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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 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Kanatzidis, Mercouri G.' _publ_contact_author_address ;Department of Chemistry 2145 Sheridan Road Northwestern University Evanston, IL 60208-3113 USA ; _publ_contact_author_phone 'Int + 847-467-1541' _publ_contact_author_fax 'Int + 847-491-5937' _publ_contact_author_email 'm-kanatzidis@northwestern.edu' #===END # 2. TITLE AND AUTHOR LIST _journal_name_full 'Inorganic Chemistry' _journal_year 2011 _journal_volume 50 _journal_page_first 10241 _journal_page_last 10248 _journal_paper_doi https://dx.doi.org/10.1021/ic201249w _publ_section_title ;Germanium Selenophosphates: The Incommensurately Modulated 1/\infty[Ge~4-x~P~x~Se~12~^4-^] and the Molecular [Ge~2~P~2~Se~14~]^6-^ ; loop_ _publ_author_name _publ_author_address 'Morris, Collin D.' ; Department of Chemistry 2145 Sheridan Road Northwestern University Evanston, IL 60208-3113 USA ; 'Malliakas, Christos D.' ; Department of Chemistry 2145 Sheridan Road Northwestern University Evanston, IL 60208-3113 USA ; 'Kanatzidis, Mercouri G.' ; Department of Chemistry 2145 Sheridan Road Northwestern University Evanston, IL 60208-3113 USA ; #===END data_K4Ge2_54P1_46Se12 _audit_creation_method SHELXL-97 _chemical_formula_moiety 'Ge2.54 P1.46 Se8, 4(Se), 4(K)' _chemical_formula_sum 'Ge2.54 K4 P1.46 Se12' _chemical_formula_weight 1311.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_name_H-M_alt P21/c loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y+1/2,-z+1/2 3 -x,-y,-z 4 x,-y-1/2,z-1/2 _cell_length_a 6.7388(7) _cell_length_b 13.4894(12) _cell_length_c 6.3904(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.025(8) _cell_angle_gamma 90.00 _cell_volume 580.81(10) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9993 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 29.62 _exptl_crystal_type_of_structure cryst _exptl_crystal_description 'rod' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.2414 _exptl_crystal_size_mid 0.0925 _exptl_crystal_size_min 0.0749 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.748 _exptl_crystal_density_method ? _exptl_crystal_F_000 578 _exptl_absorpt_coefficient_mu 22.228 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min 0.0866 _exptl_absorpt_correction_T_max 0.4360 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II' _diffrn_measurement_method 'rotation' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5044 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_unetI/netI 0.0323 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 29.16 _reflns_number_total 1555 _reflns_number_gt 1443 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+3.9986P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1555 _refine_ls_number_parameters 57 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.240 _refine_ls_restrained_S_all 1.240 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.06970(8) 0.30337(4) 0.30496(7) 0.02579(11) Uani 1 1 d . . . Se2 Se 0.24244(6) 0.03214(3) 0.22789(6) 0.01652(9) Uani 1 1 d . . . Se3A Se 0.55995(14) 0.26286(8) 0.14270(18) 0.0177(2) Uani 0.4341(13) 1 d P . . Se3B Se 0.56607(11) 0.24888(6) 0.03283(15) 0.01844(19) Uani 0.5659(13) 1 d P . . Ge1 Ge 0.24808(8) 0.18698(4) 0.11823(8) 0.01268(14) Uani 0.634(3) 1 d P . . P1 P 0.24808(8) 0.18698(4) 0.11823(8) 0.01268(14) Uani 0.366(3) 1 d P . . K1 K 0.26015(14) 0.53807(8) 0.22533(14) 0.01924(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0437(3) 0.0174(2) 0.0160(2) -0.00212(17) -0.00653(19) 0.0104(2) Se2 0.01497(18) 0.0247(2) 0.00992(17) 0.00175(16) -0.00007(14) -0.00038(16) Se3A 0.0115(4) 0.0224(5) 0.0193(5) 0.0075(4) -0.0012(4) -0.0062(4) Se3B 0.0089(3) 0.0214(4) 0.0251(4) -0.0022(3) -0.0002(3) -0.0027(3) Ge1 0.0155(3) 0.0124(2) 0.0101(2) 0.00073(19) -0.00203(19) 0.0018(2) P1 0.0155(3) 0.0124(2) 0.0101(2) 0.00073(19) -0.00203(19) 0.0018(2) K1 0.0166(4) 0.0287(5) 0.0124(4) -0.0019(4) 0.0010(3) -0.0067(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 P1 2.3202(8) 4_566 ? Se1 Ge1 2.3202(8) 4_566 ? Se1 Ge1 2.3207(7) . ? Se2 Ge1 2.2037(7) . ? Se3A Se3B 0.7289(12) . ? Se3A Ge1 2.3404(11) . ? Se3A Se3B 2.4977(12) 4_566 ? Se3B Ge1 2.3725(9) . ? Se3B Se3A 2.4977(12) 4_565 ? Ge1 Se1 2.3202(8) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Se1 Ge1 0.00(3) 4_566 4_566 ? P1 Se1 Ge1 102.50(3) 4_566 . ? Ge1 Se1 Ge1 102.50(3) 4_566 . ? P1 Se1 K1 83.55(3) 4_566 . ? Ge1 Se1 K1 83.55(3) 4_566 . ? Ge1 Se1 K1 110.29(3) . . ? Ge1 Se2 K1 125.09(3) . 