#------------------------------------------------------------------------------ #$Date: 2019-03-20 04:50:01 +0200 (Wed, 20 Mar 2019) $ #$Revision: 214211 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/25/7232522.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_7232522 loop_ _publ_author_name 'Jeong, Haewon' 'Kang, Yeji' 'Kim, Jin' 'Kim, Byung-Kwon' 'Hong, Seungwoo' _publ_section_title ; Factors that determine thione(thiol)--disulfide interconversion in a bis(thiosemicarbazone) copper(ii) complex ; _journal_issue 16 _journal_name_full 'RSC Advances' _journal_page_first 9049 _journal_paper_doi 10.1039/C9RA01115C _journal_volume 9 _journal_year 2019 _chemical_formula_moiety 'C25 H38 N14 O3 S4 Zn2' _chemical_formula_sum 'C25 H38 N14 O3 S4 Zn2' _chemical_formula_weight 841.67 _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' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2019-02-07 deposited with the CCDC. 2019-03-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.166(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.697(3) _cell_length_b 14.759(3) _cell_length_c 18.746(4) _cell_measurement_reflns_used 43448 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 25.009 _cell_measurement_theta_min 1.796 _cell_volume 3579.5(13) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_unetI/netI 0.0411 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 43448 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.009 _diffrn_reflns_theta_max 25.009 _diffrn_reflns_theta_min 1.796 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description platy _exptl_crystal_F_000 1736 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_transmission_factor_max 0.745 _exptl_transmission_factor_min 0.658 _refine_diff_density_max 0.752 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.085 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 473 _refine_ls_number_reflns 6296 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0361 _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^)+(0.0449P)^2^+3.9304P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.0916 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4843 _reflns_number_total 6296 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ra01115c2.cif _cod_data_source_block pre1_a _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_original_cell_volume 3579.5(14) _cod_database_code 7232522 _shelx_shelxl_version_number 2016/6 _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_res_file ; TITL pre1_a.res in P2(1)/c pre1_a.res created by SHELXL-2016/6 at 15:16:22 on 07-Jan-2019 CELL 0.71073 13.697 14.7588 18.7459 90 109.166 90 ZERR 4 0.003 0.0032 0.0041 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N S Zn O UNIT 100 152 56 16 8 12 L.S. 10 ACTA BOND $H FMAP 2 PLAN 1 BUMP CONF HTAB O3 N9_$8 HTAB O2 S3_$6 HTAB N13 S2_$7 HTAB N10 O3_$6 HTAB N10 O3_$5 HTAB N10 S1_$4 HTAB N6 O1_$3 HTAB N6 N2_$1 HTAB N3 N5_$2 HTAB N3 O3_$1 HTAB O1 O2 HTAB N13 O1 EQIV $8 X, Y, Z+1 EQIV $7 -X, Y+0.5, -Z+0.5 EQIV $6 -X+1, -Y+1, -Z+1 EQIV $5 X, Y, Z-1 EQIV $4 -X+1, Y+0.5, -Z+0.5 EQIV $3 -X, Y-0.5, -Z+0.5 EQIV $2 X, -Y+0.5, Z+0.5 EQIV $1 X, -Y+0.5, Z-0.5 TEMP -153 WGHT 