#------------------------------------------------------------------------------ #$Date: 2020-10-06 10:10:30 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257320 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557766.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1557766 loop_ _publ_author_name 'Cliffe, Matthew J.' 'Keyzer, Evan N.' 'Bond, Andrew D.' 'Astle, Maxwell A.' 'Grey, Clare P.' _publ_section_title ; The structures of ordered defects in thiocyanate analogues of Prussian Blue ; _journal_issue 17 _journal_name_full 'Chemical Science' _journal_page_first 4430 _journal_page_last 4438 _journal_paper_doi 10.1039/D0SC01246G _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'Bi2 C12 N12 S12 Zn3' _chemical_formula_sum 'C12 Bi2 N12 S12 Zn3' _chemical_formula_weight 1311.03 _chemical_name_systematic 'zinc hexathiocyanatobismuthate' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_primary dual _audit_creation_date 2018-05-25 _audit_creation_method ; Olex2 1.2 (compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5497) ; _audit_update_record ; 2020-02-27 deposited with the CCDC. 2020-04-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 114.3971(12) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.7331(6) _cell_length_b 13.6501(4) _cell_length_c 16.4375(4) _cell_measurement_reflns_used 5894 _cell_measurement_temperature 180 _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 0.998 _cell_volume 3623.55(19) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 180 _diffrn_detector 'CCD plate' _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.945 _diffrn_measurement_device Area _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method \w/2\q _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 -0.01477 _diffrn_orient_matrix_UB_12 -0.00672 _diffrn_orient_matrix_UB_13 0.06480 _diffrn_orient_matrix_UB_21 -0.05024 _diffrn_orient_matrix_UB_22 -0.05064 _diffrn_orient_matrix_UB_23 -0.01671 _diffrn_orient_matrix_UB_31 0.03345 _diffrn_orient_matrix_UB_32 -0.04293 _diffrn_orient_matrix_UB_33 0.02954 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_unetI/netI 0.0697 _diffrn_reflns_Laue_measured_fraction_full 0.978 _diffrn_reflns_Laue_measured_fraction_max 0.945 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 12934 _diffrn_reflns_point_group_measured_fraction_full 0.978 _diffrn_reflns_point_group_measured_fraction_max 0.945 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.451 _diffrn_reflns_theta_min 2.061 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 12.357 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.544 