 C1 2_5555 . 2_5555 30.23(11) 30.00(11) 30.38(11) ? O1 C11 C11 2_5555 . 2_5555 33.91(17) 33.70(17) 34.07(17) ? O1 C11 H111 2_5555 . . 90.39 90.32 90.52 ? O1 C11 H111 2_5555 . 2_5555 52.26 52.16 52.34 ? O1 C11 H112 2_5555 . . 143.3 143.12 143.45 ? O1 C11 H112 2_5555 . 2_5555 52.26 52.16 52.34 ? C1 C11 C1 . . 2_5555 31.68(14) 31.43(14) 32.01(14) ? C1 C11 C11 . . 2_5555 87.2(2) 86.9(2) 87.5(2) ? C1 C11 H111 . . . 98.82 98.1 99.72 ? C1 C11 H111 . . 2_5555 83.88 83.43 84.17 ? C1 C11 H112 . . . 141.13 140.78 141.5 ? C1 C11 H112 . . 2_5555 112.21 112.01 112.55 ? C1 C11 C11 2_5555 . 2_5555 59.5(2) 59.3(2) 59.8(2) ? C1 C11 H111 2_5555 . . 93.19 92.4 93.85 ? C1 C11 H111 2_5555 . 2_5555 66.61 66.26 66.95 ? C1 C11 H112 2_5555 . . 159.16 158.89 159.47 ? C1 C11 H112 2_5555 . 2_5555 81.93 81.7 82.16 ? C11 C11 H111 2_5555 . . 109.47 109.47 109.47 ? C11 C11 H111 2_5555 . 2_5555 26.65 26.63 26.68 ? C11 C11 H112 2_5555 . . 109.47 109.46 109.48 ? C11 C11 H112 2_5555 . 2_5555 26.65 26.62 26.68 ? H111 C11 H111 . . 2_5555 136.12 136.1 136.15 ? H111 C11 H112 . . . 107.51 106.9 108.21 ? H111 C11 H112 . . 2_5555 95.72 95.39 96.01 ? H111 C11 H112 2_5555 . . 95.72 95.39 96.01 ? H111 C11 H112 2_5555 . 2_5555 45.13 44.9 45.33 ? H112 C11 H112 . . 2_5555 93.37 93.3 93.43 ? O1 H41 C1 . . . 29.11 28.77 29.45 ? O1 H41 C2 . . . 57.87 57.43 58.14 ? O1 H41 C3 . . . 88.87 87.09 89.78 ? O1 H41 C4 . . . 122.51 119.36 124.69 ? O1 H41 C5 . . . 152.21 146.56 156.97 ? O1 H41 H82 . . 4_5655 92.36 75.69 107.54 ? O1 H41 H102 . . 4_5645 100.95 94.21 106.96 ? C1 H41 C2 . . . 29.22 29.05 29.33 ? C1 H41 C3 . . . 61.93 61.43 62.32 ? C1 H41 C4 . . . 98.22 97.7 98.6 ? C1 H41 C5 . . . 135.19 134.46 135.81 ? C1 H41 H82 . . 4_5655 110.92 96.54 123.34 ? C1 H41 H102 . . 4_5645 129.43 122.52 135.11 ? C2 H41 C3 . . . 33.48 32.95 33.83 ? C2 H41 C4 . . . 70.36 70.09 70.66 ? C2 H41 C5 . . . 108.1 107.63 108.62 ? C2 H41 H82 . . 4_5655 119.19 109.53 127.41 ? C2 H41 H102 . . 4_5645 158.55 151.65 164.04 ? C3 H41 C4 . . . 36.89 36.54 37.32 ? C3 H41 C5 . . . 74.64 74.12 75.3 ? C3 H41 H82 . . 4_5655 110.22 107.2 115.05 ? C3 H41 H102 . . 4_5645 164.55 162.81 166.93 ? C4 H41 C5 . . . 37.75 37.51 38 ? C4 H41 H82 . . 4_5655 92.5 86.05 97.35 ? C4 H41 H102 . . 4_5645 129.28 125.86 133.08 ? C5 H41 H82 . . 4_5655 73.5 63.78 82.84 ? C5 H41 H102 . . 4_5645 91.91 88.31 96.11 ? H82 H41 H102 4_5655 . 4_5645 58.99 56.81 61.22 ? Si1 H71 C7 . . . 47.96 47.81 48.11 ? Si1 H71 H72 . . . 70.59 70.45 70.7 ? Si1 H71 H73 . . . 70.59 70.45 70.7 ? Si1 H71 H91 . . 7_4545 95.66 89.03 101.15 ? Si1 H71 H93 . . 4_5645 140.86 134.15 148.68 ? C7 H71 H72 . . . 35.26 35.24 35.28 ? C7 H71 H73 . . . 35.26 35.24 35.29 ? C7 H71 H91 . . 7_4545 142.45 135.72 148.44 ? C7 H71 H93 . . 4_5645 114.22 106.06 121.17 ? H72 H71 H73 . . . 60 59.97 60.03 ? H72 H71 H91 . . 7_4545 154.51 151.91 157.4 ? H72 H71 H93 . . 4_5645 116.21 104 126.83 ? H73 H71 H91 . . 7_4545 136.51 132.03 142.03 ? H73 H71 H93 . . 4_5645 80.88 74.18 86.94 ? H91 H71 H93 7_4545 . 4_5645 87.77 76.34 103.79 ? Si1 H72 C7 . . . 47.96 47.81 48.11 ? Si1 H72 C9 . . 6_4545 133.04 119.81 150.52 ? Si1 H72 H71 . . . 70.59 70.46 70.72 ? Si1 H72 H73 . . . 70.59 70.46 70.72 ? Si1 H72 H91 . . 6_4545 123.96 113.85 137.26 ? Si1 H72 H92 . . 6_4545 120.97 106.12 142.37 ? Si1 H72 H93 . . 6_4545 148.61 132.9 167.74 ? Si1 H72 H103 . . 4_5645 93.11 90.88 94.83 ? C7 H72 C9 . . 6_4545 148.23 136.48 162.11 ? C7 H72 H71 . . . 35.26 35.25 35.28 ? C7 H72 H73 . . . 35.26 35.25 35.28 ? C7 H72 H91 . . 6_4545 160.81 146.94 179.43 ? C7 H72 H92 . . 6_4545 133.46 121.62 149.64 ? C7 H72 H93 . . 6_4545 141.73 131.88 153.22 ? C7 H72 H103 . . 4_5645 93.17 92.29 94.1 ? C9 H72 H71 6_4545 . . 114.69 103.43 127.89 ? C9 H72 H73 6_4545 . . 152.19 137.87 163.75 ? C9 H72 H91 6_4545 . 6_4545 17.83 17.27 18.9 ? C9 H72 H92 6_4545 . 6_4545 17.26 16.19 18.76 ? C9 H72 H93 6_4545 . 6_4545 17.45 16.45 18.8 ? C9 H72 H103 6_4545 . 4_5645 114.81 94.43 130.39 ? H71 H72 H73 . . . 60 59.97 60.03 ? H71 H72 H91 . . 6_4545 130.52 118.44 144.44 ? H71 H72 H92 . . 6_4545 101.05 90.96 114.37 ? H71 H72 H93 . . 6_4545 109.61 96.63 123.64 ? H71 H72 H103 . . 4_5645 122.49 121.5 124.3 ? H73 H72 H91 . . 6_4545 160.84 141.2 175.54 ? H73 H72 H92 . . 6_4545 151.93 145.03 160.8 ? H73 H72 H93 . . 6_4545 135.16 120.21 147.47 ? H73 H72 H103 . . 4_5645 62.58 61.59 64.32 ? H91 H72 H92 6_4545 . 6_4545 29.53 27.15 32.06 ? H91 H72 H93 6_4545 . 6_4545 31.46 29.03 34.03 ? H91 H72 H103 6_4545 . 4_5645 103.66 84.52 118.75 ? H92 H72 H93 6_4545 . 6_4545 29.38 26.61 32.12 ? H92 H72 H103 6_4545 . 4_5645 131.46 111.41 145.46 ? H93 H72 H103 6_4545 . 4_5645 108.97 85.17 128.3 ? Si1 H73 C7 . . . 47.96 47.81 48.11 ? Si1 H73 H71 . . . 70.59 70.47 70.72 ? Si1 H73 H72 . . . 70.59 70.47 70.72 ? Si1 H73 H93 . . 4_5645 130.11 120.85 141.45 ? Si1 H73 H103 . . 4_5645 102.21 98.84 104.44 ? C7 H73 H71 . . . 35.26 35.25 35.28 ? C7 H73 H72 . . . 35.26 35.25 35.28 ? C7 H73 H93 . . 4_5645 100.35 95.42 106.51 ? C7 H73 H103 . . 4_5645 115.54 113.76 116.72 ? H71 H73 H72 . . . 60 59.97 60.03 ? H71 H73 H93 . . 4_5645 66.81 61.07 74.22 ? H71 H73 H103 . . 4_5645 146.08 144.77 147.28 ? H72 H73 H93 . . 4_5645 106.42 99.68 112.23 ? H72 H73 H103 . . 4_5645 86.23 85.08 87.34 ? H93 H73 H103 4_5645 . 4_5645 127.29 118.24 135.46 ? Si1 H81 C8 . . . 47.91 47.8 48.05 ? Si1 H81 H82 . . . 70.55 70.45 70.68 ? Si1 H81 H83 . . . 70.55 70.45 70.66 ? Si1 H81 H91 . . 7_4545 96.35 93.85 99.03 ? Si1 H81 H92 . . 4_5545 151.78 146.94 158.38 ? C8 H81 H82 . . . 35.26 35.24 35.29 ? C8 H81 H83 . . . 35.27 35.24 35.29 ? C8 H81 H91 . . 7_4545 142.84 140.51 146.37 ? C8 H81 H92 . . 4_5545 129.79 127.41 133.21 ? H82 H81 H83 . . . 60 59.96 60.04 ? H82 H81 H91 . . 7_4545 136.07 131.85 141.36 ? H82 H81 H92 . . 4_5545 125.48 120.27 129.22 ? H83 H81 H91 . . 7_4545 155.73 153.05 159.62 ? H83 H81 H92 . . 4_5545 96.57 93.38 100.09 ? H91 H81 H92 7_4545 . 4_5545 85.59 79.09 89.75 ? Si1 H82 C4 . . 4_5645 106.34 102.91 108.92 ? Si1 H82 C5 . . 4_5645 109.11 106.84 111.1 ? Si1 H82 C8 . . . 47.91 47.78 48.04 ? Si1 H82 C10 . . 1_5545 163.37 155.38 168.35 ? Si1 H82 H41 . . 4_5645 117.83 111.05 123.98 ? Si1 H82 H81 . . . 70.55 70.43 70.67 ? Si1 H82 H83 . . . 70.55 70.43 70.66 ? Si1 H82 H102 . . 1_5545 167.57 157.57 174.78 ? Si1 H82 H103 . . 1_5545 154.72 141.1 168.96 ? C4 H82 C5 4_5645 . 4_5645 27.46 26.64 28.24 ? C4 H82 C8 4_5645 . . 152.99 147.85 156.91 ? C4 H82 C10 4_5645 . 1_5545 86.18 84.34 88.83 ? C4 H82 H41 4_5645 . 4_5645 18.59 17.85 19.01 ? C4 H82 H81 4_5645 . . 156.97 149.92 163.27 ? C4 H82 H83 4_5645 . . 141.65 133.68 149.7 ? C4 H82 H102 4_5645 . 1_5545 75.19 71.44 78.11 ? C4 H82 H103 4_5645 . 1_5545 85.62 82.46 88.53 ? C5 H82 C8 4_5645 . . 151.03 145.59 156.17 ? C5 H82 C10 4_5645 . 1_5545 79.83 76.73 82.12 ? C5 H82 H41 4_5645 . 4_5645 41.47 40.08 42.83 ? C5 H82 H81 4_5645 . . 130.75 123.42 139.49 ? C5 H82 H83 4_5645 . . 168.84 160.32 175.77 ? C5 H82 H102 4_5645 . 1_5545 76.51 75.09 77.61 ? C5 H82 H103 4_5645 . 1_5545 71.81 66.88 76.04 ? C8 H82 C10 . . 1_5545 118.88 116.37 121.62 ? C8 H82 H41 . . 4_5645 155.97 145.59 167.02 ? C8 H82 H81 . . . 35.26 35.24 35.29 ? C8 H82 H83 . . . 35.26 35.25 35.28 ? C8 H82 H102 . . 1_5545 127.54 126.08 128.89 ? C8 H82 H103 . . 1_5545 119.6 115.54 123.85 ? C10 H82 H41 1_5545 . 4_5645 75.41 72.87 79.35 ? C10 H82 H81 1_5545 . . 95.44 87.06 104.78 ? C10 H82 H83 1_5545 . . 101.72 96.65 107.52 ? C10 H82 H102 1_5545 . 1_5545 17.74 16.78 18.59 ? C10 H82 H103 1_5545 . 1_5545 17.42 15.91 18.42 ? H41 H82 H81 4_5645 . . 168.53 157.68 178.23 ? H41 H82 H83 4_5645 . . 128.34 119.76 137.66 ? H41 H82 H102 4_5645 . 1_5545 61.33 57.61 64.98 ? H41 H82 H103 4_5645 . 1_5545 79.87 76.77 84.22 ? H81 H82 H83 . . . 60 59.97 60.03 ? H81 H82 H102 . . 1_5545 110.91 101.53 120.4 ? H81 H82 H103 . . 1_5545 89.41 81.61 98.61 ? H83 H82 H102 . . 1_5545 101.71 97.11 107.4 ? H83 H82 H103 . . 1_5545 112.39 106.54 118.13 ? H102 H82 H103 1_5545 . 1_5545 32.81 31.27 34.24 ? Si1 H83 C8 . . . 47.91 47.79 48.06 ? Si1 H83 H81 . . . 70.55 70.43 70.67 ? Si1 H83 H82 . . . 70.55 70.44 70.67 ? Si1 H83 H101 . . 4_5545 107.15 90.23 125.57 ? C8 H83 H81 . . . 35.27 35.24 35.29 ? C8 H83 H82 . . . 35.26 35.25 35.28 ? C8 H83 H101 . . 4_5545 152.83 133.08 170.69 ? H81 H83 H82 . . . 60 59.96 60.04 ? H81 H83 H101 . . 4_5545 153.14 140.76 160.85 ? H82 H83 H101 . . 4_5545 140.33 122.12 154.25 ? Si1 H91 C9 . . . 47.93 47.78 48.16 ? Si1 H91 H71 . . 7_4545 127.62 121.8 133.1 ? Si1 H91 H72 . . 6_4445 137.41 133.76 140.27 ? Si1 H91 H81 . . 7_4545 126.94 118.34 135.69 ? Si1 H91 H92 . . . 70.56 70.44 70.76 ? Si1 H91 H93 . . . 