# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dimitris Kessissoglou' _publ_contact_author_email kessisog@chem.auth.gr loop_ _publ_author_name 'Alketa Tarushi' 'Xanthippi Totta' 'Catherine P. Raptopoulou' 'Vassilis Psycharis' 'George Psomas' ; D.P.Kessissoglou ; data_keat1027 _database_code_depnum_ccdc_archive 'CCDC 851684' #TrackingRef 'keat1027.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H30 Cl2 N4 O4 Zn' _chemical_formula_weight 742.93 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' 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4238(2) _cell_length_b 10.7481(2) _cell_length_c 15.3980(3) _cell_angle_alpha 102.9370(10) _cell_angle_beta 99.0040(10) _cell_angle_gamma 92.5320(10) _cell_volume 1654.99(5) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 17531 _cell_measurement_theta_min 6.64 _cell_measurement_theta_max 71.89 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 2.914 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.561 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19749 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 6.64 _diffrn_reflns_theta_max 65.00 _reflns_number_total 5367 _reflns_number_gt 4260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.1807P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5367 _refine_ls_number_parameters 537 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1124 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.164 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.72080(4) 0.38003(3) 0.59774(2) 0.03405(15) Uani 1 1 d . . . N1 N 0.8185(3) 0.2772(3) 0.9134(2) 0.0538(8) Uani 1 1 d . . . O1 O 0.7361(2) 0.34146(19) 0.75807(14) 0.0495(6) Uani 1 1 d . . . O2 O 0.8844(2) 0.40106(19) 0.68519(13) 0.0462(6) Uani 1 1 d . . . C1 C 0.8527(4) 0.3703(2) 0.75435(19) 0.0381(8) Uani 1 1 d . . . C2 C 0.9605(3) 0.3699(3) 0.83104(18) 0.0369(7) Uani 1 1 d . . . C3 C 1.0847(4) 0.4183(3) 0.8267(2) 0.0449(8) Uani 1 1 d . . . C4 C 1.1884(4) 0.4254(4) 0.8954(2) 0.0537(9) Uani 1 1 d . . . C5 C 1.1677(4) 0.3849(4) 0.9721(2) 0.0582(10) Uani 1 1 d . . . C6 C 1.0473(4) 0.3368(4) 0.9781(2) 0.0545(10) Uani 1 1 d . . . C7 C 0.9404(4) 0.3251(3) 0.90775(19) 0.0425(8) Uani 1 1 d . . . C8 C 0.7811(4) 0.2096(3) 0.9756(2) 0.0501(9) Uani 1 1 d . . . C9 C 0.8622(4) 0.1245(4) 1.0098(2) 0.0564(10) Uani 1 1 d . . . C10 C 0.8211(5) 0.0598(4) 1.0704(3) 0.0676(12) Uani 1 1 d . . . C11 C 0.6987(5) 0.0733(4) 1.0960(3) 0.0662(11) Uani 1 1 d . . . H11 H 0.686(4) 0.027(4) 1.140(3) 0.086 Uiso 1 1 d . . . C12 C 0.6207(4) 0.1548(3) 1.0580(2) 0.0532(9) Uani 1 1 d . . . C13 C 0.6570(4) 0.2240(3) 0.9978(2) 0.0506(9) Uani 1 1 d . . . C14 C 0.5682(4) 0.3119(4) 0.9587(3) 0.0659(11) Uani 1 1 d . . . H14A H 0.5042 0.3381 0.9982 0.099 Uiso 1 1 calc R . . H14B H 0.5228 0.2669 0.8985 0.099 Uiso 1 1 calc R . . H14C H 0.6198 0.3879 0.9541 0.099 Uiso 1 1 calc R . . Cl1 Cl 0.46558(11) 0.16751(11) 1.08666(7) 0.0795(4) Uani 1 1 d . . . N21 N 0.9282(3) 0.0931(2) 0.38051(19) 0.0461(7) Uani 1 1 d . . . O21 O 0.6344(2) 0.20146(16) 0.52917(12) 0.0352(5) Uani 1 1 d . . . O22 O 0.8213(2) 0.25448(18) 0.49411(14) 0.0457(6) Uani 1 1 d . . . C21 C 0.7235(3) 0.1753(3) 0.48187(18) 0.0321(7) Uani 1 1 d . . . C22 C 0.7097(3) 0.0558(2) 0.40953(17) 0.0295(7) Uani 1 1 d . . . C23 C 0.5922(3) -0.0197(3) 0.3874(2) 0.0343(7) Uani 1 1 d . . . C24 C 0.5705(4) -0.1274(3) 0.3166(2) 0.0410(8) Uani 1 1 d . . . C25 C 0.6690(3) -0.1610(3) 0.2674(2) 0.0397(8) Uani 1 1 d . . . C26 C 0.7876(3) -0.0904(3) 0.28754(19) 0.0358(7) Uani 1 1 d . . . C27 C 0.8111(3) 0.0204(2) 0.35926(18) 0.0313(7) Uani 1 1 d . . . C28 C 1.0309(3) 0.0785(3) 0.3291(2) 0.0382(7) Uani 1 1 d . . . C29 C 1.1078(4) -0.0233(3) 0.3309(2) 0.0479(9) Uani 1 1 d . . . C30 C 1.2135(4) -0.0321(3) 0.2864(3) 0.0535(9) Uani 1 1 d . . . C31 C 1.2433(4) 0.0579(3) 0.2405(2) 0.0466(8) Uani 1 1 d . . . C32 C 1.1654(3) 0.1582(3) 0.24035(19) 0.0388(7) Uani 1 1 d . . . C33 C 1.0567(3) 0.1724(3) 0.28347(19) 0.0376(7) Uani 1 1 d . . . C34 C 0.9742(3) 0.2821(3) 0.2799(2) 0.0472(8) Uani 1 1 d . . . H34A H 0.8987 0.2715 0.3091 0.071 Uiso 1 1 calc R . . H34B H 0.9443 0.2842 0.2167 0.071 Uiso 1 1 calc R . . H34C H 1.0256 0.3625 0.3116 0.071 Uiso 1 1 calc R . . Cl21 Cl 1.20720(9) 0.27565(9) 0.18453(6) 0.0587(3) Uani 1 1 d . . . N41 N 0.5739(2) 0.4963(2) 0.63526(15) 0.0347(6) Uani 1 1 d . . . N42 N 0.7469(2) 0.5285(2) 0.53220(14) 0.0319(6) Uani 1 1 d . . . C41 C 0.4882(3) 0.4739(3) 0.6878(2) 0.0419(8) Uani 1 1 d . . . C42 C 0.4048(4) 0.5615(3) 0.7182(2) 0.0480(9) Uani 1 1 d . . . C43 C 0.4101(4) 0.6787(3) 0.6965(2) 0.0444(8) Uani 1 1 d . . . C44 C 0.4979(3) 0.7030(3) 0.64318(19) 0.0355(7) Uani 1 1 d . . . C45 C 0.5784(3) 0.6102(2) 0.61290(17) 0.0293(6) Uani 1 1 d . . . C46 C 0.6743(3) 0.6278(2) 0.55384(17) 0.0297(7) Uani 1 1 d . . . C47 C 0.6914(3) 0.7385(3) 0.5235(2) 0.0396(8) Uani 1 1 d . . . C48 C 0.7867(3) 0.7467(3) 0.4710(2) 0.0408(8) Uani 1 1 d . . . C49 C 0.8594(3) 0.6449(3) 0.4490(2) 0.0393(8) Uani 1 1 d . . . C50 C 0.8362(3) 0.5373(3) 0.47939(19) 0.0380(7) Uani 1 1 d . . . H1N H 0.765(3) 0.289(3) 0.8775(19) 0.026(9) Uiso 1 1 d . . . H21N H 0.936(3) 0.170(3) 0.423(2) 0.066(11) Uiso 1 1 d . . . H3 H 1.094(3) 0.448(3) 0.769(2) 0.050(9) Uiso 1 1 d . . . H4 H 1.270(3) 0.457(3) 0.891(2) 0.054(11) Uiso 1 1 d . . . H5 H 1.239(3) 0.392(3) 1.023(2) 0.063(10) Uiso 1 1 d . . . H6 H 1.031(3) 0.313(3) 1.031(2) 0.059(10) Uiso 1 1 d . . . H9 H 0.948(3) 0.112(3) 0.9922(19) 0.042(9) Uiso 1 1 d . . . H10 H 0.881(4) 0.000(4) 1.094(2) 0.074(12) Uiso 1 1 d . . . H23 H 0.528(3) 0.006(3) 0.4213(18) 0.036(8) Uiso 1 1 d . . . H24 H 0.490(3) -0.178(3) 0.302(2) 0.051(10) Uiso 1 1 d . . . H25 H 0.654(3) -0.236(3) 0.213(2) 0.067(10) Uiso 1 1 d . . . H26 H 0.857(3) -0.112(2) 0.2507(18) 0.036(8) Uiso 1 1 d . . . H29 H 1.086(3) -0.083(3) 0.3641(17) 0.030(7) Uiso 1 1 d . . . H30 H 1.265(3) -0.102(3) 0.286(2) 0.063(11) Uiso 1 1 d . . . H31 H 1.316(3) 0.051(3) 0.212(2) 0.050(10) Uiso 1 1 d . . . H41 H 0.490(3) 0.3913 0.7015(18) 0.039(8) Uiso 1 1 d . . . H42 H 0.352(3) 0.540(3) 0.752(2) 0.056(11) Uiso 1 1 d . . . H43 H 0.352(3) 0.734(3) 0.717(2) 0.057(10) Uiso 1 1 d . . . H44 H 0.502(3) 0.7849 0.6289(17) 0.034(8) Uiso 1 1 d . . . H47 H 0.638(3) 0.811(3) 0.5389(19) 0.040(8) Uiso 1 1 d . . . H48 H 0.803(3) 0.823(3) 0.451(2) 0.059(10) Uiso 1 1 d . . . H49 H 0.921(3) 0.645(3) 0.4195(18) 0.030(8) Uiso 1 1 d . . . H50 H 0.887(3) 0.460(3) 0.4630(17) 0.037(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0394(3) 0.0257(2) 0.0374(2) 0.00840(15) 0.00629(19) 0.00215(17) N1 0.047(2) 0.074(2) 0.0461(17) 0.0275(15) 0.0051(16) 0.0021(17) O1 0.0482(17) 0.0446(13) 0.0550(14) 0.0206(10) -0.0053(12) 0.0007(11) O2 0.0565(16) 0.0464(12) 0.0369(11) 0.0149(9) 0.0023(11) 0.0117(11) C1 0.053(2) 0.0221(14) 0.0373(16) 0.0081(11) -0.0003(16) 0.0051(14) C2 0.041(2) 0.0348(16) 0.0349(15) 0.0094(12) 0.0044(15) 0.0053(14) C3 0.052(3) 0.0486(19) 0.0353(16) 0.0125(14) 0.0073(16) 0.0068(17) C4 0.045(3) 0.066(2) 0.052(2) 0.0201(17) 0.0071(19) 0.003(2) C5 0.054(3) 0.076(3) 0.045(2) 0.0227(18) -0.0059(19) 0.006(2) C6 0.056(3) 0.072(2) 0.0390(18) 0.0243(17) 0.0046(18) 0.001(2) C7 0.046(2) 0.0470(18) 0.0355(16) 0.0123(13) 0.0071(16) 0.0068(16) C8 0.055(3) 0.053(2) 0.0412(17) 0.0092(15) 0.0090(17) 0.0024(18) C9 0.057(3) 0.068(2) 0.052(2) 0.0255(18) 0.015(2) 0.014(2) C10 0.083(4) 0.063(3) 0.061(2) 0.0256(19) 0.008(2) 0.008(2) C11 0.064(3) 0.065(3) 0.063(2) 0.0041(19) 0.014(2) -0.013(2) C12 0.054(3) 0.058(2) 0.0430(18) 0.0058(16) 0.0082(18) -0.0137(19) C13 0.046(2) 0.058(2) 0.0412(17) 0.0032(15) 0.0025(17) -0.0051(17) C14 0.051(3) 0.079(3) 0.065(2) 0.018(2) -0.002(2) 0.006(2) Cl1 0.0657(8) 0.1017(8) 0.0643(6) 0.0026(5) 0.0225(6) -0.0208(6) N21 0.0389(18) 0.0378(15) 0.0578(17) -0.0036(12) 0.0219(14) -0.0101(13) O21 0.0388(14) 0.0297(10) 0.0390(10) 0.0081(8) 0.0118(10) 0.0039(9) O22 0.0421(15) 0.0330(11) 0.0567(13) -0.0041(9) 0.0161(11) -0.0049(10) C21 0.035(2) 0.0272(14) 0.0361(15) 0.0105(11) 0.0058(14) 0.0063(13) C22 0.0317(19) 0.0232(13) 0.0363(14) 0.0112(11) 0.0084(13) 0.0013(12) C23 0.028(2) 0.0300(15) 0.0481(17) 0.0143(13) 0.0089(15) 0.0065(13) C24 0.034(2) 0.0274(15) 0.0585(19) 0.0061(13) 0.0040(17) -0.0021(14) C25 0.039(2) 0.0323(16) 0.0438(17) 0.0023(13) 0.0050(16) 0.0021(14) C26 0.038(2) 0.0337(15) 0.0362(15) 0.0088(12) 0.0082(15) 0.0001(14) C27 0.0337(19) 0.0250(14) 0.0368(15) 0.0120(11) 0.0047(14) -0.0009(12) C28 0.032(2) 0.0333(16) 0.0468(17) 0.0031(13) 0.0099(15) -0.0071(14) C29 0.046(2) 0.0350(18) 0.067(2) 0.0141(16) 0.0192(19) 0.0003(15) C30 0.041(2) 0.040(2) 0.081(3) 0.0102(17) 0.019(2) 0.0074(17) C31 0.032(2) 0.052(2) 0.054(2) 0.0056(15) 0.0140(17) -0.0031(16) C32 0.028(2) 0.0482(18) 0.0376(15) 0.0098(13) 0.0005(14) -0.0072(14) C33 0.031(2) 0.0354(16) 0.0408(16) 0.0048(12) -0.0020(14) -0.0090(13) C34 0.040(2) 0.0448(19) 0.059(2) 0.0158(15) 0.0084(17) 0.0071(16) Cl21 0.0539(6) 0.0788(6) 0.0513(5) 0.0355(4) 0.0066(4) -0.0053(5) N41 0.0373(17) 0.0288(12) 0.0374(12) 0.0103(10) 0.0023(12) -0.0032(11) N42 