4_566 ? Ge1 Se2 K1 87.82(3) . 4_565 ? K1 Se2 K1 146.73(4) 4_566 4_565 ? Ge1 Se2 K1 89.02(3) . 2_645 ? K1 Se2 K1 84.42(3) 4_566 2_645 ? K1 Se2 K1 92.26(3) 4_565 2_645 ? Ge1 Se2 K1 91.63(3) . 2_545 ? K1 Se2 K1 86.64(3) 4_566 2_545 ? K1 Se2 K1 98.23(2) 4_565 2_545 ? K1 Se2 K1 169.51(3) 2_645 2_545 ? Se3B Se3A Ge1 83.61(11) . . ? Se3B Se3A Se3B 160.89(12) . 4_566 ? Ge1 Se3A Se3B 92.16(4) . 4_566 ? Se3B Se3A K1 88.96(12) . 2_645 ? Ge1 Se3A K1 86.66(4) . 2_645 ? Se3B Se3A K1 72.15(3) 4_566 2_645 ? Se3B Se3A K1 63.93(10) . 3_665 ? Ge1 Se3A K1 124.49(4) . 3_665 ? Se3B Se3A K1 131.74(5) 4_566 3_665 ? K1 Se3A K1 132.60(4) 2_645 3_665 ? Se3A Se3B Ge1 78.62(10) . . ? Se3A Se3B Se3A 167.87(11) . 4_565 ? Ge1 Se3B Se3A 102.03(4) . 4_565 ? Se3A Se3B K1 78.78(11) . 2_645 ? Ge1 Se3B K1 84.67(3) . 2_645 ? Se3A Se3B K1 113.35(4) 4_565 2_645 ? Se3A Se3B K1 105.36(11) . 3_665 ? Ge1 Se3B K1 134.72(4) . 3_665 ? Se3A Se3B K1 65.43(3) 4_565 3_665 ? K1 Se3B K1 140.61(4) 2_645 3_665 ? Se2 Ge1 Se1 108.42(3) . 4_565 ? Se2 Ge1 Se1 117.76(3) . . ? Se1 Ge1 Se1 98.08(3) 4_565 . ? Se2 Ge1 Se3A 114.45(4) . . ? Se1 Ge1 Se3A 118.94(4) 4_565 . ? Se1 Ge1 Se3A 98.19(4) . . ? Se2 Ge1 Se3B 115.31(3) . . ? Se1 Ge1 Se3B 103.76(3) 4_565 . ? Se1 Ge1 Se3B 111.01(3) . . ? Se3A Ge1 Se3B 17.78(3) . . ? Se2 Ge1 K1 58.21(2) . 4_565 ? Se1 Ge1 K1 60.65(2) 4_565 4_565 ? Se1 Ge1 K1 149.94(3) . 4_565 ? Se3A Ge1 K1 110.53(4) . 4_565 ? Se3B Ge1 K1 95.48(3) . 4_565 ? Se2 Ge1 K1 57.44(2) . 2_645 ? Se1 Ge1 K1 131.30(3) 4_565 2_645 ? Se1 Ge1 K1 130.37(3) . 2_645 ? Se3A Ge1 K1 57.47(3) . 2_645 ? Se3B Ge1 K1 59.00(3) . 2_645 ? K1 Ge1 K1 75.24(2) 4_565 2_645 ? Se2 K1 Se2 146.73(4) 4_565 4_566 ? Se2 K1 Se2 95.58(3) 4_565 2_655 ? Se2 K1 Se2 87.74(3) 4_566 2_655 ? Se2 K1 Se3A 120.25(3) 4_565 2_655 ? Se2 K1 Se3A 91.91(3) 4_566 2_655 ? Se2 K1 Se3A 69.22(3) 2_655 2_655 ? Se2 K1 Se2 93.36(3) 4_565 2 ? Se2 K1 Se2 81.77(2) 4_566 2 ? Se2 K1 Se2 169.51(3) 2_655 2 ? Se3A K1 Se2 110.69(3) 2_655 2 ? Se2 K1 Se3B 132.39(3) 4_565 2_655 ? Se2 K1 Se3B 79.65(3) 4_566 2_655 ? Se2 K1 Se3B 69.39(2) 2_655 2_655 ? Se3A K1 Se3B 12.26(2) 2_655 2_655 ? Se2 K1 Se3B 108.16(3) 2 2_655 ? Se2 K1 Se1 82.68(2) 4_565 . ? Se2 K1 Se1 65.21(2) 4_566 . ? Se2 K1 Se1 109.72(3) 2_655 . ? Se3A K1 Se1 157.03(4) 2_655 . ? Se2 K1 Se1 66.00(2) 2 . ? Se3B K1 Se1 144.78(3) 2_655 . ? Se2 K1 Se3B 77.92(3) 4_565 3_665 ? Se2 K1 Se3B 134.15(3) 4_566 3_665 ? Se2 K1 Se3B 73.85(2) 2_655 3_665 ? Se3A K1 Se3B 42.42(2) 2_655 3_665 ? Se2 K1 Se3B 113.54(3) 2 3_665 ? Se3B K1 Se3B 54.667(17) 2_655 3_665 ? Se1 K1 Se3B 160.55(3) . 3_665 ? Se2 K1 Se3A 67.25(3) 4_565 3_665 ? Se2 K1 Se3A 144.42(3) 4_566 3_665 ? Se2 K1 Se3A 75.05(2) 2_655 3_665 ? Se3A K1 Se3A 53.032(17) 2_655 3_665 ? Se2 K1 Se3A 113.67(3) 2 3_665 ? Se3B K1 Se3A 65.25(3) 2_655 3_665 ? Se1 K1 Se3A 149.93(3) . 3_665 ? Se3B K1 Se3A 10.71(2) 3_665 3_665 ? Se2 K1 Ge1 112.94(3) 4_565 4_566 ? Se2 K1 Ge1 33.968(14) 4_566 4_566 ? Se2 K1 Ge1 87.53(3) 2_655 4_566 ? Se3A K1 Ge1 123.06(3) 2_655 4_566 ? Se2 K1 Ge1 83.92(2) 2 4_566 ? Se3B K1 Ge1 111.23(3) 2_655 4_566 ? Se1 K1 Ge1 35.800(15) . 4_566 ? Se3B K1 Ge1 159.57(3) 3_665 4_566 ? Se3A K1 Ge1 162.40(3) 3_665 4_566 ? Se2 K1 Ge1 113.55(3) 4_565 2_655 ? Se2 K1 Ge1 86.89(2) 4_566 2_655 ? Se2 K1 Ge1 33.546(15) 2_655 2_655 ? Se3A K1 Ge1 35.87(2) 2_655 2_655 ? Se2 K1 Ge1 144.40(3) 2 2_655 ? Se3B K1 Ge1 36.333(17) 2_655 2_655 ? Se1 K1 Ge1 137.18(3) . 2_655 ? Se3B K1 Ge1 54.90(2) 3_665 2_655 ? Se3A K1 Ge1 61.59(2) 3_665 2_655 ? Ge1 K1 Ge1 104.76(2) 4_566 2_655 ? Se2 K1 K1 48.202(19) 4_565 3_665 ? Se2 K1 K1 126.06(4) 4_566 3_665 ? Se2 K1 K1 47.37(2) 2_655 3_665 ? Se3A K1 K1 96.12(3) 2_655 3_665 ? Se2 K1 K1 141.25(4) 2 3_665 ? Se3B K1 K1 103.58(3) 2_655 3_665 ? Se1 K1 K1 99.12(3) . 