# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Qin-Yu Zhu' _publ_contact_author_address ; Suzhou 215123 ; _publ_contact_author_email zhuqinyu@suda.edu.cn loop_ _publ_author_name Q.-Y.Zhu L.Yu Yu.Qin L.-B.Huo M.-Y.Shao J.Dai data_l _database_code_depnum_ccdc_archive 'CCDC 778140' #TrackingRef '- Zhu-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.5 H35 Cl2 N6 O8 S8 Zn' _chemical_formula_weight 1066.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_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' _cell_length_a 18.078(6) _cell_length_b 37.848(10) _cell_length_c 15.839(5) _cell_angle_alpha 90.00 _cell_angle_beta 123.460(4) _cell_angle_gamma 90.00 _cell_volume 9042(5) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 11561 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4368 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6126 _exptl_absorpt_correction_T_max 0.7960 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16941 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8260 _reflns_number_gt 6426 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. The restraint DFIX is applied for the bonds O4_H4, C36_O9, C35_O8, N5_O1, N5_O2, and N5_O3. ; _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^)+(0.0014P)^2^+143.1625P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8260 _refine_ls_number_parameters 533 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1216 _refine_ls_R_factor_gt 0.0980 _refine_ls_wR_factor_ref 0.1764 _refine_ls_wR_factor_gt 0.1642 _refine_ls_goodness_of_fit_ref 0.948 _refine_ls_restrained_S_all 0.977 _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 0.36885(6) 0.11518(2) 0.92031(7) 0.0576(3) Uani 1 1 d . . . Cl1 Cl 0.1621(2) 0.15856(7) 0.2953(2) 0.0980(8) Uani 1 1 d . . . Cl2 Cl 0.1114(2) 0.09448(6) 0.1757(2) 0.0973(9) Uani 1 1 d . . . S1 S 0.37544(13) 0.20366(5) 0.50387(16) 0.0586(5) Uani 1 1 d . . . S2 S 0.36975(14) 0.26460(5) 0.61215(16) 0.0566(5) Uani 1 1 d . . . S3 S 0.3571(2) 0.24855(8) 0.3346(2) 0.0897(8) Uani 1 1 d . . . S4 S 0.34236(14) 0.31711(6) 0.45504(18) 0.0672(6) Uani 1 1 d . . . S5 S -0.09369(14) 0.04893(5) 0.55298(16) 0.0582(5) Uani 1 1 d . . . S6 S 0.00671(15) -0.01671(5) 0.62343(17) 0.0648(6) Uani 1 1 d . . . S7 S -0.26323(18) 0.01137(7) 0.3951(2) 0.0940(9) Uani 1 1 d . . . S8 S -0.14505(17) -0.06235(6) 0.47054(18) 0.0700(6) Uani 1 1 d . . . O1 O 0.5037(5) 0.1130(2) 1.0239(7) 0.1330(17) Uani 1 1 d D . . O2 O 0.6364(5) 0.0927(2) 1.0946(7) 0.1330(17) Uani 1 1 d D . . O3 O 0.5261(5) 0.0662(3) 0.9776(7) 0.1330(17) Uani 1 1 d D . . O4 O 0.3487(4) 0.12302(17) 1.0348(5) 0.0697(15) Uani 1 1 d D . . H4 H 0.304(6) 0.134(3) 1.021(11) 0.18(7) Uiso 1 1 d D . . O5 O 0.1174(6) 0.1827(2) -0.0004(8) 0.139(4) Uani 1 1 d . . . O6 O 0.1891(5) 0.13657(19) 0.0078(6) 0.101(2) Uani 1 1 d . . . O7 O 0.2371(6) 0.1872(2) 0.0075(8) 0.135(3) Uani 1 1 d . . . O8 O 0.4968(5) -0.0017(2) 0.1925(6) 0.0305(17) Uiso 0.50 1 d PD . . O9 O 0.3455(12) 0.2496(5) 0.1123(14) 0.134(6) Uiso 0.50 1 d PD . . N1 N 0.3792(4) 0.11285(16) 0.7893(5) 0.0544(15) Uani 1 1 d . . . N2 N 0.3850(4) 0.17339(16) 0.9048(5) 0.0556(16) Uani 1 1 d . . . N3 N 0.2210(4) 0.12594(15) 0.8142(5) 0.0502(15) Uani 1 1 d . . . N4 N 0.3188(4) 0.05987(15) 0.8901(5) 0.0546(16) Uani 1 1 d . . . N5 N 0.5574(7) 0.0932(3) 1.0476(9) 0.1330(17) Uani 1 1 d D . . N6 N 0.1804(6) 0.1688(2) 0.0064(6) 0.078(2) Uani 1 1 d . . . C1 C 0.3776(5) 0.08827(19) 0.7280(7) 0.058(2) Uani 1 1 d . . . H1 H 0.3747 0.0644 0.7422 0.070 Uiso 1 1 calc R . . C2 C 0.3799(5) 0.0966(2) 0.6430(7) 0.064(2) Uani 1 1 d . . . H2 H 0.3787 0.0783 0.6022 0.077 Uiso 1 1 calc R . . C3 C 0.3840(5) 0.1312(2) 0.6186(6) 0.0536(18) Uani 1 1 d . . . H3 H 0.3858 0.1370 0.5620 0.064 Uiso 1 1 calc R . . C4 C 0.3853(4) 0.15753(18) 0.6816(6) 0.0514(18) Uani 1 1 d . . . C5 C 0.3827(4) 0.14648(18) 0.7633(6) 0.0468(17) Uani 1 1 d . . . C6 C 0.3864(5) 0.2047(2) 0.9467(6) 0.062(2) Uani 1 1 d . . . H6 H 0.3841 0.2045 1.0046 0.075 Uiso 1 1 calc R . . C7 C 0.3910(6) 0.2372(2) 0.9088(7) 0.066(2) Uani 1 1 d . . . H7 H 0.3953 0.2581 0.9433 0.080 Uiso 1 1 calc R . . C8 C 0.3891(5) 0.2387(2) 0.8190(6) 0.0560(19) Uani 1 1 d . . . H8 H 0.3893 0.2606 0.7909 0.067 Uiso 1 1 calc R . . C9 C 0.3869(4) 0.20705(18) 0.7722(6) 0.0463(16) Uani 1 1 d . . . C10 C 0.3850(4) 0.17618(18) 0.8191(6) 0.0481(17) Uani 1 1 d . . . C11 C 0.3850(4) 0.19700(18) 0.6823(6) 0.0491(17) Uani 1 1 d . . . C12 C 0.3792(4) 0.21891(19) 0.6101(6) 0.0484(17) Uani 1 1 d . . . C13 C 0.3632(5) 0.2449(2) 0.4485(6) 0.0557(19) Uani 1 1 d . . . C14 C 0.3597(5) 0.2733(2) 0.4972(6) 0.0558(19) Uani 1 1 d . . . C15 C 0.3537(10) 0.2044(3) 0.2982(10) 0.131(5) Uani 1 1 d . . . H15A H 0.4113 0.1936 0.3430 0.196 Uiso 1 1 calc R . . H15B H 0.3387 0.2037 0.2292 0.196 Uiso 1 1 calc R . . H15C H 0.3093 0.1916 0.3022 0.196 Uiso 1 1 calc R . . C16 C 0.4530(6) 0.3346(2) 0.5366(8) 0.082(3) Uani 1 1 d . . . H16A H 0.4720 0.3319 0.6067 0.123 Uiso 1 1 calc R . . H16B H 0.4532 0.3595 0.5218 0.123 Uiso 1 1 calc R . . H16C H 0.4933 0.3219 0.5252 0.123 Uiso 1 1 calc R . . C17 C 0.1651(5) 0.15331(19) 0.7701(6) 0.0558(19) Uani 1 1 d . . . H17 H 0.1883 0.1763 0.7877 0.067 Uiso 1 1 calc R . . C18 C 0.0760(5) 0.14934(19) 0.7006(6) 0.058(2) Uani 1 1 d . . . H18 H 0.0401 0.1695 0.6732 0.070 Uiso 1 1 calc R . . C19 C 0.0371(5) 0.1160(2) 0.6697(6) 0.0529(18) Uani 1 1 d . . . H19 H -0.0240 0.1133 0.6213 0.064 Uiso 1 1 calc R . . C20 C 0.0930(5) 0.08652(18) 0.7139(5) 0.0454(16) Uani 1 1 d . . . C21 C 0.1822(5) 0.09397(18) 0.7843(5) 0.0459(16) Uani 1 1 d . . . C22 C 0.3515(5) 0.0268(2) 0.9151(6) 0.061(2) Uani 1 1 d . . . H22 H 0.4128 0.0239 0.9620 0.074 Uiso 1 1 calc R . . C23 C 0.2988(6) -0.0032(2) 0.8750(7) 0.064(2) Uani 1 1 d . . . H23 H 0.3249 -0.0256 0.8964 0.077 Uiso 1 1 calc R . . C24 C 0.2110(6) -0.0006(2) 0.8060(6) 0.060(2) Uani 1 1 d . . . H24 H 0.1763 -0.0211 0.7790 0.073 Uiso 1 1 calc R . . C25 C 0.1714(5) 0.03296(19) 0.7745(6) 0.0507(18) Uani 1 1 d . . . C26 C 0.2314(5) 0.06133(18) 0.8215(6) 0.0493(17) Uani 1 1 d . . . C27 C 0.0829(5) 0.04763(18) 0.7036(5) 0.0475(17) Uani 1 1 d . . . C28 C 0.0081(5) 0.02931(19) 0.6367(6) 0.0505(17) Uani 1 1 d . . . C29 C -0.1509(6) 0.0100(2) 0.4909(6) 0.062(2) Uani 1 1 d . . . C30 C -0.1042(6) -0.0202(2) 0.5234(6) 0.058(2) Uani 1 1 d . . . C31 C -0.2843(8) 0.0560(3) 0.3683(13) 0.158(7) Uani 1 1 d . . . H31A H -0.2532 0.0694 0.4308 0.236 Uiso 1 1 calc R . . H31B H -0.3475 0.0603 0.3332 0.236 Uiso 1 1 calc R . . H31C H -0.2639 0.0633 0.3257 0.236 Uiso 1 1 calc R . . C32 C -0.1607(7) -0.0815(2) 0.5648(8) 0.087(3) Uani 1 1 d . . . H32A H -0.1051 -0.0810 0.6304 0.131 Uiso 1 1 calc R . . H32B H -0.1807 -0.1058 0.5465 0.131 Uiso 1 1 calc R . . H32C H -0.2049 -0.0680 0.5677 0.131 Uiso 1 1 calc R . . C33 C 0.4105(7) 0.1327(3) 1.1352(8) 0.104(4) Uani 1 1 d . . . H33A H 0.4544 0.1142 1.1689 0.155 Uiso 1 1 calc R . . H33B H 0.3804 0.1362 1.1698 0.155 Uiso 1 1 calc R . . H33C H 0.4395 0.1545 1.1368 0.155 Uiso 1 1 calc R . . C34 C 0.1797(7) 0.1310(2) 0.2202(8) 0.084(3) Uani 1 1 d . . . H34A H 0.1704 0.1446 0.1624 0.100 Uiso 1 1 calc R . . H34B H 0.2415 0.1231 0.2596 0.100 Uiso 1 1 calc R . . C35 C 0.5018(9) 0.0376(3) 0.1684(10) 0.047(3) Uiso 0.50 1 d PD . . C36 C 0.4401(13) 0.2562(6) 0.1753(17) 0.102(7) Uiso 0.50 1 d PD . . C37 C 0.5000 0.2295(5) 0.2500 0.120(6) Uiso 1 2 d S . . 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 0.0560(5) 0.0446(5) 0.0725(6) 0.0048(5) 0.0355(5) 0.0000(4) Cl1 0.117(2) 0.0710(16) 0.105(2) -0.0248(15) 0.0602(18) -0.0121(15) Cl2 0.118(2) 0.0554(14) 0.1003(19) -0.0159(13) 0.0486(17) -0.0153(14) S1 0.0577(11) 0.0525(11) 0.0690(13) -0.0035(10) 0.0371(11) -0.0006(9) S2 0.0602(12) 0.0430(10) 0.0712(13) 0.0004(9) 0.0393(11) -0.0013(9) S3 0.117(2) 0.0887(19) 0.0783(17) 0.0036(14) 0.0629(17) 0.0019(17) S4 0.0571(12) 0.0583(13) 0.0791(15) 0.0142(11) 0.0332(11) -0.0001(10) S5 0.0595(12) 0.0492(11) 0.0614(12) -0.0002(9) 0.0305(10) 0.0011(9) S6 0.0699(13) 0.0415(10) 0.0716(14) 0.0002(10) 0.0319(11) -0.0032(10) S7 0.0693(15) 0.0765(17) 0.0947(19) -0.0023(15) 0.0191(14) -0.0045(13) S8 0.0876(16) 0.0551(13) 0.0713(14) -0.0126(11) 0.0464(13) -0.0168(12) O1 0.084(3) 0.139(4) 0.145(4) 0.024(3) 0.044(3) 0.035(3) O2 0.084(3) 0.139(4) 0.145(4) 0.024(3) 0.044(3) 0.035(3) O3 0.084(3) 0.139(4) 0.145(4) 0.024(3) 0.044(3) 0.035(3) O4 0.064(4) 0.074(4) 0.064(4) 0.002(3) 0.031(3) 0.003(3) O5 0.113(6) 0.094(6) 0.239(11) -0.037(7) 0.115(8) -0.002(5) O6 0.107(6) 0.062(4) 0.133(6) 0.002(4) 0.065(5) -0.001(4) O7 0.123(7) 0.109(6) 0.208(10) -0.012(6) 0.114(7) -0.032(6) N1 0.051(4) 0.040(3) 0.075(4) -0.004(3) 0.037(3) -0.002(3) N2 0.053(4) 0.046(4) 0.073(4) -0.001(3) 0.037(3) -0.004(3) N3 0.055(4) 0.037(3) 0.059(4) 0.001(3) 0.032(3) -0.004(3) N4 0.059(4) 0.042(3) 0.069(4) 0.009(3) 0.039(4) 0.007(3) N5 0.084(3) 0.139(4) 0.145(4) 0.024(3) 0.044(3) 0.035(3) N6 0.072(5) 0.077(6) 0.088(6) -0.013(5) 0.046(5) -0.010(5) C1 0.057(5) 0.032(4) 0.085(6) 0.002(4) 0.038(4) 0.005(3) C2 0.058(5) 0.045(4) 0.087(6) -0.006(4) 0.039(5) 0.004(4) C3 0.051(4) 0.053(4) 0.059(5) -0.004(4) 0.032(4) 0.005(4) C4 0.036(4) 0.040(4) 0.078(5) -0.003(4) 0.031(4) 0.001(3) C5 0.040(4) 0.041(4) 0.062(5) -0.003(3) 0.030(4) -0.001(3) C6 0.065(5) 0.064(5) 0.067(5) -0.009(4) 0.043(5) -0.007(4) C7 0.075(6) 0.047(5) 0.087(6) -0.012(4) 0.052(5) -0.003(4) C8 0.058(5) 0.044(4) 0.070(5) 0.000(4) 0.038(4) -0.002(4) C9 0.041(4) 0.039(4) 0.064(5) -0.003(3) 0.032(4) 0.000(3) C10 0.044(4) 0.039(4) 0.065(5) -0.007(3) 0.032(4) -0.001(3) C11 0.039(4) 0.037(4) 0.073(5) -0.002(4) 0.032(4) 0.000(3) C12 0.033(3) 0.047(4) 0.060(4) -0.003(4) 0.023(3) -0.005(3) C13 0.043(4) 0.056(5) 0.065(5) 0.005(4) 0.028(4) -0.003(4) C14 0.044(4) 0.059(5) 0.066(5) -0.002(4) 0.031(4) -0.006(4) C15 0.209(15) 0.111(10) 0.127(10) -0.034(8) 0.127(11) -0.054(10) C16 0.070(6) 0.070(6) 0.103(7) -0.003(5) 0.046(6) -0.019(5) C17 0.063(5) 0.034(4) 0.073(5) 0.001(4) 0.038(4) 0.002(3) C18 0.067(5) 0.037(4) 0.075(5) 0.003(4) 0.042(5) 0.007(4) C19 0.057(4) 0.051(4) 0.052(4) 0.004(4) 0.031(4) 0.007(4) C20 0.053(4) 0.041(4) 0.050(4) 0.007(3) 0.033(4) 0.004(3) C21 0.053(4) 0.042(4) 0.054(4) 0.005(3) 0.037(4) 0.005(3) C22 0.059(5) 0.053(5) 0.077(6) 0.020(4) 0.041(4) 0.019(4) C23 0.068(5) 0.039(4) 0.085(6) 0.009(4) 0.042(5) 0.006(4) C24 0.070(5) 0.040(4) 0.074(5) 0.003(4) 0.041(5) 0.004(4) C25 0.068(5) 0.041(4) 0.058(4) 0.001(3) 0.044(4) -0.001(4) C26 0.059(5) 0.041(4) 0.059(4) 0.004(3) 0.040(4) 0.002(3) C27 0.056(4) 0.040(4) 0.054(4) 0.004(3) 0.035(4) 0.001(3) C28 0.064(5) 0.042(4) 0.052(4) 0.007(3) 0.036(4) 0.004(4) C29 0.065(5) 0.062(5) 0.064(5) -0.009(4) 0.038(4) -0.015(4) C30 0.068(5) 0.049(5) 0.063(5) 0.000(4) 0.039(4) -0.006(4) C31 0.072(7) 0.072(8) 0.242(18) 0.006(9) 0.032(9) 0.013(6) C32 0.117(8) 0.062(6) 0.093(7) -0.006(5) 0.064(7) -0.025(6) C33 0.091(8) 0.120(10) 0.079(7) 0.002(7) 0.033(6) -0.011(7) C34 0.092(7) 0.071(6) 0.089(7) -0.014(5) 0.050(6) -0.008(5) _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 O1 2.057(8) . ? Zn1 O4 2.058(6) . ? Zn1 N1 2.185(6) . ? Zn1 N4 2.225(6) . ? Zn1 N2 2.254(6) . ? Zn1 N3 2.277(6) . ? Cl1 C34 1.738(9) . ? Cl2 C34 1.725(9) . ? S1 C13 1.743(8) . ? S1 C12 1.745(8) . ? S2 C12 1.740(7) . ? S2 C14 1.758(8) . ? S3 C13 1.752(8) . ? S3 C15 1.757(11) . ? S4 C14 1.751(8) . ? S4 C16 1.806(9) . ? S5 C28 1.733(8) . ? S5 C29 1.757(8) . ? S6 C30 1.745(9) . ? S6 C28 1.753(7) . ? S7 C31 1.731(11) . ? S7 C29 1.741(9) . ? S8 C30 1.763(8) . ? S8 C32 1.817(9) . ? O1 N5 1.115(10) . ? O2 N5 1.193(10) . ? O3 N5 1.378(11) . ? O4 C33 1.398(11) . ? O4 H4 0.82(13) . ? O5 N6 1.202(10) . ? O6 N6 1.230(9) . ? O7 N6 1.231(10) . ? O8 C35 1.553(12) . ? O8 O8 1.762(14) 2_655 ? O9 C36 1.449(17) . ? N1 C1 1.334(9) . ? N1 C5 1.350(9) . ? N2 C6 1.351(9) . ? N2 C10 1.361(9) . ? N3 C17 1.343(9) . ? N3 C21 1.347(8) . ? N4 C26 1.337(9) . ? N4 C22 1.345(9) . ? C1 C2 1.406(11) . ? C1 H1 0.9400 . ? C2 C3 1.381(10) . ? C2 H2 0.9400 . ? C3 C4 1.401(10) . ? C3 H3 0.9400 . ? C4 C5 1.385(10) . ? C4 C11 1.494(9) . ? C5 C10 1.416(9) . ? C6 C7 1.391(11) . ? C6 H6 0.9400 . ? C7 C8 1.405(11) . ? C7 H7 0.9400 . ? C8 C9 1.398(10) . ? C8 H8 0.9400 . ? C9 C10 1.395(9) . ? C9 C11 1.456(10) . ? C11 C12 1.369(10) . ? C13 C14 1.344(10) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.369(10) . ? C17 H17 0.9400 . ? C18 C19 1.395(10) . ? C18 H18 0.9400 . ? C19 C20 1.405(9) . ? C19 H19 0.9400 . ? C20 C21 1.394(10) . ? C20 C27 1.481(9) . ? C21 C26 1.444(9) . ? C22 C23 1.391(11) . ? C22 H22 0.9400 . ? C23 C24 1.345(11) . ? C23 H23 0.9400 . ? C24 C25 1.406(10) . ? C24 H24 0.9400 . ? C25 C26 1.412(10) . ? C25 C27 1.466(10) . ? C27 C28 1.361(10) . ? C29 C30 1.343(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C36 C37 1.48(2) . ? C37 C36 1.48(2) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O4 90.6(3) . . ? O1 Zn1 N1 94.1(3) . . ? O4 Zn1 N1 172.5(3) . . ? O1 Zn1 N4 107.2(3) . . ? O4 Zn1 N4 94.4(2) . . ? N1 Zn1 N4 89.7(2) . . ? O1 Zn1 N2 87.6(3) . . ? O4 Zn1 N2 93.0(2) . . ? N1 Zn1 N2 81.5(2) . . ? N4 Zn1 N2 163.3(2) . . ? O1 Zn1 N3 171.5(3) . . ? O4 Zn1 N3 85.3(2) . . ? N1 Zn1 N3 89.2(2) . . ? N4 Zn1 N3 80.6(2) . . ? N2 Zn1 N3 85.1(2) . . ? C13 S1 C12 96.6(4) . . ? C12 S2 C14 97.0(4) . . ? C13 S3 C15 103.5(5) . . ? C14 S4 C16 100.4(4) . . ? C28 S5 C29 96.8(4) . . ? C30 S6 C28 96.7(4) . . ? C31 S7 C29 103.7(5) . . ? C30 S8 C32 100.7(4) . . ? N5 O1 Zn1 136.5(10) . . ? C33 O4 Zn1 128.5(6) . . ? C33 O4 H4 103(10) . . ? Zn1 O4 H4 118(10) . . ? C35 O8 O8 106.0(6) . 