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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_AgCePSe6 _publ_contact_author_name 'Kanatzidis, Mercouri G.' _publ_contact_author_address ;Department of Chemistry and Center for Fundamental Materials Research Michigan State University East Lansing Michigan 48824 USA ; _publ_contact_author_email Kanatzid@cem.msu.edu loop_ _publ_author_name _publ_author_address 'Aitken, Jennifer A.' ;Department of Chemistry and Center for Fundamental Materials Research Michigan State University East Lansing Michigan 48824 USA ; 'Evain, Michel' ;I.M.N. UMR CNRS C6502 Institut des Materiaux Jean Rouxel Laboratoire de Chimie des Solides 2 rue de la Houssiniere BP 32229 44322 Nantes Cedex 03 France ; 'Iordanidis, Lykourgos' ;Department of Chemistry and Center for Fundamental Materials Research Michigan State University East Lansing Michigan 48824 USA ; 'Kanatzidis, Mercouri G.' ;Department of Chemistry and Center for Fundamental Materials Research Michigan State University East Lansing Michigan 48824 USA ; _publ_section_title ;NaCeP~2~Se~6~, Cu~0.4~Ce~1.2~P~2~Se~6~, Ce~4~(P~2~Se~6~)~3~, and the Incommensurately Modulated AgCeP~2~Se~6~: New Selenophosphates Featuring the Ethane-Like [P~2~Se~6~]^4-^ Anion ; _journal_name_full 'Inorganic Chemistry' _journal_volume 41 _journal_page_first 180 _journal_page_last 191 _journal_year 2002 _journal_paper_doi https://doi.org/10.1021/ic010618p _exptl_crystal_type_of_structure mod _cell_length_a 9.9557(7) _cell_length_b 7.4728(5) _cell_length_c 11.7383(8) _cell_angle_alpha 90 _cell_angle_beta 145.598(5) _cell_angle_gamma 90 _cell_volume 493.41(8) _cell_measurement_radiation 'Mo K\a' _cell_measurement_reflns_used 903 _cell_measurement_temperature 273 _cell_measurement_theta_max 27.97 _cell_measurement_theta_min 3.17 _cell_measurement_wavelength 0.71073 _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.312 0 0.412 _cell_formula_units_Z 2 _space_group_crystal_system monoclinic _space_group_ssg_name_IT P21/c(\a0\g) loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,1/2+x2,1/2-x3,-x4 3 -x1,-x2,-x3,-x4 4 x1,1/2-x2,1/2+x3,x4 loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_versus_stol_list Ag 0 -0.897 1.102 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 47.000 46.139 43.964 41.157 38.154 35.192 32.416 29.910 27.707 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 25.805 24.181 22.795 21.607 20.575 19.661 18.838 18.069 17.348 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 16.651 15.977 15.316 14.669 14.035 13.415 12.813 12.229 11.669 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 11.133 10.623 10.140 9.687 9.263 7.569 7.308 7.069 6.851 ; Ce 0 -0.249 2.633 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 58.000 56.385 53.047 49.579 46.233 43.042 40.104 37.474 35.139 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 33.051 31.154 29.409 27.791 26.289 24.901 23.626 22.469 21.421 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 20.481 19.637 18.881 18.201 17.583 17.018 16.491 15.997 15.526 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 15.074 14.633 14.202 13.776 13.355 11.333 10.949 10.576 10.215 ; P 0 0.102 0.094 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 15.000 14.458 13.138 11.629 10.327 9.335 8.600 8.029 7.547 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 7.103 6.674 6.250 5.829 5.418 5.020 4.640 4.284 3.953 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 3.649 3.372 3.122 2.898 2.698 2.521 2.364 2.226 2.104 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 1.997 1.903 1.820 1.747 1.683 1.453 1.420 1.389 1.360 ; Se 0 -0.093 2.226 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' ; stol 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 f 34.000 33.280 31.449 29.175 26.962 25.001 23.288 21.751 20.328 stol 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 f 18.977 17.682 16.444 15.269 14.166 13.145 12.208 11.362 10.602 stol 0.90 0.95 1.00 1.05 1.10 1.15 1.20 1.25 1.30 f 9.928 9.332 8.809 8.352 7.952 7.604 7.299 7.032 6.795 stol 1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75 f 6.585 6.395 6.222 6.063 5.915 5.262 5.140 5.020 4.901 ; _chemical_formula_sum 'Ag1 Ce1 P2 Se6' _chemical_formula_weight 783.7 _exptl_crystal_colour orange _exptl_crystal_description block _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 5.273 _exptl_crystal_F_000 678 _exptl_absorpt_correction_type none _exptl_absorpt_coefficient_mu 28.917 _exptl_absorpt_correction_T_min 1 _exptl_absorpt_correction_T_max 1 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type STOE _diffrn_measurement_method \q/2\q _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _reflns_limit_h_min -13 _reflns_limit_h_max 7 _reflns_limit_k_max 9 _reflns_limit_l_max 15 _reflns_limit_index_m_1_min -3 _reflns_limit_index_m_1_max 3 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.97 _reflns_threshold_expression 3 _reflns_number_total 2539 _reflns_number_gt 2539 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme sigma _refine_ls_weighting_details w=1/(\s^2^(I)+0.001024I^2^) _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_gt 0.0903 _refine_ls_R_factor_all 0.0458 _refine_ls_wR_factor_ref 0.0903 _refine_ls_number_reflns 2539 _refine_ls_number_parameters 207 _refine_ls_goodness_of_fit_ref 1.56 _refine_ls_goodness_of_fit_gt 1.56 _refine_ls_shift/su_max 0.0002 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_max 3.94 _refine_diff_density_min -2.51 _refine_ls_extinction_method 'B-C type 1 Lorentzian isotropic' _refine_ls_extinction_coef 0.058075 loop_ _atom_site_label _atom_site_type_symbol _atom_site_adp_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_site_symmetry_multiplicity _atom_site_occupancy Ag Ag Uani 0.282(6) 0.5577(4) 0.5299(12) 0.042(4) 4 1 Ce Ce Uani 0.28671(18) 0.6106(2) 0.5411(2) 0.015(2) 4 1 P P Uani 0.3732(3) 0.1072(2) 0.4367(2) 0.0137(18) 4 1 Se1 Se Uani 0.12048(14) -0.01825(12) 0.37571(13) 0.0201(15) 4 1 Se2 Se Uani 0.60461(13) 0.30711(14) 0.67695(12) 0.0198(9) 4 1 Se3 Se Uani 0.21244(14) 0.21199(12) 0.1695(11) 0.0191(11) 4 1 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 Ag Ag 0.0407(14) 0.051(2) 0.032(2) 0.0025(14) 0.0293(17) -0.0083(19) Ce Ce 0.0179(6) 0.018(12) 0.0161(11) -0.0002(6) 0.0156(8) 0.0021(8) P P 0.0129(8) 0.016(11) 0.0122(8) 0.0011(7) 0.0104(7) 0.0009(7) Se1 Se 0.0223(6) 0.0211(8) 0.0238(6) 0.0007(4) 0.0203(6) 0.0031(4) Se2 Se 0.0166(3) 0.0171(5) 0.0164(4) -0.0011(4) 0.0118(3) -0.0036(4) Se3 Se 0.0185(5) 0.0227(5) 0.0141(4) -0.0005(4) 0.013(5) 0.0019(4) 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 0.312 0 0.412 2 0.624 0 0.824 3 0.936 0 1.236 loop_ _atom_site_occ_Fourier_id _atom_site_occ_Fourier_atom_site_label _atom_site_occ_Fourier_wave_vector_seq_id Ago1 Ag 1 Ceo1 Ce 1 loop_ _atom_site_occ_Fourier_param_id _atom_site_occ_Fourier_param_cos _atom_site_occ_Fourier_param_sin Ago1 0 0.5238(18) Ceo1 0 1.0299(19) 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 Agx1 Ag x 1 Agy1 Ag y 1 Agz1 Ag z 1 Agx2 Ag x 2 Agy2 Ag y 2 Agz2 Ag z 2 Cex1 Ce x 1 Cey1 Ce y 1 Cez1 Ce z 1 Cex2 Ce x 2 Cey2 Ce y 2 Cez2 Ce z 2 Px1 P x 1 Py1 P y 1 Pz1 P z 1 Px2 P x 2 Py2 P y 2 Pz2 P z 2 Se1x1 Se1 x 1 Se1y1 Se1 y 1 Se1z1 Se1 z 1 Se1x2 Se1 x 2 Se1y2 Se1 y 2 Se1z2 Se1 z 2 Se1x3 Se1 x 3 Se1y3 Se1 y 3 Se1z3 Se1 z 3 Se2x1 Se2 x 1 Se2y1 Se2 y 1 Se2z1 Se2 z 1 Se2x2 Se2 x 2 Se2y2 Se2 y 2 Se2z2 Se2 z 2 Se2x3 Se2 x 3 Se2y3 Se2 y 3 Se2z3 Se2 z 3 Se3x1 Se3 x 1 Se3y1 Se3 y 1 Se3z1 Se3 z 1 Se3x2 Se3 x 2 Se3y2 Se3 y 2 Se3z2 Se3 z 2 Se3x3 Se3 x 3 Se3y3 Se3 y 3 Se3z3 Se3 z 3 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Agx1 -0.0108(11) 0.0114(6) Agy1 0.0154(6) -0.0321(5) Agz1 -0.041(2) 0.0335(11) Agx2 0.0151(15) 0.0028(8) Agy2 0.0123(11) -0.012(7) Agz2 0.0277(15) 0.0215(9) Cex1 0.0008(4) 0.0173(2) Cey1 -0.0028(3) -0.017(3) Cez1 0.0018(4) 0.0195(2) Cex2 -0.0044(12) -0.0011(8) Cey2 0.0076(10) 0.0024(6) Cez2 -0.0112(9) -0.0013(7) Px1 -0.005(4) -0.003(4) Py1 -0.0111(4) -0.0273(4) Pz1 -0.0082(3) 0.0054(3) Px2 0.0072(11) 0.0051(10) Py2 0.0034(7) 0.0003(7) Pz2 0(9) -0.0007(9) Se1x1 -0.0347(2) 0.0053(2) Se1y1 -0.01278(18) -0.0279(2) Se1z1 -0.0324(2) 0.0091(2) Se1x2 0.0194(5) -0.0075(6) Se1y2 -0.0052(3) -0.0053(4) Se1z2 0.0142(4) -0.0042(5) Se1x3 -0.0064(10) 0.0036(11) Se1y3 0.009(7) 0.0085(6) Se1z3 -0.0071(9) 0.0016(10) Se2x1 0.0029(2) -0.0051(2) Se2y1 0.0293(2) -0.0278(2) Se2z1 -0.01662(18) 0.0017(19) Se2x2 -0.0042(5) 0.005(5) Se2y2 -0.008(3) 0.0053(4) Se2z2 0.0057(4) -0.0026(5) Se2x3 -0.0014(10) 0.0029(11) Se2y3 0.0125(6) 0.004(6) Se2z3 -0.0062(8) 0.0003(9) Se3x1 0.0137(2) -0.0296(2) Se3y1 -0.0255(17) 0.00004(18) Se3z1 0.00727(17) -0.00399(17) Se3x2 -0.0009(6) -0.0018(5) Se3y2 0.0026(4) 0.0009(3) Se3z2 -0.0004(5) 0.0022(4) Se3x3 -0.0055(11) -0.0124(10) Se3y3 0.0068(6) 0.0019(7) Se3z3 -0.005(11) -0.0034(10) 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 AgU111 Ag U11 1 AgU221 Ag U22 1 AgU331 Ag U33 1 AgU121 Ag U12 1 AgU131 Ag U13 1 AgU231 Ag U23 1 CeU111 Ce U11 1 CeU221 Ce U22 1 CeU331 Ce U33 1 CeU121 Ce U12 1 CeU131 Ce U13 1 CeU231 Ce U23 1 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 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin AgU111 0(2) -0.0014(16) AgU221 -0.016(17) -0.005(2) AgU331 0.001(3) -0.009(2) AgU121 -0.0106(13) 0.0123(14) AgU131 