70.56 70.44 70.76 ? C9 H91 H71 . . 7_4545 144.51 135.58 154.25 ? C9 H91 H72 . . 6_4445 92.63 86.95 97.29 ? C9 H91 H81 . . 7_4545 143.05 137.62 148.85 ? C9 H91 H92 . . . 35.26 35.26 35.27 ? C9 H91 H93 . . . 35.26 35.25 35.28 ? H71 H91 H72 7_4545 . 6_4445 87.51 77.18 94.7 ? H71 H91 H81 7_4545 . 7_4545 71.29 67.72 74.19 ? H71 H91 H92 7_4545 . . 110.64 102.14 119.66 ? H71 H91 H93 7_4545 . . 156.94 153.82 160.17 ? H72 H91 H81 6_4445 . 7_4545 76.24 64.74 89.07 ? H72 H91 H92 6_4445 . . 81.31 64.95 95.1 ? H72 H91 H93 6_4445 . . 70.97 67.25 77.62 ? H81 H91 H92 7_4545 . . 157.24 151.65 161.97 ? H81 H91 H93 7_4545 . . 109.45 105.86 113.94 ? H92 H91 H93 . . . 60 59.99 60.01 ? Si1 H92 C9 . . . 47.93 47.77 48.15 ? Si1 H92 H72 . . 6_4445 130.72 114.46 152.43 ? Si1 H92 H81 . . 4_5555 145.88 140.28 151.67 ? Si1 H92 H91 . . . 70.56 70.42 70.74 ? Si1 H92 H93 . . . 70.56 70.43 70.75 ? C9 H92 H72 . . 6_4445 82.94 66.84 104.64 ? C9 H92 H81 . . 4_5555 162.51 152.15 170.75 ? C9 H92 H91 . . . 35.26 35.25 35.28 ? C9 H92 H93 . . . 35.26 35.25 35.27 ? H72 H92 H81 6_4445 . 4_5555 81.17 66.79 89 ? H72 H92 H91 6_4445 . . 69.15 57.48 84.83 ? H72 H92 H93 6_4445 . . 65.74 50.75 86.92 ? H81 H92 H91 4_5555 . . 138.8 136.52 142.51 ? H81 H92 H93 4_5555 . . 130.8 118.08 143.25 ? H91 H92 H93 . . . 60 59.98 60.02 ? Si1 H93 C9 . . . 47.93 47.77 48.15 ? Si1 H93 H71 . . 4_5655 116.85 110.89 123.45 ? Si1 H93 H72 . . 6_4445 143.94 131.15 151.46 ? Si1 H93 H73 . . 4_5655 99.78 97.95 102.01 ? Si1 H93 H91 . . . 70.56 70.43 70.75 ? Si1 H93 H92 . . . 70.56 70.43 70.75 ? C9 H93 H71 . . 4_5655 158.98 156.91 161.56 ? C9 H93 H72 . . 6_4445 98.7 84.06 109.46 ? C9 H93 H73 . . 4_5655 128.71 125.46 130.73 ? C9 H93 H91 . . . 35.26 35.25 35.28 ? C9 H93 H92 . . . 35.26 35.26 35.27 ? H71 H93 H72 4_5655 . 6_4445 96.25 86.84 109.03 ? H71 H93 H73 4_5655 . 4_5655 32.31 31.44 33.53 ? H71 H93 H91 4_5655 . . 162.93 159.8 166.12 ? H71 H93 H92 4_5655 . . 134.91 128.92 140.11 ? H72 H93 H73 6_4445 . 4_5655 107.88 100.16 114.09 ? H72 H93 H91 6_4445 . . 77.53 72.88 80.72 ? H72 H93 H92 6_4445 . . 84.86 63.28 102.46 ? H73 H93 H91 4_5655 . . 163.45 159.25 165.92 ? H73 H93 H92 4_5655 . . 104.9 99.45 109.21 ? H91 H93 H92 . . . 60 59.98 60.02 ? S2 H101 C6 . . 4_5555 123.84 117.58 130.19 ? S2 H101 C10 . . . 47.57 47.54 47.65 ? S2 H101 H83 . . 4_5555 83.79 76.39 91.85 ? S2 H101 H102 . . . 70.26 70.22 70.31 ? S2 H101 H103 . . . 70.26 70.22 70.32 ? S2 H101 H111 . . 1_5455 88.57 87.41 89.73 ? C6 H101 C10 4_5555 . . 165.37 153.67 177.23 ? C6 H101 H83 4_5555 . 4_5555 55.65 39.62 69.62 ? C6 H101 H102 4_5555 . . 135.99 125.94 147.61 ? C6 H101 H103 4_5555 . . 158.73 143.99 170.78 ? C6 H101 H111 4_5555 . 1_5455 60.68 42.72 80.87 ? C10 H101 H83 . . 4_5555 124.47 107.42 139.17 ? C10 H101 H102 . . . 35.26 35.25 35.27 ? C10 H101 H103 . . . 35.26 35.26 35.27 ? C10 H101 H111 . . 1_5455 105.66 100.63 111.2 ? H83 H101 H102 4_5555 . . 148.84 142.12 154.19 ? H83 H101 H103 4_5555 . . 116.63 92.37 139.66 ? H83 H101 H111 4_5555 . 1_5455 93.34 64.57 122.66 ? H102 H101 H103 . . . 60 59.99 60.01 ? H102 H101 H111 . . 1_5455 80.89 74.4 88 ? H103 H101 H111 . . 1_5455 139.6 133.73 145.95 ? S1 H102 S2 . . . 76.36 74.63 77.84 ? S1 H102 C2 . . . 34.67 34.38 35.05 ? S1 H102 C3 . . . 57.78 57.45 58.05 ? S1 H102 C10 . . . 123.81 122.19 125.15 ? S1 H102 H41 . . 4_5655 70.73 68.97 71.9 ? S1 H102 H82 . . 1_5565 129.02 123.26 133.22 ? S1 H102 H101 . . . 136.57 134.13 138.63 ? S1 H102 H103 . . . 131.35 131.19 131.54 ? S1 H102 H111 . . 1_5455 79.36 78.59 80.23 ? S2 H102 C2 . . . 61.7 60.94 62.22 ? S2 H102 C3 . . . 37.4 37.09 37.86 ? S2 H102 C10 . . . 47.57 47.53 47.64 ? S2 H102 H41 . . 4_5655 127.11 121.19 132.5 ? S2 H102 H82 . . 1_5565 140.99 130.58 152.41 ? S2 H102 H101 . . . 70.26 70.22 70.31 ? S2 H102 H103 . . . 70.26 70.22 70.32 ? S2 H102 H111 . . 1_5455 85.32 82.05 88.66 ? C2 H102 C3 . . . 28.57 28.23 28.83 ? C2 H102 C10 . . . 101.21 101.09 101.4 ? C2 H102 H41 . . 4_5655 67.72 62.98 72.06 ? C2 H102 H82 . . 1_5565 119.57 117.37 121.31 ? C2 H102 H101 . . . 131.65 131.05 132 ? C2 H102 H103 . . . 97.25 96.44 97.98 ? C2 H102 H111 . . 1_5455 108.56 107.84 109.36 ? C3 H102 C10 . . . 72.66 72.52 72.88 ? C3 H102 H41 . . 4_5655 89.73 83.4 95.23 ? C3 H102 H82 . . 1_5565 124.7 118.36 130.32 ? C3 H102 H101 . . . 104.25 104.04 104.59 ? C3 H102 H103 . . . 74.41 74.32 74.49 ? C3 H102 H111 . . 1_5455 110.95 109.39 112.41 ? C10 H102 H41 . . 4_5655 137.12 134.1 139.66 ? C10 H102 H82 . . 1_5565 99.31 89.67 110.36 ? C10 H102 H101 . . . 35.26 35.26 35.27 ? C10 H102 H103 . . . 35.26 35.26 35.27 ? C10 H102 H111 . . 1_5455 96.81 92.38 101.19 ? H41 H102 H82 4_5655 . 1_5565 59.69 57.86 61.65 ? H41 H102 H101 4_5655 . . 152.51 149.47 156.43 ? H41 H102 H103 4_5655 . . 103.02 100.52 104.99 ? H41 H102 H111 4_5655 . 1_5455 125.87 119.94 132 ? H82 H102 H101 1_5565 . . 93.85 88.11 100.82 ? H82 H102 H103 1_5565 . . 71 60.56 82.61 ? H82 H102 H111 1_5565 . 1_5455 124.15 119.46 129.22 ? H101 H102 H103 . . . 60 60 60 ? H101 H102 H111 . . 1_5455 71.09 67.09 74.97 ? H103 H102 H111 . . 1_5455 130.1 125.81 134.31 ? S2 H103 C3 . . . 37.4 37.09 37.86 ? S2 H103 C10 . . . 47.57 47.53 47.64 ? S2 H103 H72 . . 4_5655 128.13 123.72 133.32 ? S2 H103 H73 . . 4_5655 97.74 94.37 102.33 ? S2 H103 H82 . . 1_5565 146.15 134.94 157.87 ? S2 H103 H101 . . . 70.26 70.22 70.31 ? S2 H103 H102 . . . 70.26 70.22 70.32 ? C3 H103 C10 . . . 72.66 72.53 72.89 ? C3 H103 H72 . . 4_5655 113.84 109.31 119.21 ? C3 H103 H73 . . 4_5655 85.49 80.55 90.77 ? C3 H103 H82 . . 1_5565 127.61 120.39 133.67 ? C3 H103 H101 . . . 104.25 104.04 104.6 ? C3 H103 H102 . . . 74.41 74.31 74.5 ? C10 H103 H72 . . 4_5655 162.64 159.87 165.47 ? C10 H103 H73 . . 4_5655 143.03 140.81 147.07 ? C10 H103 H82 . . 1_5565 104.13 93.88 115.37 ? C10 H103 H101 . . . 35.26 35.26 35.27 ? C10 H103 H102 . . . 35.26 35.26 35.27 ? H72 H103 H73 4_5655 . 4_5655 31.19 29.95 32.89 ? H72 H103 H82 4_5655 . 1_5565 84.46 74.91 92.25 ? H72 H103 H101 4_5655 . . 130.21 126.01 132.63 ? H72 H103 H102 4_5655 . . 159.23 155.11 162.08 ? H73 H103 H82 4_5655 . 1_5565 112.71 102.93 119.25 ? H73 H103 H101 4_5655 . . 133.66 129.32 136.01 ? H73 H103 H102 4_5655 . . 158.74 153.78 164.17 ? H82 H103 H101 1_5565 . . 96.68 90.91 103.59 ? H82 H103 H102 1_5565 . . 76.2 64.95 88.13 ? H101 H103 H102 . . . 60 59.99 60.01 ? S2 H111 O1 4_5655 . . 143.35 136.93 148.77 ? S2 H111 O1 4_5655 . 2_5555 101.42 94.88 107.06 ? S2 H111 C1 4_5655 . . 120.49 118.33 121.87 ? S2 H111 C1 4_5655 . 2_5555 106.73 103.46 108.77 ? S2 H111 C5 4_5655 . 4_5655 60.44 57.79 62.73 ? S2 H111 C11 4_5655 . . 167.03 158.12 174.93 ? S2 H111 C11 4_5655 . 2_5555 123.4 114.65 131.45 ? S2 H111 H101 4_5655 . 1_5655 79.02 71.34 86.52 ? S2 H111 H102 4_5655 . 1_5655 77.42 71.31 82.61 ? S2 H111 H111 4_5655 . 2_5555 137.16 128.36 145.23 ? S2 H111 H112 4_5655 . . 145.98 144.23 147.4 ? S2 H111 H112 4_5655 . 2_5555 107.69 98.68 116.37 ? O1 H111 O1 . . 2_5555 76.72 76.42 76.93 ? O1 H111 C1 . . . 30.04 29.63 30.35 ? O1 H111 C1 . . 2_5555 55.99 55.8 56.27 ? O1 H111 C5 . . 4_5655 84.51 79.74 89.28 ? O1 H111 C11 . . . 43.48 43.33 43.58 ? O1 H111 C11 . . 2_5555 74.46 74.01 74.85 ? O1 H111 H101 . . 1_5655 108.1 97.69 116.47 ? O1 H111 H102 . . 1_5655 124.66 119.37 127.7 ? O1 H111 H111 . . 2_5555 63.75 63.37 64.09 ? O1 H111 H112 . . . 67.11 66.88 67.29 ? O1 H111 H112 . . 2_5555 97.43 96.89 97.92 ? O1 H111 C1 2_5555 . . 55.26 55.1 55.39 ? O1 H111 C1 2_5555 . 2_5555 27.85 27.75 27.99 ? O1 H111 C5 2_5555 . 4_5655 104.69 101.46 107.06 ? O1 H111 C11 2_5555 . . 68.06 67.8 68.24 ? O1 H111 C11 2_5555 . 2_5555 33.52 33.46 33.58 ? O1 H111 H101 2_5555 . 1_5655 164.88 148.53 179.6 ? O1 H111 H102 2_5555 . 1_5655 141.18 124.13 158.81 ? O1 H111 H111 2_5555 . 2_5555 43.07 42.92 43.17 ? O1 H111 H112 2_5555 . . 99.27 99.15 99.34 ? O1 H111 H112 2_5555 . 2_5555 47.12 47.06 47.18 ? C1 H111 C1 . . 2_5555 29.03 28.75 29.3 ? C1 H111 C5 . . 4_5655 73.52 71.74 75.21 ? C1 H111 C11 . . . 60.22 59.49 60.78 ? C1 H111 C11 . . 2_5555 69.09 68.77 69.26 ? C1 H111 H101 . . 1_5655 132.47 116.41 145.86 ? C1 H111 H102 . . 1_5655 152.96 144.81 157.7 ? C1 H111 H111 . . 2_5555 64.7 64.25 65.03 ? C1 H111 H112 . . . 92.78 92.32 93.09 ? C1 H111 H112 . . 2_5555 92.97 92.69 93.17 ? C1 H111 C5 2_5555 . 4_5655 83.68 82.06 84.71 ? C1 H111 C11 2_5555 . . 67.61 67 68.34 ? C1 H111 C11 2_5555 . 2_5555 52.61 52.38 52.85 ? C1 H111 H101 2_5555 . 1_5655 159.31 142.84 170.96 ? C1 H111 H102 2_5555 . 1_5655 165.51 150.53 178.18 ? C1 H111 H111 2_5555 . 2_5555 55.35 54.93 55.74 ? C1 H111 H112 2_5555 . . 103.82 103.51 104.24 ? C1 H111 H112 2_5555 . 