2_655 ? C1 N1 C5 114.9(7) . . ? C1 N1 Zn1 137.8(5) . . ? C5 N1 Zn1 107.2(5) . . ? C6 N2 C10 114.3(6) . . ? C6 N2 Zn1 140.5(5) . . ? C10 N2 Zn1 104.8(5) . . ? C17 N3 C21 114.4(6) . . ? C17 N3 Zn1 139.7(5) . . ? C21 N3 Zn1 105.7(4) . . ? C26 N4 C22 114.1(7) . . ? C26 N4 Zn1 107.1(5) . . ? C22 N4 Zn1 138.6(6) . . ? O1 N5 O2 137.8(14) . . ? O1 N5 O3 109.3(11) . . ? O2 N5 O3 108.1(11) . . ? O5 N6 O6 122.8(9) . . ? O5 N6 O7 119.7(10) . . ? O6 N6 O7 117.4(9) . . ? N1 C1 C2 122.8(7) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 121.0(8) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 117.2(7) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.4 . . ? C5 C4 C3 117.1(7) . . ? C5 C4 C11 107.0(6) . . ? C3 C4 C11 135.8(8) . . ? N1 C5 C4 127.0(7) . . ? N1 C5 C10 123.2(7) . . ? C4 C5 C10 109.8(6) . . ? N2 C6 C7 123.6(8) . . ? N2 C6 H6 118.2 . . ? C7 C6 H6 118.2 . . ? C6 C7 C8 119.9(7) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 118.6(7) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C10 C9 C8 116.0(7) . . ? C10 C9 C11 107.9(6) . . ? C8 C9 C11 136.1(7) . . ? N2 C10 C9 127.5(6) . . ? N2 C10 C5 123.0(7) . . ? C9 C10 C5 109.5(7) . . ? C12 C11 C9 127.5(6) . . ? C12 C11 C4 126.7(7) . . ? C9 C11 C4 105.7(6) . . ? C11 C12 S2 123.3(6) . . ? C11 C12 S1 123.4(6) . . ? S2 C12 S1 113.2(4) . . ? C14 C13 S1 117.4(6) . . ? C14 C13 S3 122.1(6) . . ? S1 C13 S3 120.5(5) . . ? C13 C14 S4 126.4(6) . . ? C13 C14 S2 115.7(6) . . ? S4 C14 S2 117.8(5) . . ? S3 C15 H15A 109.5 . . ? S3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? S4 C16 H16A 109.5 . . ? S4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 123.2(7) . . ? N3 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C17 C18 C19 121.5(7) . . ? C17 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C18 C19 C20 117.3(7) . . ? C18 C19 H19 121.3 . . ? C20 C19 H19 121.3 . . ? C21 C20 C19 115.8(7) . . ? C21 C20 C27 107.9(6) . . ? C19 C20 C27 136.3(7) . . ? N3 C21 C20 127.7(7) . . ? N3 C21 C26 122.8(7) . . ? C20 C21 C26 109.5(6) . . ? N4 C22 C23 123.0(8) . . ? N4 C22 H22 118.5 . . ? C23 C22 H22 118.5 . . ? C24 C23 C22 121.0(8) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 119.8(8) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 114.0(7) . . ? C24 C25 C27 137.8(7) . . ? C26 C25 C27 108.2(6) . . ? N4 C26 C25 128.1(7) . . ? N4 C26 C21 123.6(7) . . ? C25 C26 C21 108.3(7) . . ? C28 C27 C25 126.9(7) . . ? C28 C27 C20 126.9(7) . . ? C25 C27 C20 106.0(6) . . ? C27 C28 S5 123.9(6) . . ? C27 C28 S6 122.8(6) . . ? S5 C28 S6 113.3(4) . . ? C30 C29 S7 123.0(6) . . ? C30 C29 S5 116.6(6) . . ? S7 C29 S5 120.4(5) . . ? C29 C30 S6 116.6(6) . . ? C29 C30 S8 125.2(7) . . ? S6 C30 S8 118.1(5) . . ? S7 C31 H31A 109.5 . . ? S7 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S7 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S8 C32 H32A 109.5 . . ? S8 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S8 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O4 C33 H33A 109.5 . . ? O4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Cl2 C34 Cl1 113.6(6) . . ? Cl2 C34 H34A 108.8 . . ? Cl1 C34 H34A 108.8 . . ? Cl2 C34 H34B 108.8 . . ? Cl1 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? O9 C36 C37 120.0(18) . . ? C36 C37 C36 94(2) 2_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Zn1 O1 N5 119.2(14) . . . . ? N1 Zn1 O1 N5 -66.6(14) . . . . ? N4 Zn1 O1 N5 24.4(15) . . . . ? N2 Zn1 O1 N5 -147.9(15) . . . . ? N3 Zn1 O1 N5 -179(100) . . . . ? O1 Zn1 O4 C33 15.2(9) . . . . ? N1 Zn1 O4 C33 -114.1(19) . . . . ? N4 Zn1 O4 C33 122.5(8) . . . . ? N2 Zn1 O4 C33 -72.5(8) . . . . ? N3 Zn1 O4 C33 -157.3(8) . . . . ? O1 Zn1 N1 C1 93.4(8) . . . . ? O4 Zn1 N1 C1 -137.5(17) . . . . ? N4 Zn1 N1 C1 -13.8(8) . . . . ? N2 Zn1 N1 C1 -179.6(8) . . . . ? N3 Zn1 N1 C1 -94.4(8) . . . . ? O1 Zn1 N1 C5 -91.6(5) . . . . ? O4 Zn1 N1 C5 37(2) . . . . ? N4 Zn1 N1 C5 161.2(5) . . . . ? N2 Zn1 N1 C5 -4.6(5) . . . . ? N3 Zn1 N1 C5 80.6(5) . . . . ? O1 Zn1 N2 C6 -88.5(9) . . . . ? O4 Zn1 N2 C6 2.0(9) . . . . ? N1 Zn1 N2 C6 177.0(9) . . . . ? N4 Zn1 N2 C6 118.2(10) . . . . ? N3 Zn1 N2 C6 87.1(8) . . . . ? O1 Zn1 N2 C10 99.4(5) . . . . ? O4 Zn1 N2 C10 -170.1(5) . . . . ? N1 Zn1 N2 C10 4.9(4) . . . . ? N4 Zn1 N2 C10 -53.9(10) . . . . ? N3 Zn1 N2 C10 -85.1(5) . . . . ? O1 Zn1 N3 C17 25(2) . . . . ? O4 Zn1 N3 C17 86.6(8) . . . . ? N1 Zn1 N3 C17 -88.3(8) . . . . ? N4 Zn1 N3 C17 -178.1(8) . . . . ? N2 Zn1 N3 C17 -6.8(8) . . . . ? O1 Zn1 N3 C21 -161(2) . . . . ? O4 Zn1 N3 C21 -99.1(5) . . . . ? N1 Zn1 N3 C21 86.0(5) . . . . ? N4 Zn1 N3 C21 -3.8(4) . . . . ? N2 Zn1 N3 C21 167.5(5) . . . . ? O1 Zn1 N4 C26 -179.0(5) . . . . ? O4 Zn1 N4 C26 89.0(5) . . . . ? N1 Zn1 N4 C26 -84.8(5) . . . . ? N2 Zn1 N4 C26 -27.0(11) . . . . ? N3 Zn1 N4 C26 4.5(5) . . . . ? O1 Zn1 N4 C22 -4.8(9) . . . . ? O4 Zn1 N4 C22 -96.8(8) . . . . ? N1 Zn1 N4 C22 89.4(8) . . . . ? N2 Zn1 N4 C22 147.1(8) . . . . ? N3 Zn1 N4 C22 178.6(8) . . . . ? Zn1 O1 N5 O2 164.7(13) . . . . ? Zn1 O1 N5 O3 13(2) . . . . ? C5 N1 C1 C2 0.4(11) . . . . ? Zn1 N1 C1 C2 175.2(6) . . . . ? N1 C1 C2 C3 -0.1(12) . . . . ? C1 C2 C3 C4 -0.2(11) . . . . ? C2 C3 C4 C5 0.2(10) . . . . ? C2 C3 C4 C11 -176.5(8) . . . . ? C1 N1 C5 C4 -0.5(11) . . . . ? Zn1 N1 C5 C4 -176.8(6) . . . . ? C1 N1 C5 C10 -179.9(7) . . . . ? Zn1 N1 C5 C10 3.8(8) . . . . ? C3 C4 C5 N1 0.2(11) . . . . ? C11 C4 C5 N1 177.7(7) . . . . ? C3 C4 C5 C10 179.7(6) . . . . ? C11 C4 C5 C10 -2.8(8) . . . . ? C10 N2 C6 C7 -2.5(11) . . . . ? Zn1 N2 C6 C7 -174.1(6) . . . . ? N2 C6 C7 C8 3.8(13) . . . . ? C6 C7 C8 C9 -3.0(12) . . . . ? C7 C8 C9 C10 1.2(10) . . . . ? C7 C8 C9 C11 -179.6(8) . . . . ? C6 N2 C10 C9 0.5(11) . . . . ? Zn1 N2 C10 C9 175.0(6) . . . . ? C6 N2 C10 C5 -179.3(7) . . . . ? Zn1 N2 C10 C5 -4.8(8) . . . . ? C8 C9 C10 N2 0.0(11) . . . . ? C11 C9 C10 N2 -179.4(7) . . . . ? C8 C9 C10 C5 179.9(6) . . . . ? C11 C9 C10 C5 0.4(8) . . . . ? N1 C5 C10 N2 0.9(11) . . . . ? C4 C5 C10 N2 -178.6(6) . . . . ? N1 C5 C10 C9 -179.0(6) . . . . ? C4 C5 C10 C9 1.5(8) . . . . ? C10 C9 C11 C12 174.6(7) . . . . ? C8 C9 C11 C12 -4.6(13) . . . . ? C10 C9 C11 C4 -2.1(7) . . . . ? C8 C9 C11 C4 178.7(8) . . . . ? C5 C4 C11 C12 -173.8(7) . . . . ? C3 C4 C11 C12 3.1(13) . . . . ? C5 C4 C11 C9 3.0(7) . . . . ? C3 C4 C11 C9 179.9(8) . . . . ? C9 C11 C12 S2 -1.7(10) . . . . ? C4 C11 C12 S2 174.3(5) . . . . ? C9 C11 C12 S1 -178.8(5) . . . . ? C4 C11 C12 S1 -2.8(10) . . . . ? C14 S2 C12 C11 -176.9(6) . . . . ? C14 S2 C12 S1 0.4(4) . . . . ? C13 S1 C12 C11 177.3(6) . . . . ? C13 S1 C12 S2 0.0(4) . . . . ? C12 S1 C13 C14 -0.5(6) . . . . ? C12 S1 C13 S3 178.7(4) . . . . ? C15 S3 C13 C14 -174.5(8) . . . . ? C15 S3 C13 S1 6.3(7) . . . . ? S1 C13 C14 S4 -176.7(4) . . . . ? S3 C13 C14 S4 4.1(10) . . . . ? S1 C13 C14 S2 0.9(8) . . . . ? S3 C13 C14 S2 -178.4(4) . . . . ? C16 S4 C14 C13 -105.7(8) . . . . ? C16 S4 C14 S2 76.8(5) . . . . ? C12 S2 C14 C13 -0.8(6) . . . . ? C12 S2 C14 S4 177.0(4) . . . . ? C21 N3 C17 C18 0.3(11) . . . . ? Zn1 N3 C17 C18 174.2(6) . . . . ? N3 C17 C18 C19 -1.0(12) . . . . ? C17 C18 C19 C20 0.9(11) . . . . ? C18 C19 C20 C21 -0.3(10) . . . . ? C18 C19 C20 C27 -178.1(8) . . . . ? C17 N3 C21 C20 0.4(10) . . . . ? Zn1 N3 C21 C20 -175.5(6) . . . . ? C17 N3 C21 C26 178.8(7) . . . . ? Zn1 N3 C21 C26 2.8(8) . . . . ? C19 C20 C21 N3 -0.4(11) . . . . ? C27 C20 C21 N3 178.0(7) . . . . ? C19 C20 C21 C26 -179.0(6) . . . . ? C27 C20 C21 C26 -0.5(8) . . . . ? C26 N4 C22 C23 -1.3(11) . . . . ? Zn1 N4 C22 C23 -175.2(6) . . . . ? N4 C22 C23 C24 1.5(13) . . . . ? C22 C23 C24 C25 -0.6(13) . . . . ? C23 C24 C25 C26 -0.2(11) . . . . ? C23 C24 C25 C27 178.9(8) . . . . ? C22 N4 C26 C25 0.4(11) . . . . ? Zn1 N4 C26 C25 176.2(6) . . . . ? C22 N4 C26 C21 179.5(7) . . . . ? Zn1 N4 C26 C21 -4.8(8) . . . . ? C24 C25 C26 N4 0.3(11) . . . . ? C27 C25 C26 N4 -179.0(7) . . . . ? C24 C25 C26 C21 -178.8(6) . . . . ? C27 C25 C26 C21 1.8(8) . . . . ? N3 C21 C26 N4 1.4(11) . . . . ? C20 C21 C26 N4 180.0(7) . . . . ? N3 C21 C26 C25 -179.4(6) . . . . ? C20 C21 C26 C25 -0.8(8) . . . . ? C24 C25 C27 C28 -5.6(14) . . . . ? C26 C25 C27 C28 173.6(7) . . . . ? C24 C25 C27 C20 178.8(9) . . . . ? C26 C25 C27 C20 -2.0(8) . . . . ? C21 C20 C27 C28 -174.1(7) . . . . ? C19 C20 C27 C28 3.9(13) . . . . ? C21 C20 C27 C25 1.5(7) . . . . ? C19 C20 C27 C25 179.5(8) . . . . ? C25 C27 C28 S5 -178.3(6) . . . . ? C20 C27 C28 S5 -3.5(11) . . . . ? C25 C27 C28 S6 -0.9(11) . . . . ? C20 C27 C28 S6 173.8(5) . . . . ? C29 S5 C28 C27 176.6(7) . . . . ? C29 S5 C28 S6 -1.0(5) . . . . ? C30 S6 C28 C27 -176.4(6) . . . . ? C30 S6 C28 S5 1.2(5) . . . . ? C31 S7 C29 C30 -169.6(9) . . . . ? C31 S7 C29 S5 12.4(8) . . . . ? C28 S5 C29 C30 0.3(7) . . . . ? C28 S5 C29 S7 178.5(5) . . . . ? S7 C29 C30 S6 -177.6(4) . . . . ? S5 C29 C30 S6 0.5(9) . . . . ? S7 C29 C30 S8 4.6(11) . . . . ? S5 C29 C30 S8 -177.4(4) . . . . ? C28 S6 C30 C29 -1.0(7) . . . . ? C28 S6 C30 S8 177.0(5) . . . . ? C32 S8 C30 C29 -104.3(8) . . . . ? C32 S8 C30 S6 77.9(6) . . . . ? O9 C36 C37 C36 -145(2) . . . 2_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 N6 0.82(13) 2.49(14) 3.312(11) 171(14) 1_556 O4 H4 O7 0.82(13) 2.30(8) 3.031(11) 148(14) 1_556 O4 H4 O6 0.82(13) 1.97(7) 2.722(10) 152(14) 1_556 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.534 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.088 ########End data_2 _database_code_depnum_ccdc_archive 'CCDC 778141' #TrackingRef '- Zhu-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H29 N4 O2 S8 Zn, N O3, C H4 O' _chemical_formula_sum 'C40 H33 N5 O6 S8 Zn' _chemical_formula_weight 1001.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' '-x, -y, z+1/2' _cell_length_a 16.6110(16) _cell_length_b 15.9977(15) _cell_length_c 15.7389(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4182.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14104 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.3 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 1.041 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 0.771 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39489 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7637 _reflns_number_gt 6777 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. The restraint DFIX is applied for the bonds C40_O6 and C40'_O6'. ; _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^)+(0.0503P)^2^+6.0659P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.506(16) _refine_ls_number_reflns 7637 _refine_ls_number_parameters 544 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _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 1.03496(4) 0.48417(4) 0.60567(5) 0.03890(18) Uani 1 1 d . . . S1 S 0.82552(9) 0.26300(10) 0.25916(10) 0.0388(4) Uani 1 1 d . . . S2 S 0.89112(9) 0.11846(9) 0.34741(11) 0.0423(4) Uani 1 1 d . . . S3 S 0.74546(11) 0.15750(11) 0.12312(11) 0.0505(4) Uani 1 1 d . . . S4 S 0.82409(12) -0.00261(11) 0.21510(12) 0.0527(4) Uani 1 1 d . . . S5 S 0.81268(9) 0.71006(9) 0.94354(9) 0.0367(3) Uani 1 1 d . . . S6 S 0.86890(9) 0.84952(9) 0.84039(10) 0.0381(3) Uani 1 1 d . . . S7 S 0.73399(10) 0.82379(10) 1.07383(11) 0.0464(4) Uani 1 1 d . . . S8 S 0.79199(10) 0.97960(9) 0.95160(12) 0.0448(4) Uani 1 1 d . . . O1 O 1.1423(3) 0.4743(3) 0.6698(3) 0.0549(12) Uani 1 1 d . . . O2 O 1.1582(3) 0.5178(4) 0.5394(3) 0.0753(17) Uani 1 1 d . . . O3 O 0.4024(5) 0.7115(7) 0.4338(6) 0.155(4) Uani 1 1 d . . . O4 O 0.5087(5) 0.6602(5) 0.3953(6) 0.138(3) Uani 1 1 d . . . O5 O 0.4701(9) 0.7748(6) 0.3487(7) 0.203(6) Uani 1 1 d . . . N1 N 0.9675(3) 0.4802(3) 0.4933(3) 0.0339(12) Uani 1 1 d . . . N2 N 1.0239(3) 0.3418(3) 0.5917(3) 0.0384(12) Uani 1 1 d . . . N3 N 0.9553(3) 0.4857(3) 0.7106(3) 0.0337(11) Uani 1 1 d . . . N4 N 1.0189(3) 0.6244(3) 0.6151(4) 0.0379(11) Uani 1 1 d . . . N5 N 0.4641(5) 0.7165(5) 0.3896(5) 0.0678(18) Uani 1 1 d . . . C1 C 0.9375(4) 0.5384(4) 0.4400(4) 0.0394(14) Uani 1 1 d . . . H1 H 0.9447 0.5953 0.4530 0.047 Uiso 1 1 calc R . . C2 C 0.8964(4) 0.5167(4) 0.3664(4) 0.0384(14) Uani 1 1 d . . . H2 H 0.8768 0.5587 0.3301 0.046 Uiso 1 1 calc R . . C3 C 0.8839(3) 0.4331(4) 0.3459(4) 0.0392(14) Uani 1 1 d . . . H3 H 0.8562 0.4184 0.2961 0.047 Uiso 1 1 calc R . . C4 C 0.9128(3) 0.3723(4) 0.3997(4) 0.0336(13) Uani 1 1 d . . . C5 C 0.9540(3) 0.4015(4) 0.4714(4) 0.0352(13) Uani 1 1 d . . . C6 C 1.0464(4) 0.2700(4) 0.6290(4) 0.0433(16) Uani 1 1 d . . . H6B H 1.0764 0.2730 0.6796 0.052 Uiso 1 1 calc R . . C7 C 1.0280(4) 0.1922(4) 0.5971(4) 0.0423(15) Uani 1 1 d . . . H7 H 1.0440 0.1438 0.6264 0.051 Uiso 1 1 calc R . . C8 C 0.9849(4) 0.1855(4) 0.5201(4) 0.0434(15) Uani 1 1 d . . . H8 H 0.9728 0.1328 0.4968 0.052 Uiso 1 1 calc R . . C9 C 0.9611(3) 0.2574(4) 0.4801(4) 0.0338(13) Uani 1 1 d . . . C10 C 0.9824(3) 0.3331(4) 0.5208(4) 0.0350(13) Uani 1 1 d . . . C11 C 0.9154(3) 0.2791(4) 0.4026(4) 0.0360(14) Uani 1 1 d . . . C12 C 0.8827(3) 0.2271(3) 0.3444(4) 0.0335(13) Uani 1 1 d . . . C13 C 0.8037(3) 0.1652(4) 0.2160(4) 0.0401(14) Uani 1 1 d . . . C14 C 0.8329(3) 0.0984(4) 0.2555(4) 0.0385(14) Uani 1 1 d . . . C15 C 0.7238(4) 0.2649(4) 0.0997(5) 0.0557(18) Uani 1 1 d . . . H15A H 0.6965 0.2902 0.1478 0.084 Uiso 1 1 calc R . . H15B H 0.6895 0.2681 0.0499 0.084 Uiso 1 1 calc R . . H15C H 0.7736 0.2946 0.0888 0.084 Uiso 1 1 calc R . . C16 C 0.8360(5) -0.0676(5) 0.3042(5) 0.073(2) Uani 1 1 d . . . H16A H 0.8903 -0.0618 0.3262 0.110 Uiso 1 1 calc R . . H16B H 0.8266 -0.1252 0.2879 0.110 Uiso 1 1 calc R . . H16C H 0.7977 -0.0515 0.3478 0.110 Uiso 1 1 calc R . . C17 C 0.9234(4) 0.4287(4) 0.7627(4) 0.0422(15) Uani 1 1 d . . . H17 H 0.9310 0.3717 0.7507 0.051 Uiso 1 1 calc R . . C18 C 0.8793(4) 0.4511(4) 0.8341(4) 0.0425(15) Uani 1 1 d . . . H18 H 0.8574 0.4089 0.8686 0.051 Uiso 1 1 calc R . . C19 C 0.8667(4) 0.5349(4) 0.8561(4) 0.0394(14) Uani 1 1 d . . . H19 H 0.8380 0.5499 0.9053 0.047 Uiso 1 1 calc R . . C20 C 0.8990(3) 0.5954(3) 0.8015(4) 0.0318(12) Uani 1 1 d . . . C21 C 0.9420(3) 0.5647(4) 0.7317(4) 0.0336(13) Uani 1 1 d . . . C22 C 1.0425(4) 0.6958(4) 0.5780(4) 0.0399(14) Uani 1 1 d . . . H22 H 1.0747 0.6933 0.5290 0.048 Uiso 1 1 calc R . . C23 C 1.0207(3) 0.7729(4) 0.6098(4) 0.0399(14) Uani 1 1 d . . . H23 H 1.0378 0.8212 0.5811 0.048 Uiso 1 1 calc R . . C24 C 0.9747(3) 0.7816(4) 0.6823(4) 0.0373(14) Uani 1 1 d . . . H24 H 0.9612 0.8347 0.7035 0.045 Uiso 1 1 calc R . . C25 C 0.9490(3) 0.7088(3) 0.7230(4) 0.0331(13) Uani 1 1 d . . . C26 C 0.9736(3) 0.6344(3) 0.6856(4) 0.0337(13) Uani 1 1 d . . . C27 C 0.9009(3) 0.6868(3) 0.7992(4) 0.0325(13) Uani 1 1 d . . . C28 C 0.8661(3) 0.7413(3) 0.8535(4) 0.0311(12) Uani 1 1 d . . . C29 C 0.7882(3) 0.8107(4) 0.9799(4) 0.0373(14) Uani 1 1 d . . . C30 C 0.8134(3) 0.8751(3) 0.9311(4) 0.0362(14) Uani 1 1 d . . . C31 C 0.7204(4) 0.7182(4) 1.1095(5) 0.0545(17) Uani 1 1 d . . . H31A H 0.6947 0.6858 1.0651 0.082 Uiso 1 1 calc R . . H31B H 0.6868 0.7179 1.1599 0.082 Uiso 1 1 calc R . . H31C H 0.7724 0.6939 1.1229 0.082 Uiso 1 1 calc R . . C32 C 0.8903(4) 1.0157(4) 0.9828(5) 0.0570(19) Uani 1 1 d . . . H32A H 0.9059 0.9888 1.0355 0.085 Uiso 1 1 calc R . . H32B H 0.8889 1.0758 0.9909 0.085 Uiso 1 1 calc R . . H32C H 0.9290 1.0020 0.9388 0.085 Uiso 1 1 calc R . . C33 C 1.1870(4) 0.4972(4) 0.6094(5) 0.0458(15) Uani 1 1 d . . . C34 C 1.2762(4) 0.5010(4) 0.6232(4) 0.0383(15) Uani 1 1 d . . . C35 C 1.3082(4) 0.4708(4) 0.6977(4) 0.0466(16) Uani 1 1 d . . . H35 H 1.2745 0.4494 0.7405 0.056 Uiso 1 1 calc R . . C36 C 1.3926(5) 0.4724(4) 0.7087(5) 0.060(2) Uani 1 1 d . . . H36 H 1.4158 0.4517 0.7589 0.072 Uiso 1 1 calc R . . C37 C 1.4398(4) 0.5040(4) 0.6462(5) 0.056(2) Uani 1 1 d . . . H37 H 1.4959 0.5050 0.6539 0.067 Uiso 1 1 calc R . . C38 C 1.4078(4) 0.5344(4) 0.5722(6) 0.061(2) Uani 1 1 d . . . H38 H 1.4414 0.5568 0.5299 0.073 Uiso 1 1 calc R . . C39 C 1.3259(4) 0.5316(4) 0.5608(5) 0.0495(17) Uani 1 1 d . . . H39 H 1.3035 0.5510 0.5096 0.059 Uiso 1 1 calc R . . O6 O 0.256(4) 0.778(4) 0.344(4) 0.14(2) Uiso 0.15 1 d PD . . O6' O 0.1532(6) 0.7592(6) 0.3111(6) 0.125(3) Uiso 0.85 1 d PD . . C40 C 0.193(3) 0.748(4) 0.402(4) 0.079(17) Uiso 0.15 1 d PD . . C40' C 0.2130(9) 0.7859(8) 0.3711(9) 0.093(4) Uiso 0.85 1 d PD . . 