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 2416 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.670 _refine_diff_density_min -2.363 _refine_diff_density_rms 0.249 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 370 _refine_ls_number_reflns 7822 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0507 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+19.2509P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1078 _refine_ls_wR_factor_ref 0.1206 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5919 _reflns_number_total 7822 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc01246g3.cif _cod_data_source_block 6_be_Zn3Bi2SCN12_P21c _cod_depositor_comments ;Adding full bibliography for 1557765--1557770.cif. Adding full bibliography for 1557765--1557770.cif. ; _cod_database_code 1557766 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.790 _shelx_estimated_absorpt_t_min 0.191 _olex2_refinement_description ; ; _shelx_res_file ; import.res created by SHELXL-2014/7 TITL import_a.res in P2(1)/c REM Old TITL import in P21/a #14 REM SHELXT solution in P2(1)/c REM R1 0.106, Rweak 0.006, Alpha 0.037, Orientation a'=c, b'=-b, c'=a REM Formula found by SHELXT: Zn3 Bi2 S12 C12 N12 CELL 0.71073 17.7331 13.6501 16.4375 90 114.397 90 ZERR 4 0.0006 0.0004 0.0004 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC Bi C N S Zn UNIT 8 48 48 48 12 L.S. 4 PLAN 20 SIZE 0.02 0.1 0.2 TEMP -93.15 list 4 fmap 2 ACTA OMIT 2 0 0 OMIT 1 1 0 OMIT 0 1 1 OMIT -2 1 1 REM REM REM WGHT 0.052100 19.250900 FVAR 0.12464 BI1 1 0.079182 0.838216 0.317151 11.00000 0.02802 0.02726 = 0.02454 -0.00161 0.01302 -0.00387 BI2 1 0.608022 0.689249 0.612311 11.00000 0.02714 0.03635 = 0.02014 -0.00025 0.01022 0.00082 ZN1 5 0.392022 0.876169 0.273391 11.00000 0.02999 0.03461 = 0.02537 0.00216 0.01373 0.00229 ZN2 5 0.849436 0.839291 0.462621 11.00000 0.03092 0.02875 = 0.02734 -0.00410 0.01359 -0.00215 ZN3 5 0.820804 0.484863 0.454140 11.00000 0.03862 0.02907 = 0.02728 0.00034 0.01510 0.00550 S9 4 0.809699 0.494706 0.162162 11.00000 0.03654 0.04244 = 0.02812 0.00570 0.01545 0.01128 S8 4 1.037850 0.689853 0.634201 11.00000 0.03553 0.04432 = 0.03039 0.00529 0.01393 0.00036 S11 4 1.050319 1.029535 0.690930 11.00000 0.02732 0.03557 = 0.03624 -0.00399 0.00391 -0.00413 S10 4 0.986911 0.668945 0.313285 11.00000 0.04486 0.03267 = 0.05198 -0.01481 0.03452 -0.00984 S1 4 0.188949 0.688193 0.320815 11.00000 0.03897 0.03589 = 0.06637 0.01013 0.03017 0.00234 S7 4 0.851898 0.141898 0.494181 11.00000 0.07998 0.02904 = 0.03178 0.00125 0.01856 0.00466 S4 4 0.632773 0.865143 