3_665 ? Se3B K1 K1 68.72(3) 3_665 3_665 ? Se3A K1 K1 61.38(3) 3_665 3_665 ? Ge1 K1 K1 104.82(3) 4_566 3_665 ? Ge1 K1 K1 70.80(2) 2_655 3_665 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 29.16 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.827 _refine_diff_density_min -1.407 _refine_diff_density_rms 0.199 #======================================================================= data_K4Ge4-xPxSe12_Modulated #======================================================================= # 5. CHEMICAL DATA _chemical_formula_sum 'Ge2.731 K4 P1.269 Se12' _chemical_formula_weight 1341.5 #======================================================================= # 6. CRYSTAL DATA _space_group_crystal_system monoclinic _space_group_ssg_name 'P21(\a0\g)0' loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,x2+1/2,-x3,-x4 _cell_length_a 6.7285(6) _cell_length_b 13.5089(11) _cell_length_c 6.3781(6) _cell_angle_alpha 90 _cell_angle_beta 90.875(7) _cell_angle_gamma 90 _cell_volume 579.67(9) _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.4442(6) 0.000000 0.3407(6) _cell_formula_units_Z 1 _cell_measurement_reflns_used 17881 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 100 _exptl_crystal_density_diffrn 3.8416 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 590 _exptl_absorpt_coefficient_mu 23.15 _exptl_crystal_type_of_structure mod _exptl_crystal_description rod _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_colour red _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'X-Shape2' _exptl_absorpt_correction_T_min 0.0816 _exptl_absorpt_correction_T_max 0.5464 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type 'STOE' _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 270 frames, detector distance = 100 mm ; _diffrn_reflns_number 22085 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 29.27 _diffrn_reflns_theta_full 29.27 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measured_fraction_theta_full 0.98 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_unetI/netI 0.0621 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_index_m_1_min -1 _diffrn_reflns_limit_index_m_1_max 1 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? #======================================================================= # 8. REFINEMENT DATA _reflns_number_total 9259 _reflns_number_gt 4072 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_gt 0.1640 _refine_ls_R_factor_all 0.1736 _refine_ls_wR_factor_ref 0.2020 _refine_ls_goodness_of_fit_ref 1.90 _refine_ls_goodness_of_fit_gt 2.35 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 9259 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_number_constraints 23 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.0016I^2^)' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max 0.0231 _refine_ls_shift/su_mean 0.0041 _refine_diff_density_max 7.00 _refine_diff_density_min -6.00 _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 Ge 0.1547 1.8001 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' K 0.2009 0.2494 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' P 0.1023 0.0942 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Se -0.0929 2.2259 '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 Se1 Se 0.0696(4) -0.495985 0.5537(2) Uani 0.0233(6) 2 1 d . . . Se2 Se 0.2435(3) -0.7677(2) 0.47827(19) Uani 0.0179(5) 2 1 d . . . Se3 Se 0.0713(4) -0.60362(10) 1.0543(2) Uani 0.0250(6) 2 1 d . . . Se4 Se 0.2414(3) -0.3324(2) 0.9785(2) Uani 0.0182(5) 2 1 d . . . Se5 Se 0.5666(3) -0.5492(2) 0.3083(5) Uani 0.0463(9) 2 1 d . . . Se6 Se 0.5648(4) -0.5574(3) 0.8435(5) Uani 0.0421(9) 2 1 d . . . Ge1 Ge 0.2468(5) -0.4858(3) 0.8670(4) Uani 0.0114(10) 2 0.692(17) d . . . P1 P 0.2468(5) -0.4858(3) 0.8670(4) Uani 0.0114(10) 2 0.308(17) d . . . Ge2 Ge 0.2527(9) -0.6118(5) 0.3673(9) Uani 0.0116(11) 2 0.673(17) d . . . P2 P 0.2527(9) -0.6118(5) 0.3673(9) Uani 0.0116(11) 2 0.327(17) d . . . K1 K 0.2616(6) -0.8362(4) 0.9737(4) Uani 0.0209(11) 2 1 d . . . K2 K 0.2584(7) -0.2603(3) 0.4778(5) Uani 0.0212(10) 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 Se1 Se 0.0404(15) 0.0175(9) 0.0120(6) 0.0093(9) -0.0061(7) 0.0002(6) Se2 Se 0.0242(11) 0.0263(9) 0.0031(5) -0.0010(8) -0.0014(6) -0.0013(6) Se3 Se 0.0369(15) 0.0187(9) 0.0190(7) -0.0094(9) -0.0076(8) 0.0046(7) Se4 Se 0.0113(9) 0.0243(9) 0.0191(6) 0.0015(8) -0.0008(6) -0.0058(7) Se5 Se 0.0118(10) 0.0216(9) 0.105(2) -0.0024(8) -0.0039(12) 0.0146(13) Se6 Se 0.0141(11) 0.0300(13) 0.082(2) 0.0057(10) -0.0045(11) -0.0201(14) Ge1 Ge 0.018(2) 0.0083(17) 0.0078(13) 0.0025(14) -0.0034(11) -0.0017(10) P1 P 0.018(2) 0.0083(17) 0.0078(13) 0.0025(14) -0.0034(11) -0.0017(10) Ge2 Ge 