2_5555 72.58 72.41 72.79 ? C5 H111 C11 4_5655 . . 127.92 123.29 132.39 ? C5 H111 C11 4_5655 . 2_5555 135.99 133.96 137.23 ? C5 H111 H101 4_5655 . 1_5655 85.14 63.62 107.01 ? C5 H111 H102 4_5655 . 1_5655 107.86 90.08 124.96 ? C5 H111 H111 4_5655 . 2_5555 137.09 135.89 138.19 ? C5 H111 H112 4_5655 . . 137.2 131.38 143.61 ? C5 H111 H112 4_5655 . 2_5555 149.21 144.24 153.06 ? C11 H111 C11 . . 2_5555 43.88 43.85 43.9 ? C11 H111 H101 . . 1_5655 108.31 100.57 114.07 ? C11 H111 H102 . . 1_5655 104.65 95.35 113.31 ? C11 H111 H111 . . 2_5555 30.08 30.05 30.11 ? C11 H111 H112 . . . 36.24 35.89 36.55 ? C11 H111 H112 . . 2_5555 59.96 59.75 60.22 ? C11 H111 H101 2_5555 . 1_5655 136.92 118.88 153.37 ? C11 H111 H102 2_5555 . 1_5655 115.24 98.27 132.72 ? C11 H111 H111 2_5555 . 2_5555 13.8 13.79 13.8 ? C11 H111 H112 2_5555 . . 67.43 67.34 67.55 ? C11 H111 H112 2_5555 . 2_5555 24.32 24.25 24.39 ? H101 H111 H102 1_5655 . 1_5655 28.01 24.88 30.64 ? H101 H111 H111 1_5655 . 2_5555 129.19 114.26 141.79 ? H101 H111 H112 1_5655 . . 75.32 64.69 85.94 ? H101 H111 H112 1_5655 . 2_5555 122.03 101.58 142.65 ? H102 H111 H111 1_5655 . 2_5555 113.16 97.71 128.7 ? H102 H111 H112 1_5655 . . 69.45 62.45 77.21 ? H102 H111 H112 1_5655 . 2_5555 95.44 77.99 113.68 ? H111 H111 H112 2_5555 . . 56.22 56.05 56.39 ? H111 H111 H112 2_5555 . 2_5555 33.71 33.54 33.87 ? H112 H111 H112 . . 2_5555 69.15 68.98 69.41 ? S1 H112 S2 1_5655 . 1_5655 64.86 58.98 68.52 ? S1 H112 O1 1_5655 . . 164.36 149.24 177.41 ? S1 H112 C11 1_5655 . . 126.37 116.09 135.86 ? S1 H112 C11 1_5655 . 2_5555 92.27 77.01 108.73 ? S1 H112 H111 1_5655 . . 110.49 108.82 111.72 ? S1 H112 H111 1_5655 . 2_5555 92.42 75.36 111 ? S1 H112 H112 1_5655 . 2_5555 68.78 54.8 84.24 ? S2 H112 O1 1_5655 . . 127.26 107.64 146.11 ? S2 H112 C11 1_5655 . . 153.33 135.65 167.95 ? S2 H112 C11 1_5655 . 2_5555 156.62 135.35 175.44 ? S2 H112 H111 1_5655 . . 121.5 109.58 133.03 ? S2 H112 H111 1_5655 . 2_5555 143.86 124.42 159.66 ? S2 H112 H112 1_5655 . 2_5555 133.23 113.68 151.67 ? O1 H112 C11 . . . 43.48 43.33 43.58 ? O1 H112 C11 . . 2_5555 74.46 74 74.85 ? O1 H112 H111 . . . 67.11 66.87 67.28 ? O1 H112 H111 . . 2_5555 74.25 74 74.48 ? O1 H112 H112 . . 2_5555 98.56 98.1 98.88 ? C11 H112 C11 . . 2_5555 43.88 43.85 43.91 ? C11 H112 H111 . . . 36.24 35.89 36.55 ? C11 H112 H111 . . 2_5555 59.96 59.75 60.23 ? C11 H112 H112 . . 2_5555 61.83 61.78 61.88 ? C11 H112 H111 2_5555 . . 67.43 67.33 67.55 ? C11 H112 H111 2_5555 . 2_5555 24.32 24.24 24.39 ? C11 H112 H112 2_5555 . 2_5555 24.8 24.77 24.83 ? H111 H112 H111 . . 2_5555 90.07 90.05 90.09 ? H111 H112 H112 . . 2_5555 71.55 71.42 71.65 ? H111 H112 H112 2_5555 . 2_5555 39.3 39.14 39.43 ? # start Validation Reply Form #_vrf_SYMM004_ESEM #; #PROBLEM: _symmetry_equiv_pos_as_xyz loop is missing. #RESPONSE: This CIF describes an incommensurate structure #refined using the superspace approach. Instead of #a _symmetry_equiv_pos_as_xyz loop, there is a #_space_group_symop_ssg_operation_algebraic loop. #; #_vrf_GEOM003_ESEM #; #PROBLEM: _geom_bond_distance is missing #RESPONSE: This CIF describes an incommensurate structure #refined using the superspace approach. Instead of #_geom_bond_distance there is _geom_bond_distance_av #; # end Validation Reply Form #======================================================================= data_ESEMOX _publcif_datablock.id '{b8d27531-a09f-47d8-88d1-ccb022778054}' _database_code_depnum_ccdc_archive 'CCDC 928108' #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C22 H30 O8 S3 Si2' _chemical_formula_weight 574.8 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _space_group_IT_number 2 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 10.5399(4) _cell_length_b 13.8276(5) _cell_length_c 19.9987(8) _cell_angle_alpha 79.940(2) _cell_angle_beta 84.589(2) _cell_angle_gamma 89.771(2) _cell_volume 2856.81(19) loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.6092(7) 1 0 0 0 1 0 0 0 1 2 0.3908(7) 1 0 0 0 1 0 0 0 1 _cell_formula_units_Z 4 _cell_measurement_reflns_used 9905 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 30.0 _cell_measurement_temperature 100 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 1.3361 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.385 _exptl_crystal_description block _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.28 _exptl_crystal_size_rad ? _exptl_crystal_colour 'clear yellow' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details TWINABS _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.90 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\w- and \f-scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 57022 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 30.08 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_max 0.85 _diffrn_measured_fraction_theta_full 0.85 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 13689 _reflns_number_gt 11291 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_gt 0.0413 _refine_ls_R_factor_all 0.0530 _refine_ls_wR_factor_ref 0.0422 _refine_ls_goodness_of_fit_ref 1.96 _refine_ls_goodness_of_fit_gt 2.12 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 13689 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_number_constraints 240 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0169 _refine_ls_shift/su_mean 0.0022 _refine_diff_density_max 0.45 _refine_diff_density_min -0.60 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.77446(6) 0.50526(5) 0.50468(3) Uani 0.00908(17) 2 1 d . . . S2 S 0.72955(6) 0.28490(5) 0.68127(3) Uani 0.01225(18) 2 1 d . . . S3 S 0.70884(6) 0.45411(5) 0.31639(3) Uani 0.01340(19) 2 1 d . . . Si1 Si 0.73015(8) 0.46365(6) 0.88964(4) Uani 0.0215(2) 2 1 d . . . Si2 Si 0.77675(7) 0.78808(5) 0.13862(4) Uani 0.0174(2) 2 1 d . . . O1 O 0.63794(16) 0.50577(13) 0.50937(9) Uani 0.0139(5) 2 1 d . . . O2 O 0.83646(17) 0.59553(12) 0.51035(9) Uani 0.0136(5) 2 1 d . . . O3 O 0.69837(18) 0.22703(13) 0.63194(9) Uani 0.0190(6) 2 1 d . . . O4 O 0.63009(18) 0.30754(14) 0.73025(9) Uani 0.0208(6) 2 1 d . . . O5 O 0.68168(19) 0.35776(13) 0.35553(9) Uani 0.0181(6) 2 1 d . . . O6 O 0.7624(2) 0.46391(13) 0.24688(8) Uani 0.0225(6) 2 1 d . . . O7 O 0.94381(17) 0.26061(13) 0.55024(9) Uani 0.0133(5) 2 1 d . . . O8 O 0.94873(17) 0.32328(13) 0.40531(8) Uani 0.0134(5) 2 1 d . . . C1 C 0.8278(2) 0.40505(17) 0.56135(11) Uani 0.0096(7) 2 1 d . . . C2 C 0.8891(2) 0.34330(18) 0.52422(12) Uani 0.0104(7) 2 1 d . . . C3 C 0.8917(2) 0.37629(18) 0.44905(11) Uani 0.0099(7) 2 1 d . . . C4 C 0.8360(2) 0.46291(17) 0.43038(11) Uani 0.0101(7) 2 1 d . . . C5 C 0.7977(2) 0.39934(18) 0.63469(12) Uani 0.0107(7) 2 1 d . . . C6 C 0.8094(3) 0.4775(2) 0.66580(12) Uani 0.0158(8) 2 1 d . . . C7 C 0.7792(3) 0.47980(19) 0.73616(13) Uani 0.0174(8) 2 1 d . . . C8 C 0.7581(3) 0.4822(2) 0.79588(13) Uani 0.0216(8) 2 1 d . . . C9 C 0.6975(3) 0.5826(2) 0.91799(14) Uani 0.0308(10) 2 1 d . . . C10 C 0.8774(3) 0.4057(2) 0.92168(14) Uani 0.0353(11) 2 1 d . . . C11 C 0.5893(3) 0.3807(3) 0.91452(16) Uani 0.0477(13) 2 1 d . . . C12 C 0.8555(3) 0.22896(19) 0.72503(13) Uani 0.0185(8) 2 1 d . . . C13 C 0.8121(2) 0.51567(19) 0.36293(12) Uani 0.0120(7) 2 1 d . . . C14 C 0.8550(3) 0.60775(19) 0.33840(12) Uani 0.0159(8) 2 1 d . . . C16 C 0.8149(3) 0.7163(2) 0.22126(14) Uani 0.0203(8) 2 1 d . . . C17 C 0.7621(3) 0.6986(2) 0.08047(13) Uani 0.0318(10) 2 1 d . . . C18 C 0.6251(3) 0.8519(2) 0.15529(15) Uani 0.0347(11) 2 1 d . . . C19 C 0.9085(3) 0.8763(2) 0.10448(14) Uani 0.0306(10) 2 1 d . . . C20 C 0.5678(3) 0.5227(2) 0.31944(16) Uani 0.0240(10) 2 1 d . . . C21 C 1.0181(2) 0.20990(18) 0.50112(12) Uani 0.0126(8) 2 1 d . . . C22 C 0.9577(2) 0.22063(18) 0.43555(12) Uani 0.0134(8) 2 1 d . . . S1' S 0.27679(6) -0.00255(5) 0.49149(3) Uani 0.00893(17) 2 1 d . . . S2' S 0.28833(6) 0.21795(5) 0.31683(3) Uani 0.01156(18) 2 1 d . . . S3' S 0.14566(6) 0.04680(5) 0.68106(3) Uani 0.01244(18) 2 1 d . . . Si1' Si 0.30584(7) 0.03475(6) 0.11211(4) Uani 0.0203(2) 2 1 d . . . Si2' Si 0.19676(7) -0.27944(5) 0.86443(4) Uani 0.0167(2) 2 1 d . . . O1' O 0.14226(16) -0.00283(13) 0.48582(9) Uani 0.0136(5) 2 1 d . . . O2' O 0.34163(17) -0.09336(12) 0.48609(8) Uani 0.0132(5) 2 1 d . . . O3' O 0.24510(19) 0.27617(13) 0.36705(9) Uani 0.0186(6) 2 1 d . . . O4' O 0.19992(19) 0.19658(13) 0.27087(9) Uani 0.0215(6) 2 1 d . . . O5' O 0.12938(18) 0.14279(13) 0.64233(9) Uani 0.0173(6) 2 1 d . . . O6' O 0.17568(19) 0.03684(14) 0.75025(9) Uani 0.0216(6) 2 1 d . . . O7' O 0.46459(17) 0.24060(13) 0.44665(9) Uani 0.0123(5) 2 1 d . . . O8' O 0.41642(17) 0.17646(13) 0.59155(8) Uani 