#------------------------------------------------------------------------------ #$Date: 2022-11-07 12:58:22 +0200 (Mon, 07 Nov 2022) $ #$Revision: 279031 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/51/1565163.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_1565163 loop_ _publ_author_name 'Soldevila-Sanmart\'in, Joan' 'Guerrero, Miguel' 'Choquesillo-Lazarte, Duane' 'Giner Planas, Jos\'e' 'Pons, Josefina' _publ_section_title ; Dimeric metallacycles and coordination polymers: Zn(II), Cd(II) and Hg(II) complexes of two positional isomers of a flexible N,O-hybrid bispyrazole derived ligand ; _journal_name_full 'Inorganica Chimica Acta' _journal_page_first 119549 _journal_paper_doi 10.1016/j.ica.2020.119549 _journal_volume 506 _journal_year 2020 _chemical_formula_moiety 'C22 H30 Cl2 N4 O2 Zn, 0.5(H2 O)' _chemical_formula_sum 'C22 H31 Cl2 N4 O2.5 Zn' _chemical_formula_weight 527.77 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 122.071(7) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 29.965(4) _cell_length_b 8.0447(12) _cell_length_c 23.742(4) _cell_measurement_reflns_used 5454 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 66.651 _cell_measurement_theta_min 3.481 _cell_volume 4849.8(13) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2016)' _computing_data_collection 'Bruker Apex3, 2016' _computing_data_reduction 'SAINT V8.38A (Bruker, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator multilayer _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_unetI/netI 0.0583 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 15452 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 66.860 _diffrn_reflns_theta_max 66.860 _diffrn_reflns_theta_min 3.481 _diffrn_source 'high brilliance microfocus sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.665 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.6573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0741 before and 0.0615 after correction. The Ratio of minimum to maximum transmission is 0.8731. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.446 _exptl_crystal_description block _exptl_crystal_F_000 2200 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.356 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.085 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 289 _refine_ls_number_reflns 4279 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0452 _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^)+(0.0290P)^2^+16.1725P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.1033 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3077 _reflns_number_total 4279 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ICA-2020-506-1195465.cif _cod_data_source_block js109_7 _cod_depositor_comments ; 2022-11-07 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_formula_sum 'C44 H62 Cl4 N8 O5 Zn2' _cod_original_formula_weight 1055.55 _cod_original_formula_moiety '2(C22 H30 Cl2 N4 O2 Zn), H2 O' _cod_original_formula_units_Z 4 _cod_original_cell_volume 4849.9(12) _cod_database_code 1565163 _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 0.758 _shelx_estimated_absorpt_t_min 0.711 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Riding coordinates: O3(H3A) 2.b Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C7(H7A,H7B), C6(H6A,H6B), C17(H17A,H17B), C15(H15A,H15B), C16(H16A,H16B) 2.c Aromatic/amide H refined with riding coordinates: C20(H20), C13(H13), C3(H3), C10(H10), C12(H12), C11(H11) 2.d Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C22(H22A,H22B,H22C), C2(H2A,H2B,H2C), C19(H19A,H19B,H19C) ; _shelx_res_file ; TITL JS109_7.res in C2/c js109_7.res created by SHELXL-2016/6 at 14:18:34 on 12-Mar-2018 CELL 1.54178 29.965 8.0447 23.7424 90 122.071 90 ZERR 4 0.0037 0.0012 0.0037 0 0.007 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl N O Zn UNIT 176 248 16 32 20 8 L.S. 10 PLAN 20 SIZE 0.1 0.08 0.08 TEMP -173.15 BOND $H LIST 4 fmap 2 acta REM REM REM WGHT 0.029000 16.172501 FVAR 0.20596 ZN1 6 0.406458 0.735547 0.837875 11.00000 0.02151 0.02323 = 0.02217 -0.00003 0.01083 -0.00037 CL2 3 0.487835 0.665120 0.861826 11.00000 0.02418 0.03538 = 0.03168 0.00211 0.01322 0.00535 CL1 3 0.354845 0.511642 0.797884 11.00000 0.03294 0.02751 = 0.02807 -0.00387 0.01258 -0.00833 O2 5 0.346656 0.453545 0.494104 11.00000 0.03706 0.02952 = 