0.0301(16) 0.0328(13) 0.0326(12) 0.0108(10) 0.0002(11) 0.0034(11) C41 0.044(2) 0.0365(17) 0.0507(18) 0.0174(14) 0.0152(16) -0.0019(15) C42 0.044(3) 0.053(2) 0.053(2) 0.0190(16) 0.0179(18) 0.0022(17) C43 0.038(2) 0.0472(19) 0.0495(19) 0.0124(15) 0.0076(17) 0.0095(16) C44 0.035(2) 0.0321(16) 0.0386(15) 0.0116(12) -0.0015(14) 0.0044(13) C45 0.0293(18) 0.0255(14) 0.0305(13) 0.0069(10) -0.0026(13) -0.0019(12) C46 0.0263(18) 0.0307(14) 0.0305(14) 0.0095(11) -0.0023(13) -0.0005(12) C47 0.044(2) 0.0308(16) 0.0453(17) 0.0144(13) 0.0056(16) 0.0029(15) C48 0.040(2) 0.0400(17) 0.0451(17) 0.0206(14) 0.0032(16) -0.0046(15) C49 0.030(2) 0.0510(19) 0.0389(16) 0.0165(14) 0.0050(15) -0.0034(15) C50 0.035(2) 0.0419(18) 0.0389(16) 0.0133(13) 0.0081(15) 0.0019(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Zn O2 1.970(2) . ? Zn O21 2.0620(18) . ? Zn N41 2.088(2) . ? Zn N42 2.099(2) . ? Zn O22 2.269(2) . ? Zn C21 2.508(3) . ? N1 C7 1.372(4) . ? N1 C8 1.414(4) . ? N1 H1N 0.76(3) . ? O1 C1 1.254(4) . ? O2 C1 1.269(3) . ? C1 C2 1.498(4) . ? C2 C3 1.391(5) . ? C2 C7 1.412(4) . ? C3 C4 1.375(5) . ? C3 H3 1.03(3) . ? C4 C5 1.391(5) . ? C4 H4 0.92(3) . ? C5 C6 1.360(5) . ? C5 H5 0.98(3) . ? C6 C7 1.407(5) . ? C6 H6 0.95(3) . ? C8 C13 1.395(5) . ? C8 C9 1.405(5) . ? C9 C10 1.388(5) . ? C9 H9 0.98(3) . ? C10 C11 1.398(6) . ? C10 H10 1.00(4) . ? C11 C12 1.383(6) . ? C11 H11 0.94(4) . ? C12 C13 1.397(4) . ? C12 Cl1 1.745(4) . ? C13 C14 1.506(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N21 C27 1.373(4) . ? N21 C28 1.422(4) . ? N21 H21N 0.93(3) . ? O21 C21 1.271(3) . ? O22 C21 1.262(3) . ? C21 C22 1.485(4) . ? C22 C23 1.390(4) . ? C22 C27 1.421(4) . ? C23 C24 1.383(4) . ? C23 H23 0.92(3) . ? C24 C25 1.383(4) . ? C24 H24 0.95(3) . ? C25 C26 1.376(4) . ? C25 H25 1.01(3) . ? C26 C27 1.413(4) . ? C26 H26 0.99(3) . ? C28 C29 1.387(4) . ? C28 C33 1.393(4) . ? C29 C30 1.382(5) . ? C29 H29 0.95(3) . ? C30 C31 1.372(5) . ? C30 H30 0.94(4) . ? C31 C32 1.378(4) . ? C31 H31 0.93(3) . ? C32 C33 1.397(4) . ? C32 Cl21 1.755(3) . ? C33 C34 1.495(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? N41 C41 1.344(4) . ? N41 C45 1.345(3) . ? N42 C50 1.342(4) . ? N42 C46 1.346(3) . ? C41 C42 1.365(5) . ? C41 H41 0.957(12) . ? C42 C43 1.374(4) . ? C42 H42 0.87(3) . ? C43 C44 1.375(4) . ? C43 H43 0.91(3) . ? C44 C45 1.380(4) . ? C44 H44 0.954(12) . ? C45 C46 1.486(4) . ? C46 C47 1.386(4) . ? C47 C48 1.387(4) . ? C47 H47 0.98(3) . ? C48 C49 1.369(4) . ? C48 H48 0.96(3) . ? C49 C50 1.366(4) . ? C49 H49 0.84(3) . ? C50 H50 1.01(3) . ? 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 O2 Zn O21 121.68(8) . . ? O2 Zn N41 116.97(9) . . ? O21 Zn N41 108.09(9) . . ? O2 Zn N42 102.23(9) . . ? O21 Zn N42 122.23(8) . . ? N41 Zn N42 78.19(9) . . ? O2 Zn O22 88.51(8) . . ? O21 Zn O22 60.42(7) . . ? N41 Zn O22 152.86(9) . . ? N42 Zn O22 87.80(8) . . ? O2 Zn C21 107.22(9) . . ? O21 Zn C21 30.33(8) . . ? N41 Zn C21 133.71(10) . . ? N42 Zn C21 106.09(9) . . ? O22 Zn C21 30.10(8) . . ? C7 N1 C8 129.1(3) . . ? C7 N1 H1N 114(2) . . ? C8 N1 H1N 117(2) . . ? C1 O2 Zn 105.2(2) . . ? O1 C1 O2 121.3(3) . . ? O1 C1 C2 121.6(3) . . ? O2 C1 C2 117.1(3) . . ? C3 C2 C7 119.1(3) . . ? C3 C2 C1 118.1(3) . . ? C7 C2 C1 122.8(3) . . ? C4 C3 C2 122.0(3) . . ? C4 C3 H3 122.3(18) . . ? C2 C3 H3 115.7(18) . . ? C3 C4 C5 118.9(4) . . ? C3 C4 H4 121(2) . . ? C5 C4 H4 120(2) . . ? C6 C5 C4 120.4(4) . . ? C6 C5 H5 119(2) . . ? C4 C5 H5 121(2) . . ? C5 C6 C7 121.9(3) . . ? C5 C6 H6 121(2) . . ? C7 C6 H6 117(2) . . ? N1 C7 C6 122.3(3) . . ? N1 C7 C2 120.0(3) . . ? C6 C7 C2 117.7(3) . . ? C13 C8 C9 120.7(3) . . ? C13 C8 N1 117.7(3) . . ? C9 C8 N1 121.5(3) . . ? C10 C9 C8 119.5(4) . . ? C10 C9 H9 119.9(17) . . ? C8 C9 H9 120.6(17) . . ? C9 C10 C11 121.8(4) . . ? C9 C10 H10 118(2) . . ? C11 C10 H10 120(2) . . ? C12 C11 C10 116.5(4) . . ? C12 C11 H11 131(3) . . ? C10 C11 H11 112(3) . . ? C11 C12 C13 124.5(4) . . ? C11 C12 Cl1 116.6(3) . . ? C13 C12 Cl1 118.8(3) . . ? C8 C13 C12 117.0(3) . . ? C8 C13 C14 120.8(3) . . ? C12 C13 C14 122.3(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C27 N21 C28 125.8(3) . . ? C27 N21 H21N 118(2) . . ? C28 N21 H21N 114(2) . . ? C21 O21 Zn 94.65(17) . . ? C21 O22 Zn 85.49(17) . . ? O22 C21 O21 119.4(3) . . ? O22 C21 C22 120.1(3) . . ? O21 C21 C22 120.5(3) . . ? O22 C21 Zn 64.41(15) . . ? O21 C21 Zn 55.02(13) . . ? C22 C21 Zn 173.6(2) . . ? C23 C22 C27 119.3(3) . . ? C23 C22 C21 119.1(3) . . ? C27 C22 C21 121.6(3) . . ? C24 C23 C22 121.7(3) . . ? C24 C23 H23 121.4(18) . . ? C22 C23 H23 116.9(18) . . ? C25 C24 C23 118.9(3) . . ? C25 C24 H24 120.1(19) . . ? C23 C24 H24 121.1(19) . . ? C26 C25 C24 121.6(3) . . ? C26 C25 H25 118(2) . . ? C24 C25 H25 121(2) . . ? C25 C26 C27 120.2(3) . . ? C25 C26 H26 121.6(16) . . ? C27 C26 H26 118.1(16) . . ? N21 C27 C26 121.5(3) . . ? N21 C27 C22 120.2(3) . . ? C26 C27 C22 118.3(3) . . ? C29 C28 C33 121.9(3) . . ? C29 C28 N21 119.4(3) . . ? C33 C28 N21 118.5(3) . . ? C30 C29 C28 119.3(3) . . ? C30 C29 H29 123.0(17) . . ? C28 C29 H29 117.7(17) . . ? C31 C30 C29 121.1(4) . . ? C31 C30 H30 119(2) . . ? C29 C30 H30 119(2) . . ? C30 C31 C32 118.1(3) . . ? C30 C31 H31 120(2) . . ? C32 C31 H31 122(2) . . ? C31 C32 C33 123.7(3) . . ? C31 C32 Cl21 117.9(3) . . ? C33 C32 Cl21 118.4(2) . . ? C28 C33 C32 115.8(3) . . ? C28 C33 C34 122.7(3) . . ? C32 C33 C34 121.4(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C41 N41 C45 118.4(3) . . ? C41 N41 Zn 125.94(19) . . ? C45 N41 Zn 115.09(19) . . ? C50 N42 C46 118.8(2) . . ? C50 N42 Zn 125.9(2) . . ? C46 N42 Zn 114.91(18) . . ? N41 C41 C42 122.5(3) . . ? N41 C41 H41 114.6(17) . . ? C42 C41 H41 122.9(17) . . ? C41 C42 C43 119.3(3) . . ? C41 C42 H42 117(2) . . ? C43 C42 H42 124(2) . . ? C42 C43 C44 118.7(3) . . ? C42 C43 H43 117(2) . . ? C44 C43 H43 124(2) . . ? C43 C44 C45 119.7(3) . . ? C43 C44 H44 118.5(16) . . ? C45 C44 H44 121.8(16) . . ? N41 C45 C44 121.3(3) . . ? N41 C45 C46 115.5(2) . . ? C44 C45 C46 123.1(2) . . ? N42 C46 C47 121.3(3) . . ? N42 C46 C45 115.3(2) . . ? C47 C46 C45 123.4(3) . . ? C46 C47 C48 118.8(3) . . ? C46 C47 H47 121.1(17) . . ? C48 C47 H47 120.1(17) . . ? C49 C48 C47 119.3(3) . . ? C49 C48 H48 120(2) . . ? C47 C48 H48 121(2) . . ? C50 C49 C48 119.1(3) . . ? C50 C49 H49 117.1(19) . . ? C48 C49 H49 123.7(19) . . ? N42 C50 C49 122.5(3) . . ? N42 C50 H50 116.6(16) . . ? C49 C50 H50 120.8(16) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.525 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.058 # Attachment 'psxt16.cif' data_psxt16 _database_code_depnum_ccdc_archive 'CCDC 851685' #TrackingRef 'psxt16.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H40 Cl2 N4 O5 Zn' _chemical_formula_weight 841.07 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' 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9035(2) _cell_length_b 22.1385(4) _cell_length_c 14.6228(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.3770(10) _cell_angle_gamma 90.00 _cell_volume 3964.18(11) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 15810 _cell_measurement_theta_min 6.57 _cell_measurement_theta_max 71.86 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 2.519 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.673 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27185 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 6.57 _diffrn_reflns_theta_max 65.00 _reflns_number_total 6546 _reflns_number_gt 5119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+1.9695P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6546 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1562 _refine_ls_wR_factor_gt 0.1429 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn Zn 0.23962(4) 0.494382(18) 0.97795(3) 0.03325(17) Uani 1 1 d . . . O1 O 0.2982(2) 0.57703(10) 0.99773(16) 0.0392(6) Uani 1 1 d . . . O2 O 0.1275(2) 0.58564(11) 0.99808(19) 0.0481(7) Uani 1 1 d . . . Cl1 Cl -0.29503(10) 0.72149(5) 1.12114(10) 0.0740(4) Uani 1 1 d . . . N1 N 0.0721(3) 0.68922(16) 1.0629(3) 0.0558(9) Uani 1 1 d . . . C1 C 0.2176(3) 0.60895(16) 1.0044(2) 0.0388(8) Uani 1 1 d . . . C2 C 0.2361(3) 0.67518(15) 1.0193(2) 0.0370(8) Uani 1 1 d . . . C3 C 0.3274(4) 0.70073(17) 1.0030(3) 0.0484(10) Uani 1 1 d . . . C4 C 0.3463(4) 0.76233(18) 1.0124(3) 0.0635(13) Uani 1 1 d . . . C5 C 0.2748(4) 0.79851(18) 1.0395(3) 0.0624(13) Uani 1 1 d . . . C6 C 0.1863(4) 0.77518(17) 1.0572(3) 0.0515(11) Uani 1 1 d . . . C7 C 0.1635(3) 0.71272(15) 1.0484(2) 0.0417(9) Uani 1 1 d . . . C8 C 0.0142(3) 0.71381(16) 1.1216(3) 0.0492(10) Uani 1 1 d . . . C9 C 0.0712(4) 0.74135(18) 1.2112(3) 0.0573(11) Uani 1 1 d . . . C10 C 0.0103(4) 0.7624(2) 1.2676(3) 0.0649(13) Uani 1 1 d . . . H10 H 0.0471 0.7817 1.3270 0.091 Uiso 1 1 calc R . . C11 C -0.0998(4) 0.7565(2) 1.2410(4) 0.0678(14) Uani 1 1 d . . . H11 H -0.1390 0.7712 1.2816 0.095 Uiso 1 1 calc R . . C12 C -0.1552(4) 0.72876(17) 1.1538(3) 0.0542(11) Uani 1 1 d . . . C13 C -0.0985(3) 0.70722(16) 1.0914(3) 0.0493(10) Uani 1 1 d . . . C14 C -0.1554(4) 0.6795(2) 