0.005(2) -0.004(2) AgU231 -0.0064(18) 0.016(2) CeU111 0.0011(9) 0.0019(6) CeU221 0.0049(12) -0.0015(12) CeU331 0.008(10) -0.0048(9) CeU121 -0.0059(7) 0.0027(6) CeU131 0.0035(9) -0.0011(7) CeU231 -0.0099(8) 0.0055(8) Se1U111 -0.0104(11) 0.0024(9) Se1U221 0.0001(8) -0.0014(11) Se1U331 -0.0064(11) 0.0005(8) Se1U121 0.0015(7) 0.0079(8) Se1U131 -0.0089(11) 0.0014(8) Se1U231 0.0027(7) 0.0069(8) Se2U111 -0.0002(6) -0.0004(6) Se2U221 -0.0016(11) 0.0042(9) Se2U331 0.0017(7) 0.0009(6) Se2U121 -0.0026(7) 0.0019(6) Se2U131 0.0021(5) -0.0015(5) Se2U231 0.0001(8) -0.0025(6) Se3U111 0.0043(9) 0.0015(6) Se3U221 -0.0048(8) -0.0022(9) Se3U331 0.0017(6) 0.0025(6) Se3U121 0.0001(6) 0.0004(6) Se3U131 0.0029(7) 0.0024(6) Se3U231 -0.0007(5) -0.0015(6) #======================================================================= data_NaCeP2Se6 #======================================================================= _audit_creation_method SHELXL-97 _chemical_formula_sum 'Ce Na P2 Se6' _chemical_formula_weight 698.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Na' 'Na' 0.0362 0.0249 '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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 '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 'P 21/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 12.1422(2) _cell_length_b 7.69820(10) _cell_length_c 11.7399(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.5450(10) _cell_angle_gamma 90.00 _cell_volume 1020.69(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4391 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 26.99 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_absorpt_coefficient_mu 26.138 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.439830 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_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 'Bruker SMART CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5342 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2083 _reflns_number_gt 1863 _reflns_threshold_expression >2s(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'ORTEP and Crystal-maker' _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^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2083 _refine_ls_number_parameters 91 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.002 _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 Ce1 Ce 0.34312(3) 0.10588(5) 0.58852(4) 0.00420(14) Uani 1 1 d . . . Se1 Se 0.08634(6) 0.00172(9) 0.34318(7) 0.00733(18) Uani 1 1 d . . . Se2 Se 0.11320(6) 0.20147(9) 0.05944(7) 0.00601(18) Uani 1 1 d . . . Se3 Se 0.79687(6) 0.20738(9) 0.37312(7) 0.00650(18) Uani 1 1 d . . . Se4 Se 0.31010(6) 0.17940(9) 0.85407(6) 0.00567(18) Uani 1 1 d . . . Se5 Se 0.44848(6) 0.02568(9) 0.18201(7) 0.00556(18) Uani 1 1 d . . . Se6 Se 0.59375(6) 0.19512(9) 0.56352(6) 0.00493(18) Uani 1 1 d . . . P1 P 0.19343(16) 0.1123(2) 0.24898(17) 0.0039(4) Uani 1 1 d . . . P2 P 0.68140(16) 0.0991(2) 0.75217(17) 0.0034(4) Uani 1 1 d . . . Na1 Na 0.8598(3) 0.1071(4) 0.1233(3) 0.0124(7) 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 Ce1 0.0023(2) 0.0046(2) 0.0056(2) 0.00012(15) 0.00128(17) 0.00032(14) Se1 0.0063(4) 0.0081(4) 0.0096(4) 0.0012(3) 0.0054(3) 0.0001(3) Se2 0.0023(4) 0.0084(4) 0.0054(4) 0.0016(3) -0.0008(3) 0.0000(3) Se3 0.0025(4) 0.0063(4) 0.0087(4) 0.0027(3) -0.0003(3) -0.0002(2) Se4 0.0039(4) 0.0060(4) 0.0057(4) 0.0001(3) 0.0002(3) 0.0012(3) Se5 0.0022(4) 0.0075(4) 0.0074(4) 0.0017(3) 0.0022(3) 0.0011(3) Se6 0.0031(4) 0.0063(4) 0.0042(4) 0.0007(3) -0.0001(3) 0.0011(2) P1 0.0016(9) 0.0047(9) 0.0039(9) 0.0004(7) -0.0006(7) 0.0003(7) P2 0.0015(9) 0.0043(9) 0.0041(9) 0.0009(7) 0.0008(7) 0.0009(6) Na1 0.0069(15) 0.0117(16) 0.0156(16) 0.0012(13) 0.0006(13) -0.0012(12) _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 Ce1 Se2 3.0674(8) 4_566 ? Ce1 Se3 3.0773(8) 3_656 ? Ce1 Se4 3.1078(8) 4_565 ? Ce1 Se5 3.1112(8) 3_656 ? Ce1 Se5 3.1393(8) 4_566 ? Ce1 Se6 3.1855(8) 3_656 ? Ce1 Se6 3.2365(8) . ? Ce1 Se4 3.3344(8) . ? Ce1 Se1 3.4733(9) . ? Se1 P1 2.1668(19) . ? Se1 Na1 3.102(3) 2_645 ? Se1 Na1 3.110(3) 1_455 ? Se2 P1 2.186(2) . ? Se2 Ce1 3.0675(8) 4_565 ? Se2 Na1 3.297(3) 3_655 ? Se2 Na1 3.501(3) 1_455 ? Se3 P2 2.177(2) 4_565 ? Se3 Ce1 3.0773(8) 3_656 ? Se3 Na1 3.099(3) 4_566 ? Se3 Na1 3.380(3) . ? Se4 P1 2.194(2) 4_566 ? Se4 Na1 3.097(3) 3_656 ? Se4 Ce1 3.1078(8) 4_566 ? Se5 P2 2.2140(19) 3_656 ? Se5 Ce1 3.1113(8) 3_656 ? Se5 Ce1 3.1392(8) 4_565 ? Se6 P2 2.203(2) . ? Se6 Ce1 3.1855(8) 3_656 ? Se6 Na1 3.403(3) 4_566 ? P1 Se4 2.195(2) 4_565 ? P1 P2 2.230(3) 3_656 ? P2 Se3 2.177(2) 4_566 ? P2 Se5 2.2140(19) 3_656 ? P2 P1 2.230(3) 3_656 ? Na1 Se4 3.097(3) 3_656 ? Na1 Se3 3.099(3) 4_565 ? Na1 Se1 3.102(3) 2_655 ? Na1 Se1 3.110(3) 1_655 ? Na1 Se2 3.297(3) 3_655 ? Na1 Se6 3.403(3) 4_565 ? Na1 Se2 3.501(3) 1_655 ? 