0.044900 3.930400 FVAR 0.25082 ZN1 5 0.206129 0.325551 0.249438 11.00000 0.01966 0.02776 = 0.00734 0.00190 0.00620 0.00120 ZN2 5 0.344964 0.550397 0.286008 11.00000 0.02337 0.02764 = 0.00940 0.00171 0.00705 0.00455 S1 4 0.271924 0.187855 0.316165 11.00000 0.02226 0.02221 = 0.01114 0.00041 0.00963 0.00036 S2 4 0.055947 0.286883 0.146366 11.00000 0.01910 0.03863 = 0.01103 -0.00192 0.00625 -0.00455 S3 4 0.506189 0.566431 0.270309 11.00000 0.02209 0.02348 = 0.01479 -0.00099 0.00619 -0.00221 S4 4 0.266826 0.683534 0.309313 11.00000 0.03589 0.02385 = 0.01673 0.00326 0.01219 0.00750 N1 3 0.165855 0.350665 0.345476 11.00000 0.01592 0.01822 = 0.00823 0.00258 0.00256 -0.00091 N2 3 0.189096 0.290500 0.405031 11.00000 0.02413 0.01648 = 0.00824 0.00300 0.00641 0.00093 N3 3 0.265219 0.157751 0.453041 11.00000 0.03698 0.02205 = 0.01108 0.00300 0.01265 0.00689 N4 3 0.279899 0.317269 0.168831 11.00000 0.01798 0.01425 = 0.01000 -0.00014 0.00492 -0.00030 N5 3 0.222509 0.300193 0.093969 11.00000 0.01858 0.01822 = 0.00667 -0.00060 0.00358 -0.00119 N6 3 0.066608 0.262224 0.009395 11.00000 0.02003 0.02953 = 0.01192 -0.00136 0.00454 -0.00060 N7 3 0.148404 0.477104 0.238376 11.00000 0.01618 0.01893 = 0.01128 0.00124 0.00354 -0.00032 N8 3 0.291475 0.528467 0.170337 11.00000 0.02171 0.01541 = 0.01192 0.00202 0.00864 -0.00153 N9 3 0.361533 0.530006 0.131199 11.00000 0.02208 0.02294 = 0.01520 -0.00043 0.01157 -0.00411 N10 3 0.529101 0.540887 0.137272 11.00000 0.02747 0.04131 = 0.02402 -0.01072 0.01647 -0.01405 N11 3 0.342281 0.511021 0.390738 11.00000 0.01811 0.01897 = 0.01085 -0.00405 0.00466 -0.00385 N12 3 0.289412 0.564302 0.427105 11.00000 0.02206 0.02154 = 0.01298 -0.00359 0.00748 0.00215 N13 3 0.199803 0.693500 0.426165 11.00000 0.03099 0.03041 = 0.02011 -0.00228 0.01282 0.00789 N14 3 0.391749 0.377589 0.308798 11.00000 0.01946 0.01591 = 0.01247 0.00046 0.00663 -0.00285 O1 6 0.147010 0.660535 0.569678 11.00000 0.03537 0.03408 = 0.01937 -0.00138 0.00966 0.00451 O2 6 0.260413 0.513671 0.632831 11.00000 0.05081 0.03530 = 0.06637 0.00283 0.00314 0.00403 O3 6 0.365901 0.520057 0.981011 11.00000 0.03982 0.02397 = 0.02033 -0.00089 0.01660 -0.00291 C1 1 0.239687 0.216762 0.395227 11.00000 0.01671 0.01843 = 0.00808 -0.00087 0.00376 -0.00605 C2 1 0.122971 0.283681 0.082058 11.00000 0.01998 0.01537 = 0.01026 0.00070 0.00377 -0.00142 C3 1 0.434925 0.301419 0.130200 11.00000 0.02385 0.02562 = 0.01556 -0.00043 0.00995 -0.00180 AFIX 137 H3C 2 0.411174 0.244180 0.103683 11.00000 -1.50000 H3D 2 0.509453 0.298074 0.157038 11.00000 -1.50000 H3E 2 0.420544 0.351154 0.093565 11.00000 -1.50000 AFIX 0 C4 1 0.378994 0.318092 0.186003 11.00000 0.02157 0.01127 = 0.01346 0.00022 0.00891 -0.00081 C5 1 0.439436 0.330845 0.267128 11.00000 0.02028 0.01382 = 0.01570 0.00052 0.00738 -0.00198 C6 1 0.535680 0.291090 0.299570 11.00000 0.01801 0.02144 = 0.02307 -0.00660 0.00335 -0.00032 AFIX 43 H6 2 0.569462 0.262439 0.268741 11.00000 -1.20000 AFIX 0 C7 1 0.581886 0.293499 0.376896 11.00000 0.02362 0.02760 = 0.02566 -0.00558 -0.00071 0.00729 AFIX 43 H7 2 0.646505 0.264566 0.400166 11.00000 -1.20000 AFIX 0 C8 1 0.532359 0.338980 0.420290 11.00000 0.02816 0.02376 = 0.01498 -0.00369 -0.00196 0.00089 AFIX 43 H8 2 0.561689 0.340106 0.473777 11.00000 -1.20000 AFIX 0 C9 1 0.439465 0.382694 0.384315 11.00000 0.02083 0.01709 = 0.01394 -0.00098 0.00371 -0.00415 C10 1 0.389050 0.440334 0.426317 11.00000 0.01530 0.01741 = 0.01203 -0.00013 0.00120 -0.00410 C11 1 0.393760 0.415766 0.505250 11.00000 0.02856 0.02120 = 0.01156 0.00109 0.00563 -0.00200 AFIX 137 H11A 2 0.387366 0.470792 0.532642 11.00000 -1.50000 H11B 2 0.459954 0.386246 0.531413 11.00000 -1.50000 H11C 2 0.337030 0.374253 0.503123 11.00000 -1.50000 AFIX 0 C12 1 0.458688 0.544414 0.173270 11.00000 0.02354 0.01648 = 0.01677 -0.00185 0.00984 -0.00561 C13 1 0.252372 0.640691 0.391767 11.00000 0.01827 0.02433 = 0.01415 -0.00156 0.00343 -0.00207 C14 1 0.154939 0.530875 0.045613 11.00000 0.02750 0.03877 = 0.01321 0.00179 0.00529 -0.00157 AFIX 137 H14A 2 0.183318 0.584660 0.028835 11.00000 -1.50000 H14B 2 0.079307 0.534497 0.027866 11.00000 -1.50000 H14C 2 0.176548 0.476431 0.024849 11.00000 -1.50000 AFIX 0 C15 1 0.194279 0.526330 0.130431 11.00000 0.02433 0.01426 = 0.01468 0.00097 0.00619 -0.00004 C16 1 0.120909 0.525787 0.173814 11.00000 0.02135 0.01877 = 0.01502 0.00514 0.00574 0.00015 C17 1 0.033528 0.579219 0.151241 11.00000 0.03235 0.04236 = 0.02905 0.02115 0.01433 0.01533 AFIX 43 H17 2 0.012954 0.608819 0.103603 11.00000 -1.20000 AFIX 0 C18 1 -0.023672 0.588786 0.199653 11.00000 0.04255 0.06930 = 0.05032 0.03673 0.02941 0.03498 AFIX 43 H18 2 -0.082880 0.626846 0.186183 11.00000 -1.20000 AFIX 0 C19 1 0.005718 0.542966 0.267148 11.00000 0.03679 0.06088 = 0.04024 0.02535 0.02760 0.02517 AFIX 43 H19 2 -0.030937 0.550934 0.301816 11.00000 -1.20000 AFIX 0 C20 1 0.090356 0.484488 0.283956 11.00000 0.01893 0.02551 = 0.01714 0.00339 0.00764 0.00287 C21 1 0.116369 0.423669 0.350588 11.00000 0.01265 0.02390 = 0.01549 0.00240 0.00514 0.00048 C22 1 0.082606 0.447183 0.416888 11.00000 0.02982 0.02241 = 0.02297 0.00351 0.01518 0.00508 AFIX 137 H22A 2 0.016584 0.417396 0.411383 11.00000 -1.50000 H22B 2 0.074285 0.512979 0.418972 11.00000 -1.50000 H22C 2 0.134921 0.426516 0.463564 11.00000 -1.50000 AFIX 0 C23 1 0.160928 0.710979 0.636910 11.00000 0.03855 0.04091 = 0.03000 -0.01113 0.00595 0.00322 AFIX 137 H23A 2 0.215827 0.683167 0.678679 11.00000 -1.50000 H23B 2 0.096336 0.711144 0.648722 11.00000 -1.50000 H23C 2 0.180216 0.773399 0.629674 11.00000 -1.50000 AFIX 0 C24 1 0.212624 0.430531 0.631832 11.00000 0.04732 0.04146 = 0.02990 0.00693 0.01458 0.00094 AFIX 137 H24A 2 0.221818 0.411523 0.683724 11.00000 -1.50000 H24B 2 0.243621 0.385350 0.607487 11.00000 -1.50000 H24C 2 0.138690 0.436016 0.603579 11.00000 -1.50000 AFIX 0 C25 1 0.326186 0.598116 0.935273 11.00000 0.12790 0.04994 = 0.07808 0.03055 0.07666 0.03507 AFIX 137 H25A 2 0.350197 0.653108 0.965196 11.00000 -1.50000 H25B 2 0.250467 0.596425 0.917634 11.00000 -1.50000 H25C 2 0.350723 0.598216 0.891700 11.00000 -1.50000 AFIX 0 H3A 2 0.298689 0.108463 0.451734 11.00000 -1.20000 H3B 2 0.248551 0.169923 0.494608 11.00000 -1.20000 H6A 2 0.102943 0.247264 -0.018897 11.00000 -1.20000 H6B 2 0.003148 0.242045 0.001151 11.00000 -1.20000 H10A 2 0.592266 0.563854 0.157774 11.00000 -1.20000 H10B 2 0.505527 0.537400 