0.9981(3) 0.0646(12) Uani 1 1 d . . . H14A H -0.2328 0.6744 0.9918 0.097 Uiso 1 1 calc R . . H14B H -0.1230 0.6400 0.9940 0.097 Uiso 1 1 calc R . . H14C H -0.1485 0.7056 0.9462 0.097 Uiso 1 1 calc R . . O21 O 0.3957(2) 0.45391(11) 1.11008(16) 0.0442(6) Uani 1 1 d . . . O22 O 0.22077(19) 0.45859(10) 1.09529(16) 0.0370(6) Uani 1 1 d . . . Cl2 Cl 0.95016(8) 0.42050(4) 1.34943(7) 0.0510(3) Uani 1 1 d . . . N21 N 0.5350(2) 0.43229(14) 1.2827(2) 0.0414(7) Uani 1 1 d . . . C21 C 0.3187(3) 0.44578(14) 1.1445(2) 0.0353(8) Uani 1 1 d . . . C22 C 0.3386(3) 0.42145(13) 1.2438(2) 0.0324(8) Uani 1 1 d . . . C23 C 0.2499(3) 0.40360(15) 1.2720(3) 0.0368(8) Uani 1 1 d . . . C24 C 0.2623(3) 0.38140(16) 1.3629(3) 0.0402(9) Uani 1 1 d . . . C25 C 0.3669(3) 0.37622(15) 1.4273(3) 0.0420(9) Uani 1 1 d . . . C26 C 0.4563(3) 0.39331(15) 1.4018(3) 0.0387(8) Uani 1 1 d . . . C27 C 0.4449(3) 0.41680(14) 1.3100(2) 0.0355(8) Uani 1 1 d . . . C28 C 0.6405(3) 0.44585(14) 1.3442(2) 0.0350(8) Uani 1 1 d . . . C29 C 0.6560(3) 0.47782(16) 1.4294(3) 0.0384(8) Uani 1 1 d . . . C30 C 0.7601(3) 0.48981(16) 1.4892(3) 0.0422(9) Uani 1 1 d . . . C31 C 0.8493(3) 0.47193(16) 1.4644(3) 0.0405(9) Uani 1 1 d . . . C32 C 0.8339(3) 0.44213(15) 1.3786(3) 0.0369(8) Uani 1 1 d . . . C33 C 0.7303(3) 0.42740(14) 1.3160(2) 0.0349(8) Uani 1 1 d . . . C34 C 0.7141(3) 0.39242(17) 1.2246(2) 0.0470(9) Uani 1 1 d . . . H34A H 0.7848 0.3778 1.2221 0.070 Uiso 1 1 calc R . . H34B H 0.6809 0.4187 1.1691 0.070 Uiso 1 1 calc R . . H34C H 0.6659 0.3579 1.2230 0.070 Uiso 1 1 calc R . . N41 N 0.0992(2) 0.47016(11) 0.86723(18) 0.0314(6) Uani 1 1 d . . . N42 N 0.3098(2) 0.45049(11) 0.88559(19) 0.0331(6) Uani 1 1 d . . . C41 C -0.0043(3) 0.47800(16) 0.8614(2) 0.0382(8) Uani 1 1 d . . . C42 C -0.0898(3) 0.45452(18) 0.7876(3) 0.0443(9) Uani 1 1 d . . . C43 C -0.0690(3) 0.42302(17) 0.7147(3) 0.0404(9) Uani 1 1 d . . . C44 C 0.0394(3) 0.41542(14) 0.7157(2) 0.0318(7) Uani 1 1 d . . . C45 C 0.0711(3) 0.38557(15) 0.6418(2) 0.0366(8) Uani 1 1 d . . . C46 C 0.1764(3) 0.38016(16) 0.6472(2) 0.0395(9) Uani 1 1 d . . . C47 C 0.2622(3) 0.40170(14) 0.7288(2) 0.0333(7) Uani 1 1 d . . . C48 C 0.3736(3) 0.39418(16) 0.7416(3) 0.0418(9) Uani 1 1 d . . . C49 C 0.4489(3) 0.41305(17) 0.8258(3) 0.0469(9) Uani 1 1 d . . . C50 C 0.4148(3) 0.44084(16) 0.8971(3) 0.0383(8) Uani 1 1 d . . . C51 C 0.2342(3) 0.43070(13) 0.8034(2) 0.0290(7) Uani 1 1 d . . . C52 C 0.1217(3) 0.43918(13) 0.7948(2) 0.0281(7) Uani 1 1 d . . . O61 O 0.5518(2) 0.17289(11) 0.16950(19) 0.0492(7) Uani 1 1 d . . . C61 C 0.4647(4) 0.2658(2) 0.1763(5) 0.0891(18) Uani 1 1 d . . . H61A H 0.4769 0.3075 0.1998 0.134 Uiso 1 1 calc R . . H61B H 0.4118 0.2464 0.2023 0.134 Uiso 1 1 calc R . . H61C H 0.4363 0.2659 0.1058 0.134 Uiso 1 1 calc R . . C62 C 0.5716(4) 0.2315(2) 0.2090(4) 0.0637(12) Uani 1 1 d . . . C63 C 0.6476(3) 0.13572(19) 0.1942(4) 0.0509(10) Uani 1 1 d . . . C64 C 0.6158(3) 0.07331(17) 0.1626(3) 0.0522(10) Uani 1 1 d . . . H64A H 0.6814 0.0494 0.1680 0.078 Uiso 1 1 calc R . . H64B H 0.5684 0.0735 0.0955 0.078 Uiso 1 1 calc R . . H64C H 0.5765 0.0555 0.2035 0.078 Uiso 1 1 calc R . . H1N H 0.057(3) 0.6514(16) 1.043(2) 0.036(10) Uiso 1 1 d . . . H21N H 0.526(3) 0.4404(15) 1.227(3) 0.036(10) Uiso 1 1 d . . . H3 H 0.371(3) 0.6737(18) 0.987(3) 0.051(11) Uiso 1 1 d . . . H4 H 0.405(3) 0.7779(17) 1.000(3) 0.053(12) Uiso 1 1 d . . . H5 H 0.291(3) 0.8395(18) 1.047(3) 0.049(11) Uiso 1 1 d . . . H6 H 0.132(3) 0.7998(19) 1.070(3) 0.071(14) Uiso 1 1 d . . . H9 H 0.149(3) 0.7383(17) 1.235(3) 0.049(12) Uiso 1 1 d . . . H23 H 0.185(3) 0.4072(15) 1.229(2) 0.035(10) Uiso 1 1 d . . . H24 H 0.203(3) 0.3703(14) 1.377(2) 0.029(9) Uiso 1 1 d . . . H25 H 0.379(3) 0.3609(16) 1.491(3) 0.048(10) Uiso 1 1 d . . . H26 H 0.528(3) 0.3873(18) 1.444(3) 0.063(13) Uiso 1 1 d . . . H29 H 0.601(3) 0.4883(15) 1.446(2) 0.031(10) Uiso 1 1 d . . . H30 H 0.771(3) 0.5110(15) 1.548(3) 0.039(10) Uiso 1 1 d . . . H31 H 0.918(3) 0.4771(18) 1.503(3) 0.053(12) Uiso 1 1 d . . . H41 H -0.020(3) 0.4999(16) 0.908(3) 0.049(11) Uiso 1 1 d . . . H42 H -0.159(3) 0.4581(15) 0.788(3) 0.042(10) Uiso 1 1 d . . . H43 H -0.120(3) 0.4042(15) 0.666(2) 0.034(9) Uiso 1 1 d . . . H45 H 0.016(3) 0.3684(16) 0.590(3) 0.049(11) Uiso 1 1 d . . . H46 H 0.197(3) 0.3616(16) 0.603(3) 0.047(11) Uiso 1 1 d . . . H48 H 0.398(3) 0.3748(18) 0.694(3) 0.058(12) Uiso 1 1 d . . . H49 H 0.528(3) 0.4068(17) 0.841(3) 0.058(12) Uiso 1 1 d . . . H50 H 0.464(3) 0.4568(14) 0.960(2) 0.033(9) Uiso 1 1 d . . . H62A H 0.593(5) 0.220(3) 0.278(5) 0.13(2) Uiso 1 1 d . . . H62B H 0.632(4) 0.250(2) 0.175(3) 0.077(14) Uiso 1 1 d . . . H63A H 0.680(4) 0.137(2) 0.257(4) 0.084(17) Uiso 1 1 d . . . H63B H 0.703(4) 0.148(2) 0.159(4) 0.092(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.0363(3) 0.0304(3) 0.0318(3) -0.00477(17) 0.0089(2) -0.00147(18) O1 0.0478(15) 0.0323(13) 0.0393(13) -0.0053(10) 0.0164(12) -0.0015(11) O2 0.0471(16) 0.0388(14) 0.0608(17) -0.0144(12) 0.0204(14) -0.0092(12) Cl1 0.0678(8) 0.0532(7) 0.1085(10) 0.0138(6) 0.0388(7) 0.0059(5) N1 0.059(2) 0.042(2) 0.072(2) -0.0193(17) 0.0281(19) -0.0009(17) C1 0.050(2) 0.0340(19) 0.0302(18) -0.0042(14) 0.0091(17) -0.0020(17) C2 0.054(2) 0.0263(17) 0.0321(17) -0.0036(13) 0.0153(17) -0.0044(16) C3 0.067(3) 0.039(2) 0.049(2) -0.0108(17) 0.032(2) -0.009(2) C4 0.094(4) 0.040(2) 0.073(3) -0.020(2) 0.050(3) -0.029(2) C5 0.110(4) 0.029(2) 0.063(3) -0.0120(18) 0.047(3) -0.016(2) C6 0.075(3) 0.033(2) 0.050(2) -0.0033(17) 0.025(2) 0.006(2) C7 0.053(2) 0.0349(19) 0.0373(19) -0.0025(15) 0.0149(18) -0.0007(17) C8 0.058(3) 0.034(2) 0.057(2) 0.0083(17) 0.021(2) 0.0070(18) C9 0.073(3) 0.043(2) 0.058(3) -0.0074(19) 0.023(3) 0.003(2) C10 0.092(4) 0.053(3) 0.048(2) 0.0015(19) 0.020(3) 0.003(3) C11 0.061(3) 0.054(3) 0.097(4) 0.033(3) 0.038(3) 0.013(2) C12 0.072(3) 0.032(2) 0.065(3) 0.0093(18) 0.031(2) 0.007(2) C13 0.060(3) 0.0295(19) 0.056(2) 0.0061(16) 0.015(2) 0.0012(18) C14 0.063(3) 0.049(2) 0.081(3) -0.006(2) 0.021(3) -0.005(2) O21 0.0445(16) 0.0538(16) 0.0326(13) 0.0015(11) 0.0095(12) -0.0015(12) O22 0.0345(14) 0.0359(13) 0.0336(12) -0.0011(10) 0.0007(11) 0.0032(10) Cl2 0.0444(6) 0.0518(6) 0.0610(6) 0.0018(4) 0.0227(5) 0.0004(4) N21 0.0342(18) 0.056(2) 0.0312(17) 0.0048(14) 0.0063(15) 0.0003(14) C21 0.044(2) 0.0253(17) 0.0316(17) -0.0092(13) 0.0052(17) -0.0011(15) C22 0.037(2) 0.0218(16) 0.0357(18) -0.0027(13) 0.0071(16) 0.0007(14) C23 0.038(2) 0.0283(17) 0.039(2) -0.0040(14) 0.0053(18) -0.0014(16) C24 0.044(2) 0.0333(19) 0.045(2) -0.0046(15) 0.017(2) -0.0079(17) C25 0.058(3) 0.0310(18) 0.036(2) 0.0029(14) 0.0121(19) 0.0015(17) C26 0.045(2) 0.0331(18) 0.0330(18) 0.0012(14) 0.0044(18) 0.0028(17) C27 0.043(2) 0.0268(17) 0.0346(18) -0.0010(13) 0.0085(17) 0.0025(15) C28 0.037(2) 0.0307(17) 0.0323(17) 0.0040(13) 0.0040(16) 0.0013(15) C29 0.040(2) 0.0344(19) 0.039(2) 0.0017(15) 0.0112(19) 0.0025(17) C30 0.056(3) 0.0316(19) 0.037(2) -0.0045(15) 0.0104(19) -0.0064(17) C31 0.043(2) 0.0351(19) 0.040(2) -0.0009(15) 0.0068(19) -0.0080(17) C32 0.038(2) 0.0293(17) 0.044(2) 0.0069(14) 0.0145(17) -0.0009(15) C33 0.045(2) 0.0254(16) 0.0327(17) 0.0057(13) 0.0103(16) -0.0016(15) C34 0.055(3) 0.049(2) 0.037(2) -0.0043(16) 0.0129(19) -0.0036(19) N41 0.0325(16) 0.0294(14) 0.0324(14) 0.0007(11) 0.0102(13) 0.0010(12) N42 0.0342(17) 0.0274(14) 0.0352(15) -0.0031(11) 0.0075(13) -0.0030(12) C41 0.041(2) 0.041(2) 0.0324(19) -0.0030(15) 0.0120(17) 0.0018(17) C42 0.037(2) 0.055(2) 0.041(2) 0.0006(17) 0.0131(19) -0.0022(19) C43 0.035(2) 0.045(2) 0.036(2) -0.0024(16) 0.0049(18) -0.0079(17) C44 0.037(2) 0.0292(17) 0.0283(16) 0.0022(13) 0.0082(15) -0.0005(14) C45 0.043(2) 0.0353(19) 0.0275(17) -0.0019(14) 0.0051(17) -0.0028(16) C46 0.052(3) 0.0373(19) 0.0315(18) -0.0048(14) 0.0166(18) 0.0002(17) C47 0.037(2) 0.0287(17) 0.0353(18) -0.0009(13) 0.0124(16) 0.0019(15) C48 0.046(2) 0.041(2) 0.042(2) -0.0051(16) 0.0199(19) 0.0013(17) C49 0.040(2) 0.049(2) 0.054(2) -0.0034(18) 0.017(2) 0.0032(19) C50 0.034(2) 0.040(2) 0.041(2) -0.0042(16) 0.0105(17) 0.0005(16) C51 0.0299(19) 0.0251(16) 0.0298(16) -0.0007(12) 0.0064(14) -0.0014(13) C52 0.0339(19) 0.0226(15) 0.0275(16) 0.0025(12) 0.0092(14) -0.0006(13) O61 0.0479(16) 0.0420(15) 0.0617(16) -0.0026(12) 0.0230(14) -0.0056(12) C61 0.082(4) 0.047(3) 0.145(5) -0.007(3) 0.045(4) 0.005(3) C62 0.081(4) 0.045(2) 0.066(3) -0.005(2) 0.025(3) -0.008(2) C63 0.036(2) 0.055(3) 0.056(3) 0.009(2) 0.006(2) 0.0031(19) C64 0.051(3) 0.053(2) 0.052(2) 0.0055(18) 0.015(2) 0.0095(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Zn O1 1.966(2) . ? Zn O22 1.973(2) . ? Zn N41 2.083(3) . ? Zn N42 2.088(3) . ? Zn O21 2.478(2) . ? Zn C21 2.562(3) . ? Zn C1 2.595(3) . ? O1 C1 1.287(4) . ? O2 C1 1.249(4) . ? Cl1 C12 1.723(5) . ? N1 C7 1.365(5) . ? N1 C8 1.413(5) . ? N1 H1N 0.89(3) . ? C1 C2 1.490(5) . ? C2 C3 1.394(5) . ? C2 C7 1.414(5) . ? C3 C4 1.384(5) . ? C3 H3 0.91(4) . ? C4 C5 1.371(6) . ? C4 H4 0.90(4) . ? C5 C6 1.350(6) . ? C5 H5 0.93(4) . ? C6 C7 1.411(5) . ? C6 H6 0.95(4) . ? C8 C13 1.388(5) . ? C8 