#------------------------------------------------------------------------------ #$Date: 2023-10-27 03:59:32 +0300 (Fri, 27 Oct 2023) $ #$Revision: 287133 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/75/7247587.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_7247587 loop_ _publ_author_name 'Zhang, Lirong' 'Zhao, Huiling' 'Liu, Xin' 'Teri, Gele' 'Baiyin, Menghe' _publ_section_title ; Syntheses, crystal structure, and photoelectric properties of two Zn-based chalcogenidoantimonates Zn-Sb-Q (Q = S, Se). ; _journal_name_full 'Physical chemistry chemical physics : PCCP' _journal_paper_doi 10.1039/d3cp04074g _journal_year 2023 _chemical_formula_moiety 'C16 H48 N10 S6 Sb2 Zn2' _chemical_formula_sum 'C16 H48 N10 S6 Sb2 Zn2' _chemical_formula_weight 947.24 _space_group_crystal_system tetragonal _space_group_IT_number 88 _space_group_name_Hall '-I 4ad' _space_group_name_H-M_alt 'I 41/a :2' _atom_sites_solution_hydrogens geom _audit_creation_date 2023-05-05 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2023-07-09 deposited with the CCDC. 2023-10-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 25.9513(11) _cell_length_b 25.9513(11) _cell_length_c 9.8863(7) _cell_measurement_reflns_used 9999 _cell_measurement_temperature 273.15 _cell_measurement_theta_max 28.00 _cell_measurement_theta_min 2.50 _cell_volume 6658.1(6) _computing_cell_refinement 'SAINT V8.40A (?, 2016)' _computing_data_reduction 'SAINT V8.40A (?, 2016)' _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 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_unetI/netI 0.0242 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 71281 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.120 _diffrn_reflns_theta_min 3.129 _exptl_absorpt_coefficient_mu 3.432 _exptl_absorpt_correction_T_max 0.165 _exptl_absorpt_correction_T_min 0.143 _exptl_absorpt_correction_type none _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2)' _exptl_crystal_colour 'clear light white' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary white _exptl_crystal_density_diffrn 1.890 _exptl_crystal_description block _exptl_crystal_F_000 3776 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.5 _refine_diff_density_max 1.751 _refine_diff_density_min -3.424 _refine_diff_density_rms 0.158 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 158 _refine_ls_number_reflns 3679 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0472 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0476P)^2^+111.8368P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1145 _refine_ls_wR_factor_ref 0.1207 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3135 _reflns_number_total 3679 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 230426c_0m I -4 R = 0.12 