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 0.0390(4) 0.0408(3) 0.0369(3) -0.0058(3) -0.0012(4) -0.0002(3) S1 0.0419(8) 0.0342(8) 0.0402(8) -0.0033(7) -0.0020(7) -0.0006(6) S2 0.0473(8) 0.0333(8) 0.0461(9) -0.0024(7) -0.0060(8) -0.0007(7) S3 0.0556(10) 0.0489(10) 0.0470(10) -0.0101(8) -0.0117(8) 0.0023(8) S4 0.0659(11) 0.0386(9) 0.0537(10) -0.0091(8) -0.0001(9) -0.0041(8) S5 0.0426(8) 0.0304(7) 0.0372(8) -0.0005(6) 0.0021(7) 0.0002(6) S6 0.0430(8) 0.0280(7) 0.0433(8) -0.0007(7) 0.0029(8) -0.0010(6) S7 0.0517(10) 0.0430(9) 0.0445(9) -0.0052(7) 0.0066(8) 0.0019(7) S8 0.0445(9) 0.0309(8) 0.0591(10) -0.0078(8) -0.0079(8) 0.0038(7) O1 0.039(2) 0.057(3) 0.069(3) -0.010(3) 0.007(2) -0.005(2) O2 0.057(3) 0.118(5) 0.051(3) -0.028(3) -0.012(3) 0.024(3) O3 0.114(6) 0.247(12) 0.104(6) -0.022(7) 0.028(6) -0.007(7) O4 0.122(6) 0.122(7) 0.169(9) 0.001(6) -0.002(6) 0.057(5) O5 0.379(19) 0.091(6) 0.139(8) 0.031(6) 0.087(10) 0.000(8) N1 0.035(3) 0.029(3) 0.038(3) 0.001(2) 0.005(2) -0.005(2) N2 0.036(3) 0.041(3) 0.038(3) -0.003(2) -0.002(2) 0.002(2) N3 0.037(3) 0.031(3) 0.033(3) -0.004(2) -0.006(2) 0.000(2) N4 0.039(3) 0.036(3) 0.039(3) -0.004(2) 0.002(3) -0.001(2) N5 0.082(5) 0.058(4) 0.063(4) -0.003(4) 0.003(4) -0.007(4) C1 0.043(3) 0.030(3) 0.046(4) -0.008(3) 0.007(3) 0.000(3) C2 0.046(4) 0.032(3) 0.038(3) 0.004(3) -0.001(3) -0.002(3) C3 0.037(3) 0.043(3) 0.038(3) 0.001(3) 0.002(3) 0.000(3) C4 0.032(3) 0.034(3) 0.034(3) 0.003(3) 0.002(3) 0.002(2) C5 0.026(3) 0.038(3) 0.041(3) 0.000(3) 0.009(3) 0.002(2) C6 0.048(4) 0.048(4) 0.034(4) 0.003(3) -0.002(3) 0.008(3) C7 0.053(4) 0.033(3) 0.041(4) 0.002(3) -0.007(3) 0.001(3) C8 0.046(4) 0.037(3) 0.048(4) 0.002(3) 0.000(3) -0.002(3) C9 0.029(3) 0.038(3) 0.034(3) -0.003(3) 0.004(3) 0.001(2) C10 0.030(3) 0.036(3) 0.038(3) -0.006(3) 0.008(3) -0.001(2) C11 0.035(3) 0.036(3) 0.037(3) -0.001(3) 0.006(3) -0.002(3) C12 0.032(3) 0.034(3) 0.035(3) -0.003(3) 0.006(3) -0.001(2) C13 0.035(3) 0.040(3) 0.045(4) -0.009(3) -0.001(3) -0.004(3) C14 0.036(3) 0.037(3) 0.043(3) -0.001(3) 0.001(3) -0.001(3) C15 0.048(4) 0.060(4) 0.059(4) 0.008(4) 0.006(4) 0.008(3) C16 0.100(6) 0.039(4) 0.081(6) -0.003(4) -0.014(5) 0.004(4) C17 0.048(4) 0.035(3) 0.044(4) 0.004(3) 0.001(3) 0.001(3) C18 0.051(4) 0.034(3) 0.042(4) 0.008(3) -0.002(3) -0.001(3) C19 0.045(4) 0.034(3) 0.039(3) 0.002(3) 0.003(3) 0.004(3) C20 0.030(3) 0.030(3) 0.035(3) 0.000(3) -0.006(3) 0.001(2) C21 0.033(3) 0.034(3) 0.034(3) 0.003(3) -0.005(3) 0.001(2) C22 0.041(3) 0.037(3) 0.042(3) 0.000(3) 0.003(3) -0.009(3) C23 0.038(3) 0.039(3) 0.043(3) 0.009(3) -0.004(3) -0.010(2) C24 0.038(3) 0.032(3) 0.042(3) 0.006(3) -0.001(3) -0.001(3) C25 0.028(3) 0.030(3) 0.040(3) -0.003(3) -0.010(3) 0.000(2) C26 0.035(3) 0.032(3) 0.034(3) 0.001(2) -0.009(3) -0.004(2) C27 0.034(3) 0.028(3) 0.035(3) 0.001(2) -0.004(3) 0.004(2) C28 0.032(3) 0.029(3) 0.032(3) -0.001(3) -0.005(3) 0.001(2) C29 0.035(3) 0.036(3) 0.041(3) -0.006(3) -0.005(3) 0.002(3) C30 0.036(3) 0.030(3) 0.042(4) -0.006(3) -0.003(3) 0.007(2) C31 0.058(4) 0.057(4) 0.048(4) 0.004(4) 0.012(4) 0.006(3) C32 0.052(4) 0.045(4) 0.075(5) -0.016(4) -0.012(4) -0.001(3) C33 0.040(3) 0.051(4) 0.047(4) -0.027(3) -0.002(4) 0.001(3) C34 0.040(3) 0.035(3) 0.041(4) -0.008(3) 0.007(3) -0.002(2) C35 0.048(4) 0.042(4) 0.049(4) -0.004(3) -0.001(3) 0.001(3) C36 0.061(5) 0.055(4) 0.064(5) -0.013(4) -0.020(4) 0.017(4) C37 0.039(4) 0.044(4) 0.085(6) -0.025(4) 0.006(4) 0.001(3) C38 0.058(5) 0.043(4) 0.082(5) -0.009(4) 0.019(5) -0.003(3) C39 0.055(4) 0.043(4) 0.050(4) -0.004(3) 0.009(3) 0.010(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 O1 2.056(5) . ? Zn1 N1 2.095(5) . ? Zn1 N3 2.116(5) . ? Zn1 N4 2.264(5) . ? Zn1 N2 2.295(5) . ? Zn1 O2 2.360(6) . ? Zn1 C33 2.536(6) . ? S1 C12 1.742(6) . ? S1 C13 1.744(6) . ? S2 C12 1.744(6) . ? S2 C14 1.770(6) . ? S3 C13 1.757(6) . ? S3 C15 1.794(7) . ? S4 C14 1.742(6) . ? S4 C16 1.757(8) . ? S5 C28 1.745(6) . ? S5 C29 1.755(6) . ? S6 C28 1.744(5) . ? S6 C30 1.749(6) . ? S7 C29 1.744(6) . ? S7 C31 1.794(7) . ? S8 C30 1.739(6) . ? S8 C32 1.800(7) . ? O1 C33 1.261(8) . ? O2 C33 1.245(9) . ? O3 N5 1.241(10) . ? O4 N5 1.170(9) . ? O5 N5 1.138(10) . ? N1 C5 1.325(7) . ? N1 C1 1.348(8) . ? N2 C10 1.318(8) . ? N2 C6 1.344(7) . ? N3 C21 1.327(7) . ? N3 C17 1.336(8) . ? N4 C22 1.342(7) . ? N4 C26 1.351(8) . ? C1 C2 1.390(9) . ? C1 H1 0.9400 . ? C2 C3 1.390(8) . ? C2 H2 0.9400 . ? C3 C4 1.376(8) . ? C3 H3 0.9400 . ? C4 C5 1.400(8) . ? C4 C11 1.492(8) . ? C5 C10 1.423(8) . ? C6 C7 1.376(8) . ? C6 H6B 0.9400 . ? C7 C8 1.411(9) . ? C7 H7 0.9400 . ? C8 C9 1.370(8) . ? C8 H8 0.9400 . ? C9 C10 1.415(8) . ? C9 C11 1.477(8) . ? C11 C12 1.352(8) . ? C13 C14 1.329(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.388(9) . ? C17 H17 0.9400 . ? C18 C19 1.401(9) . ? C18 H18 0.9400 . ? C19 C20 1.401(8) . ? C19 H19 0.9400 . ? C20 C21 1.400(8) . ? C20 C27 1.463(8) . ? C21 C26 1.429(8) . ? C22 C23 1.378(8) . ? C22 H22 0.9400 . ? C23 C24 1.379(9) . ? C23 H23 0.9400 . ? C24 C25 1.396(8) . ? C24 H24 0.9400 . ? C25 C26 1.390(8) . ? C25 C27 1.484(8) . ? C27 C28 1.351(8) . ? C29 C30 1.351(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.499(8) . ? C34 C39 1.374(8) . ? C34 C35 1.374(9) . ? C35 C36 1.413(10) . ? C35 H35 0.9400 . ? C36 C37 1.356(11) . ? C36 H36 0.9400 . ? C37 C38 1.370(11) . ? C37 H37 0.9400 . ? C38 C39 1.373(10) . ? C38 H38 0.9400 . ? C39 H39 0.9400 . ? O6 C40 1.48(2) . ? O6' C40' 1.436(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N1 151.21(19) . . ? O1 Zn1 N3 99.23(19) . . ? N1 Zn1 N3 108.95(17) . . ? O1 Zn1 N4 98.43(18) . . ? N1 Zn1 N4 91.26(19) . . ? N3 Zn1 N4 82.19(18) . . ? O1 Zn1 N2 92.31(18) . . ? N1 Zn1 N2 81.15(18) . . ? N3 Zn1 N2 92.06(18) . . ? N4 Zn1 N2 168.49(16) . . ? O1 Zn1 O2 58.77(17) . . ? N1 Zn1 O2 95.61(18) . . ? N3 Zn1 O2 152.23(18) . . ? N4 Zn1 O2 84.57(19) . . ? N2 Zn1 O2 104.67(19) . . ? O1 Zn1 C33 29.6(2) . . ? N1 Zn1 C33 123.7(2) . . ? N3 Zn1 C33 127.2(2) . . ? N4 Zn1 C33 91.99(18) . . ? N2 Zn1 C33 99.41(18) . . ? O2 Zn1 C33 29.2(2) . . ? C12 S1 C13 96.8(3) . . ? C12 S2 C14 96.6(3) . . ? C13 S3 C15 102.3(3) . . ? C14 S4 C16 104.3(3) . . ? C28 S5 C29 96.9(3) . . ? C28 S6 C30 97.0(3) . . ? C29 S7 C31 102.5(3) . . ? C30 S8 C32 100.0(3) . . ? C33 O1 Zn1 96.8(4) . . ? C33 O2 Zn1 83.3(4) . . ? C5 N1 C1 115.6(5) . . ? C5 N1 Zn1 109.8(4) . . ? C1 N1 Zn1 134.6(4) . . ? C10 N2 C6 115.1(5) . . ? C10 N2 Zn1 103.2(4) . . ? C6 N2 Zn1 141.6(4) . . ? C21 N3 C17 115.5(5) . . ? C21 N3 Zn1 108.1(4) . . ? C17 N3 Zn1 136.0(4) . . ? C22 N4 C26 114.8(5) . . ? C22 N4 Zn1 141.4(4) . . ? C26 N4 Zn1 103.7(4) . . ? O5 N5 O4 128.3(11) . . ? O5 N5 O3 116.3(11) . . ? O4 N5 O3 115.5(10) . . ? N1 C1 C2 121.8(5) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C1 C2 C3 120.5(6) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 119.1(6) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 115.4(5) . . ? C3 C4 C11 137.4(6) . . ? C5 C4 C11 107.1(5) . . ? N1 C5 C4 127.6(6) . . ? N1 C5 C10 122.2(6) . . ? C4 C5 C10 110.2(5) . . ? N2 C6 C7 123.5(6) . . ? N2 C6 H6B 118.3 . . ? C7 C6 H6B 118.3 . . ? C6 C7 C8 119.7(6) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 118.5(6) . . ? C9 C8 H8 120.8 . . ? C7 C8 H8 120.8 . . ? C8 C9 C10 116.0(6) . . ? C8 C9 C11 136.5(6) . . ? C10 C9 C11 107.5(5) . . ? N2 C10 C9 127.2(6) . . ? N2 C10 C5 123.6(5) . . ? C9 C10 C5 109.1(5) . . ? C12 C11 C9 128.4(5) . . ? C12 C11 C4 125.6(5) . . ? C9 C11 C4 106.0(5) . . ? C11 C12 S1 122.6(4) . . ? C11 C12 S2 124.3(5) . . ? S1 C12 S2 113.1(3) . . ? C14 C13 S1 117.6(5) . . ? C14 C13 S3 122.3(5) . . ? S1 C13 S3 120.1(4) . . ? C13 C14 S4 123.0(5) . . ? C13 C14 S2 115.8(5) . . ? S4 C14 S2 120.8(4) . . ? S3 C15 H15A 109.5 . . ? S3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? S4 C16 H16A 109.5 . . ? S4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 122.0(6) . . ? N3 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C17 C18 C19 121.8(6) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C20 C19 C18 116.9(6) . . ? C20 C19 H19 121.6 . . ? C18 C19 H19 121.6 . . ? C21 C20 C19 115.8(5) . . ? C21 C20 C27 108.6(5) . . ? C19 C20 C27 135.5(6) . . ? N3 C21 C20 128.0(5) . . ? N3 C21 C26 123.7(5) . . ? C20 C21 C26 108.3(5) . . ? N4 C22 C23 121.8(6) . . ? N4 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C22 C23 C24 122.4(6) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C23 C24 C25 117.7(5) . . ? C23 C24 H24 121.1 . . ? C25 C24 H24 121.1 . . ? C26 C25 C24 115.5(6) . . ? C26 C25 C27 107.3(5) . . ? C24 C25 C27 137.3(5) . . ? N4 C26 C25 127.8(5) . . ? N4 C26 C21 122.0(5) . . ? C25 C26 C21 110.2(5) . . ? C28 C27 C20 128.3(5) . . ? C28 C27 C25 126.0(5) . . ? C20 C27 C25 105.6(5) . . ? C27 C28 S6 123.7(5) . . ? C27 C28 S5 123.1(4) . . ? S6 C28 S5 113.2(3) . . ? C30 C29 S7 123.3(5) . . ? C30 C29 S5 116.3(5) . . ? S7 C29 S5 120.4(4) . . ? C29 C30 S8 124.4(5) . . ? C29 C30 S6 116.6(4) . . ? S8 C30 S6 118.9(3) . . ? S7 C31 H31A 109.5 . . ? S7 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S7 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S8 C32 H32A 109.5 . . ? S8 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S8 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 C33 O1 121.2(6) . . ? O2 C33 C34 119.9(7) . . ? O1 C33 C34 119.0(7) . . ? O2 C33 Zn1 67.6(4) . . ? O1 C33 Zn1 53.6(3) . . ? C34 C33 Zn1 172.6(6) . . ? C39 C34 C35 120.3(6) . . ? C39 C34 C33 120.3(6) . . ? C35 C34 C33 119.4(6) . . ? C34 C35 C36 118.8(7) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C37 C36 C35 119.4(7) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C36 C37 C38 121.7(7) . . ? C36 C37 H37 119.2 . . ? C38 C37 H37 119.2 . . ? C37 C38 C39 119.0(7) . . ? C37 C38 H38 120.5 . . ? C39 C38 H38 120.5 . . ? C38 C39 C34 120.8(7) . . ? C38 C39 H39 119.6 . . ? C34 C39 H39 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Zn1 O1 C33 29.4(6) . . . . ? N3 Zn1 O1 C33 -162.4(4) . . . . ? N4 Zn1 O1 C33 -79.0(4) . . . . ? N2 Zn1 O1 C33 105.1(4) . . . . ? O2 Zn1 O1 C33 -0.7(4) . . . . ? O1 Zn1 O2 C33 0.7(4) . . . . ? N1 Zn1 O2 C33 -165.3(4) . . . . ? N3 Zn1 O2 C33 42.2(6) . . . . ? N4 Zn1 O2 C33 104.0(4) . . . . ? N2 Zn1 O2 C33 -83.0(4) . . . . ? O1 Zn1 N1 C5 77.8(5) . . . . ? N3 Zn1 N1 C5 -89.8(4) . . . . ? N4 Zn1 N1 C5 -172.0(4) . . . . ? N2 Zn1 N1 C5 -0.7(4) . . . . ? O2 Zn1 N1 C5 103.3(4) . . . . ? C33 Zn1 N1 C5 94.8(4) . . . . ? O1 Zn1 N1 C1 -100.8(6) . . . . ? N3 Zn1 N1 C1 91.6(6) . . . . ? N4 Zn1 N1 C1 9.4(6) . . . . ? N2 Zn1 N1 C1 -179.3(6) . . . . ? O2 Zn1 N1 C1 -75.3(6) . . . . ? C33 Zn1 N1 C1 -83.8(6) . . . . ? O1 Zn1 N2 C10 -151.1(4) . . . . ? N1 Zn1 N2 C10 0.7(4) . . . . ? N3 Zn1 N2 C10 109.6(4) . . . . ? N4 Zn1 N2 C10 49.9(12) . . . . ? O2 Zn1 N2 C10 -92.8(4) . . . . ? C33 Zn1 N2 C10 -122.2(4) . . . . ? O1 Zn1 N2 C6 26.7(7) . . . . ? N1 Zn1 N2 C6 178.5(7) . . . . ? N3 Zn1 N2 C6 -72.6(7) . . . . ? N4 Zn1 N2 C6 -132.3(10) . . . . ? O2 Zn1 N2 C6 85.0(7) . . . . ? C33 Zn1 N2 C6 55.6(7) . . . . ? O1 Zn1 N3 C21 92.7(4) . . . . ? N1 Zn1 N3 C21 -93.3(4) . . . . ? N4 Zn1 N3 C21 -4.6(4) . . . . ? N2 Zn1 N3 C21 -174.6(4) . . . . ? O2 Zn1 N3 C21 57.7(6) . . . . ? C33 Zn1 N3 C21 81.9(4) . . . . ? O1 Zn1 N3 C17 -79.4(6) . . . . ? N1 Zn1 N3 C17 94.6(6) . . . . ? N4 Zn1 N3 C17 -176.8(6) . . . . ? N2 Zn1 N3 C17 13.2(6) . . . . ? O2 Zn1 N3 C17 -114.5(6) . . . . ? C33 Zn1 N3 C17 -90.2(6) . . . . ? O1 Zn1 N4 C22 81.7(7) . . . . ? N1 Zn1 N4 C22 -71.0(7) . . . . ? N3 Zn1 N4 C22 180.0(7) . . . . ? N2 Zn1 N4 C22 -119.5(10) . . . . ? O2 Zn1 N4 C22 24.5(7) . . . . ? C33 Zn1 N4 C22 52.7(7) . . . . ? O1 Zn1 N4 C26 -93.2(4) . . . . ? N1 Zn1 N4 C26 114.0(4) . . . . ? N3 Zn1 N4 C26 5.0(4) . . . . ? N2 Zn1 N4 C26 65.6(12) . . . . ? O2 Zn1 N4 C26 -150.5(4) . . . . ? C33 Zn1 N4 C26 -122.2(4) . . . . ? C5 N1 C1 C2 -1.0(8) . . . . ? Zn1 N1 C1 C2 177.5(4) . . . . ? N1 C1 C2 C3 0.8(9) . . . . ? C1 C2 C3 C4 0.2(9) . . . . ? C2 C3 C4 C5 -0.8(8) . . . . ? C2 C3 C4 C11 -178.1(6) . . . . ? C1 N1 C5 C4 0.3(8) . . . . ? Zn1 N1 C5 C4 -178.6(5) . . . . ? C1 N1 C5 C10 179.5(5) . . . . ? Zn1 N1 C5 C10 0.6(7) . . . . ? C3 C4 C5 N1 0.7(9) . . . . ? C11 C4 C5 N1 178.7(5) . . . . ? C3 C4 C5 C10 -178.7(5) . . . . ? C11 C4 C5 C10 -0.6(6) . . . . ? C10 N2 C6 C7 -0.3(9) . . . . ? Zn1 N2 C6 C7 -178.0(5) . . . . ? N2 C6 C7 C8 1.6(10) . . . . ? C6 C7 C8 C9 -1.4(9) . . . . ? C7 C8 C9 C10 -0.1(8) . . . . ? C7 C8 C9 C11 -178.6(6) . . . . ? C6 N2 C10 C9 -1.4(9) . . . . ? Zn1 N2 C10 C9 177.1(5) . . . . ? C6 N2 C10 C5 -179.1(5) . . . . ? Zn1 N2 C10 C5 -0.6(6) . . . . ? C8 C9 C10 N2 1.6(9) . . . . ? C11 C9 C10 N2 -179.5(5) . . . . ? C8 C9 C10 C5 179.6(5) . . . . ? C11 C9 C10 C5 -1.5(6) . . . . ? N1 C5 C10 N2 0.1(9) . . . . ? C4 C5 C10 N2 179.4(5) . . . . ? N1 C5 C10 C9 -178.1(5) . . . . ? C4 C5 C10 C9 1.3(6) . . . . ? C8 C9 C11 C12 -1.0(11) . . . . ? C10 C9 C11 C12 -179.6(6) . . . . ? C8 C9 C11 C4 179.7(7) . . . . ? C10 C9 C11 C4 1.1(6) . . . . ? C3 C4 C11 C12 -2.2(11) . . . . ? C5 C4 C11 C12 -179.6(5) . . . . ? C3 C4 C11 C9 177.1(7) . . . . ? C5 C4 C11 C9 -0.3(6) . . . . ? C9 C11 C12 S1 176.3(4) . . . . ? C4 C11 C12 S1 -4.5(8) . . . . ? C9 C11 C12 S2 -2.3(9) . . . . ? C4 C11 C12 S2 176.9(4) . . . . ? C13 S1 C12 C11 -178.9(5) . . . . ? C13 S1 C12 S2 -0.1(4) . . . . ? C14 S2 C12 C11 178.7(5) . . . . ? C14 S2 C12 S1 0.0(4) . . . . ? C12 S1 C13 C14 0.3(6) . . . . ? C12 S1 C13 S3 -179.4(4) . . . . ? C15 S3 C13 C14 179.9(5) . . . . ? C15 S3 C13 S1 -0.4(5) . . . . ? S1 C13 C14 S4 -174.0(3) . . . . ? S3 C13 C14 S4 5.7(8) . . . . ? S1 C13 C14 S2 -0.4(7) . . . . ? S3 C13 C14 S2 179.3(3) . . . . ? C16 S4 C14 C13 -158.5(6) . . . . ? C16 S4 C14 S2 28.1(5) . . . . ? C12 S2 C14 C13 0.3(5) . . . . ? C12 S2 C14 S4 174.0(4) . . . . ? C21 N3 C17 C18 0.0(9) . . . . ? Zn1 N3 C17 C18 171.8(4) . . . . ? N3 C17 C18 C19 -0.9(10) . . . . ? C17 C18 C19 C20 1.6(9) . . . . ? C18 C19 C20 C21 -1.5(8) . . . . ? C18 C19 C20 C27 -179.8(6) . . . . ? C17 N3 C21 C20 0.0(9) . . . . ? Zn1 N3 C21 C20 -174.0(5) . . . . ? C17 N3 C21 C26 177.7(5) . . . . ? Zn1 N3 C21 C26 3.7(7) . . . . ? C19 C20 C21 N3 0.8(9) . . . . ? C27 C20 C21 N3 179.5(6) . . . . ? C19 C20 C21 C26 -177.2(5) . . . . ? C27 C20 C21 C26 1.5(6) . . . . ? C26 N4 C22 C23 -0.8(9) . . . . ? Zn1 N4 C22 C23 -175.4(5) . . . . ? N4 C22 C23 C24 1.2(10) . . . . ? C22 C23 C24 C25 -1.0(9) . . . . ? C23 C24 C25 C26 0.4(8) . . . . ? C23 C24 C25 C27 179.9(6) . . . . ? C22 N4 C26 C25 0.3(9) . . . . ? Zn1 N4 C26 C25 176.8(5) . . . . ? C22 N4 C26 C21 178.6(5) . . . . ? Zn1 N4 C26 C21 -4.9(6) . . . . ? C24 C25 C26 N4 -0.1(9) . . . . ? C27 C25 C26 N4 -179.7(5) . . . . ? C24 C25 C26 C21 -178.6(5) . . . . ? C27 C25 C26 C21 1.8(6) . . . . ? N3 C21 C26 N4 1.2(9) . . . . ? C20 C21 C26 N4 179.3(5) . . . . ? N3 C21 C26 C25 179.8(5) . . . . ? C20 C21 C26 C25 -2.1(6) . . . . ? C21 C20 C27 C28 178.9(6) . . . . ? C19 C20 C27 C28 -2.7(11) . . . . ? C21 C20 C27 C25 -0.4(6) . . . . ? C19 C20 C27 C25 178.0(6) . . . . ? C26 C25 C27 C28 179.8(5) . . . . ? C24 C25 C27 C28 0.3(11) . . . . ? C26 C25 C27 C20 -0.9(6) . . . . ? C24 C25 C27 C20 179.7(6) . . . . ? C20 C27 C28 S6 -176.6(4) . . . . ? C25 C27 C28 S6 2.6(8) . . . . ? C20 C27 C28 S5 2.6(9) . . . . ? C25 C27 C28 S5 -178.2(4) . . . . ? C30 S6 C28 C27 179.8(5) . . . . ? C30 S6 C28 S5 0.5(4) . . . . ? C29 S5 C28 C27 179.5(5) . . . . ? C29 S5 C28 S6 -1.2(4) . . . . ? C31 S7 C29 C30 -178.9(5) . . . . ? C31 S7 C29 S5 1.4(5) . . . . ? C28 S5 C29 C30 1.7(5) . . . . ? C28 S5 C29 S7 -178.5(4) . . . . ? S7 C29 C30 S8 -3.0(8) . . . . ? S5 C29 C30 S8 176.7(3) . . . . ? S7 C29 C30 S6 178.6(3) . . . . ? S5 C29 C30 S6 -1.6(6) . . . . ? C32 S8 C30 C29 109.6(6) . . . . ? C32 S8 C30 S6 -72.2(4) . . . . ? C28 S6 C30 C29 0.6(5) . . . . ? C28 S6 C30 S8 -177.8(3) . . . . ? Zn1 O2 C33 O1 -1.1(6) . . . . ? Zn1 O2 C33 C34 -179.9(5) . . . . ? Zn1 O1 C33 O2 1.3(7) . . . . ? Zn1 O1 C33 C34 -179.9(4) . . . . ? O1 Zn1 C33 O2 -178.8(6) . . . . ? N1 Zn1 C33 O2 17.7(5) . . . . ? N3 Zn1 C33 O2 -156.9(4) . . . . ? N4 Zn1 C33 O2 -75.2(4) . . . . ? N2 Zn1 C33 O2 103.3(4) . . . . ? N1 Zn1 C33 O1 -163.5(3) . . . . ? N3 Zn1 C33 O1 21.9(4) . . . . ? N4 Zn1 C33 O1 103.6(4) . . . . ? N2 Zn1 C33 O1 -77.9(4) . . . . ? O2 Zn1 C33 O1 178.8(6) . . . . ? O1 Zn1 C33 C34 1(3) . . . . ? N1 Zn1 C33 C34 -163(3) . . . . ? N3 Zn1 C33 C34 23(3) . . . . ? N4 Zn1 C33 C34 104(3) . . . . ? N2 Zn1 C33 C34 -77(3) . . . . ? O2 Zn1 C33 C34 180(100) . . . . ? O2 C33 C34 C39 3.7(9) . . . . ? O1 C33 C34 C39 -175.1(6) . . . . ? Zn1 C33 C34 C39 -176(3) . . . . ? O2 C33 C34 C35 -173.9(6) . . . . ? O1 C33 C34 C35 7.3(8) . . . . ? Zn1 C33 C34 C35 7(3) . . . . ? C39 C34 C35 C36 0.4(9) . . . . ? C33 C34 C35 C36 178.0(5) . . . . ? C34 C35 C36 C37 0.4(10) . . . . ? C35 C36 C37 C38 -0.2(10) . . . . ? C36 C37 C38 C39 -0.9(10) . . . . ? C37 C38 C39 C34 1.7(10) . . . . ? C35 C34 C39 C38 -1.5(9) . . . . ? C33 C34 C39 C38 -179.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.470 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.067 ########End data_3 _database_code_depnum_ccdc_archive 'CCDC 778142' #TrackingRef '- Zhu-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H44 Cl8 N6 O2 S12 Zn3' _chemical_formula_weight 1625.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 25.410(4) _cell_length_b 11.2071(15) _cell_length_c 23.501(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.552(2) _cell_angle_gamma 90.00 _cell_volume 6648.