0.084041 11.00000 -1.20000 H13A 2 0.183530 0.674031 0.461974 11.00000 -1.20000 H13B 2 0.159956 0.741493 0.396245 11.00000 -1.20000 H1S 2 0.176050 0.605089 0.579922 11.00000 -1.20000 H2S 2 0.337617 0.503956 0.664433 11.00000 -1.20000 H3S 2 0.352651 0.521620 1.019451 11.00000 -1.20000 HKLF 4 REM pre1_a.res in P2(1)/c REM R1 = 0.0361 for 4843 Fo > 4sig(Fo) and 0.0581 for all 6296 data REM 473 parameters refined using 2 restraints END WGHT 0.0452 3.9697 REM Highest difference peak 0.752, deepest hole -0.520, 1-sigma level 0.085 Q1 1 0.1765 0.5760 0.8214 11.00000 0.05 0.75 ; _shelx_res_checksum 36879 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 Zn1 Zn 0.20613(3) 0.32555(3) 0.24944(2) 0.01782(11) Uani 1 1 d . . Zn2 Zn 0.34496(3) 0.55040(3) 0.28601(2) 0.01972(12) Uani 1 1 d . . S1 S 0.27192(7) 0.18786(6) 0.31617(4) 0.01752(19) Uani 1 1 d . . S2 S 0.05595(7) 0.28688(7) 0.14637(4) 0.0226(2) Uani 1 1 d . . S3 S 0.50619(7) 0.56643(6) 0.27031(5) 0.0201(2) Uani 1 1 d . . S4 S 0.26683(8) 0.68353(6) 0.30931(5) 0.0246(2) Uani 1 1 d . . N1 N 0.1659(2) 0.35066(18) 0.34548(14) 0.0145(6) Uani 1 1 d . . N2 N 0.1891(2) 0.29050(18) 0.40503(14) 0.0160(6) Uani 1 1 d . . N3 N 0.2652(3) 0.1578(2) 0.45304(16) 0.0222(7) Uani 1 1 d . . N4 N 0.2799(2) 0.31727(18) 0.16883(14) 0.0140(6) Uani 1 1 d . . N5 N 0.2225(2) 0.30019(18) 0.09397(14) 0.0146(6) Uani 1 1 d . . N6 N 0.0666(2) 0.2622(2) 0.00940(15) 0.0207(7) Uani 1 1 d . . N7 N 0.1484(2) 0.47710(18) 0.23838(14) 0.0157(6) Uani 1 1 d . . N8 N 0.2915(2) 0.52847(18) 0.17034(14) 0.0156(6) Uani 1 1 d . . N9 N 0.3615(2) 0.53001(19) 0.13120(15) 0.0187(6) Uani 1 1 d . . N10 N 0.5291(3) 0.5409(2) 0.13727(18) 0.0290(8) Uani 1 1 d . . N11 N 0.3423(2) 0.51102(19) 0.39074(14) 0.0160(6) Uani 1 1 d . . N12 N 0.2894(2) 0.56430(19) 0.42710(15) 0.0184(6) Uani 1 1 d . . N13 N 0.1998(3) 0.6935(2) 0.42617(17) 0.0261(7) Uani 1 1 d . . N14 N 0.3917(2) 0.37759(18) 0.30880(14) 0.0156(6) Uani 1 1 d . . O1 O 0.1470(2) 0.66053(18) 0.56968(13) 0.0294(6) Uani 1 1 d . . O2 O 0.2604(3) 0.5137(2) 0.6328(2) 0.0548(9) Uani 1 1 d . . O3 O 0.3659(2) 0.52006(17) 0.98101(13) 0.0264(6) Uani 1 1 d . . C1 C 0.2397(2) 0.2168(2) 0.39523(16) 0.0145(7) Uani 1 1 d . . C2 C 0.1230(3) 0.2837(2) 0.08206(17) 0.0155(7) Uani 1 1 d . . C3 C 0.4349(3) 0.3014(2) 0.13020(18) 0.0208(8) Uani 1 1 d . . H3C H 0.411174 0.244180 0.103683 0.031 Uiso 1 1 calc R U H3D H 0.509453 0.298074 0.157038 0.031 Uiso 1 1 calc R U H3E H 0.420544 0.351154 0.093565 0.031 Uiso 1 1 calc R U C4 C 0.3790(3) 0.3181(2) 0.18600(17) 0.0147(7) Uani 1 1 d . . C5 C 0.4394(3) 0.3308(2) 0.26713(18) 0.0162(7) Uani 1 1 d . . C6 C 0.5357(3) 0.2911(2) 0.29957(19) 0.0217(8) Uani 1 1 d . . H6 H 0.569462 0.262439 0.268741 0.026 Uiso 1 1 calc R U C7 C 0.5819(3) 0.2935(3) 0.3769(2) 0.0278(9) Uani 1 1 d . . H7 H 0.646505 0.264566 0.400166 0.033 Uiso 1 1 calc R U C8 C 0.5324(3) 0.3390(2) 0.42029(19) 0.0245(8) Uani 1 1 d . . H8 H 0.561689 0.340106 0.473777 0.029 Uiso 1 1 calc R U C9 C 0.4395(3) 0.3827(2) 0.38432(18) 0.0178(7) Uani 1 1 d . . C10 C 0.3891(2) 0.4403(2) 0.42632(17) 0.0157(7) Uani 1 1 d . . C11 C 0.3938(3) 0.4158(2) 0.50525(17) 0.0207(8) Uani 1 1 d . . H11A H 0.387366 0.470792 0.532642 