#------------------------------------------------------------------------------ #$Date: 2024-10-04 01:09:57 +0300 (Fri, 04 Oct 2024) $ #$Revision: 295021 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/27/1572757.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_1572757 loop_ _publ_author_name 'Anju, B. S.' 'Nair, Neeraja R.' 'Rajput, Janavi' 'Bertke, Jeffery A.' 'Mondal, Bhaskar' 'Kundu, Subrata' _publ_section_title ; Role of Ancillary Ligands in S-nitrosothiol and NO Generation from Nitrite-Thiol Interactions at Mononuclear Zinc(II) Sites ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC04853A _journal_year 2024 _chemical_formula_moiety 'C28 H47 N8 O P Zn, 2(Cl O4)' _chemical_formula_sum 'C28 H47 Cl2 N8 O9 P Zn' _chemical_formula_weight 806.97 _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_hydrogens geom _atom_sites_solution_primary intrinsic _audit_creation_method SHELXL-2019/1 _audit_update_record ; 2024-05-16 deposited with the CCDC. 2024-10-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.188(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.5047(13) _cell_length_b 21.305(4) _cell_length_c 20.512(3) _cell_measurement_reflns_used 9933 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.95 _cell_measurement_theta_min 2.15 _cell_volume 3713.9(11) _computing_cell_refinement 'SAINT V8.37A (Bruker, 2005)' _computing_data_collection 'APEX3 V2016.5-0 (Bruker, 2016)' _computing_data_reduction ; SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) ; _computing_molecular_graphics 'SHELXLE v932 (Hubschle, 2011)' _computing_publication_material 'XCIF V2014-2 (Bruker, 2014)' _computing_structure_refinement 'SHELXL-2019/1 (Sheldrick, 2019)' _computing_structure_solution 'SHELX-2014-5 (Sheldrick, 2015)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'Bruker ApexII CCD' _diffrn_measurement_method 'profile data from \f and \w scans' _diffrn_radiation_monochromator 'multilayer mirrors' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_unetI/netI 0.0490 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 65502 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.645 _diffrn_reflns_theta_min 1.379 _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2016/2 (Bruker, 2016)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1688 _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.085 _exptl_crystal_size_min 0.045 _refine_diff_density_max 1.188 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 621 _refine_ls_number_reflns 9412 _refine_ls_number_restraints 535 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.0786 _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^)+(0.0614P)^2^+4.1664P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1221 _refine_ls_wR_factor_ref 0.1367 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6802 _reflns_number_total 9412 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc04853a2.cif _cod_data_source_block ABS1364 _cod_original_cell_volume 3713.9(10) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1572757 _shelx_shelxl_version_number 2019/1 _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_min 0.907 _shelx_estimated_absorpt_t_max 0.960 _shelx_res_file ; TITL abs1364_a.res in P2(1)/c ABS1364.res created by SHELXL-2019/1 at 15:56:23 on 21-Sep-2023 REM Old TITL ABS1364 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.162, Rweak 0.009, Alpha 0.047 REM 0.755 for 225 systematic absences, Orientation as input REM Formula found by SHELXT: C33 N7 O6 P3 Zn CELL 0.71073 8.5047 21.3052 20.5117 90 92.188 90 ZERR 4 0.0013 0.0036 0.0033 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O P Zn UNIT 112 188 8 32 36 4 4 L.S. 20 PLAN 20 SIZE 0.045 0.085 0.11 TEMP -123.15 BOND $H LIST 4 FMAP 2 53 ACTA SIMU 0.01 0.02 O1 > C28B SADI 0.02 ZN1 O1 ZN1 O1B SIMU 0.01 0.02 CL1 > O5B SIMU 0.01 0.02 CL2 > O9B WGHT 0.061400 4.166400 FVAR 0.32536 0.80181 0.63692 0.64954 ZN1 7 0.725688 0.665756 0.739848 11.00000 0.02214 0.02342 = 0.01799 0.00193 -0.00280 0.00158 PART 1 21 O1 5 0.767423 0.586572 0.692871 21.00000 0.06563 0.02647 = 0.03644 -0.00486 0.00228 0.00074 P1 6 0.761274 0.542772 0.635968 21.00000 0.04868 0.02373 = 0.03503 -0.00831 -0.01102 0.00591 C23 1 0.796318 0.582791 0.560687 21.00000 0.08462 0.06387 = 0.05474 -0.01310 -0.01167 0.02467 AFIX 23 H23A 2 0.717450 0.616760 0.555335 21.00000 -1.20000 H23B 2 0.901064 0.602969 0.564956 21.00000 -1.20000 AFIX 0 C24 1 0.791285 0.544702 0.499833 21.00000 0.11130 0.07703 = 0.04920 -0.03229 -0.03065 0.04161 AFIX 137 H24A 2 0.831984 0.569628 0.464035 21.00000 -1.50000 H24B 2 0.682405 0.532349 0.489000 21.00000 -1.50000 H24C 2 0.856152 0.507046 0.506388 21.00000 -1.50000 AFIX 0 C25 1 0.568788 0.508682 0.626932 