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 Se2 Ce1 Se3 82.31(2) 4_566 3_656 ? Se2 Ce1 Se4 80.10(2) 4_566 4_565 ? Se3 Ce1 Se4 130.38(2) 3_656 4_565 ? Se2 Ce1 Se5 132.17(2) 4_566 3_656 ? Se3 Ce1 Se5 86.30(2) 3_656 3_656 ? Se4 Ce1 Se5 137.68(2) 4_565 3_656 ? Se2 Ce1 Se5 80.76(2) 4_566 4_566 ? Se3 Ce1 Se5 146.40(2) 3_656 4_566 ? Se4 Ce1 Se5 74.49(2) 4_565 4_566 ? Se5 Ce1 Se5 83.910(14) 3_656 4_566 ? Se2 Ce1 Se6 133.30(2) 4_566 3_656 ? Se3 Ce1 Se6 76.79(2) 3_656 3_656 ? Se4 Ce1 Se6 82.53(2) 4_565 3_656 ? Se5 Ce1 Se6 87.81(2) 3_656 3_656 ? Se5 Ce1 Se6 134.59(2) 4_566 3_656 ? Se2 Ce1 Se6 137.30(2) 4_566 . ? Se3 Ce1 Se6 140.17(2) 3_656 . ? Se4 Ce1 Se6 68.07(2) 4_565 . ? Se5 Ce1 Se6 69.80(2) 3_656 . ? Se5 Ce1 Se6 64.145(19) 4_566 . ? Se6 Ce1 Se6 71.08(2) 3_656 . ? Se2 Ce1 Se4 66.74(2) 4_566 . ? Se3 Ce1 Se4 74.55(2) 3_656 . ? Se4 Ce1 Se4 135.814(16) 4_565 . ? Se5 Ce1 Se4 65.449(19) 3_656 . ? Se5 Ce1 Se4 72.134(19) 4_566 . ? Se6 Ce1 Se4 141.60(2) 3_656 . ? Se6 Ce1 Se4 119.25(2) . . ? Se2 Ce1 Se1 61.067(19) 4_566 . ? Se3 Ce1 Se1 64.19(2) 3_656 . ? Se4 Ce1 Se1 66.661(19) 4_565 . ? Se5 Ce1 Se1 147.13(2) 3_656 . ? Se5 Ce1 Se1 128.68(2) 4_566 . ? Se6 Ce1 Se1 72.236(19) 3_656 . ? Se6 Ce1 Se1 124.15(2) . . ? Se4 Ce1 Se1 115.78(2) . . ? P1 Se1 Na1 108.14(8) . 2_645 ? P1 Se1 Na1 89.29(8) . 1_455 ? Na1 Se1 Na1 116.22(8) 2_645 1_455 ? P1 Se1 Ce1 78.95(5) . . ? Na1 Se1 Ce1 92.16(6) 2_645 . ? Na1 Se1 Ce1 151.53(6) 1_455 . ? P1 Se2 Ce1 89.50(5) . 4_565 ? P1 Se2 Na1 108.82(8) . 3_655 ? Ce1 Se2 Na1 96.70(6) 4_565 3_655 ? P1 Se2 Na1 79.34(7) . 1_455 ? Ce1 Se2 Na1 155.81(6) 4_565 1_455 ? Na1 Se2 Na1 107.18(7) 3_655 1_455 ? P2 Se3 Ce1 111.94(5) 4_565 3_656 ? P2 Se3 Na1 100.27(8) 4_565 4_566 ? Ce1 Se3 Na1 100.34(6) 3_656 4_566 ? P2 Se3 Na1 83.51(7) 4_565 . ? Ce1 Se3 Na1 105.13(6) 3_656 . ? Na1 Se3 Na1 150.71(10) 4_566 . ? P1 Se4 Na1 104.82(8) 4_566 3_656 ? P1 Se4 Ce1 87.48(5) 4_566 4_566 ? Na1 Se4 Ce1 100.15(6) 3_656 4_566 ? P1 Se4 Ce1 82.69(5) 4_566 . ? Na1 Se4 Ce1 105.77(6) 3_656 . ? Ce1 Se4 Ce1 153.85(3) 4_566 . ? P2 Se5 Ce1 90.78(5) 3_656 3_656 ? P2 Se5 Ce1 105.25(5) 3_656 4_565 ? Ce1 Se5 Ce1 133.97(3) 3_656 4_565 ? P2 Se6 Ce1 101.09(5) . 3_656 ? P2 Se6 Ce1 87.76(5) . . ? Ce1 Se6 Ce1 108.92(2) 3_656 . ? P2 Se6 Na1 82.60(8) . 4_566 ? Ce1 Se6 Na1 92.04(5) 3_656 4_566 ? Ce1 Se6 Na1 158.31(6) . 4_566 ? Se1 P1 Se2 121.08(9) . . ? Se1 P1 Se4 112.62(8) . 4_565 ? Se2 P1 Se4 107.29(8) . 4_565 ? Se1 P1 P2 104.73(9) . 3_656 ? Se2 P1 P2 105.83(9) . 3_656 ? Se4 P1 P2 103.65(9) 4_565 3_656 ? Se3 P2 Se6 112.57(8) 4_566 . ? Se3 P2 Se5 116.10(8) 4_566 3_656 ? Se6 P2 Se5 110.69(8) . 3_656 ? Se3 P2 P1 103.08(9) 4_566 3_656 ? Se6 P2 P1 108.51(9) . 3_656 ? Se5 P2 P1 105.05(9) 3_656 3_656 ? Se4 Na1 Se3 118.00(10) 3_656 4_565 ? Se4 Na1 Se1 143.39(11) 3_656 2_655 ? Se3 Na1 Se1 68.65(7) 4_565 2_655 ? Se4 Na1 Se1 99.04(9) 3_656 1_655 ? Se3 Na1 Se1 137.88(11) 4_565 1_655 ? Se1 Na1 Se1 93.96(9) 2_655 1_655 ? Se4 Na1 Se2 76.78(7) 3_656 3_655 ? Se3 Na1 Se2 76.35(8) 4_565 3_655 ? Se1 Na1 Se2 136.16(11) 2_655 3_655 ? Se1 Na1 Se2 94.76(8) 1_655 3_655 ? Se4 Na1 Se3 73.65(7) 3_656 . ? Se3 Na1 Se3 131.42(10) 4_565 . ? Se1 Na1 Se3 76.74(7) 2_655 . ? Se1 Na1 Se3 75.66(7) 1_655 . ? Se2 Na1 Se3 146.86(10) 3_655 . ? Se4 Na1 Se6 74.02(7) 3_656 4_565 ? Se3 Na1 Se6 73.35(7) 4_565 4_565 ? Se1 Na1 Se6 74.22(7) 2_655 4_565 ? Se1 Na1 Se6 140.47(11) 1_655 4_565 ? Se2 Na1 Se6 120.13(10) 3_655 4_565 ? Se3 Na1 Se6 64.98(6) . 4_565 ? Se4 Na1 Se2 146.27(10) 3_656 1_655 ? Se3 Na1 Se2 68.36(6) 4_565 1_655 ? Se1 Na1 Se2 70.29(6) 2_655 1_655 ? Se1 Na1 Se2 69.68(6) 1_655 1_655 ? Se2 Na1 Se2 72.83(7) 3_655 1_655 ? Se3 Na1 Se2 129.42(10) . 1_655 ? Se6 Na1 Se2 134.86(9) 4_565 1_655 ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 2.039 _refine_diff_density_min -2.913 _refine_diff_density_rms 0.433 #===END #======================================================================= data_Cu0-4Ce1-2P2Se6 #======================================================================= _audit_creation_method SHELXL-97 _chemical_formula_sum 'Ce1.20 Cu0.40 P2 Se6' _chemical_formula_weight 729.26 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' 'Cu' 'Cu' 0.3201 1.2651 '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' 'Ce' 'Ce' -0.2486 2.6331 '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 'P 21/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 12.0409(14) _cell_length_b 7.6418(8) _cell_length_c 11.6999(13) _cell_angle_alpha 90.00 _cell_angle_beta 111.269(2) _cell_angle_gamma 90.00 _cell_volume 