0.012(2) 0.009(2) 0.0138(13) 0.0050(16) 0.0002(12) -0.0020(12) P2 P 0.012(2) 0.009(2) 0.0138(13) 0.0050(16) 0.0002(12) -0.0020(12) K1 K 0.021(2) 0.039(2) 0.0025(10) 0.0056(18) -0.0040(11) 0.0067(12) K2 K 0.017(2) 0.0161(16) 0.0308(15) -0.0049(15) 0.0031(14) -0.0001(14) loop_ _atom_site_Fourier_wave_vector_seq_id _atom_site_Fourier_wave_vector_x _atom_site_Fourier_wave_vector_y _atom_site_Fourier_wave_vector_z 1 0.4442 0.000000 0.3407 loop_ _atom_site_occ_Fourier_id _atom_site_occ_Fourier_atom_site_label _atom_site_occ_Fourier_wave_vector_seq_id Ge1o1 Ge1 1 P1o1 P1 1 Ge2o1 Ge2 1 P2o1 P2 1 loop_ _atom_site_occ_Fourier_param_id _atom_site_occ_Fourier_param_cos _atom_site_occ_Fourier_param_sin Ge1o1 0.057(12) 0.196(14) P1o1 -0.057(12) -0.196(14) Ge2o1 -0.105(14) -0.223(16) P2o1 0.105(14) 0.223(16) 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 Se1x1 Se1 x 1 Se1y1 Se1 y 1 Se1z1 Se1 z 1 Se1x2 Se2 x 1 Se1y2 Se2 y 1 Se1z2 Se2 z 1 Se1x3 Se3 x 1 Se1y3 Se3 y 1 Se1z3 Se3 z 1 Se1x4 Se4 x 1 Se1y4 Se4 y 1 Se1z4 Se4 z 1 Se1x5 Se5 x 1 Se1y5 Se5 y 1 Se1z5 Se5 z 1 Se1x6 Se6 x 1 Se1y6 Se6 y 1 Se1z6 Se6 z 1 Ge1x1 Ge1 x 1 Ge1y1 Ge1 y 1 Ge1z1 Ge1 z 1 P1x1 P1 x 1 P1y1 P1 y 1 P1z1 P1 z 1 Ge2x1 Ge2 x 1 Ge2y1 Ge2 y 1 Ge2z1 Ge2 z 1 P2x1 P2 x 1 P2y1 P2 y 1 P2z1 P2 z 1 K1x1 K1 x 1 K1y1 K1 y 1 K1z1 K1 z 1 K2x1 K2 x 1 K2y1 K2 y 1 K2z1 K2 z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Se1x1 -0.0075(7) 0.0156(6) Se1y1 -0.0019(2) 0.0025(2) Se1z1 -0.0040(3) -0.0053(4) Se1x2 -0.0025(6) -0.0004(6) Se1y2 -0.0010(2) 0.0044(2) Se1z2 0.0000(3) 0.0013(3) Se1x3 0.0077(7) -0.0138(6) Se1y3 -0.0015(2) 0.0032(2) Se1z3 0.0041(4) 0.0074(4) Se1x4 0.0022(6) -0.0002(5) Se1y4 -0.0002(2) 0.0054(2) Se1z4 -0.0001(4) -0.0020(4) Se1x5 -0.0024(5) -0.0003(6) Se1y5 0.0025(3) -0.0010(3) Se1z5 0.0302(6) 0.0269(7) Se1x6 0.0036(6) -0.0032(6) Se1y6 0.0104(3) -0.0053(4) Se1z6 -0.0692(6) 0.0079(8) Ge1x1 0.0038(15) 0.0002(11) Ge1y1 0.0022(6) -0.0016(6) Ge1z1 -0.0059(12) 0.0016(9) P1x1 -0.018(11) -0.037(6) P1y1 -0.016(5) 0.018(3) P1z1 0.013(8) 0.004(5) Ge2x1 0.0004(19) 0.009(2) Ge2y1 0.0025(6) 0.0018(12) Ge2z1 0.0023(14) -0.003(2) P2x1 0.002(11) -0.018(11) P2y1 -0.017(3) 0.002(6) P2z1 0.017(8) 0.005(11) K1x1 -0.0015(12) 0.0000(12) K1y1 -0.0008(5) 0.0040(5) K1z1 -0.0013(7) 0.0007(7) K2x1 0.0019(12) -0.0001(12) K2y1 -0.0011(5) 0.0050(5) K2z1 -0.0008(9) -0.0038(9) 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 Se1U111 Se1 U11 1 Se1U221 Se1 U22 1 Se1U331 Se1 U33 1 Se1U121 Se1 U12 1 Se1U131 Se1 U13 1 Se1U231 Se1 U23 1 Se2U111 Se2 U11 1 Se2U221 Se2 U22 1 Se2U331 Se2 U33 1 Se2U121 Se2 U12 1 Se2U131 Se2 U13 1 Se2U231 Se2 U23 1 Se3U111 Se3 U11 1 Se3U221 Se3 U22 1 Se3U331 Se3 U33 1 Se3U121 Se3 U12 1 Se3U131 Se3 U13 1 Se3U231 Se3 U23 1 Se4U111 Se4 U11 1 Se4U221 Se4 U22 1 Se4U331 Se4 U33 1 Se4U121 Se4 U12 1 Se4U131 Se4 U13 1 Se4U231 Se4 U23 1 Se5U111 Se5 U11 1 Se5U221 Se5 U22 1 Se5U331 Se5 U33 1 Se5U121 Se5 U12 1 Se5U131 Se5 U13 1 Se5U231 Se5 U23 1 Se6U111 Se6 U11 1 Se6U221 Se6 U22 1 Se6U331 Se6 U33 1 Se6U121 Se6 U12 1 Se6U131 Se6 U13 1 Se6U231 Se6 U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Se1U111 0.006(2) -0.006(3) Se1U221 0.0008(14) 0.0014(15) Se1U331 0.0008(11) 0.0029(9) Se1U121 0.0022(16) -0.0036(15) Se1U131 -0.0006(13) -0.0003(11) Se1U231 -0.0001(8) 0.0028(9) Se2U111 0.0015(19) -0.0006(19) Se2U221 0.0012(16) 0.0053(15) Se2U331 0.0003(8) -0.0010(8) Se2U121 0.0028(14) -0.0025(13) Se2U131 0.0001(10) -0.0001(10) Se2U231 -0.0004(8) 0.0011(8) Se3U111 -0.005(2) 0.001(3) Se3U221 0.0007(15) 0.0017(15) Se3U331 0.0014(12) -0.0051(10) Se3U121 -0.0013(16) 0.0035(15) Se3U131 0.0035(14) 0.0038(12) Se3U231 0.0002(9) -0.0026(10) Se4U111 0.0010(16) 0.0015(17) Se4U221 -0.0003(16) -0.0111(16) Se4U331 -0.0012(10) -0.0003(10) Se4U121 0.0019(13) -0.0002(13) Se4U131 -0.0011(11) 0.0004(11) Se4U231 0.0025(9) 0.0008(9) Se5U111 -0.0135(13) 0.0031(17) Se5U221 -0.0052(16) -0.002(2) Se5U331 0.120(3) 0.043(2) Se5U121 -0.0025(12) -0.0024(18) Se5U131 -0.0039(14) -0.0020(18) Se5U231 0.0449(16) 0.0160(19) Se6U111 -0.0152(14) 0.0021(19) Se6U221 -0.0025(18) -0.023(2) Se6U331 0.069(2) 0.016(3) Se6U121 -0.0014(14) -0.0008(18) Se6U131 -0.0050(13) 0.002(2) Se6U231 -0.0212(17) 0.014(2) #======================================================================= # 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 Se1 Se3 . 