21.00000 0.07245 0.06250 = 0.09024 -0.02991 -0.01813 0.01337 AFIX 23 H25A 2 0.493249 0.542242 0.614121 21.00000 -1.20000 H25B 2 0.569267 0.477949 0.590740 21.00000 -1.20000 AFIX 0 C26 1 0.511674 0.477082 0.684868 21.00000 0.06091 0.05288 = 0.16043 0.00037 0.00954 -0.00791 AFIX 137 H26A 2 0.428303 0.447392 0.671782 21.00000 -1.50000 H26B 2 0.469835 0.508339 0.714672 21.00000 -1.50000 H26C 2 0.598671 0.454375 0.706913 21.00000 -1.50000 AFIX 0 C27 1 0.900377 0.479780 0.645730 21.00000 0.06227 0.04446 = 0.05365 -0.01696 -0.01426 0.01251 AFIX 23 H27A 2 0.869151 0.452155 0.681826 21.00000 -1.20000 H27B 2 0.899987 0.454422 0.605279 21.00000 -1.20000 AFIX 0 C28 1 1.065498 0.505115 0.660494 21.00000 0.05032 0.07565 = 0.05915 -0.02611 -0.01397 -0.00364 AFIX 137 H28A 2 1.136571 0.470219 0.671706 21.00000 -1.50000 H28B 2 1.063193 0.534438 0.697256 21.00000 -1.50000 H28C 2 1.102908 0.526981 0.622014 21.00000 -1.50000 AFIX 0 PART 2 -21 SAME 0.01 O1 > C28 O1B 5 0.691991 0.596658 0.673304 -21.00000 0.04728 0.02604 = 0.03646 -0.00954 0.00017 0.00394 P1B 6 0.749747 0.546414 0.628880 -21.00000 0.06685 0.03602 = 0.05605 -0.01488 -0.01168 0.01634 C23B 1 0.848648 0.584222 0.563620 -21.00000 0.06865 0.04643 = 0.04803 -0.01604 -0.01439 0.01347 AFIX 23 H23C 2 0.905869 0.620825 0.582470 -21.00000 -1.20000 H23D 2 0.928961 0.554604 0.548282 -21.00000 -1.20000 AFIX 0 C24B 1 0.758128 0.606136 0.506493 -21.00000 0.09101 0.06561 = 0.06244 -0.00747 0.00256 0.01463 AFIX 137 H24D 2 0.830044 0.619104 0.472798 -21.00000 -1.50000 H24E 2 0.692927 0.641915 0.518568 -21.00000 -1.50000 H24F 2 0.690411 0.572155 0.489617 -21.00000 -1.50000 AFIX 0 C25B 1 0.578879 0.506158 0.596902 -21.00000 0.05962 0.04504 = 0.06166 -0.01649 -0.01147 0.01463 AFIX 23 H25C 2 0.501994 0.537145 0.578987 -21.00000 -1.20000 H25D 2 0.608975 0.478257 0.560852 -21.00000 -1.20000 AFIX 0 C26B 1 0.504372 0.468212 0.648299 -21.00000 0.05138 0.04319 = 0.07515 0.00913 0.01292 -0.00434 AFIX 137 H26D 2 0.427057 0.439505 0.627905 -21.00000 -1.50000 H26E 2 0.451623 0.496218 0.678430 -21.00000 -1.50000 H26F 2 0.585401 0.443941 0.672386 -21.00000 -1.50000 AFIX 0 C27B 1 0.890163 0.490701 0.660738 -21.00000 0.06567 0.04656 = 0.05326 -0.02017 -0.01732 0.00781 AFIX 23 H27C 2 0.923910 0.502768 0.705735 -21.00000 -1.20000 H27D 2 0.840690 0.448701 0.662445 -21.00000 -1.20000 AFIX 0 C28B 1 1.035407 0.487814 0.617613 -21.00000 0.06518 0.07275 = 0.09201 0.00116 -0.01796 -0.00199 AFIX 137 H28D 2 1.095896 0.449703 0.627930 -21.00000 -1.50000 H28E 2 1.101732 0.524758 0.626081 -21.00000 -1.50000 H28F 2 1.000559 0.487153 0.571523 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 31 CL1 3 0.325580 0.653608 0.497437 31.00000 0.04304 0.02884 = 0.02717 0.00129 -0.00956 0.00839 O2 5 0.279758 0.618151 0.551915 31.00000 0.08639 0.04939 = 0.08284 0.03035 0.03165 0.00913 O3 5 0.491411 0.645115 0.492936 31.00000 0.04930 0.06748 = 0.07002 0.00209 0.00761 0.02697 O4 5 0.294909 0.719206 0.508872 31.00000 0.03955 0.02676 = 0.03888 -0.00443 -0.01467 0.00878 O5 5 0.252362 0.634968 0.438041 31.00000 0.10845 0.04495 = 0.06873 -0.02537 -0.05281 0.01820 PART 2 -31 SAME 0.01 CL1 > O5 CL1B 3 0.302299 0.647737 0.499090 -31.00000 0.04245 0.02452 = 0.03816 -0.00261 0.00001 0.00701 O2B 5 0.354497 0.617953 0.557464 -31.00000 0.07462 0.04002 = 0.05695 0.00922 -0.02367 0.00477 O3B 5 0.394211 0.626675 0.447244 -31.00000 0.09865 0.06329 = 0.06457 -0.01414 0.03823 0.00704 O4B 5 0.315785 0.714755 0.504962 -31.00000 0.04058 0.02941 = 0.02897 -0.00475 -0.00967 0.00319 O5B 5 0.144330 0.631030 0.483062 -31.00000 0.04970 0.04343 = 0.09393 -0.00569 -0.02582 -0.01005 PART 0 PART 1 41 CL2 3 0.112621 0.429034 0.857761 41.00000 0.02387 0.02657 = 0.04355 -0.00032 -0.00195 0.00066 O6 5 0.041282 0.401856 0.913571 41.00000 0.07543 0.10365 = 0.07683 0.04220 0.02116 0.01359 O7 5 0.236273 0.391416 0.836424 41.00000 0.06189 0.08004 = 0.09689 -0.02253 -0.00342 0.02941 O8 5 0.164754 0.488422 0.879180 41.00000 0.03789 0.04250 = 0.14842 -0.01448 -0.01906 0.00025 O9 5 -0.007280 0.434575 0.808183 41.00000 0.06011 0.08445 = 0.04531 -0.00346 -0.02383 0.00863 PART 2 -41 SAME 0.01 CL2 > O9 CL2B 3 0.130935 0.430311 0.840968 -41.00000 0.03542 0.03449 = 0.07860 -0.01413 0.01561 -0.00152 O6B 5 0.136240 0.466439 0.900410 -41.00000 0.05251 0.08363 = 0.03882 -0.03099 -0.01065 0.01560 O7B 5 0.258562 0.388006 0.845552 -41.00000 0.03952 0.03981 = 0.08885 0.02101 0.02588 0.01977 O8B 5 0.138517 0.474723 0.791062 -41.00000 0.09784 0.07405 = 0.08716 0.02997 0.01633 0.02801 O9B 5 -0.012266 0.397193 0.836224 -41.00000 0.05276 0.08416 = 0.12941 -0.03121 0.01446 -0.01697 PART 0 N1 4 0.548122 0.731433 0.741610 11.00000 0.02830 0.03303 = 0.02265 -0.00221 -0.00125 0.00756 N2 4 0.503489 0.761659 