C9 1.422(6) . ? C9 C10 1.387(6) . ? C9 H9 0.95(4) . ? C10 C11 1.357(6) . ? C10 H10 0.9500 . ? C11 C12 1.393(7) . ? C11 H11 0.9500 . ? C12 C13 1.419(6) . ? C13 C14 1.465(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O21 C21 1.261(4) . ? O22 C21 1.273(4) . ? Cl2 C32 1.751(4) . ? N21 C27 1.386(4) . ? N21 C28 1.407(4) . ? N21 H21N 0.81(3) . ? C21 C22 1.492(5) . ? C22 C23 1.390(5) . ? C22 C27 1.412(5) . ? C23 C24 1.379(5) . ? C23 H23 0.88(3) . ? C24 C25 1.386(5) . ? C24 H24 0.89(3) . ? C25 C26 1.373(5) . ? C25 H25 0.96(4) . ? C26 C27 1.403(5) . ? C26 H26 0.95(4) . ? C28 C29 1.391(5) . ? C28 C33 1.408(5) . ? C29 C30 1.379(5) . ? C29 H29 0.86(4) . ? C30 C31 1.370(5) . ? C30 H30 0.95(4) . ? C31 C32 1.375(5) . ? C31 H31 0.89(4) . ? C32 C33 1.399(5) . ? C33 C34 1.501(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? N41 C41 1.323(4) . ? N41 C52 1.368(4) . ? N42 C50 1.329(4) . ? N42 C51 1.359(4) . ? C41 C42 1.378(5) . ? C41 H41 0.92(4) . ? C42 C43 1.368(5) . ? C42 H42 0.90(4) . ? C43 C44 1.405(5) . ? C43 H43 0.90(3) . ? C44 C52 1.403(4) . ? C44 C45 1.431(5) . ? C45 C46 1.342(5) . ? C45 H45 0.94(4) . ? C46 C47 1.429(5) . ? C46 H46 0.88(4) . ? C47 C48 1.400(5) . ? C47 C51 1.408(4) . ? C48 C49 1.371(5) . ? C48 H48 0.95(4) . ? C49 C50 1.396(5) . ? C49 H49 0.99(4) . ? C50 H50 1.00(3) . ? C51 C52 1.429(4) . ? O61 C62 1.410(5) . ? O61 C63 1.433(5) . ? C61 C62 1.515(7) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.99(6) . ? C62 H62B 1.13(5) . ? C63 C64 1.473(6) . ? C63 H63A 0.88(5) . ? C63 H63B 1.04(5) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? 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 Zn O22 113.14(9) . . ? O1 Zn N41 123.62(10) . . ? O22 Zn N41 104.89(10) . . ? O1 Zn N42 107.65(10) . . ? O22 Zn N42 124.96(10) . . ? N41 Zn N42 79.95(10) . . ? O1 Zn O21 92.37(9) . . ? O22 Zn O21 57.96(9) . . ? N41 Zn O21 143.78(9) . . ? N42 Zn O21 85.67(9) . . ? O1 Zn C21 103.39(10) . . ? O22 Zn C21 29.07(10) . . ? N41 Zn C21 128.21(11) . . ? N42 Zn C21 107.20(11) . . ? O21 Zn C21 28.92(9) . . ? O1 Zn C1 28.78(11) . . ? O22 Zn C1 102.32(10) . . ? N41 Zn C1 104.97(11) . . ? N42 Zn C1 129.92(11) . . ? O21 Zn C1 109.72(10) . . ? C21 Zn C1 107.34(10) . . ? C1 O1 Zn 103.9(2) . . ? C7 N1 C8 126.6(3) . . ? C7 N1 H1N 115(2) . . ? C8 N1 H1N 117(2) . . ? O2 C1 O1 121.6(3) . . ? O2 C1 C2 121.3(3) . . ? O1 C1 C2 117.1(3) . . ? O2 C1 Zn 74.24(19) . . ? O1 C1 Zn 47.36(16) . . ? C2 C1 Zn 164.5(3) . . ? C3 C2 C7 119.2(3) . . ? C3 C2 C1 118.6(3) . . ? C7 C2 C1 122.1(3) . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H3 125(3) . . ? C2 C3 H3 114(2) . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 121(3) . . ? C3 C4 H4 119(3) . . ? C6 C5 C4 121.2(4) . . ? C6 C5 H5 122(2) . . ? C4 C5 H5 117(2) . . ? C5 C6 C7 121.5(4) . . ? C5 C6 H6 123(3) . . ? C7 C6 H6 116(3) . . ? N1 C7 C6 121.6(4) . . ? N1 C7 C2 120.6(3) . . ? C6 C7 C2 117.7(4) . . ? C13 C8 N1 117.9(4) . . ? C13 C8 C9 121.6(4) . . ? N1 C8 C9 120.4(4) . . ? C10 C9 C8 117.8(5) . . ? C10 C9 H9 122(2) . . ? C8 C9 H9 119(2) . . ? C11 C10 C9 122.4(5) . . ? C11 C10 H10 118.8 . . ? C9 C10 H10 118.8 . . ? C10 C11 C12 119.5(5) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C13 121.2(4) . . ? C11 C12 Cl1 119.0(3) . . ? C13 C12 Cl1 119.8(3) . . ? C8 C13 C12 117.4(4) . . ? C8 C13 C14 120.5(4) . . ? C12 C13 C14 122.1(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C21 O21 Zn 79.3(2) . . ? C21 O22 Zn 102.1(2) . . ? C27 N21 C28 126.8(3) . . ? C27 N21 H21N 119(3) . . ? C28 N21 H21N 114(3) . . ? O21 C21 O22 120.6(3) . . ? O21 C21 C22 121.6(3) . . ? O22 C21 C22 117.8(3) . . ? O21 C21 Zn 71.82(19) . . ? O22 C21 Zn 48.87(16) . . ? C22 C21 Zn 166.2(3) . . ? C23 C22 C27 119.3(3) . . ? C23 C22 C21 119.0(3) . . ? C27 C22 C21 121.7(3) . . ? C24 C23 C22 122.1(4) . . ? C24 C23 H23 121(2) . . ? C22 C23 H23 117(2) . . ? C23 C24 C25 118.5(4) . . ? C23 C24 H24 119(2) . . ? C25 C24 H24 123(2) . . ? C26 C25 C24 121.0(4) . . ? C26 C25 H25 118(2) . . ? C24 C25 H25 121(2) . . ? C25 C26 C27 121.2(4) . . ? C25 C26 H26 122(2) . . ? C27 C26 H26 117(2) . . ? N21 C27 C26 121.5(3) . . ? N21 C27 C22 120.4(3) . . ? C26 C27 C22 118.0(3) . . ? C29 C28 N21 121.2(3) . . ? C29 C28 C33 120.7(3) . . ? N21 C28 C33 118.1(3) . . ? C30 C29 C28 120.1(4) . . ? C30 C29 H29 120(2) . . ? C28 C29 H29 120(2) . . ? C31 C30 C29 120.6(4) . . ? C31 C30 H30 119(2) . . ? C29 C30 H30 120(2) . . ? C30 C31 C32 119.2(4) . . ? C30 C31 H31 123(3) . . ? C32 C31 H31 118(3) . . ? C31 C32 C33 122.9(4) . . ? C31 C32 Cl2 117.7(3) . . ? C33 C32 Cl2 119.5(3) . . ? C32 C33 C28 116.5(3) . . ? C32 C33 C34 122.6(3) . . ? C28 C33 C34 120.9(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C41 N41 C52 118.2(3) . . ? C41 N41 Zn 129.0(2) . . ? C52 N41 Zn 112.7(2) . . ? C50 N42 C51 118.6(3) . . ? C50 N42 Zn 128.7(2) . . ? C51 N42 Zn 112.7(2) . . ? N41 C41 C42 122.9(3) . . ? N41 C41 H41 119(3) . . ? C42 C41 H41 118(3) . . ? C43 C42 C41 119.8(4) . . ? C43 C42 H42 119(2) . . ? C41 C42 H42 121(2) . . ? C42 C43 C44 119.5(3) . . ? C42 C43 H43 125(2) . . ? C44 C43 H43 116(2) . . ? C52 C44 C43 117.1(3) . . ? C52 C44 C45 118.2(3) . . ? C43 C44 C45 124.6(3) . . ? C46 C45 C44 121.4(3) . . ? C46 C45 H45 121(2) . . ? C44 C45 H45 118(2) . . ? C45 C46 C47 121.5(3) . . ? C45 C46 H46 122(2) . . ? C47 C46 H46 116(2) . . ? C48 C47 C51 117.0(3) . . ? C48 C47 C46 124.4(3) . . ? C51 C47 C46 118.6(3) . . ? C49 C48 C47 119.4(3) . . ? C49 C48 H48 120(2) . . ? C47 C48 H48 121(2) . . ? C48 C49 C50 120.2(4) . . ? C48 C49 H49 123(2) . . ? C50 C49 H49 117(2) . . ? N42 C50 C49 121.7(3) . . ? N42 C50 H50 112.8(18) . . ? C49 C50 H50 125.4(18) . . ? N42 C51 C47 123.0(3) . . ? N42 C51 C52 117.5(3) . . ? C47 C51 C52 119.5(3) . . ? N41 C52 C44 122.4(3) . . ? N41 C52 C51 117.0(3) . . ? C44 C52 C51 120.5(3) . . ? C62 O61 C63 113.2(3) . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O61 C62 C61 107.7(4) . . ? O61 C62 H62A 97(4) . . ? C61 C62 H62A 113(4) . . ? O61 C62 H62B 102(2) . . ? C61 C62 H62B 112(2) . . ? H62A C62 H62B 122(4) . . ? O61 C63 C64 109.1(3) . . ? O61 C63 H63A 110(3) . . ? C64 C63 H63A 110(3) . . ? O61 C63 H63B 114(3) . . ? C64 C63 H63B 105(3) . . ? H63A C63 H63B 110(4) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.670 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.069 # Attachment 'psxt17.cif' data_psxt17 _database_code_depnum_ccdc_archive 'CCDC 851686' #TrackingRef 'psxt17.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H19 Cl2 N3 O2 Zn' _chemical_formula_weight 541.71 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' 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.23360(10) _cell_length_b 16.8821(3) _cell_length_c 30.6278(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.5960(10) _cell_angle_gamma 90.00 _cell_volume 4751.59(13) _cell_formula_units_Z 8 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 33180 _cell_measurement_theta_min 6.70 _cell_measurement_theta_max 71.90 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 3.746 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.451 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33486 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 6.71 _diffrn_reflns_theta_max 65.00 _reflns_number_total 8014 _reflns_number_gt 7291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+5.7984P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8014 _refine_ls_number_parameters 765 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.29295(4) 0.56956(2) 0.179098(13) 0.03304(12) Uani 1 1 d . . . Cl1 Cl 0.42742(7) 0.62851(4) 0.23418(3) 0.04145(18) Uani 1 1 d . . . N1 N 0.0696(2) 0.59288(14) 0.17718(8) 0.0351(5) Uani 1 1 d . . . N2 N 0.2237(2) 0.46191(13) 0.20058(7) 0.0308(5) Uani 1 1 d . . . C1 C -0.0062(3) 0.6557(2) 0.16287(13) 0.0503(9) Uani 1 1 d . . . C2 C -0.1564(4) 0.6614(2) 0.16435(15) 0.0579(10) Uani 1 1 d . . . C3 C -0.2290(3) 0.6013(2) 0.18197(12) 0.0465(8) Uani 1 1 d . . . C4 C -0.1532(3) 0.53320(18) 0.19710(9) 0.0351(6) Uani 1 1 d . . . C5 C -0.2201(3) 0.4663(2) 0.21575(10) 0.0396(7) Uani 1 1 d . . . C6 C -0.1422(3) 0.4017(2) 0.22836(10) 0.0397(7) Uani 1 1 d . . . C7 C 0.0101(3) 0.39669(17) 0.22374(9) 0.0335(6) Uani 1 1 d . . . C8 C 0.0959(4) 0.33027(18) 0.23569(10) 0.0419(7) Uani 1 1 d . . . C9 C 0.2408(4) 0.33090(19) 0.22983(11) 0.0439(7) Uani 1 1 d . . . C10 C 0.3017(3) 0.39775(18) 0.21209(10) 0.0385(7) Uani 1 1 d . . . C11 C 0.0791(3) 0.46182(16) 0.20632(8) 0.0285(6) Uani 1 1 d . . . C12 C -0.0030(3) 0.53117(16) 0.19320(9) 0.0300(6) Uani 1 1 d . . . O21 O 0.4608(2) 0.51212(13) 0.13596(7) 0.0449(5) Uani 1 1 d . . . O22 O 0.3304(2) 0.61841(13) 0.12167(7) 0.0465(5) Uani 1 1 d . . . Cl2 Cl 1.01366(14) 0.25073(7) 0.13375(4) 0.0857(4) Uani 1 1 d . . . N21 N 0.6805(3) 0.48454(17) 0.08713(10) 0.0459(7) Uani 1 1 d . . . C21 C 0.4278(3) 0.57053(19) 0.11166(10) 0.0400(7) Uani 1 1 d . . . C22 C 0.4983(3) 0.58605(19) 0.07090(10) 0.0399(7) Uani 1 1 d . . . C23 C 0.4390(4) 0.6446(2) 0.04257(12) 0.0513(8) Uani 1 1 d . . . C24 C 0.4956(5) 0.6613(3) 0.00360(13) 