New:I41/a 230426c_0m_pl.res created by SHELXL-2018/3 at 16:06:05 on 05-May-2023 CELL 0.71073 25.9513 25.9513 9.8863 90 90 90 ZERR 8 0.0011 0.0011 0.0007 0 0 0 LATT 2 SYMM 0.75-Y,0.25+X,0.25+Z SYMM 0.5-X,-Y,0.5+Z SYMM 0.75+Y,0.75-X,0.75+Z SFAC C H N S Sb Zn UNIT 128 384 80 48 16 16 DELU 0.0001 0.0002 S1 S3 Sb1 S2 S2 EADP Zn1 S3 L.S. 10 PLAN 7 SIZE 0.5 0.5 0.5 TEMP 0 BIND Zn1 N1 CONF MORE -1 BOND $H fmap 2 acta OMIT -1 2 1 OMIT 1 2 1 REM REM REM WGHT 0.047600 111.836800 FVAR 0.09725 ZN1 6 0.063568 -0.069093 0.143265 11.00000 0.03336 0.03350 = 0.02682 -0.00150 0.00115 0.00327 SB1 5 0.019766 0.047407 0.397272 11.00000 0.02383 0.01948 = 0.02504 0.00196 0.00019 -0.00228 S3 4 0.051740 0.028712 0.179813 11.00000 0.03336 0.03350 = 0.02682 -0.00150 0.00115 0.00327 S2 4 0.063877 -0.005107 0.568856 11.00000 0.02014 0.02787 = 0.03041 0.00481 -0.00358 -0.00288 S1 4 0.013012 0.132543 0.464711 11.00000 0.03384 0.01995 = 0.03766 -0.00066 0.00702 -0.00326 N2 3 0.077670 -0.057013 -0.073186 11.00000 0.03331 0.03668 = 0.02694 0.00143 -0.00100 0.00681 AFIX 13 H2 2 0.047479 -0.039667 -0.111553 11.00000 -1.20000 AFIX 0 N3 3 0.146562 -0.045898 0.136051 11.00000 0.02844 0.02848 = 0.03535 0.00153 -0.00250 0.00625 AFIX 13 H3 2 0.147581 -0.011032 0.174029 11.00000 -1.20000 AFIX 0 N4 3 0.096074 -0.106279 0.319675 11.00000 0.03161 0.03361 = 0.02650 -0.00198 -0.00451 0.00376 AFIX 23 H4A 2 0.074922 -0.101635 0.389481 11.00000 -1.20000 H4B 2 0.098201 -0.139997 0.304206 11.00000 -1.20000 AFIX 0 N1 3 -0.015397 -0.082373 0.197887 11.00000 0.02692 0.03526 = 0.06967 -0.01659 0.00704 -0.00164 AFIX 137 H1A 2 -0.025455 -0.053990 0.154800 11.00000 -1.20000 H1B 2 0.018776 -0.084888 0.194199 11.00000 -1.20000 H1C 2 -0.025406 -0.080785 0.283891 11.00000 -1.20000 AFIX 0 N5 3 0.048651 -0.147600 0.059146 11.00000 0.03010 0.02614 = 0.02921 -0.00265 -0.00687 0.00784 AFIX 13 H5 2 0.078227 -0.169752 0.079583 11.00000 -1.20000 AFIX 0 C1 1 0.043230 -0.143463 -0.088464 11.00000 0.04593 0.03671 = 0.03006 -0.01156 -0.00842 0.00898 AFIX 23 H1D 2 0.009205 -0.130557 -0.110865 11.00000 -1.20000 H1E 2 0.047224 -0.177181 -0.129489 11.00000 -1.20000 AFIX 0 C4 1 -0.038511 -0.127353 0.133615 11.00000 0.02782 0.03338 = 0.04517 -0.00264 -0.00342 -0.00489 AFIX 23 H4C 2 -0.050775 -0.118533 0.043870 11.00000 -1.20000 H4D 2 -0.067503 -0.139542 0.186635 11.00000 -1.20000 AFIX 0 C6 1 0.166066 -0.040630 -0.002222 11.00000 0.02878 0.05308 = 0.04743 0.00817 0.00324 -0.00202 AFIX 23 H6A 2 0.179483 -0.073413 -0.033541 11.00000 -1.20000 H6B 2 0.193803 -0.015589 -0.004441 11.00000 -1.20000 AFIX 0 C8 1 0.122699 -0.023267 -0.092910 11.00000 0.04422 0.04973 = 0.03502 0.01180 0.00407 0.00235 AFIX 23 H8A 2 0.113497 0.012052 -0.071747 11.00000 -1.20000 H8B 2 0.133678 -0.024623 -0.186629 11.00000 -1.20000 AFIX 0 C2 1 0.147434 -0.086778 0.355833 11.00000 0.03562 0.03958 = 0.03552 -0.00216 -0.01068 0.00902 AFIX 23 H2A 2 0.165312 -0.111824 0.411527 11.00000 -1.20000 H2B 2 0.144217 -0.055035 0.406945 11.00000 -1.20000 AFIX 0 C5 1 0.002755 -0.169061 0.124640 11.00000 0.04690 0.02560 = 0.03959 0.00038 -0.00571 -0.00097 AFIX 23 H5A 2 0.011428 -0.181192 0.214610 11.00000 -1.20000 H5B 2 -0.010087 -0.198046 0.072665 11.00000 -1.20000 AFIX 0 C3 1 0.083650 -0.107376 -0.142391 11.00000 0.04865 0.04364 = 0.02614 -0.00906 0.00009 0.01477 AFIX 23 H3A 2 0.117737 -0.121275 -0.125369 11.00000 -1.20000 H3B 2 0.079469 -0.103110 -0.239246 11.00000 -1.20000 AFIX 0 C7 1 0.177622 -0.077073 0.226936 11.00000 0.02733 0.03639 = 0.04751 0.00156 -0.00707 0.00895 AFIX 23 H7A 2 0.209506 -0.059275 0.247895 11.00000 -1.20000 H7B 2 0.186113 -0.109599 0.184039 11.00000 -1.20000 AFIX 0 HKLF 4 1 0 1 0 -1 0 0 0 0 1 REM 230426c_0m I -4 R = 0.12 New:I41/a REM wR2 = 0.1207, GooF = S = 1.090, Restrained GooF = 1.094 for all data REM R1 = 0.0472 for 3135 Fo > 4sig(Fo) and 0.0577 for all 3679 data REM 158 parameters refined using 6 restraints END WGHT 0.0477 111.8292 REM Highest difference peak 1.751, deepest hole -3.424, 1-sigma level 0.158 Q1 1 0.0250 0.0671 0.3889 11.00000 0.05 0.91 Q2 1 0.0022 0.0463 0.3793 11.00000 0.05 0.88 Q3 1 -0.0098 -0.0703 0.1291 11.00000 0.05 0.56 Q4 1 0.0502 -0.0083 0.5673 11.00000 0.05 0.55 Q5 1 0.0918 -0.0393 0.1815 11.00000 0.05 0.54 Q6 1 0.0074 0.1405 0.4123 11.00000 0.05 0.53 Q7 1 0.0214 0.1222 0.5084 11.00000 0.05 0.51 REM The information below was added by Olex2. REM REM R1 = 0.0472 for 3135 Fo > 4sig(Fo) and 0.0577 for all 73825 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.75, deepest hole -3.42 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0577 REM R1_gt = 0.0472 REM wR_ref = 0.1207 REM GOOF = 1.090 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 73825 REM Reflections_gt = 3135 REM Parameters = n/a REM Hole = -3.42 REM Peak = 1.75 REM Flack = n/a ; _cod_data_source_file d3cp04074g2.cif _cod_data_source_block 230426c_0m_pl _cod_original_cell_volume 6658.1(7) _cod_original_sg_symbol_H-M 'I 41/a' _cod_database_code 7247587 _shelx_shelxl_version_number 2018/3 _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 0.279 _shelx_estimated_absorpt_t_min 0.279 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H) groups, All N(H,H) groups, All N(H,H,H) groups 2. Rigid bond restraints S1, S3, Sb1, S2, S2 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0002 3. Uiso/Uaniso restraints and constraints Uanis(Zn1) = Uanis(S3) 4.a Ternary CH refined with riding coordinates: N2(H2), N3(H3), N5(H5) 4.b Secondary CH2 refined with riding coordinates: N4(H4A,H4B), C1(H1D,H1E), C4(H4C,H4D), C6(H6A,H6B), C8(H8A,H8B), C2(H2A,H2B), C5(H5A,H5B), C3(H3A,H3B), C7(H7A,H7B) 4.c Idealised Me refined as rotating group: N1(H1A,H1B,H1C) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' 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 Zn1 Zn 0.06357(3) -0.06909(3) 0.14326(8) 0.03123(17) Uani 1 1 d . . . . . Sb1 Sb 0.01977(2) 0.04741(2) 0.39727(4) 0.02279(13) Uani 1 1 d . U . . . S3 S 0.05174(6) 0.02871(6) 0.17981(16) 0.03123(17) Uani 1 1 d . U . . . S2 S 0.06388(5) -0.00511(6) 0.56886(16) 0.0261(3) Uani 1 1 d . U . . . S1 S 0.01301(6) 0.13254(6) 0.46471(17) 0.0305(3) Uani 1 1 d . U . . . N2 N 0.0777(2) -0.0570(2) -0.0732(5) 0.0323(12) Uani 1 1 d . . . . . H2 H 0.047479 -0.039667 -0.111553 0.039 Uiso 1 1 calc R . . . . N3 N 0.1466(2) -0.0459(2) 0.1361(6) 0.0308(12) Uani 1 1 d . . . . . H3 H 0.147581 -0.011032 0.174029 0.037 Uiso 1 1 calc R . . . . N4 N 0.0961(2) -0.1063(2) 0.3197(5) 0.0306(11) Uani 1 1 d . . . . . H4A H 0.074922 -0.101635 0.389481 0.037 Uiso 1 1 calc R . . . . H4B H 0.098201 -0.139997 0.304206 0.037 Uiso 1 1 calc R . . . . N1 N -0.0154(2) -0.0824(2) 0.1979(7) 0.0439(16) Uani 1 1 d . . . . . H1A H -0.025455 -0.053990 0.154800 0.053 Uiso 1 1 calc GR . . . . H1B H 0.018776 -0.084888 0.194199 0.053 Uiso 1 1 calc GR . . . . H1C H -0.025406 -0.080785 0.283891 0.053 Uiso 1 1 calc GR . . . . N5 N 0.0487(2) -0.1476(2) 0.0591(5) 0.0285(11) Uani 1 1 d . . . . . H5 H 0.078227 -0.169752 0.079583 0.034 Uiso 1 1 calc R . . . . C1 C 0.0432(3) -0.1435(3) -0.0885(7) 0.0376(16) Uani 1 1 d . . . . . H1D H 0.009205 -0.130557 -0.110865 0.045 Uiso 1 1 calc R . . . . H1E H 0.047224 -0.177181 -0.129489 0.045 Uiso 1 1 calc R . . . . C4 C -0.0385(3) -0.1274(3) 0.1336(8) 0.0355(15) Uani 1 1 d . . . . . H4C H -0.050775 -0.118533 0.043870 0.043 Uiso 1 1 calc R . . . . H4D H -0.067503 -0.139542 0.186635 0.043 Uiso 1 1 calc R . . . . C6 C 0.1661(3) -0.0406(3) -0.0022(8) 0.0431(17) Uani 1 1 d . . . . . H6A H 0.179483 -0.073413 -0.033541 0.052 Uiso 1 1 calc R . . . . H6B H 0.193803 -0.015589 -0.004441 0.052 Uiso 1 1 calc R . . . . C8 C 0.1227(3) -0.0233(3) -0.0929(8) 0.0430(17) Uani 1 1 d . . . . . H8A H 0.113497 0.012052 -0.071747 0.052 Uiso 1 1 calc R . . . . H8B H 0.133678 -0.024623 -0.186629 0.052 Uiso 1 1 calc R . . . . C2 C 0.1474(3) -0.0868(3) 0.3558(7) 0.0369(15) Uani 1 1 d . . . . . H2A H 0.165312 -0.111824 0.411527 0.044 Uiso 1 1 calc R . . . . H2B H 0.144217 -0.055035 0.406945 0.044 Uiso 1 1 calc R . . . . C5 C 0.0028(3) -0.1691(3) 0.1246(8) 0.0374(15) Uani 1 1 d . . . . . H5A H 0.011428 -0.181192 0.214610 0.045 Uiso 1 1 calc R . . . . H5B H -0.010087 -0.198046 0.072665 0.045 Uiso 1 1 calc R . . . . C3 C 0.0837(3) -0.1074(3) -0.1424(7) 0.0395(16) Uani 1 1 d . . . . . H3A H 0.117737 -0.121275 -0.125369 0.047 Uiso 1 1 calc R . . . . H3B H 0.079469 -0.103110 -0.239246 0.047 Uiso 1 1 calc R . . . . C7 C 0.1776(3) -0.0771(3) 0.2269(8) 0.0371(15) Uani 1 1 d . . . . . H7A H 0.209506 -0.059275 0.247895 0.044 Uiso 1 1 calc R . . . . H7B H 0.186113 -0.109599 0.184039 0.044 Uiso 1 1 calc R . . . . 