0.03295 0.00084 0.02390 0.00613 O1 5 0.382639 0.882654 0.627515 11.00000 0.03021 0.02680 = 0.02250 -0.00078 0.01048 0.00404 N3 4 0.416768 0.164927 0.423502 11.00000 0.02661 0.02129 = 0.02305 -0.00264 0.01385 0.00148 N2 4 0.387461 1.021169 0.740892 11.00000 0.02244 0.02656 = 0.02456 0.00232 0.01509 0.00029 N4 4 0.424125 0.257386 0.476552 11.00000 0.02784 0.02449 = 0.02345 0.00068 0.01406 0.00174 N1 4 0.368527 0.920275 0.770185 11.00000 0.02199 0.02550 = 0.02409 -0.00093 0.01445 -0.00015 O3 5 0.500000 0.408670 0.750000 10.50000 0.08504 0.07346 = 0.06102 0.00000 0.04792 0.00000 AFIX 3 H3A 2 0.494320 0.454950 0.784020 11.00000 -1.50000 AFIX 0 C20 1 0.440814 0.000939 0.511333 11.00000 0.02801 0.02722 = 0.02806 0.01088 0.01428 0.00149 AFIX 43 H20 2 0.449716 -0.095668 0.538248 11.00000 -1.20000 AFIX 0 C14 1 0.289921 0.698349 0.463840 11.00000 0.02944 0.02986 = 0.02979 -0.00282 0.01989 0.00013 C9 1 0.323212 0.811948 0.513354 11.00000 0.02267 0.03119 = 0.02396 -0.00130 0.01231 0.00262 C18 1 0.438693 0.159828 0.529967 11.00000 0.02772 0.03406 = 0.02476 0.00534 0.01519 0.00031 C13 1 0.251649 0.757587 0.401200 11.00000 0.02592 0.04442 = 0.03017 -0.00572 0.01297 0.00272 AFIX 43 H13 2 0.228566 0.680995 0.367896 11.00000 -1.20000 AFIX 0 C3 1 0.311677 1.127519 0.715596 11.00000 0.02730 0.02893 = 0.02744 -0.00290 0.01364 0.00509 AFIX 43 H3 2 0.281707 1.197665 0.698466 11.00000 -1.20000 AFIX 0 C8 1 0.364552 0.749942 0.580555 11.00000 0.02796 0.02977 = 0.02650 -0.00410 0.01299 0.00195 AFIX 23 H8A 2 0.349847 0.660143 0.594484 11.00000 -1.20000 H8B 2 0.394425 0.703689 0.578841 11.00000 -1.20000 AFIX 0 C4 1 0.353481 1.146280 0.706551 11.00000 0.02883 0.02111 = 0.02359 0.00057 0.01297 0.00414 C1 1 0.321944 0.987157 0.754326 11.00000 0.02112 0.02850 = 0.02153 0.00137 0.00776 0.00148 C7 1 0.420581 0.827875 0.692251 11.00000 0.02648 0.03173 = 0.02600 0.00088 0.01453 0.00634 AFIX 23 H7A 2 0.452733 0.790226 0.693959 11.00000 -1.20000 H7B 2 0.406493 0.733555 0.704954 11.00000 -1.20000 AFIX 0 C6 1 0.433491 0.971920 0.739490 11.00000 0.02213 0.03677 = 0.02314 -0.00107 0.01345 -0.00059 AFIX 23 H6A 2 0.462111 0.939210 0.784726 11.00000 -1.20000 H6B 2 0.446014 1.067313 0.725197 11.00000 -1.20000 AFIX 0 C10 1 0.317449 0.981132 0.498171 11.00000 0.02970 0.03043 = 0.03133 -0.00227 0.01576 -0.00277 AFIX 43 H10 2 0.339809 1.059252 0.531281 11.00000 -1.20000 AFIX 0 C5 1 0.363694 1.273273 0.669281 11.00000 0.04836 0.02934 = 0.04544 0.00924 0.03115 0.00825 AFIX 137 H5A 2 0.398490 1.322834 0.698673 11.00000 -1.50000 H5B 2 0.336697 1.360123 0.653226 11.00000 -1.50000 H5C 2 0.362630 1.220618 0.631364 11.00000 -1.50000 AFIX 0 C17 1 0.414463 0.435712 0.469818 11.00000 0.03777 0.02037 = 0.02762 -0.00115 0.01891 -0.00054 AFIX 23 H17A 2 0.424593 0.481025 0.439382 11.00000 -1.20000 H17B 2 0.437239 0.488686 0.513772 11.00000 -1.20000 AFIX 0 C15 1 0.295496 0.513850 0.476120 11.00000 0.03143 0.02659 = 0.03700 -0.00750 0.01790 -0.00302 AFIX 23 H15A 2 0.289405 0.487364 0.512234 11.00000 -1.20000 H15B 2 0.268233 0.455747 0.435468 11.00000 -1.20000 AFIX 0 C16 1 0.357769 0.481703 0.443653 11.00000 0.03914 0.03012 = 0.03085 0.00047 0.02114 0.00782 AFIX 23 H16A 2 0.351818 0.600172 0.430345 11.00000 -1.20000 H16B 2 0.334007 0.413536 0.404079 11.00000 -1.20000 AFIX 0 C21 1 0.427493 0.006749 0.445480 11.00000 0.02382 0.02197 = 0.03007 0.00089 0.01246 0.00166 C12 1 0.246556 0.925532 0.386487 11.00000 0.03161 0.03755 = 0.02360 0.00285 0.01215 0.00922 AFIX 43 H12 2 0.220730 0.963890 0.343311 11.00000 -1.20000 AFIX 0 C11 1 0.279435 1.036235 0.435285 11.00000 0.03757 0.02795 = 0.03234 0.00740 0.01755 0.00650 AFIX 43 H11 2 0.276009 1.151849 0.425709 11.00000 -1.20000 AFIX 0 C22 1 0.425772 -0.133452 0.403428 11.00000 0.03826 0.02340 = 0.03791 0.00270 0.01590 0.00322 AFIX 137 H22A 2 0.389071 -0.165501 0.372115 11.00000 -1.50000 H22B 2 0.445171 -0.228492 0.431801 11.00000 -1.50000 H22C 2 0.441943 -0.098643 0.378690 11.00000 -1.50000 AFIX 0 C2 1 0.290064 0.912682 0.779277 11.00000 0.02708 0.04313 = 0.04524 0.00535 0.02255 0.00245 AFIX 137 H2A 2 0.290396 0.791303 0.776012 11.00000 -1.50000 H2B 2 0.253726 0.953068 0.752431 11.00000 -1.50000 H2C 2 0.305116 0.944728 0.825788 11.00000 -1.50000 AFIX 0 C19 1 0.450550 0.227443 0.594881 11.00000 0.04675 0.04605 = 0.02835 0.00826 0.02331 0.00941 AFIX 137 H19A 2 0.482950 0.293473 0.615026 11.00000 -1.50000 H19B 2 0.455178 0.135402 0.624565 11.00000 -1.50000 H19C 2 0.421328 0.297968 0.587788 11.00000 -1.50000 AFIX 0 HKLF 4 REM JS109_7.res in C2/c REM R1 = 0.0452 for 3077 Fo > 4sig(Fo) and 0.0766 for all 4279 data REM 289 parameters refined using 0 restraints END WGHT 0.0290 16.1586 REM Highest difference peak 0.356, deepest hole -0.527, 1-sigma level 0.085 Q1 1 0.4330 0.5903 0.8196 11.00000 0.05 0.36 Q2 1 0.1973 0.8487 0.3825 11.00000 0.05 0.35 Q3 1 0.4248 0.5178 0.7786 11.00000 0.05 0.35 Q4 1 0.4439 0.7500 0.8084 11.00000 0.05 0.35 Q5 1 0.4199 0.5818 0.8689 11.00000 0.05 0.34 Q6 1 0.3548 0.9115 0.4805 11.00000 0.05 0.33 Q7 1 0.4327 0.8633 0.8170 11.00000 0.05 0.30 Q8 1 0.3864 0.9044 0.8029 11.00000 0.05 0.30 Q9 1 0.2316 1.0794 0.7200 11.00000 0.05 0.29 Q10 1 0.2979 1.2459 0.5686 11.00000 0.05 0.29 Q11 1 0.4428 0.5560 0.7507 11.00000 0.05 0.29 Q12 1 0.4672 0.7818 0.8921 11.00000 0.05 0.28 Q13 1 0.3252 0.6587 0.8062 11.00000 0.05 0.28 Q14 1 0.3319 1.2990 0.6170 11.00000 0.05 0.28 Q15 1 0.2988 0.6223 0.5683 11.00000 0.05 0.28 Q16 1 0.2455 0.4614 0.4993 11.00000 0.05 0.28 Q17 1 0.1999 0.8433 0.3215 11.00000 0.05 0.28 Q18 1 0.3135 1.5319 0.6092 11.00000 0.05 0.28 Q19 1 0.3961 0.1670 0.3774 11.00000 0.05 0.28 Q20 1 0.4557 0.6555 0.8911 11.00000 0.05 0.28 ; _shelx_res_checksum 1959 _shelx_hkl_file ; -2 0 0 348.068 10.2751 1 2 0 0 343.990 12.8569 7 2 0 0 319.012 12.5755 5 -2 0 0 330.060 12.5078 5 -2 0 0 346.499 12.8056 7 -4 0 0 6132.65 179.166 5 4 0 0 6234.74 179.230 5 -4 0 0 5874.81 174.164 1 -4 0 0 6300.69 179.025 7 -4 0 0 6063.89 174.012 1 -6 0 0 1625.02 44.7033 1 -6 0 0 1476.69 51.5008 7 -6 0 0 1477.37 52.4839 5 6 0 0 1498.33 52.2785 5 -6 0 0 1478.27 44.5829 1 -8 0 0 7.48354 6.87742 7 -8 0 0 10.9850 2.80888 1 -8 0 0 13.5877 2.29473 1 8 0 0 2.67557 12.8132 5 -10 0 0 143.774 5.92909 1 -10 0 0 144.725 6.07161 1 -10 0 0 145.550 15.5762 7 10 0 0 142.023 21.9456 5 -12 0 0 1455.73 61.0700 7 12 0 0 1524.86 65.1437 5 -14 0 0 1659.80 72.4953 7 14 0 0 1852.76 87.0815 5 -14 0 0 1747.03 59.4686 2 -16 0 0 30.6012 13.4004 6 16 0 0 155.057 56.5517 5 -18 0 0 596.728 31.4341 2 -18 0 0 674.753 30.1578 6 -20 0 0 234.610 21.7266 6 -20 0 0 247.301 18.8794 2 -22 0 0 193.354 24.6945 6 -22 0 0 207.339 18.1178 2 -24 0 0 33.5867 14.2349 2 -26 0 0 275.148 18.8128 2 -28 0 0 47.2058 10.0793 2 -30 0 0 88.2536 10.8498 2 1 -1 0 417.155 15.9247 7 -1 -1 0 417.881 14.8288 1 -1 -1 0 411.323 14.1113 5 1 -1 0 420.197 15.1959 1 -1 1 0 387.403 15.3797 1 -1 1 0 419.931 17.0006 5 -1 1 0 433.444 15.3190 7 3 -1 0 36.0331 9.37873 5 3 -1 0 29.4361 4.96883 1 -3 -1 0 32.9261 3.90603 1 -3 1 0 36.7110 6.78843 7 3 1 0 26.2528 6.26785 7 -3 1 0 34.7328 6.76887 5 5 -1 0 455.061 24.5424 5 -5 -1 0 464.136 16.1497 1 5 -1 0 475.197 18.9878 1 -5 1 0 485.731 18.0420 1 -5 1 0 482.441 25.0230 5 -5 1 0 460.280 21.2284 7 5 1 0 474.565 16.6699 5 7 -1 0 4479.52 143.312 5 -7 -1 0 4304.11 130.352 1 -7 -1 0 4624.20 137.743 7 7 1 0 4546.79 134.496 5 -7 1 0 4408.86 139.614 7 -7 1 0 4797.71 133.003 1 -9 -1 0 169.023 17.5185 7 9 -1 0 196.696 29.8115 5 -9 -1 0 206.779 8.13055 1 -9 -1 0 206.386 8.63893 1 9 1 0 183.491 18.1822 5 -9 1 0 197.590 19.5624 7 -9 1 0 208.856 12.2419 1 11 -1 0 97.1522 28.2028 5 11 1 0 46.3560 17.3211 5 -11 1 0 53.1332 6.50383 1 -11 1 0 68.4878 8.53109 1 -11 1 0 66.3201 15.1037 7 -13 -1 0 915.133 34.5087 6 13 -1 0 972.497 60.4048 5 -13 1 0 931.718 31.1966 1 13 1 0 953.077 46.7858 5 -13 1 0 959.349 37.4181 2 -13 1 0 877.218 48.9604 7 -13 1 0 1008.13 32.0084 1 15 -1 0 -51.597 51.9727 5 -15 -1 0 1.23357 11.0151 6 -15 -1 0 16.1810 9.01573 2 -15 1 0 -13.341 27.2789 7 15 1 0 12.1588 37.6470 5 -15 1 0 15.1418 9.42548 2 -17 -1 0 1366.72 46.6694 6 -17 -1 0 1314.19 47.6524 2 17 -1 0 1271.92 101.950 5 -17 1 0 1263.12 76.7689 7 -17 1 0 1236.80 48.1546 2 -19 -1 0 132.940 19.3339 2 -19 -1 0 137.062 14.5983 6 -19 1 0 131.939 15.0723 2 -21 -1 0 427.758 24.9995 2 -21 -1 0 447.615 26.2247 6 -21 1 0 465.493 26.4683 2 -23 -1 0 24.5046 11.9139 2 -23 -1 0 16.9914 11.7858 6 -23 1 0 18.0931 11.7457 2 -25 -1 0 -13.148 9.78308 6 -25 -1 0 5.99639 9.65456 2 -25 1 0 8.09841 9.52954 2 -27 -1 0 18.9477 13.7819 2 -27 1 0 13.4081 9.32133 2 -29 1 0 5.57678 8.48897 2 0 -2 0 30.9851 5.29539 1 0 -2 0 29.4295 8.09658 5 0 2 0 25.8876 5.24790 7 -2 -2 0 2219.95 67.0276 5 2 -2 0 2242.81 69.6289 1 2 -2 0 2156.88 74.2963 5 -2 -2 0 2225.09 68.4009 1 -2 2 0 2232.60 69.1000 7 -4 -2 0 29.8566 5.54824 1 4 -2 0 37.0290 8.85326 1 4 -2 0 28.9262 10.7090 5 -4 2 0 6.64800 12.9040 1 -4 2 0 37.4966 8.91810 7 6 -2 0 2179.85 82.6246 5 -6 -2 0 2243.62 70.1206 1 6 -2 0 2398.43 74.4281 1 -6 2 0 2328.62 76.7301 7 8 -2 0 18.9825 16.3208 5 8 -2 0 -3.6829 18.6117 1 -8 -2 0 33.7487 5.13259 1 -8 2 0 32.6202 10.0224 7 -8 2 0 32.2928 8.61022 1 10 -2 0 2020.86 88.0619 5 -10 -2 0 1895.05 60.6005 1 -10 2 0 1962.68 66.5777 1 -10 2 0 2071.76 77.1731 7 12 -2 0 873.382 70.4731 5 -12 -2 0 838.865 27.7872 1 -12 -2 0 882.278 33.3491 6 -12 -2 0 843.614 27.5571 1 -12 2 0 846.815 33.4373 2 -12 2 0 867.239 47.1925 7 -12 2 0 840.809 34.9743 1 -14 -2 0 375.144 24.5684 2 14 -2 0 402.709 27.1784 3 14 -2 0 323.233 65.8708 5 -14 -2 0 419.915 22.2341 6 -14 2 0 409.461 21.5777 2 -14 2 0 373.766 23.1624 1 -14 2 0 397.996 21.8076 1 -14 2 0 415.444 38.3974 7 -16 -2 0 364.585 21.0027 2 -16 -2 0 340.864 20.1439 6 -16 2 0 447.613 54.2058 7 -16 2 0 362.185 19.2137 1 -16 2 0 406.986 25.0056 2 -16 2 0 419.889 22.7234 1 -18 -2 0 114.288 18.6114 2 -18 -2 0 91.3636 12.9766 6 -18 2 0 110.811 14.8491 2 -18 2 0 91.1507 35.7057 7 -20 -2 0 13.0068 16.1996 2 -20 -2 0 38.5489 10.9209 6 -20 2 0 42.5140 12.3942 2 -22 -2 0 324.255 23.6662 6 -22 -2 0 361.726 22.9320 2 -22 2 0 351.013 24.1198 2 -24 -2 0 175.639 15.5863 6 -24 -2 0 205.971 20.4511 2 -24 2 0 187.337 18.0699 2 -26 -2 0 256.655 19.8604 6 -26 2 0 249.784 18.7660 2 -28 2 0 271.404 17.5539 2 -1 -3 0 -4.6706 7.09028 1 1 -3 0 -0.8327 8.98869 1 1 -3 0 -3.7249 10.1209 5 -1 -3 0 4.09631 7.63213 5 -1 3 0 6.81354 7.14356 7 1 3 0 0.79434 5.49163 7 3 -3 0 1879.06 63.1598 1 -3 -3 0 1776.85 60.3133 1 -3 -3 0 1816.04 56.5615 5 3 -3 0 1752.15 69.0113 5 3 3 0 1822.92 56.0845 7 -3 3 0 1803.44 60.9405 7 5 -3 0 343.285 37.6536 5 5 -3 0 329.488 20.9794 1 -5 -3 0 310.201 16.6720 1 -5 3 0 304.613 19.6788 7 7 -3 0 55.3415 21.9495 5 7 -3 0 94.4152 20.0313 1 -7 -3 0 64.1542 10.0053 1 -7 3 0 97.9228 17.2380 7 -9 -3 0 697.197 28.7795 1 9 -3 0 721.342 63.2415 5 -9 -3 0 713.212 29.7961 6 -9 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41.4867 15.1204 1 2 -4 0 23.8873 20.4570 5 -2 -4 0 34.5142 19.4354 5 -2 4 0 29.7097 11.7053 7 2 4 0 36.6278 9.60297 3 -2 4 0 44.7433 9.60894 3 4 -4 0 1544.99 61.0546 1 -4 -4 0 1401.51 56.9616 1 4 -4 0 1637.69 73.4750 5 -4 4 0 1470.04 51.8640 3 4 4 0 1532.18 51.0385 3 -4 4 0 1512.14 57.4670 7 -6 -4 0 623.561 33.4297 1 -6 -4 0 742.860 29.7016 8 -6 -4 0 700.648 29.9084 6 6 -4 0 724.410 56.9801 5 -6 4 0 672.053 36.1079 7 -6 4 0 671.013 28.5671 3 6 4 0 695.407 30.0678 3 -8 -4 0 36.6056 13.7994 1 -8 -4 0 54.8386 13.0204 6 -8 -4 0 82.2968 13.7055 8 8 -4 0 20.7374 51.5576 5 -8 4 0 69.9536 22.8422 7 8 4 0 54.9793 10.4279 3 -8 4 0 41.2948 15.7937 2 -10 -4 0 37.6477 13.6438 8 -10 -4 0 10.8723 12.3910 1 10 -4 0 -58.016 67.4931 5 -10 -4 0 4.21121 12.1330 6 10 4 0 9.77333 13.6464 3 -10 4 0 53.3365 25.3987 7 -10 4 0 20.1047 10.6656 2 -12 -4 0 118.120 13.6857 6 -12 -4 0 121.847 16.4945 8 -12 -4 0 119.226 16.2283 1 -12 4 0 127.693 32.6232 7 12 4 0 118.830 17.7900 3 -12 4 0 133.757 18.3165 2 -14 -4 0 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6 8 -2 -24 173.407 17.9584 8 -8 -2 24 198.208 25.7851 4 6 -2 -24 112.763 12.1663 6 -6 -2 24 99.8243 17.5005 4 6 -2 -24 114.646 16.0262 8 4 -2 -24 170.760 15.5295 8 -4 -2 24 149.441 24.7375 4 4 2 -24 132.447 15.9752 8 2 -2 -24 -0.1552 7.38413 8 2 -2 -24 25.2329 7.92605 6 2 2 -24 -8.2309 8.60831 8 27 -3 -24 -9.8304 9.42721 6 -27 3 24 -20.021 15.5520 4 27 3 -24 1.29904 12.3439 3 25 -3 -24 0.60332 8.74063 6 -25 3 24 4.25589 14.8450 4 25 3 -24 -6.2142 9.86415 3 23 -3 -24 93.5279 12.4836 6 -23 -3 24 75.3322 29.7230 4 -23 3 24 96.8250 17.9233 4 -21 -3 24 -15.687 16.4417 4 21 -3 -24 8.19073 8.64421 6 -21 3 24 33.4179 15.9153 4 -19 -3 24 27.2348 15.9936 4 19 -3 -24 -1.9840 8.16787 6 -19 3 24 -17.883 15.0463 4 17 -3 -24 91.2303 12.1936 6 -17 -3 24 87.1207 23.6701 4 -17 3 24 59.1707 24.1557 4 15 -3 -24 2.51680 11.8029 6 -15 -3 24 27.1482 20.8413 4 -15 3 24 6.71180 18.3038 4 -13 -3 24 4.10265 13.9960 4 13 -3 -24 -0.7138 11.5053 6 11 -3 -24 146.223 15.7269 6 -11 -3 24 139.203 23.4932 4 -9 -3 24 12.9312 19.4811 4 9 -3 -24 13.1277 8.60234 6 9 -3 -24 15.6250 13.2268 8 7 -3 -24 35.2095 9.53386 8 -7 -3 24 15.4386 14.1644 4 7 -3 -24 29.6714 12.4750 6 -5 -3 24 12.7708 15.7292 4 5 -3 -24 3.64399 7.64757 8 5 -3 -24 13.9061 7.57455 6 22 -4 -24 20.7865 10.0060 6 -22 4 24 17.5782 7.83797 3 20 -4 -24 57.8474 10.5548 6 18 -4 -24 -19.952 8.46657 6 16 -4 -24 154.602 16.6928 6 14 -4 -24 84.0486 11.1602 6 -14 -4 24 54.2406 17.5863 4 12 -4 -24 49.1623 13.0589 6 -12 -4 24 60.7439 17.5230 4 10 -4 -24 39.2496 12.3649 6 -10 -4 24 27.2732 16.7776 4 8 -4 -24 1.85665 6.92172 6 -19 5 24 75.1238 9.90052 3 -17 5 24 30.6374 9.83127 3 15 -5 -24 3.52729 8.24438 6 -15 5 24 28.1545 7.24310 3 -13 5 24 19.7031 6.89617 3 30 0 -25 23.5674 13.0420 3 -30 0 25 -3.0086 6.91363 2 -28 0 25 38.0341 23.7564 4 28 0 -25 6.97183 9.77884 3 -26 0 25 22.5927 22.1928 4 -24 0 25 42.6978 20.7239 4 -22 0 25 0.63079 14.1374 4 -20 0 25 4.79540 14.2390 4 -18 0 25 14.3407 14.4958 4 -16 0 25 22.5103 21.0780 4 14 0 -25 5.38301 8.05587 6 -14 0 25 -4.4725 15.3454 4 -12 0 25 -3.5423 15.0396 4 -10 0 25 18.5849 21.7872 4 -8 0 25 18.0695 22.7058 4 8 0 -25 -3.1126 12.6537 6 6 0 -25 18.5154 13.2793 6 -6 0 25 16.4400 18.8496 4 6 0 -25 30.3330 13.0423 8 4 0 -25 31.7747 12.9232 8 29 -1 -25 99.7962 13.1829 3 -29 1 25 66.5191 10.0984 2 29 1 -25 102.586 12.1023 3 -27 -1 25 -7.0441 16.8866 4 -27 1 25 1.13031 8.09655 2 27 1 -25 -16.612 13.9904 3 -25 -1 25 35.7797 15.8895 4 -25 1 25 67.0113 15.7402 4 -23 -1 25 47.7063 16.3760 4 -23 1 25 68.8181 22.0089 4 -21 -1 25 25.2306 20.7932 4 -21 1 25 49.4147 21.2592 4 -19 -1 25 569.308 33.6952 4 -19 1 25 502.879 37.3106 4 -17 -1 25 152.657 21.9588 4 -17 1 25 143.550 20.9689 4 -15 -1 25 51.7192 16.3652 4 15 -1 -25 51.8646 12.9101 6 -15 1 25 66.3630 17.6260 4 13 -1 -25 259.365 17.0518 6 -13 -1 25 227.257 28.0280 4 13 1 -25 242.278 16.8352 6 -13 1 25 282.864 24.8491 4 -11 -1 25 51.1279 21.1508 4 11 -1 -25 112.892 14.6182 6 -11 1 25 80.8019 24.9958 4 11 1 -25 74.9337 14.5225 6 9 -1 -25 184.888 17.0304 6 -9 -1 25 187.163 21.3458 4 9 1 -25 173.940 18.3745 6 7 -1 -25 127.996 15.6981 8 7 -1 -25 89.6934 11.8269 6 5 -1 -25 -12.680 8.88119 8 5 -1 -25 -8.2716 11.3803 6 3 -1 -25 28.4315 8.33477 8 28 2 -25 -4.8575 9.73572 3 -26 2 25 -21.610 13.6394 4 -24 -2 25 -51.214 22.3397 4 -24 2 25 12.8201 20.3560 4 -22 -2 25 18.4549 22.2325 4 -22 2 25 50.2317 20.7751 4 -20 -2 25 20.3031 15.0193 4 -20 2 25 18.2626 14.8799 4 18 -2 -25 -7.8814 10.6579 6 -18 -2 25 15.3126 20.7984 4 -18 2 25 11.5141 21.8740 4 -16 -2 25 -10.814 19.3577 4 16 -2 -25 0.30924 7.68903 6 -16 2 25 -33.198 15.1466 4 -14 -2 25 90.5269 17.5630 4 14 -2 -25 133.957 13.3856 6 -14 2 25 97.3249 25.3783 4 14 2 -25 116.577 16.8300 6 -12 -2 25 8.83372 13.7482 4 12 -2 -25 -13.918 10.4431 6 -12 2 25 -1.9115 18.0550 4 -10 -2 25 7.72370 13.3493 4 10 -2 -25 14.1784 8.27256 6 -8 -2 25 -35.529 19.6527 4 8 -2 -25 7.62526 7.81774 6 8 -2 -25 8.58662 9.35138 8 6 -2 -25 29.0833 9.05507 8 -6 -2 25 24.1606 23.4804 4 6 -2 -25 4.95600 7.65549 6 25 -3 -25 84.0452 10.5916 6 23 -3 -25 4.13381 11.6249 6 -23 3 25 -13.679 15.8776 4 21 -3 -25 32.0294 9.16358 6 -21 -3 25 -16.876 17.9665 4 -21 3 25 17.7270 16.3612 4 19 -3 -25 26.7100 8.84566 6 -19 -3 25 32.7183 17.2322 4 -19 3 25 54.5569 17.4580 4 -17 -3 25 30.5916 22.7737 4 17 -3 -25 8.41045 8.67876 6 -17 3 25 -20.950 18.2480 4 -15 -3 25 14.8885 15.5182 4 15 -3 -25 4.27353 11.3375 6 13 -3 -25 132.915 16.0583 6 -13 -3 25 153.671 19.3316 4 -11 -3 25 -4.5143 14.1754 4 11 -3 -25 16.4654 11.4372 6 9 -3 -25 125.511 12.6166 6 -9 -3 25 203.260 27.0873 4 7 -3 -25 -7.2170 10.7047 8 7 -3 -25 25.1574 7.45628 6 22 -4 -25 -10.644 9.29847 6 -22 4 25 -12.620 7.44679 3 20 -4 -25 83.8022 10.7975 6 18 -4 -25 -25.352 10.9436 6 16 -4 -25 21.8531 11.2882 6 14 -4 -25 -8.6964 7.21874 6 12 -4 -25 -2.9356 6.61906 6 -28 0 26 86.6805 10.1465 2 -26 0 26 51.1521 16.3984 4 -24 0 26 206.038 21.7404 4 -22 0 26 229.661 22.6360 4 -20 0 26 377.896 27.5812 4 -18 0 26 498.612 30.9404 4 -16 0 26 42.8895 15.8871 4 16 0 -26 69.0608 10.6527 6 -14 0 26 31.0135 20.8389 4 14 0 -26 49.9851 9.64480 6 -12 0 26 24.3270 15.0091 4 12 0 -26 -14.440 11.2342 6 10 0 -26 25.0807 8.80840 6 -10 0 26 56.0456 24.1185 4 8 0 -26 5.10900 8.83733 6 -27 1 26 26.8588 16.5972 4 -27 1 26 7.26232 8.86400 2 -25 -1 26 17.4035 22.7789 4 -25 1 26 61.7511 21.5672 4 -23 -1 26 23.6120 15.0427 4 -23 1 26 -5.5251 14.2713 4 -21 -1 26 20.8135 14.4722 4 -21 1 26 19.0408 15.1836 4 -19 -1 26 9.74506 14.8053 4 -19 1 26 54.5479 21.6754 4 17 -1 -26 9.09858 8.01759 6 -17 -1 26 -7.2863 20.0746 