0.543944 11.00000 0.03767 0.05190 = 0.03713 0.00430 0.00468 -0.01087 S6 4 0.563073 0.581623 0.452644 11.00000 0.03314 0.05808 = 0.03656 -0.01677 0.01491 -0.00736 S5 4 0.779547 0.665025 0.671464 11.00000 0.03253 0.09135 = 0.03277 0.02331 0.01294 0.00865 S3 4 0.433956 0.776327 0.019645 11.00000 0.03751 0.08992 = 0.03427 -0.02147 0.01980 -0.00586 S2 4 0.376194 1.218880 0.227824 11.00000 0.10818 0.03181 = 0.03478 -0.00150 0.03637 0.00394 S12 4 0.622247 0.982573 0.223288 11.00000 0.06070 0.04733 = 0.04211 -0.00264 -0.00131 0.02194 N7 3 0.821037 0.341477 0.466452 11.00000 0.05063 0.03282 = 0.04155 0.01046 0.02104 0.00713 N11 3 0.936362 0.924019 0.546065 11.00000 0.02967 0.03417 = 0.03728 -0.00634 0.01441 0.00180 N1 3 0.302855 0.802844 0.286421 11.00000 0.03154 0.04101 = 0.03673 0.00352 0.01525 -0.00119 N12 3 0.759331 0.912741 0.372670 11.00000 0.04613 0.03668 = 0.04123 -0.00317 0.01282 0.00497 N4 3 0.495061 0.853860 0.380621 11.00000 0.04088 0.05179 = 0.03683 0.00578 0.01770 -0.00190 N5 3 0.810015 0.761050 0.538254 11.00000 0.02741 0.03773 = 0.03868 0.00164 0.01673 -0.00367 N2 3 0.379959 1.019818 0.265603 11.00000 0.04441 0.03459 = 0.03343 -0.00368 0.01793 0.00322 N9 3 0.822759 0.510358 0.337369 11.00000 0.03890 0.02501 = 0.03718 0.00411 0.01758 0.00613 N3 3 0.403203 0.832291 0.166639 11.00000 0.03525 0.05029 = 0.03192 0.00173 0.02095 0.00042 C7 2 0.832995 0.259003 0.478466 11.00000 0.03228 0.02849 = 0.03320 0.00160 0.02195 -0.00040 N6 3 0.718216 0.532621 0.460105 11.00000 0.04530 0.03515 = 0.02714 -0.00700 0.01783 -0.00207 C9 2 0.818131 0.503028 0.264982 11.00000 0.02338 0.02299 = 0.03457 0.00102 0.01210 0.00322 C11 2 0.984396 0.968510 0.606614 11.00000 0.01964 0.02345 = 0.02538 0.00287 0.01137 0.00276 N10 3 0.900511 0.751968 0.405370 11.00000 0.04323 0.03971 = 0.03159 -0.00327 0.02033 0.00271 N8 3 0.917658 0.548685 0.545665 11.00000 0.04508 0.04118 = 0.03235 0.00512 0.01315 0.01033 C10 2 0.935916 0.718082 0.368026 11.00000 0.02598 0.02945 = 0.02536 0.00598 0.01072 -0.00194 C1 2 0.256073 0.756175 0.300466 11.00000 0.02962 0.03281 = 0.02591 -0.00008 0.00746 0.00243 C8 2 0.967680 0.605362 0.584272 11.00000 0.03485 0.03676 = 0.03258 0.00471 0.01414 0.01044 C4 2 0.550857 0.858209 0.446595 11.00000 0.02804 0.03402 = 0.03136 0.01005 0.01098 0.00063 C2 2 0.378396 1.101754 0.251747 11.00000 0.04067 0.03757 = 0.02400 -0.00430 0.01538 0.00035 C12 2 0.703146 0.940978 0.310113 11.00000 0.04577 0.03139 = 0.04233 -0.00113 0.02048 0.00300 C3 2 0.415273 0.809004 0.106590 11.00000 0.02893 0.04796 = 0.04284 -0.00245 0.01891 -0.00148 C5 2 0.796915 0.722215 0.592288 11.00000 