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 19189 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.6 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 1.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4643 _exptl_absorpt_correction_T_max 0.7132 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30896 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11232 _reflns_number_gt 9430 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. The restraint DFIX is applied for the bonds Zn3a_Cl5a, Zn3b_Cl5b Zn3c_Cl5c, Zn3a_Cl5d, C48_S12, C49a_Cl7a, C49a_Cl8a, C49b_Cl7b, C49b_Cl8b, C49c_Cl7c, and C49c_Cl8c. ; _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^)+(0.0002P)^2^+42.3529P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11232 _refine_ls_number_parameters 743 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.1033 _refine_ls_wR_factor_ref 0.1862 _refine_ls_wR_factor_gt 0.1797 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.010 _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 0.23687(4) 0.69507(8) 0.40284(3) 0.0438(2) Uani 1 1 d . . . Zn2 Zn 0.02714(4) 0.37007(11) 0.61938(5) 0.0659(3) Uani 1 1 d . . . Zn3A Zn 0.52421(14) 0.8457(3) 0.35971(16) 0.0881(10) Uiso 0.40 1 d PD . . Zn3B Zn 0.5254(3) 0.8577(8) 0.4500(4) 0.208(3) Uiso 0.40 1 d PD . . Zn3C Zn 0.5418(3) 0.7658(7) 0.4640(3) 0.096(2) Uiso 0.20 1 d PD . . Cl1 Cl 0.24214(10) 0.49690(17) 0.40314(9) 0.0583(5) Uani 1 1 d . . . Cl2 Cl -0.03105(12) 0.5142(3) 0.60550(12) 0.0927(9) Uani 1 1 d . . . Cl3 Cl 0.00267(10) 0.1829(3) 0.62059(12) 0.0825(8) Uani 1 1 d . . . Cl4A Cl 0.6030(4) 0.7655(10) 0.4023(4) 0.112(3) Uiso 0.40 1 d P . . Cl4B Cl 0.6012(3) 0.8275(9) 0.4026(4) 0.081(2) Uiso 0.40 1 d P . . Cl4C Cl 0.4610(11) 0.729(2) 0.4216(12) 0.1296(16) Uiso 0.20 1 d P . . Cl5A Cl 0.4607(11) 0.771(2) 0.4090(14) 0.1296(16) Uiso 0.25 1 d PD . . Cl5B Cl 0.5403(8) 0.8240(18) 0.5458(6) 0.1296(16) Uiso 0.25 1 d PD . . Cl5C Cl 0.5846(8) 0.8730(17) 0.3948(7) 0.1296(16) Uiso 0.25 1 d PD . . Cl5D Cl 0.5569(11) 0.888(2) 0.5434(10) 0.1296(16) Uiso 0.25 1 d P . . Cl6A Cl 0.4592(5) 0.8038(11) 0.4103(6) 0.1296(16) Uiso 0.50 1 d P . . Cl6B Cl 0.575(2) 0.872(6) 0.543(3) 0.134(19) Uiso 0.10 1 d P . . Cl6C Cl 0.5053(5) 0.7986(8) 0.2677(4) 0.1296(16) Uiso 0.40 1 d P . . Cl7A Cl 0.0619(8) 0.837(2) 0.7004(9) 0.167(7) Uiso 0.30 1 d PD . . Cl7B Cl 0.0501(12) 0.733(2) 0.6805(13) 0.214(11) Uiso 0.30 1 d PD . . Cl7C Cl 0.0618(6) 0.7432(15) 0.7132(7) 0.151(5) Uiso 0.40 1 d PD . . Cl8A Cl -0.0448(10) 0.8659(19) 0.6558(10) 0.189(8) Uiso 0.30 1 d PD . . Cl8B Cl -0.0102(10) 0.831(2) 0.6176(12) 0.220(9) Uiso 0.30 1 d PD . . Cl8C Cl 0.0015(10) 0.9040(18) 0.6586(10) 0.223(7) Uiso 0.40 1 d PD . . S1 S 0.26328(9) 0.84743(18) 0.09850(8) 0.0484(5) Uani 1 1 d . . . S2 S 0.15278(8) 0.90616(19) 0.10704(8) 0.0498(5) Uani 1 1 d . . . S3 S 0.25583(12) 0.9164(2) -0.02679(9) 0.0697(7) Uani 1 1 d . . . S4 S 0.13269(11) 0.9731(2) -0.01950(9) 0.0711(7) Uani 1 1 d . . . S5 S 0.30981(10) 0.90250(19) 0.70077(8) 0.0566(6) Uani 1 1 d . . . S6 S 0.19936(10) 0.83904(19) 0.70747(8) 0.0549(5) Uani 1 1 d . . . S7 S 0.32877(14) 0.9715(2) 0.82663(10) 0.0818(9) Uani 1 1 d . . . S8 S 0.20353(14) 0.9150(2) 0.83140(9) 0.0808(9) Uani 1 1 d . . . S9 S 0.31123(10) 0.5219(2) 0.62422(12) 0.0743(7) Uani 1 1 d . . . S10 S 0.29139(10) 0.5655(2) 0.74196(12) 0.0698(7) Uani 1 1 d . . . S11 S 0.42562(14) 0.5967(4) 0.6454(2) 0.1298(15) Uani 1 1 d . . . S12 S 0.40433(13) 0.6349(3) 0.78156(18) 0.1106(12) Uani 1 1 d D . . O1A O 0.5974(16) 0.505(3) 0.5094(16) 0.231(15) Uiso 0.50 1 d P . . O1B O 0.6342(7) 0.4880(14) 0.5210(7) 0.090(4) Uiso 0.50 1 d P . . O2 O 0.5389(4) 1.0452(8) 0.3469(5) 0.1296(16) Uiso 1 1 d D . . N1 N 0.1829(3) 0.7764(5) 0.3420(2) 0.0422(14) Uani 1 1 d . . . N2 N 0.2924(2) 0.7191(5) 0.3313(2) 0.0411(14) Uani 1 1 d . . . N3 N 0.2861(3) 0.7783(6) 0.4668(3) 0.0476(15) Uani 1 1 d . . . N4 N 0.1773(3) 0.7092(5) 0.4741(2) 0.0424(14) Uani 1 1 d . . . N5 N 0.0937(3) 0.3888(6) 0.5736(3) 0.0512(16) Uani 1 1 d . . . N6 N 0.0806(3) 0.4242(7) 0.6925(3) 0.0582(18) Uani 1 1 d . . . C1 C 0.1310(3) 0.8086(7) 0.3393(3) 0.0484(18) Uani 1 1 d . . . H1 H 0.1138 0.8034 0.3725 0.058 Uiso 1 1 calc R . . C2 C 0.1032(3) 0.8486(8) 0.2895(3) 0.056(2) Uani 1 1 d . . . H2 H 0.0675 0.8701 0.2899 0.067 Uiso 1 1 calc R . . C3 C 0.1259(3) 0.8588(7) 0.2380(3) 0.0490(19) Uani 1 1 d . . . H3 H 0.1061 0.8846 0.2040 0.059 Uiso 1 1 calc R . . C4 C 0.1802(3) 0.8282(6) 0.2397(3) 0.0382(16) Uani 1 1 d . . . C5 C 0.2041(3) 0.7875(6) 0.2927(3) 0.0391(16) Uani 1 1 d . . . C6 C 0.3418(3) 0.7006(7) 0.3199(3) 0.0441(17) Uani 1 1 d . . . H6 H 0.3671 0.6741 0.3495 0.053 Uiso 1 1 calc R . . C7 C 0.3574(3) 0.7194(7) 0.2646(3) 0.0483(18) Uani 1 1 d . . . H7 H 0.3928 0.7053 0.2584 0.058 Uiso 1 1 calc R . . C8 C 0.3213(3) 0.7584(6) 0.2193(3) 0.0437(17) Uani 1 1 d . . . H8 H 0.3312 0.7694 0.1823 0.052 Uiso 1 1 calc R . . C9 C 0.2691(3) 0.7805(6) 0.2315(3) 0.0388(16) Uani 1 1 d . . . C10 C 0.2590(3) 0.7588(6) 0.2872(3) 0.0373(16) Uani 1 1 d . . . C11 C 0.2197(3) 0.8242(6) 0.1993(3) 0.0379(16) Uani 1 1 d . . . C12 C 0.2130(3) 0.8550(6) 0.1413(3) 0.0382(16) Uani 1 1 d . . . C13 C 0.2257(4) 0.8939(7) 0.0357(3) 0.0484(19) Uani 1 1 d . . . C14 C 0.1749(4) 0.9200(7) 0.0393(3) 0.049(2) Uani 1 1 d . . . C15 C 0.2972(5) 0.7896(10) -0.0300(4) 0.087(3) Uani 1 1 d . . . H15A H 0.3257 0.7927 0.0012 0.130 Uiso 1 1 calc R . . H15B H 0.3121 0.7891 -0.0662 0.130 Uiso 1 1 calc R . . H15C H 0.2765 0.7177 -0.0267 0.130 Uiso 1 1 calc R . . C16 C 0.0715(5) 0.9798(12) 0.0060(5) 0.101(4) Uani 1 1 d . . . H16A H 0.0552 0.9015 0.0033 0.151 Uiso 1 1 calc R . . H16B H 0.0491 1.0363 -0.0167 0.151 Uiso 1 1 calc R . . H16C H 0.0760 1.0054 0.0457 0.151 Uiso 1 1 calc R . . C17 C 0.3364(3) 0.8154(8) 0.4698(3) 0.056(2) Uani 1 1 d . . . H17 H 0.3543 0.8127 0.4370 0.068 Uiso 1 1 calc R . . C18 C 0.3625(4) 0.8575(10) 0.5207(4) 0.075(3) Uani 1 1 d . . . H18 H 0.3980 0.8817 0.5216 0.090 Uiso 1 1 calc R . . C19 C 0.3380(3) 0.8655(9) 0.5708(4) 0.063(2) Uani 1 1 d . . . H19 H 0.3561 0.8953 0.6050 0.075 Uiso 1 1 calc R . . C20 C 0.2860(3) 0.8274(7) 0.5676(3) 0.0455(18) Uani 1 1 d . . . C21 C 0.2633(3) 0.7863(6) 0.5150(3) 0.0394(16) Uani 1 1 d . . . C22 C 0.1282(4) 0.6832(7) 0.4853(3) 0.053(2) Uani 1 1 d . . . H22 H 0.1036 0.6546 0.4555 0.063 Uiso 1 1 calc R . . C23 C 0.1123(3) 0.6969(7) 0.5395(3) 0.0494(19) Uani 1 1 d . . . H23 H 0.0776 0.6750 0.5455 0.059 Uiso 1 1 calc R . . C24 C 0.1456(3) 0.7413(7) 0.5844(3) 0.0493(19) Uani 1 1 d . . . H24 H 0.1341 0.7514 0.6207 0.059 Uiso 1 1 calc R . . C25 C 0.1970(3) 0.7711(6) 0.5745(3) 0.0445(18) Uani 1 1 d . . . C26 C 0.2091(3) 0.7511(6) 0.5183(3) 0.0390(16) Uani 1 1 d . . . C27 C 0.2456(3) 0.8189(7) 0.6073(3) 0.0442(17) Uani 1 1 d . . . C28 C 0.2507(3) 0.8492(6) 0.6647(3) 0.0465(18) Uani 1 1 d . . . C29 C 0.2854(5) 0.9144(7) 0.7684(3) 0.059(2) Uani 1 1 d . . . C30 C 0.2360(5) 0.8878(7) 0.7712(3) 0.062(3) Uani 1 1 d . . . C31 C 0.3896(5) 0.9736(11) 0.8031(5) 0.101(4) Uani 1 1 d . . . H31A H 0.3997 0.8930 0.7939 0.151 Uiso 1 1 calc R . . H31B H 0.4154 1.0058 0.8328 0.151 Uiso 1 1 calc R . . H31C H 0.3885 1.0231 0.7691 0.151 Uiso 1 1 calc R . . C32 C 0.1756(5) 0.7753(9) 0.8443(4) 0.092(4) Uani 1 1 d . . . H32A H 0.1483 0.7563 0.8133 0.138 Uiso 1 1 calc R . . H32B H 0.1601 0.7780 0.8802 0.138 Uiso 1 1 calc R . . H32C H 0.2030 0.7146 0.8466 0.138 Uiso 1 1 calc R . . C33 C 0.1068(4) 0.3745(8) 0.5212(4) 0.063(2) Uani 1 1 d . . . H33 H 0.0808 0.3492 0.4921 0.075 Uiso 1 1 calc R . . C34 C 0.1579(4) 0.3956(8) 0.5077(4) 0.068(3) Uani 1 1 d . . . H34 H 0.1652 0.3842 0.4698 0.081 Uiso 1 1 calc R . . C35 C 0.1994(4) 0.4341(8) 0.5494(4) 0.066(2) Uani 1 1 d . . . H35 H 0.2338 0.4485 0.5402 0.079 Uiso 1 1 calc R . . C36 C 0.1860(4) 0.4491(7) 0.6046(4) 0.054(2) Uani 1 1 d . . . C37 C 0.1334(3) 0.4237(7) 0.6122(4) 0.0499(19) Uani 1 1 d . . . C38 C 0.0825(4) 0.4458(9) 0.7492(4) 0.071(3) Uani 1 1 d . . . H38 H 0.0512 0.4345 0.7664 0.085 Uiso 1 1 calc R . . C39 C 0.1260(4) 0.4824(9) 0.7830(4) 0.069(3) Uani 1 1 d . . . H39 H 0.1243 0.4957 0.8222 0.083 Uiso 1 1 calc R . . C40 C 0.1730(4) 0.5003(8) 0.7601(4) 0.061(2) Uani 1 1 d . . . H40 H 0.2038 0.5247 0.7832 0.073 Uiso 1 1 calc R . . C41 C 0.1735(3) 0.4808(7) 0.7012(4) 0.055(2) Uani 1 1 d . . . C42 C 0.1265(3) 0.4427(7) 0.6716(3) 0.0500(19) Uani 1 1 d . . . C43 C 0.2139(3) 0.4858(7) 0.6598(4) 0.055(2) Uani 1 1 d . . . C44 C 0.2655(4) 0.5209(7) 0.6718(4) 0.059(2) Uani 1 1 d . . . C45 C 0.3649(4) 0.5734(9) 0.6722(5) 0.072(3) Uani 1 1 d . . . C46 C 0.3568(4) 0.5886(8) 0.7278(6) 0.079(3) Uani 1 1 d . . . C47 C 0.4585(9) 0.4623(19) 0.6627(10) 0.201(10) Uani 1 1 d . . . H47A H 0.4669 0.4568 0.7039 0.301 Uiso 1 1 calc R . . H47B H 0.4909 0.4596 0.6446 0.301 Uiso 1 1 calc R . . H47C H 0.4358 0.3961 0.6491 0.301 Uiso 1 1 calc R . . C48 C 0.3687(5) 0.6428(12) 0.8436(5) 0.102(4) Uani 1 1 d D . . H48A H 0.3512 0.5672 0.8485 0.154 Uiso 1 1 calc R . . H48B H 0.3424 0.7058 0.8383 0.154 Uiso 1 1 calc R . . H48C H 0.3933 0.6596 0.8773 0.154 Uiso 1 1 calc R . . C49A C 0.0040(11) 0.760(3) 0.6744(18) 0.098(12) Uiso 0.30 1 d PD . . C49B C 0.0443(18) 0.883(3) 0.663(2) 0.117(16) Uiso 0.30 1 d PD . . C49C C 0.069(2) 0.882(18) 0.681(17) 1.0(4) Uiso 0.40 1 d PD . . C50 C 0.5259(6) 1.1224(14) 0.3067(7) 0.1296(3) Uiso 1 1 d 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 0.0627(6) 0.0432(5) 0.0250(4) -0.0012(4) 0.0023(4) -0.0023(4) Zn2 0.0548(6) 0.0859(8) 0.0564(6) 0.0098(6) 0.0037(5) -0.0063(5) Cl1 0.0889(15) 0.0415(10) 0.0456(11) 0.0022(9) 0.0122(10) -0.0012(10) Cl2 0.0806(18) 0.112(2) 0.0787(18) 0.0045(16) -0.0179(14) 0.0234(16) Cl3 0.0718(16) 0.0894(18) 0.0902(19) -0.0009(15) 0.0265(14) -0.0226(14) S1 0.0682(13) 0.0529(11) 0.0251(8) 0.0002(8) 0.0102(8) 0.0014(10) S2 0.0631(12) 0.0574(12) 0.0275(9) 0.0019(8) -0.0015(8) -0.0005(10) S3 0.114(2) 0.0694(15) 0.0291(10) 0.0048(10) 0.0219(11) 0.0033(14) S4 0.0850(17) 0.0892(18) 0.0352(11) 0.0129(11) -0.0106(11) -0.0025(14) S5 0.0790(15) 0.0535(12) 0.0339(10) -0.0065(9) -0.0089(10) 0.0053(11) S6 0.0855(15) 0.0558(12) 0.0238(9) -0.0004(8) 0.0073(9) 0.0031(11) S7 0.134(3) 0.0651(15) 0.0379(12) -0.0075(11) -0.0265(14) 0.0051(15) S8 0.160(3) 0.0569(14) 0.0280(10) -0.0017(10) 0.0227(13) 0.0051(15) S9 0.0628(15) 0.0729(16) 0.0893(19) 0.0074(14) 0.0185(13) -0.0054(12) S10 0.0599(14) 0.0641(15) 0.0819(17) -0.0030(12) -0.0065(12) 0.0033(11) S11 0.076(2) 0.142(3) 0.178(4) -0.009(3) 0.043(2) -0.032(2) S12 0.0751(19) 0.119(3) 0.131(3) -0.035(2) -0.0165(19) -0.0084(18) N1 0.061(4) 0.046(4) 0.020(3) 0.001(2) 0.008(3) -0.007(3) N2 0.053(4) 0.039(3) 0.032(3) 0.002(3) 0.007(3) -0.002(3) N3 0.059(4) 0.047(4) 0.036(3) -0.005(3) 0.003(3) -0.006(3) N4 0.055(4) 0.043(3) 0.027(3) -0.004(3) -0.002(3) -0.005(3) N5 0.055(4) 0.058(4) 0.040(4) 0.012(3) 0.002(3) -0.002(3) N6 0.058(4) 0.073(5) 0.042(4) 0.011(3) -0.001(3) -0.004(4) C1 0.052(5) 0.063(5) 0.032(4) -0.002(4) 0.013(3) 0.002(4) C2 0.051(5) 0.070(6) 0.048(5) 0.007(4) 0.011(4) 0.008(4) C3 0.058(5) 0.058(5) 0.031(4) 0.005(3) 0.007(3) 0.007(4) C4 0.055(4) 0.036(4) 0.023(3) -0.001(3) 0.002(3) -0.002(3) C5 0.050(4) 0.036(4) 0.031(4) -0.003(3) 0.005(3) -0.004(3) C6 0.049(4) 0.046(4) 0.037(4) -0.002(3) 0.001(3) 0.001(3) C7 0.048(4) 0.049(5) 0.049(5) -0.004(4) 0.008(4) 0.000(4) C8 0.056(5) 0.041(4) 0.037(4) 0.005(3) 0.016(3) -0.002(3) C9 0.057(4) 0.035(4) 0.026(3) -0.005(3) 0.011(3) -0.005(3) C10 0.054(4) 0.034(4) 0.025(3) 0.001(3) 0.006(3) -0.002(3) C11 0.053(4) 0.038(4) 0.022(3) -0.004(3) 0.002(3) 0.001(3) C12 0.054(4) 0.038(4) 0.023(3) -0.003(3) 0.008(3) -0.002(3) C13 0.084(6) 0.044(4) 0.018(3) 0.001(3) 0.006(3) 0.000(4) C14 0.088(6) 0.039(4) 0.019(3) -0.001(3) -0.001(4) -0.003(4) C15 0.115(9) 0.091(8) 0.059(6) -0.002(6) 0.035(6) -0.004(7) C16 0.094(8) 0.120(10) 0.084(8) 0.021(7) -0.012(7) 0.034(7) C17 0.057(5) 0.071(6) 0.043(5) -0.013(4) 0.015(4) -0.008(4) C18 0.055(5) 0.110(8) 0.060(6) -0.020(6) 0.010(4) -0.019(5) C19 0.058(5) 0.087(7) 0.042(5) -0.009(4) 0.002(4) -0.005(5) C20 0.057(5) 0.043(4) 0.036(4) -0.006(3) 0.002(3) -0.003(4) C21 0.054(4) 0.040(4) 0.024(3) -0.002(3) 0.003(3) 0.004(3) C22 0.072(6) 0.047(5) 0.038(4) -0.001(3) 0.002(4) -0.013(4) C23 0.059(5) 0.050(5) 0.039(4) -0.001(3) 0.007(4) -0.008(4) C24 0.063(5) 0.048(4) 0.040(4) 0.009(3) 0.018(4) -0.001(4) C25 0.067(5) 0.036(4) 0.029(4) -0.001(3) -0.002(3) 0.003(3) C26 0.053(4) 0.038(4) 0.027(3) -0.001(3) 0.004(3) 0.002(3) C27 0.060(5) 0.045(4) 0.028(4) 0.003(3) 0.005(3) 0.003(4) C28 0.067(5) 0.039(4) 0.030(4) -0.003(3) -0.008(3) 0.004(4) C29 0.112(8) 0.039(4) 0.024(4) 0.001(3) -0.006(4) 0.010(5) C30 0.121(9) 0.041(5) 0.023(4) -0.002(3) 0.003(5) 0.010(5) C31 0.114(10) 0.083(8) 0.092(8) -0.011(6) -0.047(8) 0.000(7) C32 0.150(11) 0.072(7) 0.058(6) -0.009(5) 0.032(7) -0.004(7) C33 0.078(6) 0.055(5) 0.055(5) 0.011(4) 0.003(5) 0.002(5) C34 0.110(8) 0.053(5) 0.043(5) 0.015(4) 0.022(5) 0.015(5) C35 0.067(6) 0.056(5) 0.076(7) 0.025(5) 0.013(5) 0.011(4) C36 0.068(5) 0.041(4) 0.053(5) 0.021(4) 0.012(4) 0.008(4) C37 0.048(4) 0.046(4) 0.055(5) 0.018(4) 0.002(4) 0.002(4) C38 0.075(6) 0.099(7) 0.040(5) 0.011(5) 0.010(4) 0.011(6) C39 0.073(6) 0.076(6) 0.056(6) 0.002(5) 0.000(5) 0.007(5) C40 0.068(6) 0.053(5) 0.056(5) 0.001(4) -0.018(4) 0.004(4) C41 0.064(5) 0.038(4) 0.060(5) 0.013(4) -0.003(4) 0.004(4) C42 0.050(5) 0.053(5) 0.044(4) 0.013(4) -0.005(4) 0.002(4) C43 0.051(5) 0.044(4) 0.069(6) 0.016(4) 0.003(4) 0.005(4) C44 0.064(5) 0.040(4) 0.073(6) 0.013(4) 0.008(4) 0.004(4) C45 0.049(5) 0.067(6) 0.101(8) -0.003(6) 0.012(5) -0.014(4) C46 0.064(6) 0.049(5) 0.122(10) -0.005(6) 0.001(6) 0.004(5) C47 0.21(2) 0.19(2) 0.20(2) -0.013(17) 0.052(18) 0.070(18) C48 0.115(10) 0.104(9) 0.087(8) -0.024(7) 0.005(7) 0.001(8) _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 N3 2.065(6) . ? Zn1 N1 2.076(6) . ? Zn1 Cl1 2.225(2) . ? Zn1 N2 2.331(6) . ? Zn1 N4 2.387(6) . ? Zn2 N5 2.116(7) . ? Zn2 N6 2.153(7) . ? Zn2 Cl3 2.189(3) . ? Zn2 Cl2 2.189(3) . ? Zn3A Cl6A 2.194(12) . ? Zn3A Cl6C 2.225(10) . ? Zn3A Cl5A 2.250(18) . ? Zn3A O2 2.293(10) . ? Zn3A Cl4A 2.315(11) . ? Zn3B Cl6A 1.924(17) . ? Zn3B Cl5B 2.273(15) . ? Zn3B Cl5D 2.28(3) . ? Zn3B Cl4B 2.357(12) . ? Zn3B Cl6B 2.41(6) . ? Zn3C Cl4C 2.22(3) . ? Zn3C Cl5D 2.31(3) . ? Zn3C Cl6A 2.362(17) . ? Zn3C Cl5C 2.381(15) . ? Cl4C Cl6A 0.87(2) . ? Cl5B Cl5D 0.84(3) . ? Cl5B Cl6B 1.05(6) . ? Cl5D Cl6B 0.50(6) . ? Cl6C Cl6C 0.843(18) 2_655 ? Cl7A C49A 1.756(19) . ? Cl7B C49B 1.74(2) . ? Cl7C C49C 1.75(2) . ? Cl8A C49A 1.735(19) . ? Cl8B C49B 1.75(2) . ? Cl8C C49C 1.75(2) . ? S1 C12 1.716(7) . ? S1 C13 1.744(7) . ? S2 C12 1.744(7) . ? S2 C14 1.753(8) . ? S3 C13 1.749(8) . ? S3 C15 1.775(11) . ? S4 C16 1.730(12) . ? S4 C14 1.755(8) . ? S5 C28 1.744(8) . ? S5 C29 1.776(9) . ? S6 C28 1.740(9) . ? S6 C30 1.758(9) . ? S7 C31 1.701(14) . ? S7 C29 1.775(9) . ? S8 C30 1.745(10) . ? S8 C32 1.760(11) . ? S9 C44 1.703(10) . ? S9 C45 1.764(10) . ? S10 C46 1.752(11) . ? S10 C44 1.775(10) . ? S11 C47 1.75(2) . ? S11 C45 1.750(10) . ? S12 C46 1.725(12) . ? S12 C48 1.804(11) . ? O1A O1B 0.96(4) . ? O2 C50 1.294(13) . ? N1 C5 1.337(9) . ? N1 C1 1.361(10) . ? N2 C6 1.329(9) . ? N2 C10 1.339(9) . ? N3 C21 1.332(9) . ? N3 C17 1.340(10) . ? N4 C26 1.327(9) . ? N4 C22 1.336(10) . ? N5 C33 1.321(11) . ? N5 C37 1.337(10) . ? N6 C42 1.332(10) . ? N6 C38 1.349(11) . ? C1 C2 1.371(11) . ? C1 H1 0.9400 . ? C2 C3 1.404(11) . ? C2 H2 0.9400 . ? C3 C4 1.416(11) . ? C3 H3 0.9400 . ? C4 C5 1.398(9) . ? C4 C11 1.461(10) . ? C5 C10 1.451(10) . ? C6 C7 1.417(10) . ? C6 H6 0.9400 . ? C7 C8 1.396(10) . ? C7 H7 0.9400 . ? C8 C9 1.410(10) . ? C8 H8 0.9400 . ? C9 C10 1.383(9) . ? C9 C11 1.473(10) . ? C11 C12 1.397(9) . ? C13 C14 1.336(12) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.382(12) . ? C17 H17 0.9400 . ? C18 C19 1.394(12) . ? C18 H18 0.9400 . ? C19 C20 1.385(11) . ? C19 H19 0.9400 . ? C20 C21 1.382(9) . ? C20 C27 1.467(11) . ? C21 C26 1.443(10) . ? C22 C23 1.389(11) . ? C22 H22 0.9400 . ? C23 C24 1.369(11) . ? C23 H23 0.9400 . ? C24 C25 1.394(11) . ? C24 H24 0.9400 . ? C25 C26 1.408(10) . ? C25 C27 1.480(11) . ? C27 C28 1.381(10) . ? C29 C30 1.299(14) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.391(14) . ? C33 H33 0.9400 . ? C34 C35 1.422(14) . ? C34 H34 0.9400 . ? C35 C36 1.388(12) . ? C35 H35 0.9400 . ? C36 C37 1.396(11) . ? C36 C43 1.464(12) . ? C37 C42 1.442(11) . ? C38 C39 1.350(13) . ? C38 H38 0.9400 . ? C39 C40 1.380(13) . ? C39 H39 0.9400 . ? C40 C41 1.402(12) . ? C40 H40 0.9400 . ? C41 C42 1.380(11) . ? C41 C43 1.495(12) . ? C43 C44 1.368(12) . ? C45 C46 1.357(15) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C47 H47C 0.9700 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C48 H48C 0.9700 . ? 