0.0627(10) Uani 1 1 d . . . C25 C 0.6134(4) 0.6175(3) -0.00782(13) 0.0622(10) Uani 1 1 d . . . C26 C 0.6744(4) 0.5596(2) 0.01917(12) 0.0514(9) Uani 1 1 d . . . C27 C 0.6211(3) 0.54327(19) 0.05967(10) 0.0420(7) Uani 1 1 d . . . C28 C 0.8217(3) 0.4532(2) 0.09058(10) 0.0446(8) Uani 1 1 d . . . C29 C 0.9411(4) 0.4966(3) 0.07924(12) 0.0538(9) Uani 1 1 d . . . C30 C 1.0789(4) 0.4625(4) 0.08477(13) 0.0672(13) Uani 1 1 d . . . C31 C 1.1005(4) 0.3881(3) 0.10148(13) 0.0684(12) Uani 1 1 d . . . C32 C 0.9821(4) 0.3463(2) 0.11310(11) 0.0583(10) Uani 1 1 d . . . C33 C 0.8411(4) 0.3764(2) 0.10798(11) 0.0490(8) Uani 1 1 d . . . C34 C 0.7132(5) 0.3298(2) 0.11977(14) 0.0552(9) Uani 1 1 d . . . Zn2 Zn 0.78497(4) 0.90034(2) 0.154064(13) 0.03583(12) Uani 1 1 d . . . Cl3 Cl 0.92613(7) 0.85077(5) 0.21119(2) 0.0459(2) Uani 1 1 d . . . N41 N 0.7148(2) 1.01220(15) 0.17165(8) 0.0361(5) Uani 1 1 d . . . N42 N 0.5629(2) 0.87876(15) 0.15372(8) 0.0350(5) Uani 1 1 d . . . C41 C 0.7925(3) 1.0768(2) 0.18227(11) 0.0439(7) Uani 1 1 d . . . C42 C 0.7315(4) 1.1455(2) 0.19794(12) 0.0520(8) Uani 1 1 d . . . C43 C 0.5861(4) 1.1476(2) 0.20198(12) 0.0508(8) Uani 1 1 d . . . C44 C 0.4993(3) 1.08108(19) 0.19079(10) 0.0401(7) Uani 1 1 d . . . C45 C 0.3453(4) 1.0767(2) 0.19418(12) 0.0491(9) Uani 1 1 d . . . C46 C 0.2688(3) 1.0109(2) 0.18351(11) 0.0467(8) Uani 1 1 d . . . C47 C 0.3372(3) 0.94160(19) 0.16831(9) 0.0371(7) Uani 1 1 d . . . C48 C 0.2636(3) 0.8707(2) 0.15676(11) 0.0448(8) Uani 1 1 d . . . C49 C 0.3393(3) 0.8067(2) 0.14361(12) 0.0462(8) Uani 1 1 d . . . C50 C 0.4902(3) 0.8132(2) 0.14265(11) 0.0427(7) Uani 1 1 d . . . C51 C 0.4886(3) 0.94304(18) 0.16559(9) 0.0328(6) Uani 1 1 d . . . C52 C 0.5696(3) 1.01372(18) 0.17608(9) 0.0340(6) Uani 1 1 d . . . O61 O 0.8082(2) 0.81682(13) 0.10463(7) 0.0440(5) Uani 1 1 d . . . O62 O 0.9317(2) 0.92696(12) 0.10426(7) 0.0408(5) Uani 1 1 d . . . N61 N 1.1538(3) 0.93344(15) 0.05317(9) 0.0386(6) Uani 1 1 d . . . Cl4 Cl 1.4861(2) 1.17336(9) 0.07949(5) 0.1406(8) Uani 1 1 d . . . C61 C 0.9045(3) 0.85796(18) 0.08902(9) 0.0365(7) Uani 1 1 d . . . C62 C 0.9831(3) 0.82468(18) 0.05313(9) 0.0348(6) Uani 1 1 d . . . C63 C 0.9334(4) 0.7518(2) 0.03545(11) 0.0475(8) Uani 1 1 d . . . C64 C 0.9998(5) 0.7152(3) 0.00256(13) 0.0611(10) Uani 1 1 d . . . C65 C 1.1154(4) 0.7525(2) -0.01414(12) 0.0588(10) Uani 1 1 d . . . C66 C 1.1662(4) 0.8241(2) 0.00188(10) 0.0468(8) Uani 1 1 d . . . C67 C 1.1039(3) 0.86108(18) 0.03672(9) 0.0353(6) Uani 1 1 d . . . C68 C 1.2951(3) 0.9641(2) 0.05445(9) 0.0409(7) Uani 1 1 d . . . C69 C 1.4158(3) 0.9162(3) 0.04953(11) 0.0523(9) Uani 1 1 d . . . C70 C 1.5539(4) 0.9475(4) 0.05244(13) 0.0741(14) Uani 1 1 d . . . C71 C 1.5754(5) 1.0248(4) 0.06141(14) 0.0860(18) Uani 1 1 d . . . C72 C 1.4581(6) 1.0736(3) 0.06698(13) 0.0801(16) Uani 1 1 d . . . C73 C 1.3113(4) 1.0455(2) 0.06283(11) 0.0546(9) Uani 1 1 d . . . C74 C 1.1805(7) 1.0962(3) 0.06706(18) 0.0763(14) Uani 1 1 d . . . H21N H 0.639(4) 0.474(2) 0.1059(11) 0.042(10) Uiso 1 1 d . . . H1 H 0.045(4) 0.698(2) 0.1535(12) 0.053(10) Uiso 1 1 d . . . H2 H -0.202(4) 0.706(2) 0.1529(13) 0.068(12) Uiso 1 1 d . . . H3 H -0.325(4) 0.602(2) 0.1842(11) 0.051(10) Uiso 1 1 d . . . H5 H -0.322(4) 0.470(2) 0.2188(11) 0.055(10) Uiso 1 1 d . . . H6 H -0.183(4) 0.358(2) 0.2400(11) 0.044(9) Uiso 1 1 d . . . H8 H 0.047(4) 0.286(2) 0.2470(11) 0.046(9) Uiso 1 1 d . . . H9 H 0.300(4) 0.292(2) 0.2388(13) 0.061(11) Uiso 1 1 d . . . H10 H 0.402(3) 0.3993(17) 0.2081(10) 0.033(8) Uiso 1 1 d . . . H23 H 0.360(4) 0.674(2) 0.0503(11) 0.050(10) Uiso 1 1 d . . . H24 H 0.453(4) 0.697(2) -0.0134(13) 0.059(11) Uiso 1 1 d . . . H25 H 0.654(4) 0.625(2) -0.0351(13) 0.064(11) Uiso 1 1 d . . . H26 H 0.749(4) 0.527(2) 0.0104(11) 0.048(9) Uiso 1 1 d . . . H29 H 0.931(3) 0.546(2) 0.0680(10) 0.036(9) Uiso 1 1 d . . . H30 H 1.142(5) 0.495(2) 0.0771(13) 0.063(12) Uiso 1 1 d . . . H31 H 1.199(5) 0.362(3) 0.1058(16) 0.098(16) Uiso 1 1 d . . . H34A H 0.735(5) 0.271(3) 0.1220(16) 0.103(17) Uiso 1 1 d . . . H34B H 0.675(5) 0.348(3) 0.1428(15) 0.074(14) Uiso 1 1 d . . . H34C H 0.634(4) 0.335(2) 0.0976(14) 0.065(12) Uiso 1 1 d . . . H61N H 1.100(3) 0.9543(18) 0.0700(10) 0.033(8) Uiso 1 1 d . . . H41 H 0.892(4) 1.0731(19) 0.1794(11) 0.044(9) Uiso 1 1 d . . . H42 H 0.795(4) 1.188(2) 0.2060(12) 0.055(10) Uiso 1 1 d . . . H43 H 0.543(4) 1.191(2) 0.2134(13) 0.067(12) Uiso 1 1 d . . . H45 H 0.304(4) 1.119(2) 0.2043(11) 0.047(9) Uiso 1 1 d . . . H46 H 0.162(4) 1.008(2) 0.1866(12) 0.058(10) Uiso 1 1 d . . . H48 H 0.160(4) 0.868(2) 0.1587(12) 0.056(10) Uiso 1 1 d . . . H49 H 0.293(4) 0.760(2) 0.1354(12) 0.056(11) Uiso 1 1 d . . . H50 H 0.538(4) 0.770(2) 0.1343(11) 0.043(9) Uiso 1 1 d . . . H63 H 0.851(4) 0.727(2) 0.0484(12) 0.056(10) Uiso 1 1 d . . . H64 H 0.967(4) 0.668(3) -0.0083(14) 0.075(13) Uiso 1 1 d . . . H65 H 1.159(4) 0.733(2) -0.0374(14) 0.072(12) Uiso 1 1 d . . . H66 H 1.240(4) 0.8493(19) -0.0096(11) 0.042(9) Uiso 1 1 d . . . H69 H 1.407(5) 0.855(3) 0.0476(16) 0.093(16) Uiso 1 1 d . . . H70 H 1.657(7) 0.912(4) 0.047(2) 0.16(3) Uiso 1 1 d . . . H71 H 1.678(6) 1.050(3) 0.0653(17) 0.111(17) Uiso 1 1 d . . . H74A H 1.201(6) 1.150(4) 0.0691(18) 0.111(18) Uiso 1 1 d . . . H74B H 1.140(5) 1.085(3) 0.0951(18) 0.095(16) Uiso 1 1 d . . . H74C H 1.107(5) 1.082(3) 0.0451(17) 0.086(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02415(19) 0.0319(2) 0.0442(2) 0.00289(16) 0.00899(16) -0.00432(14) Cl1 0.0318(3) 0.0402(4) 0.0532(4) -0.0079(3) 0.0084(3) -0.0088(3) N1 0.0257(11) 0.0307(12) 0.0495(14) 0.0027(11) 0.0071(10) -0.0031(9) N2 0.0274(11) 0.0314(12) 0.0341(12) -0.0008(10) 0.0052(9) -0.0035(9) C1 0.0351(16) 0.0353(17) 0.080(3) 0.0126(17) 0.0048(16) -0.0036(14) C2 0.0338(17) 0.0388(19) 0.099(3) 0.0061(19) -0.0023(18) 0.0056(14) C3 0.0225(15) 0.049(2) 0.069(2) -0.0097(16) 0.0055(14) 0.0017(13) C4 0.0262(14) 0.0414(16) 0.0383(15) -0.0087(13) 0.0062(11) -0.0058(12) C5 0.0284(15) 0.0536(19) 0.0381(16) -0.0087(14) 0.0106(12) -0.0131(13) C6 0.0395(17) 0.0452(18) 0.0358(16) -0.0022(14) 0.0110(13) -0.0188(14) C7 0.0372(15) 0.0360(16) 0.0275(14) -0.0032(12) 0.0047(12) -0.0109(12) C8 0.0519(19) 0.0323(16) 0.0408(17) 0.0021(13) 0.0007(14) -0.0120(14) C9 0.0471(18) 0.0301(16) 0.0528(19) -0.0014(14) -0.0043(15) 0.0021(14) C10 0.0325(16) 0.0363(16) 0.0461(18) -0.0037(13) 0.0014(13) 0.0033(12) C11 0.0265(13) 0.0318(14) 0.0276(13) -0.0046(11) 0.0057(10) -0.0058(11) C12 0.0250(13) 0.0323(14) 0.0333(14) -0.0054(11) 0.0063(11) -0.0057(11) O21 0.0419(12) 0.0462(13) 0.0492(13) 0.0043(11) 0.0171(10) -0.0090(10) O22 0.0391(12) 0.0534(13) 0.0493(13) 0.0038(11) 0.0157(10) -0.0010(10) Cl2 0.1038(9) 0.0843(8) 0.0649(6) -0.0230(6) -0.0129(6) 0.0395(6) N21 0.0406(15) 0.0488(17) 0.0510(17) -0.0033(14) 0.0182(13) -0.0058(12) C21 0.0303(15) 0.0473(19) 0.0435(17) -0.0073(15) 0.0085(13) -0.0142(13) C22 0.0356(15) 0.0428(17) 0.0429(17) -0.0045(14) 0.0118(13) -0.0123(13) C23 0.050(2) 0.057(2) 0.049(2) 0.0031(17) 0.0135(16) -0.0018(17) C24 0.068(2) 0.072(3) 0.049(2) 0.014(2) 0.0136(19) 0.001(2) C25 0.066(2) 0.081(3) 0.043(2) 0.002(2) 0.0221(18) -0.014(2) C26 0.0475(19) 0.063(2) 0.047(2) -0.0092(17) 0.0182(16) -0.0093(17) C27 0.0400(16) 0.0445(18) 0.0428(17) -0.0062(14) 0.0101(14) -0.0138(14) C28 0.0386(17) 0.053(2) 0.0433(17) -0.0192(15) 0.0094(14) -0.0058(14) C29 0.046(2) 0.065(3) 0.052(2) -0.0185(19) 0.0120(16) -0.0146(17) C30 0.041(2) 0.112(4) 0.050(2) -0.033(2) 0.0145(17) -0.023(2) C31 0.048(2) 0.108(4) 0.048(2) -0.032(2) 0.0019(17) 0.013(2) C32 0.059(2) 0.072(3) 0.0424(19) -0.0263(18) -0.0030(16) 0.0126(19) C33 0.0519(19) 0.054(2) 0.0400(17) -0.0211(16) 0.0006(15) 0.0003(16) C34 0.063(2) 0.049(2) 0.053(2) -0.0099(18) 0.000(2) -0.0075(18) Zn2 0.02242(19) 0.0424(2) 0.0433(2) -0.00732(17) 0.00629(16) 0.00457(15) Cl3 0.0278(3) 0.0667(5) 0.0434(4) -0.0069(4) 0.0040(3) 0.0132(3) N41 0.0284(12) 0.0436(14) 0.0368(13) 0.0009(11) 0.0059(10) 0.0039(10) N42 0.0245(11) 0.0412(14) 0.0398(13) 0.0009(11) 0.0048(10) 0.0059(10) C41 0.0345(17) 0.0452(19) 0.0518(19) -0.0007(15) 0.0036(14) -0.0023(14) C42 0.054(2) 0.0423(19) 0.058(2) -0.0034(16) -0.0015(17) 0.0008(16) C43 0.058(2) 0.0434(19) 0.052(2) -0.0029(16) 0.0058(16) 0.0169(16) C44 0.0413(17) 0.0444(18) 0.0354(16) 0.0065(13) 0.0080(13) 0.0129(14) C45 0.0437(19) 0.057(2) 0.0491(19) 0.0044(16) 0.0161(15) 0.0247(17) C46 0.0310(16) 0.065(2) 0.0461(18) 0.0108(16) 0.0129(13) 0.0165(15) C47 0.0265(14) 0.0519(18) 0.0337(15) 0.0120(13) 0.0074(12) 0.0076(12) C48 0.0251(15) 0.061(2) 0.0490(19) 0.0175(16) 0.0056(13) 0.0018(14) C49 0.0326(16) 0.050(2) 0.056(2) 0.0104(16) 0.0016(14) -0.0061(14) C50 0.0313(15) 0.0432(18) 0.0537(19) -0.0002(15) 0.0039(14) 0.0037(14) C51 0.0254(13) 0.0439(16) 0.0298(14) 0.0084(12) 0.0059(11) 0.0076(12) C52 0.0312(14) 0.0434(17) 0.0281(14) 0.0045(12) 0.0065(11) 0.0097(12) O61 0.0358(11) 0.0540(13) 0.0440(12) -0.0046(10) 0.0134(9) -0.0048(10) O62 0.0402(11) 0.0397(12) 0.0445(12) -0.0055(9) 0.0132(9) 0.0064(9) N61 0.0339(13) 0.0398(14) 0.0434(15) -0.0030(12) 0.0107(12) 0.0011(11) Cl4 0.2254(19) 