4 -17 1 26 -22.238 14.4484 4 15 -1 -26 13.8238 7.51373 6 -15 -1 26 34.4130 14.8593 4 15 1 -26 -3.9691 8.33484 6 -15 1 26 -5.8480 15.3440 4 13 -1 -26 70.8444 10.4313 6 -13 -1 26 84.8754 17.0716 4 13 1 -26 64.2211 10.8427 6 -13 1 26 66.0412 23.4743 4 -11 -1 26 -4.2207 20.1708 4 11 -1 -26 17.3241 8.42080 6 -11 1 26 26.6776 20.2185 4 11 1 -26 -1.7600 8.99090 6 -9 -1 26 42.9478 17.2858 4 7 -1 -26 6.35730 7.58046 6 26 -2 -26 12.6444 7.80522 6 24 -2 -26 24.9448 8.37683 6 -24 2 26 16.6798 21.6364 4 -22 -2 26 7.19630 16.4439 4 22 -2 -26 -7.3036 10.6573 6 -22 2 26 5.70137 20.7624 4 20 -2 -26 10.3971 11.4495 6 -20 -2 26 7.98981 15.1959 4 -20 2 26 -10.461 14.9497 4 18 -2 -26 83.2637 11.3095 6 -18 -2 26 33.0675 21.3090 4 -18 2 26 59.5246 23.1733 4 16 -2 -26 174.343 13.7734 6 -16 -2 26 184.472 21.0901 4 14 -2 -26 69.2927 12.9991 6 -14 -2 26 -19.156 19.9126 4 -14 2 26 78.9248 21.2897 4 12 -2 -26 33.5634 9.06486 6 -12 -2 26 78.0126 21.4896 4 -10 -2 26 -20.385 15.0001 4 10 -2 -26 6.39930 7.59735 6 8 -2 -26 526.090 22.7879 6 23 -3 -26 15.4879 7.50491 6 21 -3 -26 47.3053 8.99656 6 19 -3 -26 16.3598 7.94091 6 -17 -3 26 9.66905 20.0445 4 17 -3 -26 23.8521 8.52734 6 15 -3 -26 16.1116 7.90177 6 13 -3 -26 5.00466 7.45175 6 11 -3 -26 12.3629 7.35962 6 -24 0 27 2.23062 15.1168 4 -22 0 27 4.74950 14.1852 4 -20 0 27 11.1235 14.0283 4 18 0 -27 0.71497 8.03288 6 -18 0 27 5.56778 19.9450 4 16 0 -27 -0.5044 8.11350 6 -16 0 27 -6.7514 14.3506 4 14 0 -27 -8.2099 7.46127 6 -14 0 27 -16.778 22.0594 4 12 0 -27 14.9675 8.09365 6 10 0 -27 16.0301 13.2016 6 -23 -1 27 105.543 19.3087 4 -23 1 27 162.003 21.3773 4 -21 -1 27 51.9266 22.6889 4 21 -1 -27 92.9163 10.7915 6 -21 1 27 131.659 19.1837 4 -19 -1 27 133.583 22.9318 4 19 -1 -27 123.499 15.0542 6 -19 1 27 160.006 20.5003 4 -17 -1 27 86.8232 16.8920 4 17 -1 -27 87.1384 11.0747 6 -17 1 27 60.8097 17.4263 4 17 1 -27 57.0329 12.1157 6 -15 -1 27 -17.829 14.1326 4 15 -1 -27 -7.7273 10.4185 6 15 1 -27 28.6821 8.64664 6 -15 1 27 -17.192 16.7156 4 13 -1 -27 1.80850 7.32857 6 -13 -1 27 16.9010 16.0163 4 13 1 -27 -13.546 8.92292 6 11 -1 -27 -8.4414 7.25697 6 24 -2 -27 7.11929 7.11944 6 22 -2 -27 6.13485 6.97611 6 20 -2 -27 21.1744 7.66169 6 -18 -2 27 4.97622 16.0952 4 18 -2 -27 8.00328 7.76873 6 18 2 -27 15.2142 12.4846 6 16 -2 -27 -1.6795 6.79082 6 14 -2 -27 3.40698 6.95414 6 12 -2 -27 2.15203 6.85438 6 22 0 -28 108.564 10.1607 6 20 0 -28 -0.9879 6.80686 6 18 0 -28 1.46685 6.46728 6 16 0 -28 1.67157 7.53620 6 21 -1 -28 89.0807 9.89581 6 19 -1 -28 31.0699 7.27080 6 19 1 -28 22.5858 10.7457 6 17 -1 -28 -4.1371 6.70208 6 17 1 -28 -18.715 8.42840 6 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.6573 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.54169 29.989 8.050 23.774 90.015 122.078 89.988 ) ; _shelx_hkl_checksum 52604 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 0.40646(2) 0.73555(6) 0.83788(2) 0.02268(14) Uani 1 1 d . . . . . Cl2 Cl 0.48783(4) 0.66512(13) 0.86183(5) 0.0312(2) Uani 1 1 d . . . . . Cl1 Cl 0.35485(4) 0.51164(13) 0.79788(5) 0.0313(2) Uani 1 1 d . . . . . O2 O 0.34666(11) 0.4535(3) 0.49410(14) 0.0306(7) Uani 1 1 d . . . . . O1 O 0.38264(10) 0.8827(3) 0.62752(13) 0.0282(6) Uani 1 1 d . . . . . N3 N 0.41677(12) 0.1649(4) 0.42350(15) 0.0233(7) Uani 1 1 d . . . . . N2 N 0.38746(11) 1.0212(4) 0.74089(15) 0.0232(7) Uani 1 1 d . . . . . N4 N 0.42412(12) 0.2574(4) 0.47655(15) 0.0250(7) Uani 1 1 d . . . . . N1 N 0.36853(11) 0.9203(4) 0.77019(15) 0.0228(7) Uani 1 1 d . . . . . O3 O 0.500000 0.4087(7) 0.750000 0.0687(16) Uani 1 2 d S T P . . H3A H 0.494320 0.454950 0.784020 0.103 Uiso 1 1 d R . . . . C20 C 0.44081(15) 0.0009(5) 0.5113(2) 0.0281(9) Uani 1 1 d . . . . . H20 H 0.449716 -0.095668 0.538248 0.034 Uiso 1 1 calc R . . . . C14 C 0.28992(15) 0.6983(5) 0.4638(2) 0.0276(9) Uani 1 1 d . . . . . C9 C 0.32321(15) 0.8119(5) 0.51335(19) 0.0260(9) Uani 1 1 d . . . . . C18 C 0.43869(15) 0.1598(5) 0.5300(2) 0.0282(9) Uani 1 1 d . . . . . C13 C 0.25165(15) 0.7576(6) 0.4012(2) 0.0345(10) Uani 1 1 d . . . . . H13 H 0.228566 0.680995 0.367896 0.041 Uiso 1 1 calc R . . . . C3 C 0.31168(15) 1.1275(5) 0.7156(2) 0.0283(9) Uani 1 1 d . . . . . H3 H 0.281707 1.197665 0.698466 0.034 Uiso 1 1 calc R . . . . C8 C 0.36455(15) 0.7499(5) 0.58056(19) 0.0288(9) Uani 1 1 d . . . . . H8A H 0.349847 0.660143 0.594484 0.035 Uiso 1 1 calc R . . . . H8B H 0.394425 0.703689 0.578841 0.035 Uiso 1 1 calc R . . . . C4 C 0.35348(15) 1.1463(5) 0.70655(19) 0.0250(9) Uani 1 1 d . . . . . C1 C 0.32194(14) 0.9872(5) 0.75433(19) 0.0255(9) Uani 1 1 d . . . . . C7 C 0.42058(15) 0.8279(5) 0.69225(19) 0.0278(9) Uani 1 1 d . . . . . H7A H 0.452733 0.790226 0.693959 0.033 Uiso 1 1 calc R . . . . H7B H 0.406493 0.733555 0.704954 0.033 Uiso 1 1 calc R . . . . C6 C 0.43349(14) 0.9719(5) 0.73949(19) 0.0266(9) Uani 1 1 d . . . . . H6A H 0.462111 0.939210 0.784726 0.032 Uiso 1 1 calc R . . . . H6B H 0.446014 1.067313 0.725197 0.032 Uiso 1 1 calc R . . . . C10 C 0.31745(16) 0.9811(5) 0.4982(2) 0.0307(10) Uani 1 1 d . . . . . H10 H 0.339809 1.059252 0.531281 0.037 Uiso 1 1 calc R . . . . C5 C 0.36369(18) 1.2733(6) 0.6693(2) 0.0380(11) Uani 1 1 d . . . . . H5A H 0.398490 1.322834 0.698673 0.057 Uiso 1 1 calc GR . . . . H5B H 0.336697 1.360123 0.653226 0.057 Uiso 1 1 calc GR . . . . H5C H 0.362630 1.220618 0.631364 0.057 Uiso 1 1 calc GR . . . . C17 C 0.41446(16) 0.4357(5) 0.4698(2) 0.0278(9) Uani 1 1 d . . . . . H17A H 0.424593 0.481025 0.439382 0.033 Uiso 1 1 calc R . . . . H17B H 0.437239 0.488686 0.513772 0.033 Uiso 1 1 calc R . . . . C15 C 0.29550(16) 0.5138(5) 0.4761(2) 0.0318(10) Uani 1 1 d . . . . . H15A H 0.289405 0.487364 0.512234 0.038 Uiso 1 1 calc R . . . . H15B H 0.268233 0.455747 0.435468 0.038 Uiso 1 1 calc R . . . . C16 C 0.35777(16) 0.4817(6) 0.4437(2) 0.0321(10) Uani 1 1 d . . . . . H16A H 0.351818 0.600172 0.430345 0.039 Uiso 1 1 calc R . . . . H16B H 0.334007 0.413536 0.404079 0.039 Uiso 1 1 calc R . . . . C21 C 0.42749(15) 0.0067(5) 0.4455(2) 0.0262(9) Uani 1 1 d . . . . . C12 C 0.24656(16) 0.9255(6) 0.3865(2) 0.0322(10) Uani 1 1 d . . . . . H12 H 0.220730 0.963890 0.343311 0.039 Uiso 1 1 calc R . . . . C11 C 0.27943(16) 1.0362(6) 0.4353(2) 0.0331(10) Uani 1 1 d . . . . . H11 H 0.276009 1.151849 0.425709 0.040 Uiso 1 1 calc R . . . . C22 C 0.42577(17) -0.1335(5) 0.4034(2) 0.0353(10) Uani 1 1 d . . . . . H22A H 0.389071 -0.165501 0.372115 0.053 Uiso 1 1 calc GR . . . . H22B H 0.445171 -0.228492 0.431801 0.053 Uiso 1 1 calc GR . . . . H22C H 0.441943 -0.098643 0.378690 0.053 Uiso 1 1 calc GR . . . . C2 C 0.29006(16) 0.9127(6) 0.7793(2) 0.0368(11) Uani 1 1 d . . . . . H2A H 0.290396 0.791303 0.776012 0.055 Uiso 1 1 calc GR . . . . H2B H 0.253726 0.953068 0.752431 0.055 Uiso 1 1 calc GR . . . . H2C H 0.305116 0.944728 0.825788 0.055 Uiso 1 1 calc GR . . . . C19 C 0.45055(18) 0.2274(6) 0.5949(2) 0.0387(11) Uani 1 1 d . . . . . H19A H 0.482950 0.293473 0.615026 0.058 Uiso 1 1 calc GR . . . . H19B H 0.455178 0.135402 0.624565 0.058 Uiso 1 1 calc GR . . . . H19C H 0.421328 0.297968 0.587788 0.058 Uiso 1 1 calc GR . . . . 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 0.0215(2) 0.0232(3) 0.0222(3) 0.0000(2) 0.0108(2) -0.0004(2) Cl2 0.0242(5) 0.0354(6) 0.0317(5) 0.0021(4) 0.0132(4) 0.0054(4) Cl1 0.0329(5) 0.0275(6) 0.0281(5) -0.0039(4) 0.0126(4) -0.0083(4) O2 0.0371(16) 0.0295(17) 0.0329(16) 0.0008(13) 0.0239(14) 0.0061(13) O1 0.0302(15) 0.0268(16) 0.0225(14) -0.0008(12) 0.0105(12) 0.0040(12) N3 0.0266(17) 0.0213(18) 0.0231(17) -0.0026(14) 0.0139(15) 0.0015(14) N2 0.0224(16) 0.0266(19) 0.0246(17) 0.0023(15) 0.0151(14) 0.0003(14) N4 0.0278(17) 0.0245(19) 0.0235(17) 0.0007(15) 0.0141(14) 0.0017(15) N1 0.0220(16) 0.0255(19) 0.0241(17) -0.0009(14) 0.0144(15) -0.0002(14) O3 0.085(4) 0.073(4) 0.061(4) 0.000 0.048(3) 0.000 C20 0.028(2) 0.027(2) 0.028(2) 0.0109(18) 0.0143(18) 0.0015(17) C14 0.029(2) 0.030(2) 0.030(2) -0.0028(18) 0.0199(19) 0.0001(17) C9 0.023(2) 0.031(2) 0.024(2) -0.0013(17) 0.0123(17) 0.0026(17) C18 0.028(2) 0.034(3) 0.025(2) 0.0053(19) 0.0152(18) 0.0003(18) C13 0.026(2) 0.044(3) 0.030(2) -0.006(2) 0.0130(18) 0.003(2) C3 0.027(2) 0.029(2) 0.027(2) -0.0029(18) 0.0136(19) 0.0051(17) C8 0.028(2) 0.030(2) 0.027(2) -0.0041(19) 0.0130(17) 0.0020(19) C4 0.029(2) 0.021(2) 0.024(2) 0.0006(17) 0.0130(18) 0.0041(17) C1 0.0211(19) 0.029(2) 0.022(2) 0.0014(17) 0.0078(17) 0.0015(17) C7 0.026(2) 0.032(2) 0.026(2) 0.0009(18) 0.0145(18) 0.0063(18) C6 0.0221(19) 0.037(3) 0.023(2) -0.0011(18) 0.0134(17) -0.0006(18) C10 0.030(2) 0.030(3) 0.031(2) -0.0023(19) 0.0158(19) -0.0028(18) C5 0.048(3) 0.029(3) 0.045(3) 0.009(2) 0.031(2) 0.008(2) C17 0.038(2) 0.020(2) 0.028(2) -0.0011(17) 0.0189(19) -0.0005(18) C15 0.031(2) 0.027(2) 0.037(2) -0.0075(19) 0.018(2) -0.0030(18) C16 0.039(2) 0.030(3) 0.031(2) 0.0005(19) 0.021(2) 0.0078(19) C21 0.0238(19) 0.022(2) 0.030(2) 0.0009(18) 0.0125(18) 0.0017(17) C12 0.032(2) 0.038(3) 0.024(2) 0.0029(19) 0.0121(19) 0.0092(19) C11 0.038(2) 0.028(3) 0.032(2) 0.0074(19) 0.018(2) 0.0065(19) C22 0.038(2) 0.023(2) 0.038(3) 0.0027(19) 0.016(2) 0.0032(19) C2 0.027(2) 0.043(3) 0.045(3) 0.005(2) 0.023(2) 0.002(2) C19 0.047(3) 0.046(3) 0.028(2) 0.008(2) 0.023(2) 0.009(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 '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 Cl1 Zn1 Cl2 108.41(4) . . N3 Zn1 Cl2 105.89(9) 6_566 . N3 Zn1 Cl1 116.28(9) 6_566 . N1 Zn1 Cl2 117.18(9) . . N1 Zn1 Cl1 106.45(10) . . N1 Zn1 N3 102.99(13) . 6_566 C16 O2 C15 112.7(3) . . C7 O1 C8 111.7(3) . . N4 N3 Zn1 124.3(2) . 6_565 C21 N3 Zn1 129.2(3) . 6_565 C21 N3 N4 105.5(3) . . N1 N2 C6 120.2(3) . . C4 N2 N1 111.3(3) . . C4 N2 C6 127.5(3) . . N3 N4 C17 120.4(3) . . C18 N4 N3 111.1(3) . . C18 N4 C17 128.4(3) . . N2 N1 Zn1 128.6(2) . . C1 N1 Zn1 124.9(3) . . C1 N1 N2 105.5(3) . . C18 C20 H20 126.4 . . C18 C20 C21 107.3(4) . . C21 C20 H20 126.4 . . C9 C14 C15 121.6(4) . . C13 C14 C9 119.2(4) . . C13 C14 C15 119.2(4) . . C14 C9 C8 119.7(4) . . C10 C9 C14 118.9(4) . . C10 C9 C8 121.4(4) . . N4 C18 C20 106.7(4) . . N4 C18 C19 122.7(4) . . C20 C18 C19 130.6(4) . . C14 C13 H13 119.3 . . C12 C13 C14 121.4(4) . . C12 C13 H13 119.3 . . C4 C3 H3 126.5 . . C1 C3 H3 126.5 . . C1 C3 C4 106.9(4) . . O1 C8 C9 109.9(3) . . O1 C8 H8A 109.7 . . O1 C8 H8B 109.7 . . C9 C8 H8A 109.7 . . C9 C8 H8B 109.7 . . H8A C8 H8B 108.2 . . N2 C4 C3 106.1(3) . . N2 C4 C5 122.9(3) . . C3 C4 C5 131.0(4) . . N1 C1 C3 110.0(3) . . N1 C1 C2 121.0(4) . . C3 C1 C2 128.9(4) . . O1 C7 H7A 110.1 . . O1 C7 H7B 110.1 . . O1 C7 C6 108.0(3) . . H7A C7 H7B 108.4 . . C6 C7 H7A 110.1 . . C6 C7 H7B 110.1 . . N2 C6 C7 110.7(3) . . N2 C6 H6A 109.5 . . N2 C6 H6B 109.5 . . C7 C6 H6A 109.5 . . C7 C6 H6B 109.5 . . H6A C6 H6B 108.1 . . C9 C10 H10 119.7 . . C11 C10 C9 120.6(4) . . C11 C10 H10 119.7 . . C4 C5 H5A 109.5 . . C4 C5 H5B 109.5 . . C4 C5 H5C 109.5 . . H5A C5 H5B 109.5 . . H5A C5 H5C 109.5 . . H5B C5 H5C 109.5 . . N4 C17 H17A 108.8 . . N4 C17 H17B 108.8 . . N4 C17 C16 113.6(3) . . H17A C17 H17B 107.7 . . C16 C17 H17A 108.8 . . C16 C17 H17B 108.8 . . O2 C15 C14 112.4(3) . . O2 C15 H15A 109.1 . . O2 C15 H15B 109.1 . . C14 C15 H15A 109.1 . . C14 C15 H15B 109.1 . . H15A C15 H15B 107.9 . . O2 C16 C17 109.2(3) . . O2 C16 H16A 109.8 . . O2 C16 H16B 109.8 . . C17 C16 H16A 109.8 . . C17 C16 H16B 109.8 . . H16A C16 H16B 108.3 . . N3 C21 C20 109.5(4) . . N3 C21 C22 122.6(4) . . C20 C21 C22 127.9(4) . . C13 C12 H12 120.5 . . C11 C12 C13 119.1(4) . . C11 C12 H12 120.5 . . C10 C11 H11 119.6 . . C12 C11 C10 120.8(4) . . C12 C11 H11 119.6 . . C21 C22 H22A 109.5 . . C21 C22 H22B 109.5 . . C21 C22 H22C 109.5 . . H22A C22 H22B 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . C1 C2 H2A 109.5 . . C1 C2 H2B 109.5 . . C1 C2 H2C 109.5 . . H2A C2 H2B 109.5 . . H2A C2 H2C 109.5 . . H2B C2 H2C 109.5 . . C18 C19 H19A 109.5 . . C18 C19 H19B 109.5 . . C18 C19 H19C 109.5 . . H19A C19 H19B 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 Cl2 2.2623(11) . Zn1 Cl1 2.2313(11) . Zn1 N3 2.050(3) 6_566 Zn1 N1 2.036(3) . O2 C15 1.440(5) . O2 C16 1.421(5) . O1 C8 1.427(5) . O1 C7 1.412(4) . N3 N4 1.376(4) . N3 C21 1.348(5) . N2 N1 1.372(4) . N2 C4 1.354(5) . N2 C6 1.452(4) . N4 C18 1.352(5) . N4 C17 1.455(5) . N1 C1 1.350(5) . O3 H3A 0.9828 . C20 H20 0.9500 . C20 C18 1.365(6) . C20 C21 1.394(6) . C14 C9 1.402(6) . C14 C13 1.394(6) . C14 C15 1.505(6) . C9 C8 1.493(5) . C9 C10 1.395(6) . C18 C19 1.489(6) . C13 H13 0.9500 . C13 C12 1.384(6) . C3 H3 0.9500 . C3 C4 1.387(5) . C3 C1 1.384(6) . C8 H8A 0.9900 . C8 H8B 0.9900 . C4 C5 1.486(6) . C1 C2 1.491(5) . C7 H7A 0.9900 . C7 H7B 0.9900 . C7 C6 1.513(5) . C6 H6A 0.9900 . C6 H6B 0.9900 . C10 H10 0.9500 . C10 C11 1.385(6) . C5 H5A 0.9800 . C5 H5B 0.9800 . C5 H5C 0.9800 . C17 H17A 0.9900 . C17 H17B 0.9900 . C17 C16 1.513(5) . C15 H15A 0.9900 . C15 H15B 0.9900 . C16 H16A 0.9900 . C16 H16B 0.9900 . C21 C22 1.489(6) . C12 H12 0.9500 . C12 C11 1.376(6) . C11 H11 0.9500 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . C2 H2A 0.9800 . C2 H2B 0.9800 . C2 H2C 0.9800 . C19 H19A 0.9800 . C19 H19B 0.9800 . C19 H19C 0.9800 .