1003.23(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1566 _cell_measurement_theta_min 3.23 _cell_measurement_theta_max 27.12 _exptl_crystal_description yellow _exptl_crystal_colour plate _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1261 _exptl_absorpt_coefficient_mu 28.258 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.694397 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_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 'Bruker SMART CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5033 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_unetI/netI 0.0658 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.12 _reflns_number_total 2150 _reflns_number_gt 1586 _reflns_threshold_expression >2\s(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'ORTEP and crystal-maker' _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^)+(0.0530P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2150 _refine_ls_number_parameters 102 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _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_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ce1 Ce 0.34521(6) 0.10723(8) 0.59066(5) 0.01718(18) Uani 1 1 d . . . Se1 Se 0.07631(11) -0.00855(14) 0.33234(10) 0.0211(3) Uani 1 1 d . . . Se2 Se 0.11195(11) 0.20214(15) 0.05700(9) 0.0198(3) Uani 1 1 d . . . Se3 Se 0.79822(11) 0.20691(15) 0.37616(10) 0.0244(3) Uani 1 1 d . . . Se4 Se 0.30382(11) 0.17902(14) 0.85441(9) 0.0181(3) Uani 1 1 d . . . Se5 Se 0.44748(10) 0.02295(14) 0.18031(9) 0.0162(3) Uani 1 1 d . . . Se6 Se 0.59711(10) 0.19570(13) 0.56492(9) 0.0158(3) Uani 1 1 d . . . P1 P 0.1898(2) 0.1141(3) 0.2457(2) 0.0125(6) Uani 1 1 d . . . P2 P 0.6834(3) 0.0995(3) 0.7531(2) 0.0118(5) Uani 1 1 d . . . Ce2 Ce 0.8563(3) 0.1145(5) 0.1148(3) 0.0285(10) Uani 0.1984(17) 1 d P . . Cu1 Cu 0.9350(4) 0.2224(5) 0.2860(4) 0.0382(15) Uani 0.405(5) 1 d P . . 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 Ce1 0.0211(4) 0.0151(3) 0.0180(3) 0.0004(2) 0.0103(3) 0.0003(3) Se1 0.0260(7) 0.0193(6) 0.0253(6) 0.0046(4) 0.0179(5) 0.0031(5) Se2 0.0197(7) 0.0227(6) 0.0128(5) 0.0034(4) 0.0011(4) 0.0002(5) Se3 0.0188(7) 0.0188(6) 0.0297(6) 0.0122(5) 0.0016(5) -0.0023(5) Se4 0.0235(7) 0.0153(5) 0.0153(5) 0.0021(4) 0.0069(5) 0.0044(5) Se5 0.0142(6) 0.0181(5) 0.0186(5) 0.0047(4) 0.0088(5) 0.0029(5) Se6 0.0197(7) 0.0148(5) 0.0117(5) 0.0015(4) 0.0044(4) 0.0028(5) P1 0.0123(15) 0.0139(13) 0.0116(11) 0.0002(10) 0.0048(11) 0.0022(11) P2 0.0136(15) 0.0107(12) 0.0120(11) 0.0016(10) 0.0056(11) 0.0027(11) Ce2 0.027(2) 0.029(2) 0.0307(19) -0.0004(15) 0.0117(16) 0.0004(16) Cu1 0.044(3) 0.028(2) 0.055(3) 0.0121(19) 0.033(2) 0.0117(19) _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 Ce1 Se2 3.0599(14) 4_566 ? Ce1 Se3 3.0631(13) 3_656 ? Ce1 Se5 3.0900(13) 3_656 ? Ce1 Se4 3.0916(12) 4_565 ? Ce1 Se5 3.1091(12) 4_566 ? Ce1 Se6 3.1736(12) 3_656 ? Ce1 Se6 3.2265(14) . ? Ce1 Se4 3.3448(12) . ? Ce1 Se1 3.6471(14) . ? Se1 P1 2.186(3) . ? Se1 Cu1 2.374(4) 1_455 ? Se1 Cu1 2.455(4) 2_645 ? Se1 Ce2 2.996(4) 2_645 ? Se1 Ce2 3.080(4) 1_455 ? Se2 P1 2.169(3) . ? Se2 Ce1 3.0600(14) 4_565 ? Se2 Ce2 3.255(4) 3_655 ? Se2 Ce2 3.448(4) 1_455 ? Se3 P2 2.175(3) 4_565 ? Se3 Cu1 2.258(4) . ? Se3 Ce2 2.955(4) 4_566 ? Se3 Ce1 3.0631(13) 3_656 ? Se3 Ce2 3.448(4) . ? Se4 P1 2.176(3) 4_566 ? Se4 Ce2 3.063(4) 3_656 ? Se4 Ce1 3.0915(12) 4_566 ? Se5 P2 2.204(3) 3_656 ? Se5 Ce1 3.0900(13) 3_656 ? Se5 Ce1 3.1091(12) 4_565 ? Se6 P2 2.193(3) . ? Se6 Ce1 3.1736(12) 3_656 ? Se6 Ce2 3.296(4) 4_566 ? P1 Se4 2.176(3) 4_565 ? P1 P2 2.231(4) 3_656 ? P2 Se3 2.175(3) 4_566 ? P2 Se5 2.204(3) 3_656 ? P2 P1 2.231(4) 3_656 ? Ce2 Cu1 2.052(6) . ? Ce2 Se3 2.955(4) 4_565 ? Ce2 Se1 2.996(4) 2_655 ? Ce2 Se4 3.063(4) 3_656 ? Ce2 Se1 3.080(4) 1_655 ? Ce2 Se2 3.255(4) 3_655 ? Ce2 Se6 3.296(4) 4_565 ? Ce2 Se2 3.448(4) 1_655 ? Cu1 Se1 2.374(4) 1_655 ? Cu1 Se1 2.455(4) 2_655 ? 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 Se2 Ce1 Se3 81.72(4) 4_566 3_656 ? Se2 Ce1 Se5 132.84(3) 4_566 3_656 ? Se3 Ce1 Se5 87.31(3) 3_656 3_656 ? Se2 Ce1 Se4 77.91(3) 4_566 4_565 ? Se3 Ce1 Se4 127.73(4) 3_656 4_565 ? Se5 Ce1 Se4 139.72(4) 3_656 4_565 ? Se2 Ce1 Se5 80.99(3) 4_566 4_566 ? Se3 Ce1 Se5 147.37(4) 3_656 4_566 ? Se5 Ce1 Se5 84.47(2) 3_656 4_566 ? Se4 Ce1 Se5 74.75(3) 4_565 4_566 ? Se2 Ce1 Se6 130.92(3) 4_566 3_656 ? Se3 Ce1 Se6 75.63(3) 3_656 3_656 ? Se5 Ce1 Se6 89.23(3) 3_656 3_656 ? Se4 Ce1 Se6 82.55(3) 4_565 3_656 ? Se5 Ce1 Se6 135.58(4) 4_566 3_656 ? Se2 Ce1 Se6 137.58(3) 4_566 . ? Se3 Ce1 Se6 140.21(4) 3_656 . ? Se5 Ce1 Se6 69.96(3) 3_656 . ? Se4 Ce1 Se6 70.00(3) 4_565 . ? Se5 Ce1 Se6 64.55(3) 4_566 . ? Se6 Ce1 Se6 71.98(3) 3_656 . ? Se2 Ce1 Se4 66.65(3) 4_566 . ? Se3 Ce1 Se4 74.46(3) 3_656 . ? Se5 Ce1 Se4 66.21(3) 3_656 . ? Se4 Ce1 Se4 135.12(3) 4_565 . ? Se5 Ce1 Se4 73.32(3) 4_566 . ? Se6 Ce1 Se4 141.78(3) 3_656 . ? Se6 Ce1 Se4 120.76(3) . . ? Se2 Ce1 Se1 60.75(3) 4_566 . ? Se3 Ce1 Se1 62.81(3) 3_656 . ? Se5 Ce1 Se1 146.68(3) 3_656 . ? Se4 Ce1 Se1 65.20(3) 4_565 . ? Se5 Ce1 Se1 128.61(3) 4_566 . ? Se6 Ce1 Se1 70.18(3) 3_656 . ? Se6 Ce1 Se1 123.75(3) . . ? Se4 Ce1 Se1 114.82(3) . . ? P1 Se1 Cu1 95.30(12) . 