1_5545 3.504(4) 3.442(4) 3.567(4) ? Se1 Se3 . . 3.512(4) 3.453(4) 3.569(4) ? Se1 Ge1 . . 2.318(9) 2.266(8) 2.366(9) ? Se1 P1 . . 2.33(5) 2.27(5) 2.41(4) ? Se1 Ge2 . . 2.330(14) 2.293(14) 2.366(14) ? Se1 P2 . . 2.34(7) 2.15(7) 2.52(7) ? Se1 K2 . . 3.466(9) 3.410(9) 3.521(9) ? Se2 Ge2 . . 2.223(14) 2.185(14) 2.261(14) ? Se2 P2 . . 2.22(7) 1.97(5) 2.48(5) ? Se2 K1 . 1_5545 3.353(6) 3.323(6) 3.384(6) ? Se2 K1 . . 3.293(6) 3.276(6) 3.311(6) ? Se2 K2 . 2_5465 3.395(10) 3.385(11) 3.408(11) ? Se2 K2 . 2_6465 3.361(10) 3.343(10) 3.380(10) ? Se3 Ge1 . . 2.325(10) 2.268(10) 2.380(10) ? Se3 P1 . . 2.33(5) 2.06(6) 2.59(6) ? Se3 Ge2 . 1_5565 2.330(14) 2.298(14) 2.357(14) ? Se3 P2 . 1_5565 2.33(6) 2.22(6) 2.44(6) ? Se3 K1 . . 3.436(9) 3.381(10) 3.491(10) ? Se4 Ge1 . . 2.193(10) 2.111(10) 2.274(10) ? Se4 P1 . . 2.20(5) 1.94(5) 2.45(5) ? Se4 K1 . 2_5575 3.404(10) 3.391(10) 3.418(10) ? Se4 K1 . 2_6575 3.355(10) 3.340(10) 3.370(10) ? Se4 K2 . . 3.343(7) 3.305(7) 3.381(7) ? Se4 K2 . 1_5565 3.331(7) 3.324(7) 3.337(7) ? Se5 Se6 . 1_5545 2.970(8) 2.278(7) 3.665(7) ? Se5 Se6 . . 3.421(8) 2.998(7) 3.833(7) ? Se5 Ge1 . 1_5545 3.623(10) 3.415(9) 3.835(9) ? Se5 Ge2 . . 2.317(15) 2.220(16) 2.414(15) ? Se5 P2 . . 2.32(7) 2.20(7) 2.42(7) ? Se5 K2 . 2_6465 3.372(9) 3.310(10) 3.432(9) ? Se6 Ge1 . . 2.375(11) 2.345(11) 2.396(10) ? Se6 P1 . . 2.40(6) 2.05(5) 2.73(4) ? Se6 Ge2 . . 3.753(14) 3.480(15) 4.042(15) ? Se6 P2 . . 3.75(6) 3.41(7) 4.08(7) ? Se6 K1 . 2_6575 3.426(10) 3.381(10) 3.470(10) ? Se6 K2 . 2_6465 3.648(10) 3.494(9) 3.827(9) ? Ge1 P1 . . 0.34(6) 0.29(6) 0.38(5) ? Ge1 P2 . 1_5565 3.62(6) 3.37(5) 3.87(5) ? P1 Ge2 . 1_5565 3.63(5) 3.41(5) 3.84(5) ? Ge2 P2 . . 0.24(7) 0.19(7) 0.28(5) ? 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 Se3 Se1 Se3 1_5545 . . 130.82(12) 129.50(13) 132.03(12) ? Se3 Se1 Ge1 1_5545 . . 143.1(3) 138.9(3) 147.0(3) ? Se3 Se1 P1 1_5545 . . 143.4(11) 135.7(10) 151.1(11) ? Se3 Se1 Ge2 1_5545 . . 41.2(4) 40.3(4) 42.2(4) ? Se3 Se1 P2 1_5545 . . 41.2(17) 38.6(19) 43.4(16) ? Se3 Se1 K2 1_5545 . . 104.35(15) 102.16(15) 106.49(15) ? Se3 Se1 Ge1 . . . 40.9(2) 39.4(2) 42.4(2) ? Se3 Se1 P1 . . . 41.2(11) 34.9(11) 47.1(11) ? Se3 Se1 Ge2 . . . 101.0(4) 99.1(4) 103.0(4) ? Se3 Se1 P2 . . . 101.0(18) 96.6(17) 106(2) ? Se3 Se1 K2 . . . 120.72(16) 118.72(16) 122.77(16) ? Ge1 Se1 P1 . . . 8.1(11) 7.0(11) 9.3(12) ? Ge1 Se1 Ge2 . . . 102.1(5) 99.3(5) 104.8(5) ? Ge1 Se1 P2 . . . 102.3(18) 96.7(16) 108.5(19) ? Ge1 Se1 K2 . . . 83.2(3) 79.2(3) 87.1(3) ? P1 Se1 Ge2 . . . 102.4(14) 94.4(12) 110.4(13) ? P1 Se1 P2 . . . 103(2) 94(2) 111(2) ? P1 Se1 K2 . . . 83.0(13) 77.8(13) 88.0(13) ? Ge2 Se1 P2 . . . 4.7(19) 2.5(17) 6(2) ? Ge2 Se1 K2 . . . 110.4(4) 107.0(4) 113.7(4) ? P2 Se1 K2 . . . 110.4(17) 104.4(17) 116.7(19) ? Ge2 Se2 P2 . . . 3.2(19) 0.1(17) 5.0(19) ? Ge2 Se2 K1 . . 1_5545 87.4(4) 86.0(3) 88.7(3) ? Ge2 Se2 K1 . . . 124.8(4) 122.8(4) 126.9(4) ? Ge2 Se2 K2 . . 2_5465 91.8(4) 88.4(4) 95.1(4) ? Ge2 Se2 K2 . . 2_6465 88.0(4) 86.9(4) 89.1(4) ? P2 Se2 K1 . . 1_5545 87.4(16) 85.8(14) 89.1(17) ? P2 Se2 K1 . . . 124.8(16) 123.1(15) 126.3(12) ? P2 Se2 K2 . . 2_5465 91.8(19) 90.2(19) 93.3(19) ? P2 Se2 K2 . . 2_6465 88.0(19) 84.5(19) 91.7(19) ? K1 Se2 K1 1_5545 . . 147.4(2) 146.3(2) 148.4(2) ? K1 Se2 K2 1_5545 . 2_5465 97.9(2) 96.8(2) 99.1(2) ? K1 Se2 K2 1_5545 . 2_6465 92.1(2) 91.2(2) 93.1(2) ? K1 Se2 K2 . . 2_5465 87.2(2) 87.1(2) 87.3(2) ? K1 Se2 K2 . . 2_6465 84.6(2) 84.4(2) 84.8(2) ? K2 Se2 K2 2_5465 . 2_6465 169.78(19) 168.5(2) 170.87(18) ? Se1 Se3 Se1 . . 1_5565 130.85(13) 129.39(13) 132.01(13) ? Se1 Se3 Ge1 . . . 40.8(2) 39.8(2) 41.8(2) ? Se1 Se3 P1 . . . 41.0(9) 39.3(9) 43.8(10) ? Se1 Se3 Ge2 . . 1_5565 142.4(4) 139.7(4) 144.9(4) ? Se1 Se3 P2 . . 1_5565 142.5(19) 134.4(19) 150.7(19) ? Se1 Se3 K1 . . . 103.77(14) 101.12(14) 106.53(14) ? Se1 Se3 Ge1 1_5565 . . 101.0(2) 100.4(2) 101.5(2) ? Se1 Se3 P1 1_5565 . . 101.2(10) 97.5(9) 105.2(10) ? Se1 Se3 Ge2 1_5565 . 1_5565 41.2(4) 40.0(4) 42.4(4) ? Se1 Se3 P2 1_5565 . 1_5565 41.3(19) 37(2) 45.1(18) ? Se1 Se3 K1 1_5565 . . 121.41(15) 119.70(15) 123.27(15) ? Ge1 Se3 P1 . . . 5.8(11) 0.7(9) 9.2(12) ? Ge1 Se3 Ge2 . . 1_5565 102.0(5) 100.0(5) 103.8(5) ? Ge1 Se3 P2 . . 1_5565 102.0(19) 95(2) 109.3(19) ? Ge1 Se3 K1 . . . 110.8(3) 106.3(3) 115.4(3) ? P1 Se3 Ge2 . . 1_5565 102.3(13) 101.0(11) 103.7(13) ? P1 Se3 P2 . . 