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 Zn1 0.0334(4) 0.0335(4) 0.0268(3) -0.0015(2) 0.0011(2) 0.0033(3) Sb1 0.0238(2) 0.01948(19) 0.0250(2) 0.00196(14) 0.00019(14) -0.00228(14) S3 0.0334(4) 0.0335(4) 0.0268(3) -0.0015(2) 0.0011(2) 0.0033(3) S2 0.0201(6) 0.0279(6) 0.0304(4) 0.0048(5) -0.0036(5) -0.0029(5) S1 0.0338(8) 0.0199(3) 0.0377(7) -0.0007(4) 0.0070(6) -0.0033(5) N2 0.033(3) 0.037(3) 0.027(3) 0.001(2) -0.001(2) 0.007(2) N3 0.028(3) 0.028(3) 0.035(3) 0.002(2) -0.002(2) 0.006(2) N4 0.032(3) 0.034(3) 0.027(3) -0.002(2) -0.005(2) 0.004(2) N1 0.027(3) 0.035(3) 0.070(5) -0.017(3) 0.007(3) -0.002(2) N5 0.030(3) 0.026(3) 0.029(3) -0.003(2) -0.007(2) 0.008(2) C1 0.046(4) 0.037(4) 0.030(3) -0.012(3) -0.008(3) 0.009(3) C4 0.028(3) 0.033(3) 0.045(4) -0.003(3) -0.003(3) -0.005(3) C6 0.029(3) 0.053(4) 0.047(4) 0.008(4) 0.003(3) -0.002(3) C8 0.044(4) 0.050(4) 0.035(4) 0.012(3) 0.004(3) 0.002(3) C2 0.036(3) 0.040(4) 0.036(4) -0.002(3) -0.011(3) 0.009(3) C5 0.047(4) 0.026(3) 0.040(4) 0.000(3) -0.006(3) -0.001(3) C3 0.049(4) 0.044(4) 0.026(3) -0.009(3) 0.000(3) 0.015(3) C7 0.027(3) 0.036(4) 0.048(4) 0.002(3) -0.007(3) 0.009(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 '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' Sb Sb -0.5866 1.5461 '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 N2 Zn1 S3 90.91(15) . . ? N2 Zn1 N3 76.7(2) . . ? N2 Zn1 N5 78.2(2) . . ? N3 Zn1 S3 81.63(14) . . ? N4 Zn1 S3 111.83(15) . . ? N4 Zn1 N2 141.7(2) . . ? N4 Zn1 N3 76.7(2) . . ? N4 Zn1 N5 87.8(2) . . ? N1 Zn1 S3 90.52(16) . . ? N1 Zn1 N2 115.3(2) . . ? N1 Zn1 N3 165.9(2) . . ? N1 Zn1 N4 95.6(2) . . ? N1 Zn1 N5 77.4(2) . . ? N5 Zn1 S3 158.10(14) . . ? N5 Zn1 N3 113.6(2) . . ? S3 Sb1 S2 110.11(6) . 9_556 ? S3 Sb1 S2 110.59(6) . . ? S2 Sb1 S2 94.00(5) 9_556 . ? S1 Sb1 S3 119.10(6) . . ? S1 Sb1 S2 108.69(6) . 9_556 ? S1 Sb1 S2 111.45(6) . . ? Sb1 S3 Zn1 111.85(7) . . ? Sb1 S2 Sb1 86.00(5) 9_556 . ? Zn1 N2 H2 108.1 . . ? C8 N2 Zn1 110.3(4) . . ? C8 N2 H2 108.1 . . ? C8 N2 C3 112.3(6) . . ? C3 N2 Zn1 110.0(4) . . ? C3 N2 H2 108.1 . . ? Zn1 N3 H3 105.2 . . ? C6 N3 Zn1 112.8(4) . . ? C6 N3 H3 105.2 . . ? C7 N3 Zn1 111.4(4) . . ? C7 N3 H3 105.2 . . ? C7 N3 C6 115.9(5) . . ? Zn1 N4 H4A 108.9 . . ? Zn1 N4 H4B 108.9 . . ? H4A N4 H4B 107.7 . . ? C2 N4 Zn1 113.3(4) . . ? C2 N4 H4A 108.9 . . ? C2 N4 H4B 108.9 . . ? Zn1 N1 H1A 91.5 . . ? Zn1 N1 H1B 18.3 . . ? Zn1 N1 H1C 120.8 . . ? H1A N1 H1B 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C4 N1 Zn1 