0.0121(5) 2 1 d . . . C1' C 0.3515(2) 0.09766(17) 0.43512(11) Uani 0.0102(7) 2 1 d . . . C2' C 0.3993(2) 0.15833(17) 0.47250(12) Uani 0.0090(7) 2 1 d . . . C3' C 0.3739(2) 0.12513(17) 0.54768(11) Uani 0.0095(7) 2 1 d . . . C4' C 0.3107(2) 0.03982(18) 0.56544(11) Uani 0.0104(7) 2 1 d . . . C5' C 0.3440(2) 0.10389(19) 0.36218(12) Uani 0.0112(7) 2 1 d . . . C6' C 0.3662(3) 0.0254(2) 0.33070(13) Uani 0.0139(8) 2 1 d . . . C8' C 0.3400(3) 0.01869(19) 0.20214(13) Uani 0.0184(8) 2 1 d . . . C9' C 0.2865(3) -0.0869(2) 0.08727(14) Uani 0.0324(10) 2 1 d . . . C10' C 0.4417(3) 0.1055(2) 0.06023(14) Uani 0.0364(11) 2 1 d . . . C11' C 0.1554(3) 0.1050(2) 0.10728(16) Uani 0.0371(11) 2 1 d . . . C12' C 0.4254(3) 0.2734(2) 0.26954(13) Uani 0.0213(9) 2 1 d . . . C13' C 0.2651(2) -0.01347(18) 0.63340(12) Uani 0.0109(7) 2 1 d . . . C14' C 0.3040(3) -0.10497(19) 0.65748(12) Uani 0.0145(8) 2 1 d . . . C15' C 0.2663(3) -0.16141(19) 0.72263(13) Uani 0.0167(8) 2 1 d . . . C16' C 0.2406(3) -0.21094(19) 0.77773(13) Uani 0.0181(8) 2 1 d . . . C17' C 0.1849(3) -0.1861(2) 0.92211(13) Uani 0.0292(10) 2 1 d . . . C18' C 0.0430(3) -0.3425(2) 0.86290(14) Uani 0.0296(10) 2 1 d . . . C19' C 0.3258(3) -0.3678(2) 0.88686(13) Uani 0.0271(9) 2 1 d . . . C20' C 0.0072(3) -0.0226(2) 0.67931(15) Uani 0.0235(10) 2 1 d . . . C21' C 0.5206(2) 0.29058(18) 0.49552(11) Uani 0.0115(8) 2 1 d . . . C22' C 0.4373(2) 0.27986(18) 0.56154(13) Uani 0.0137(8) 2 1 d . . . C7' C 0.3514(3) 0.02275(19) 0.26087(13) Uani 0.0169(8) 2 1 d . . . C15 C 0.8318(3) 0.66538(19) 0.27472(13) Uani 0.0177(8) 2 1 d . . . H61 H 0.841285 0.537395 0.637558 Uiso 0.0189 2 1 d . . . H121 H 0.926349 0.220674 0.692785 Uiso 0.0222 2 1 d . . . H122 H 0.880999 0.269743 0.755765 Uiso 0.0222 2 1 d . . . H123 H 0.827683 0.165972 0.750415 Uiso 0.0222 2 1 d . . . H141 H 0.906227 0.637434 0.366711 Uiso 0.019 2 1 d . . . H201 H 0.534594 0.520181 0.366104 Uiso 0.0288 2 1 d . . . H202 H 0.586028 0.589768 0.298533 Uiso 0.0288 2 1 d . . . H203 H 0.505954 0.495661 0.295344 Uiso 0.0288 2 1 d . . . H211 H 1.023673 0.141481 0.520172 Uiso 0.0151 2 1 d . . . H212 H 1.103068 0.236833 0.492465 Uiso 0.0151 2 1 d . . . H221 H 1.007512 0.186769 0.404393 Uiso 0.016 2 1 d . . . H222 H 0.873963 0.191396 0.443939 Uiso 0.016 2 1 d . . . H61' H 0.394411 -0.033582 0.35779 Uiso 0.0167 2 1 d . . . H121' H 0.463513 0.229615 0.241257 Uiso 0.0256 2 1 d . . . H122' H 0.402895 0.333308 0.241373 Uiso 0.0256 2 1 d . . . H123' H 0.485085 0.287515 0.300081 Uiso 0.0256 2 1 d . . . H141' H 0.36283 -0.134707 0.627706 Uiso 0.0174 2 1 d . . . H201' H -0.0173 -0.013174 0.6336 Uiso 0.0282 2 1 d . . . H202' H 0.023536 -0.09093 0.694391 Uiso 0.0282 2 1 d . . . H203' H -0.060429 -0.001739 0.708979 Uiso 0.0282 2 1 d . . . H211' H 0.532612 0.359005 0.476564 Uiso 0.0138 2 1 d . . . H212' H 0.602894 0.263686 0.503921 Uiso 0.0138 2 1 d . . . H221' H 0.476744 0.312748 0.592833 Uiso 0.0165 2 1 d . . . H222' H 0.356767 0.310281 0.553566 Uiso 0.0165 2 1 d . . . H91 H 0.676202 0.571441 0.966485 Uiso 0.037 2 1 d . . . H92 H 0.771835 0.62422 0.906554 Uiso 0.037 2 1 d . . . H93 H 0.627525 0.613724 0.895642 Uiso 0.037 2 1 d . . . H101 H 0.879333 0.410797 0.968831 Uiso 0.0424 2 1 d . . . H102 H 0.877985 0.337667 0.917178 Uiso 0.0424 2 1 d . . . H103 H 0.950736 0.438592 0.895583 Uiso 0.0424 2 1 d . . . H111 H 0.575696 0.364792 0.963355 Uiso 0.0572 2 1 d . . . H112 H 0.515403 0.412816 0.896921 Uiso 0.0572 2 1 d . . . H113 H 0.603799 0.321493 0.896143 Uiso 0.0572 2 1 d . . . H171 H 0.724472 0.729983 0.040514 Uiso 0.0382 2 1 d . . . H172 H 0.845087 0.675226 0.067404 Uiso 0.0382 2 1 d . . . H173 H 0.709163 0.644199 0.103419 Uiso 0.0382 2 1 d . . . H181 H 0.593011 0.879047 0.112733 Uiso 0.0416 2 1 d . . . H182 H 0.563911 0.805922 0.18177 Uiso 0.0416 2 1 d . . . H183 H 0.639853 0.903725 0.180012 Uiso 0.0416 2 1 d . . . H191 H 0.890664 0.912029 0.060798 Uiso 0.0367 2 1 d . . . H192 H 0.91644 0.921436 0.135342 Uiso 0.0367 2 1 d . . . H193 H 0.986682 0.8413 0.099588 Uiso 0.0367 2 1 d . . . H91' H 0.264627 -0.078175 0.041095 Uiso 0.0389 2 1 d . . . H92' H 0.364978 -0.122158 0.090774 Uiso 0.0389 2 1 d . . . H93' H 0.219983 -0.123507 0.117068 Uiso 0.0389 2 1 d . . . H101' H 0.426218 0.116377 0.01297 Uiso 0.0437 2 1 d . . . H102' H 0.450149 0.167507 0.07479 Uiso 0.0437 2 1 d . . . H103' H 0.518702 0.069011 0.066156 Uiso 0.0437 2 1 d . . . H111' H 0.126984 0.108764 0.062697 Uiso 0.0445 2 1 d . . . H112' H 0.091431 0.072418 0.140939 Uiso 0.0445 2 1 d . . . H113' H 0.170095 0.170079 0.115716 Uiso 0.0445 2 1 d . . . H171' H 0.167002 -0.21871 0.968521 Uiso 0.035 2 1 d . . . H172' H 0.264118 -0.150412 0.91741 Uiso 0.035 2 1 d . . . H173' H 0.117599 -0.141383 0.909996 Uiso 0.035 2 1 d . . . H181' H 0.011375 -0.371645 0.90854 Uiso 0.0355 2 1 d . . . H182' H -0.017356 -0.295848 0.843937 Uiso 0.0355 2 1 d . . . H183' H 0.055108 -0.392828 0.835427 Uiso 0.0355 2 1 d . . . H191' H 0.30482 -0.404461 0.931921 Uiso 0.0325 2 1 d . . . H192' H 0.33473 -0.412095 0.854745 Uiso 0.0325 2 1 d . . . H193' H 0.404552 -0.33255 0.885491 Uiso 0.0325 2 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 S 0.0082(3) 0.0069(3) 0.0123(3) 0.0004(3) -0.0026(2) -0.0011(2) S2 S 0.0105(3) 0.0123(3) 0.0131(3) -0.0007(3) -0.0001(3) -0.0004(2) S3 S 0.0142(3) 0.0129(3) 0.0141(3) -0.0003(3) -0.0040(3) -0.0037(2) Si1 Si 0.0241(4) 0.0273(4) 0.0132(3) -0.0038(4) 0.0017(3) -0.0055(3) Si2 Si 0.0196(4) 0.0175(3) 0.0143(3) -0.0006(3) -0.0055(3) 0.0017(3) O1 O 0.0041(8) 0.0140(9) 0.0240(9) 0.0020(8) -0.0034(8) -0.0031(7) O2 O 0.0133(10) 0.0071(8) 0.0204(9) -0.0018(8) -0.0025(8) -0.0016(7) O3 O 0.0216(11) 0.0170(10) 0.0182(9) -0.0098(9) -0.0031(8) -0.0020(8) O4 O 0.0146(10) 0.0205(10) 0.0245(10) -0.0014(8) 0.0068(8) -0.0010(8) O5 O 0.0228(11) 0.0120(9) 0.0196(9) -0.0031(8) -0.0046(8) -0.0015(7) O6 O 0.0341(12) 0.0215(10) 0.0126(9) -0.0048(10) -0.0009(9) -0.0057(8) O7 O 0.0140(10) 0.0107(9) 0.0147(9) 0.0063(7) -0.0014(7) -0.0011(7) O8 O 0.0165(10) 0.0097(9) 0.0139(8) 0.0019(7) -0.0010(7) -0.0025(7) C1 C 0.0078(12) 0.0091(12) 0.0114(11) 0.0002(10) -0.0008(9) -0.0008(9) C2 C 0.0071(12) 0.0107(12) 0.0131(11) -0.0021(11) -0.0013(10) -0.0009(10) C3 C 0.0066(12) 0.0123(12) 0.0107(11) -0.0018(10) 0.0010(9) -0.0025(9) C4 C 0.0095(12) 0.0099(12) 0.0111(11) -0.0010(10) -0.0024(10) -0.0016(9) C5 C 0.0081(13) 0.0110(12) 0.0123(11) 0.0013(10) -0.0002(10) -0.0004(10) C6 C 0.0187(15) 0.0156(14) 0.0119(12) 0.0018(12) -0.0011(11) 0.0003(10) C7 C 0.0212(15) 0.0123(12) 0.0191(12) -0.0006(11) -0.0018(11) -0.0034(10) C8 C 0.0268(16) 0.0190(14) 0.0198(13) 0.0000(12) -0.0025(12) -0.0058(11) C9 C 0.0236(17) 0.0444(18) 0.0283(14) -0.0001(14) -0.0011(13) -0.0175(13) C10 C 0.043(2) 0.0359(17) 0.0242(14) 0.0092(16) -0.0048(14) 0.0036(13) C11 C 0.048(2) 0.057(2) 0.0379(18) -0.022(2) 0.0061(17) -0.0127(17) C12 C 0.0165(14) 0.0170(13) 0.0201(13) 0.0006(12) -0.0039(11) 0.0032(11) C13 C 0.0090(13) 0.0146(13) 0.0116(11) -0.0010(11) -0.0011(10) -0.0002(10) C14 C 0.0145(14) 0.0181(14) 0.0152(12) -0.0020(11) -0.0058(11) -0.0011(11) C16 C 0.0185(15) 0.0179(14) 0.0231(13) -0.0019(11) -0.0037(11) 0.0013(11) C17 C 0.0358(19) 0.0321(16) 0.0303(15) -0.0038(14) -0.0126(14) -0.0079(13) C18 C 0.0338(18) 0.0419(19) 0.0302(16) 0.0131(15) -0.0118(14) -0.0068(14) C19 C 0.040(2) 0.0295(16) 0.0210(13) -0.0088(15) 0.0023(13) -0.0031(12) C20 C 0.0155(16) 0.0200(16) 0.0405(18) 0.0039(13) -0.0129(14) -0.0112(14) C21 C 0.0103(14) 0.0078(12) 0.0195(13) 0.0002(10) 0.0012(10) -0.0037(10) C22 C 0.0142(14) 0.0088(13) 0.0175(12) 0.0000(10) -0.0008(10) -0.0036(10) S1' S 0.0083(3) 0.0072(3) 0.0114(3) -0.0013(3) -0.0017(2) -0.0015(2) S2' S 0.0110(3) 0.0109(3) 0.0123(3) 0.0004(3) -0.0018(2) -0.0003(2) S3' S 0.0135(3) 0.0121(3) 0.0119(3) -0.0001(3) 0.0004(3) -0.0035(2) Si1' Si 0.0197(4) 0.0289(4) 0.0131(3) 0.0019(3) -0.0031(3) -0.0052(3) Si2' Si 0.0176(4) 0.0172(4) 0.0135(3) -0.0007(3) 0.0002(3) 0.0013(3) O1' O 0.0078(9) 0.0107(9) 0.0225(9) -0.0030(8) 0.0002(7) -0.0043(7) O2' O 0.0152(10) 0.0076(8) 0.0167(8) 0.0003(8) -0.0002(8) -0.0028(7) O3' O 0.0215(11) 0.0159(10) 0.0183(9) 0.0072(9) -0.0011(8) -0.0038(8) O4' O 0.0227(11) 0.0187(10) 0.0252(10) 0.0003(9) -0.0143(9) -0.0031(8) O5' O 0.0175(10) 0.0154(10) 0.0186(9) 0.0053(8) -0.0021(8) -0.0018(8) O6' O 0.0308(12) 0.0210(10) 0.0139(9) 0.0016(9) -0.0019(9) -0.0055(8) O7' O 0.0144(10) 0.0076(9) 0.0144(8) -0.0061(7) -0.0014(7) -0.0005(7) O8' O 0.0137(9) 0.0106(9) 0.0130(8) -0.0024(7) -0.0035(7) -0.0031(7) C1' C 0.0087(12) 0.0087(12) 0.0120(11) 0.0005(10) 0.0000(9) 0.0011(9) C2' C 0.0070(12) 0.0051(11) 