0.031 Uiso 1 1 calc R U H11B H 0.459954 0.386246 0.531413 0.031 Uiso 1 1 calc R U H11C H 0.337030 0.374253 0.503123 0.031 Uiso 1 1 calc R U C12 C 0.4587(3) 0.5444(2) 0.17327(18) 0.0181(7) Uani 1 1 d . . C13 C 0.2524(3) 0.6407(2) 0.39177(18) 0.0194(8) Uani 1 1 d . . C14 C 0.1549(3) 0.5309(3) 0.04561(18) 0.0268(9) Uani 1 1 d . . H14A H 0.183318 0.584660 0.028835 0.040 Uiso 1 1 calc R U H14B H 0.079307 0.534497 0.027866 0.040 Uiso 1 1 calc R U H14C H 0.176548 0.476431 0.024849 0.040 Uiso 1 1 calc R U C15 C 0.1943(3) 0.5263(2) 0.13043(18) 0.0178(7) Uani 1 1 d . . C16 C 0.1209(3) 0.5258(2) 0.17381(18) 0.0184(8) Uani 1 1 d . . C17 C 0.0335(3) 0.5792(3) 0.1512(2) 0.0335(10) Uani 1 1 d . . H17 H 0.012954 0.608819 0.103603 0.040 Uiso 1 1 calc R U C18 C -0.0237(4) 0.5888(3) 0.1997(3) 0.0506(13) Uani 1 1 d . . H18 H -0.082880 0.626846 0.186183 0.061 Uiso 1 1 calc R U C19 C 0.0057(3) 0.5430(3) 0.2671(2) 0.0423(12) Uani 1 1 d . . H19 H -0.030937 0.550934 0.301816 0.051 Uiso 1 1 calc R U C20 C 0.0904(3) 0.4845(2) 0.28396(18) 0.0201(8) Uani 1 1 d . . C21 C 0.1164(3) 0.4237(2) 0.35059(18) 0.0172(7) Uani 1 1 d . . C22 C 0.0826(3) 0.4472(2) 0.41689(19) 0.0235(8) Uani 1 1 d . . H22A H 0.016584 0.417396 0.411383 0.035 Uiso 1 1 calc R U H22B H 0.074285 0.512979 0.418972 0.035 Uiso 1 1 calc R U H22C H 0.134921 0.426516 0.463564 0.035 Uiso 1 1 calc R U C23 C 0.1609(3) 0.7110(3) 0.6369(2) 0.0378(10) Uani 1 1 d . . H23A H 0.215827 0.683167 0.678679 0.057 Uiso 1 1 calc R U H23B H 0.096336 0.711144 0.648722 0.057 Uiso 1 1 calc R U H23C H 0.180216 0.773399 0.629674 0.057 Uiso 1 1 calc R U C24 C 0.2126(3) 0.4305(3) 0.6318(2) 0.0391(10) Uani 1 1 d . . H24A H 0.221818 0.411523 0.683724 0.059 Uiso 1 1 calc R U H24B H 0.243621 0.385350 0.607487 0.059 Uiso 1 1 calc R U H24C H 0.138690 0.436016 0.603579 0.059 Uiso 1 1 calc R U C25 C 0.3262(5) 0.5981(3) 0.9353(3) 0.0748(19) Uani 1 1 d . . H25A H 0.350197 0.653108 0.965196 0.112 Uiso 1 1 calc R U H25B H 0.250467 0.596425 0.917634 0.112 Uiso 1 1 calc R U H25C H 0.350723 0.598216 0.891700 0.112 Uiso 1 1 calc R U H3A H 0.299(4) 0.108(4) 0.452(3) 0.090 Uiso 1 1 d . U H3B H 0.249(4) 0.170(4) 0.495(3) 0.090 Uiso 1 1 d . U H6A H 0.103(4) 0.247(4) -0.019(3) 0.090 Uiso 1 1 d . U H6B H 0.003(5) 0.242(4) 0.001(3) 0.090 Uiso 1 1 d . U H10A H 0.592(5) 0.564(4) 0.158(3) 0.090 Uiso 1 1 d . U H10B H 0.506(4) 0.537(4) 0.084(3) 0.090 Uiso 1 1 d . U H13A H 0.184(5) 0.674(4) 0.462(3) 0.090 Uiso 1 1 d . U H13B H 0.160(4) 0.741(4) 0.396(3) 0.090 Uiso 1 1 d . U H1S H 0.176(4) 0.605(3) 0.580(2) 0.090 Uiso 1 1 d . U H2S H 0.338(5) 0.504(4) 0.664(3) 0.090 Uiso 1 1 d . U H3S H 0.353(5) 0.522(4) 1.019(3) 0.090 Uiso 1 1 d . U 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 0.0197(2) 0.0278(2) 0.00734(18) 0.00190(16) 0.00620(16) 0.00120(18) Zn2 0.0234(2) 0.0276(2) 0.00940(19) 0.00171(16) 0.00705(16) 0.00455(19) S1 0.0223(5) 0.0222(5) 0.0111(4) 0.0004(3) 0.0096(3) 0.0004(4) S2 0.0191(5) 0.0386(5) 0.0110(4) -0.0019(4) 0.0063(3) -0.0045(4) S3 0.0221(5) 0.0235(5) 0.0148(4) -0.0010(4) 0.0062(4) -0.0022(4) S4 0.0359(6) 0.0238(5) 0.0167(4) 0.0033(4) 0.0122(4) 0.0075(4) N1 0.0159(15) 0.0182(15) 0.0082(13) 0.0026(11) 0.0026(11) -0.0009(12) N2 