1_455 ? P1 Se1 Cu1 90.78(12) . 2_645 ? Cu1 Se1 Cu1 127.26(7) 1_455 2_645 ? P1 Se1 Ce2 109.87(11) . 2_645 ? Cu1 Se1 Ce2 151.65(14) 1_455 2_645 ? Cu1 Se1 Ce2 42.82(12) 2_645 2_645 ? P1 Se1 Ce2 88.91(10) . 1_455 ? Cu1 Se1 Ce2 41.75(13) 1_455 1_455 ? Cu1 Se1 Ce2 86.25(13) 2_645 1_455 ? Ce2 Se1 Ce2 123.46(10) 2_645 1_455 ? P1 Se1 Ce1 76.34(8) . . ? Cu1 Se1 Ce1 110.88(12) 1_455 . ? Cu1 Se1 Ce1 121.43(12) 2_645 . ? Ce2 Se1 Ce1 88.26(8) 2_645 . ? Ce2 Se1 Ce1 148.17(8) 1_455 . ? P1 Se2 Ce1 88.79(8) . 4_565 ? P1 Se2 Ce2 107.07(10) . 3_655 ? Ce1 Se2 Ce2 97.21(8) 4_565 3_655 ? P1 Se2 Ce2 80.05(10) . 1_455 ? Ce1 Se2 Ce2 155.53(7) 4_565 1_455 ? Ce2 Se2 Ce2 106.84(8) 3_655 1_455 ? P2 Se3 Cu1 92.95(13) 4_565 . ? P2 Se3 Ce2 100.79(10) 4_565 4_566 ? Cu1 Se3 Ce2 117.03(15) . 4_566 ? P2 Se3 Ce1 111.39(9) 4_565 3_656 ? Cu1 Se3 Ce1 129.83(11) . 3_656 ? Ce2 Se3 Ce1 101.15(8) 4_566 3_656 ? P2 Se3 Ce2 80.62(9) 4_565 . ? Cu1 Se3 Ce2 34.86(13) . . ? Ce2 Se3 Ce2 151.39(12) 4_566 . ? Ce1 Se3 Ce2 104.89(7) 3_656 . ? P1 Se4 Ce2 108.08(11) 4_566 3_656 ? P1 Se4 Ce1 90.09(7) 4_566 4_566 ? Ce2 Se4 Ce1 100.71(7) 3_656 4_566 ? P1 Se4 Ce1 81.57(7) 4_566 . ? Ce2 Se4 Ce1 107.41(7) 3_656 . ? Ce1 Se4 Ce1 151.87(4) 4_566 . ? P2 Se5 Ce1 90.74(8) 3_656 3_656 ? P2 Se5 Ce1 105.00(8) 3_656 4_565 ? Ce1 Se5 Ce1 132.98(4) 3_656 4_565 ? P2 Se6 Ce1 102.06(8) . 3_656 ? P2 Se6 Ce1 87.42(8) . . ? Ce1 Se6 Ce1 108.02(3) 3_656 . ? P2 Se6 Ce2 84.06(10) . 4_566 ? Ce1 Se6 Ce2 91.85(7) 3_656 4_566 ? Ce1 Se6 Ce2 159.64(7) . 4_566 ? Se2 P1 Se4 108.52(12) . 4_565 ? Se2 P1 Se1 119.52(13) . . ? Se4 P1 Se1 114.10(11) 4_565 . ? Se2 P1 P2 106.00(12) . 3_656 ? Se4 P1 P2 104.05(14) 4_565 3_656 ? Se1 P1 P2 103.01(13) . 3_656 ? Se3 P2 Se6 113.12(12) 4_566 . ? Se3 P2 Se5 114.79(11) 4_566 3_656 ? Se6 P2 Se5 111.00(13) . 3_656 ? Se3 P2 P1 102.95(14) 4_566 3_656 ? Se6 P2 P1 108.98(13) . 3_656 ? Se5 P2 P1 105.21(13) 3_656 3_656 ? Cu1 Ce2 Se3 127.14(19) . 4_565 ? Cu1 Ce2 Se1 54.38(14) . 2_655 ? Se3 Ce2 Se1 72.81(9) 4_565 2_655 ? Cu1 Ce2 Se4 105.47(17) . 3_656 ? Se3 Ce2 Se4 120.40(13) 4_565 3_656 ? Se1 Ce2 Se4 144.55(13) 2_655 3_656 ? Cu1 Ce2 Se1 50.37(14) . 1_655 ? Se3 Ce2 Se1 139.44(14) 4_565 1_655 ? Se1 Ce2 Se1 92.04(10) 2_655 1_655 ? Se4 Ce2 Se1 93.94(10) 3_656 1_655 ? Cu1 Ce2 Se2 141.7(2) . 3_655 ? Se3 Ce2 Se2 78.49(8) 4_565 3_655 ? Se1 Ce2 Se2 139.34(13) 2_655 3_655 ? Se4 Ce2 Se2 75.42(8) 3_656 3_655 ? Se1 Ce2 Se2 91.43(10) 1_655 3_655 ? Cu1 Ce2 Se6 93.90(17) . 4_565 ? Se3 Ce2 Se6 75.23(9) 4_565 4_565 ? Se1 Ce2 Se6 77.38(9) 2_655 4_565 ? Se4 Ce2 Se6 75.34(9) 3_656 4_565 ? Se1 Ce2 Se6 139.10(12) 1_655 4_565 ? Se2 Ce2 Se6 122.24(12) 3_655 4_565 ? Cu1 Ce2 Se2 89.11(17) . 1_655 ? Se3 Ce2 Se2 69.34(8) 4_565 1_655 ? Se1 Ce2 Se2 70.10(8) 2_655 1_655 ? Se4 Ce2 Se2 144.11(12) 3_656 1_655 ? Se1 Ce2 Se2 70.13(8) 1_655 1_655 ? Se2 Ce2 Se2 73.16(8) 3_655 1_655 ? Se6 Ce2 Se2 137.31(11) 4_565 1_655 ? Cu1 Ce2 Se3 38.97(14) . . ? Se3 Ce2 Se3 133.52(12) 4_565 . ? Se1 Ce2 Se3 75.33(8) 2_655 . ? Se4 Ce2 Se3 72.95(8) 3_656 . ? Se1 Ce2 Se3 73.74(8) 1_655 . ? Se2 Ce2 Se3 143.78(12) 3_655 . ? Se6 Ce2 Se3 65.37(7) 4_565 . ? Se2 Ce2 Se3 128.08(11) 1_655 . ? Ce2 Cu1 Se3 106.2(2) . . ? Ce2 Cu1 Se1 87.89(18) . 1_655 ? Se3 Cu1 Se1 115.99(16) . 1_655 ? Ce2 Cu1 Se1 82.80(17) . 2_655 ? Se3 Cu1 Se1 114.00(16) . 2_655 ? Se1 Cu1 Se1 129.80(18) 1_655 2_655 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.160 _refine_diff_density_min -1.675 _refine_diff_density_rms 0.399 #===END #======================================================================= data_Ce1-33P2Se6 #======================================================================= _audit_creation_method SHELXL-97 _chemical_formula_sum 'Ce1.33 P2 Se6' _chemical_formula_weight 722.06 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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ce' 'Ce' -0.2486 2.6331 '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 'P 21/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 6.8057(5) _cell_length_b 22.9685(15) _cell_length_c 11.7226(8) _cell_angle_alpha 90.00 _cell_angle_beta 124.0960(10) _cell_angle_gamma 90.00 _cell_volume 1517.44(18) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3195 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 