1_5565 102(2) 96(2) 109(3) ? P1 Se3 K1 . . . 110.8(14) 106.6(11) 114.9(11) ? Ge2 Se3 P2 1_5565 . 1_5565 6(2) 4.4(18) 7(2) ? Ge2 Se3 K1 1_5565 . . 83.8(4) 80.3(3) 87.4(3) ? P2 Se3 K1 1_5565 . . 83.9(16) 80.7(16) 87.2(18) ? Ge1 Se4 P1 . . . 6.5(11) 4.9(9) 7.7(12) ? Ge1 Se4 K1 . . 2_5575 92.0(3) 90.2(3) 93.9(3) ? Ge1 Se4 K1 . . 2_6575 89.6(3) 88.0(3) 91.2(3) ? Ge1 Se4 K2 . . . 88.0(3) 85.7(3) 90.2(3) ? Ge1 Se4 K2 . . 1_5565 125.9(3) 123.1(3) 128.7(3) ? P1 Se4 K1 . . 2_5575 92.0(15) 83.2(13) 100.3(13) ? P1 Se4 K1 . . 2_6575 89.7(15) 84.0(13) 95.8(13) ? P1 Se4 K2 . . . 87.8(12) 84.2(15) 90.9(12) ? P1 Se4 K2 . . 1_5565 125.9(12) 123.0(13) 129.3(15) ? K1 Se4 K1 2_5575 . 2_6575 169.31(17) 168.22(18) 170.08(16) ? K1 Se4 K2 2_5575 . . 98.0(2) 96.8(2) 99.1(2) ? K1 Se4 K2 2_5575 . 1_5565 86.5(2) 86.1(2) 86.8(2) ? K1 Se4 K2 2_6575 . . 92.4(2) 91.9(2) 93.0(2) ? K1 Se4 K2 2_6575 . 1_5565 84.1(2) 83.6(2) 84.7(2) ? K2 Se4 K2 . . 1_5565 145.8(2) 144.4(2) 147.2(2) ? Se6 Se5 Se6 1_5545 . . 175.6(2) 173.6(3) 177.3(2) ? Se6 Se5 Ge1 1_5545 . 1_5545 40.58(17) 37.11(15) 44.42(19) ? Se6 Se5 Ge2 1_5545 . . 98.8(4) 94.8(4) 102.2(4) ? Se6 Se5 P2 1_5545 . . 99.0(17) 96.8(17) 101.1(18) ? Se6 Se5 K2 1_5545 . 2_6465 111.3(2) 108.77(19) 113.4(2) ? Se6 Se5 Ge1 . . 1_5545 140.6(2) 136.9(2) 144.06(19) ? Se6 Se5 Ge2 . . . 79.1(4) 74.2(4) 83.9(4) ? Se6 Se5 P2 . . . 78.9(17) 75.8(17) 81.9(18) ? Se6 Se5 K2 . . 2_6465 64.83(18) 61.45(18) 67.97(19) ? Ge1 Se5 Ge2 1_5545 . . 71.1(4) 68.1(4) 73.9(4) ? Ge1 Se5 P2 1_5545 . . 71.2(18) 69.4(18) 72.7(18) ? Ge1 Se5 K2 1_5545 . 2_6465 135.5(2) 130.7(2) 140.1(2) ? Ge2 Se5 P2 . . . 4(2) 1.0(19) 7(2) ? Ge2 Se5 K2 . . 2_6465 86.3(4) 83.0(3) 89.5(4) ? P2 Se5 K2 . . 2_6465 86.3(17) 81.8(15) 90.2(15) ? Se5 Se6 Se5 . . 1_5565 175.2(2) 169.6(3) 179.45(19) ? Se5 Se6 Ge1 . . . 93.7(2) 83.3(2) 104.3(2) ? Se5 Se6 P1 . . . 94.1(9) 82.2(8) 107.1(9) ? Se5 Se6 Ge2 . . . 37.5(3) 32.8(2) 42.5(3) ? Se5 Se6 P2 . . . 37.5(11) 35.4(10) 39.7(12) ? Se5 Se6 K1 . . 2_6575 107.9(2) 97.84(17) 118.4(2) ? Se5 Se6 K2 . . 2_6465 57.02(16) 51.57(15) 62.61(17) ? Se5 Se6 Ge1 1_5565 . . 84.8(2) 75.3(2) 93.9(3) ? Se5 Se6 P1 1_5565 . . 84.2(9) 72.3(9) 94.2(8) ? Se5 Se6 Ge2 1_5565 . . 144.2(3) 136.5(3) 151.3(3) ? Se5 Se6 P2 1_5565 . . 144.3(11) 139.9(12) 148.8(10) ? Se5 Se6 K1 1_5565 . 2_6575 67.84(18) 62.59(15) 72.2(2) ? Se5 Se6 K2 1_5565 . 2_6465 126.7(2) 117.2(2) 136.3(2) ? Ge1 Se6 P1 . . . 5.3(11) 0.6(11) 8.6(11) ? Ge1 Se6 Ge2 . . . 68.1(3) 62.4(3) 73.3(3) ? Ge1 Se6 P2 . . . 68.3(12) 60.9(11) 75.6(13) ? Ge1 Se6 K1 . . 2_6575 85.0(3) 83.6(3) 87.3(3) ? Ge1 Se6 K2 . . 2_6465 129.4(3) 121.8(3) 135.4(3) ? P1 Se6 Ge2 . . . 68.3(11) 64.1(10) 72.4(11) ? P1 Se6 P2 . . . 68.6(16) 62.3(16) 74.8(17) ? P1 Se6 K1 . . 2_6575 84.9(13) 79.2(12) 89.3(14) ? P1 Se6 K2 . . 2_6465 128.6(12) 124.1(10) 131.7(13) ? Ge2 Se6 P2 . . . 3.6(12) 2.6(10) 4.4(13) ? Ge2 Se6 K1 . . 2_6575 129.2(3) 117.8(3) 140.4(3) ? Ge2 Se6 K2 . . 2_6465 64.9(3) 60.1(3) 69.8(3) ? P2 Se6 K1 . . 2_6575 129.4(10) 119.6(12) 139.4(14) ? P2 Se6 K2 . . 2_6465 65.0(11) 60.5(10) 70.0(10) ? K1 Se6 K2 2_6575 . 2_6465 136.7(2) 130.2(2) 141.2(3) ? Se1 Ge1 Se3 . . . 98.3(4) 95.8(4) 100.8(4) ? Se1 Ge1 Se4 . . . 108.9(4) 106.7(4) 111.1(4) ? Se1 Ge1 Se5 . . 1_5565 161.1(4) 159.5(4) 163.0(4) ? Se1 Ge1 Se6 . . . 112.2(4) 104.8(3) 119.6(4) ? Se1 Ge1 P1 . . . 88(6) 74(6) 106(6) ? Se1 Ge1 P2 . . 1_5565 137.1(13) 131.2(12) 143.1(13) ? Se3 Ge1 Se4 . . . 118.0(4) 116.5(3) 119.6(4) ? Se3 Ge1 Se5 . . 1_5565 75.0(2) 71.0(2) 79.2(3) ? Se3 Ge1 Se6 . . . 102.7(4) 97.9(4) 107.2(4) ? Se3 Ge1 P1 . . . 89(7) 8(7) 174(7) ? Se3 Ge1 P2 . . 1_5565 39.1(12) 35.4(11) 42.9(13) ? Se4 Ge1 Se5 . . 1_5565 89.1(3) 86.5(2) 91.6(3) ? Se4 Ge1 Se6 . . . 115.3(4) 113.4(5) 117.5(5) ? Se4 Ge1 P1 . . . 89(7) 31(6) 146(6) ? Se4 Ge1 P2 . . 1_5565 99.0(13) 97.5(14) 100.5(13) ? Se5 Ge1 Se6 1_5565 . . 54.6(2) 41.7(2) 67.6(2) ? Se5 Ge1 P1 1_5565 . . 91(7) 58(6) 126(6) ? Se5 Ge1 P2 1_5565 . 1_5565 37.5(12) 35.4(11) 39.9(12) ? Se6 Ge1 P1 . . . 92(8) 4(7) 168(6) ? Se6 Ge1 P2 . . 1_5565 82.1(12) 72.8(13) 91.6(11) ? P1 Ge1 P2 . . 1_5565 88(8) 41(9) 135(10) ? Se1 P1 Se3 . . . 98(2) 92(2) 105(3) ? Se1 P1 Se4 . . . 109(2) 97.0(16) 122(2) ? Se1 P1 Se6 . . . 110.8(19) 106(2) 117(2) ? Se1 P1 Ge1 . . . 84(8) 66(6) 97(7) ? Se1 P1 Ge2 . . 1_5565 136(2) 129(2) 145(3) ? Se3 P1 Se4 . . . 