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 N3 Zn1 N1 126.9(2) . . ? N3 Zn1 Cl1 114.69(19) . . ? N1 Zn1 Cl1 118.36(17) . . ? N3 Zn1 N2 96.1(2) . . ? N1 Zn1 N2 81.9(2) . . ? Cl1 Zn1 N2 94.40(16) . . ? N3 Zn1 N4 80.8(2) . . ? N1 Zn1 N4 91.9(2) . . ? Cl1 Zn1 N4 96.13(16) . . ? N2 Zn1 N4 169.4(2) . . ? N5 Zn2 N6 84.8(3) . . ? N5 Zn2 Cl3 110.3(2) . . ? N6 Zn2 Cl3 114.4(2) . . ? N5 Zn2 Cl2 114.6(2) . . ? N6 Zn2 Cl2 105.4(2) . . ? Cl3 Zn2 Cl2 121.40(12) . . ? Cl6A Zn3A Cl6C 112.6(5) . . ? Cl6A Zn3A Cl5A 9.4(9) . . ? Cl6C Zn3A Cl5A 108.9(10) . . ? Cl6A Zn3A O2 115.1(4) . . ? Cl6C Zn3A O2 97.1(4) . . ? Cl5A Zn3A O2 124.5(7) . . ? Cl6A Zn3A Cl4A 110.5(5) . . ? Cl6C Zn3A Cl4A 114.1(4) . . ? Cl5A Zn3A Cl4A 105.6(9) . . ? O2 Zn3A Cl4A 106.8(4) . . ? Cl6A Zn3B Cl5B 117.8(8) . . ? Cl6A Zn3B Cl5D 134.9(9) . . ? Cl5B Zn3B Cl5D 21.2(7) . . ? Cl6A Zn3B Cl4B 116.2(6) . . ? Cl5B Zn3B Cl4B 113.0(6) . . ? Cl5D Zn3B Cl4B 105.1(8) . . ? Cl6A Zn3B Cl6B 143.4(16) . . ? Cl5B Zn3B Cl6B 25.8(14) . . ? Cl5D Zn3B Cl6B 11.9(15) . . ? Cl4B Zn3B Cl6B 93.6(13) . . ? Cl4C Zn3C Cl5D 122.1(10) . . ? Cl4C Zn3C Cl6A 21.7(6) . . ? Cl5D Zn3C Cl6A 112.3(8) . . ? Cl4C Zn3C Cl5C 104.9(9) . . ? Cl5D Zn3C Cl5C 101.9(9) . . ? Cl6A Zn3C Cl5C 89.5(6) . . ? Cl6A Cl4C Zn3C 88.5(19) . . ? Cl5D Cl5B Cl6B 28(4) . . ? Cl5D Cl5B Zn3B 80(2) . . ? Cl6B Cl5B Zn3B 84(3) . . ? Cl6B Cl5D Cl5B 100(10) . . ? Cl6B Cl5D Zn3B 99(9) . . ? Cl5B Cl5D Zn3B 79(2) . . ? Cl6B Cl5D Zn3C 81(9) . . ? Cl5B Cl5D Zn3C 61(2) . . ? Zn3B Cl5D Zn3C 28.9(4) . . ? Cl4C Cl6A Zn3B 98.1(19) . . ? Cl4C Cl6A Zn3A 110.7(19) . . ? Zn3B Cl6A Zn3A 61.6(4) . . ? Cl4C Cl6A Zn3C 69.8(18) . . ? Zn3B Cl6A Zn3C 28.8(4) . . ? Zn3A Cl6A Zn3C 69.5(4) . . ? Cl5D Cl6B Cl5B 51(7) . . ? Cl5D Cl6B Zn3B 69(9) . . ? Cl5B Cl6B Zn3B 70(3) . . ? Cl6C Cl6C Zn3A 165.2(9) 2_655 . ? C12 S1 C13 96.3(4) . . ? C12 S2 C14 95.3(4) . . ? C13 S3 C15 103.8(4) . . ? C16 S4 C14 103.5(5) . . ? C28 S5 C29 95.3(5) . . ? C28 S6 C30 96.5(5) . . ? C31 S7 C29 105.1(5) . . ? C30 S8 C32 102.8(5) . . ? C44 S9 C45 96.8(5) . . ? C46 S10 C44 97.1(5) . . ? C47 S11 C45 101.8(9) . . ? C46 S12 C48 103.5(6) . . ? C50 O2 Zn3A 135.7(10) . . ? C5 N1 C1 114.7(6) . . ? C5 N1 Zn1 109.8(5) . . ? C1 N1 Zn1 135.1(5) . . ? C6 N2 C10 115.3(6) . . ? C6 N2 Zn1 142.2(5) . . ? C10 N2 Zn1 102.4(5) . . ? C21 N3 C17 116.0(6) . . ? C21 N3 Zn1 111.3(5) . . ? C17 N3 Zn1 132.4(5) . . ? C26 N4 C22 115.0(6) . . ? C26 N4 Zn1 101.2(5) . . ? C22 N4 Zn1 143.6(5) . . ? C33 N5 C37 114.6(8) . . ? C33 N5 Zn2 139.8(6) . . ? C37 N5 Zn2 105.6(5) . . ? C42 N6 C38 113.8(8) . . ? C42 N6 Zn2 104.3(5) . . ? C38 N6 Zn2 141.9(7) . . ? N1 C1 C2 121.9(7) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 122.6(8) . . ? C1 C2 H2 118.7 . . ? C3 C2 H2 118.7 . . ? C2 C3 C4 116.8(7) . . ? C2 C3 H3 121.6 . . ? C4 C3 H3 121.6 . . ? C5 C4 C3 115.3(6) . . ? C5 C4 C11 107.9(6) . . ? C3 C4 C11 136.8(6) . . ? N1 C5 C4 128.7(7) . . ? N1 C5 C10 122.9(6) . . ? C4 C5 C10 108.5(6) . . ? N2 C6 C7 122.0(7) . . ? N2 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C6 121.3(7) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C7 C8 C9 116.8(7) . . ? C7 C8 H8 121.6 . . ? C9 C8 H8 121.6 . . ? C10 C9 C8 116.3(7) . . ? C10 C9 C11 107.7(6) . . ? C8 C9 C11 136.0(6) . . ? N2 C10 C9 128.3(7) . . ? N2 C10 C5 122.4(6) . . ? C9 C10 C5 109.3(6) . . ? C12 C11 C4 127.6(6) . . ? C12 C11 C9 125.8(7) . . ? C4 C11 C9 106.6(5) . . ? C11 C12 S1 123.0(6) . . ? C11 C12 S2 122.3(6) . . ? S1 C12 S2 114.7(4) . . ? C14 C13 S1 116.7(6) . . ? C14 C13 S3 122.8(6) . . ? S1 C13 S3 120.2(5) . . ? C13 C14 S2 116.8(6) . . ? C13 C14 S4 122.1(6) . . ? S2 C14 S4 121.0(6) . . ? S3 C15 H15A 109.5 . . ? S3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? S4 C16 H16A 109.5 . . ? S4 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S4 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 120.8(8) . . ? N3 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C19 122.4(9) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C20 C19 C18 116.7(8) . . ? C20 C19 H19 121.6 . . ? C18 C19 H19 121.6 . . ? C21 C20 C19 116.6(7) . . ? C21 C20 C27 107.3(7) . . ? C19 C20 C27 136.0(7) . . ? N3 C21 C20 127.3(7) . . ? N3 C21 C26 122.5(6) . . ? C20 C21 C26 110.2(6) . . ? N4 C22 C23 122.2(7) . . ? N4 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C24 C23 C22 121.9(8) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 117.9(7) . . ? C23 C24 H24 121.1 . . ? C25 C24 H24 121.1 . . ? C24 C25 C26 115.4(7) . . ? C24 C25 C27 137.9(7) . . ? C26 C25 C27 106.7(7) . . ? N4 C26 C25 127.7(7) . . ? N4 C26 C21 123.7(6) . . ? C25 C26 C21 108.6(6) . . ? C28 C27 C20 127.5(7) . . ? C28 C27 C25 125.4(7) . . ? C20 C27 C25 107.1(6) . . ? C27 C28 S6 123.6(6) . . ? C27 C28 S5 122.7(7) . . ? S6 C28 S5 113.7(4) . . ? C30 C29 S7 124.2(7) . . ? C30 C29 S5 117.8(6) . . ? S7 C29 S5 117.9(7) . . ? C29 C30 S8 123.3(7) . . ? C29 C30 S6 116.7(7) . . ? S8 C30 S6 119.5(7) . . ? S7 C31 H31A 109.5 . . ? S7 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S7 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S8 C32 H32A 109.5 . . ? S8 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S8 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C33 C34 122.3(9) . . ? N5 C33 H33 118.9 . . ? C34 C33 H33 118.9 . . ? C33 C34 C35 122.1(9) . . ? C33 C34 H34 119.0 . . ? C35 C34 H34 119.0 . . ? C36 C35 C34 116.1(9) . . ? C36 C35 H35 121.9 . . ? C34 C35 H35 121.9 . . ? C35 C36 C37 115.8(8) . . ? C35 C36 C43 135.7(9) . . ? C37 C36 C43 108.5(7) . . ? N5 C37 C36 129.2(8) . . ? N5 C37 C42 122.2(7) . . ? C36 C37 C42 108.6(7) . . ? N6 C38 C39 124.7(10) . . ? N6 C38 H38 117.7 . . ? C39 C38 H38 117.7 . . ? C38 C39 C40 120.2(9) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C39 C40 C41 117.8(8) . . ? C39 C40 H40 121.1 . . ? C41 C40 H40 121.1 . . ? C42 C41 C40 116.3(8) . . ? C42 C41 C43 107.6(8) . . ? C40 C41 C43 136.1(8) . . ? N6 C42 C41 127.2(8) . . ? N6 C42 C37 123.0(7) . . ? C41 C42 C37 109.8(8) . . ? C44 C43 C36 128.3(9) . . ? C44 C43 C41 126.2(8) . . ? C36 C43 C41 105.5(7) . . ? C43 C44 S9 125.2(8) . . ? C43 C44 S10 121.2(7) . . ? S9 C44 S10 113.6(5) . . ? C46 C45 S11 124.3(8) . . ? C46 C45 S9 117.7(8) . . ? S11 C45 S9 117.9(7) . . ? C45 C46 S12 125.0(9) . . ? C45 C46 S10 114.6(8) . . ? S12 C46 S10 120.3(8) . . ? S11 C47 H47A 109.5 . . ? S11 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? S11 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? S12 C48 H48A 109.5 . . ? S12 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? S12 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? Cl8A C49A Cl7A 107.3(19) . . ? Cl7B C49B Cl8B 81.8(18) . . ? Cl8C C49C Cl7C 96.2(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl5D Zn3C Cl4C Cl6A 69(2) . . . . ? Cl5C Zn3C Cl4C Cl6A -46(2) . . . . ? Cl6A Zn3B Cl5B Cl5D -148(2) . . . . ? Cl4B Zn3B Cl5B Cl5D 72(3) . . . . ? Cl6B Zn3B Cl5B Cl5D 28(4) . . . . ? Cl6A Zn3B Cl5B Cl6B -176(3) . . . . ? Cl5D Zn3B Cl5B Cl6B -28(4) . . . . ? Cl4B Zn3B Cl5B Cl6B 44(4) . . . . ? Zn3B Cl5B Cl5D Cl6B -97(10) . . . . ? Cl6B Cl5B Cl5D Zn3B 97(10) . . . . ? Cl6B Cl5B Cl5D Zn3C 74(10) . . . . ? Zn3B Cl5B Cl5D Zn3C -23.7(9) . . . . ? Cl6A Zn3B Cl5D Cl6B 140(10) . . . . ? Cl5B Zn3B Cl5D Cl6B 99(10) . . . . ? Cl4B Zn3B Cl5D Cl6B -16(10) . . . . ? Cl6A Zn3B Cl5D Cl5B 41(3) . . . . ? Cl4B Zn3B Cl5D Cl5B -115(3) . . . . ? Cl6B Zn3B Cl5D Cl5B -99(10) . . . . ? Cl6A Zn3B Cl5D Zn3C 87.6(12) . . . . ? Cl5B Zn3B Cl5D Zn3C 46(2) . . . . ? Cl4B Zn3B Cl5D Zn3C -68.7(7) . . . . ? Cl6B Zn3B Cl5D Zn3C -53(10) . . . . ? Cl4C Zn3C Cl5D Cl6B 172(9) . . . . ? Cl6A Zn3C Cl5D Cl6B -166(9) . . . . ? Cl5C Zn3C Cl5D Cl6B -72(10) . . . . ? Cl4C Zn3C Cl5D Cl5B 65(3) . . . . ? Cl6A Zn3C Cl5D Cl5B 87(3) . . . . ? Cl5C Zn3C Cl5D Cl5B -179(3) . . . . ? Cl4C Zn3C Cl5D Zn3B -60.4(11) . . . . ? Cl6A Zn3C Cl5D Zn3B -38.6(8) . . . . ? Cl5C Zn3C Cl5D Zn3B 55.9(8) . . . . ? Zn3C Cl4C Cl6A Zn3B -5.2(10) . . . . ? Zn3C Cl4C Cl6A Zn3A 57.5(13) . . . . ? Cl5B Zn3B Cl6A Cl4C -53(2) . . . . ? Cl5D Zn3B Cl6A Cl4C -69(2) . . . . ? Cl4B Zn3B Cl6A Cl4C 85(2) . . . . ? Cl6B Zn3B Cl6A Cl4C -56(3) . . . . ? Cl5B Zn3B Cl6A Zn3A -162.6(8) . . . . ? Cl5D Zn3B Cl6A Zn3A -178.2(12) . . . . ? Cl4B Zn3B Cl6A Zn3A -23.9(5) . . . . ? Cl6B Zn3B Cl6A Zn3A -165(2) . . . . ? Cl5B Zn3B Cl6A Zn3C -63.7(9) . . . . ? Cl5D Zn3B Cl6A Zn3C -79.3(12) . . . . ? Cl4B Zn3B Cl6A Zn3C 75.1(8) . . . . ? Cl6B Zn3B Cl6A Zn3C -66(2) . . . . ? Cl6C Zn3A Cl6A Cl4C 85(2) . . . . ? Cl5A Zn3A Cl6A Cl4C 17(8) . . . . ? O2 Zn3A Cl6A Cl4C -165(2) . . . . ? Cl4A Zn3A Cl6A Cl4C -43(2) . . . . ? Cl6C Zn3A Cl6A Zn3B 173.6(5) . . . . ? Cl5A Zn3A Cl6A Zn3B 105(8) . . . . ? O2 Zn3A Cl6A Zn3B -76.4(6) . . . . ? Cl4A Zn3A Cl6A Zn3B 44.7(6) . . . . ? Cl6C Zn3A Cl6A Zn3C 143.1(4) . . . . ? Cl5A Zn3A Cl6A Zn3C 74(8) . . . . ? O2 Zn3A Cl6A Zn3C -106.9(5) . . . . ? Cl4A Zn3A Cl6A Zn3C 14.2(5) . . . . ? Cl5D Zn3C Cl6A Cl4C -121(2) . . . . ? Cl5C Zn3C Cl6A Cl4C 136(2) . . . . ? Cl4C Zn3C Cl6A Zn3B 169(2) . . . . ? Cl5D Zn3C Cl6A Zn3B 47.8(10) . . . . ? Cl5C Zn3C Cl6A Zn3B -54.9(8) . . . . ? Cl4C Zn3C Cl6A Zn3A -123(2) . . . . ? Cl5D Zn3C Cl6A Zn3A 115.9(8) . . . . ? Cl5C Zn3C Cl6A Zn3A 13.2(6) . . . . ? Zn3B Cl5D Cl6B Cl5B -81(4) . . . . ? Zn3C Cl5D Cl6B Cl5B -58(4) . . . . ? Cl5B Cl5D Cl6B Zn3B 81(4) . . . . ? Zn3C Cl5D Cl6B Zn3B 23(3) . . . . ? Zn3B Cl5B Cl6B Cl5D 79(9) . . . . ? Cl5D Cl5B Cl6B Zn3B -79(9) . . . . ? Cl6A Zn3B Cl6B Cl5D -50(11) . . . . ? Cl5B Zn3B Cl6B Cl5D -55(8) . . . . ? Cl4B Zn3B Cl6B Cl5D 164(10) . . . . ? Cl6A Zn3B Cl6B Cl5B 6(5) . . . . ? Cl5D Zn3B Cl6B Cl5B 55(8) . . . . ? Cl4B Zn3B Cl6B Cl5B -140(3) . . . . ? Cl6A Zn3A Cl6C Cl6C 87(8) . . . 2_655 ? Cl5A Zn3A Cl6C Cl6C 96(8) . . . 2_655 ? O2 Zn3A Cl6C Cl6C -34(8) . . . 2_655 ? Cl4A Zn3A Cl6C Cl6C -146(8) . . . 2_655 ? Cl6A Zn3A O2 C50 -98.2(16) . . . . ? Cl6C Zn3A O2 C50 20.9(16) . . . . ? Cl5A Zn3A O2 C50 -97.9(19) . . . . ? Cl4A Zn3A O2 C50 138.8(15) . . . . ? N3 Zn1 N1 C5 98.8(5) . . . . ? Cl1 Zn1 N1 C5 -83.4(5) . . . . ? N2 Zn1 N1 C5 7.2(5) . . . . ? N4 Zn1 N1 C5 178.6(5) . . . . ? N3 Zn1 N1 C1 -89.0(8) . . . . ? Cl1 Zn1 N1 C1 88.8(7) . . . . ? N2 Zn1 N1 C1 179.4(7) . . . . ? N4 Zn1 N1 C1 -9.2(7) . . . . ? N3 Zn1 N2 C6 52.1(8) . . . . ? N1 Zn1 N2 C6 178.6(8) . . . . ? Cl1 Zn1 N2 C6 -63.4(8) . . . . ? N4 Zn1 N2 C6 124.3(11) . . . . ? N3 Zn1 N2 C10 -133.5(4) . . . . ? N1 Zn1 N2 C10 -7.0(4) . . . . ? Cl1 Zn1 N2 C10 111.0(4) . . . . ? N4 Zn1 N2 C10 -61.2(13) . . . . ? N1 Zn1 N3 C21 91.7(5) . . . . ? Cl1 Zn1 N3 C21 -86.2(5) . . . . ? N2 Zn1 N3 C21 176.1(5) . . . . ? N4 Zn1 N3 C21 6.3(5) . . . . ? N1 Zn1 N3 C17 -94.6(8) . . . . ? Cl1 Zn1 N3 C17 87.5(8) . . . . ? N2 Zn1 N3 C17 -10.2(8) . . . . ? N4 Zn1 N3 C17 -180.0(8) . . . . ? N3 Zn1 N4 C26 -6.3(4) . . . . ? N1 Zn1 N4 C26 -133.4(4) . . . . ? Cl1 Zn1 N4 C26 107.8(4) . . . . ? N2 Zn1 N4 C26 -79.9(12) . . . . ? N3 Zn1 N4 C22 -179.3(9) . . . . ? N1 Zn1 N4 C22 53.6(9) . . . . ? Cl1 Zn1 N4 C22 -65.2(9) . . . . ? N2 Zn1 N4 C22 107.1(13) . . . . ? N6 Zn2 N5 C33 178.2(9) . . . . ? Cl3 Zn2 N5 C33 64.0(9) . . . . ? Cl2 Zn2 N5 C33 -77.3(9) . . . . ? N6 Zn2 N5 C37 -0.1(5) . . . . ? Cl3 Zn2 N5 C37 -114.3(5) . . . . ? Cl2 Zn2 N5 C37 104.4(5) . . . . ? N5 Zn2 N6 C42 0.9(5) . . . . ? Cl3 Zn2 N6 C42 110.8(5) . . . . ? Cl2 Zn2 N6 C42 -113.2(5) . . . . ? N5 Zn2 N6 C38 179.7(11) . . . . ? Cl3 Zn2 N6 C38 -70.4(11) . . . . ? Cl2 Zn2 N6 C38 65.5(11) . . . . ? C5 N1 C1 C2 0.3(11) . . . . ? Zn1 N1 C1 C2 -171.6(6) . . . . ? N1 C1 C2 C3 0.2(13) . . . . ? C1 C2 C3 C4 -1.5(13) . . . . ? C2 C3 C4 C5 2.0(10) . . . . ? C2 C3 C4 C11 180.0(8) . . . . ? C1 N1 C5 C4 0.5(11) . . . . ? Zn1 N1 C5 C4 174.4(6) . . . . ? C1 N1 C5 C10 179.3(7) . . . . ? Zn1 N1 C5 C10 -6.8(8) . . . . ? C3 C4 C5 N1 -1.7(11) . . . . ? C11 C4 C5 N1 179.8(7) . . . . ? C3 C4 C5 C10 179.3(6) . . . . ? C11 C4 C5 C10 0.8(8) . . . . ? C10 N2 C6 C7 -1.2(10) . . . . ? Zn1 N2 C6 C7 172.8(6) . . . . ? N2 C6 C7 C8 -0.1(11) . . . . ? C6 C7 C8 C9 1.4(11) . . . . ? C7 C8 C9 C10 -1.3(10) . . . . ? C7 C8 C9 C11 178.0(7) . . . . ? C6 N2 C10 C9 1.3(11) . . . . ? Zn1 N2 C10 C9 -174.9(6) . . . . ? C6 N2 C10 C5 -177.8(6) . . . . ? Zn1 N2 C10 C5 5.9(7) . . . . ? C8 C9 C10 N2 0.0(11) . . . . ? C11 C9 C10 N2 -179.5(7) . . . . ? C8 C9 C10 C5 179.2(6) . . . . ? C11 C9 C10 C5 -0.3(8) . . . . ? N1 C5 C10 N2 -0.1(11) . . . . ? C4 C5 C10 N2 178.9(6) . . . . ? N1 C5 C10 C9 -179.4(6) . . . . ? C4 C5 C10 C9 -0.3(8) . . . . ? C5 C4 C11 C12 179.0(7) . . . . ? C3 C4 C11 C12 0.9(14) . . . . ? C5 C4 C11 C9 -1.0(7) . . . . ? C3 C4 C11 C9 -179.0(8) . . . . ? C10 C9 C11 C12 -179.2(7) . . . . ? C8 C9 C11 C12 1.5(13) . . . . ? C10 C9 C11 C4 0.7(7) . . . . ? C8 C9 C11 C4 -178.5(8) . . . . ? C4 C11 C12 S1 179.4(6) . . . . ? C9 C11 C12 S1 -0.7(10) . . . . ? C4 C11 C12 S2 0.2(10) . . . . ? C9 C11 C12 S2 -179.9(5) . . . . ? C13 S1 C12 C11 178.7(6) . . . . ? C13 S1 C12 S2 -2.0(5) . . . . ? C14 S2 C12 C11 -178.4(6) . . . . ? C14 S2 C12 S1 2.4(5) . . . . ? C12 S1 C13 C14 0.7(7) . . . . ? C12 S1 C13 S3 175.4(5) . . . . ? C15 S3 C13 C14 -140.6(7) . . . . ? C15 S3 C13 S1 45.0(6) . . . . ? S1 C13 C14 S2 0.9(9) . . . . ? S3 C13 C14 S2 -173.7(4) . . . . ? S1 C13 C14 S4 177.6(4) . . . . ? S3 C13 C14 S4 3.0(10) . . . . ? C12 S2 C14 C13 -1.9(7) . . . . ? C12 S2 C14 S4 -178.7(5) . . . . ? C16 S4 C14 C13 175.0(8) . . . . ? C16 S4 C14 S2 -8.4(7) . . . . ? C21 N3 C17 C18 0.8(13) . . . . ? Zn1 N3 C17 C18 -172.7(7) . . . . ? N3 C17 C18 C19 -1.0(16) . . . . ? C17 C18 C19 C20 0.8(15) . . . . ? C18 C19 C20 C21 -0.5(13) . . . . ? C18 C19 C20 C27 179.9(9) . . . . ? C17 N3 C21 C20 -0.5(12) . . . . ? Zn1 N3 C21 C20 174.3(6) . . . . ? C17 N3 C21 C26 179.3(7) . . . . ? Zn1 N3 C21 C26 -5.8(9) . . . . ? C19 C20 C21 N3 0.4(12) . . . . ? C27 C20 C21 N3 -179.9(7) . . . . ? C19 C20 C21 C26 -179.4(7) . . . . ? C27 C20 C21 C26 0.2(8) . . . . ? C26 N4 C22 C23 -1.2(11) . . . . ? Zn1 N4 C22 C23 171.3(6) . . . . ? N4 C22 C23 C24 1.9(13) . . . . ? C22 C23 C24 C25 -1.1(12) . . . . ? C23 C24 C25 C26 -0.3(10) . . . . ? C23 C24 C25 C27 -179.4(8) . . . . ? C22 N4 C26 C25 -0.3(11) . . . . ? Zn1 N4 C26 C25 -175.7(6) . . . . ? C22 N4 C26 C21 -179.0(7) . . . . ? Zn1 N4 C26 C21 5.6(8) . . . . ? C24 C25 C26 N4 1.0(11) . . . . ? C27 C25 C26 N4 -179.6(7) . . . . ? C24 C25 C26 C21 179.9(6) . . . . ? C27 C25 C26 C21 -0.7(8) . . . . ? N3 C21 C26 N4 -0.6(11) . . . . ? C20 C21 C26 N4 179.3(7) . . . . ? N3 C21 C26 C25 -179.6(7) . . . . ? C20 C21 C26 C25 0.3(8) . . . . ? C21 C20 C27 C28 179.4(7) . . . . ? C19 C20 C27 C28 -1.0(15) . . . . ? C21 C20 C27 C25 -0.7(8) . . . . ? C19 C20 C27 C25 178.9(9) . . . . ? C24 C25 C27 C28 -0.1(14) . . . . ? C26 