114.3(4) . . ? C4 N1 H1A 109.5 . . ? C4 N1 H1B 109.5 . . ? C4 N1 H1C 109.5 . . ? Zn1 N5 H5 108.8 . . ? C1 N5 Zn1 108.6(4) . . ? C1 N5 H5 108.8 . . ? C5 N5 Zn1 108.8(4) . . ? C5 N5 H5 108.8 . . ? C5 N5 C1 112.9(5) . . ? N5 C1 H1D 109.8 . . ? N5 C1 H1E 109.8 . . ? N5 C1 C3 109.3(6) . . ? H1D C1 H1E 108.3 . . ? C3 C1 H1D 109.8 . . ? C3 C1 H1E 109.8 . . ? N1 C4 H4C 110.2 . . ? N1 C4 H4D 110.2 . . ? N1 C4 C5 107.7(5) . . ? H4C C4 H4D 108.5 . . ? C5 C4 H4C 110.2 . . ? C5 C4 H4D 110.2 . . ? N3 C6 H6A 109.9 . . ? N3 C6 H6B 109.9 . . ? N3 C6 C8 109.0(6) . . ? H6A C6 H6B 108.3 . . ? C8 C6 H6A 109.9 . . ? C8 C6 H6B 109.9 . . ? N2 C8 C6 109.6(6) . . ? N2 C8 H8A 109.7 . . ? N2 C8 H8B 109.7 . . ? C6 C8 H8A 109.7 . . ? C6 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? N4 C2 H2A 109.9 . . ? N4 C2 H2B 109.9 . . ? N4 C2 C7 108.7(5) . . ? H2A C2 H2B 108.3 . . ? C7 C2 H2A 109.9 . . ? C7 C2 H2B 109.9 . . ? N5 C5 C4 109.1(5) . . ? N5 C5 H5A 109.9 . . ? N5 C5 H5B 109.9 . . ? C4 C5 H5A 109.9 . . ? C4 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? N2 C3 C1 108.2(5) . . ? N2 C3 H3A 110.1 . . ? N2 C3 H3B 110.1 . . ? C1 C3 H3A 110.1 . . ? C1 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? N3 C7 C2 109.0(5) . . ? N3 C7 H7A 109.9 . . ? N3 C7 H7B 109.9 . . ? C2 C7 H7A 109.9 . . ? C2 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? 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 Zn1 S3 2.5821(18) . ? Zn1 N2 2.193(5) . ? Zn1 N3 2.237(5) . ? Zn1 N4 2.164(5) . ? Zn1 N1 2.147(6) . ? Zn1 N5 2.234(5) . ? Sb1 S3 2.3549(17) . ? Sb1 S2 2.4554(15) 9_556 ? Sb1 S2 2.4587(15) . ? Sb1 S1 2.3144(15) . ? N2 H2 0.9800 . ? N2 C8 1.473(9) . ? N2 C3 1.483(8) . ? N3 H3 0.9800 . ? N3 C6 1.464(9) . ? N3 C7 1.453(8) . ? N4 H4A 0.8900 . ? N4 H4B 0.8900 . ? N4 C2 1.470(9) . ? N1 H1A 0.8900 . ? N1 H1B 0.8900 . ? N1 H1C 0.8900 . ? N1 C4 1.458(8) . ? N5 H5 0.9800 . ? N5 C1 1.470(8) . ? N5 C5 1.466(9) . ? C1 H1D 0.9700 . ? C1 H1E 0.9700 . ? C1 C3 1.504(11) . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C4 C5 1.525(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C8 1.508(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C7 1.517(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Zn1 N2 C8 C6 45.9(7) . . . . ? Zn1 N2 C3 C1 42.5(6) . . . . ? Zn1 N3 C6 C8 31.3(7) . . . . ? Zn1 N3 C7 C2 -38.7(6) . . . . ? Zn1 N4 C2 C7 -38.9(6) . . . . ? Zn1 N1 C4 C5 36.7(7) . . . . ? Zn1 N5 C1 C3 42.2(6) . . . . ? Zn1 N5 C5 C4 43.2(6) . . . . ? N3 C6 C8 N2 -50.9(8) . . . . ? N4 C2 C7 N3 50.8(7) . . . . ? N1 C4 C5 N5 -52.7(8) . . . . ? N5 C1 C3 N2 -57.1(7) . . . . ? C1 N5 C5 C4 -77.5(7) . . . . ? C6 N3 C7 C2 -169.5(6) . . . . ? C8 N2 C3 C1 165.7(6) . . . . ? C5 N5 C1 C3 163.0(5) . . . . ? C3 N2 C8 C6 -77.1(7) . . . . ? C7 N3 C6 C8 161.4(6) . . . . ?