0.1046(11) 0.0830(8) 0.0290(8) -0.0296(10) -0.1151(12) C61 0.0288(14) 0.0451(18) 0.0354(15) 0.0015(13) 0.0018(12) 0.0079(12) C62 0.0317(14) 0.0418(17) 0.0310(14) -0.0030(12) 0.0028(12) 0.0019(12) C63 0.0464(18) 0.054(2) 0.0429(18) -0.0106(15) 0.0057(15) -0.0080(15) C64 0.070(2) 0.060(2) 0.054(2) -0.0258(19) 0.0102(18) -0.011(2) C65 0.063(2) 0.071(3) 0.044(2) -0.0238(18) 0.0137(17) 0.0032(19) C66 0.0392(17) 0.066(2) 0.0365(17) -0.0051(16) 0.0117(14) -0.0003(16) C67 0.0310(14) 0.0422(16) 0.0326(15) -0.0022(13) 0.0021(11) 0.0048(12) C68 0.0406(16) 0.0515(19) 0.0306(15) 0.0088(13) 0.0027(12) -0.0089(14) C69 0.0324(17) 0.085(3) 0.0391(18) 0.0141(18) 0.0023(14) 0.0004(17) C70 0.041(2) 0.132(4) 0.048(2) 0.034(3) -0.0030(17) -0.018(2) C71 0.057(3) 0.150(5) 0.048(2) 0.042(3) -0.011(2) -0.040(3) C72 0.119(4) 0.079(3) 0.039(2) 0.024(2) -0.010(2) -0.058(3) C73 0.073(2) 0.053(2) 0.0363(17) 0.0113(15) -0.0021(16) -0.0205(18) C74 0.123(4) 0.038(2) 0.067(3) 0.000(2) 0.008(3) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O22 2.003(2) . ? Zn1 N2 2.056(2) . ? Zn1 N1 2.095(2) . ? Zn1 Cl1 2.2292(8) . ? Zn1 O21 2.343(2) . ? Zn1 C21 2.514(3) . ? N1 C1 1.321(4) . ? N1 C12 1.356(3) . ? N2 C10 1.329(4) . ? N2 C11 1.364(3) . ? C1 C2 1.396(5) . ? C1 H1 0.92(4) . ? C2 C3 1.356(5) . ? C2 H2 0.91(4) . ? C3 C4 1.402(4) . ? C3 H3 0.90(4) . ? C4 C12 1.404(4) . ? C4 C5 1.432(4) . ? C5 C6 1.342(5) . ? C5 H5 0.96(4) . ? C6 C7 1.430(4) . ? C6 H6 0.92(3) . ? C7 C8 1.401(4) . ? C7 C11 1.402(4) . ? C8 C9 1.367(5) . ? C8 H8 0.96(3) . ? C9 C10 1.394(4) . ? C9 H9 0.88(4) . ? C10 H10 0.95(3) . ? C11 C12 1.431(4) . ? O21 C21 1.255(4) . ? O22 C21 1.268(4) . ? Cl2 C32 1.747(4) . ? N21 C27 1.379(4) . ? N21 C28 1.401(4) . ? N21 H21N 0.74(3) . ? C21 C22 1.486(4) . ? C22 C23 1.392(5) . ? C22 C27 1.415(4) . ? C23 C24 1.378(5) . ? C23 H23 0.93(4) . ? C24 C25 1.388(6) . ? C24 H24 0.87(4) . ? C25 C26 1.366(6) . ? C25 H25 0.95(4) . ? C26 C27 1.406(4) . ? C26 H26 0.94(3) . ? C28 C29 1.396(5) . ? C28 C33 1.407(5) . ? C29 C30 1.391(6) . ? C29 H29 0.91(3) . ? C30 C31 1.364(7) . ? C30 H30 0.85(4) . ? C31 C32 1.376(6) . ? C31 H31 1.00(5) . ? C32 C33 1.392(5) . ? C33 C34 1.493(5) . ? C34 H34A 1.02(5) . ? C34 H34B 0.88(5) . ? C34 H34C 0.95(4) . ? Zn2 N42 2.082(2) . ? Zn2 N41 2.084(2) . ? Zn2 O61 2.095(2) . ? Zn2 O62 2.184(2) . ? Zn2 Cl3 2.2395(8) . ? Zn2 C61 2.475(3) . ? N41 C41 1.328(4) . ? N41 C52 1.361(3) . ? N42 C50 1.321(4) . ? N42 C51 1.352(4) . ? C41 C42 1.395(5) . ? C41 H41 0.93(3) . ? C42 C43 1.361(5) . ? C42 H42 0.95(4) . ? C43 C44 1.403(5) . ? C43 H43 0.93(4) . ? C44 C52 1.405(4) . ? C44 C45 1.437(4) . ? C45 C46 1.339(5) . ? C45 H45 0.88(4) . ? C46 C47 1.430(4) . ? C46 H46 1.00(4) . ? C47 C48 1.405(5) . ? C47 C51 1.409(4) . ? C48 C49 1.368(5) . ? C48 H48 0.97(4) . ? C49 C50 1.400(4) . ? C49 H49 0.92(4) . ? C50 H50 0.90(3) . ? C51 C52 1.428(4) . ? O61 C61 1.259(4) . ? O62 C61 1.271(4) . ? N61 C67 1.383(4) . ? N61 C68 1.401(4) . ? N61 H61N 0.83(3) . ? Cl4 C72 1.740(5) . ? C61 C62 1.486(4) . ? C62 C63 1.404(4) . ? C62 C67 1.408(4) . ? C63 C64 1.376(5) . ? C63 H63 0.98(4) . ? C64 C65 1.379(6) . ? C64 H64 0.90(4) . ? C65 C66 1.370(5) . ? C65 H65 0.91(4) . ? C66 C67 1.407(4) . ? C66 H66 0.90(3) . ? C68 C69 1.398(5) . ? C68 C73 1.403(5) . ? C69 C70 1.376(5) . ? C69 H69 1.03(5) . ? C70 C71 1.344(8) . ? C70 H70 1.15(7) . ? C71 C72 1.385(8) . ? C71 H71 1.04(5) . ? C72 C73 1.430(6) . ? C73 C74 1.496(7) . ? C74 H74A 0.92(6) . ? C74 H74B 0.99(5) . ? C74 H74C 0.94(5) . ? 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 O22 Zn1 N2 136.95(9) . . ? O22 Zn1 N1 98.74(9) . . ? N2 Zn1 N1 80.74(9) . . ? O22 Zn1 Cl1 110.45(7) . . ? N2 Zn1 Cl1 108.67(7) . . ? N1 Zn1 Cl1 114.30(7) . . ? O22 Zn1 O21 59.65(8) . . ? N2 Zn1 O21 93.33(8) . . ? N1 Zn1 O21 139.97(9) . . ? Cl1 Zn1 O21 105.15(6) . . ? O22 Zn1 C21 29.99(10) . . ? N2 Zn1 C21 117.59(10) . . ? N1 Zn1 C21 122.75(10) . . ? Cl1 Zn1 C21 109.57(7) . . ? O21 Zn1 C21 29.69(9) . . ? C1 N1 C12 118.2(2) . . ? C1 N1 Zn1 130.4(2) . . ? C12 N1 Zn1 111.44(18) . . ? C10 N2 C11 118.5(2) . . ? C10 N2 Zn1 128.91(19) . . ? C11 N2 Zn1 112.41(18) . . ? N1 C1 C2 122.7(3) . . ? N1 C1 H1 117(2) . . ? C2 C1 H1 120(2) . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H2 123(3) . . ? C1 C2 H2 118(3) . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3 124(2) . . ? C4 C3 H3 117(2) . . ? C3 C4 C12 117.2(3) . . ? C3 C4 C5 123.9(3) . . ? C12 C4 C5 118.9(3) . . ? C6 C5 C4 121.0(3) . . ? C6 C5 H5 122(2) . . ? C4 C5 H5 117(2) . . ? C5 C6 C7 121.7(3) . . ? C5 C6 H6 123(2) . . ? C7 C6 H6 115(2) . . ? C8 C7 C11 117.5(3) . . ? C8 C7 C6 124.0(3) . . ? C11 C7 C6 118.6(3) . . ? C9 C8 C7 119.7(3) . . ? C9 C8 H8 124(2) . . ? C7 C8 H8 117(2) . . ? C8 C9 C10 119.6(3) . . ? C8 C9 H9 122(3) . . ? C10 C9 H9 118(3) . . ? N2 C10 C9 122.3(3) . . ? N2 C10 H10 117.0(18) . . ? C9 C10 H10 120.7(18) . . ? N2 C11 C7 122.5(3) . . ? N2 C11 C12 117.5(2) . . ? C7 C11 C12 120.1(2) . . ? N1 C12 C4 122.6(3) . . ? N1 C12 C11 117.6(2) . . ? C4 C12 C11 119.8(2) . . ? C21 O21 Zn1 82.72(17) . . ? C21 O22 Zn1 97.9(2) . . ? C27 N21 C28 129.0(3) . . ? C27 N21 H21N 116(3) . . ? C28 N21 H21N 114(3) . . ? O21 C21 O22 119.6(3) . . ? O21 C21 C22 122.4(3) . . ? O22 C21 C22 118.0(3) . . ? O21 C21 Zn1 67.59(16) . . ? O22 C21 Zn1 52.12(15) . . ? C22 C21 Zn1 169.7(2) . . ? C23 C22 C27 119.1(3) . . ? C23 C22 C21 118.1(3) . . ? C27 C22 C21 122.8(3) . . ? C24 C23 C22 121.7(4) . . ? C24 C23 H23 119(2) . . ? C22 C23 H23 119(2) . . ? C23 C24 C25 118.8(4) . . ? C23 C24 H24 118(3) . . ? C25 C24 H24 123(3) . . ? C26 C25 C24 121.0(3) . . ? C26 C25 H25 116(2) . . ? C24 C25 H25 122(2) . . ? C25 C26 C27 121.0(3) . . ? C25 C26 H26 121(2) . . ? C27 C26 H26 118(2) . . ? N21 C27 C26 121.8(3) . . ? N21 C27 C22 120.0(3) . . ? C26 C27 C22 118.2(3) . . ? C29 C28 N21 122.4(3) . . ? C29 C28 C33 120.2(3) . . ? N21 C28 C33 117.4(3) . . ? C30 C29 C28 119.2(4) . . ? C30 C29 H29 119(2) . . ? C28 C29 H29 122(2) . . ? C31 C30 C29 121.7(4) . . ? C31 C30 H30 128(3) . . ? C29 C30 H30 111(3) . . ? C30 C31 C32 118.5(4) . . ? C30 C31 H31 123(3) . . ? C32 C31 H31 118(3) . . ? C31 C32 C33 122.8(4) . . ? C31 C32 Cl2 117.3(3) . . ? C33 C32 Cl2 119.9(3) . . ? C32 C33 C28 117.5(3) . . ? C32 C33 C34 122.3(4) . . ? C28 C33 C34 120.2(3) . . ? C33 C34 H34A 112(3) . . ? C33 C34 H34B 113(3) . . ? H34A C34 H34B 113(4) . . ? C33 C34 H34C 110(2) . . ? H34A C34 H34C 106(4) . . ? H34B C34 H34C 102(4) . . ? N42 Zn2 N41 80.16(9) . . ? N42 Zn2 O61 92.79(9) . . ? N41 Zn2 O61 148.51(9) . . ? N42 Zn2 O62 135.28(9) . . ? N41 Zn2 O62 102.92(8) . . ? O61 Zn2 O62 61.28(8) . . ? N42 Zn2 Cl3 115.88(7) . . ? N41 Zn2 Cl3 107.97(7) . . ? O61 Zn2 Cl3 102.73(7) . . ? O62 Zn2 Cl3 105.61(6) . . ? N42 Zn2 C61 117.50(10) . . ? N41 Zn2 C61 130.09(10) . . ? O61 Zn2 C61 30.55(9) . . ? O62 Zn2 C61 30.85(9) . . ? Cl3 Zn2 C61 104.45(7) . . ? C41 N41 C52 118.3(3) . . ? C41 N41 Zn2 129.3(2) . . ? C52 N41 Zn2 112.14(19) . . ? C50 N42 C51 118.9(2) . . ? C50 N42 Zn2 128.6(2) . . ? C51 N42 Zn2 112.54(19) . . ? N41 C41 C42 122.7(3) . . ? N41 C41 H41 116(2) . . ? C42 C41 H41 121(2) . . ? C43 C42 C41 119.2(3) . . ? C43 C42 H42 123(2) . . ? C41 C42 H42 118(2) . . ? C42 C43 C44 120.1(3) . . ? C42 C43 H43 122(3) . . ? C44 C43 H43 118(3) . . ? C43 C44 C52 117.1(3) . . ? C43 C44 C45 124.7(3) . . ? C52 C44 C45 118.2(3) . . ? C46 C45 C44 121.8(3) . . ? C46 C45 H45 122(2) . . ? C44 C45 H45 117(2) . . ? C45 C46 C47 121.2(3) . . ? C45 C46 H46 122(2) . . ? C47 C46 H46 117(2) . . ? C48 C47 C51 117.3(3) . . ? C48 C47 C46 124.1(3) . . ? C51 C47 C46 118.5(3) . . ? C49 C48 C47 119.9(3) . . ? C49 C48 H48 121(2) . . ? C47 C48 H48 119(2) . . ? C48 C49 C50 118.8(3) . . ? C48 C49 H49 121(2) . . ? C50 C49 H49 120(2) . . ? N42 C50 C49 122.8(3) . . ? N42 C50 H50 120(2) . . ? C49 C50 H50 118(2) . . ? N42 C51 C47 122.3(3) . . ? N42 C51 C52 117.6(2) . . ? C47 C51 C52 120.1(3) . . ? N41 C52 C44 122.5(3) . . ? N41 C52 C51 117.5(2) . . ? C44 C52 C51 120.0(3) . . ? C61 O61 Zn2 91.66(18) . . ? C61 O62 Zn2 87.35(17) . . ? C67 N61 C68 127.8(3) . . ? C67 N61 H61N 114(2) . . ? C68 N61 H61N 116(2) . . ? O61 C61 O62 119.2(3) . . ? O61 C61 C62 119.1(3) . . ? O62 C61 C62 121.7(3) . . ? O61 C61 Zn2 57.79(15) . . ? O62 C61 Zn2 61.79(15) . . ? C62 C61 Zn2 173.4(2) . . ? C63 C62 C67 119.0(3) . . ? C63 C62 C61 116.9(3) . . ? C67 C62 C61 124.1(3) . . ? C64 C63 C62 121.6(3) . . ? C64 C63 H63 122(2) . . ? C62 C63 H63 117(2) . . ? C63 C64 C65 118.9(4) . . ? C63 C64 H64 121(3) . . ? C65 C64 H64 120(3) . . ? C66 C65 C64 121.3(3) . . ? C66 C65 H65 116(3) . . ? C64 C65 H65 122(3) . . ? C65 C66 C67 120.8(3) . . ? C65 C66 H66 121(2) . . ? C67 C66 H66 118(2) . . ? N61 C67 C66 121.5(3) . . ? N61 C67 C62 120.2(3) . . ? C66 C67 C62 118.3(3) . . ? C69 C68 N61 122.2(3) . . ? C69 C68 C73 121.0(3) . . ? N61 C68 C73 116.7(3) . . ? C70 C69 C68 120.9(4) . . ? C70 C69 H69 117(3) . . ? C68 C69 H69 122(3) . . ? C71 C70 C69 120.3(5) . . ? C71 C70 H70 116(3) . . ? C69 C70 H70 124(3) . . ? C70 C71 C72 120.1(4) . . ? C70 C71 H71 123(3) . . ? C72 