27.01 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1867 _exptl_absorpt_coefficient_mu 27.774 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.335814 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_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 'Bruker SMART CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8751 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_unetI/netI 0.0917 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.01 _reflns_number_total 3285 _reflns_number_gt 1822 _reflns_threshold_expression >2\s(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'ORTEP and Crystal-maker' _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^)+(0.0609P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3285 _refine_ls_number_parameters 139 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1474 _refine_ls_wR_factor_gt 0.1350 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.912 _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 Ce1 Ce 0.7935(6) 0.13020(17) 0.7496(3) 0.0525(12) Uani 0.345(3) 1 d P . . Ce2 Ce 0.1996(2) 0.20631(4) 0.24594(11) 0.0181(3) Uani 0.778(2) 1 d P . . Ce3 Ce 0.78861(17) 0.03602(3) 0.25224(9) 0.0133(3) Uani 0.875(3) 1 d P . . Se1 Se 0.2935(2) 0.06602(6) 0.96022(14) 0.0152(3) Uani 1 1 d . . . Se2 Se 0.0964(3) 0.22883(6) 0.93713(14) 0.0183(4) Uani 1 1 d . . . Se3 Se 0.8909(2) 0.06417(6) 0.55389(14) 0.0156(3) Uani 1 1 d . . . Se4 Se 0.2708(3) 0.10024(6) 0.44563(14) 0.0173(3) Uani 1 1 d . . . Se5 Se 0.7059(3) 0.23254(6) 0.53932(14) 0.0179(4) Uani 1 1 d . . . Se6 Se 0.6184(3) 0.16312(6) 0.23134(13) 0.0165(3) Uani 1 1 d . . . Se7 Se 0.3834(3) 0.17049(6) 0.76306(14) 0.0185(4) Uani 1 1 d . . . Se8 Se 0.8931(2) 0.10216(6) 0.06052(14) 0.0150(3) Uani 1 1 d . . . Se9 Se 0.6245(3) 0.00539(6) 0.73349(14) 0.0179(3) Uani 1 1 d . . . P1 P 0.1262(6) 0.13190(16) 0.5622(3) 0.0117(7) Uani 1 1 d . . . P2 P 0.1273(6) 0.03520(14) 0.0652(3) 0.0101(7) Uani 1 1 d . . . P3 P 0.8719(7) 0.20279(14) 0.4352(4) 0.0120(8) 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 Ce1 0.041(2) 0.063(2) 0.046(2) -0.0061(18) 0.0197(17) 0.0036(19) Ce2 0.0216(7) 0.0151(6) 0.0197(6) -0.0004(4) 0.0128(5) -0.0001(4) Ce3 0.0148(6) 0.0099(4) 0.0154(5) -0.0011(4) 0.0085(4) -0.0017(4) Se1 0.0163(8) 0.0148(7) 0.0222(7) -0.0022(5) 0.0154(7) -0.0039(6) Se2 0.0195(9) 0.0153(7) 0.0251(8) 0.0020(6) 0.0155(7) 0.0055(6) Se3 0.0140(8) 0.0135(7) 0.0212(7) 0.0016(5) 0.0111(7) -0.0009(6) Se4 0.0178(9) 0.0162(7) 0.0257(8) -0.0021(6) 0.0169(7) 0.0005(6) Se5 0.0167(9) 0.0204(8) 0.0242(8) -0.0003(6) 0.0162(7) 0.0026(6) Se6 0.0160(8) 0.0148(7) 0.0142(7) -0.0016(5) 0.0059(7) 0.0041(6) Se7 0.0165(9) 0.0167(7) 0.0156(7) -0.0028(5) 0.0048(7) 0.0016(6) Se8 0.0148(8) 0.0115(7) 0.0224(7) -0.0018(5) 0.0126(7) 0.0004(6) Se9 0.0154(8) 0.0209(8) 0.0144(7) 0.0023(6) 0.0066(7) -0.0025(6) P1 0.0108(19) 0.0107(16) 0.0150(16) 0.0004(14) 0.0082(15) -0.0006(15) P2 0.0079(19) 0.0091(16) 0.0137(17) -0.0011(13) 0.0064(16) -0.0033(14) P3 0.010(2) 0.0108(18) 0.0164(18) 0.0010(13) 0.0080(17) 0.0006(13) _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 Ce1 Se2 3.022(4) 1_655 ? Ce1 Se7 3.027(4) . ? Ce1 Se9 3.055(4) . ? Ce1 Se3 3.115(4) . ? Ce1 Se5 3.210(4) . ? Ce1 Se1 3.230(4) 1_655 ? Ce1 Se8 3.375(4) 1_556 ? Ce1 Se4 3.408(4) . ? Ce2 Se7 3.0548(16) 4_565 ? Ce2 Se2 3.0824(16) 4_565 ? Ce2 Se6 3.1118(18) . ? Ce2 Se8 3.1168(17) 1_455 ? Ce2 Se5 3.1631(19) 4_465 ? Ce2 Se4 3.2216(16) . ? Ce2 Se5 3.2829(19) . ? Ce2 Se2 3.3188(17) 1_554 ? Ce3 Se9 3.0603(17) 3_656 ? Ce3 Se6 3.0993(16) . ? Ce3 Se8 3.1076(15) . ? Ce3 Se3 3.1083(16) 3_756 ? Ce3 Se4 3.1213(17) 1_655 ? Ce3 Se1 3.2323(15) 3_656 ? Ce3 Se1 3.2580(17) 1_554 ? Ce3 Se3 3.2631(16) . ? Se1 P2 2.203(3) 1_556 ? Se1 Ce1 3.230(4) 1_455 ? Se1 Ce3 3.2323(15) 3_656 ? Se1 Ce3 3.2580(17) 1_556 ? Se2 P3 2.182(4) 4_466 ? Se2 Ce1 3.022(4) 1_455 ? Se2 Ce2 3.0825(16) 4_566 ? Se2 Ce2 3.3187(17) 1_556 ? Se3 P1 2.195(4) 1_655 ? Se3 Ce3 3.1083(16) 3_756 ? Se4 P1 2.207(3) . ? Se4 Ce3 3.1214(17) 1_455 ? Se5 P3 2.186(4) . ? Se5 Ce2 3.1631(19) 4_666 ? Se6 P3 2.213(4) . ? Se7 P1 2.185(4) . ? Se7 Ce2 3.0547(16) 4_566 ? Se8 P2 2.194(4) 1_655 ? Se8 Ce2 3.1169(17) 1_655 ? Se8 Ce1 3.375(4) 1_554 ? Se9 P2 2.196(4) 3_656 ? Se9 Ce3 3.0603(17) 3_656 ? P1 Se3 2.195(4) 1_455 ? P1 P3 2.230(5) 1_455 ? P2 Se8 2.193(4) 1_455 ? P2 Se9 2.196(4) 3_656 ? P2 Se1 2.203(3) 1_554 ? P2 P2 2.232(7) 3 ? P3 Se2 2.182(4) 4_665 ? P3 P1 2.230(5) 1_655 ? 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 Se2 Ce1 Se7 90.32(10) 1_655 . ? Se2 Ce1 Se9 145.88(13) 1_655 . ? Se7 Ce1 Se9 87.93(10) . . ? Se2 Ce1 Se3 124.11(13) 1_655 . ? Se7 Ce1 Se3 140.36(13) . . ? Se9 Ce1 Se3 74.09(9) . . ? Se2 Ce1 Se5 76.53(10) 1_655 . ? Se7 Ce1 Se5 92.08(10) . . ? Se9 Ce1 Se5 137.58(12) . . ? Se3 Ce1 Se5 79.39(9) . . ? Se2 Ce1 Se1 77.84(9) 1_655 1_655 ? Se7 Ce1 Se1 134.96(12) . 