0.0241(16) 0.0165(15) 0.0082(13) 0.0030(11) 0.0064(12) 0.0009(13) N3 0.0370(19) 0.0220(17) 0.0111(14) 0.0030(12) 0.0127(13) 0.0069(14) N4 0.0180(16) 0.0143(14) 0.0100(13) -0.0001(11) 0.0049(11) -0.0003(12) N5 0.0186(16) 0.0182(15) 0.0067(12) -0.0006(11) 0.0036(11) -0.0012(12) N6 0.0200(17) 0.0295(18) 0.0119(14) -0.0014(13) 0.0045(12) -0.0006(14) N7 0.0162(15) 0.0189(15) 0.0113(13) 0.0012(11) 0.0035(11) -0.0003(12) N8 0.0217(16) 0.0154(15) 0.0119(13) 0.0020(11) 0.0086(12) -0.0015(12) N9 0.0221(16) 0.0229(16) 0.0152(14) -0.0004(12) 0.0116(13) -0.0041(13) N10 0.0275(19) 0.041(2) 0.0240(17) -0.0107(15) 0.0165(15) -0.0141(16) N11 0.0181(15) 0.0190(15) 0.0109(13) -0.0041(12) 0.0047(12) -0.0038(13) N12 0.0221(16) 0.0215(16) 0.0130(13) -0.0036(12) 0.0075(12) 0.0021(13) N13 0.0310(19) 0.0304(19) 0.0201(16) -0.0023(14) 0.0128(14) 0.0079(15) N14 0.0195(15) 0.0159(15) 0.0125(13) 0.0005(11) 0.0066(12) -0.0029(12) O1 0.0354(16) 0.0341(15) 0.0194(13) -0.0014(11) 0.0097(12) 0.0045(13) O2 0.051(2) 0.0353(18) 0.066(2) 0.0028(16) 0.0031(18) 0.0040(17) O3 0.0398(16) 0.0240(14) 0.0203(13) -0.0009(11) 0.0166(12) -0.0029(12) C1 0.0167(18) 0.0184(18) 0.0081(15) -0.0009(13) 0.0038(13) -0.0061(15) C2 0.0200(19) 0.0154(17) 0.0103(15) 0.0007(13) 0.0038(14) -0.0014(15) C3 0.024(2) 0.026(2) 0.0156(16) -0.0004(15) 0.0099(15) -0.0018(16) C4 0.0216(19) 0.0113(16) 0.0135(15) 0.0002(13) 0.0089(14) -0.0008(15) C5 0.0203(18) 0.0138(17) 0.0157(16) 0.0005(14) 0.0074(14) -0.0020(15) C6 0.0180(19) 0.0214(19) 0.0231(18) -0.0066(15) 0.0033(15) -0.0003(16) C7 0.024(2) 0.028(2) 0.0257(19) -0.0056(17) -0.0007(16) 0.0073(17) C8 0.028(2) 0.024(2) 0.0150(17) -0.0037(15) -0.0020(15) 0.0009(17) C9 0.0208(19) 0.0171(18) 0.0139(16) -0.0010(14) 0.0037(14) -0.0041(15) C10 0.0153(18) 0.0174(18) 0.0120(15) -0.0001(14) 0.0012(13) -0.0041(15) C11 0.029(2) 0.0212(19) 0.0116(16) 0.0011(14) 0.0056(15) -0.0020(16) C12 0.024(2) 0.0165(18) 0.0168(16) -0.0018(14) 0.0098(15) -0.0056(15) C13 0.0183(19) 0.024(2) 0.0142(16) -0.0016(15) 0.0034(14) -0.0021(16) C14 0.027(2) 0.039(2) 0.0132(17) 0.0018(16) 0.0053(15) -0.0016(18) C15 0.024(2) 0.0143(17) 0.0147(16) 0.0010(14) 0.0062(15) 0.0000(15) C16 0.0213(19) 0.0188(18) 0.0150(16) 0.0051(14) 0.0057(14) 0.0001(15) C17 0.032(2) 0.042(2) 0.029(2) 0.0212(19) 0.0143(18) 0.015(2) C18 0.043(3) 0.069(3) 0.050(3) 0.037(3) 0.029(2) 0.035(3) C19 0.037(3) 0.061(3) 0.040(2) 0.025(2) 0.028(2) 0.025(2) C20 0.0189(19) 0.0255(19) 0.0171(17) 0.0034(15) 0.0076(15) 0.0029(16) C21 0.0127(17) 0.0239(19) 0.0155(16) 0.0024(14) 0.0051(14) 0.0005(15) C22 0.030(2) 0.0224(19) 0.0230(18) 0.0035(15) 0.0152(16) 0.0051(17) C23 0.039(3) 0.041(3) 0.030(2) -0.0111(19) 0.0060(19) 0.003(2) C24 0.047(3) 0.041(3) 0.030(2) 0.0069(19) 0.015(2) 0.001(2) C25 0.128(5) 0.050(3) 0.078(4) 0.031(3) 0.077(4) 0.035(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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 N4 Zn1 N1 165.69(10) N4 Zn1 N7 102.75(10) N1 Zn1 N7 74.39(10) N4 Zn1 S2 83.84(8) N1 Zn1 S2 109.90(8) N7 Zn1 S2 88.89(7) N4 Zn1 S1 98.05(8) N1 Zn1 S1 82.00(8) N7 Zn1 S1 154.95(7) S2 Zn1 S1 107.22(4) N11 Zn2 N8 147.36(11) N11 Zn2 S3 117.56(8) N8 Zn2 S3 84.73(8) N11 Zn2 