0.0139(11) -0.0006(10) 0.0000(10) 0.0005(9) C3' C 0.0086(12) 0.0073(12) 0.0130(11) 0.0010(10) -0.0009(10) -0.0033(9) C4' C 0.0109(13) 0.0116(12) 0.0096(10) 0.0006(10) -0.0016(9) -0.0040(9) C5' C 0.0083(13) 0.0124(12) 0.0121(11) -0.0022(10) -0.0003(10) -0.0005(10) C6' C 0.0141(14) 0.0131(13) 0.0153(12) -0.0019(11) -0.0031(11) -0.0037(11) C8' C 0.0184(14) 0.0195(14) 0.0179(12) 0.0007(11) -0.0023(11) -0.0046(11) C9' C 0.0312(18) 0.0427(18) 0.0288(15) 0.0016(15) -0.0054(14) -0.0198(13) C10' C 0.0320(18) 0.048(2) 0.0264(15) -0.0043(16) 0.0001(14) -0.0016(14) C11' C 0.0339(19) 0.0437(19) 0.0346(17) 0.0162(16) -0.0095(15) -0.0063(15) C12' C 0.0174(15) 0.0194(14) 0.0226(14) -0.0034(12) 0.0044(11) 0.0058(11) C13' C 0.0092(12) 0.0115(12) 0.0122(11) -0.0038(11) -0.0011(10) -0.0029(10) C14' C 0.0131(14) 0.0147(13) 0.0148(12) -0.0006(11) -0.0003(10) -0.0010(10) C15' C 0.0149(14) 0.0159(13) 0.0188(12) 0.0038(11) -0.0020(11) -0.0016(10) C16' C 0.0189(14) 0.0163(13) 0.0186(12) 0.0047(11) -0.0031(11) -0.0013(10) C17' C 0.0358(19) 0.0260(15) 0.0252(14) 0.0029(14) 0.0013(13) -0.0052(12) C18' C 0.0283(17) 0.0285(16) 0.0302(15) -0.0098(14) 0.0054(13) -0.0043(13) C19' C 0.0341(18) 0.0287(15) 0.0166(12) 0.0083(14) -0.0052(13) 0.0025(11) C20' C 0.0135(16) 0.0235(17) 0.0342(17) -0.0015(13) 0.0042(13) -0.0105(14) C21' C 0.0097(13) 0.0095(13) 0.0163(12) -0.0043(10) -0.0031(10) -0.0032(10) C22' C 0.0145(14) 0.0067(12) 0.0211(13) 0.0001(10) -0.0046(11) -0.0042(10) C7' C 0.0165(14) 0.0141(13) 0.0210(13) -0.0011(11) -0.0004(11) -0.0060(11) C15 C 0.0190(15) 0.0119(13) 0.0224(13) -0.0039(11) -0.0074(12) -0.0002(11) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 O1 . . 1.4333(19) ? S1 O2 . . 1.438(2) ? S1 C1 . . 1.757(2) ? S1 C4 . . 1.758(3) ? S2 O3 . . 1.435(2) ? S2 O4 . . 1.438(2) ? S2 C12 . . 1.761(3) ? S3 O5 . . 1.4374(18) ? S3 O6 . . 1.4341(19) ? S3 C20 . . 1.762(3) ? Si1 C8 . . 1.843(3) ? Si1 C9 . . 1.852(4) ? Si1 C10 . . 1.860(4) ? Si1 C11 . . 1.856(4) ? Si2 C16 . . 1.851(3) ? Si2 C17 . . 1.857(3) ? Si2 C18 . . 1.853(4) ? Si2 C19 . . 1.851(3) ? O7 C2 . . 1.324(3) ? O7 C21 . . 1.470(3) ? O8 C3 . . 1.336(3) ? O8 C22 . . 1.449(3) ? C1 C2 . . 1.351(4) ? C1 C5 . . 1.460(3) ? C2 C3 . . 1.490(3) ? C3 C4 . . 1.341(4) ? C4 C13 . . 1.461(3) ? C5 C6 . . 1.349(4) ? C6 C7 . . 1.419(4) ? C6 H61 . . 0.96 ? C7 C8 . . 1.200(4) ? C9 H91 . . 0.96 ? C9 H92 . . 0.96 ? C9 H93 . . 0.96 ? C10 H101 . . 0.96 ? C10 H102 . . 0.96 ? C10 H103 . . 0.96 ? C11 H111 . . 0.96 ? C11 H112 . . 0.96 ? C11 H113 . . 0.96 ? C12 H121 . . 0.96 ? C12 H122 . . 0.96 ? C12 H123 . . 0.96 ? C13 C14 . . 1.345(4) ? C14 C15 . . 1.421(4) ? C14 H141 . . 0.96 ? C16 C15 . . 1.201(4) ? C17 H171 . . 0.96 ? C17 H172 . . 0.96 ? C17 H173 . . 0.96 ? C18 H181 . . 0.96 ? C18 H182 . . 0.96 ? C18 H183 . . 0.96 ? C19 H191 . . 0.96 ? C19 H192 . . 0.96 ? C19 H193 . . 0.96 ? C20 H201 . . 0.96 ? C20 H202 . . 0.96 ? C20 H203 . . 0.96 ? C21 C22 . . 1.495(4) ? C21 H211 . . 0.96 ? C21 H212 . . 0.96 ? C22 H221 . . 0.96 ? C22 H222 . . 0.96 ? S1' O1' . . 1.433(2) ? S1' O2' . . 1.443(2) ? S1' C1' . . 1.763(2) ? S1' C4' . . 1.750(3) ? S2' O3' . . 1.434(2) ? S2' O4' . . 1.435(2) ? S2' C12' . . 1.752(3) ? S3' O5' . . 1.4335(19) ? S3' O6' . . 1.432(2) ? S3' C20' . . 1.757(3) ? Si1' C8' . . 1.845(3) ? Si1' C9' . . 1.853(4) ? Si1' C10' . . 1.860(3) ? Si1' C11' . . 1.857(4) ? Si2' C16' . . 1.843(3) ? Si2' C17' . . 1.872(3) ? Si2' C18' . . 1.849(3) ? Si2' C19' . . 1.859(3) ? O7' C2' . . 1.330(3) ? O7' C21' . . 1.459(3) ? O8' C3' . . 1.330(3) ? O8' C22' . . 1.460(3) ? C1' C2' . . 1.345(4) ? C1' C5' . . 1.456(4) ? C2' C3' . . 1.492(3) ? C3' C4' . . 1.333(4) ? C4' C13' . . 1.467(3) ? C5' C6' . . 1.356(4) ? C6' C7' . . 1.426(4) ? C6' H61' . . 0.96 ? C8' C7' . . 1.203(4) ? C9' H91' . . 0.96 ? C9' H92' . . 0.96 ? C9' H93' . . 0.96 ? C10' H101' . . 0.96 ? C10' H102' . . 0.96 ? C10' H103' . . 0.96 ? C11' H111' . . 0.96 ? C11' H112' . . 0.96 ? C11' H113' . . 0.96 ? C12' H121' . . 0.96 ? C12' H122' . . 0.96 ? C12' H123' . . 0.96 ? C13' C14' . . 1.350(4) ? C14' C15' . . 1.419(3) ? C14' H141' . . 0.96 ? C15' C16' . . 1.199(3) ? C17' H171' . . 0.96 ? C17' H172' . . 0.96 ? C17' H173' . . 0.96 ? C18' H181' . . 0.96 ? C18' H182' . . 0.96 ? C18' H183' . . 0.96 ? C19' H191' . . 0.96 ? C19' H192' . . 0.96 ? C19' H193' . . 0.96 ? C20' H201' . . 0.96 ? C20' H202' . . 0.96 ? C20' H203' . . 0.96 ? C21' C22' . . 1.500(4) ? C21' H211' . . 0.96 ? C21' H212' . . 0.96 ? C22' H221' . . 0.96 ? C22' H222' . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 S1 O2 . . . 116.42(12) ? O1 S1 C1 . . . 110.31(12) ? O1 S1 C4 . . . 110.39(13) ? O2 S1 C1 . . . 111.83(12) ? O2 S1 C4 . . . 110.71(12) ? C1 S1 C4 . . . 95.17(12) ? O3 S2 O4 . . . 118.76(13) ? O3 S2 C12 . . . 109.02(13) ? O4 S2 C12 . . . 108.88(13) ? O5 S3 O6 . . . 119.41(12) ? O5 S3 C20 . . . 107.94(13) ? O6 S3 C20 . . . 109.03(14) ? C8 Si1 C9 . . . 110.18(13) ? C8 Si1 C10 . . . 105.49(14) ? C8 Si1 C11 . . . 106.89(16) ? C9 Si1 C10 . . . 112.38(16) ? C9 Si1 C11 . . . 109.87(17) ? C10 Si1 C11 . . . 111.81(16) ? C16 Si2 C17 . . . 106.58(14) ? C16 Si2 C18 . . . 106.93(14) ? C16 Si2 C19 . . . 109.15(14) ? C17 Si2 C18 . . . 112.31(17) ? C17 Si2 C19 . . . 110.09(14) ? C18 Si2 C19 . . . 111.56(15) ? C2 O7 C21 . . . 116.02(19) ? C3 O8 C22 . . . 112.17(19) ? S1 C1 C2 . . . 108.17(18) ? S1 C1 C5 . . . 119.7(2) ? C2 C1 C5 . . . 132.1(2) ? O7 C2 C1 . . . 124.7(2) ? O7 C2 C3 . . . 121.3(2) ? C1 C2 C3 . . . 113.9(2) ? O8 C3 C2 . . . 121.3(2) ? O8 C3 C4 . . . 124.2(2) ? C2 C3 C4 . . . 114.5(2) ? S1 C4 C3 . . . 108.19(18) ? S1 C4 C13 . . . 120.9(2) ? C3 C4 C13 . . . 130.7(2) ? C1 C5 C6 . . . 122.3(2) ? C5 C6 C7 . . . 126.4(2) ? C5 C6 H61 . . . 116.79 ? C7 C6 H61 . . . 116.79 ? C6 C7 C8 . . . 177.7(3) ? Si1 C8 C7 . . . 170.4(3) ? Si1 C9 H91 . . . 109.47 ? Si1 C9 H92 . . . 109.47 ? Si1 C9 H93 . . . 109.47 ? H91 C9 H92 . . . 109.47 ? H91 C9 H93 . . . 109.47 ? H92 C9 H93 . . . 109.47 ? Si1 C10 H101 . . . 109.47 ? Si1 C10 H102 . . . 109.47 ? Si1 C10 H103 . . . 109.47 ? H101 C10 H102 . . . 109.47 ? H101 C10 H103 . . . 109.47 ? H102 C10 H103 . . . 109.47 ? Si1 C11 H111 . . . 109.47 ? Si1 C11 H112 . . . 109.47 ? Si1 C11 H113 . . . 109.47 ? H111 C11 H112 . . . 109.47 ? H111 C11 H113 . . . 109.47 ? H112 C11 H113 . . . 109.47 ? S2 C12 H121 . . . 109.47 ? S2 C12 H122 . . . 109.47 ? S2 C12 H123 . . . 109.47 ? H121 C12 H122 . . . 109.47 ? H121 C12 H123 . . . 109.47 ? H122 C12 H123 . . . 109.47 ? C4 C13 C14 . . . 122.9(3) ? C13 C14 C15 . . . 126.4(3) ? C13 C14 H141 . . . 116.79 ? C15 C14 H141 . . . 116.79 ? Si2 C16 C15 . . . 175.1(3) ? Si2 C17 H171 . . . 109.47 ? Si2 C17 H172 . . . 109.47 ? Si2 C17 H173 . . . 109.47 ? H171 C17 H172 . . . 109.47 ? H171 C17 H173 . . . 109.47 ? H172 C17 H173 . . . 109.47 ? Si2 C18 H181 . . . 109.47 ? Si2 C18 H182 . . . 109.47 ? Si2 C18 H183 . . . 109.47 ? H181 C18 H182 . . . 109.47 ? H181 C18 H183 . . . 109.47 ? H182 C18 H183 . . . 109.47 ? Si2 C19 H191 . . . 109.47 ? Si2 C19 H192 . . . 109.47 ? Si2 C19 H193 . . . 109.47 ? H191 C19 H192 . . . 109.47 ? H191 C19 H193 . . . 109.47 ? H192 C19 H193 . . . 109.47 ? S3 C20 H201 . . . 109.47 ? S3 C20 H202 . . . 109.47 ? S3 C20 H203 . . . 109.47 ? H201 C20 H202 . . . 109.47 ? H201 C20 H203 . . . 109.47 ? H202 C20 H203 . . . 109.47 ? O7 C21 C22 . . . 110.9(2) ? O7 C21 H211 . . . 109.47 ? O7 C21 H212 . . . 109.47 ? C22 C21 H211 . . . 109.47 ? C22 C21 H212 . . . 109.47 ? H211 C21 H212 . . . 107.97 ? O8 C22 C21 . . . 110.7(2) ? O8 C22 H221 . . . 109.47 ? O8 C22 H222 . . . 109.47 ? C21 C22 H221 . . . 109.47 ? C21 C22 H222 . . . 109.47 ? H221 C22 H222 . . . 108.17 ? O1' S1' O2' . . . 116.19(12) ? O1' S1' C1' . . . 110.53(12) ? O1' S1' C4' . . . 110.90(13) ? O2' S1' C1' . . . 111.69(12) ? O2' S1' C4' . . . 110.76(12) ? C1' S1' C4' . . . 94.75(12) ? O3' S2' O4' . . . 118.08(13) ? O3' S2' C12' . . . 108.80(14) ? O4' S2' C12' . . . 109.15(13) ? O5' S3' O6' . . . 119.58(12) ? O5' S3' C20' . . . 107.93(14) ? O6' S3' C20' . . . 108.57(14) ? C8' Si1' C9' . . . 109.81(13) ? C8' Si1' C10' . . . 107.19(14) ? C8' Si1' C11' . . . 105.60(15) ? C9' Si1' C10' . . . 111.42(16) ? C9' Si1' C11' . . . 111.00(17) ? C10' Si1' C11' . . . 111.58(15) ? C16' Si2' C17' . . . 106.21(13) ? C16' Si2' C18' . . . 107.20(14) ? C16' Si2' C19' . . . 108.07(13) ? C17' Si2' C18' . . . 112.52(15) ? C17' Si2' C19' . . . 110.59(15) ? C18' Si2' C19' . . . 111.93(14) ? C2' O7' C21' . . . 116.25(19) ? C3' O8' C22' . . . 112.02(19) ? S1' C1' C2' . . . 108.18(18) ? S1' C1' C5' . . . 118.7(2) ? C2' C1' C5' . . . 133.0(2) ? O7' C2' C1' . . . 124.6(2) ? O7' C2' C3' . . . 