1_655 ? Se9 Ce1 Se1 79.49(9) . 1_655 ? Se3 Ce1 Se1 76.88(9) . 1_655 ? Se5 Ce1 Se1 125.73(12) . 1_655 ? Se2 Ce1 Se8 73.45(8) 1_655 1_556 ? Se7 Ce1 Se8 68.58(8) . 1_556 ? Se9 Ce1 Se8 74.23(9) . 1_556 ? Se3 Ce1 Se8 134.87(13) . 1_556 ? Se5 Ce1 Se8 143.83(12) . 1_556 ? Se1 Ce1 Se8 66.38(7) 1_655 1_556 ? Se2 Ce1 Se4 142.99(13) 1_655 . ? Se7 Ce1 Se4 70.35(8) . . ? Se9 Ce1 Se4 67.03(8) . . ? Se3 Ce1 Se4 70.13(8) . . ? Se5 Ce1 Se4 73.11(8) . . ? Se1 Ce1 Se4 137.92(12) 1_655 . ? Se8 Ce1 Se4 123.40(11) 1_556 . ? Se7 Ce2 Se2 75.90(4) 4_565 4_565 ? Se7 Ce2 Se6 86.85(5) 4_565 . ? Se2 Ce2 Se6 141.55(5) 4_565 . ? Se7 Ce2 Se8 147.79(5) 4_565 1_455 ? Se2 Ce2 Se8 122.80(5) 4_565 1_455 ? Se6 Ce2 Se8 89.57(4) . 1_455 ? Se7 Ce2 Se5 81.90(4) 4_565 4_465 ? Se2 Ce2 Se5 76.40(4) 4_565 4_465 ? Se6 Ce2 Se5 135.40(5) . 4_465 ? Se8 Ce2 Se5 78.37(4) 1_455 4_465 ? Se7 Ce2 Se4 139.78(5) 4_565 . ? Se2 Ce2 Se4 80.78(4) 4_565 . ? Se6 Ce2 Se4 91.70(4) . . ? Se8 Ce2 Se4 72.28(4) 1_455 . ? Se5 Ce2 Se4 123.68(5) 4_465 . ? Se7 Ce2 Se5 67.08(4) 4_565 . ? Se2 Ce2 Se5 71.50(4) 4_565 . ? Se6 Ce2 Se5 70.15(4) . . ? Se8 Ce2 Se5 140.40(5) 1_455 . ? Se5 Ce2 Se5 139.57(4) 4_465 . ? Se4 Ce2 Se5 74.67(4) . . ? Se7 Ce2 Se2 75.87(4) 4_565 1_554 ? Se2 Ce2 Se2 136.27(4) 4_565 1_554 ? Se6 Ce2 Se2 68.29(4) . 1_554 ? Se8 Ce2 Se2 73.10(4) 1_455 1_554 ? Se5 Ce2 Se2 67.12(4) 4_465 1_554 ? Se4 Ce2 Se2 139.83(5) . 1_554 ? Se5 Ce2 Se2 124.77(5) . 1_554 ? Se9 Ce3 Se6 89.02(4) 3_656 . ? Se9 Ce3 Se8 141.37(5) 3_656 . ? Se6 Ce3 Se8 73.10(4) . . ? Se9 Ce3 Se3 91.13(4) 3_656 3_756 ? Se6 Ce3 Se3 146.43(5) . 3_756 ? Se8 Ce3 Se3 122.64(5) . 3_756 ? Se9 Ce3 Se4 136.98(5) 3_656 1_655 ? Se6 Ce3 Se4 78.84(4) . 1_655 ? Se8 Ce3 Se4 73.78(4) . 1_655 ? Se3 Ce3 Se4 78.33(4) 3_756 1_655 ? Se9 Ce3 Se1 92.84(4) 3_656 3_656 ? Se6 Ce3 Se1 136.60(5) . 3_656 ? Se8 Ce3 Se1 78.93(4) . 3_656 ? Se3 Ce3 Se1 76.93(4) 3_756 3_656 ? Se4 Ce3 Se1 124.03(4) 1_655 3_656 ? Se9 Ce3 Se1 71.48(4) 3_656 1_554 ? Se6 Ce3 Se1 66.25(4) . 1_554 ? Se8 Ce3 Se1 70.00(4) . 1_554 ? Se3 Ce3 Se1 144.43(5) 3_756 1_554 ? Se4 Ce3 Se1 135.25(4) 1_655 1_554 ? Se1 Ce3 Se1 73.35(4) 3_656 1_554 ? Se9 Ce3 Se3 69.31(4) 3_656 . ? Se6 Ce3 Se3 75.06(4) . . ? Se8 Ce3 Se3 133.68(4) . . ? Se3 Ce3 Se3 73.65(4) 3_756 . ? Se4 Ce3 Se3 67.70(4) 1_655 . ? Se1 Ce3 Se3 144.92(4) 3_656 . ? Se1 Ce3 Se3 124.29(4) 1_554 . ? P2 Se1 Ce1 85.58(12) 1_556 1_455 ? P2 Se1 Ce3 106.03(10) 1_556 3_656 ? Ce1 Se1 Ce3 95.10(7) 1_455 3_656 ? P2 Se1 Ce3 84.13(10) 1_556 1_556 ? Ce1 Se1 Ce3 157.79(8) 1_455 1_556 ? Ce3 Se1 Ce3 106.65(4) 3_656 1_556 ? P3 Se2 Ce1 110.12(13) 4_466 1_455 ? P3 Se2 Ce2 95.06(10) 4_466 4_566 ? Ce1 Se2 Ce2 100.01(8) 1_455 4_566 ? P3 Se2 Ce2 80.93(10) 4_466 1_556 ? Ce1 Se2 Ce2 108.53(8) 1_455 1_556 ? Ce2 Se2 Ce2 150.84(6) 4_566 1_556 ? P1 Se3 Ce3 107.26(10) 1_655 3_756 ? P1 Se3 Ce1 94.21(12) 1_655 . ? Ce3 Se3 Ce1 100.01(8) 3_756 . ? P1 Se3 Ce3 84.00(9) 1_655 . ? Ce3 Se3 Ce3 106.35(4) 3_756 . ? Ce1 Se3 Ce3 152.90(8) . . ? P1 Se4 Ce3 87.32(10) . 1_455 ? P1 Se4 Ce2 105.26(10) . . ? Ce3 Se4 Ce2 99.27(5) 1_455 . ? P1 Se4 Ce1 81.53(11) . . ? Ce3 Se4 Ce1 155.66(8) 1_455 . ? Ce2 Se4 Ce1 104.51(8) . . ? P3 Se5 Ce2 84.64(11) . 4_666 ? P3 Se5 Ce1 105.54(12) . . ? Ce2 Se5 Ce1 94.41(8) 4_666 . ? P3 Se5 Ce2 85.71(11) . . ? Ce2 Se5 Ce2 157.55(5) 4_666 . ? Ce1 Se5 Ce2 107.70(8) . . ? P3 Se6 Ce3 105.78(10) . . ? P3 Se6 Ce2 89.60(10) . . ? Ce3 Se6 Ce2 127.53(5) . . ? P1 Se7 Ce1 91.43(12) . . ? P1 Se7 Ce2 104.70(11) . 4_566 ? Ce1 Se7 Ce2 129.44(9) . 4_566 ? P2 Se8 Ce3 95.56(9) 1_655 . ? P2 Se8 Ce2 109.15(10) 1_655 1_655 ? Ce3 Se8 Ce2 101.88(5) . 1_655 ? P2 Se8 Ce1 82.18(11) 1_655 1_554 ? Ce3 Se8 Ce1 152.32(8) . 1_554 ? Ce2 Se8 Ce1 104.91(8) 1_655 1_554 ? P2 Se9 Ce1 107.21(12) 3_656 . ? P2 Se9 Ce3 89.20(10) 3_656 3_656 ? Ce1 Se9 Ce3 127.87(8) . 3_656 ? Se7 P1 Se3 117.33(14) . 1_455 ? Se7 P1 Se4 115.78(16) . . ? Se3 P1 Se4 107.85(15) 1_455 . ? Se7 P1 P3 106.04(17) . 1_455 ? Se3 P1 P3 102.36(17) 1_455 1_455 ? Se4 P1 P3 106.01(16) . 1_455 ? Se8 P2 Se9 115.76(15) 1_455 3_656 ? Se8 P2 Se1 110.74(15) 1_455 1_554 ? Se9 P2 Se1 114.21(16) 3_656 1_554 ? Se8 P2 P2 102.5(2) 1_455 3 ? Se9 P2 P2 105.2(2) 3_656 3 ? Se1 P2 P2 107.2(2) 1_554 3 ? Se2 P3 Se5 110.31(15) 4_665 . ? Se2 P3 Se6 115.16(15) 4_665 . ? Se5 P3 Se6 113.42(17) . . ? Se2 P3 P1 104.00(18) 4_665 1_655 ? Se5 P3 P1 107.82(16) . 1_655 ? Se6 P3 P1 105.29(16) . 1_655 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.316 _refine_diff_density_min -2.138 _refine_diff_density_rms 0.430 #===END