C25 C27 C28 -179.2(7) . . . . ? C24 C25 C27 C20 180.0(9) . . . . ? C26 C25 C27 C20 0.9(8) . . . . ? C20 C27 C28 S6 178.2(6) . . . . ? C25 C27 C28 S6 -1.7(11) . . . . ? C20 C27 C28 S5 -1.3(11) . . . . ? C25 C27 C28 S5 178.8(6) . . . . ? C30 S6 C28 C27 178.9(7) . . . . ? C30 S6 C28 S5 -1.5(5) . . . . ? C29 S5 C28 C27 -178.2(7) . . . . ? C29 S5 C28 S6 2.2(5) . . . . ? C31 S7 C29 C30 172.9(8) . . . . ? C31 S7 C29 S5 -11.7(7) . . . . ? C28 S5 C29 C30 -2.3(8) . . . . ? C28 S5 C29 S7 -178.1(5) . . . . ? S7 C29 C30 S8 5.0(12) . . . . ? S5 C29 C30 S8 -170.4(4) . . . . ? S7 C29 C30 S6 177.1(4) . . . . ? S5 C29 C30 S6 1.6(10) . . . . ? C32 S8 C30 C29 -128.0(9) . . . . ? C32 S8 C30 S6 60.1(7) . . . . ? C28 S6 C30 C29 0.0(8) . . . . ? C28 S6 C30 S8 172.3(5) . . . . ? C37 N5 C33 C34 -0.7(12) . . . . ? Zn2 N5 C33 C34 -178.9(6) . . . . ? N5 C33 C34 C35 0.0(13) . . . . ? C33 C34 C35 C36 0.1(12) . . . . ? C34 C35 C36 C37 0.4(11) . . . . ? C34 C35 C36 C43 180.0(8) . . . . ? C33 N5 C37 C36 1.4(12) . . . . ? Zn2 N5 C37 C36 -179.8(7) . . . . ? C33 N5 C37 C42 -179.5(7) . . . . ? Zn2 N5 C37 C42 -0.7(9) . . . . ? C35 C36 C37 N5 -1.3(12) . . . . ? C43 C36 C37 N5 179.0(8) . . . . ? C35 C36 C37 C42 179.5(7) . . . . ? C43 C36 C37 C42 -0.2(9) . . . . ? C42 N6 C38 C39 -0.2(14) . . . . ? Zn2 N6 C38 C39 -178.9(8) . . . . ? N6 C38 C39 C40 0.0(16) . . . . ? C38 C39 C40 C41 0.8(14) . . . . ? C39 C40 C41 C42 -1.3(12) . . . . ? C39 C40 C41 C43 -178.2(9) . . . . ? C38 N6 C42 C41 -0.3(13) . . . . ? Zn2 N6 C42 C41 178.8(7) . . . . ? C38 N6 C42 C37 179.2(8) . . . . ? Zn2 N6 C42 C37 -1.6(9) . . . . ? C40 C41 C42 N6 1.1(12) . . . . ? C43 C41 C42 N6 178.8(8) . . . . ? C40 C41 C42 C37 -178.5(7) . . . . ? C43 C41 C42 C37 -0.8(9) . . . . ? N5 C37 C42 N6 1.7(12) . . . . ? C36 C37 C42 N6 -179.0(7) . . . . ? N5 C37 C42 C41 -178.6(7) . . . . ? C36 C37 C42 C41 0.6(9) . . . . ? C35 C36 C43 C44 1.8(15) . . . . ? C37 C36 C43 C44 -178.6(8) . . . . ? C35 C36 C43 C41 -179.9(9) . . . . ? C37 C36 C43 C41 -0.3(8) . . . . ? C42 C41 C43 C44 179.0(8) . . . . ? C40 C41 C43 C44 -3.9(15) . . . . ? C42 C41 C43 C36 0.6(8) . . . . ? C40 C41 C43 C36 177.7(9) . . . . ? C36 C43 C44 S9 -3.9(12) . . . . ? C41 C43 C44 S9 178.1(6) . . . . ? C36 C43 C44 S10 178.5(6) . . . . ? C41 C43 C44 S10 0.5(11) . . . . ? C45 S9 C44 C43 -178.9(8) . . . . ? C45 S9 C44 S10 -1.1(6) . . . . ? C46 S10 C44 C43 176.8(7) . . . . ? C46 S10 C44 S9 -1.0(6) . . . . ? C47 S11 C45 C46 82.1(13) . . . . ? C47 S11 C45 S9 -95.6(10) . . . . ? C44 S9 C45 C46 3.8(9) . . . . ? C44 S9 C45 S11 -178.3(6) . . . . ? S11 C45 C46 S12 0.9(14) . . . . ? S9 C45 C46 S12 178.6(6) . . . . ? S11 C45 C46 S10 177.2(6) . . . . ? S9 C45 C46 S10 -5.1(11) . . . . ? C48 S12 C46 C45 177.8(10) . . . . ? C48 S12 C46 S10 1.6(8) . . . . ? C44 S10 C46 C45 3.6(9) . . . . ? C44 S10 C46 S12 -179.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.462 _refine_diff_density_min -1.439 _refine_diff_density_rms 0.105 ########End data_5 _database_code_depnum_ccdc_archive 'CCDC 778143' #TrackingRef '- Zhu-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55.5 H54 Cl6 N6 O1.5 S12 Zn3' _chemical_formula_weight 1622.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' _symmetry_Int_Tables_number 13 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 25.617(5) _cell_length_b 11.331(2) _cell_length_c 24.005(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.519(3) _cell_angle_gamma 90.00 _cell_volume 6946(2) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 22104 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 1.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2870 _exptl_absorpt_correction_T_max 0.7320 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23903 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.50 _reflns_number_total 12780 _reflns_number_gt 9588 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. The restraint DFIX is applied for the bonds O2_c56, O2'_C56', O1_C55, O1_C55', C33_C34, C35_C36, C33'_C34', C35'_C36', C51_C52, C53_C54, C51'_C52', C53'_C54', S7_C33', S7_C33, S12_C53, S11_C51, S11_C51', S8_C35, and S8_C35'. One solvent molecule MeOH is disordered over four sites with the occupancy factor of 0.32/0.32/0.18/0.18. ; _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^)+(0.1353P)^2^+15.5747P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12780 _refine_ls_number_parameters 730 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1267 _refine_ls_R_factor_gt 0.1003 _refine_ls_wR_factor_ref 0.2934 _refine_ls_wR_factor_gt 0.2698 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.057 _refine_ls_shift/su_mean 0.002 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 0.72736(4) 0.21232(8) 0.38831(3) 0.0429(3) Uani 1 1 d . . . Zn2 Zn 0.52641(4) -0.10341(9) 0.62581(4) 0.0500(3) Uani 1 1 d . . . Zn3 Zn 0.97031(7) 0.33448(18) 0.06732(8) 0.1155(6) Uani 1 1 d . . . Cl1 Cl 0.73219(9) 0.01687(17) 0.39649(8) 0.0503(5) Uani 1 1 d . . . Cl2 Cl 0.46762(12) 0.0380(3) 0.61852(10) 0.0842(9) Uani 1 1 d . . . Cl3 Cl 0.50287(10) -0.2898(2) 0.62426(11) 0.0709(7) Uani 1 1 d . . . Cl4 Cl 0.9447(3) 0.3422(7) -0.0282(3) 0.1326(13) Uiso 0.619(6) 1 d P A 1 Cl5 Cl 1.0425(3) 0.2405(8) 0.0865(4) 0.1326(13) Uiso 0.619(6) 1 d P A 1 Cl6 Cl 0.8970(4) 0.2905(8) 0.1062(5) 0.1326(13) Uiso 0.619(6) 1 d P A 1 Cl4' Cl 0.9740(6) 0.2899(12) -0.0221(6) 0.1326(13) Uiso 0.381(6) 1 d P A 2 Cl5' Cl 1.0501(5) 0.3019(12) 0.1161(6) 0.1326(13) Uiso 0.381(6) 1 d P A 2 Cl6' Cl 0.9018(7) 0.3274(13) 0.1141(7) 0.1326(13) Uiso 0.381(6) 1 d P A 2 S1 S 0.64257(9) 0.39367(18) 0.09886(8) 0.0491(5) Uani 1 1 d . . . S2 S 0.74943(9) 0.31911(19) 0.08496(8) 0.0497(5) Uani 1 1 d . . . S3 S 0.62086(11) 0.4668(2) -0.02133(9) 0.0638(6) Uani 1 1 d . . . S4 S 0.74209(11) 0.3721(2) -0.03856(9) 0.0685(7) Uani 1 1 d . . . S5 S 0.80529(9) 0.4278(2) 0.67321(9) 0.0531(5) Uani 1 1 d . . . S6 S 0.69873(9) 0.35543(19) 0.68992(8) 0.0498(5) Uani 1 1 d . . . S7 S 0.83072(13) 0.4826(3) 0.79582(10) 0.0771(8) Uani 1 1 d D . . S8 S 0.70911(12) 0.4104(2) 0.81300(9) 0.0660(7) Uani 1 1 d D . . S9 S 0.80015(10) 0.0460(3) 0.59170(14) 0.0773(8) Uani 1 1 d . . . S10 S 0.79492(10) 0.0874(2) 0.71023(13) 0.0741(8) Uani 1 1 d . . . S11 S 0.91245(16) 0.1263(5) 0.5920(2) 0.146(2) Uani 1 1 d D . . S12 S 0.90745(15) 0.1672(4) 0.7260(2) 0.1255(15) Uani 1 1 d D . . O1 O 0.9781(6) 0.5075(13) 0.0799(6) 0.169(5) Uiso 1 1 d D A . N1 N 0.6738(3) 0.2891(5) 0.3300(2) 0.0406(14) Uani 1 1 d . . . N2 N 0.7800(3) 0.2234(5) 0.3156(3) 0.0441(15) Uani 1 1 d . . . N3 N 0.7748(3) 0.3052(6) 0.4451(3) 0.0442(15) Uani 1 1 d . . . N4 N 0.6677(3) 0.2353(5) 0.4617(2) 0.0413(14) Uani 1 1 d . . . N5 N 0.5874(2) -0.0784(5) 0.5729(3) 0.0417(14) Uani 1 1 d . . . N6 N 0.5838(3) -0.0644(6) 0.6917(3) 0.0480(16) Uani 1 1 d . . . C1 C 0.6241(3) 0.3235(7) 0.3293(3) 0.0478(19) Uani 1 1 d . . . H1 H 0.6073 0.3225 0.3627 0.057 Uiso 1 1 calc R . . C2 C 0.5964(3) 0.3607(8) 0.2805(4) 0.055(2) Uani 1 1 d . . . H2 H 0.5616 0.3856 0.2823 0.066 Uiso 1 1 calc R . . C3 C 0.6176(3) 0.3630(7) 0.2297(3) 0.0450(18) Uani 1 1 d . . . H3 H 0.5980 0.3876 0.1971 0.054 Uiso 1 1 calc R . . C4 C 0.6701(3) 0.3267(6) 0.2290(3) 0.0397(16) Uani 1 1 d . . . C5 C 0.6953(3) 0.2926(6) 0.2807(3) 0.0381(16) Uani 1 1 d . . . C6 C 0.8288(3) 0.1943(7) 0.3012(3) 0.0507(19) Uani 1 1 d . . . H6 H 0.8539 0.1676 0.3290 0.061 Uiso 1 1 calc R . . C7 C 0.8421(3) 0.2032(7) 0.2472(3) 0.0490(19) Uani 1 1 d . . . H7 H 0.8763 0.1829 0.2393 0.059 Uiso 1 1 calc R . . C8 C 0.8072(3) 0.2408(7) 0.2036(3) 0.0472(18) Uani 1 1 d . . . H8 H 0.8170 0.2468 0.1668 0.057 Uiso 1 1 calc R . . C9 C 0.7567(3) 0.2694(6) 0.2172(3) 0.0400(16) Uani 1 1 d . . . C10 C 0.7467(3) 0.2588(6) 0.2736(3) 0.0374(16) Uani 1 1 d . . . C11 C 0.7084(3) 0.3138(6) 0.1872(3) 0.0397(16) Uani 1 1 d . . . C12 C 0.7008(3) 0.3382(6) 0.1308(3) 0.0418(17) Uani 1 1 d . . . C13 C 0.6633(4) 0.3994(7) 0.0305(3) 0.053(2) Uani 1 1 d . . . C14 C 0.7124(4) 0.3652(7) 0.0244(3) 0.050(2) Uani 1 1 d . . . C15 C 0.5650(5) 0.3686(11) -0.0277(6) 0.091(4) Uani 1 1 d . . . H15A H 0.5759 0.2901 -0.0393 0.109 Uiso 1 1 calc R . . H15B H 0.5500 0.3612 0.0085 0.109 Uiso 1 1 calc R . . C16 C 0.5253(5) 0.4173(13) -0.0698(7) 0.112(5) Uani 1 1 d . . . H16A H 0.5211 0.5012 -0.0633 0.168 Uiso 1 1 calc R . . H16B H 0.4921 0.3776 -0.0667 0.168 Uiso 1 1 calc R . . H16C H 0.5368 0.4051 -0.1069 0.168 Uiso 1 1 calc R . . C17 C 0.7974(5) 0.2674(13) -0.0278(4) 0.094(4) Uani 1 1 d . . . H17A H 0.8226 0.2954 0.0021 0.113 Uiso 1 1 calc R . . H17B H 0.7847 0.1894 -0.0174 0.113 Uiso 1 1 calc R . . C18 C 0.8230(6) 0.2603(15) -0.0826(6) 0.119(5) Uani 1 1 d . . . H18A H 0.7977 0.2314 -0.1117 0.179 Uiso 1 1 calc R . . H18B H 0.8526 0.2069 -0.0786 0.179 Uiso 1 1 calc R . . H18C H 0.8349 0.3382 -0.0927 0.179 Uiso 1 1 calc R . . C19 C 0.8237(4) 0.3486(9) 0.4445(4) 0.062(2) Uani 1 1 d . . . H19 H 0.8400 0.3476 0.4108 0.074 Uiso 1 1 calc R . . C20 C 0.8510(4) 0.3952(10) 0.4922(4) 0.070(3) Uani 1 1 d . . . H20 H 0.8855 0.4222 0.4904 0.085 Uiso 1 1 calc R . . C21 C 0.8273(4) 0.4020(9) 0.5427(4) 0.062(2) Uani 1 1 d . . . H21 H 0.8451 0.4348 0.5748 0.074 Uiso 1 1 calc R . . C22 C 0.7768(3) 0.3592(7) 0.5441(3) 0.0449(18) Uani 1 1 d . . . C23 C 0.7525(3) 0.3153(6) 0.4939(3) 0.0412(17) Uani 1 1 d . . . C24 C 0.6197(3) 0.2084(7) 0.4760(3) 0.0470(18) Uani 1 1 d . . . H24 H 0.5950 0.1787 0.4484 0.056 Uiso 1 1 calc R . . C25 C 0.6050(3) 0.2227(7) 0.5299(3) 0.0486(19) Uani 1 1 d . . . H25 H 0.5709 0.2017 0.5382 0.058 Uiso 1 1 calc R . . C26 C 0.6402(3) 0.2682(7) 0.5725(3) 0.0495(19) Uani 1 1 d . . . H26 H 0.6305 0.2778 0.6092 0.059 Uiso 1 1 calc R . . C27 C 0.6903(3) 0.2986(6) 0.5581(3) 0.0423(17) Uani 1 1 d . . . C28 C 0.6998(3) 0.2786(6) 0.5015(3) 0.0357(15) Uani 1 1 d . . . C29 C 0.7382(3) 0.3481(7) 0.5869(3) 0.0439(17) Uani 1 1 d . . . C30 C 0.7461(3) 0.3729(7) 0.6433(3) 0.0471(19) Uani 1 1 d . . . C31 C 0.7869(4) 0.4296(7) 0.7424(3) 0.050(2) Uani 1 1 d . . . C32 C 0.7379(4) 0.3965(7) 0.7498(3) 0.050(2) Uani 1 1 d . . . C33 C 0.8905(10) 0.494(4) 0.7602(13) 0.111(4) Uiso 0.50 1 d PD . . C33' C 0.8960(8) 0.422(2) 0.8011(12) 0.111(4) Uiso 0.50 1 d PD . . C34 C 0.9331(12) 0.539(3) 0.8009(12) 0.111(4) Uiso 0.50 1 d PD . . C34' C 0.8991(14) 0.506(4) 0.7542(14) 0.111(4) Uiso 0.50 1 d PD . . C35 C 0.6866(10) 0.2579(16) 0.8235(13) 0.073(3) Uiso 0.50 1 d PD . . C35' C 0.6760(9) 0.2665(16) 0.8184(13) 0.073(3) Uiso 0.50 1 d PD . . C36 C 0.6410(9) 0.249(2) 0.8589(9) 0.073(3) Uiso 0.50 1 d PD . . C36' C 0.6256(9) 0.286(2) 0.8435(10) 0.073(3) Uiso 0.50 1 d PD . . C37 C 0.5949(3) -0.0834(7) 0.5184(3) 0.0451(18) Uani 1 1 d . . . H37 H 0.5664 -0.0997 0.4924 0.054 Uiso 1 1 calc R . . C38 C 0.6445(4) -0.0648(7) 0.4995(3) 0.052(2) Uani 1 1 d . . . H38 H 0.6487 -0.0715 0.4611 0.062 Uiso 1 1 calc R . . C39 C 0.6869(3) -0.0372(7) 0.5351(3) 0.049(2) Uani 1 1 d . . . H39 H 0.7200 -0.0246 0.5216 0.058 Uiso 1 1 calc R . . C40 C 0.6798(3) -0.0280(6) 0.5925(3) 0.0450(18) Uani 1 1 d . . . C41 C 0.6289(3) -0.0512(6) 0.6069(3) 0.0414(17) Uani 1 1 d . . . C42 C 0.5889(4) -0.0527(8) 0.7482(3) 0.053(2) Uani 1 1 d . . . H42 H 0.5593 -0.0640 0.7683 0.064 Uiso 1 1 calc R . . C43 C 0.6360(4) -0.0248(7) 0.7769(3) 0.055(2) Uani 1 1 d . . . H43 H 0.6380 -0.0198 0.8161 0.066 Uiso 1 1 calc R . . C44 C 0.6808(4) -0.0039(7) 0.7489(3) 0.052(2) Uani 1 1 d . . . H44 H 0.7129 0.0140 0.7688 0.062 Uiso 1 1 calc R . . C45 C 0.6768(3) -0.0103(6) 0.6903(3) 0.0451(18) Uani 1 1 d . . . C46 C 0.6277(3) -0.0431(6) 0.6662(3) 0.0430(17) Uani 1 1 d . . . C47 C 0.7110(3) 0.0007(6) 0.6449(4) 0.0468(18) Uani 1 1 d . . . C48 C 0.7624(4) 0.0380(7) 0.6479(4) 0.057(2) Uani 1 1 d . . . C49 C 0.8580(4) 0.0937(11) 0.6289(7) 0.092(4) Uani 1 1 d . . . C50 C 0.8562(4) 0.1081(10) 0.6835(6) 0.084(3) Uani 1 1 d . . . C51 C 0.9097(16) 0.016(3) 0.5356(12) 0.135(4) Uiso 0.50 1 d PD . . C51' C 0.9299(15) -0.011(2) 0.5597(14) 0.135(4) Uiso 0.50 1 d PD . . C52 C 0.8841(14) 0.048(3) 0.4786(13) 0.135(4) Uiso 0.50 1 d PD . . C52' C 0.9032(15) -0.021(3) 0.5021(15) 0.135(4) Uiso 0.50 1 d PD . . C53 C 0.9054(15) 0.081(3) 0.7906(10) 0.135(4) Uiso 0.50 1 d PD . . C53' C 0.8906(14) 0.127(3) 0.7995(16) 0.135(4) Uiso 0.50 1 d PD . . C54 C 0.9440(15) 0.106(3) 0.8401(15) 0.135(4) Uiso 0.50 1 d PD . . C54' C 0.9403(15) 0.173(3) 0.8307(16) 0.135(4) Uiso 0.50 1 d PD . . C55 C 0.9567(19) 0.564(4) 0.1287(15) 0.141(9) Uiso 0.50 1 d PD . . C55' C 0.965(2) 0.601(3) 0.1182(17) 0.141(9) Uiso 0.50 1 d PD . . C56 C 0.5078(11) 0.369(2) 0.7349(12) 0.064(7) Uiso 0.316(10) 1 d PD . 1 O2 O 0.5527(7) 0.3083(17) 0.7132(8) 0.048(4) Uiso 0.316(10) 1 d PD . 1 C56' C 0.5172(16) 0.252(5) 0.735(2) 0.064(7) Uiso 0.184(10) 1 d PD . 2 O2' O 0.5630(11) 0.258(3) 0.7044(12) 0.048(4) Uiso 0.184(10) 1 d PD . 2 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 0.0562(6) 0.0434(5) 0.0290(4) 0.0009(3) 0.0024(4) 0.0011(4) Zn2 0.0453(6) 0.0677(6) 0.0372(5) 0.0023(4) 0.0036(4) 0.0039(4) Zn3 0.0859(11) 0.1417(15) 0.1241(14) -0.0193(12) 0.0413(10) -0.0184(10) Cl1 0.0680(13) 0.0425(10) 0.0411(10) 0.0034(8) 0.0088(9) 0.0045(9) Cl2 0.0871(19) 0.114(2) 0.0502(13) -0.0023(13) -0.0016(12) 0.0502(17) Cl3 0.0563(14) 0.0801(16) 0.0767(16) 0.0082(13) 0.0076(12) -0.0181(12) S1 0.0611(13) 0.0535(11) 0.0323(9) 0.0030(8) 0.0017(9) -0.0022(9) S2 0.0661(14) 0.0562(12) 0.0278(9) 0.0011(8) 0.0104(9) -0.0013(10) S3 0.0891(18) 0.0571(13) 0.0423(11) 0.0112(10) -0.0138(11) -0.0146(12) S4 0.0896(19) 0.0865(17) 0.0309(10) 0.0043(11) 0.0137(11) 0.0004(14) S5 0.0611(13) 0.0592(12) 0.0387(10) -0.0026(9) 0.0020(9) -0.0038(10) S6 0.0670(14) 0.0523(11) 0.0309(9) -0.0025(8) 0.0085(9) -0.0043(10) S7 0.100(2) 0.0817(17) 0.0457(12) 0.0037(12) -0.0175(13) -0.0190(15) S8 0.116(2) 0.0489(12) 0.0352(11) -0.0032(9) 0.0187(12) -0.0067(13) S9 0.0541(15) 0.0770(17) 0.102(2) -0.0067(16) 0.0161(14) -0.0089(13) S10 0.0567(15) 0.0666(15) 0.096(2) -0.0163(14) -0.0130(14) -0.0014(12) S11 0.072(2) 0.178(4) 0.193(5) -0.050(4) 0.042(3) -0.039(3) S12 0.071(2) 0.125(3) 0.176(4) -0.033(3) -0.021(2) -0.024(2) N1 0.050(4) 0.043(3) 0.029(3) -0.002(3) 0.008(3) 0.003(3) N2 0.051(4) 0.046(3) 0.035(3) 0.002(3) 0.005(3) 0.000(3) N3 0.049(4) 0.049(4) 0.036(3) 0.001(3) 0.010(3) -0.001(3) N4 0.056(4) 0.038(3) 0.030(3) -0.003(3) 0.007(3) 0.001(3) N5 0.043(4) 0.044(3) 0.038(3) 0.003(3) 0.001(3) -0.006(3) N6 0.052(4) 0.057(4) 0.035(3) 0.008(3) 0.004(3) 0.012(3) C1 0.046(5) 0.058(5) 0.039(4) 0.003(4) 0.009(3) 0.004(4) C2 0.048(5) 0.067(5) 0.051(5) 0.001(4) 0.010(4) 0.007(4) C3 0.044(4) 0.057(5) 0.034(4) 0.004(3) 0.003(3) 0.008(4) C4 0.049(4) 0.037(4) 0.034(4) 0.003(3) 0.007(3) 0.001(3) C5 0.047(4) 0.039(4) 0.030(3) 0.003(3) 0.012(3) -0.004(3) C6 0.056(5) 0.051(4) 0.045(4) 0.003(4) 0.004(4) 0.011(4) C7 0.051(5) 0.055(5) 0.043(4) 0.000(4) 0.014(4) 0.008(4) C8 0.053(5) 0.050(4) 0.039(4) -0.003(3) 0.010(4) 0.001(4) C9 0.054(5) 0.036(4) 0.030(3) -0.001(3) 0.009(3) -0.001(3) C10 0.050(4) 0.035(3) 0.028(3) 0.002(3) 0.006(3) 0.004(3) C11 0.045(4) 0.045(4) 0.030(3) -0.005(3) 0.009(3) -0.003(3) C12 0.057(5) 0.039(4) 0.030(4) -0.001(3) 0.006(3) -0.003(3) C13 0.085(7) 0.046(4) 0.026(4) 0.004(3) 0.000(4) -0.016(4) C14 0.069(6) 0.049(4) 0.034(4) -0.003(3) 0.008(4) -0.007(4) C15 0.075(8) 0.091(8) 0.104(9) 0.029(7) -0.017(7) -0.004(6) C16 0.086(9) 0.106(10) 0.137(13) 0.023(9) -0.027(9) -0.002(7) C17 0.095(9) 0.143(11) 0.048(6) 0.014(7) 0.035(6) 0.012(8) C18 0.126(12) 0.158(14) 0.081(9) 0.021(9) 0.044(9) 0.017(11) C19 0.062(6) 0.081(6) 0.044(5) -0.008(4) 0.018(4) -0.009(5) C20 0.049(5) 0.103(8) 0.061(6) -0.018(5) 0.015(4) -0.019(5) C21 0.064(6) 0.078(6) 0.042(5) -0.009(4) -0.003(4) -0.006(5) C22 0.044(4) 0.052(4) 0.041(4) -0.008(3) 0.011(3) 0.000(3) C23 0.054(5) 0.042(4) 0.027(3) -0.004(3) 0.006(3) -0.002(3) C24 0.049(5) 0.049(4) 0.043(4) 0.003(3) 0.007(4) -0.002(4) C25 0.054(5) 0.043(4) 0.050(5) 0.001(4) 0.010(4) -0.004(4) C26 0.056(5) 0.055(5) 0.038(4) -0.004(4) 0.009(4) -0.004(4) C27 0.054(5) 0.040(4) 0.034(4) -0.001(3) 0.011(3) 0.001(3) C28 0.044(4) 0.035(3) 0.028(3) -0.003(3) 0.006(3) 0.001(3) C29 0.055(5) 0.044(4) 0.034(4) -0.009(3) 0.011(3) 0.001(3) C30 0.067(5) 0.041(4) 0.034(4) 0.001(3) 0.004(4) 0.007(4) C31 0.072(6) 0.040(4) 0.034(4) 0.004(3) -0.008(4) 0.003(4) C32 0.080(6) 0.036(4) 0.033(4) 0.002(3) -0.001(4) -0.009(4) C37 0.064(5) 0.045(4) 0.026(3) -0.002(3) 0.005(3) -0.006(4) C38 0.078(6) 0.047(4) 0.033(4) 0.001(3) 0.009(4) 0.004(4) C39 0.053(5) 0.042(4) 0.054(5) 0.008(4) 0.024(4) 0.008(4) C40 0.051(5) 0.033(4) 0.050(4) 0.006(3) 0.004(4) 0.009(3) C41 0.047(4) 0.040(4) 0.037(4) 0.005(3) 0.006(3) 0.001(3) C42 0.063(5) 0.066(5) 0.030(4) -0.001(4) 0.008(4) 0.011(4) C43 0.076(6) 0.052(5) 0.035(4) -0.006(4) -0.003(4) 0.012(4) C44 0.063(5) 0.039(4) 0.050(5) -0.004(3) -0.021(4) 0.009(4) C45 0.052(5) 0.035(4) 0.047(4) -0.003(3) -0.006(4) 0.006(3) C46 0.054(5) 0.038(4) 0.037(4) -0.001(3) -0.002(3) 0.005(3) C47 0.045(4) 0.035(4) 0.061(5) 0.005(3) 0.006(4) -0.002(3) C48 0.054(5) 0.041(4) 0.075(6) -0.005(4) -0.003(4) 0.000(4) C49 0.050(6) 0.090(8) 0.138(12) -0.024(8) 0.017(7) -0.004(6) C50 0.059(6) 0.072(7) 0.120(11) -0.023(7) -0.003(7) -0.010(5) _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 N3 2.046(7) . ? Zn1 N1 2.072(6) . ? Zn1 Cl1 2.226(2) . ? Zn1 N2 2.291(6) . ? Zn1 N4 2.435(6) . ? Zn2 N5 2.108(6) . ? Zn2 N6 2.118(7) . ? Zn2 Cl2 2.196(3) . ? Zn2 Cl3 2.196(3) . ? Zn3 O1 1.991(15) . ? Zn3 Cl6' 2.158(17) . ? Zn3 Cl5 2.151(8) . ? Zn3 Cl4' 2.215(13) . ? Zn3 Cl6 2.218(11) . ? Zn3 Cl5' 2.304(14) . ? Zn3 Cl4 2.336(9) . ? S1 C12 1.740(8) . ? S1 C13 1.766(8) . ? S2 C12 1.740(8) . ? S2 C14 1.751(9) . ? S3 C13 1.761(9) . ? S3 C15 1.810(12) . ? S4 C14 1.747(8) . ? S4 C17 1.851(13) . ? S5 C30 1.742(9) . ? S5 C31 1.761(8) . ? S6 C30 1.725(8) . ? S6 C32 1.750(8) . ? S7 C31 1.743(8) . ? S7 C33' 1.801(17) . ? S7 C33 1.817(19) . ? S8 C32 1.745(8) . ? S8 C35 1.846(16) . ? S8 C35' 1.847(16) . ? S9 C48 1.724(10) . ? S9 C49 1.754(13) . ? S10 C48 1.746(10) . ? S10 C50 1.758(12) . ? S11 C49 1.751(13) . ? S11 C51' 1.814(18) . ? S11 C51 1.840(18) . ? S12 C50 1.733(12) . ? S12 C53 1.838(18) . ? S12 C53' 1.91(4) . ? O1 C55' 1.459(18) . ? O1 C55 1.477(18) . ? N1 C1 1.331(10) . ? N1 C5 1.343(8) . ? N2 C10 1.330(9) . ? N2 C6 1.365(10) . ? N3 C19 1.346(11) . ? N3 C23 1.349(9) . ? N4 C28 1.307(9) . ? N4 C24 1.339(10) . ? N5 C41 1.325(10) . ? N5 C37 1.339(9) . ? N6 C46 1.345(10) . ? N6 C42 1.358(10) . ? C1 C2 1.386(12) . ? C1 H1 0.9400 . ? C2 C3 1.373(11) . ? C2 H2 0.9400 . ? C3 C4 1.408(11) . ? C3 H3 0.9400 . ? C4 C5 1.407(10) . ? C4 C11 1.465(10) . ? C5 C10 1.396(10) . ? C6 C7 1.370(11) . ? C6 H6 0.9400 . ? C7 C8 1.390(12) . ? C7 H7 0.9400 . ? C8 C9 1.395(11) . ? C8 H8 0.9400 . ? C9 C10 1.403(9) . ? C9 C11 1.471(11) . ? C11 C12 1.380(10) . ? C13 C14 1.335(13) . ? C15 C16 1.482(16) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.519(14) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C20 1.397(13) . ? C19 H19 0.9400 . ? C20 C21 1.401(12) . ? C20 H20 0.9400 . ? C21 C22 1.383(12) . ? C21 H21 0.9400 . ? C22 C23 1.404(11) . ? C22 C29 1.486(10) . ? C23 C28 1.436(10) . ? C24 C25 1.387(11) . ? C24 H24 0.9400 . ? C25 C26 1.408(12) . ? C25 H25 0.9400 . ? C26 C27 1.398(11) . ? C26 H26 0.9400 . ? C27 C28 1.417(9) . ? C27 C29 1.470(11) . ? C29 C30 1.383(10) . ? C31 C32 1.336(12) . ? C33 C34 1.50(2) . ? C33' C34' 1.480(19) . ? C35 C36 1.501(17) . ? C35' C36' 1.484(17) . ? C37 C38 1.397(12) . ? C37 H37 0.9400 . ? C38 C39 1.366(12) . ? C38 H38 0.9400 . ? C39 C40 1.408(11) . ? C39 H39 0.9400 . ? C40 C41 1.401(11) . ? C40 C47 1.471(12) . ? C41 C46 1.428(10) . ? C42 C43 1.379(13) . ? C42 H42 0.9400 . ? C43 C44 1.395(13) . ? C43 H43 0.9400 . ? C44 C45 1.405(11) . ? C44 H44 0.9400 . ? C45 C46 1.392(11) . ? C45 C47 1.456(11) . ? C47 C48 1.380(12) . ? C49 C50 1.324(18) . ? C51 C52 1.512(19) . ? C51' C52' 1.497(19) . ? C53 C54 1.513(19) . ? C53' C54' 1.520(19) . ? C56 C56 0.85(5) 2_656 ? C56 O2 1.473(18) . ? C56' C56' 1.17(6) 2_656 ? C56' O2' 1.440(19) . ? 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 N3 Zn1 N1 124.2(3) . . ? N3 Zn1 Cl1 115.26(19) . . ? N1 Zn1 Cl1 120.44(18) . . ? N3 Zn1 N2 97.2(2) . . ? N1 Zn1 N2 81.9(2) . . ? Cl1 Zn1 N2 95.14(17) . . ? N3 Zn1 N4 80.6(2) . . ? N1 Zn1 N4 91.4(2) . . ? Cl1 Zn1 N4 94.38(15) . . ? N2 Zn1 N4 170.2(2) . . ? N5 Zn2 N6 85.3(2) . . ? N5 Zn2 Cl2 112.94(19) . . ? N6 Zn2 Cl2 109.8(2) . . ? N5 Zn2 Cl3 109.56(19) . . ? N6 Zn2 Cl3 112.7(2) . . ? Cl2 Zn2 Cl3 120.96(13) . . ? O1 Zn3 Cl6' 91.9(6) . . ? O1 Zn3 Cl5 112.4(5) . . ? Cl6' Zn3 Cl5 126.2(5) . . ? O1 Zn3 Cl4' 111.1(5) . . ? Cl6' Zn3 Cl4' 126.4(6) . . ? Cl5 Zn3 Cl4' 89.6(4) . . ? O1 Zn3 Cl6 103.6(5) . . ? Cl6' Zn3 Cl6 12.3(5) . . ? Cl5 Zn3 Cl6 122.7(4) . . ? Cl4' Zn3 Cl6 117.3(5) . . ? O1 Zn3 Cl5' 90.4(5) . . ? Cl6' Zn3 Cl5' 117.1(6) . . ? Cl5 Zn3 Cl5' 25.7(3) . . ? Cl4' Zn3 Cl5' 110.6(5) . . ? Cl6 Zn3 Cl5' 119.8(4) . . ? O1 Zn3 Cl4 97.4(5) . . ? Cl6' Zn3 Cl4 109.6(5) . . ? Cl5 Zn3 Cl4 113.5(3) . . ? Cl4' Zn3 Cl4 24.1(3) . . ? Cl6 Zn3 Cl4 103.9(4) . . ? Cl5' Zn3 Cl4 132.3(4) . . ? C12 S1 C13 96.4(4) . . ? C12 S2 C14 96.9(4) . . ? C13 S3 C15 103.5(5) . . ? C14 S4 C17 103.3(4) . . ? C30 S5 C31 95.9(4) . . ? C30 S6 C32 96.6(4) . . ? C31 S7 C33' 117.5(10) . . ? C31 S7 C33 101.2(11) . . ? C33' S7 C33 41.2(17) . . ? C32 S8 C35 101.1(9) . . ? C32 S8 C35' 102.1(9) . . ? C35 S8 C35' 9.5(16) . . ? C48 S9 C49 96.9(6) . . ? C48 S10 C50 96.3(6) . . ? C49 S11 C51' 105.5(14) . . ? C49 S11 C51 104.1(14) . . ? C51' S11 C51 25.5(14) . . ? C50 S12 C53 102.7(13) . . ? C50 S12 C53' 103.6(12) . . ? C53 S12 C53' 21.1(15) . . ? C55' O1 C55 21(3) . . ? C55' O1 Zn3 142(2) . . ? C55 O1 Zn3 120.5(19) . . ? C1 N1 C5 115.9(7) . . ? C1 N1 Zn1 135.5(5) . . ? C5 N1 Zn1 108.2(5) . . ? C10 N2 C6 115.2(6) . . ? C10 N2 Zn1 102.4(5) . . ? C6 N2 Zn1 141.8(5) . . ? C19 N3 C23 116.0(7) . . ? C19 N3 Zn1 133.3(5) . . ? C23 N3 Zn1 110.6(5) . . ? C28 N4 C24 115.9(6) . . ? C28 N4 Zn1 100.1(5) . . ? C24 N4 Zn1 143.4(5) . . ? C41 N5 C37 116.2(7) . . ? C41 N5 Zn2 104.9(5) . . ? C37 N5 Zn2 138.9(6) . . ? C46 N6 C42 114.7(7) . . ? C46 N6 Zn2 104.7(5) . . ? C42 N6 Zn2 140.6(6) . . ? N1 C1 C2 121.7(7) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 122.9(8) . . ? C3 C2 H2 118.5 . . ? C1 C2 H2 118.5 . . ? C2 C3 C4 116.8(7) . . ? C2 C3 H3 121.6 . . ? C4 C3 H3 121.6 . . ? C5 C4 C3 116.2(6) . . ? C5 C4 C11 106.9(7) . . ? C3 C4 C11 136.9(7) . . ? N1 C5 C10 123.7(7) . . ? N1 C5 C4 126.5(7) . . ? C10 C5 C4 109.8(6) . . ? N2 C6 C7 121.5(8) . . ? N2 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C6 C7 C8 122.8(8) . . ? C6 C7 H7 118.6 . . ? C8 C7 H7 118.6 . . ? C7 C8 C9 116.6(7) . . ? C7 C8 H8 121.7 . . ? C9 C8 H8 121.7 . . ? C8 C9 C10 116.7(7) . . ? C8 C9 C11 136.4(7) . . ? C10 C9 C11 106.9(6) . . ? N2 C10 C5 123.0(6) . . ? N2 C10 C9 127.1(7) . . ? C5 C10 C9 109.9(7) . . ? C12 C11 C4 126.9(7) . . ? C12 C11 C9 126.6(7) . . ? C4 C11 C9 106.4(6) . . ? C11 C12 S2 122.9(6) . . ? C11 C12 S1 123.7(6) . . ? S2 C12 S1 113.5(4) . . ? C14 C13 S3 125.7(6) . . ? C14 C13 S1 116.5(6) . . ? S3 C13 S1 117.3(6) . . ? C13 C14 S4 124.0(7) . . ? C13 C14 S2 116.7(6) . . ? S4 C14 S2 119.2(5) . . ? C16 C15 S3 108.9(9) . . ? C16 C15 H15A 109.9 . . ? S3 C15 H15A 109.9 . . ? C16 C15 H15B 109.9 . . ? S3 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 S4 106.9(9) . . ? C18 C17 H17A 110.3 . . ? S4 C17 H17A 110.3 . . ? C18 C17 H17B 110.3 . . ? S4 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 122.4(8) . . ? N3 C19 H19 118.8 . . ? C20 C19 H19 118.8 . . ? C19 C20 C21 120.4(9) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C22 C21 C20 118.2(8) . . ? C22 C21 H21 120.9 . . ? C20 C21 H21 120.9 . . ? C21 C22 C23 117.1(7) . . ? C21 C22 C29 136.2(8) . . ? C23 C22 C29 106.7(7) . . ? N3 C23 C22 125.8(7) . . ? N3 C23 C28 123.6(7) . . ? C22 C23 C28 110.6(6) . . ? N4 C24 C25 122.4(8) . . ? N4 C24 H24 118.8 . . ? C25 C24 H24 118.8 . . ? C24 C25 C26 121.0(8) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 117.3(7) . . ? C27 C26 H26 121.3 . . ? C25 C26 H26 121.3 . . ? C26 C27 C28 115.4(7) . . ? C26 C27 C29 136.5(7) . . ? C28 C27 C29 108.1(6) . . ? N4 C28 C27 128.0(7) . . ? N4 C28 C23 123.9(6) . . ? C27 C28 C23 108.0(6) . . ? C30 C29 C27 126.1(7) . . ? C30 C29 C22 127.3(8) . . ? C27 C29 C22 106.5(6) . . ? C29 C30 S6 123.8(7) . . ? C29 C30 S5 122.1(6) . . ? S6 C30 S5 114.1(4) . . ? C32 C31 S7 123.7(6) . . ? C32 C31 S5 116.5(6) . . ? S7 C31 S5 119.6(5) . . ? C31 C32 S8 123.9(6) . . ? C31 C32 S6 116.7(6) . . ? S8 C32 S6 118.9(6) . . ? C34 C33 S7 108(2) . . ? C34' C33' S7 79.0(17) . . ? C36 C35 S8 114.1(16) . . ? C36' C35' S8 108.4(15) . . ? N5 C37 C38 121.0(8) . . ? N5 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C39 C38 C37 122.1(7) . . ? C39 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? C38 C39 C40 118.1(7) . . ? C38 C39 H39 121.0 . . ? C40 C39 H39 121.0 . . ? C41 C40 C39 115.0(7) . . ? C41 C40 C47 106.4(7) . . ? C39 C40 C47 138.5(8) . . ? N5 C41 C40 127.5(7) . . ? N5 C41 C46 123.4(7) . . ? C40 C41 C46 109.1(7) . . ? N6 C42 C43 122.3(8) . . ? N6 C42 H42 118.8 . . ? C43 C42 H42 118.8 . . ? C42 C43 C44 121.2(8) . . ? C42 C43 H43 119.4 . . ? C44 C43 H43 119.4 . . ? C45 C44 C43 118.5(8) . . ? C45 C44 H44 120.8 . . ? C43 C44 H44 120.8 . . ? C44 C45 C46 114.9(8) . . ? C44 C45 C47 138.1(8) . . ? C46 C45 C47 106.8(7) . . ? N6 C46 C45 128.3(7) . . ? N6 C46 C41 121.7(7) . . ? C45 C46 C41 110.0(7) . . ? C48 C47 C45 127.9(8) . . ? C48 C47 C40 124.3(8) . . ? C45 C47 C40 107.6(7) . . ? C47 C48 S9 124.5(7) . . ? C47 C48 S10 122.2(7) . . ? S9 C48 S10 113.2(5) . . ? C50 C49 S11 124.5(10) . . ? C50 C49 S9 116.6(9) . . ? S11 C49 S9 118.8(9) . . ? C49 C50 S12 123.1(10) . . ? C49 C50 S10 116.5(9) . . ? S12 C50 S10 119.5(8) . . ? C52 C51 S11 120(2) . . ? C52' C51' S11 110(2) . . ? C54 C53 S12 120(2) . . ? C54' C53' S12 98(3) . . ? C56 C56 O2 137(4) 2_656 . ? C56' C56' O2' 174(7) 2_656 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl6' Zn3 O1 C55' 24(4) . . . . ? Cl5 Zn3 O1 C55' -107(4) . . . . ? Cl4' Zn3 O1 C55' 155(4) . . . . ? Cl6 Zn3 O1 C55' 28(4) . . . . ? Cl5' Zn3 O1 C55' -93(4) . . . . ? Cl4 Zn3 O1 C55' 134(4) . . . . ? Cl6' Zn3 O1 C55 25(3) . . . . ? Cl5 Zn3 O1 C55 -106(3) . . . . ? Cl4' Zn3 O1 C55 155(3) . . . . ? Cl6 Zn3 O1 C55 29(3) . . . . ? Cl5' Zn3 O1 C55 -92(3) . . . . ? Cl4 Zn3 O1 C55 135(3) . . . . ? N3 Zn1 N1 C1 -87.6(8) . . . . ? Cl1 Zn1 N1 C1 87.9(8) . . . . ? N2 Zn1 N1 C1 179.1(8) . . . . ? N4 Zn1 N1 C1 -8.1(8) . . . . ? N3 Zn1 N1 C5 99.8(5) . . . . ? Cl1 Zn1 N1 C5 -84.7(5) . . . . ? N2 Zn1 N1 C5 6.6(5) . . . . ? N4 Zn1 N1 C5 179.4(5) . . . . ? N3 Zn1 N2 C10 -131.0(5) . . . . ? N1 Zn1 N2 C10 -7.3(5) . . . . ? Cl1 Zn1 N2 C10 112.7(4) . . . . ? N4 Zn1 N2 C10 -54.7(15) . . . . ? N3 Zn1 N2 C6 59.1(9) . . . . ? N1 Zn1 N2 C6 -177.3(9) . . . . ? Cl1 Zn1 N2 C6 -57.2(9) . . . . ? N4 Zn1 N2 C6 135.4(13) . . . . ? N1 Zn1 N3 C19 -91.9(9) . . . . ? Cl1 Zn1 N3 C19 92.4(8) . . . . ? N2 Zn1 N3 C19 -6.8(9) . . . . ? N4 Zn1 N3 C19 -177.2(9) . . . . ? N1 Zn1 N3 C23 93.7(5) . . . . ? Cl1 Zn1 N3 C23 -82.0(5) . . . . ? N2 Zn1 N3 C23 178.8(5) . . . . ? N4 Zn1 N3 C23 8.4(5) . . . . ? N3 Zn1 N4 C28 -9.1(4) . . . . ? N1 Zn1 N4 C28 -133.5(5) . . . . ? Cl1 Zn1 N4 C28 105.9(4) . . . . ? N2 Zn1 N4 C28 -86.7(14) . . . . ? N3 Zn1 N4 C24 -178.4(9) . . . . ? N1 Zn1 N4 C24 57.2(9) . . . . ? Cl1 Zn1 N4 C24 -63.5(8) . . . . ? N2 Zn1 N4 C24 103.9(15) . . . . ? N6 Zn2 N5 C41 -0.4(5) . . . . ? Cl2 Zn2 N5 C41 109.1(5) . . . . ? Cl3 Zn2 N5 C41 -112.9(5) . . . . ? N6 Zn2 N5 C37 178.8(8) . . . . ? Cl2 Zn2 N5 C37 -71.7(8) . . . . ? Cl3 Zn2 N5 C37 66.3(8) . . . . ? N5 Zn2 N6 C46 0.8(5) . . . . ? Cl2 Zn2 N6 C46 -111.9(5) . . . . ? Cl3 Zn2 N6 C46 110.0(5) . . . . ? N5 Zn2 N6 C42 178.9(9) . . . . ? Cl2 Zn2 N6 C42 66.2(9) . . . . ? Cl3 Zn2 N6 C42 -71.8(9) . . . . ? C5 N1 C1 C2 -0.2(12) . . . . ? Zn1 N1 C1 C2 -172.3(6) . . . . ? N1 C1 C2 C3 1.2(14) . . . . ? C1 C2 C3 C4 -0.9(13) . . . . ? C2 C3 C4 C5 -0.3(11) . . . . ? C2 C3 C4 C11 179.9(9) . . . . ? C1 N1 C5 C10 -179.4(7) . . . . ? Zn1 N1 C5 C10 -5.2(8) . . . . ? C1 N1 C5 C4 -1.1(11) . . . . ? Zn1 N1 C5 C4 173.0(6) . . . . ? C3 C4 C5 N1 1.4(11) . . . . ? C11 C4 C5 N1 -178.8(7) . . . . ? C3 C4 C5 C10 179.9(7) . . . . ? C11 C4 C5 C10 -0.3(8) . . . . ? C10 N2 C6 C7 0.9(11) . . . . ? Zn1 N2 C6 C7 170.0(6) . . . . ? N2 C6 C7 C8 -0.6(13) . . . . ? C6 C7 C8 C9 -0.3(12) . . . . ? C7 C8 C9 C10 0.9(11) . . . . ? C7 C8 C9 C11 178.4(8) . . . . ? C6 N2 C10 C5 -179.6(7) . . . . ? Zn1 N2 C10 C5 7.3(8) . . . . ? C6 N2 C10 C9 -0.2(11) . . . . ? Zn1 N2 C10 C9 -173.4(6) . . . . ? N1 C5 C10 N2 -2.2(11) . . . . ? C4 C5 C10 N2 179.3(7) . . . . ? N1 C5 C10 C9 178.4(7) . . . . ? C4 C5 C10 C9 -0.2(9) . . . . ? C8 C9 C10 N2 -0.7(11) . . . . ? C11 C9 C10 N2 -178.9(7) . . . . ? C8 C9 C10 C5 178.8(7) . . . . ? C11 C9 C10 C5 0.6(8) . . . . ? C5 C4 C11 C12 -179.6(7) . . . . ? C3 C4 C11 C12 0.2(14) . . . . ? C5 C4 C11 C9 0.6(8) . . . . ? C3 C4 C11 C9 -179.6(9) . . . . ? C8 C9 C11 C12 1.8(14) . . . . ? C10 C9 C11 C12 179.5(7) . . . . ? C8 C9 C11 C4 -178.4(8) . . . . ? C10 C9 C11 C4 -0.7(8) . . . . ? C4 C11 C12 S2 -179.9(6) . . . . ? C9 C11 C12 S2 -0.1(11) . . . . ? C4 C11 C12 S1 1.6(11) . . . . ? C9 C11 C12 S1 -178.6(6) . . . . ? C14 S2 C12 C11 179.8(7) . . . . ? C14 S2 C12 S1 -1.5(5) . . . . ? C13 S1 C12 C11 -179.8(7) . . . . ? C13 S1 C12 S2 1.6(5) . . . . ? C15 S3 C13 C14 122.3(9) . . . . ? C15 S3 C13 S1 -66.5(7) . . . . ? C12 S1 C13 C14 -1.0(7) . . . . ? C12 S1 C13 S3 -173.1(5) . . . . ? S3 C13 C14 S4 -4.7(11) . . . . ? S1 C13 C14 S4 -176.0(4) . . . . ? S3 C13 C14 S2 171.4(5) . . . . ? S1 C13 C14 S2 0.1(9) . . . . ? C17 S4 C14 C13 -160.3(8) . . . . ? C17 S4 C14 S2 23.7(7) . . . . ? C12 S2 C14 C13 0.9(7) . . . . ? C12 S2 C14 S4 177.2(5) . . . . ? C13 S3 C15 C16 178.8(10) . . . . ? C14 S4 C17 C18 175.5(10) . . . . ? C23 N3 C19 C20 3.6(14) . . . . ? Zn1 N3 C19 C20 -170.5(8) . . . . ? N3 C19 C20 C21 -2.2(17) . . . . ? C19 C20 C21 C22 1.3(16) . . . . ? C20 C21 C22 C23 -2.0(13) . . . . ? C20 C21 C22 C29 179.5(9) . . . . ? C19 N3 C23 C22 -4.5(12) . . . . ? Zn1 N3 C23 C22 170.9(7) . . . . ? C19 N3 C23 C28 177.2(8) . . . . ? Zn1 N3 C23 C28 -7.4(9) . . . . ? C21 C22 C23 N3 3.8(13) . . . . ? C29 C22 C23 N3 -177.3(7) . . . . ? C21 C22 C23 C28 -177.7(7) . . . . ? C29 C22 C23 C28 1.2(9) . . . . ? C28 N4 C24 C25 -1.4(11) . . . . ? Zn1 N4 C24 C25 166.9(6) . . . . ? N4 C24 C25 C26 0.8(12) . . . . ? C24 C25 C26 C27 0.3(12) . . . . ? C25 C26 C27 C28 -0.5(11) . . . . ? C25 C26 C27 C29 179.3(8) . . . . ? C24 N4 C28 C27 1.2(11) . . . . ? Zn1 N4 C28 C27 -171.8(6) . . . . ? C24 N4 C28 C23 -178.5(7) . . . . ? Zn1 N4 C28 C23 8.5(8) . . . . ? C26 C27 C28 N4 -0.3(11) . . . . ? C29 C27 C28 N4 179.9(7) . . . . ? C26 C27 C28 C23 179.5(7) . . . . ? C29 C27 C28 C23 -0.4(8) . . . . ? N3 C23 C28 N4 -2.2(12) . . . . ? C22 C23 C28 N4 179.2(7) . . . . ? N3 C23 C28 C27 178.0(7) . . . . ? C22 C23 C28 C27 -0.5(9) . . . . ? C26 C27 C29 C30 4.5(15) . . . . ? C28 C27 C29 C30 -175.7(7) . . . . ? C26 C27 C29 C22 -178.8(9) . . . . ? C28 C27 C29 C22 1.1(8) . . . . ? C21 C22 C29 C30 -6.1(16) . . . . ? C23 C22 C29 C30 175.3(8) . . . . ? C21 C22 C29 C27 177.2(10) . . . . ? C23 C22 C29 C27 -1.4(8) . . . . ? C27 C29 C30 S6 -3.1(12) . . . . ? C22 C29 C30 S6 -179.2(6) . . . . ? C27 C29 C30 S5 178.1(6) . . . . ? C22 C29 C30 S5 2.0(12) . . . . ? C32 S6 C30 C29 177.6(7) . . . . ? C32 S6 C30 S5 -3.6(5) . . . . ? C31 S5 C30 C29 -177.4(7) . . . . ? C31 S5 C30 S6 3.7(5) . . . . ? C33' S7 C31 C32 133.2(12) . . . . ? C33 S7 C31 C32 173.6(15) . . . . ? C33' S7 C31 S5 -51.5(11) . . . . ? C33 S7 C31 S5 -11.1(15) . . . . ? C30 S5 C31 C32 -2.4(7) . . . . ? C30 S5 C31 S7 -178.1(5) . . . . ? S7 C31 C32 S8 4.4(11) . . . . ? S5 C31 C32 S8 -171.1(4) . . . . ? S7 C31 C32 S6 175.7(4) . . . . ? S5 C31 C32 S6 0.2(9) . . . . ? C35 S8 C32 C31 -126.2(12) . . . . ? C35' S8 C32 C31 -135.8(11) . . . . ? C35 S8 C32 S6 62.7(10) . . . . ? C35' S8 C32 S6 53.1(10) . . . . ? C30 S6 C32 C31 2.0(7) . . . . ? C30 S6 C32 S8 173.8(5) . . . . ? C31 S7 C33 C34 -180(2) . . . . ? C33' S7 C33 C34 -61(2) . . . . ? C31 S7 C33' C34' 78(2) . . . . ? C33 S7 C33' C34' 3(3) . . . . ? C32 S8 C35 C36 -154.4(19) . . . . ? C35' S8 C35 C36 -57(9) . . . . ? C32 S8 C35' C36' -143.0(18) . . . . ? C35 S8 C35' C36' 132(11) . . . . ? C41 N5 C37 C38 2.1(11) . . . . ? Zn2 N5 C37 C38 -177.0(6) . . . . ? N5 C37 C38 C39 -2.1(12) . . . . ? C37 C38 C39 C40 0.3(12) . . . . ? C38 C39 C40 C41 1.2(10) . . . . ? C38 C39 C40 C47 -178.2(8) . . . . ? C37 N5 C41 C40 -0.6(11) . . . . ? Zn2 N5 C41 C40 178.8(6) . . . . ? C37 N5 C41 C46 -179.5(7) . . . . ? Zn2 N5 C41 C46 -0.1(8) . . . . ? C39 C40 C41 N5 -1.1(11) . . . . ? C47 C40 C41 N5 178.5(7) . . . . ? C39 C40 C41 C46 177.9(6) . . . . ? C47 C40 C41 C46 -2.5(8) . . . . ? C46 N6 C42 C43 -2.0(12) . . . . ? Zn2 N6 C42 C43 180.0(6) . . . . ? N6 C42 C43 C44 1.8(13) . . . . ? C42 C43 C44 C45 0.9(12) . . . . ? C43 C44 C45 C46 -2.9(10) . . . . ? C43 C44 C45 C47 -177.9(8) . . . . ? C42 N6 C46 C45 -0.5(12) . . . . ? Zn2 N6 C46 C45 178.2(7) . . . . ? C42 N6 C46 C41 -179.8(7) . . . . ? Zn2 N6 C46 C41 -1.1(8) . . . . ? C44 C45 C46 N6 2.9(12) . . . . ? C47 C45 C46 N6 179.4(7) . . . . ? C44 C45 C46 C41 -177.7(6) . . . . ? C47 C45 C46 C41 -1.2(8) . . . . ? N5 C41 C46 N6 0.9(12) . . . . ? C40 C41 C46 N6 -178.2(7) . . . . ? N5 C41 C46 C45 -178.5(7) . . . . ? C40 C41 C46 C45 2.4(9) . . . . ? C44 C45 C47 C48 -9.0(15) . . . . ? C46 C45 C47 C48 175.8(8) . . . . ? C44 C45 C47 C40 174.9(9) . . . . ? C46 C45 C47 C40 -0.3(8) . . . . ? C41 C40 C47 C48 -174.6(7) . . . . ? C39 C40 C47 C48 4.9(14) . . . . ? C41 C40 C47 C45 1.8(8) . . . . ? C39 C40 C47 C45 -178.8(8) . . . . ? C45 C47 C48 S9 179.0(6) . . . . ? C40 C47 C48 S9 -5.4(12) . . . . ? C45 C47 C48 S10 -3.3(12) . . . . ? C40 C47 C48 S10 172.2(6) . . . . ? C49 S9 C48 C47 -178.0(8) . . . . ? C49 S9 C48 S10 4.1(6) . . . . ? C50 S10 C48 C47 176.2(8) . . . . ? C50 S10 C48 S9 -5.9(6) . . . . ? C51' S11 C49 C50 120.8(16) . . . . ? C51 S11 C49 C50 147.1(16) . . . . ? C51' S11 C49 S9 -62.8(14) . . . . ? C51 S11 C49 S9 -36.5(14) . . . . ? C48 S9 C49 C50 0.1(11) . . . . ? C48 S9 C49 S11 -176.6(7) . . . . ? S11 C49 C50 S12 2.5(18) . . . . ? S9 C49 C50 S12 -173.9(7) . . . . ? S11 C49 C50 S10 172.1(7) . . . . ? S9 C49 C50 S10 -4.3(15) . . . . ? C53 S12 C50 C49 -143.2(16) . . . . ? C53' S12 C50 C49 -164.8(16) . . . . ? C53 S12 C50 S10 47.5(14) . . . . ? C53' S12 C50 S10 25.9(14) . . . . ? C48 S10 C50 C49 6.2(11) . . . . ? C48 S10 C50 S12 176.2(7) . . . . ? C49 S11 C51 C52 95(3) . . . . ? C51' S11 C51 C52 -168(7) . . . . ? C49 S11 C51' C52' 92(3) . . . . ? C51 S11 C51' C52' 2(4) . . . . ? C50 S12 C53 C54 -179(3) . . . . ? C53' S12 C53 C54 -84(5) . . . . ? C50 S12 C53' C54' 175(2) . . . . ? C53 S12 C53' C54' 85(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.947 _refine_diff_density_min -1.447 _refine_diff_density_rms 0.137 ########End data_6 _database_code_depnum_ccdc_archive 'CCDC 778144' #TrackingRef '- Zhu-R2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H32 Cl2 N4 O8 S8 Zn' _chemical_formula_weight 1041.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'P 21/a' _symmetry_space_group_name_Hall '-P 2yab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 9.982(5) _cell_length_b 14.264(6) _cell_length_c 14.747(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.191(7) _cell_angle_gamma 90.00 _cell_volume 2059.8(17) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7554 _exptl_absorpt_correction_T_max 0.9109 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10357 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4684 _reflns_number_gt 3448 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0452P)^2^+5.3734P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4684 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.1708 _refine_ls_wR_factor_gt 0.1530 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _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 0.0000 0.0000 0.0000 0.0298(2) Uani 1 2 d S . . Cl1 Cl -0.27101(15) -0.08083(10) -0.15090(12) 0.0463(4) Uani 1 1 d . . . S2 S 0.41983(14) 0.16958(10) -0.33403(11) 0.0365(3) Uani 1 1 d . . . S1 S 0.31776(14) 0.34353(9) -0.27058(10) 0.0349(3) Uani 1 1 d . . . S3 S 0.46272(17) 0.46510(12) -0.38721(14) 0.0568(5) Uani 1 1 d . . . S4 S 0.56506(15) 0.26215(13) -0.46892(11) 0.0485(4) Uani 1 1 d . . . O1 O -0.1823(4) -0.0071(3) -0.1074(3) 0.0459(11) Uani 1 1 d . . . O2 O -0.3636(4) -0.0416(3) -0.2273(3) 0.0567(12) Uani 1 1 d . . . O3 O -0.1829(7) -0.1488(4) -0.1846(5) 0.109(2) Uani 1 1 d . . . O4 O -0.3374(6) -0.1245(6) -0.0898(5) 0.125(3) Uani 1 1 d . . . N1 N 0.0333(4) 0.1429(3) -0.0403(3) 0.0304(10) Uani 1 1 d . . . N2 N 0.1314(4) -0.0323(3) -0.1015(3) 0.0340(10) Uani 1 1 d . . . C15 C 0.3019(8) 0.5223(5) -0.4169(7) 0.076(3) Uani 1 1 d . . . H15A H 0.2572 0.5204 -0.3633 0.091 Uiso 1 1 calc R . . H15B H 0.3175 0.5883 -0.4301 0.091 Uiso 1 1 calc R . . C16 C 0.2091(9) 0.4820(6) -0.4964(8) 0.111(4) Uani 1 1 d . . . H16A H 0.2479 0.4894 -0.5514 0.167 Uiso 1 1 calc R . . H16B H 0.1218 0.5141 -0.5051 0.167 Uiso 1 1 calc R . . H16C H 0.1960 0.4159 -0.4855 0.167 Uiso 1 1 calc R . . C18 C 0.5007(8) 0.2388(6) -0.6550(5) 0.073(2) Uani 1 1 d . . . H18A H 0.5646 0.2889 -0.6599 0.110 Uiso 1 1 calc R . . H18B H 0.4305 0.2371 -0.7106 0.110 Uiso 1 1 calc R . . H18C H 0.5488 0.1794 -0.6476 0.110 Uiso 1 1 calc R . . C11 C 0.2538(5) 0.1729(3) -0.2057(4) 0.0280(11) Uani 1 1 d . . . C10 C 0.1627(5) 0.0514(3) -0.1318(4) 0.0275(11) Uani 1 1 d . . . C12 C 0.3205(5) 0.2214(3) -0.2633(4) 0.0285(11) Uani 1 1 d . . . C4 C 0.1696(5) 0.2131(3) -0.1434(4) 0.0266(11) Uani 1 1 d . . . C3 C 0.1368(5) 0.3020(4) -0.1172(4) 0.0319(12) Uani 1 1 d . . . H3 H 0.1706 0.3557 -0.1422 0.038 Uiso 1 1 calc R . . C9 C 0.2495(5) 0.0701(3) -0.1938(4) 0.0278(11) Uani 1 1 d . . . C8 C 0.3124(5) -0.0070(4) -0.2259(4) 0.0345(12) Uani 1 1 d . . . H8 H 0.3735 0.0002 -0.2666 0.041 Uiso 1 1 calc R . . C1 C 0.0014(5) 0.2297(4) -0.0174(4) 0.0340(12) Uani 1 1 d . . . H1 H -0.0578 0.2371 0.0244 0.041 Uiso 1 1 calc R . . C7 C 0.2810(6) -0.0949(4) -0.1951(5) 0.0429(15) Uani 1 1 d . . . H7 H 0.3210 -0.1485 -0.2159 0.051 Uiso 1 1 calc R . . C5 C 0.1147(5) 0.1379(3) -0.1015(4) 0.0273(11) Uani 1 1 d . . . C13 C 0.4177(5) 0.3530(4) -0.3549(4) 0.0371(13) Uani 1 1 d . . . C14 C 0.4630(5) 0.2731(4) -0.3851(4) 0.0382(13) Uani 1 1 d . . . C2 C 0.0523(5) 0.3094(4) -0.0529(4) 0.0353(13) Uani 1 1 d . . . H2 H 0.0294 0.3690 -0.0332 0.042 Uiso 1 1 calc R . . C17 C 0.4359(7) 0.2559(6) -0.5729(5) 0.065(2) Uani 1 1 d . . . H17A H 0.3720 0.2050 -0.5674 0.078 Uiso 1 1 calc R . . H17B H 0.3844 0.3148 -0.5813 0.078 Uiso 1 1 calc R . . C6 C 0.1920(6) -0.1052(4) -0.1345(4) 0.0422(14) Uani 1 1 d . . . H6 H 0.1733 -0.1660 -0.1156 0.051 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0351(5) 0.0245(4) 0.0333(5) 0.0022(4) 0.0156(4) -0.0021(3) Cl1 0.0487(8) 0.0389(8) 0.0472(10) 0.0074(7) -0.0009(7) -0.0117(6) S2 0.0407(8) 0.0379(8) 0.0357(8) 0.0037(6) 0.0193(6) 0.0003(6) S1 0.0408(7) 0.0302(7) 0.0367(8) 0.0050(6) 0.0150(6) -0.0042(5) S3 0.0535(10) 0.0520(10) 0.0656(13) 0.0228(9) 0.0135(9) -0.0186(8) S4 0.0374(8) 0.0765(12) 0.0355(9) 0.0109(8) 0.0170(7) 0.0000(7) O1 0.045(2) 0.032(2) 0.055(3) 0.000(2) -0.004(2) -0.0071(17) O2 0.047(3) 0.062(3) 0.053(3) 0.011(2) -0.011(2) -0.003(2) O3 0.126(5) 0.072(4) 0.114(6) -0.038(4) -0.018(4) 0.045(4) O4 0.088(4) 0.184(7) 0.097(5) 0.076(5) -0.001(4) -0.069(4) N1 0.035(2) 0.026(2) 0.033(3) -0.0004(19) 0.0137(19) -0.0035(17) N2 0.038(2) 0.028(2) 0.038(3) 0.003(2) 0.014(2) -0.0037(19) C15 0.082(6) 0.037(4) 0.116(8) 0.026(5) 0.039(6) 0.003(4) C16 0.083(6) 0.081(7) 0.157(12) 0.061(7) -0.007(7) -0.011(5) C18 0.097(6) 0.078(6) 0.046(5) -0.010(4) 0.013(4) -0.009(5) C11 0.030(3) 0.025(3) 0.031(3) 0.004(2) 0.011(2) -0.0010(19) C10 0.028(2) 0.030(3) 0.025(3) 0.003(2) 0.007(2) 0.0007(19) C12 0.031(3) 0.028(3) 0.028(3) -0.003(2) 0.008(2) -0.003(2) C4 0.023(2) 0.027(3) 0.029(3) 0.003(2) 0.003(2) -0.0006(18) C3 0.033(3) 0.030(3) 0.033(3) 0.006(2) 0.007(2) -0.004(2) C9 0.027(2) 0.025(2) 0.032(3) 0.003(2) 0.008(2) -0.0032(19) C8 0.042(3) 0.028(3) 0.037(3) 0.003(2) 0.019(2) 0.004(2) C1 0.040(3) 0.032(3) 0.032(3) -0.001(2) 0.015(2) -0.001(2) C7 0.053(4) 0.030(3) 0.052(4) -0.003(3) 0.028(3) 0.004(3) C5 0.029(2) 0.030(3) 0.024(3) 0.004(2) 0.008(2) -0.0010(19) C13 0.034(3) 0.044(3) 0.034(3) 0.014(3) 0.007(2) -0.006(2) C14 0.031(3) 0.053(4) 0.035(3) 0.012(3) 0.015(2) -0.001(2) C2 0.044(3) 0.026(3) 0.039(3) -0.002(2) 0.015(3) 0.003(2) C17 0.063(4) 0.092(6) 0.043(5) -0.011(4) 0.016(4) -0.009(4) C6 0.058(4) 0.022(3) 0.051(4) 0.002(3) 0.023(3) 0.000(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 N1 2.166(4) 3 ? Zn1 N1 2.166(4) . ? Zn1 O1 2.170(4) 3 ? Zn1 O1 2.170(4) . ? Zn1 N2 2.221(4) 3 ? Zn1 N2 2.221(4) . ? Cl1 O4 1.368(5) . ? Cl1 O2 1.426(4) . ? Cl1 O1 1.443(4) . ? Cl1 O3 1.459(6) . ? S2 C12 1.738(5) . ? S2 C14 1.749(6) . ? S1 C13 1.744(5) . ? S1 C12 1.746(5) . ? S3 C13 1.751(6) . ? S3 C15 1.778(8) . ? S4 C14 1.754(5) . ? S4 C17 1.804(7) . ? N1 C5 1.327(6) . ? N1 C1 1.339(6) . ? N2 C10 1.334(6) . ? N2 C6 1.341(7) . ? C15 C16 1.464(13) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C18 C17 1.500(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C11 C12 1.365(7) . ? C11 C4 1.476(7) . ? C11 C9 1.479(7) . ? C10 C9 1.402(6) . ? C10 C5 1.427(7) . ? C4 C3 1.383(7) . ? C4 C5 1.402(6) . ? C3 C2 1.391(7) . ? C3 H3 0.9400 . ? C9 C8 1.393(7) . ? C8 C7 1.391(7) . ? C8 H8 0.9400 . ? C1 C2 1.388(7) . ? C1 H1 0.9400 . ? C7 C6 1.386(7) . ? C7 H7 0.9400 . ? C13 C14 1.335(8) . ? C2 H2 0.9400 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C6 H6 0.9400 . ? 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 N1 Zn1 N1 180.0(2) 3 . ? N1 Zn1 O1 89.73(16) 3 3 ? N1 Zn1 O1 90.27(16) . 3 ? N1 Zn1 O1 90.27(16) 3 . ? N1 Zn1 O1 89.73(16) . . ? O1 Zn1 O1 180.0(2) 3 . ? N1 Zn1 N2 82.43(16) 3 3 ? N1 Zn1 N2 97.57(16) . 3 ? O1 Zn1 N2 91.13(17) 3 3 ? O1 Zn1 N2 88.87(17) . 3 ? N1 Zn1 N2 97.57(16) 3 . ? N1 Zn1 N2 82.43(16) . . ? O1 Zn1 N2 88.87(17) 3 . ? O1 Zn1 N2 91.13(17) . . ? N2 Zn1 N2 180.00(18) 3 . ? O4 Cl1 O2 112.1(3) . . ? O4 Cl1 O1 111.9(4) . . ? O2 Cl1 O1 108.3(3) . . ? O4 Cl1 O3 108.8(5) . . ? O2 Cl1 O3 109.4(4) . . ? O1 Cl1 O3 106.1(3) . . ? C12 S2 C14 96.7(3) . . ? C13 S1 C12 96.7(3) . . ? C13 S3 C15 102.7(3) . . ? C14 S4 C17 100.7(3) . . ? Cl1 O1 Zn1 135.6(2) . . ? C5 N1 C1 115.3(4) . . ? C5 N1 Zn1 106.4(3) . . ? C1 N1 Zn1 138.1(3) . . ? C10 N2 C6 114.9(4) . . ? C10 N2 Zn1 104.4(3) . . ? C6 N2 Zn1 140.6(4) . . ? C16 C15 S3 114.7(6) . . ? C16 C15 H15A 108.6 . . ? S3 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? S3 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C11 C4 126.6(4) . . ? C12 C11 C9 127.2(5) . . ? C4 C11 C9 106.2(4) . . ? N2 C10 C9 127.2(5) . . ? N2 C10 C5 123.6(4) . . ? C9 C10 C5 109.2(4) . . ? C11 C12 S2 124.2(4) . . ? C11 C12 S1 122.7(4) . . ? S2 C12 S1 113.0(3) . . ? C3 C4 C5 116.4(5) . . ? C3 C4 C11 136.4(5) . . ? C5 C4 C11 107.2(4) . . ? C4 C3 C2 117.9(5) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C8 C9 C10 116.6(4) . . ? C8 C9 C11 135.8(4) . . ? C10 C9 C11 107.5(4) . . ? C7 C8 C9 117.1(5) . . ? C7 C8 H8 121.5 . . ? C9 C8 H8 121.5 . . ? N1 C1 C2 122.7(5) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C6 C7 C8 121.3(5) . . ? C6 C7 H7 119.3 . . ? C8 C7 H7 119.3 . . ? N1 C5 C4 127.0(5) . . ? N1 C5 C10 123.1(4) . . ? C4 C5 C10 109.8(4) . . ? C14 C13 S1 116.7(4) . . ? C14 C13 S3 124.6(4) . . ? S1 C13 S3 118.5(4) . . ? C13 C14 S2 116.7(4) . . ? C13 C14 S4 126.3(4) . . ? S2 C14 S4 117.0(3) . . ? C1 C2 C3 120.6(5) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C18 C17 S4 110.2(5) . . ? C18 C17 H17A 109.6 . . ? S4 C17 H17A 109.6 . . ? C18 C17 H17B 109.6 . . ? S4 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? N2 C6 C7 122.9(5) . . ? N2 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Cl1 O1 Zn1 64.4(5) . . . . ? O2 Cl1 O1 Zn1 -171.5(4) . . . . ? O3 Cl1 O1 Zn1 -54.2(5) . . . . ? N1 Zn1 O1 Cl1 -13.6(4) 3 . . . ? N1 Zn1 O1 Cl1 166.4(4) . . . . ? O1 Zn1 O1 Cl1 89(6) 3 . . . ? N2 Zn1 O1 Cl1 -96.0(4) 3 . . . ? N2 Zn1 O1 Cl1 84.0(4) . . . . ? N1 Zn1 N1 C5 -2(46) 3 . . . ? O1 Zn1 N1 C5 87.6(4) 3 . . . ? O1 Zn1 N1 C5 -92.4(4) . . . . ? N2 Zn1 N1 C5 178.8(4) 3 . . . ? N2 Zn1 N1 C5 -1.2(4) . . . . ? N1 Zn1 N1 C1 -177(50) 3 . . . ? O1 Zn1 N1 C1 -87.9(6) 3 . . . ? O1 Zn1 N1 C1 92.1(6) . . . . ? N2 Zn1 N1 C1 3.3(6) 3 . . . ? N2 Zn1 N1 C1 -176.7(6) . . . . ? N1 Zn1 N2 C10 -179.0(3) 3 . . . ? N1 Zn1 N2 C10 1.0(3) . . . . ? O1 Zn1 N2 C10 -89.4(3) 3 . . . ? O1 Zn1 N2 C10 90.6(3) . . . . ? N2 Zn1 N2 C10 47(100) 3 . . . ? N1 Zn1 N2 C6 -4.8(7) 3 . . . ? N1 Zn1 N2 C6 175.2(7) . . . . ? O1 Zn1 N2 C6 84.8(7) 3 . . . ? O1 Zn1 N2 C6 -95.2(7) . . . . ? N2 Zn1 N2 C6 -139(100) 3 . . . ? C13 S3 C15 C16 -64.0(7) . . . . ? C6 N2 C10 C9 0.6(8) . . . . ? Zn1 N2 C10 C9 176.6(5) . . . . ? C6 N2 C10 C5 -176.7(5) . . . . ? Zn1 N2 C10 C5 -0.7(6) . . . . ? C4 C11 C12 S2 179.2(4) . . . . ? C9 C11 C12 S2 -1.6(8) . . . . ? C4 C11 C12 S1 1.0(8) . . . . ? C9 C11 C12 S1 -179.8(4) . . . . ? C14 S2 C12 C11 178.5(5) . . . . ? C14 S2 C12 S1 -3.1(4) . . . . ? C13 S1 C12 C11 -179.2(5) . . . . ? C13 S1 C12 S2 2.5(3) . . . . ? C12 C11 C4 C3 -4.9(10) . . . . ? C9 C11 C4 C3 175.8(6) . . . . ? C12 C11 C4 C5 176.7(5) . . . . ? C9 C11 C4 C5 -2.6(6) . . . . ? C5 C4 C3 C2 -0.5(8) . . . . ? C11 C4 C3 C2 -178.9(6) . . . . ? N2 C10 C9 C8 -1.5(8) . . . . ? C5 C10 C9 C8 176.1(5) . . . . ? N2 C10 C9 C11 -179.4(5) . . . . ? C5 C10 C9 C11 -1.8(6) . . . . ? C12 C11 C9 C8 6.1(10) . . . . ? C4 C11 C9 C8 -174.6(6) . . . . ? C12 C11 C9 C10 -176.6(5) . . . . ? C4 C11 C9 C10 2.7(6) . . . . ? C10 C9 C8 C7 1.4(8) . . . . ? C11 C9 C8 C7 178.5(6) . . . . ? C5 N1 C1 C2 -1.6(8) . . . . ? Zn1 N1 C1 C2 173.6(4) . . . . ? C9 C8 C7 C6 -0.6(10) . . . . ? C1 N1 C5 C4 0.1(8) . . . . ? Zn1 N1 C5 C4 -176.6(4) . . . . ? C1 N1 C5 C10 178.0(5) . . . . ? Zn1 N1 C5 C10 1.3(6) . . . . ? C3 C4 C5 N1 1.0(8) . . . . ? C11 C4 C5 N1 179.8(5) . . . . ? C3 C4 C5 C10 -177.2(5) . . . . ? C11 C4 C5 C10 1.6(6) . . . . ? N2 C10 C5 N1 -0.5(8) . . . . ? C9 C10 C5 N1 -178.1(5) . . . . ? N2 C10 C5 C4 177.8(5) . . . . ? C9 C10 C5 C4 0.1(6) . . . . ? C12 S1 C13 C14 -0.6(5) . . . . ? C12 S1 C13 S3 -175.6(3) . . . . ? C15 S3 C13 C14 131.7(6) . . . . ? C15 S3 C13 S1 -53.7(5) . . . . ? S1 C13 C14 S2 -1.6(7) . . . . ? S3 C13 C14 S2 173.1(3) . . . . ? S1 C13 C14 S4 -179.9(3) . . . . ? S3 C13 C14 S4 -5.2(8) . . . . ? C12 S2 C14 C13 2.9(5) . . . . ? C12 S2 C14 S4 -178.6(3) . . . . ? C17 S4 C14 C13 -88.7(6) . . . . ? C17 S4 C14 S2 92.9(4) . . . . ? N1 C1 C2 C3 2.1(9) . . . . ? C4 C3 C2 C1 -0.9(8) . . . . ? C14 S4 C17 C18 -175.7(6) . . . . ? C10 N2 C6 C7 0.3(9) . . . . ? Zn1 N2 C6 C7 -173.5(5) . . . . ? C8 C7 C6 N2 -0.3(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1 O4 0.94 2.51 3.241(7) 134.5 2_455 C15 H15A O2 0.98 2.55 3.524(10) 171.5 4_665 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.750 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.094 ########End