121.4(2) ? C1' C2' C3' . . . 113.9(2) ? O8' C3' C2' . . . 121.2(2) ? O8' C3' C4' . . . 124.5(2) ? C2' C3' C4' . . . 114.2(2) ? S1' C4' C3' . . . 108.92(18) ? S1' C4' C13' . . . 121.3(2) ? C3' C4' C13' . . . 129.7(3) ? C1' C5' C6' . . . 122.0(2) ? C5' C6' C7' . . . 125.8(3) ? C5' C6' H61' . . . 117.1 ? C7' C6' H61' . . . 117.11 ? Si1' C8' C7' . . . 169.0(3) ? Si1' C9' H91' . . . 109.47 ? Si1' C9' H92' . . . 109.47 ? Si1' C9' H93' . . . 109.47 ? H91' C9' H92' . . . 109.47 ? H91' C9' H93' . . . 109.47 ? H92' C9' H93' . . . 109.47 ? Si1' C10' H101' . . . 109.47 ? Si1' C10' H102' . . . 109.47 ? Si1' C10' H103' . . . 109.47 ? H101' C10' H102' . . . 109.47 ? H101' C10' H103' . . . 109.47 ? H102' C10' H103' . . . 109.47 ? Si1' C11' H111' . . . 109.47 ? Si1' C11' H112' . . . 109.47 ? Si1' C11' H113' . . . 109.47 ? H111' C11' H112' . . . 109.47 ? H111' C11' H113' . . . 109.47 ? H112' C11' H113' . . . 109.47 ? S2' C12' H121' . . . 109.47 ? S2' C12' H122' . . . 109.47 ? S2' C12' H123' . . . 109.47 ? H121' C12' H122' . . . 109.47 ? H121' C12' H123' . . . 109.47 ? H122' C12' H123' . . . 109.47 ? C4' C13' C14' . . . 122.4(2) ? C13' C14' C15' . . . 126.2(3) ? C13' C14' H141' . . . 116.9 ? C15' C14' H141' . . . 116.9 ? C14' C15' C16' . . . 176.7(3) ? Si2' C16' C15' . . . 176.1(3) ? Si2' C17' H171' . . . 109.47 ? Si2' C17' H172' . . . 109.47 ? Si2' C17' H173' . . . 109.47 ? H171' C17' H172' . . . 109.47 ? H171' C17' H173' . . . 109.47 ? H172' C17' H173' . . . 109.47 ? Si2' C18' H181' . . . 109.47 ? Si2' C18' H182' . . . 109.47 ? Si2' C18' H183' . . . 109.47 ? H181' C18' H182' . . . 109.47 ? H181' C18' H183' . . . 109.47 ? H182' C18' H183' . . . 109.47 ? Si2' C19' H191' . . . 109.47 ? Si2' C19' H192' . . . 109.47 ? Si2' C19' H193' . . . 109.47 ? H191' C19' H192' . . . 109.47 ? H191' C19' H193' . . . 109.47 ? H192' C19' H193' . . . 109.47 ? S3' C20' H201' . . . 109.47 ? S3' C20' H202' . . . 109.47 ? S3' C20' H203' . . . 109.47 ? H201' C20' H202' . . . 109.47 ? H201' C20' H203' . . . 109.47 ? H202' C20' H203' . . . 109.47 ? O7' C21' C22' . . . 111.2(2) ? O7' C21' H211' . . . 109.47 ? O7' C21' H212' . . . 109.47 ? C22' C21' H211' . . . 109.47 ? C22' C21' H212' . . . 109.47 ? H211' C21' H212' . . . 107.65 ? O8' C22' C21' . . . 110.9(2) ? O8' C22' H221' . . . 109.47 ? O8' C22' H222' . . . 109.47 ? C21' C22' H221' . . . 109.47 ? C21' C22' H222' . . . 109.47 ? H221' C22' H222' . . . 108.04 ? C6' C7' C8' . . . 178.7(3) ? C14 C15 C16 . . . 177.9(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C21 H212 O2 . . 2_766 0.96 2.40 3.065(3) 126.36 ? C21' H212' O2' . . 2_656 0.96 2.40 3.066(3) 125.84 ? # start Validation Reply Form #_vrf_PLAT029_ESEMOX #; #PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.850 #RESPONSE: The crystal was twinned with many close and overlapping #reflections. Despite collecting a full reciprocal sphere with large #detector distance, many reflections are lost due to the integration #software being unable to handle the situation. The situation is #aggravated by the monoclinic symmetry. # #It has to be noted though that a reflection (observed) to #data ratio of 11291:632~17(!) is certainly enough for a good structure #determination. #; #_vrf_PLAT924_ESEMOX #; #CHECKCIF is confused by the HKLF5 data and miscalculates Rho(min) #; #_vrf_PLAT925_ESEMOX #; #CHECKCIF is confused by the HKLF5 data and miscalculates Rho(max) #; #_vrf_PLAT220_ESEMOX #; #This is a polytypic structure, the methyl groups of the trimethylsilyl #groups at the layer interface are enlarged. A certain amount of disorder #is expected and the data quality is certainly not perfect, given the #twinning. #; #_vrf_PLAT911_ESEMOX #; #See comment above on problems with the integration software. #; #_vrf_PLAT902_ESEMOX #; #PROBLEM: No (Interpretable) Reflections found in FCF .... Please Check #RESPONSE: This structure was refined from HKLF5 style reflection data #which CHECKCIF cannot parse correctly #; #======================================================================= data_NSEM _publcif_datablock.id '{41f0a419-e27e-48b5-8992-071e663b2bfa}' _database_code_depnum_ccdc_archive 'CCDC 927470' #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C22 H38 S2 Si2' _chemical_formula_weight 422.8 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2xab;2ybc;2zac' _space_group_IT_number 19 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,-y,z+1/2 3 -x,y+1/2,-z+1/2 4 x+1/2,-y+1/2,-z _cell_length_a 7.7849(4) _cell_length_b 10.5146(5) _cell_length_c 31.2712(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2559.7(2) loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.97(3) 1 0 0 0 1 0 0 0 1 2 0.03(3) -1 0 0 0 -1 0 0 0 -1 _cell_formula_units_Z 4 _cell_measurement_reflns_used 80665 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 35.0 _cell_measurement_temperature 100 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 1.0969 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.306 _exptl_crystal_description 'block' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.50 _exptl_crystal_size_rad ? _exptl_crystal_colour 'clear colourless' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.81 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\w- and \f-scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 101389 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 35.05 _diffrn_reflns_theta_full 35.05 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_unetI/netI 0.0132 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 11125 _reflns_number_gt 10833 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_gt 0.0399 _refine_ls_R_factor_all 0.0280 _refine_ls_wR_factor_ref 0.0400 _refine_ls_goodness_of_fit_ref 2.72 _refine_ls_goodness_of_fit_gt 2.75 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 11125 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_number_constraints 152 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0052 _refine_ls_shift/su_mean 0.0003 _refine_diff_density_max 0.33 _refine_diff_density_min -0.28 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; 4896 of Friedel pairs used in the refinement ; _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.31980(3) 0.13191(2) 0.966480(8) Uani 0.01959(6) 4 1 d . . . S2 S 0.42766(4) -0.18580(2) 1.013392(7) Uani 0.01960(6) 4 1 d . . . Si1 Si 0.62095(3) 0.36183(2) 0.852907(7) Uani 0.01126(6) 4 1 d . . . Si2 Si 0.58464(3) -0.26250(2) 1.167524(7) Uani 0.01138(6) 4 1 d . . . C1 C 0.51165(12) 0.05694(8) 0.98191(3) Uani 0.0137(2) 4 1 d . . . C2 C 0.65741(12) 0.08312(8) 0.96038(3) Uani 0.0156(2) 4 1 d . . . C3 C 0.66058(11) 0.16972(8) 0.92544(3) Uani 0.0149(2) 4 1 d . . . C4 C 0.65625(11) 0.24438(8) 0.89564(3) Uani 0.0150(2) 4 1 d . . . C5 C 0.57399(15) 0.51746(9) 0.87892(3) Uani 0.0210(2) 4 1 d . . . C6 C 0.81656(12) 0.37560(9) 0.81894(3) Uani 0.0198(2) 4 1 d . . . C7 C 0.43273(12) 0.30347(8) 0.82011(3) Uani 0.0149(2) 4 1 d . . . C8 C 0.27671(13) 0.28141(10) 0.84927(4) Uani 0.0238(3) 4 1 d . . . C9 C 0.47868(15) 0.17811(10) 0.79778(4) Uani 0.0246(3) 4 1 d . . . C10 C 0.38554(15) 0.40383(10) 0.78635(4) Uani 0.0267(3) 4 1 d . . . C11 C 0.15980(13) 0.07253(10) 1.00315(3) Uani 0.0217(3) 4 1 d . . . C12 C 0.51395(11) -0.03211(8) 1.01867(3) Uani 0.0132(2) 4 1 d . . . C13 C 0.57667(13) 0.00640(8) 1.05691(3) Uani 0.0150(2) 4 1 d . . . C14 C 0.58212(12) -0.07488(8) 1.09330(3) Uani 0.0140(2) 4 1 d . . . C15 C 0.58584(12) -0.14501(8) 1.12401(3) Uani 0.01438(19) 4 1 d . . . C16 C 0.81091(13) -0.31039(10) 1.17887(4) Uani 0.0228(3) 4 1 d . . . C17 C 0.48757(15) -0.18925(9) 1.21607(3) Uani 0.0217(3) 4 1 d . . . C18 C 0.45279(11) -0.40215(7) 1.14844(3) Uani 0.0134(2) 4 1 d . . . C19 C 0.53857(13) -0.46278(9) 1.10924(3) Uani 0.0197(2) 4 1 d . . . C20 C 0.27156(12) -0.35929(10) 1.13670(4) Uani 0.0243(3) 4 1 d . . . C21 C 0.44214(14) -0.50147(9) 1.18440(3) Uani 0.0223(3) 4 1 d . . . C22 C 0.42036(16) -0.20946(10) 0.95631(3) Uani 0.0237(3) 4 1 d . . . H2 H 0.762168 0.042114 0.968871 Uiso 0.0187 4 1 d . . . H13 H 0.619086 0.091762 1.0596 Uiso 0.018 4 1 d . . . H51 H 0.560229 0.581693 0.857371 Uiso 0.0252 4 1 d . . . H52 H 0.470165 0.510688 0.895325 Uiso 0.0252 4 1 d . . . H53 H 0.667379 0.540164 0.897454 Uiso 0.0252 4 1 d . . . H61 H 0.789393 0.42229 0.793441 Uiso 0.0237 4 1 d . . . H62 H 0.904823 0.419436 0.834508 Uiso 0.0237 4 1 d . . . H63 H 0.856308 0.292157 0.811361 Uiso 0.0237 4 1 d . . . H161 H 0.811641 -0.378246 1.199413 Uiso 0.0273 4 1 d . . . H162 H 0.864564 -0.338637 1.152913 Uiso 0.0273 4 1 d . . . H163 H 0.872941 -0.238937 1.190129 Uiso 0.0273 