C71 H71 117(3) . . ? C71 C72 C73 122.5(4) . . ? C71 C72 Cl4 120.1(4) . . ? C73 C72 Cl4 117.4(5) . . ? C68 C73 C72 115.1(4) . . ? C68 C73 C74 120.3(4) . . ? C72 C73 C74 124.6(4) . . ? C73 C74 H74A 114(3) . . ? C73 C74 H74B 110(3) . . ? H74A C74 H74B 103(4) . . ? C73 C74 H74C 109(3) . . ? H74A C74 H74C 115(4) . . ? H74B C74 H74C 106(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.232 _refine_diff_density_min -1.319 _refine_diff_density_rms 0.059 # Attachment 'psxt3a.cif' data_psxt3a _database_code_depnum_ccdc_archive 'CCDC 851687' #TrackingRef 'psxt3a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H74 Cl6 N6 O14 Zn3' _chemical_formula_weight 1824.32 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' 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' Cl Cl 0.3639 0.7018 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.3955(2) _cell_length_b 11.1192(2) _cell_length_c 24.9784(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.7500(10) _cell_angle_gamma 90.00 _cell_volume 3961.68(11) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 20344 _cell_measurement_theta_min 6.55 _cell_measurement_theta_max 71.91 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 3.503 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26010 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.0978 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 6.55 _diffrn_reflns_theta_max 65.00 _reflns_number_total 6453 _reflns_number_gt 4420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6453 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.0000 0.0000 0.5000 0.0277(2) Uani 1 2 d S . . Zn2 Zn 1.05119(4) 0.30055(5) 0.47162(2) 0.0294(2) Uani 1 1 d . . . N1 N 0.7988(3) 0.1057(3) 0.61018(16) 0.0370(11) Uani 1 1 d . . . O1 O 0.9052(2) 0.1227(2) 0.52757(10) 0.0294(7) Uani 1 1 d . . . O2 O 0.9423(2) 0.3122(2) 0.50937(11) 0.0296(7) Uani 1 1 d . . . Cl1 Cl 0.61481(12) -0.26248(13) 0.66298(6) 0.0801(5) Uani 1 1 d . . . C1 C 0.8919(3) 0.2337(4) 0.52925(15) 0.0269(10) Uani 1 1 d . . . C2 C 0.8128(3) 0.2832(4) 0.55531(16) 0.0279(11) Uani 1 1 d . . . C3 C 0.7793(4) 0.3997(4) 0.54083(19) 0.0348(13) Uani 1 1 d . . . C4 C 0.7136(3) 0.4575(5) 0.56609(19) 0.0384(12) Uani 1 1 d . . . C5 C 0.6798(4) 0.3996(5) 0.6078(2) 0.0417(14) Uani 1 1 d . . . C6 C 0.7068(3) 0.2839(4) 0.62295(18) 0.0375(12) Uani 1 1 d . . . C7 C 0.7727(3) 0.2233(4) 0.59628(16) 0.0294(11) Uani 1 1 d . . . C8 C 0.7617(3) 0.0381(4) 0.64989(17) 0.0340(11) Uani 1 1 d . . . C9 C 0.7749(4) 0.0774(5) 0.70305(19) 0.0414(13) Uani 1 1 d . . . C10 C 0.7395(4) 0.0130(5) 0.7427(2) 0.0503(15) Uani 1 1 d . . . C11 C 0.6906(4) -0.0902(5) 0.7304(2) 0.0539(15) Uani 1 1 d . . . C12 C 0.6786(4) -0.1302(4) 0.6774(2) 0.0487(14) Uani 1 1 d . . . C13 C 0.7124(3) -0.0682(4) 0.63543(17) 0.0339(11) Uani 1 1 d . . . C14 C 0.6987(3) -0.1139(4) 0.57792(17) 0.0493(14) Uani 1 1 d . . . H14A H 0.6337 -0.1406 0.5683 0.074 Uiso 1 1 calc R . . H14B H 0.7412 -0.1816 0.5747 0.074 Uiso 1 1 calc R . . H14C H 0.7123 -0.0492 0.5535 0.074 Uiso 1 1 calc R . . N21 N 0.9105(3) -0.0895(3) 0.33813(15) 0.0373(11) Uani 1 1 d . . . O21 O 1.0485(2) 0.2234(2) 0.40349(11) 0.0386(8) Uani 1 1 d . . . O22 O 0.9731(2) 0.0559(2) 0.42147(10) 0.0299(7) Uani 1 1 d . . . Cl2 Cl 0.92646(10) -0.51250(10) 0.25627(5) 0.0534(4) Uani 1 1 d . . . C21 C 1.0076(3) 0.1246(4) 0.38946(17) 0.0288(10) Uani 1 1 d . . . C22 C 1.0033(3) 0.0919(4) 0.33125(15) 0.0276(10) Uani 1 1 d . . . C23 C 1.0477(3) 0.1688(4) 0.29867(17) 0.0335(11) Uani 1 1 d . . . C24 C 1.0489(4) 0.1456(5) 0.24428(19) 0.0390(13) Uani 1 1 d . . . C25 C 1.0041(4) 0.0424(4) 0.22248(18) 0.0375(13) Uani 1 1 d . . . C26 C 0.9607(3) -0.0336(4) 0.25316(17) 0.0310(11) Uani 1 1 d . . . C27 C 0.9573(3) -0.0119(4) 0.30875(16) 0.0275(11) Uani 1 1 d . . . C28 C 0.8626(3) -0.1946(4) 0.31622(15) 0.0291(11) Uani 1 1 d . . . C29 C 0.7663(4) -0.1982(4) 0.30943(17) 0.0341(12) Uani 1 1 d . . . C30 C 0.7197(4) -0.2985(5) 0.2861(2) 0.0416(14) Uani 1 1 d . . . C31 C 0.7683(4) -0.3936(4) 0.26939(17) 0.0354(12) Uani 1 1 d . . . C32 C 0.8648(3) -0.3890(4) 0.27729(16) 0.0324(11) Uani 1 1 d . . . C33 C 0.9155(3) -0.2921(4) 0.30183(16) 0.0305(11) Uani 1 1 d . . . C34 C 1.0200(3) -0.2914(4) 0.3124(2) 0.0503(14) Uani 1 1 d . . . H34A H 1.0427 -0.3726 0.3222 0.075 Uiso 1 1 calc R . . H34B H 1.0407 -0.2360 0.3422 0.075 Uiso 1 1 calc R . . H34C H 1.0454 -0.2651 0.2799 0.075 Uiso 1 1 calc R . . N41 N 1.2597(3) -0.0512(4) 0.56784(17) 0.0371(11) Uani 1 1 d . . . H41N H 1.214(3) -0.039(5) 0.559(2) 0.048 Uiso 1 1 d . . . O41 O 1.1713(2) 0.2968(2) 0.51492(10) 0.0313(7) Uani 1 1 d . . . O42 O 1.1274(2) 0.1079(2) 0.52430(10) 0.0319(7) Uani 1 1 d . . . Cl3 Cl 1.45811(9) -0.43590(10) 0.55908(5) 0.0491(4) Uani 1 1 d . . . C41 C 1.1902(3) 0.1893(4) 0.53172(15) 0.0280(11) Uani 1 1 d . . . C42 C 1.2849(3) 0.1641(4) 0.55933(15) 0.0268(10) Uani 1 1 d . . . C43 C 1.3480(4) 0.2609(4) 0.56773(18) 0.0367(12) Uani 1 1 d . . . C44 C 1.4364(4) 0.2461(5) 0.5938(2) 0.0461(14) Uani 1 1 d . . . C45 C 1.4659(4) 0.1328(5) 0.6132(2) 0.0464(14) Uani 1 1 d . . . C46 C 1.4076(4) 0.0369(4) 0.60482(18) 0.0360(12) Uani 1 1 d . . . C47 C 1.3164(3) 0.0482(4) 0.57707(16) 0.0301(11) Uani 1 1 d . . . C48 C 1.2852(3) -0.1685(4) 0.58667(17) 0.0326(11) Uani 1 1 d . . . C49 C 1.2397(4) -0.2171(4) 0.62752(19) 0.0376(12) Uani 1 1 d . . . C50 C 1.2607(4) -0.3340(4) 0.6461(2) 0.0405(13) Uani 1 1 d . . . C51 C 1.3276(4) -0.4001(4) 0.62447(19) 0.0381(13) Uani 1 1 d . . . C52 C 1.3724(3) -0.3503(4) 0.58463(17) 0.0355(12) Uani 1 1 d . . . C53 C 1.3530(3) -0.2345(4) 0.56407(17) 0.0343(12) Uani 1 1 d . . . C54 C 1.4018(3) -0.1860(4) 0.51903(16) 0.0399(12) Uani 1 1 d . . . H54A H 1.3676 -0.1158 0.5029 0.060 Uiso 1 1 calc R . . H54B H 1.4036 -0.2482 0.4914 0.060 Uiso 1 1 calc R . . H54C H 1.4659 -0.1625 0.5334 0.060 Uiso 1 1 calc R . . O1M O 1.0281(2) 0.4690(3) 0.44139(12) 0.0353(9) Uani 1 1 d . . . C1M C 0.9404(4) 0.4901(4) 0.40762(18) 0.0536(16) Uani 1 1 d . . . H1M1 H 0.9377 0.5739 0.3953 0.080 Uiso 1 1 calc R . . H1M2 H 0.8884 0.4745 0.4283 0.080 Uiso 1 1 calc R . . H1M3 H 0.9353 0.4364 0.3763 0.080 Uiso 1 1 calc R . . H1N H 0.824(3) 0.071(4) 0.5881(17) 0.044(16) Uiso 1 1 d . . . H21N H 0.906(3) -0.076(3) 0.3654(14) 0.018(13) Uiso 1 1 d . . . H1OM H 1.043(4) 0.531(5) 0.453(2) 0.08(2) Uiso 1 1 d . . . H3 H 0.800(2) 0.432(3) 0.5166(13) 0.009(11) Uiso 1 1 d . . . H4 H 0.696(3) 0.545(4) 0.5562(17) 0.061(15) Uiso 1 1 d . . . H5 H 0.642(3) 0.430(3) 0.6264(14) 0.022(12) Uiso 1 1 d . . . H6 H 0.681(2) 0.242(3) 0.6538(13) 0.014(10) Uiso 1 1 d . . . H9 H 0.812(3) 0.146(4) 0.7135(16) 0.045(14) Uiso 1 1 d . . . H10 H 0.754(3) 0.045(4) 0.7763(19) 0.067(17) Uiso 1 1 d . . . H11 H 0.663(3) -0.144(4) 0.7611(19) 0.076(16) Uiso 1 1 d . . . H23 H 1.072(3) 0.247(4) 0.3161(15) 0.040(13) Uiso 1 1 d . . . H24 H 1.070(3) 0.198(4) 0.2245(16) 0.038(14) Uiso 1 1 d . . . H25 H 1.006(2) 0.026(3) 0.1868(14) 0.020(10) Uiso 1 1 d . . . H26 H 0.923(3) -0.094(4) 0.2375(18) 0.059(16) Uiso 1 1 d . . . H29 H 0.739(2) -0.131(3) 0.3233(12) 0.010(10) Uiso 1 1 d . . . H30 H 0.662(3) -0.296(3) 0.2818(14) 0.013(12) Uiso 1 1 d . . . H31 H 0.738(3) -0.461(4) 0.2532(15) 0.039(13) Uiso 1 1 d . . . H43 H 1.324(3) 0.335(4) 0.5573(16) 0.044(14) Uiso 1 1 d . . . H44 H 1.481(3) 0.303(4) 0.5975(18) 0.051(15) Uiso 1 1 d . . . H45 H 1.527(3) 0.118(3) 0.6313(15) 0.030(12) Uiso 1 1 d . . . H46 H 1.424(3) -0.043(4) 0.6181(15) 0.034(12) Uiso 1 1 d . . . H49 H 1.194(3) -0.165(4) 0.6420(16) 0.043(14) Uiso 1 1 d . . . H50 H 1.229(3) -0.364(4) 0.6761(18) 0.065(16) Uiso 1 1 d . . . H51 H 1.337(3) -0.486(4) 0.6351(16) 0.042(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0427(6) 0.0185(5) 0.0210(4) -0.0001(3) 0.0016(4) 0.0010(4) Zn2 0.0437(5) 0.0183(4) 0.0258(3) -0.0019(2) 0.0033(3) -0.0018(3) N1 0.057(3) 0.023(2) 0.035(2) 0.0003(19) 0.018(2) -0.001(2) O1 0.0412(19) 0.0189(16) 0.0274(15) 0.0000(13) 0.0020(14) 0.0010(14) O2 0.041(2) 0.0164(16) 0.0326(16) 0.0018(13) 0.0095(15) -0.0035(14) Cl1 0.1109(14) 0.0493(9) 0.0821(11) 0.0044(8) 0.0198(10) -0.0399(9) C1 0.041(3) 0.018(2) 0.021(2) 0.0000(19) 0.000(2) 0.000(2) C2 0.040(3) 0.017(2) 0.025(2) -0.0054(18) -0.001(2) -0.001(2) C3 0.049(4) 0.023(3) 0.030(3) 0.003(2) 0.000(2) -0.003(2) C4 0.045(3) 0.024(3) 0.044(3) -0.007(2) -0.001(3) 0.006(3) C5 0.041(4) 0.046(3) 0.039(3) -0.013(3) 0.006(3) 0.004(3) C6 0.050(4) 0.032(3) 0.030(3) -0.003(2) 0.004(2) -0.002(2) C7 0.039(3) 0.019(2) 0.029(2) -0.0035(19) -0.002(2) -0.002(2) C8 0.042(3) 0.027(3) 0.033(2) 0.007(2) 0.007(2) 0.000(2) C9 0.045(4) 0.041(3) 0.036(3) -0.008(2) 0.001(2) -0.013(3) C10 0.062(4) 0.064(4) 0.026(3) 0.002(3) 0.009(3) -0.014(3) C11 0.073(4) 0.054(4) 0.037(3) 0.014(3) 0.012(3) -0.010(3) C12 0.064(4) 0.035(3) 0.047(3) 0.010(2) 0.007(3) -0.016(3) C13 0.038(3) 0.031(3) 0.032(2) 0.003(2) 0.004(2) -0.001(2) C14 0.070(4) 0.035(3) 0.043(3) -0.007(2) 0.004(3) -0.013(3) N21 0.062(3) 0.030(2) 0.019(2) -0.0041(19) 0.004(2) -0.015(2) O21 0.061(2) 0.0241(18) 0.0312(16) -0.0043(14) 0.0086(16) -0.0106(16) O22 