0.685699 11.00000 0.02228 0.02674 = 0.03603 0.00334 -0.00570 0.00275 N3 4 0.815912 0.714696 0.659515 11.00000 0.02590 0.02798 = 0.02203 0.00326 -0.00273 -0.00259 N4 4 0.714187 0.742745 0.615742 11.00000 0.02835 0.03011 = 0.02156 0.00695 -0.00579 -0.00634 N5 4 0.630435 0.603670 0.810865 11.00000 0.02535 0.04320 = 0.02937 0.01533 -0.00709 -0.00342 N6 4 0.734024 0.576276 0.855196 11.00000 0.02804 0.03182 = 0.02588 0.00861 -0.00561 -0.00147 N7 4 0.894904 0.690388 0.809001 11.00000 0.02680 0.02743 = 0.02181 0.00204 -0.00528 -0.00058 N8 4 0.951280 0.646430 0.852685 11.00000 0.02308 0.02980 = 0.02004 -0.00038 -0.00564 0.00301 C1 1 0.486109 0.764701 0.790062 11.00000 0.03034 0.05208 = 0.04063 -0.01851 0.00183 0.00588 C2 1 0.401625 0.814476 0.763794 11.00000 0.03457 0.04035 = 0.07525 -0.02071 0.00365 0.01108 AFIX 43 H2 2 0.344497 0.844607 0.787493 11.00000 -1.20000 AFIX 0 C3 1 0.414623 0.812772 0.697846 11.00000 0.02627 0.02551 = 0.07534 0.00045 -0.00436 0.00490 C4 1 0.516557 0.747330 0.859842 11.00000 0.06024 0.09286 = 0.03377 -0.02196 0.00699 0.01555 AFIX 137 H4A 2 0.423503 0.726480 0.876459 11.00000 -1.50000 H4B 2 0.539327 0.785302 0.885464 11.00000 -1.50000 H4C 2 0.606846 0.718795 0.863455 11.00000 -1.50000 AFIX 0 C5 1 0.352990 0.855149 0.645134 11.00000 0.04913 0.04373 = 0.11042 0.02612 -0.01370 0.01697 AFIX 137 H5A 2 0.440892 0.876996 0.625517 11.00000 -1.50000 H5B 2 0.281570 0.885988 0.663523 11.00000 -1.50000 H5C 2 0.295930 0.830363 0.611658 11.00000 -1.50000 AFIX 0 C6 1 0.548395 0.735669 0.624569 11.00000 0.02609 0.03503 = 0.02642 0.00736 -0.01013 -0.00557 AFIX 23 H6A 2 0.489177 0.757010 0.588473 11.00000 -1.20000 H6B 2 0.520714 0.690544 0.623040 11.00000 -1.20000 AFIX 0 C7 1 0.958128 0.721330 0.635327 11.00000 0.02819 0.04079 = 0.02887 0.00197 0.00148 -0.00565 C8 1 0.945008 0.752882 0.575913 11.00000 0.03415 0.06515 = 0.03322 0.01120 0.00467 -0.01720 AFIX 43 H8 2 1.028724 0.763127 0.548450 11.00000 -1.20000 AFIX 0 C9 1 0.790509 0.766264 0.564551 11.00000 0.04136 0.04729 = 0.02609 0.01276 -0.00297 -0.01616 C10 1 1.101373 0.696911 0.670847 11.00000 0.02557 0.06867 = 0.04287 0.00865 0.00165 0.00243 AFIX 137 H10A 2 1.149170 0.730458 0.697610 11.00000 -1.50000 H10B 2 1.176953 0.682266 0.639322 11.00000 -1.50000 H10C 2 1.072259 0.661939 0.698982 11.00000 -1.50000 AFIX 0 C11 1 0.704899 0.801367 0.510930 11.00000 0.05525 0.08271 = 0.03745 0.03263 -0.01242 -0.02156 AFIX 137 H11A 2 0.614692 0.776535 0.494650 11.00000 -1.50000 H11B 2 0.776115 0.808971 0.475319 11.00000 -1.50000 H11C 2 0.667809 0.841590 0.527694 11.00000 -1.50000 AFIX 0 C12 1 0.489067 0.583729 0.826423 11.00000 0.02917 0.05458 = 0.03321 0.01123 -0.00188 -0.00932 C13 1 0.502251 0.543397 0.880424 11.00000 0.04282 0.05587 = 0.03283 0.01230 0.00417 -0.01675 AFIX 43 H13 2 0.418507 0.522930 0.901219 11.00000 -1.20000 AFIX 0 C14 1 0.658710 0.539263 0.897294 11.00000 0.04119 0.03839 = 0.02622 0.00799 -0.00031 -0.00308 C15 1 0.344762 0.603675 0.788281 11.00000 0.02708 0.09355 = 0.04929 0.02734 -0.00763 -0.00989 AFIX 137 H15A 2 0.297647 0.639924 0.809536 11.00000 -1.50000 H15B 2 0.269021 0.568999 0.786292 11.00000 -1.50000 H15C 2 0.372821 0.615207 0.743958 11.00000 -1.50000 AFIX 0 C16 1 0.743631 0.502926 0.950373 11.00000 0.06103 0.04821 = 0.03243 0.01987 0.00051 0.00454 AFIX 137 H16A 2 0.825405 0.476979 0.931457 11.00000 -1.50000 H16B 2 0.668803 0.475903 0.972291 11.00000 -1.50000 H16C 2 0.792213 0.532134 0.982079 11.00000 -1.50000 AFIX 0 C17 1 0.899709 0.582204 0.845176 11.00000 0.02627 0.02919 = 0.02648 0.00220 -0.00660 0.00339 AFIX 23 H17A 2 0.922592 0.567349 0.800800 11.00000 -1.20000 H17B 2 0.958890 0.555408 0.876993 11.00000 -1.20000 AFIX 0 C18 1 1.048787 0.673146 0.898714 11.00000 0.02147 0.04340 = 0.02423 -0.00902 -0.00631 0.00538 C19 1 1.053552 0.735518 0.884566 11.00000 0.03529 0.04015 = 0.03603 -0.01189 -0.00994 -0.00456 AFIX 43 H19 2 1.111783 0.766720 0.908128 11.00000 -1.20000 AFIX 0 C20 1 0.957232 0.744983 0.829178 11.00000 0.03447 0.03031 = 0.03328 -0.00496 -0.00311 -0.00449 C21 1 1.129229 0.635849 0.951384 11.00000 0.04109 0.05389 = 0.03422 -0.00912 -0.01809 0.01348 AFIX 137 H21A 2 1.051682 0.621520 0.982232 11.00000 -1.50000 H21B 2 1.208292 0.662016 0.974337 11.00000 -1.50000 H21C 2 1.180741 0.599426 0.932302 11.00000 -1.50000 AFIX 0 C22 1 0.921158 0.804931 0.794239 11.00000 0.06983 0.02670 = 0.05315 -0.00190 -0.01514 -0.01146 AFIX 137 H22A 2 0.992623 0.809937 0.758237 11.00000 -1.50000 H22B 2 0.934929 0.840175 0.824624 11.00000 -1.50000 H22C 2 0.812206 0.804091 0.776888 11.00000 -1.50000 AFIX 0 HKLF 4 REM abs1364_a.res in P2(1)/c REM wR2 = 0.1367, GooF = S = 1.032, Restrained GooF = 1.066 for all data REM R1 = 0.0507 for 6802 Fo > 4sig(Fo) and 0.0786 for all 9412 