4 1 d . . . H171 H 0.470166 -0.253531 1.237433 Uiso 0.026 4 1 d . . . H172 H 0.563276 -0.124994 1.227042 Uiso 0.026 4 1 d . . . H173 H 0.379227 -0.15146 1.208749 Uiso 0.026 4 1 d . . . H81 H 0.237255 0.361474 0.860279 Uiso 0.0285 4 1 d . . . H82 H 0.186324 0.241879 0.833161 Uiso 0.0285 4 1 d . . . H83 H 0.30906 0.22708 0.872592 Uiso 0.0285 4 1 d . . . H91 H 0.512649 0.116444 0.818784 Uiso 0.0295 4 1 d . . . H92 H 0.380463 0.147189 0.782405 Uiso 0.0295 4 1 d . . . H93 H 0.571674 0.192246 0.778193 Uiso 0.0295 4 1 d . . . H101 H 0.364474 0.483854 0.800171 Uiso 0.0321 4 1 d . . . H102 H 0.478628 0.412947 0.76645 Uiso 0.0321 4 1 d . . . H103 H 0.28406 0.377381 0.771349 Uiso 0.0321 4 1 d . . . H191 H 0.652662 -0.48963 1.116601 Uiso 0.0236 4 1 d . . . H192 H 0.472625 -0.535 1.100119 Uiso 0.0236 4 1 d . . . H193 H 0.544073 -0.401631 1.086486 Uiso 0.0236 4 1 d . . . H201 H 0.217415 -0.322156 1.16129 Uiso 0.0292 4 1 d . . . H202 H 0.277349 -0.297454 1.114156 Uiso 0.0292 4 1 d . . . H203 H 0.205911 -0.431296 1.127256 Uiso 0.0292 4 1 d . . . H211 H 0.556005 -0.52461 1.19325 Uiso 0.0268 4 1 d . . . H212 H 0.38075 -0.466276 1.208248 Uiso 0.0268 4 1 d . . . H213 H 0.383 -0.575577 1.174157 Uiso 0.0268 4 1 d . . . H111 H 0.054953 0.119323 0.999468 Uiso 0.0261 4 1 d . . . H112 H 0.139313 -0.015933 0.997516 Uiso 0.0261 4 1 d . . . H113 H 0.200019 0.082599 1.031971 Uiso 0.0261 4 1 d . . . H221 H 0.348167 -0.280987 0.949901 Uiso 0.0285 4 1 d . . . H222 H 0.374774 -0.134702 0.942833 Uiso 0.0285 4 1 d . . . H223 H 0.534249 -0.225307 0.945816 Uiso 0.0285 4 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 S 0.01709(9) 0.02357(11) 0.01810(11) 0.00327(8) -0.00015(8) 0.00759(8) S2 S 0.03032(12) 0.01448(9) 0.01399(10) -0.00688(9) -0.00140(9) 0.00100(7) Si1 Si 0.01318(10) 0.00958(9) 0.01102(10) 0.00007(7) -0.00039(8) 0.00175(8) Si2 Si 0.01431(10) 0.01065(9) 0.00919(10) 0.00030(8) -0.00048(8) 0.00210(7) C1 C 0.0176(4) 0.0137(3) 0.0099(4) -0.0009(3) -0.0020(3) 0.0016(3) C2 C 0.0169(4) 0.0168(4) 0.0131(4) 0.0005(3) -0.0004(3) 0.0052(3) C3 C 0.0148(3) 0.0173(3) 0.0125(4) 0.0001(3) 0.0002(3) 0.0027(3) C4 C 0.0159(4) 0.0152(3) 0.0137(4) 0.0006(3) -0.0002(3) 0.0012(3) C5 C 0.0248(4) 0.0150(4) 0.0233(5) 0.0021(3) -0.0049(4) -0.0041(3) C6 C 0.0196(4) 0.0187(4) 0.0210(4) -0.0022(3) 0.0036(3) 0.0047(3) C7 C 0.0169(4) 0.0120(3) 0.0159(4) 0.0008(3) -0.0039(3) 0.0000(3) C8 C 0.0149(4) 0.0263(4) 0.0301(5) -0.0034(3) -0.0017(4) -0.0008(4) C9 C 0.0280(5) 0.0192(4) 0.0266(5) 0.0025(4) -0.0054(4) -0.0087(4) C10 C 0.0303(5) 0.0252(5) 0.0248(5) 0.0013(4) -0.0134(4) 0.0062(4) C11 C 0.0190(4) 0.0255(4) 0.0207(5) 0.0012(4) 0.0038(3) -0.0009(3) C12 C 0.0151(3) 0.0131(3) 0.0114(4) -0.0009(3) -0.0011(3) 0.0024(3) C13 C 0.0202(4) 0.0133(3) 0.0116(4) -0.0031(3) -0.0027(3) 0.0026(3) C14 C 0.0173(3) 0.0139(3) 0.0109(4) -0.0016(3) -0.0020(3) 0.0004(3) C15 C 0.0181(3) 0.0130(3) 0.0121(4) -0.0014(3) -0.0004(3) 0.0006(3) C16 C 0.0165(4) 0.0246(4) 0.0272(5) 0.0001(3) -0.0052(4) 0.0052(4) C17 C 0.0346(5) 0.0179(4) 0.0125(4) 0.0003(4) 0.0022(4) -0.0003(3) C18 C 0.0138(3) 0.0102(3) 0.0163(4) 0.0001(2) 0.0021(3) 0.0007(3) C19 C 0.0241(4) 0.0169(4) 0.0180(4) -0.0016(3) 0.0037(3) -0.0049(3) C20 C 0.0156(4) 0.0189(4) 0.0385(6) 0.0005(3) -0.0049(4) -0.0026(4) C21 C 0.0287(5) 0.0143(4) 0.0239(5) -0.0016(3) 0.0082(4) 0.0047(3) C22 C 0.0323(5) 0.0214(4) 0.0175(4) -0.0024(4) -0.0050(4) -0.0054(3) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 C1 . . 1.7564(9) ? S2 C12 . . 1.7578(9) ? Si1 C4 . . 1.8401(9) ? Si1 C5 . . 1.8636(10) ? Si1 C6 . . 1.8623(10) ? Si1 C7 . . 1.8909(9) ? Si2 C15 . . 1.8379(9) ? Si2 C16 . . 1.8662(11) ? Si2 C17 . . 1.8624(10) ? Si2 C18 . . 1.8883(8) ? C1 C2 . . 1.3479(13) ? C1 C12 . . 1.4828(12) ? C2 C3 . . 1.4225(12) ? C2 H2 . . 0.96 ? C3 C4 . . 1.2190(12) ? C5 H51 . . 0.96 ? C5 H52 . . 0.96 ? C5 H53 . . 0.96 ? C6 H61 . . 0.96 ? C6 H62 . . 0.96 ? C6 H63 . . 0.96 ? C7 C8 . . 1.5364(14) ? C7 C9 . . 1.5338(13) ? C7 C10 . . 1.5372(14) ? C8 H81 . . 0.96 ? C8 H82 . . 0.96 ? C8 H83 . . 0.96 ? C9 H91 . . 0.96 ? C9 H92 . . 0.96 ? C9 H93 . . 0.96 ? C10 H101 . . 0.96 ? C10 H102 . . 0.96 ? C10 H103 . . 0.96 ? C11 H111 . . 0.96 ? C11 H112 . . 0.96 ? C11 H113 . . 0.96 ? C12 C13 . . 1.3536(12) ? C13 C14 . . 1.4237(12) ? C13 H13 . . 0.96 ? C14 C15 . . 1.2111(12) ? C16 H161 . . 0.96 ? C16 H162 . . 0.96 ? C16 H163 . . 0.96 ? C17 H171 . . 0.96 ? C17 H172 . . 0.96 ? C17 H173 . . 0.96 ? C18 C19 . . 1.5345(13) ? C18 C20 . . 1.5259(13) ? C18 C21 . . 1.5369(13) ? C19 H191 . . 0.96 ? C19 H192 . . 0.96 ? C19 H193 . . 0.96 ? C20 H201 . . 0.96 ? C20 H202 . . 0.96 ? C20 H203 . . 0.96 ? C21 H211 . . 0.96 ? C21 H212 . . 0.96 ? C21 H213 . . 0.96 ? C22 H221 . . 0.96 ? C22 H222 . . 0.96 ? C22 H223 . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C4 Si1 C5 . . . 107.56(4) ? C4 Si1 C6 . . . 110.13(4) ? C4 Si1 C7 . . . 106.96(4) ? C5 Si1 C6 . . . 109.94(5) ? C5 Si1 C7 . . . 111.69(4) ? C6 Si1 C7 . . . 110.46(4) ? C15 Si2 C16 . . . 108.50(5) ? C15 Si2 C17 . . . 109.12(4) ? C15 Si2 C18 . . . 106.95(4) ? C16 Si2 C17 . . . 109.85(5) ? C16 Si2 C18 . . . 111.31(4) ? C17 Si2 C18 . . . 111.02(4) ? S1 C1 C2 . . . 119.14(7) ? S1 C1 C12 . . . 120.44(7) ? C2 C1 C12 . . . 120.41(8) ? C1 C2 C3 . . . 121.94(8) ? C1 C2 H2 . . . 119.03 ? C3 C2 H2 . . . 119.03 ? C2 C3 C4 . . . 177.41(9) ? Si1 C4 C3 . . . 172.52(8) ? Si1 C5 H51 . . . 109.47 ? Si1 C5 H52 . . . 109.47 ? Si1 C5 H53 . . . 109.47 ? H51 C5 H52 . . . 109.47 ? H51 C5 H53 . . . 109.47 ? H52 C5 H53 . . . 109.47 ? Si1 C6 H61 . . . 109.47 ? Si1 C6 H62 . . . 109.47 ? Si1 C6 H63 . . . 109.47 ? H61 C6 H62 . . . 109.47 ? H61 C6 H63 . . . 109.47 ? H62 C6 H63 . . . 109.47 ? Si1 C7 C8 . . . 109.86(6) ? Si1 C7 C9 . . . 110.18(7) ? Si1 C7 C10 . . . 109.56(6) ? C8 C7 C9 . . . 108.95(8) ? C8 C7 C10 . . . 108.81(8) ? C9 C7 C10 . . . 109.46(8) ? C7 C8 H81 . . . 109.47 ? C7 C8 H82 . . . 109.47 ? C7 C8 H83 . . . 109.47 ? H81 C8 H82 . . . 109.47 ? H81 C8 H83 . . . 109.47 ? H82 C8 H83 . . . 109.47 ? C7 C9 H91 . . . 109.47 ? C7 C9 H92 . . . 109.47 ? C7 C9 H93 . . . 109.47 ? H91 C9 H92 . . . 109.47 ? H91 C9 H93 . . . 109.47 ? H92 C9 H93 . . . 109.47 ? C7 C10 H101 . . . 109.47 ? C7 C10 H102 . . . 109.47 ? C7 C10 H103 . . . 109.47 ? H101 C10 H102 . . . 109.47 ? H101 C10 H103 . . . 109.47 ? H102 C10 H103 . . . 109.47 ? H111 C11 H112 . . . 109.47 ? H111 C11 H113 . . . 109.47 ? H112 C11 H113 . . . 109.47 ? S2 C12 C1 . . . 120.20(6) ? S2 C12 C13 . . . 119.73(7) ? C1 C12 C13 . . . 120.02(8) ? C12 C13 C14 . . . 122.49(8) ? C12 C13 H13 . . . 118.76 ? C14 C13 H13 . . . 118.76 ? C13 C14 C15 . . . 179.31(9) ? Si2 C15 C14 . . . 175.00(8) ? Si2 C16 H161 . . . 109.47 ? Si2 C16 H162 . . . 109.47 ? Si2 C16 H163 . . . 109.47 ? H161 C16 H162 . . . 109.47 ? H161 C16 H163 . . . 109.47 ? H162 C16 H163 . . . 109.47 ? Si2 C17 H171 . . . 109.47 ? Si2 C17 H172 . . . 109.47 ? Si2 C17 H173 . . . 109.47 ? H171 C17 H172 . . . 109.47 ? H171 C17 H173 . . . 109.47 ? H172 C17 H173 . . . 109.47 ? Si2 C18 C19 . . . 109.81(6) ? Si2 C18 C20 . . . 110.42(6) ? Si2 C18 C21 . . . 109.06(6) ? C19 C18 C20 . . . 109.44(8) ? C19 C18 C21 . . . 109.00(7) ? C20 C18 C21 . . . 109.08(8) ? C18 C19 H191 . . . 109.47 ? C18 C19 H192 . . . 109.47 ? C18 C19 H193 . . . 109.47 ? H191 C19 H192 . . . 109.47 ? H191 C19 H193 . . . 109.47 ? H192 C19 H193 . . . 109.47 ? C18 C20 H201 . . . 109.47 ? C18 C20 H202 . . . 109.47 ? C18 C20 H203 . . . 109.47 ? H201 C20 H202 . . . 109.47 ? H201 C20 H203 . . . 109.47 ? H202 C20 H203 . . . 109.47 ? C18 C21 H211 . . . 109.47 ? C18 C21 H212 . . . 109.47 ? C18 C21 H213 . . . 109.47 ? H211 C21 H212 . . . 109.47 ? H211 C21 H213 . . . 109.47 ? H212 C21 H213 . . . 109.47 ? H221 C22 H222 . . . 109.47 ? H221 C22 H223 . . . 109.47 ? H222 C22 H223 . . . 109.47 ? # start Validation Reply Form #_vrf_PLAT230_NSEM #; #PROBLEM: #RESPONSE: Hirshfeld tests are not relevant for atoms heavier than O. #; #======================================================================= data_TSEM _publcif_datablock.id '{070f41a4-7152-41b9-a7d0-dc2949d10aee}' _database_code_depnum_ccdc_archive 'CCDC 928110' #======================================================================= # 5. CHEMICAL DATA _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C20 H28 S3 Si2' _chemical_formula_weight 420.8 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration ? #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'I2/c' _space_group_name_Hall -I _space_group_IT_number ? loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y,-z+1/2 3 -x,-y,-z 4 x,-y,z+1/2 5 x+1/2,y+1/2,z+1/2 6 -x+1/2,y+1/2,-z 7 -x+1/2,-y+1/2,-z+1/2 8 x+1/2,-y+1/2,z _cell_length_a 34.443(3) _cell_length_b 6.7415(4) _cell_length_c 10.1978(8) _cell_angle_alpha 90 _cell_angle_beta 96.889(5) _cell_angle_gamma 90 _cell_volume 2350.8(3) loop_ _twin_individual_id _twin_individual_mass_fraction_refined _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.5039(17) 1 0 0 0 1 0 0 0 1 2 0.4961(17) 1 0 0 0 1 0 0 0 1 _cell_formula_units_Z 4 _cell_measurement_reflns_used 5646 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 30.1 _cell_measurement_temperature 100 _exptl_crystal_type_of_structure cryst _exptl_crystal_density_diffrn 1.1886 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.419 _exptl_crystal_description fragment _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_size_rad ? _exptl_crystal_colour 'clear yellow' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 1.00 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type 'Mo K\a' _diffrn_source 'X-ray tube' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_detector ? _diffrn_detector_area_resol_mean ? _diffrn_measurement_method '\w- and \f-scans' _diffrn_measurement_specimen_support ? _diffrn_reflns_number 29932 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 30.16 _diffrn_reflns_theta_full 30.16 _diffrn_measured_fraction_theta_max 0.871 _diffrn_measured_fraction_theta_full 0.871 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_unetI/netI 0.0622 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_radiation_probe x-ray #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 3045 _reflns_number_gt 2366 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0780 _refine_ls_wR_factor_gt 0.0608 _refine_ls_R_factor_all 0.1095 _refine_ls_wR_factor_ref 0.0625 _refine_ls_goodness_of_fit_ref 2.56 _refine_ls_goodness_of_fit_gt 2.84 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 3045 _refine_ls_number_parameters 115 _refine_ls_number_restraints 0 _refine_ls_number_constraints 56 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(F)+0.0001F^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0265 _refine_ls_shift/su_mean 0.0048 _refine_diff_density_max 1.53 _refine_diff_density_min -1.41 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Si 0.0817 0.0704 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si -0.17864(4) -0.36480(15) 0.68787(12) Uani 0.0154(3) 8 1 d . . . S1 S 0 -0.22083(19) 0.25 Uani 0.0152(4) 4 1 d . . . S2 S -0.08137(3) -0.10021(14) 0.35864(10) Uani 0.0170(3) 8 1 d . . . C1 C -0.02870(12) -0.3979(6) 0.3133(4) Uani 0.0123(12) 8 1 d . . . C2 C -0.01647(11) -0.5848(6) 0.2847(4) Uani 0.0151(12) 8 1 d . . . C3 C -0.06067(12) -0.3398(5) 0.3859(4) Uani 0.0122(11) 8 1 d . . . C4 C -0.07320(11) -0.4556(6) 0.4803(4) Uani 0.0154(13) 8 1 d . . . C5 C -0.10600(12) -0.4149(5) 0.5489(4) Uani 0.0155(12) 8 1 d . . . C6 C -0.13393(12) -0.3922(6) 0.6078(4) Uani 0.0149(12) 8 1 d . . . C7 C -0.19606(13) -0.6184(6) 0.7226(5) Uani 0.0300(16) 8 1 d . . . C8 C -0.16822(12) -0.2209(6) 0.8438(4) Uani 0.0208(13) 8 1 d . . . C9 C -0.21539(14) -0.2299(8) 0.5731(5) Uani 0.0333(17) 8 1 d . . . C10 C -0.09552(13) -0.0950(6) 0.1823(4) Uani 0.0235(14) 8 1 d . . . H2 H -0.029085 -0.703636 0.309605 Uiso 0.0181 8 1 d . . . H4 H -0.058824 -0.575155 0.503069 Uiso 0.0185 8 1 d . . . H71 H -0.220878 -0.60969 0.756175 Uiso 0.0361 8 1 d . . . H72 H -0.198861 -0.694786 0.64255 Uiso 0.0361 8 1 d . . . H73 H -0.177451 -0.681535 0.786874 Uiso 0.0361 8 1 d . . . H81 H -0.191167 -0.217735 0.888635 Uiso 0.0249 8 1 d . . . H82 H -0.147198 -0.282719 0.899423 Uiso 0.0249 8 1 d . . . H83 H -0.160904 -0.087883 0.823657 Uiso 0.0249 8 1 d . . . H91 H -0.237127 -0.193175 0.618695 Uiso 0.0399 8 1 d . . . H92 H -0.203698 -0.112647 0.541497 Uiso 0.0399 8 1 d . . . H93 H -0.224351 -0.314004 0.499707 Uiso 0.0399 8 1 d . . . H101 H -0.108871 0.027068 0.158395 Uiso 0.0282 8 1 d . . . H102 H -0.072614 -0.104701 0.137528 Uiso 0.0282 8 1 d . . . H103 H -0.112592 -0.204705 0.15728 Uiso 0.0282 8 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Si1 Si 0.0132(6) 0.0181(5) 0.0160(6) -0.0025(5) 0.0065(6) -0.0005(5) S1 S 0.0179(8) 0.0113(6) 0.0184(7) 0 0.0101(8) 0 S2 S 0.0253(6) 0.0114(5) 0.0160(5) 0.0038(5) 0.0095(5) 0.0006(4) C1 C 0.013(2) 0.016(2) 0.0083(18) 0.0002(18) 0.0018(17) 0.0011(17) C2 C 0.013(2) 0.015(2) 0.017(2) -0.0028(16) 0.0019(16) 0.0011(16) C3 C 0.015(2) 0.0075(17) 0.014(2) -0.0009(16) 0.0017(17) -0.0026(15) C4 C 0.013(2) 0.016(2) 0.019(2) 0.0015(16) 0.0065(18) 0.0000(18) C5 C 0.020(2) 0.0131(19) 0.014(2) -0.0021(18) 0.0060(19) 0.0020(16) C6 C 0.020(2) 0.0089(19) 0.016(2) -0.0018(17) 0.0042(18) -0.0007(16) C7 C 0.033(3) 0.025(2) 0.035(3) -0.015(2) 0.017(2) -0.007(2) C8 C 0.019(2) 0.024(2) 0.020(2) -0.0024(19) 0.0071(19) -0.0006(18) C9 C 0.022(3) 0.053(3) 0.026(3) 0.009(2) 0.007(2) 0.000(2) C10 C 0.027(3) 0.025(2) 0.019(2) 0.009(2) 0.0055(18) 0.0035(18) #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Si1 C6 . . 1.837(5) ? Si1 C7 . . 1.860(4) ? Si1 C8 . . 1.860(4) ? Si1 C9 . . 1.856(5) ? S1 C1 . . 1.724(4) ? S1 C1 . 2_555 1.724(4) ? S2 C3 . . 1.774(4) ? C1 C2 . . 1.371(6) ? C1 C3 . . 1.452(6) ? C2 C2 . 2_555 1.408(6) ? C2 H2 . . 0.96 ? C3 C4 . . 1.349(6) ? C4 C5 . . 1.425(6) ? C4 H4 . . 0.96 ? C5 C6 . . 1.204(6) ? C7 H71 . . 0.96 ? C7 H72 . . 0.96 ? C7 H73 . . 0.96 ? C8 H81 . . 0.96 ? C8 H82 . . 0.96 ? C8 H83 . . 0.96 ? C9 H91 . . 0.96 ? C9 H92 . . 0.96 ? C9 H93 . . 0.96 ? C10 H101 . . 0.96 ? C10 H102 . . 0.96 ? C10 H103 . . 0.96 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C6 Si1 C7 . . . 107.41(19) ? C6 Si1 C8 . . . 110.26(19) ? C6 Si1 C9 . . . 108.3(2) ? C7 Si1 C8 . . . 110.5(2) ? C7 Si1 C9 . . . 111.1(2) ? C8 Si1 C9 . . . 109.3(2) ? C1 S1 C1 . . 2_555 92.4(2) ? S1 C1 C2 . . . 110.6(3) ? S1 C1 C3 . . . 120.6(3) ? C2 C1 C3 . . . 128.8(4) ? C1 C2 C2 . . 2_555 113.2(4) ? C1 C2 H2 . . . 123.41 ? C2 C2 H2 2_555 . . 123.41 ? S2 C3 C1 . . . 118.7(3) ? S2 C3 C4 . . . 118.8(3) ? C1 C3 C4 . . . 122.3(3) ? C3 C4 C5 . . . 125.4(4) ? C3 C4 H4 . . . 117.3 ? C5 C4 H4 . . . 117.3 ? C4 C5 C6 . . . 176.2(4) ? Si1 C6 C5 . . . 176.1(4) ? Si1 C7 H71 . . . 109.47 ? Si1 C7 H72 . . . 109.47 ? Si1 C7 H73 . . . 109.47 ? H71 C7 H72 . . . 109.47 ? H71 C7 H73 . . . 109.47 ? H72 C7 H73 . . . 109.47 ? Si1 C8 H81 . . . 109.47 ? Si1 C8 H82 . . . 109.47 ? Si1 C8 H83 . . . 109.47 ? H81 C8 H82 . . . 109.47 ? H81 C8 H83 . . . 109.47 ? H82 C8 H83 . . . 109.47 ? Si1 C9 H91 . . . 109.47 ? Si1 C9 H92 . . . 109.47 ? Si1 C9 H93 . . . 109.47 ? H91 C9 H92 . . . 109.47 ? H91 C9 H93 . . . 109.47 ? H92 C9 H93 . . . 109.47 ? H101 C10 H102 . . . 109.47 ? H101 C10 H103 . . . 109.47 ? H102 C10 H103 . . . 109.47 ? # start Validation Reply Form #_vrf_PLAT029_TSEM #; #PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.871 #RESPONSE: The crystal was twinned with many close and overlapping #reflections. Despite collecting a full reciprocal sphere with large #detector distance, many reflections are lost due to the integration #software being unable to handle the situation. # #It has to be noted though that a reflection (observed) to #parameter ratio of 2366:115\~20 is certainly enough for a good structure #determination. #; #_vrf_PLAT924_TSEM #; #PROBLEM: The Reported and Calculated Rho(min) Differ by . 2.47 eA-3 #RESPONSE: CHECKCIF is confused by the HKLF5 data and miscalculates Rho(min) #; #_vrf_PLAT925_TSEM #; #PROBLEM: The Reported and Calculated Rho(max) Differ by . 2.12 eA-3 #RESPONSE: CHECKCIF is confused by the HKLF5 data and miscalculates Rho(max) #; #_vrf_PLAT902_TSEM #; #PROBLEM: No (Interpretable) Reflections found in FCF .... Please Check #RESPONSE: This structure was refined from HKLF5 style reflection data #which CHECKCIF cannot parse correctly #; _publcif_info_exptl_table_max_cols 4 _publcif_info_exptl_table_use_headnotes n loop_ _publcif_info_datablock.id _publcif_info_datablock.publ_exptl _publcif_info_datablock.publ_geom _publcif_info_datablock.structure '{8155da1e-8a83-443a-bcc9-ed40a73704dc}' y y y '{4740eb5d-65a9-4075-bc68-4cd2da624df7}' y y y '{fb1d8f59-01f8-4c16-90b1-7499f77f1e79}' y y y '{3421d942-ae4a-47e8-bc97-5d77493da92e}' y y y '{b87663d1-9ceb-45f2-9a7e-76ba56bdd648}' y y y '{d6b6d973-fc2a-4196-8550-5f6f0e7a4ba6}' y y y '{a2613522-21c0-4ad1-b1f4-e52d4ca08d07}' y y y '{d2cdb962-33e0-412d-984c-7ec7759e844c}' y y y '{b8d27531-a09f-47d8-88d1-ccb022778054}' y y y '{41f0a419-e27e-48b5-8992-071e663b2bfa}' y y y '{070f41a4-7152-41b9-a7d0-dc2949d10aee}' y y y loop_ _publcif_info_exptl_table_extra_item sin_theta_over_lambda_max loop_ _publcif_info_exptl_table_header_item ?