0.01912 0.04101 = 0.03723 0.00073 0.00726 0.00492 C6 2 0.654120 0.552549 0.457265 11.00000 0.04470 0.03283 = 0.02315 -0.00346 0.01905 -0.00487 HKLF 4 REM import_a.res in P2(1)/c REM R1 = 0.0507 for 5919 Fo > 4sig(Fo) and 0.0780 for all 7822 data REM 370 parameters refined using 0 restraints END WGHT 0.0521 19.2510 REM Highest difference peak 1.670, deepest hole -2.363, 1-sigma level 0.249 Q1 1 0.0837 0.7701 0.3223 11.00000 0.05 1.67 Q2 1 0.6075 0.6229 0.6148 11.00000 0.05 1.59 Q3 1 0.6650 0.6491 0.6945 11.00000 0.05 1.42 Q4 1 0.0227 0.7995 0.2388 11.00000 0.05 1.39 Q5 1 0.0792 0.9053 0.3203 11.00000 0.05 1.35 Q6 1 0.0768 0.8381 0.3666 11.00000 0.05 1.23 Q7 1 1.0743 1.0114 0.8094 11.00000 0.05 1.21 Q8 1 0.6136 0.6818 0.5557 11.00000 0.05 1.16 Q9 1 0.0255 0.8836 0.2358 11.00000 0.05 1.15 Q10 1 0.6614 0.7400 0.6928 11.00000 0.05 1.14 Q11 1 0.0199 0.8837 0.3265 11.00000 0.05 1.12 Q12 1 0.0191 0.9071 0.2625 11.00000 0.05 1.10 Q13 1 0.9912 0.7164 0.6601 11.00000 0.05 1.07 Q14 1 1.0831 0.9458 0.8153 11.00000 0.05 1.06 Q15 1 0.5519 0.7265 0.5228 11.00000 0.05 1.05 Q16 1 0.1347 0.7848 0.3870 11.00000 0.05 1.04 Q17 1 0.1363 0.8806 0.4000 11.00000 0.05 1.03 Q18 1 0.0881 0.8491 0.2725 11.00000 0.05 1.03 Q19 1 0.7109 0.8436 0.4611 11.00000 0.05 1.02 Q20 1 0.1401 0.8340 0.2897 11.00000 0.05 1.01 ; _shelx_res_checksum 13141 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.07918(2) 0.83822(2) 0.31715(2) 0.02589(11) Uani 1 1 d . . . . . Bi2 Bi 0.60802(2) 0.68925(3) 0.61231(2) 0.02773(11) Uani 1 1 d . . . . . Zn1 Zn 0.39202(7) 0.87617(8) 0.27339(7) 0.0292(2) Uani 1 1 d . . . . . Zn2 Zn 0.84944(7) 0.83929(7) 0.46262(7) 0.0285(2) Uani 1 1 d . . . . . Zn3 Zn 0.82080(7) 0.48486(8) 0.45414(7) 0.0312(3) Uani 1 1 d . . . . . S9 S 0.80970(16) 0.49471(19) 0.16216(16) 0.0350(6) Uani 1 1 d . . . . . S8 S 1.03785(17) 0.68985(19) 0.63420(17) 0.0366(6) Uani 1 1 d . . . . . S11 S 1.05032(16) 1.02954(18) 0.69093(17) 0.0361(6) Uani 1 1 d . . . . . S10 S 0.98691(18) 0.66894(18) 0.31328(19) 0.0384(6) Uani 1 1 d . . . . . S1 S 0.18895(19) 0.68819(19) 0.3208(2) 0.0443(7) Uani 1 1 d . . . . . S7 S 0.8519(2) 0.14190(19) 0.49418(18) 0.0484(8) Uani 1 1 d . . . . . S4 S 0.63277(18) 0.8651(2) 0.54394(18) 0.0458(7) Uani 1 1 d . . . . . S6 S 0.56307(17) 0.5816(2) 0.45264(18) 0.0424(7) Uani 1 1 d . . . . . S5 S 0.77955(19) 0.6650(3) 0.67146(19) 0.0524(8) Uani 1 1 d . . . . . S3 S 0.43396(19) 0.7763(3) 0.01964(19) 0.0522(8) Uani 1 1 d . . . . . S2 S 0.3762(3) 1.2189(2) 0.22782(19) 0.0560(9) Uani 1 1 d . . . . . S12 S 0.6222(2) 0.9826(2) 0.2233(2) 0.0575(9) Uani 1 1 d . . . . . N7 N 0.8210(6) 