117(2) 108.9(18) 126(2) ? Se3 P1 Se6 . . . 103(2) 86.1(15) 123(2) ? Se3 P1 Ge1 . . . 85(9) 5(9) 171(12) ? Se3 P1 Ge2 . . 1_5565 38.9(8) 36.8(7) 41.2(9) ? Se4 P1 Se6 . . . 114(2) 108(3) 123(3) ? Se4 P1 Ge1 . . . 85(9) 29(6) 143(8) ? Se4 P1 Ge2 . . 1_5565 98.5(14) 94.7(12) 102.2(13) ? Se6 P1 Ge1 . . . 83(10) 11(6) 176(9) ? Se6 P1 Ge2 . . 1_5565 82.7(14) 65.4(9) 102.4(15) ? Ge1 P1 Ge2 . . 1_5565 85(8) 39(9) 133(11) ? Se1 Ge2 Se2 . . . 117.1(6) 115.8(6) 118.5(6) ? Se1 Ge2 Se3 . . 1_5545 97.5(5) 95.4(5) 99.7(5) ? Se1 Ge2 Se5 . . . 109.2(6) 108.7(5) 109.6(5) ? Se1 Ge2 Se6 . . . 75.5(4) 72.7(3) 78.3(4) ? Se1 Ge2 P1 . . 1_5545 97.8(8) 92.0(7) 103.9(8) ? Se1 Ge2 P2 . . . 89(19) 30(20) 150(20) ? Se2 Ge2 Se3 . . 1_5545 107.5(6) 105.1(5) 110.0(5) ? Se2 Ge2 Se5 . . . 115.3(6) 113.7(6) 117.1(6) ? Se2 Ge2 Se6 . . . 87.0(4) 82.9(4) 91.4(5) ? Se2 Ge2 P1 . . 1_5545 136.3(9) 131.1(8) 141.7(8) ? Se2 Ge2 P2 . . . 89(19) 2(15) 179(15) ? Se3 Ge2 Se5 1_5545 . . 108.3(6) 103.9(5) 112.8(5) ? Se3 Ge2 Se6 1_5545 . . 164.8(6) 158.4(6) 171.5(5) ? Se3 Ge2 P1 1_5545 . 1_5545 38.8(7) 36.0(8) 41.4(7) ? Se3 Ge2 P2 1_5545 . . 88(18) 61(18) 114(18) ? Se5 Ge2 Se6 . . . 63.5(3) 57.3(3) 69.9(4) ? Se5 Ge2 P1 . . 1_5545 71.8(8) 65.4(7) 78.2(8) ? Se5 Ge2 P2 . . . 90(19) 10(20) 170(20) ? Se6 Ge2 P1 . . 1_5545 128.3(8) 118.1(8) 138.4(9) ? Se6 Ge2 P2 . . . 87(18) 70(20) 110(20) ? P1 Ge2 P2 1_5545 . . 86(18) 37(15) 135(16) ? Se1 P2 Se2 . . . 117(3) 110(3) 124(3) ? Se1 P2 Se3 . . 1_5545 98(3) 92(2) 104(3) ? Se1 P2 Se5 . . . 109(3) 100.5(19) 118(2) ? Se1 P2 Se6 . . . 75.4(16) 72.6(17) 77.5(18) ? Se1 P2 Ge1 . . 1_5545 98(2) 90.3(14) 106.2(18) ? Se1 P2 Ge2 . . . 86(17) 30(18) 140(20) ? Se2 P2 Se3 . . 1_5545 107(3) 103(2) 111(2) ? Se2 P2 Se5 . . . 115(3) 108(3) 123(3) ? Se2 P2 Se6 . . . 87.1(19) 81.7(18) 93(2) ? Se2 P2 Ge1 . . 1_5545 136(2) 134(2) 139(2) ? Se2 P2 Ge2 . . . 88(19) 1(11) 178(13) ? Se3 P2 Se5 1_5545 . . 108(3) 105(2) 111(3) ? Se3 P2 Se6 1_5545 . . 165(3) 158(2) 173(2) ? Se3 P2 Ge1 1_5545 . 1_5545 38.9(10) 34.8(8) 43.3(9) ? Se3 P2 Ge2 1_5545 . . 86(16) 61(14) 113(18) ? Se5 P2 Se6 . . . 63.6(15) 58.8(15) 68.0(15) ? Se5 P2 Ge1 . . 1_5545 71.3(16) 70.0(17) 73(2) ? Se5 P2 Ge2 . . . 86(18) 10(20) 170(20) ? Se6 P2 Ge1 . . 1_5545 128(2) 125(2) 131.7(19) ? Se6 P2 Ge2 . . . 90(16) 70(19) 110(20) ? Ge1 P2 Ge2 1_5545 . . 87(16) 38(11) 137(13) ? Se2 K1 Se2 . . 1_5565 147.4(3) 146.5(3) 148.2(3) ? Se2 K1 Se3 . . . 83.0(2) 81.3(2) 84.8(2) ? Se2 K1 Se4 . . 2_5475 93.4(2) 93.3(2) 93.5(2) ? Se2 K1 Se4 . . 2_6475 96.0(2) 95.5(2) 96.5(2) ? Se2 K1 Se6 . . 2_6475 125.6(3) 117.7(2) 133.5(3) ? Se2 K1 Se3 1_5565 . . 65.47(16) 64.12(16) 66.78(17) ? Se2 K1 Se4 1_5565 . 2_5475 81.89(19) 80.86(19) 82.88(19) ? Se2 K1 Se4 1_5565 . 2_6475 87.66(19) 87.25(19) 88.09(19) ? Se2 K1 Se6 1_5565 . 2_6475 86.07(19) 78.50(18) 93.5(2) ? Se3 K1 Se4 . . 2_5475 66.4(2) 66.2(2) 66.56(19) ? Se3 K1 Se4 . . 2_6475 110.2(3) 108.1(3) 112.3(3) ? Se3 K1 Se6 . . 2_6475 151.3(2) 143.3(2) 159.0(2) ? Se4 K1 Se4 2_5475 . 2_6475 169.4(2) 168.6(2) 170.02(19) ? Se4 K1 Se6 2_5475 . 2_6475 108.4(3) 107.8(3) 108.9(2) ? Se4 K1 Se6 2_6475 . 2_6475 69.4(2) 68.0(2) 70.8(2) ? Se1 K2 Se2 . . 2_5565 66.06(19) 65.82(19) 66.3(2) ? Se1 K2 Se2 . . 2_6565 109.1(3) 106.6(2) 111.8(3) ? Se1 K2 Se4 . . 1_5545 81.81(19) 80.40(19) 83.25(19) ? Se1 K2 Se4 . . . 65.22(16) 63.78(16) 66.65(17) ? Se1 K2 Se5 . . 2_6565 148.0(2) 143.4(2) 152.7(2) ? Se1 K2 Se6 . . 2_6565 153.7(2) 147.1(2) 160.6(2) ? Se2 K2 Se2 2_5565 . 2_6565 169.7(2) 168.0(2) 171.4(2) ? Se2 K2 Se4 2_5565 . 1_5545 92.9(2) 92.7(2) 93.1(2) ? Se2 K2 Se4 2_5565 . . 82.1(2) 81.0(2) 83.3(2) ? Se2 K2 Se5 2_5565 . 2_6565 109.4(2) 108.0(2) 110.9(3) ? Se2 K2 Se6 2_5565 . 2_6565 113.7(2) 111.9(2) 115.6(2) ? Se2 K2 Se4 2_6565 . 1_5545 95.2(2) 95.1(2) 95.4(2) ? Se2 K2 Se4 2_6565 . . 87.7(2) 87.1(2) 88.3(2) ? Se2 K2 Se5 2_6565 . 2_6565 69.5(2) 68.1(2) 70.7(2) ? Se2 K2 Se6 2_6565 . 2_6565 74.7(2) 73.6(2) 75.7(2) ? Se4 K2 Se4 1_5545 . . 145.8(3) 144.8(3) 146.9(3) ? Se4 K2 Se5 1_5545 . 2_6565 130.0(3) 124.3(3) 135.4(3) ? Se4 K2 Se6 1_5545 . 2_6565 72.00(18) 64.07(17) 80.2(2) ? Se4 K2 Se5 . . 2_6565 82.9(2) 78.22(19) 87.7(2) ? Se4 K2 Se6 . . 2_6565 140.6(3) 132.8(3) 147.9(3) ? Se5 K2 Se6 2_6565 . 