S4 84.65(8) N8 Zn2 S4 107.41(8) S3 Zn2 S4 116.55(4) C1 S1 Zn1 94.57(12) C2 S2 Zn1 93.26(11) C12 S3 Zn2 93.90(12) C13 S4 Zn2 93.03(12) C21 N1 N2 117.6(3) C21 N1 Zn1 120.4(2) N2 N1 Zn1 121.9(2) C1 N2 N1 113.9(2) C1 N3 H3A 121(4) C1 N3 H3B 120(4) H3A N3 H3B 119(5) C4 N4 N5 117.1(3) C4 N4 Zn1 122.8(2) N5 N4 Zn1 119.8(2) C2 N5 N4 114.3(2) C2 N6 H6A 115(4) C2 N6 H6B 117(4) H6A N6 H6B 122(5) C20 N7 C16 118.4(3) C20 N7 Zn1 105.7(2) C16 N7 Zn1 124.8(2) C15 N8 N9 117.0(3) C15 N8 Zn2 123.4(2) N9 N8 Zn2 118.8(2) C12 N9 N8 115.0(3) C12 N10 H10A 122(4) C12 N10 H10B 119(3) H10A N10 H10B 115(5) C10 N11 N12 117.0(3) C10 N11 Zn2 124.1(2) N12 N11 Zn2 118.9(2) C13 N12 N11 114.4(3) C13 N13 H13A 121(4) C13 N13 H13B 116(3) H13A N13 H13B 119(5) C9 N14 C5 118.1(3) C23 O1 H1S 111.4(18) C24 O2 H2S 106(3) C25 O3 H3S 111(4) N2 C1 N3 115.3(3) N2 C1 S1 127.4(2) N3 C1 S1 117.3(3) N5 C2 N6 115.0(3) N5 C2 S2 128.6(2) N6 C2 S2 116.4(3) C4 C3 H3C 109.5 C4 C3 H3D 109.5 H3C C3 H3D 109.5 C4 C3 H3E 109.5 H3C C3 H3E 109.5 H3D C3 H3E 109.5 N4 C4 C5 116.4(3) N4 C4 C3 124.0(3) C5 C4 C3 119.5(3) N14 C5 C6 122.0(3) N14 C5 C4 116.2(3) C6 C5 C4 121.7(3) C7 C6 C5 119.5(3) C7 C6 H6 120.3 C5 C6 H6 120.3 C6 C7 C8 118.9(3) C6 C7 H7 120.5 C8 C7 H7 120.5 C9 C8 C7 119.0(3) C9 C8 H8 120.5 C7 C8 H8 120.5 N14 C9 C8 122.2(3) N14 C9 C10 116.1(3) C8 C9 C10 121.6(3) N11 C10 C9 115.5(3) N11 C10 C11 123.9(3) C9 C10 C11 120.6(3) C10 C11 H11A 109.5 C10 C11 H11B 109.5 H11A C11 H11B 109.5 C10 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 N9 C12 N10 116.1(3) N9 C12 S3 127.4(3) N10 C12 S3 116.4(3) N12 C13 N13 115.3(3) N12 C13 S4 128.2(3) N13 C13 S4 116.5(3) C15 C14 H14A 109.5 C15 C14 H14B 109.5 H14A C14 H14B 109.5 C15 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 N8 C15 C16 115.8(3) N8 C15 C14 123.6(3) C16 C15 C14 120.5(3) N7 C16 C17 122.5(3) N7 C16 C15 117.0(3) C17 C16 C15 120.3(3) C16 C17 C18 118.5(3) C16 C17 H17 120.7 C18 C17 H17 120.7 C19 C18 C17 119.7(4) C19 C18 H18 120.2 C17 C18 H18 120.2 C18 C19 C20 118.9(4) C18 C19 H19 120.6 C20 C19 H19 120.6 N7 C20 C19 121.7(3) N7 C20 C21 117.1(3) C19 C20 C21 121.1(3) N1 C21 C20 115.4(3) N1 C21 C22 124.4(3) C20 C21 C22 120.2(3) C21 C22 H22A 109.5 C21 C22 H22B 109.5 H22A C22 H22B 109.5 C21 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 O1 C23 H23A 109.5 O1 C23 H23B 109.5 H23A C23 H23B 109.5 O1 C23 H23C 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 O2 C24 H24A 109.5 O2 C24 H24B 109.5 H24A C24 H24B 109.5 O2 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 O3 C25 H25A 109.5 O3 C25 H25B 109.5 H25A C25 H25B 109.5 O3 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Zn1 N4 2.079(3) Zn1 N1 2.082(3) Zn1 N7 2.359(3) Zn1 S2 2.3834(10) Zn1 S1 2.4014(10) Zn2 N11 2.059(3) Zn2 N8 2.074(3) Zn2 S3 2.3336(11) Zn2 S4 2.3461(10) S1 C1 1.733(3) S2 C2 1.739(3) S3 C12 1.750(3) S4 C13 1.740(3) N1 C21 1.293(4) N1 N2 1.379(4) N2 C1 1.335(4) N3 C1 1.344(4) N3 H3A 0.86(6) N3 H3B 0.90(6) N4 C4 1.288(4) N4 N5 1.388(3) N5 C2 1.330(4) N6 C2 1.364(4) N6 H6A 0.87(6) N6 H6B 0.88(6) N7 C20 1.349(4) N7 C16 1.350(4) N8 C15 1.296(4) N8 N9 1.386(4) N9 C12 1.322(4) N10 C12 1.347(4) N10 H10A 0.89(6) N10 H10B 0.94(6) N11 C10 1.290(4) N11 N12 1.390(4) N12 