0.3415(6) 0.4665(6) 0.041(2) Uani 1 1 d . . . . . N11 N 0.9364(5) 0.9240(6) 0.5461(5) 0.0335(19) Uani 1 1 d . . . . . N1 N 0.3029(5) 0.8028(6) 0.2864(6) 0.036(2) Uani 1 1 d . . . . . N12 N 0.7593(6) 0.9127(6) 0.3727(6) 0.043(2) Uani 1 1 d . . . . . N4 N 0.4951(6) 0.8539(7) 0.3806(6) 0.043(2) Uani 1 1 d . . . . . N5 N 0.8100(5) 0.7610(6) 0.5383(6) 0.0336(19) Uani 1 1 d . . . . . N2 N 0.3800(5) 1.0198(6) 0.2656(5) 0.037(2) Uani 1 1 d . . . . . N9 N 0.8228(5) 0.5104(5) 0.3374(5) 0.0331(19) Uani 1 1 d . . . . . N3 N 0.4032(5) 0.8323(6) 0.1666(6) 0.037(2) Uani 1 1 d . . . . . C7 C 0.8330(6) 0.2590(7) 0.4785(6) 0.029(2) Uani 1 1 d . . . . . N6 N 0.7182(6) 0.5326(6) 0.4601(5) 0.0349(19) Uani 1 1 d . . . . . C9 C 0.8181(6) 0.5030(6) 0.2650(6) 0.027(2) Uani 1 1 d . . . . . C11 C 0.9844(5) 0.9685(6) 0.6066(6) 0.0221(18) Uani 1 1 d . . . . . N10 N 0.9005(6) 0.7520(6) 0.4054(5) 0.037(2) Uani 1 1 d . . . . . N8 N 0.9177(6) 0.5487(7) 0.5457(6) 0.040(2) Uani 1 1 d . . . . . C10 C 0.9359(6) 0.7181(7) 0.3680(6) 0.027(2) Uani 1 1 d . . . . . C1 C 0.2561(6) 0.7562(7) 0.3005(6) 0.031(2) Uani 1 1 d . . . . . C8 C 0.9677(7) 0.6054(7) 0.5843(7) 0.035(2) Uani 1 1 d . . . . . C4 C 0.5509(6) 0.8582(7) 0.4466(7) 0.032(2) Uani 1 1 d . . . . . C2 C 0.3784(7) 1.1018(8) 0.2517(6) 0.033(2) Uani 1 1 d . . . . . C12 C 0.7031(7) 0.9410(7) 0.3101(7) 0.039(2) Uani 1 1 d . . . . . C3 C 0.4153(7) 0.8090(8) 0.1066(7) 0.039(2) Uani 1 1 d . . . . . C5 C 0.7969(6) 0.7222(7) 0.5923(7) 0.034(2) Uani 1 1 d . . . . . C6 C 0.6541(7) 0.5525(7) 0.4573(6) 0.032(2) 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 Bi1 0.0280(2) 0.02726(19) 0.02454(18) -0.00161(14) 0.01302(16) -0.00387(14) Bi2 0.0271(2) 0.0364(2) 0.02014(18) -0.00025(14) 0.01022(15) 0.00082(15) Zn1 0.0300(7) 0.0346(6) 0.0254(5) 0.0022(5) 0.0137(5) 0.0023(5) Zn2 0.0309(6) 0.0287(5) 0.0273(5) -0.0041(4) 0.0136(5) -0.0021(5) Zn3 0.0386(7) 0.0291(5) 0.0273(6) 0.0003(5) 0.0151(5) 0.0055(5) S9 0.0365(15) 0.0424(14) 0.0281(12) 0.0057(11) 0.0154(11) 0.0113(11) S8 0.0355(15) 0.0443(14) 0.0304(13) 0.0053(11) 0.0139(12) 0.0004(11) S11 0.0273(14) 0.0356(13) 0.0362(13) -0.0040(11) 0.0039(11) -0.0041(11) S10 0.0449(17) 0.0327(12) 0.0520(16) -0.0148(12) 0.0345(14) -0.0098(11) S1 0.0390(17) 0.0359(13) 0.0664(19) 0.0101(13) 0.0302(16) 0.0023(12) S7 0.080(2) 0.0290(13) 0.0318(14) 0.0012(11) 0.0186(15) 0.0047(13) S4 0.0377(17) 0.0519(16) 0.0371(14) 0.0043(13) 0.0047(13) -0.0109(13) S6 0.0331(16) 0.0581(17) 0.0366(14) -0.0168(13) 0.0149(13) -0.0074(13) S5 0.0325(16) 0.091(2) 0.0328(14) 0.0233(15) 0.0129(13) 0.0087(15) S3 0.0375(17) 0.090(2) 0.0343(14) -0.0215(15) 