0.048(2) 0.0209(16) 0.0199(14) -0.0009(13) -0.0004(14) -0.0066(15) Cl2 0.0689(10) 0.0336(7) 0.0573(8) -0.0177(6) 0.0072(7) 0.0041(6) C21 0.033(3) 0.023(3) 0.030(2) 0.001(2) 0.002(2) 0.003(2) C22 0.042(3) 0.018(2) 0.022(2) 0.0002(18) 0.000(2) -0.001(2) C23 0.045(3) 0.025(3) 0.029(2) 0.002(2) 0.003(2) 0.000(2) C24 0.054(4) 0.034(3) 0.029(3) 0.006(2) 0.005(2) -0.005(3) C25 0.057(4) 0.035(3) 0.019(2) -0.002(2) 0.000(2) 0.000(3) C26 0.040(3) 0.030(3) 0.023(2) -0.004(2) 0.000(2) 0.001(2) C27 0.039(3) 0.018(2) 0.024(2) -0.0013(18) 0.001(2) 0.003(2) C28 0.045(3) 0.021(3) 0.020(2) -0.0004(18) 0.001(2) -0.002(2) C29 0.053(4) 0.022(3) 0.027(2) -0.002(2) 0.005(2) 0.006(2) C30 0.039(4) 0.040(3) 0.044(3) 0.005(2) -0.001(3) -0.008(3) C31 0.052(4) 0.024(3) 0.027(2) 0.000(2) -0.005(2) -0.008(3) C32 0.048(3) 0.021(3) 0.026(2) -0.0017(19) -0.002(2) 0.001(2) C33 0.033(3) 0.028(3) 0.028(2) -0.001(2) -0.004(2) -0.005(2) C34 0.053(4) 0.039(3) 0.057(3) -0.007(2) -0.001(3) -0.001(3) N41 0.039(3) 0.022(2) 0.046(2) 0.0067(18) -0.008(2) 0.002(2) O41 0.044(2) 0.0140(16) 0.0346(16) 0.0020(13) 0.0000(15) -0.0010(14) O42 0.040(2) 0.0230(17) 0.0309(16) 0.0008(13) -0.0015(14) -0.0035(15) Cl3 0.0620(9) 0.0316(7) 0.0505(7) -0.0043(6) -0.0033(7) 0.0130(6) C41 0.042(3) 0.021(2) 0.021(2) -0.0021(18) 0.005(2) 0.000(2) C42 0.034(3) 0.023(2) 0.023(2) 0.0008(19) 0.002(2) 0.006(2) C43 0.047(4) 0.019(3) 0.041(3) -0.004(2) -0.005(2) -0.001(2) C44 0.043(4) 0.029(3) 0.061(3) -0.006(3) -0.011(3) -0.012(3) C45 0.052(4) 0.030(3) 0.051(3) -0.002(2) -0.016(3) 0.005(3) C46 0.047(3) 0.023(3) 0.036(3) -0.004(2) -0.005(2) -0.003(3) C47 0.041(3) 0.021(2) 0.028(2) -0.0022(19) 0.002(2) -0.001(2) C48 0.048(3) 0.016(2) 0.030(2) 0.0008(19) -0.011(2) 0.002(2) C49 0.045(3) 0.028(3) 0.038(3) 0.000(2) -0.001(3) 0.000(2) C50 0.050(4) 0.030(3) 0.039(3) 0.010(2) -0.001(3) -0.005(3) C51 0.050(4) 0.020(3) 0.040(3) 0.006(2) -0.009(2) 0.001(2) C52 0.044(3) 0.023(3) 0.035(2) -0.005(2) -0.010(2) 0.005(2) C53 0.052(3) 0.016(2) 0.030(2) 0.001(2) -0.010(2) -0.002(2) C54 0.055(3) 0.031(3) 0.031(2) 0.002(2) -0.006(2) 0.005(2) O1M 0.049(2) 0.0183(18) 0.0361(18) -0.0009(15) -0.0022(16) -0.0021(16) C1M 0.082(4) 0.035(3) 0.038(3) 0.006(2) -0.015(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O22 2.044(2) . ? Zn1 O22 2.044(2) 3_756 ? Zn1 O1 2.110(3) 3_756 ? Zn1 O1 2.110(3) . ? Zn1 O42 2.207(3) 3_756 ? Zn1 O42 2.207(3) . ? Zn2 O21 1.901(3) . ? Zn2 O41 1.913(3) . ? Zn2 O2 1.940(3) . ? Zn2 O1M 2.030(3) . ? N1 C7 1.391(5) . ? N1 C8 1.406(5) . ? N1 H1N 0.80(4) . ? O1 C1 1.251(4) . ? O2 C1 1.277(4) . ? Cl1 C12 1.745(5) . ? C1 C2 1.491(6) . ? C2 C7 1.408(5) . ? C2 C3 1.412(6) . ? C3 C4 1.367(6) . ? C3 H3 0.80(3) . ? C4 C5 1.369(6) . ? C4 H4 1.03(4) . ? C5 C6 1.382(6) . ? C5 H5 0.83(4) . ? C6 C7 1.403(6) . ? C6 H6 1.01(3) . ? C8 C9 1.386(6) . ? C8 C13 1.401(6) . ? C9 C10 1.375(6) . ? C9 H9 0.95(4) . ? C10 C11 1.359(7) . ? C10 H10 0.91(5) . ? C11 C12 1.384(6) . ? C11 H11 1.09(5) . ? C12 C13 1.397(5) . ? C13 C14 1.512(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N21 C27 1.368(5) . ? N21 C28 1.428(5) . ? N21 H21N 0.71(3) . ? O21 C21 1.273(5) . ? O22 C21 1.255(4) . ? Cl2 C32 1.754(4) . ? C21 C22 1.492(5) . ? C22 C23 1.393(5) . ? C22 C27 1.410(5) . ? C23 C24 1.385(6) . ? C23 H23 1.01(4) . ? C24 C25 1.391(6) . ? C24 H24 0.85(4) . ? C25 C26 1.349(6) . ? C25 H25 0.91(3) . ? C26 C27 1.417(5) . ? C26 H26 0.92(5) . ? C28 C29 1.375(6) . ? C28 C33 1.399(5) . ? C29 C30 1.387(6) . ? C29 H29 0.93(3) . ? C30 C31 1.364(6) . ? C30 H30 0.83(3) . ? C31 C32 1.377(6) . ? C31 H31 0.93(4) . ? C32 C33 1.396(5) . ? C33 C34 1.492(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? N41 C47 1.375(6) . ? N41 C48 1.418(5) . ? N41 H41N 0.68(4) . ? O41 C41 1.284(4) . ? O42 C41 1.275(5) . ? Cl3 C52 1.746(4) . ? C41 C42 1.470(5) . ? C42 C43 1.405(6) . ? C42 C47 1.417(5) . ? C43 C44 1.359(6) . ? C43 H43 0.92(4) . ? C44 C45 1.395(6) . ? C44 H44 0.90(4) . ? C45 C46 1.355(6) . ? C45 H45 0.95(4) . ? C46 C47 1.405(6) . ? C46 H46 0.96(4) . ? C48 C49 1.393(6) . ? C48 C53 1.400(6) . ? C49 C50 1.399(6) . ? C49 H49 0.98(4) . ? C50 C51 1.379(6) . ? C50 H50 0.99(4) . ? C51 C52 1.374(6) . ? C51 H51 1.00(4) . ? C52 C53 1.400(6) . ? C53 C54 1.504(6) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? O1M C1M 1.440(5) . ? O1M H1OM 0.77(5) . ? C1M H1M1 0.9800 . ? C1M H1M2 0.9800 . ? C1M H1M3 0.9800 . ? 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 O22 Zn1 O22 180.000(1) . 3_756 ? O22 Zn1 O1 86.02(10) . 3_756 ? O22 Zn1 O1 93.98(10) 3_756 3_756 ? O22 Zn1 O1 93.98(10) . . ? O22 Zn1 O1 86.02(10) 3_756 . ? O1 Zn1 O1 180.00(12) 3_756 . ? O22 Zn1 O42 81.89(10) . 3_756 ? O22 Zn1 O42 98.11(10) 3_756 3_756 ? O1 Zn1 O42 96.26(10) 3_756 3_756 ? O1 Zn1 O42 83.74(10) . 3_756 ? O22 Zn1 O42 98.11(10) . . ? O22 Zn1 O42 81.89(10) 3_756 . ? O1 Zn1 O42 83.74(10) 3_756 . ? O1 Zn1 O42 96.26(10) . . ? O42 Zn1 O42 180.00(9) 3_756 . ? O21 Zn2 O41 113.85(13) . . ? O21 Zn2 O2 123.01(13) . . ? O41 Zn2 O2 117.06(12) . . ? O21 Zn2 O1M 95.78(13) . . ? O41 Zn2 O1M 108.70(13) . . ? O2 Zn2 O1M 90.95(12) . . ? C7 N1 C8 124.3(4) . . ? C7 N1 H1N 114(3) . . ? C8 N1 H1N 119(3) . . ? C1 O1 Zn1 139.3(3) . . ? C1 O2 Zn2 133.0(3) . . ? O1 C1 O2 124.3(4) . . ? O1 C1 C2 120.5(4) . . ? O2 C1 C2 115.2(4) . . ? C7 C2 C3 117.5(4) . . ? C7 C2 C1 123.7(4) . . ? C3 C2 C1 118.7(4) . . ? C4 C3 C2 123.1(5) . . ? C4 C3 H3 119(3) . . ? C2 C3 H3 118(3) . . ? C3 C4 C5 118.0(5) . . ? C3 C4 H4 120(2) . . ? C5 C4 H4 122(2) . . ? C4 C5 C6 122.1(5) . . ? C4 C5 H5 124(3) . . ? C6 C5 H5 114(3) . . ? C5 C6 C7 120.0(5) . . ? C5 C6 H6 121(2) . . ? C7 C6 H6 119(2) . . ? N1 C7 C6 120.6(4) . . ? N1 C7 C2 120.2(4) . . ? C6 C7 C2 119.2(4) . . ? C9 C8 C13 120.8(4) . . ? C9 C8 N1 119.4(4) . . ? C13 C8 N1 119.8(4) . . ? C10 C9 C8 120.6(5) . . ? C10 C9 H9 118(3) . . ? C8 C9 H9 121(3) . . ? C11 C10 C9 120.4(5) . . ? C11 C10 H10 126(3) . . ? C9 C10 H10 113(3) . . ? C10 C11 C12 118.9(5) . . ? C10 C11 H11 122(3) . . ? C12 C11 H11 119(3) . . ? C11 C12 C13 123.2(5) . . ? C11 C12 Cl1 117.6(4) . . ? C13 C12 Cl1 119.2(4) . . ? C12 C13 C8 116.0(4) . . ? C12 C13 C14 122.3(4) . . ? C8 C13 C14 121.7(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C27 N21 C28 123.9(4) . . ? C27 N21 H21N 119(3) . . ? C28 N21 H21N 116(3) . . ? C21 O21 Zn2 126.1(3) . . ? C21 O22 Zn1 139.2(3) . . ? O22 C21 O21 123.9(4) . . ? O22 C21 C22 120.3(4) . . ? O21 C21 C22 115.8(4) . . ? C23 C22 C27 119.8(4) . . ? C23 C22 C21 117.3(4) . . ? C27 C22 C21 122.9(4) . . ? C24 C23 C22 121.7(5) . . ? C24 C23 H23 122(2) . . ? C22 C23 H23 115(2) . . ? C23 C24 C25 118.1(5) . . ? C23 C24 H24 120(3) . . ? C25 C24 H24 122(3) . . ? C26 C25 C24 121.3(4) . . ? C26 C25 H25 120(2) . . ? C24 C25 H25 119(2) . . ? C25 C26 C27 122.0(5) . . ? C25 C26 H26 121(3) . . ? C27 C26 H26 116(3) . . ? N21 C27 C22 122.8(4) . . ? N21 C27 C26 120.2(4) . . ? C22 C27 C26 117.0(4) . . ? C29 C28 C33 121.4(4) . . ? C29 C28 N21 119.8(4) . . ? C33 C28 N21 118.8(4) . . ? C28 C29 C30 119.8(5) . . ? C28 C29 H29 113(2) . . ? C30 C29 H29 127(2) . . ? C31 C30 C29 120.9(5) . . ? C31 C30 H30 122(3) . . ? C29 C30 H30 117(3) . . ? C30 C31 C32 118.4(5) . . ? C30 C31 H31 122(3) . . ? C32 C31 H31 119(3) . . ? C31 C32 C33 123.4(4) . . ? C31 C32 Cl2 118.0(3) . . ? C33 C32 Cl2 118.7(4) . . ? C32 C33 C28 116.1(4) . . ? C32 C33 C34 122.5(4) . . ? C28 C33 C34 121.4(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C47 N41 C48 124.3(4) . . ? C47 N41 H41N 115(5) . . ? C48 N41 H41N 119(5) . . ? C41 O41 Zn2 109.9(3) . . ? C41 O42 Zn1 166.5(3) . . ? O42 C41 O41 119.9(4) . . ? O42 C41 C42 121.9(4) . . ? O41 C41 C42 118.2(4) . . ? C43 C42 C47 118.5(4) . . ? C43 C42 C41 117.6(4) . . ? C47 C42 C41 123.9(4) . . ? C44 C43 C42 121.5(5) . . ? C44 C43 H43 122(3) . . ? C42 C43 H43 116(3) . . ? C43 C44 C45 119.8(5) . . ? C43 C44 H44 125(3) . . ? C45 C44 H44 115(3) . . ? C46 C45 C44 120.2(5) . . ? C46 C45 H45 117(2) . . ? C44 C45 H45 123(2) . . ? C45 C46 C47 121.6(5) . . ? C45 C46 H46 124(2) . . ? C47 C46 H46 115(2) . . ? N41 C47 C46 120.3(4) . . ? N41 C47 C42 121.4(4) . . ? C46 C47 C42 118.3(4) . . ? C49 C48 C53 121.0(4) . . ? C49 C48 N41 118.3(4) . . ? C53 C48 N41 120.7(4) . . ? C48 C49 C50 120.1(5) . . ? C48 C49 H49 117(2) . . ? C50 C49 H49 123(2) . . ? C51 C50 C49 119.8(5) . . ? C51 C50 H50 123(3) . . ? C49 C50 H50 117(3) . . ? C52 C51 C50 119.3(5) . . ? C52 C51 H51 121(2) . . ? C50 C51 H51 119(3) . . ? C51 C52 C53 123.1(4) . . ? C51 C52 Cl3 118.0(4) . . ? C53 C52 Cl3 118.9(4) . . ? C48 C53 C52 116.7(4) . . ? C48 C53 C54 122.4(4) . . ? C52 C53 C54 120.9(4) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C1M O1M Zn2 117.1(3) . . ? C1M O1M H1OM 105(4) . . ? Zn2 O1M H1OM 132(4) . . ? O1M C1M H1M1 109.5 . . ? O1M C1M H1M2 109.5 . . ? H1M1 C1M H1M2 109.5 . . ? O1M C1M H1M3 109.5 . . ? H1M1 C1M H1M3 109.5 . . ? H1M2 C1M H1M3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 65.00 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.755 _refine_diff_density_min -1.273 _refine_diff_density_rms 0.099