data REM 621 parameters refined using 535 restraints END WGHT 0.0614 4.1664 REM Highest difference peak 1.188, deepest hole -0.455, 1-sigma level 0.082 Q1 1 0.9703 0.5407 0.6410 11.00000 0.05 1.19 Q2 1 0.7010 0.5428 0.5525 11.00000 0.05 1.14 Q3 1 0.6817 0.4748 0.6709 11.00000 0.05 0.97 Q4 1 0.6201 0.6641 0.7413 11.00000 0.05 0.53 Q5 1 0.1758 0.4864 0.8343 11.00000 0.05 0.53 Q6 1 0.2388 0.4368 0.8001 11.00000 0.05 0.51 Q7 1 0.6578 0.5349 0.6404 11.00000 0.05 0.50 Q8 1 0.0462 0.3788 0.8745 11.00000 0.05 0.47 Q9 1 0.8248 0.6627 0.7382 11.00000 0.05 0.47 Q10 1 0.1823 0.6204 0.5227 11.00000 0.05 0.42 Q11 1 0.0794 0.4432 0.7830 11.00000 0.05 0.38 Q12 1 0.7071 0.6582 0.7006 11.00000 0.05 0.36 Q13 1 0.5822 0.5358 0.8838 11.00000 0.05 0.35 Q14 1 0.3276 0.6416 0.4367 11.00000 0.05 0.34 Q15 1 0.8477 0.5200 0.6426 11.00000 0.05 0.34 Q16 1 1.0284 0.7025 0.9020 11.00000 0.05 0.33 Q17 1 0.4953 0.5553 0.8548 11.00000 0.05 0.32 Q18 1 0.1006 0.4352 0.9155 11.00000 0.05 0.32 Q19 1 1.1068 0.7016 0.7185 11.00000 0.05 0.32 Q20 1 0.1825 0.6226 0.4575 11.00000 0.05 0.32 ; _shelx_res_checksum 40748 _shelx_hkl_file ; 2 0 0 682.83 35.40 -2 0 0 754.22 35.50 3 0 0 70.79 7.90 -3 0 0 79.19 6.10 -3 0 0 100.89 8.80 4 0 0 2025.90 100.09 -4 0 0 2100.19 97.69 -4 0 0 2072.49 97.29 -5 0 0 3097.89 145.59 -5 0 0 3161.08 145.99 5 0 0 3057.79 149.09 -6 0 0 165.08 12.20 -6 0 0 184.28 13.00 -6 0 0 171.68 13.10 6 0 0 145.59 16.60 -7 0 0 40.80 7.00 -7 0 0 36.20 6.90 7 0 0 33.90 10.70 -7 0 0 28.50 6.70 -8 0 0 111.59 12.40 -8 0 0 119.49 12.30 -8 0 0 109.69 12.00 -8 0 0 102.39 11.90 8 0 0 98.29 17.00 -9 0 0 153.68 14.70 -9 0 0 135.29 14.90 -9 0 0 127.59 14.00 -9 0 0 141.89 14.40 -10 0 0 3.10 7.00 -10 0 0 8.40 6.50 -10 0 0 10.60 7.60 -10 0 0 3.10 7.50 -11 0 0 4.50 7.70 -11 0 0 5.30 8.20 -11 0 0 -12.60 7.20 0 -1 0 0.30 0.50 0 -1 0 0.20 0.60 0 -1 0 0.10 0.30 0 -1 0 0.70 0.40 0 -1 0 0.20 0.50 0 1 0 -0.80 0.50 0 1 0 1.70 0.50 0 1 0 0.10 0.30 0 1 0 0.30 0.60 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-27 1.80 10.80 -1 -2 27 109.69 19.80 -1 -2 27 119.59 21.30 1 -2 -27 90.09 18.30 1 2 -27 160.98 20.90 -1 2 27 87.39 20.20 -1 2 27 116.69 20.40 0 -2 27 8.50 13.10 0 -2 27 6.70 11.00 0 -2 -27 -4.60 11.80 0 2 27 7.60 13.60 0 2 -27 3.90 11.60 0 2 27 3.30 12.50 -1 -2 -27 226.08 28.20 1 -2 27 205.58 24.70 1 -2 27 157.68 25.80 1 2 27 226.38 26.90 -1 2 -27 188.18 24.90 1 2 27 154.68 26.50 -2 -3 27 19.40 13.40 -1 -3 27 22.40 13.50 -1 -3 27 11.10 12.50 1 -3 -27 41.10 14.90 -1 3 27 17.70 14.10 -1 3 27 42.20 16.70 1 3 -27 18.30 12.80 0 -3 27 39.10 16.70 0 -3 27 71.99 16.10 0 -3 -27 61.19 16.60 0 3 27 66.49 17.70 0 3 -27 35.30 15.10 0 3 27 64.69 18.50 -1 -3 -27 30.60 20.40 1 -3 27 7.30 15.10 -1 3 -27 4.00 12.90 1 3 27 -8.60 12.90 -1 -4 27 106.89 19.20 -1 -4 27 53.99 17.40 1 -4 -27 69.19 17.80 -1 4 27 102.39 19.60 -1 4 27 43.70 15.90 1 4 -27 72.09 16.60 0 -4 27 11.10 11.90 0 -4 -27 15.50 13.90 0 -4 27 -0.30 13.90 0 4 27 19.40 14.20 0 4 27 4.80 12.80 0 4 -27 11.00 12.20 -1 5 27 -0.80 11.80 0 5 27 6.10 13.40 -1 6 27 2.80 12.90 0 6 27 -13.40 11.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 92791 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 Zn1 Zn 0.72569(4) 0.66576(2) 0.73985(2) 0.02127(10) Uani 1 1 d D . . . . O1 O 0.7674(5) 0.58657(14) 0.69287(16) 0.0428(9) Uani 0.802(5) 1 d D U P A 1 P1 P 0.7613(3) 0.54277(12) 0.63597(11) 0.0361(4) Uani 0.802(5) 1 d D U P A 1 C23 C 0.7963(9) 0.5828(3) 0.5607(3) 0.0681(16) Uani 0.802(5) 1 d D U P A 1 H23A H 0.717450 0.616760 0.555335 0.082 Uiso 0.802(5) 1 calc R U P A 1 H23B H 0.901064 0.602969 0.564956 0.082 Uiso 0.802(5) 1 calc R U P A 1 C24 C 0.7913(8) 0.5447(3) 0.4998(3) 0.080(2) Uani 0.802(5) 1 d D U P A 1 H24A H 0.831984 0.569628 0.464035 0.120 Uiso 0.802(5) 1 calc R U P A 1 H24B H 0.682405 0.532349 0.489000 0.120 Uiso 0.802(5) 1 calc R U P A 1 H24C H 0.856152 0.507046 0.506388 0.120 Uiso 0.802(5) 1 calc R U P A 1 C25 C 0.5688(7) 0.5087(3) 0.6269(4) 0.0756(17) Uani 0.802(5) 1 d D U P A 1 H25A H 0.493249 0.542242 0.614121 0.091 Uiso 0.802(5) 1 calc R U P A 1 H25B H 0.569267 0.477949 0.590740 0.091 Uiso 0.802(5) 1 calc R U P A 1 C26 C 0.5117(9) 0.4771(4) 0.6849(5) 0.091(3) Uani 0.802(5) 1 d D U P A 1 H26A H 0.428303 0.447392 0.671782 0.137 Uiso 0.802(5) 1 calc R U P A 1 H26B H 0.469835 0.508339 0.714672 0.137 Uiso 0.802(5) 1 calc R U P A 1 H26C H 0.598671 0.454375 0.706913 0.137 Uiso 0.802(5) 1 calc R U P A 1 C27 C 0.9004(7) 0.4798(2) 0.6457(3) 0.0539(14) Uani 0.802(5) 1 d D U P A 1 H27A H 0.869151 0.452155 0.681826 0.065 Uiso 0.802(5) 1 calc R U P A 1 H27B H 0.899987 0.454422 0.605279 0.065 Uiso 0.802(5) 1 calc R U P A 1 C28 C 1.0655(6) 0.5051(3) 0.6605(3) 0.0621(15) Uani 0.802(5) 1 d D U P A 1 H28A H 1.136571 0.470219 0.671706 