0.0198(13) -0.0059(16) S2 0.108(3) 0.0318(14) 0.0348(15) -0.0015(12) 0.0364(17) 0.0039(16) S12 0.061(2) 0.0473(17) 0.0421(16) -0.0026(14) -0.0013(15) 0.0219(15) N7 0.051(6) 0.033(5) 0.042(5) 0.010(4) 0.021(5) 0.007(4) N11 0.030(5) 0.034(4) 0.037(5) -0.006(4) 0.014(4) 0.002(4) N1 0.032(5) 0.041(5) 0.037(5) 0.004(4) 0.015(4) -0.001(4) N12 0.046(6) 0.037(5) 0.041(5) -0.003(4) 0.013(5) 0.005(4) N4 0.041(6) 0.052(6) 0.037(5) 0.006(4) 0.018(5) -0.002(4) N5 0.027(5) 0.038(5) 0.039(5) 0.002(4) 0.017(4) -0.004(4) N2 0.044(6) 0.035(5) 0.033(5) -0.004(4) 0.018(4) 0.003(4) N9 0.039(5) 0.025(4) 0.037(5) 0.004(4) 0.018(4) 0.006(4) N3 0.035(5) 0.050(5) 0.032(5) 0.002(4) 0.021(4) 0.000(4) C7 0.032(6) 0.028(5) 0.033(5) 0.002(4) 0.022(5) 0.000(4) N6 0.045(6) 0.035(4) 0.027(4) -0.007(4) 0.018(4) -0.002(4) C9 0.023(5) 0.023(4) 0.035(5) 0.001(4) 0.012(4) 0.003(4) C11 0.020(5) 0.023(4) 0.025(5) 0.003(4) 0.011(4) 0.003(4) N10 0.043(6) 0.040(5) 0.032(4) -0.003(4) 0.020(4) 0.003(4) N8 0.045(6) 0.041(5) 0.032(5) 0.005(4) 0.013(4) 0.010(5) C10 0.026(5) 0.029(5) 0.025(5) 0.006(4) 0.011(4) -0.002(4) C1 0.030(6) 0.033(5) 0.026(5) 0.000(4) 0.007(4) 0.002(4) C8 0.035(6) 0.037(6) 0.033(5) 0.005(5) 0.014(5) 0.010(5) C4 0.028(6) 0.034(5) 0.031(5) 0.010(4) 0.011(5) 0.001(4) C2 0.041(6) 0.038(6) 0.024(5) -0.004(4) 0.015(5) 0.000(5) C12 0.046(7) 0.031(5) 0.042(6) -0.001(5) 0.020(6) 0.003(5) C3 0.029(6) 0.048(6) 0.043(6) -0.002(5) 0.019(5) -0.001(5) C5 0.019(5) 0.041(6) 0.037(5) 0.001(5) 0.007(5) 0.005(4) C6 0.045(7) 0.033(5) 0.023(5) -0.003(4) 0.019(5) -0.005(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 S9 Bi1 S11 91.99(8) 2_655 3_676 ? S9 Bi1 S7 80.35(8) 2_655 3_666 ? S8 Bi1 S9 95.30(7) 4_475 2_655 ? S8 Bi1 S11 100.68(8) 4_475 3_676 ? S8 Bi1 S10 88.38(8) 4_475 1_455 ? S8 Bi1 S7 170.43(9) 4_475 3_666 ? S10 Bi1 S9 172.35(8) 1_455 2_655 ? S10 Bi1 S11 93.92(7) 1_455 3_676 ? S10 Bi1 S7 95.00(8) 1_455 3_666 ? S1 Bi1 S9 96.07(8) . 2_655 ? S1 Bi1 S8 78.22(9) . 4_475 ? S1 Bi1 S11 171.92(8) . 3_676 ? S1 Bi1 S10 78.08(8) . 1_455 ? S1 Bi1 S7 93.70(9) . 3_666 ? S7 Bi1 S11 88.04(8) 3_666 3_676 ? S4 Bi2 S6 96.06(9) . . ? S4 Bi2 S5 84.93(9) . . ? S4 Bi2 S3 87.62(9) . 4_576 ? S4 Bi2 S2 91.22(9) . 3_676 ? S4 Bi2 S12 165.03(9) . 4_576 ? S6 Bi2 S3 76.23(9) . 4_576 ? S6 Bi2 S12 94.66(9) . 4_576 ? S5 Bi2 S6 96.34(9) . . ? S5 Bi2 S3 168.88(7) . 4_576 ? S5 Bi2 S2 93.06(11) . 3_676 ? S5 Bi2 S12 83.52(9) . 4_576 ? S3 Bi2 S12 105.10(9) 4_576 4_576 ? S2 Bi2 S6 168.57(10) 3_676 . ? S2 Bi2 S3 95.34(10) 3_676 4_576 ? S2 Bi2 S12 79.93(9) 3_676 4_576 ? N1 Zn1 N4 108.4(4) . . ? N1 Zn1 N2 116.4(4) . . ? N4 Zn1 N2 104.3(4) . . ? N3 Zn1 N1 109.3(4) . . ? N3 Zn1 N4 111.0(4) . . ? N3 Zn1 N2 107.3(3) . . ? N11 Zn2 N5 105.0(3) . . ? N12 Zn2 N11 112.9(4) . . ? N12 Zn2 N5 111.3(4) . . ? N12 Zn2 N10 110.2(4) . . ? N10 Zn2 N11 108.0(3) . . ? N10 Zn2 N5 109.2(3) . . ? N7 Zn3 N6 106.6(4) . . ? N9 Zn3 N7 106.1(3) . . ? N9 Zn3 N6 112.3(3) . . ? N8 Zn3 N7 113.5(4) . . ? N8 Zn3 N9 107.9(4) . . ? N8 Zn3 N6 110.4(3) . . ? C9 S9 Bi1 99.6(3) . 2_645 ? C8 S8 Bi1 104.3(3) . 4_676 ? C11 S11 Bi1 90.2(3) . 3_676 ? C10 S10 Bi1 95.6(3) . 1_655 ? C1 S1 Bi1 97.9(3) . . ? C7 S7 Bi1 92.7(3) . 3_666 ? C4 S4 Bi2 96.9(3) . . ? C6 S6 Bi2 100.9(3) . . ? C5 S5 Bi2 101.5(4) . . ? C3 S3 Bi2 93.0(4) . 4_575 ? C2 S2 Bi2 103.1(3) . 3_676 ? C12 S12 Bi2 94.8(4) . 4_575 ? C7 N7 Zn3 170.4(9) . . ? C11 N11 Zn2 168.8(7) . . ? C1 N1 Zn1 173.9(9) . . ? C12 N12 Zn2 167.6(8) . . ? C4 N4 Zn1 166.8(9) . . ? C5 N5 Zn2 169.7(8) . . ? C2 N2 Zn1 169.3(8) . . ? C9 N9 Zn3 164.2(7) . . ? C3 N3 Zn1 175.2(9) . . ? N7 C7 S7 178.3(9) . . ? C6 N6 Zn3 172.7(8) . . ? N9 C9 S9 178.6(9) . . ? N11 C11 S11 179.4(8) . . ? C10 N10 Zn2 166.4(8) . . ? C8 N8 Zn3 162.7(8) . . ? N10 C10 S10 179.7(10) . . ? N1 C1 S1 179.6(9) . . ? N8 C8 S8 176.8(9) . . ? N4 C4 S4 179.7(12) . . ? N2 C2 S2 177.7(9) . . ? N12 C12 S12 178.3(10) . . ? N3 C3 S3 179.2(11) . . ? N5 C5 S5 179.0(9) . . ? N6 C6 S6 179.5(10) . . ? 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 Bi1 S9 2.830(2) 2_655 ? Bi1 S8 2.812(2) 4_475 ? Bi1 S11 2.881(3) 3_676 ? Bi1 S10 2.817(2) 1_455 ? Bi1 S1 2.809(3) . ? Bi1 S7 2.838(3) 3_666 ? Bi2 S4 2.762(3) . ? Bi2 S6 2.820(3) . ? Bi2 S5 2.804(3) . ? Bi2 S3 2.861(3) 4_576 ? Bi2 S2 2.819(3) 3_676 ? Bi2 S12 2.917(3) 4_576 ? Zn1 N1 1.956(9) . ? Zn1 N4 1.969(10) . ? Zn1 N2 1.971(9) . ? Zn1 N3 1.940(8) . ? Zn2 N11 1.962(9) . ? Zn2 N12 1.947(10) . ? Zn2 N5 1.973(8) . ? Zn2 N10 1.957(8) . ? Zn3 N7 1.967(8) . ? Zn3 N9 1.965(8) . ? Zn3 N6 1.973(9) . ? Zn3 N8 1.959(10) . ? S9 Bi1 2.830(2) 2_645 ? S9 C9 1.638(9) . ? S8 Bi1 2.812(2) 4_676 ? S8 C8 1.646(12) . ? S11 Bi1 2.881(3) 3_676 ? S11 C11 1.626(9) . ? S10 Bi1 2.817(2) 1_655 ? S10 C10 1.658(9) . ? S1 C1 1.649(10) . ? S7 Bi1 2.838(3) 3_666 ? S7 C7 1.632(9) . ? S4 C4 1.661(11) . ? S6 C6 1.634(11) . ? S5 C5 1.652(11) . ? S3 Bi2 2.861(3) 4_575 ? S3 C3 1.656(10) . ? S2 Bi2 2.819(3) 3_676 ? S2 C2 1.643(11) . ? S12 Bi2 2.917(3) 4_575 ? S12 C12 1.651(12) . ? N7 C7 1.148(12) . ? N11 C11 1.177(11) . ? N1 C1 1.143(12) . ? N12 C12 1.163(14) . ? N4 C4 1.128(13) . ? N5 C5 1.138(12) . ? N2 C2 1.139(12) . ? N9 C9 1.163(11) . ? N3 C3 1.138(12) . ? N6 C6 1.151(12) . ? N10 C10 1.142(11) . ? N8 C8 1.150(13) . ?