C13 1.322(4) N13 C13 1.359(4) N13 H13A 0.83(6) N13 H13B 0.96(6) N14 C9 1.353(4) N14 C5 1.359(4) O1 C23 1.422(4) O1 H1S 0.90(5) O2 C24 1.388(5) O2 H2S 1.04(6) O3 C25 1.432(5) O3 H3S 0.80(6) C3 C4 1.506(4) C3 H3C 0.9800 C3 H3D 0.9800 C3 H3E 0.9800 C4 C5 1.486(4) C5 C6 1.388(5) C6 C7 1.379(5) C6 H6 0.9500 C7 C8 1.391(5) C7 H7 0.9500 C8 C9 1.388(5) C8 H8 0.9500 C9 C10 1.476(5) C10 C11 1.504(4) C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C14 C15 1.503(4) C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C15 C16 1.486(5) C16 C17 1.379(5) C17 C18 1.387(5) C17 H17 0.9500 C18 C19 1.373(6) C18 H18 0.9500 C19 C20 1.396(5) C19 H19 0.9500 C20 C21 1.483(5) C21 C22 1.502(4) C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3S N9 0.80(6) 2.06(6) 2.839(4) 164(6) 1_556 O2 H2S S3 1.04(6) 2.33(6) 3.332(4) 161(5) 3_666 N13 H13B S2 0.96(6) 2.88(6) 3.591(4) 132(4) 2 N10 H10B O3 0.94(6) 2.59(6) 3.144(4) 118(4) 3_666 N10 H10B O3 0.94(6) 2.24(6) 3.061(4) 145(5) 1_554 N10 H10A S1 0.89(6) 2.54(6) 3.366(3) 155(5) 2_655 N6 H6B O1 0.88(6) 2.38(6) 3.188(4) 153(5) 2_545 N6 H6A N2 0.87(6) 2.20(6) 3.066(4) 178(5) 4_565 N3 H3B N5 0.90(6) 2.06(6) 2.953(4) 176(5) 4_566 N3 H3A O3 0.86(6) 2.10(6) 2.931(4) 161(5) 4_565 O1 H1S O2 0.90(5) 1.84(6) 2.703(4) 159(2) . N13 H13A O1 0.83(6) 2.24(6) 3.045(4) 164(6) . 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 C21 N1 N2 C1 179.7(3) Zn1 N1 N2 C1 0.6(4) C4 N4 N5 C2 168.3(3) Zn1 N4 N5 C2 -4.8(3) C15 N8 N9 C12 171.3(3) Zn2 N8 N9 C12 1.0(4) C10 N11 N12 C13 173.1(3) Zn2 N11 N12 C13 -5.3(4) N1 N2 C1 N3 178.7(3) N1 N2 C1 S1 -3.4(4) Zn1 S1 C1 N2 3.8(3) Zn1 S1 C1 N3 -178.3(3) N4 N5 C2 N6 -176.8(3) N4 N5 C2 S2 3.8(4) Zn1 S2 C2 N5 -1.1(3) Zn1 S2 C2 N6 179.6(2) N5 N4 C4 C5 -176.4(3) Zn1 N4 C4 C5 -3.5(4) N5 N4 C4 C3 -0.3(5) Zn1 N4 C4 C3 172.6(2) C9 N14 C5 C6 -1.8(5) C9 N14 C5 C4 173.2(3) N4 C4 C5 N14 -27.5(4) C3 C4 C5 N14 156.2(3) N4 C4 C5 C6 147.6(3) C3 C4 C5 C6 -28.7(5) N14 C5 C6 C7 4.4(5) C4 C5 C6 C7 -170.4(3) C5 C6 C7 C8 -2.5(6) C6 C7 C8 C9 -1.8(6) C5 N14 C9 C8 -2.7(5) C5 N14 C9 C10 175.1(3) C7 C8 C9 N14 4.5(5) C7 C8 C9 C10 -173.2(3) N12 N11 C10 C9 176.8(3) Zn2 N11 C10 C9 -4.9(4) N12 N11 C10 C11 -3.2(5) Zn2 N11 C10 C11 175.1(2) N14 C9 C10 N11 -33.8(4) C8 C9 C10 N11 144.0(3) N14 C9 C10 C11 146.2(3) C8 C9 C10 C11 -36.0(5) N8 N9 C12 N10 176.2(3) N8 N9 C12 S3 -3.1(4) Zn2 S3 C12 N9 3.2(3) Zn2 S3 C12 N10 -176.2(3) N11 N12 C13 N13 179.6(3) N11 N12 C13 S4 -3.1(4) Zn2 S4 C13 N12 7.9(3) Zn2 S4 C13 N13 -174.8(3) N9 N8 C15 C16 -179.3(3) Zn2 N8 C15 C16 -9.5(4) N9 N8 C15 C14 -3.7(5) Zn2 N8 C15 C14 166.2(3) C20 N7 C16 C17 -3.0(5) Zn1 N7 C16 C17 135.6(3) C20 N7 C16 C15 171.6(3) Zn1 N7 C16 C15 -49.8(4) N8 C15 C16 N7 -37.9(4) C14 C15 C16 N7 146.3(3) N8 C15 C16 C17 136.9(4) C14 C15 C16 C17 -38.9(5) N7 C16 C17 C18 5.2(6) C15 C16 C17 C18 -169.3(4) C16 C17 C18 C19 -2.1(7) C17 C18 C19 C20 -2.8(8) C16 N7 C20 C19 -2.2(5) Zn1 N7 C20 C19 -147.8(3) C16 N7 C20 C21 174.2(3) Zn1 N7 C20 C21 28.6(3) C18 C19 C20 N7 5.1(7) C18 C19 C20 C21 -171.2(4) N2 N1 C21 C20 -178.1(3) Zn1 N1 C21 C20 1.0(4) N2 N1 C21 C22 0.0(5) Zn1 N1 C21 C22 179.1(3) N7 C20 C21 N1 -22.7(5) C19 C20 C21 N1 153.7(4) N7 C20 C21 C22 159.2(3) C19 C20 C21 C22 -24.4(5)