0.093 Uiso 0.802(5) 1 calc R U P A 1 H28B H 1.063193 0.534438 0.697256 0.093 Uiso 0.802(5) 1 calc R U P A 1 H28C H 1.102908 0.526981 0.622014 0.093 Uiso 0.802(5) 1 calc R U P A 1 O1B O 0.6920(17) 0.5967(5) 0.6733(6) 0.037(2) Uani 0.198(5) 1 d D U P A 2 P1B P 0.7497(15) 0.5464(6) 0.6289(6) 0.0533(19) Uani 0.198(5) 1 d D U P A 2 C23B C 0.849(2) 0.5842(11) 0.5636(8) 0.055(3) Uani 0.198(5) 1 d D U P A 2 H23C H 0.905869 0.620825 0.582470 0.066 Uiso 0.198(5) 1 calc R U P A 2 H23D H 0.928961 0.554604 0.548282 0.066 Uiso 0.198(5) 1 calc R U P A 2 C24B C 0.758(3) 0.6061(12) 0.5065(9) 0.073(5) Uani 0.198(5) 1 d D U P A 2 H24D H 0.830044 0.619104 0.472798 0.110 Uiso 0.198(5) 1 calc R U P A 2 H24E H 0.692927 0.641915 0.518568 0.110 Uiso 0.198(5) 1 calc R U P A 2 H24F H 0.690411 0.572155 0.489617 0.110 Uiso 0.198(5) 1 calc R U P A 2 C25B C 0.579(2) 0.5062(9) 0.5969(9) 0.056(3) Uani 0.198(5) 1 d D U P A 2 H25C H 0.501994 0.537145 0.578987 0.067 Uiso 0.198(5) 1 calc R U P A 2 H25D H 0.608975 0.478257 0.560852 0.067 Uiso 0.198(5) 1 calc R U P A 2 C26B C 0.504(3) 0.4682(12) 0.6483(12) 0.056(5) Uani 0.198(5) 1 d D U P A 2 H26D H 0.427057 0.439505 0.627905 0.084 Uiso 0.198(5) 1 calc R U P A 2 H26E H 0.451623 0.496218 0.678430 0.084 Uiso 0.198(5) 1 calc R U P A 2 H26F H 0.585401 0.443941 0.672386 0.084 Uiso 0.198(5) 1 calc R U P A 2 C27B C 0.890(2) 0.4907(10) 0.6607(10) 0.056(3) Uani 0.198(5) 1 d D U P A 2 H27C H 0.923910 0.502768 0.705735 0.067 Uiso 0.198(5) 1 calc R U P A 2 H27D H 0.840690 0.448701 0.662445 0.067 Uiso 0.198(5) 1 calc R U P A 2 C28B C 1.035(2) 0.4878(12) 0.6176(13) 0.077(5) Uani 0.198(5) 1 d D U P A 2 H28D H 1.095896 0.449703 0.627930 0.116 Uiso 0.198(5) 1 calc R U P A 2 H28E H 1.101732 0.524758 0.626081 0.116 Uiso 0.198(5) 1 calc R U P A 2 H28F H 1.000559 0.487153 0.571523 0.116 Uiso 0.198(5) 1 calc R U P A 2 Cl1 Cl 0.3256(5) 0.6536(3) 0.4974(2) 0.0333(8) Uani 0.637(6) 1 d D U P B 1 O2 O 0.2798(9) 0.6182(4) 0.5519(4) 0.072(2) Uani 0.637(6) 1 d D U P B 1 O3 O 0.4914(5) 0.6451(2) 0.4929(3) 0.0621(15) Uani 0.637(6) 1 d D U P B 1 O4 O 0.2949(14) 0.7192(3) 0.5089(7) 0.035(2) Uani 0.637(6) 1 d D U P B 1 O5 O 0.2524(8) 0.6350(2) 0.4380(3) 0.0755(19) Uani 0.637(6) 1 d D U P B 1 Cl1B Cl 0.3023(9) 0.6477(4) 0.4991(4) 0.0351(15) Uani 0.363(6) 1 d D U P B 2 O2B O 0.3545(13) 0.6180(6) 0.5575(5) 0.058(3) Uani 0.363(6) 1 d D U P B 2 O3B O 0.3942(13) 0.6267(4) 0.4472(4) 0.075(3) Uani 0.363(6) 1 d D U P B 2 O4B O 0.316(2) 0.7148(5) 0.5050(11) 0.033(3) Uani 0.363(6) 1 d D U P B 2 O5B O 0.1443(9) 0.6310(4) 0.4831(5) 0.063(2) Uani 0.363(6) 1 d D U P B 2 Cl2 Cl 0.1126(4) 0.42903(17) 0.85776(14) 0.0314(6) Uani 0.650(6) 1 d D U P C 1 O6 O 0.0413(6) 0.4019(3) 0.9136(3) 0.0848(19) Uani 0.650(6) 1 d D U P C 1 O7 O 0.2363(10) 0.3914(5) 0.8364(6) 0.080(3) Uani 0.650(6) 1 d D U P C 1 O8 O 0.1648(8) 0.4884(3) 0.8792(4) 0.077(2) Uani 0.650(6) 1 d D U P C 1 O9 O -0.0073(6) 0.4346(3) 0.8082(2) 0.0640(15) Uani 0.650(6) 1 d D U P C 1 Cl2B Cl 0.1309(8) 0.4303(4) 0.8410(3) 0.0492(16) Uani 0.350(6) 1 d D U P C 2 O6B O 0.1362(14) 0.4664(6) 0.9004(4) 0.059(3) Uani 0.350(6) 1 d D U P C 2 O7B O 0.2586(15) 0.3880(6) 0.8456(9) 0.055(3) Uani 0.350(6) 1 d D U P C 2 O8B O 0.1385(12) 0.4747(4) 0.7911(5) 0.086(3) Uani 0.350(6) 1 d D U P C 2 O9B O -0.0123(10) 0.3972(5) 0.8362(7) 0.088(3) Uani 0.350(6) 1 d D U P C 2 N1 N 0.5481(3) 0.73143(12) 0.74161(11) 0.0280(5) Uani 1 1 d . . . . . N2 N 0.5035(3) 0.76166(12) 0.68570(12) 0.0285(5) Uani 1 1 d . . . . . N3 N 0.8159(3) 0.71470(11) 0.65952(11) 0.0254(5) Uani 1 1 d . . . . . N4 N 0.7142(3) 0.74274(12) 0.61574(11) 0.0268(5) Uani 1 1 d . . . . . N5 N 0.6304(3) 0.60367(13) 0.81087(12) 0.0328(6) Uani 1 1 d . . . . . N6 N 0.7340(3) 0.57628(12) 0.85520(12) 0.0288(5) Uani 1 1 d . . . . . N7 N 0.8949(3) 0.69039(11) 0.80900(11) 0.0255(5) Uani 1 1 d . . . . . N8 N 0.9513(3) 0.64643(11) 0.85269(11) 0.0245(5) Uani 1 1 d . . . . . C1 C 0.4861(4) 0.76470(18) 0.79006(17) 0.0410(8) Uani 1 1 d . . . . . C2 C 0.4016(4) 0.81448(18) 0.7638(2) 0.0500(10) Uani 1 1 d . . . . . H2 H 0.344497 0.844607 0.787493 0.060 Uiso 1 1 calc R U . . . C3 C 0.4146(4) 0.81277(15) 0.6978(2) 0.0425(9) Uani 1 1 d . . . . . C4 C 0.5166(5) 0.7473(2) 0.85984(18) 0.0622(12) Uani 1 1 d . . . . . H4A H 0.423503 0.726480 0.876459 0.093 Uiso 1 1 calc R U . . . H4B H 0.539327 0.785302 0.885464 0.093 Uiso 1 1 calc R U . . . H4C H 0.606846 0.718795 0.863455 0.093 Uiso 1 1 calc R U . . . C5 C 0.3530(5) 0.8551(2) 0.6451(3) 0.0682(13) Uani 1 1 d . . . . . H5A H 0.440892 0.876996 0.625517 0.102 Uiso 1 1 calc R U . . . H5B H 0.281570 0.885988 0.663523 0.102 Uiso 1 1 calc R U . . . H5C H 0.295930 0.830363 0.611658 0.102 Uiso 1 1 calc R U . . . C6 C 0.5484(3) 0.73567(15) 0.62457(14) 