2_6565 58.12(18) 51.18(18) 65.07(19) ? #======================================================================= data_rb6ge2p2se14 #======================================================================= _audit_creation_method SHELXL-97 _chemical_formula_moiety 'Ge2 P2 Se14, 6(Rb)' _chemical_formula_sum 'Ge2 P2 Rb6 Se14' _chemical_formula_weight 1825.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rb' 'Rb' -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_name_H-M_alt P-1 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 7.2463(8) _cell_length_b 9.7071(11) _cell_length_c 11.9866(14) _cell_angle_alpha 79.516(9) _cell_angle_beta 89.524(9) _cell_angle_gamma 68.281(9) _cell_volume 768.60(15) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16409 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 29.54 _exptl_crystal_type_of_structure cryst _exptl_crystal_description 'block' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.0914 _exptl_crystal_size_mid 0.0534 _exptl_crystal_size_min 0.0452 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 28.066 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2087 _exptl_absorpt_correction_T_max 0.4034 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS II' _diffrn_measurement_method 'rotation' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14609 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_unetI/netI 0.0317 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 29.24 _reflns_number_total 4135 _reflns_number_gt 3539 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ;Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+1.4322P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4135 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.295 _refine_ls_restrained_S_all 1.295 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.2286(2) 0.06850(17) 0.21878(12) 0.0174(3) Uani 1 1 d . . . Ge1 Ge 0.39997(9) 0.56355(7) 0.37222(5) 0.01892(13) Uani 1 1 d . . . Rb1 Rb 0.61626(10) 0.19545(8) 0.01481(5) 0.03265(15) Uani 1 1 d . . . Rb2 Rb 0.67943(10) 0.12269(8) 0.39641(6) 0.03071(14) Uani 1 1 d . . . Rb3 Rb 0.06357(11) 0.47282(8) 0.79032(6) 0.03474(16) Uani 1 1 d . . . Se1 Se 0.11005(11) 0.22290(8) 0.05694(5) 0.02958(15) Uani 1 1 d . . . Se2 Se 0.15079(10) 0.16840(7) 0.36781(5) 0.02596(14) Uani 1 1 d . . . Se3 Se 0.46218(9) 0.07732(8) 0.77599(6) 0.02753(14) Uani 1 1 d . . . Se4 Se 0.04177(9) 0.92895(7) 0.19668(5) 0.02168(13) Uani 1 1 d . . . Se5 Se 0.08328(9) 0.76410(7) 0.37105(5) 0.02402(13) Uani 1 1 d . . . Se6 Se 0.46641(10) 0.48303(7) 0.20551(5) 0.02562(14) Uani 1 1 d . . . Se7 Se 0.34495(10) 0.39450(7) 0.53097(5) 0.02389(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0161(6) 0.0200(7) 0.0158(6) -0.0027(5) 0.0007(5) -0.0069(6) Ge1 0.0200(3) 0.0208(3) 0.0152(3) -0.0035(2) 0.0004(2) -0.0068(2) Rb1 0.0306(3) 0.0404(4) 0.0256(3) -0.0001(3) 0.0015(2) -0.0147(3) Rb2 0.0301(3) 0.0278(3) 0.0311(3) -0.0068(2) -0.0015(2) -0.0067(3) Rb3 0.0331(3) 0.0319(3) 0.0385(4) -0.0044(3) -0.0001(3) -0.0125(3) Se1 0.0321(3) 0.0353(4) 0.0173(3) 0.0041(2) -0.0024(2) -0.0122(3) Se2 0.0315(3) 0.0282(3) 0.0177(3) -0.0066(2) 0.0028(2) -0.0097(3) Se3 0.0157(3) 0.0288(3) 0.0371(3) -0.0085(3) 0.0009(2) -0.0062(2) Se4 0.0165(3) 0.0255(3) 0.0237(3) -0.0038(2) -0.0022(2) -0.0091(2) Se5 0.0216(3) 0.0230(3) 0.0262(3) -0.0050(2) 0.0081(2) -0.0069(2) Se6 0.0335(3) 0.0261(3) 0.0178(3) -0.0069(2) 0.0033(2) -0.0106(3) Se7 0.0253(3) 0.0319(3) 0.0192(3) -0.0027(2) 0.0015(2) -0.0171(3) _geom_special_details ;All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 Se3 2.1566(16) 2_656 ? P1 Se2 2.1584(16) . ? P1 Se1 2.1827(16) . ? P1 Se4 2.2873(16) 1_545 ? Ge1 Se6 2.2605(9) . ? Ge1 Se7 2.3862(9) 2_666 ? Ge1 Se5 2.3959(9) . ? Ge1 Se7 2.4100(9) . ? Se3 P1 2.1566(16) 2_656 ? Se4 P1 2.2873(16) 1_565 ? Se4 Se5 2.3360(9) . ? Se7 Ge1 2.3862(9) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se3 P1 Se2 113.29(7) 2_656 . ? Se3 P1 Se1 115.08(7) 2_656 . ? Se2 P1 Se1 115.22(7) . . ? Se3 P1 Se4 107.70(7) 2_656 1_545 ? Se2 P1 Se4 110.54(7) . 1_545 ? Se1 P1 Se4 92.80(6) . 1_545 ? Se6 Ge1 Se7 118.20(4) . 2_666 ? Se6 Ge1 Se5 114.61(4) . . ? Se7 Ge1 Se5 111.46(4) 2_666 . ? Se6 Ge1 Se7 117.89(4) . . ? Se7 Ge1 Se7 95.59(3) 2_666 . ? Se5 Ge1 Se7 95.55(3) . . ? P1 Se4 Se5 105.14(5) 1_565 . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.24 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.905 _refine_diff_density_min -1.060 _refine_diff_density_rms 0.242