0.0295(6) Uani 1 1 d . . . . . H6A H 0.489177 0.757010 0.588473 0.035 Uiso 1 1 calc R U . . . H6B H 0.520714 0.690544 0.623040 0.035 Uiso 1 1 calc R U . . . C7 C 0.9581(3) 0.72133(16) 0.63533(15) 0.0326(7) Uani 1 1 d . . . . . C8 C 0.9450(4) 0.75288(19) 0.57591(16) 0.0441(9) Uani 1 1 d . . . . . H8 H 1.028724 0.763127 0.548450 0.053 Uiso 1 1 calc R U . . . C9 C 0.7905(4) 0.76626(17) 0.56455(15) 0.0384(8) Uani 1 1 d . . . . . C10 C 1.1014(4) 0.6969(2) 0.67085(18) 0.0457(9) Uani 1 1 d . . . . . H10A H 1.149170 0.730458 0.697610 0.069 Uiso 1 1 calc R U . . . H10B H 1.176953 0.682266 0.639322 0.069 Uiso 1 1 calc R U . . . H10C H 1.072259 0.661939 0.698982 0.069 Uiso 1 1 calc R U . . . C11 C 0.7049(5) 0.8014(2) 0.51093(18) 0.0588(12) Uani 1 1 d . . . . . H11A H 0.614692 0.776535 0.494650 0.088 Uiso 1 1 calc R U . . . H11B H 0.776115 0.808971 0.475319 0.088 Uiso 1 1 calc R U . . . H11C H 0.667809 0.841590 0.527694 0.088 Uiso 1 1 calc R U . . . C12 C 0.4891(4) 0.58373(17) 0.82642(16) 0.0391(8) Uani 1 1 d . . . . . C13 C 0.5023(4) 0.54340(18) 0.88042(16) 0.0438(9) Uani 1 1 d . . . . . H13 H 0.418507 0.522930 0.901219 0.053 Uiso 1 1 calc R U . . . C14 C 0.6587(4) 0.53926(16) 0.89729(15) 0.0353(7) Uani 1 1 d . . . . . C15 C 0.3448(4) 0.6037(2) 0.78828(19) 0.0569(11) Uani 1 1 d . . . . . H15A H 0.297647 0.639924 0.809536 0.085 Uiso 1 1 calc R U . . . H15B H 0.269021 0.568999 0.786292 0.085 Uiso 1 1 calc R U . . . H15C H 0.372821 0.615207 0.743958 0.085 Uiso 1 1 calc R U . . . C16 C 0.7436(5) 0.50293(18) 0.95037(17) 0.0473(9) Uani 1 1 d . . . . . H16A H 0.825405 0.476979 0.931457 0.071 Uiso 1 1 calc R U . . . H16B H 0.668803 0.475903 0.972291 0.071 Uiso 1 1 calc R U . . . H16C H 0.792213 0.532134 0.982079 0.071 Uiso 1 1 calc R U . . . C17 C 0.8997(3) 0.58220(14) 0.84518(14) 0.0275(6) Uani 1 1 d . . . . . H17A H 0.922592 0.567349 0.800800 0.033 Uiso 1 1 calc R U . . . H17B H 0.958890 0.555408 0.876993 0.033 Uiso 1 1 calc R U . . . C18 C 1.0488(3) 0.67315(15) 0.89871(14) 0.0299(6) Uani 1 1 d . . . . . C19 C 1.0536(4) 0.73552(16) 0.88457(16) 0.0374(7) Uani 1 1 d . . . . . H19 H 1.111783 0.766720 0.908128 0.045 Uiso 1 1 calc R U . . . C20 C 0.9572(4) 0.74498(15) 0.82918(15) 0.0328(7) Uani 1 1 d . . . . . C21 C 1.1292(4) 0.63585(18) 0.95138(17) 0.0436(8) Uani 1 1 d . . . . . H21A H 1.051682 0.621520 0.982232 0.065 Uiso 1 1 calc R U . . . H21B H 1.208292 0.662016 0.974337 0.065 Uiso 1 1 calc R U . . . H21C H 1.180741 0.599426 0.932302 0.065 Uiso 1 1 calc R U . . . C22 C 0.9212(5) 0.80493(16) 0.79424(19) 0.0503(10) Uani 1 1 d . . . . . H22A H 0.992623 0.809937 0.758237 0.076 Uiso 1 1 calc R U . . . H22B H 0.934929 0.840175 0.824624 0.076 Uiso 1 1 calc R U . . . H22C H 0.812206 0.804091 0.776888 0.076 Uiso 1 1 calc R 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 0.02214(16) 0.02342(17) 0.01799(15) 0.00193(12) -0.00280(11) 0.00158(13) O1 0.066(2) 0.0265(15) 0.0364(17) -0.0049(13) 0.0023(16) 0.0007(15) P1 0.0487(8) 0.0237(7) 0.0350(8) -0.0083(6) -0.0110(6) 0.0059(6) C23 0.085(4) 0.064(3) 0.055(3) -0.013(2) -0.012(3) 0.025(3) C24 0.111(5) 0.077(4) 0.049(3) -0.032(3) -0.031(3) 0.042(4) C25 0.072(3) 0.062(3) 0.090(4) -0.030(3) -0.018(3) 0.013(3) C26 0.061(4) 0.053(4) 0.160(8) 0.000(5) 0.010(5) -0.008(3) C27 0.062(3) 0.044(3) 0.054(3) -0.017(2) -0.014(2) 0.013(2) C28 0.050(3) 0.076(4) 0.059(3) -0.026(3) -0.014(2) -0.004(3) O1B 0.047(5) 0.026(4) 0.036(5) -0.010(4) 0.000(4) 0.004(4) P1B 0.067(3) 0.036(3) 0.056(3) -0.015(3) -0.012(3) 0.016(3) C23B 0.069(6) 0.046(5) 0.048(5) -0.016(5) -0.014(5) 0.013(5) C24B 0.091(10) 0.066(10) 0.062(9) -0.007(8) 0.003(9) 0.015(9) C25B 0.060(5) 0.045(5) 0.062(6) -0.016(6) -0.011(6) 0.015(5) C26B 0.051(9) 0.043(9) 0.075(11) 0.009(9) 0.013(9) -0.004(8) C27B 0.066(5) 0.047(5) 0.053(5) -0.020(5) -0.017(5) 0.008(5) C28B 0.065(9) 0.073(10) 0.092(10) 0.001(9) -0.018(9) -0.002(9) Cl1 0.0430(13) 0.0288(14) 0.0272(12) 0.0013(9) -0.0096(9) 0.0084(10) O2 0.086(5) 0.049(3) 0.083(4) 0.030(3) 0.032(4) 0.009(4) O3 0.049(3) 0.067(3) 0.070(3) 0.002(2) 0.008(2) 0.027(2) O4 0.040(4) 0.027(3) 0.039(4) -0.004(3) -0.015(3) 0.009(2) O5 0.108(5) 0.045(3) 0.069(3) -0.025(2) -0.053(3) 0.018(3) Cl1B 0.042(2) 0.025(2) 0.038(2) -0.0026(16) 0.0000(16) 0.0070(17) O2B 0.075(6) 0.040(4) 0.057(5) 0.009(4) -0.024(5) 0.005(5) O3B 0.099(6) 0.063(5) 0.065(5) -0.014(4) 0.038(5) 0.007(5) O4B 0.041(6) 0.029(6) 0.029(5) -0.005(4) -0.010(5) 0.003(4) O5B 0.050(4) 0.043(4) 0.094(6) -0.006(4) -0.026(4) -0.010(3) Cl2 0.0239(10) 0.0266(8) 0.0435(11) -0.0003(8) -0.0019(9) 0.0007(7) O6 0.075(3) 0.104(4) 0.077(3) 0.042(3) 0.021(3) 0.014(3) O7 0.062(4) 0.080(5) 0.097(5) -0.023(4) -0.003(4) 0.029(4) O8 0.038(3) 0.043(3) 0.148(6) -0.014(3) -0.019(3) 0.000(2) O9 0.060(3) 0.084(4) 0.045(3) -0.003(2) -0.024(2) 0.009(3) Cl2B 0.0354(19) 0.034(2) 0.079(4) -0.014(2) 0.016(2) -0.0015(14) O6B 0.053(5) 0.084(7) 0.039(4) -0.031(5) -0.011(4) 0.016(5) O7B 0.040(5) 0.040(5) 0.089(7) 0.021(5) 0.026(5) 0.020(4) O8B 0.098(6) 0.074(6) 0.087(6) 0.030(5) 0.016(5) 0.028(5) O9B 0.053(5) 0.084(6) 0.129(8) -0.031(6) 0.014(5) -0.017(5) N1 0.0283(12) 0.0330(14) 0.0226(12) -0.0022(10) -0.0013(10) 0.0076(10) N2 0.0223(11) 0.0267(13) 0.0360(14) 0.0033(10) -0.0057(10) 0.0028(10) N3 0.0259(12) 0.0280(13) 0.0220(11) 0.0033(9) -0.0027(9) -0.0026(10) N4 0.0283(12) 0.0301(13) 0.0216(11) 0.0070(10) -0.0058(9) -0.0063(10) N5 0.0254(12) 0.0432(16) 0.0294(13) 0.0153(11) -0.0071(10) -0.0034(11) N6 0.0280(12) 0.0318(14) 0.0259(12) 0.0086(10) -0.0056(10) -0.0015(10) N7 0.0268(12) 0.0274(12) 0.0218(11) 0.0020(9) -0.0053(9) -0.0006(10) N8 0.0231(11) 0.0298(13) 0.0200(11) -0.0004(9) -0.0056(9) 0.0030(10) C1 0.0303(16) 0.052(2) 0.0406(18) -0.0185(16) 0.0018(14) 0.0059(15) C2 0.0346(18) 0.040(2) 0.075(3) -0.0207(19) 0.0037(18) 0.0111(15) C3 0.0263(15) 0.0255(16) 0.075(3) 0.0005(16) -0.0044(16) 0.0049(13) C4 0.060(3) 0.093(3) 0.0338(19) -0.022(2) 0.0070(18) 0.016(2) C5 0.049(2) 0.044(2) 0.110(4) 0.026(2) -0.014(2) 0.0170(19) C6 0.0261(14) 0.0350(16) 0.0264(14) 0.0074(12) -0.0101(11) -0.0056(12) C7 0.0282(15) 0.0408(18) 0.0289(15) 0.0020(13) 0.0015(12) -0.0057(13) C8 0.0341(17) 0.065(2) 0.0332(17) 0.0112(16) 0.0047(14) -0.0172(16) C9 0.0414(18) 0.047(2) 0.0261(15) 0.0128(14) -0.0030(13) -0.0162(15) C10 0.0256(16) 0.069(3) 0.0429(19) 0.0087(18) 0.0016(14) 0.0024(16) C11 0.055(2) 0.083(3) 0.037(2) 0.033(2) -0.0124(17) -0.022(2) C12 0.0292(16) 0.055(2) 0.0332(17) 0.0112(15) -0.0019(13) -0.0093(15) C13 0.0428(19) 0.056(2) 0.0328(17) 0.0123(16) 0.0042(15) -0.0167(17) C14 0.0412(18) 0.0384(18) 0.0262(15) 0.0080(13) -0.0003(13) -0.0031(14) C15 0.0271(17) 0.094(3) 0.049(2) 0.027(2) -0.0076(15) -0.0099(19) C16 0.061(2) 0.048(2) 0.0324(17) 0.0199(16) 0.0005(16) 0.0045(18) C17 0.0263(14) 0.0292(15) 0.0265(14) 0.0022(11) -0.0066(11) 0.0034(12) C18 0.0215(13) 0.0434(18) 0.0242(14) -0.0090(13) -0.0063(11) 0.0054(12) C19 0.0353(17) 0.0401(19) 0.0360(17) -0.0119(14) -0.0099(13) -0.0046(14) C20 0.0345(16) 0.0303(16) 0.0333(16) -0.0050(13) -0.0031(13) -0.0045(13) C21 0.0411(18) 0.054(2) 0.0342(17) -0.0091(16) -0.0181(14) 0.0135(16) C22 0.070(3) 0.0267(17) 0.053(2) -0.0019(16) -0.0151(19) -0.0115(17) 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 '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' 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 O1 Zn1 N7 114.86(15) . . ? O1B Zn1 N7 137.0(4) . . ? O1 Zn1 N1 137.04(15) . . ? O1B Zn1 N1 114.9(4) . . ? N7 Zn1 N1 108.04(10) . . ? O1 Zn1 N3 87.93(11) . . ? O1B Zn1 N3 83.1(4) . . ? N7 Zn1 N3 98.43(9) . . ? N1 Zn1 N3 88.10(10) . . ? O1 Zn1 N5 83.38(12) . . ? O1B Zn1 N5 87.8(4) . . ? N7 Zn1 N5 87.79(9) . . ? N1 Zn1 N5 96.35(10) . . ? N3 Zn1 N5 170.88(10) . . ? P1 O1 Zn1 155.5(3) . . ? O1 P1 C25 109.8(3) . . ? O1 P1 C27 112.1(2) . . ? C25 P1 C27 107.7(3) . . ? O1 P1 C23 111.9(3) . . ? C25 P1 C23 106.5(3) . . ? C27 P1 C23 108.7(3) . . ? C24 C23 P1 117.5(5) . . ? C24 C23 H23A 107.9 . . ? P1 C23 H23A 107.9 . . ? C24 C23 H23B 107.9 . . ? P1 C23 H23B 107.9 . . ? H23A C23 H23B 107.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 P1 115.6(5) . . ? C26 C25 H25A 108.4 . . ? P1 C25 H25A 108.4 . . ? C26 C25 H25B 108.4 . . ? P1 C25 H25B 108.4 . . ? H25A C25 H25B 107.4 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 P1 110.8(4) . . ? C28 C27 H27A 109.5 . . ? P1 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? P1 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? P1B O1B Zn1 152.7(10) . . ? O1B P1B C27B 118.7(9) . . ? O1B P1B C25B 106.5(9) . . ? C27B P1B C25B 109.7(9) . . ? O1B P1B C23B 107.8(9) . . ? C27B P1B C23B 104.1(8) . . ? C25B P1B C23B 109.8(8) . . ? C24B C23B P1B 119.7(12) . . ? C24B C23B H23C 107.4 . . ? P1B C23B H23C 107.4 . . ? C24B C23B H23D 107.4 . . ? P1B C23B H23D 107.4 . . ? H23C C23B H23D 106.9 . . ? C23B C24B H24D 109.5 . . ? C23B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C23B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C26B C25B P1B 111.2(11) . . ? C26B C25B H25C 109.4 . . ? P1B C25B H25C 109.4 . . ? C26B C25B H25D 109.4 . . ? P1B C25B H25D 109.4 . . ? H25C C25B H25D 108.0 . . ? C25B C26B H26D 109.5 . . ? C25B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C25B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C28B C27B P1B 110.7(11) . . ? C28B C27B H27C 109.5 . . ? P1B C27B H27C 109.5 . . ? C28B C27B H27D 109.5 . . ? P1B C27B H27D 109.5 . . ? H27C C27B H27D 108.1 . . ? C27B C28B H28D 109.5 . . ? C27B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C27B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? O5 Cl1 O2 114.1(6) . . ? O5 Cl1 O3 108.3(5) . . ? O2 Cl1 O3 106.6(4) . . ? O5 Cl1 O4 109.8(6) . . ? O2 Cl1 O4 109.4(6) . . ? O3 Cl1 O4 108.6(6) . . ? O2B Cl1B O5B 110.4(7) . . ? O2B Cl1B O3B 109.2(8) . . ? O5B Cl1B O3B 107.0(8) . . ? O2B Cl1B O4B 110.7(9) . . ? O5B Cl1B O4B 109.9(9) . . ? O3B Cl1B O4B 109.5(10) . . ? O7 Cl2 O8 112.3(6) . . ? O7 Cl2 O9 110.5(5) . . ? O8 Cl2 O9 111.0(5) . . ? O7 Cl2 O6 111.2(6) . . ? O8 Cl2 O6 104.6(5) . . ? O9 Cl2 O6 106.9(4) . . ? O8B Cl2B O9B 110.7(9) . . ? O8B Cl2B O7B 115.1(8) . . ? O9B Cl2B O7B 110.2(9) . . ? O8B Cl2B O6B 104.9(7) . . ? O9B Cl2B O6B 109.0(8) . . ? O7B Cl2B O6B 106.6(10) . . ? C1 N1 N2 105.6(3) . . ? C1 N1 Zn1 132.8(2) . . ? N2 N1 Zn1 119.29(18) . . ? C3 N2 N1 111.5(3) . . ? C3 N2 C6 129.8(3) . . ? N1 N2 C6 118.7(2) . . ? C7 N3 N4 105.7(2) . . ? C7 N3 Zn1 134.7(2) . . ? N4 N3 Zn1 119.29(17) . . ? C9 N4 N3 111.3(2) . . ? C9 N4 C6 129.8(2) . . ? N3 N4 C6 118.2(2) . . ? C12 N5 N6 105.6(2) . . ? C12 N5 Zn1 136.8(2) . . ? N6 N5 Zn1 117.51(18) . . ? C14 N6 N5 111.4(2) . . ? C14 N6 C17 129.4(3) . . ? N5 N6 C17 118.4(2) . . ? C20 N7 N8 105.5(2) . . ? C20 N7 Zn1 134.1(2) . . ? N8 N7 Zn1 119.76(18) . . ? C18 N8 N7 110.9(2) . . ? C18 N8 C17 130.3(2) . . ? N7 N8 C17 118.7(2) . . ? N1 C1 C2 109.3(3) . . ? N1 C1 C4 121.3(3) . . ? C2 C1 C4 129.4(3) . . ? C3 C2 C1 107.9(3) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? N2 C3 C2 105.7(3) . . ? N2 C3 C5 122.5(4) . . ? C2 C3 C5 131.7(4) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 N4 111.4(2) . . ? N2 C6 H6A 109.3 . . ? N4 C6 H6A 109.3 . . ? N2 C6 H6B 109.3 . . ? N4 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? N3 C7 C8 109.5(3) . . ? N3 C7 C10 121.2(3) . . ? C8 C7 C10 129.3(3) . . ? C9 C8 C7 107.3(3) . . ? C9 C8 H8 126.4 . . ? C7 C8 H8 126.4 . . ? N4 C9 C8 106.2(3) . . ? N4 C9 C11 121.5(3) . . ? C8 C9 C11 132.3(3) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N5 C12 C13 109.9(3) . . ? N5 C12 C15 121.2(3) . . ? C13 C12 C15 128.9(3) . . ? C14 C13 C12 106.7(3) . . ? C14 C13 H13 126.6 . . ? C12 C13 H13 126.6 . . ? N6 C14 C13 106.4(3) . . ? N6 C14 C16 122.6(3) . . ? C13 C14 C16 131.0(3) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 N8 111.3(2) . . ? N6 C17 H17A 109.4 . . ? N8 C17 H17A 109.4 . . ? N6 C17 H17B 109.4 . . ? N8 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N8 C18 C19 106.5(3) . . ? N8 C18 C21 122.2(3) . . ? C19 C18 C21 131.3(3) . . ? C18 C19 C20 107.1(3) . . ? C18 C19 H19 126.4 . . ? C20 C19 H19 126.4 . . ? N7 C20 C19 109.9(3) . . ? N7 C20 C22 121.6(3) . . ? C19 C20 C22 128.4(3) . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? 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 O1 1.982(3) . ? Zn1 O1B 2.021(10) . ? Zn1 N7 2.050(2) . ? Zn1 N1 2.060(2) . ? Zn1 N3 2.118(2) . ? Zn1 N5 2.149(2) . ? O1 P1 1.494(3) . ? P1 C25 1.794(6) . ? P1 C27 1.795(5) . ? P1 C23 1.799(6) . ? C23 C24 1.488(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.465(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.524(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O1B P1B 1.501(8) . ? P1B C27B 1.790(9) . ? P1B C25B 1.790(10) . ? P1B C23B 1.798(10) . ? C23B C24B 1.454(12) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? C25B C26B 1.489(13) . ? C25B H25C 0.9900 . ? C25B H25D 0.9900 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? C27B C28B 1.548(11) . ? C27B H27C 0.9900 . ? C27B H27D 0.9900 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? Cl1 O5 1.404(5) . ? Cl1 O2 1.416(5) . ? Cl1 O3 1.428(5) . ? Cl1 O4 1.443(5) . ? Cl1B O2B 1.412(7) . ? Cl1B O5B 1.416(8) . ? Cl1B O3B 1.417(8) . ? Cl1B O4B 1.437(7) . ? Cl2 O7 1.405(6) . ? Cl2 O8 1.406(6) . ? Cl2 O9 1.417(4) . ? Cl2 O6 1.438(5) . ? Cl2B O8B 1.397(8) . ? Cl2B O9B 1.408(8) . ? Cl2B O7B 1.411(8) . ? Cl2B O6B 1.441(8) . ? N1 C1 1.345(4) . ? N1 N2 1.357(3) . ? N2 C3 1.354(4) . ? N2 C6 1.436(4) . ? N3 C7 1.332(4) . ? N3 N4 1.361(3) . ? N4 C9 1.352(4) . ? N4 C6 1.436(4) . ? N5 C12 1.326(4) . ? N5 N6 1.372(3) . ? N6 C14 1.349(4) . ? N6 C17 1.437(4) . ? N7 C20 1.337(4) . ? N7 N8 1.370(3) . ? N8 C18 1.358(4) . ? N8 C17 1.443(4) . ? C1 C2 1.379(5) . ? C1 C4 1.491(5) . ? C2 C3 1.362(6) . ? C2 H2 0.9500 . ? C3 C5 1.489(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.393(4) . ? C7 C10 1.489(4) . ? C8 C9 1.356(5) . ? C8 H8 0.9500 . ? C9 C11 1.496(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.403(4) . ? C12 C15 1.492(5) . ? C13 C14 1.365(5) . ? C13 H13 0.9500 . ? C14 C16 1.499(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.361(5) . ? C18 C21 1.487(4) . ? C19 C20 1.390(4) . ? C19 H19 0.9500 . ? C20 C22 1.491(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ?