# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2004 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Dipankar Datta' 'Michael G. B. Brew' 'Kiranmoy Chowdhury' 'Shubhamoy Chowdhury' 'Derek A. Tocher' _publ_contact_author_name 'Dr Dipankar Datta' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science Calcutta 700 032 INDIA ; _publ_contact_author_email ICDD@MAHENDRA.IACS.RES.IN _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Zinc(II) mediated synthesis of an N-substituted 2-(2-pyridyl)-imidazole from a 1,2-diketone and 2-(aminomethyl)pyridine and its ligational behaviour ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands ; data_ZnL'Cl2_(1) _database_code_depnum_ccdc_archive 'CCDC 222262' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H20 Cl2 N4 Zn' _chemical_formula_weight 524.73 _chemical_melting_point ? _chemical_compound_source ? 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' Cl Cl 0.1484 0.1585 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.777(3) _cell_length_b 10.409(2) _cell_length_c 15.932(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.05(3) _cell_angle_gamma 90.00 _cell_volume 2389.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9 _cell_measurement_theta_max 14 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method ? _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.273 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.95 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nicolet R3mV' _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1% _diffrn_reflns_number 4188 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4188 _reflns_number_observed 2960 _reflns_observed_criterion >2sigma(I) _computing_data_collection P3 _computing_cell_refinement P3 _computing_data_reduction XDISK _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _computing_publication_material CIFTAB _refine_special_details ; Refinement on F^2^ for ALL reflections except for 54 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0667P)^2^+3.0039P] 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 fixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4134 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1102 _refine_ls_R_factor_obs 0.0464 _refine_ls_wR_factor_all 0.3237 _refine_ls_wR_factor_obs 0.1135 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 0.974 _refine_ls_restrained_S_all 2.303 _refine_ls_restrained_S_obs 0.974 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.12282(3) 0.19518(5) 0.03505(4) 0.0423(2) Uani 1 d . . Cl1 Cl 0.16242(9) 0.02148(12) -0.01968(10) 0.0653(4) Uani 1 d . . Cl2 Cl 0.11138(9) 0.18079(14) 0.16831(9) 0.0615(4) Uani 1 d . . N1 N 0.0048(2) 0.2804(4) -0.0613(2) 0.0436(9) Uani 1 d . . N2 N 0.1768(2) 0.3638(3) 0.0158(2) 0.0369(8) Uani 1 d . . N3 N 0.1544(2) 0.5549(3) -0.0491(3) 0.0418(8) Uani 1 d . . N4 N 0.1408(3) 0.5405(5) -0.2278(3) 0.0706(13) Uani 1 d . . C1 C -0.0795(3) 0.2263(5) -0.0989(4) 0.0560(13) Uani 1 d . . H1A H -0.0862(3) 0.1390(5) -0.0831(4) 0.080 Uiso 1 d R . C2 C -0.1560(3) 0.2912(5) -0.1589(4) 0.0583(13) Uani 1 d . . H2A H -0.2154(3) 0.2496(5) -0.1859(4) 0.080 Uiso 1 d R . C3 C -0.1462(3) 0.4133(6) -0.1787(3) 0.0608(14) Uani 1 d . . H3A H -0.1991(3) 0.4604(6) -0.2198(3) 0.080 Uiso 1 d R . C4 C -0.0599(3) 0.4729(5) -0.1413(3) 0.0562(13) Uani 1 d . . H4A H -0.0524(3) 0.5609(5) -0.1550(3) 0.080 Uiso 1 d R . C5 C 0.0155(3) 0.4031(4) -0.0838(3) 0.0388(9) Uani 1 d . . C6 C 0.1135(3) 0.4435(4) -0.0409(3) 0.0359(9) Uani 1 d . . C7 C 0.1170(3) 0.6631(5) -0.1116(4) 0.0587(14) Uani 1 d . . H7A H 0.1414(3) 0.7416(5) -0.0790(4) 0.080 Uiso 1 d R . H7B H 0.0507(3) 0.6651(5) -0.1329(4) 0.080 Uiso 1 d R . C8 C 0.1423(3) 0.6553(5) -0.1937(4) 0.0537(12) Uani 1 d . . C9 C 0.1682(5) 0.7637(7) -0.2261(4) 0.083(2) Uani 1 d . . H9A H 0.1673(5) 0.8465(7) -0.2000(4) 0.080 Uiso 1 d R . C10 C 0.1941(6) 0.7509(10) -0.2994(5) 0.120(3) Uani 1 d . . H10A H 0.2101(6) 0.8252(10) -0.3256(5) 0.080 Uiso 1 d R . C11 C 0.1942(6) 0.6301(12) -0.3348(5) 0.119(3) Uani 1 d . . H11A H 0.2164(6) 0.6170(12) -0.3820(5) 0.080 Uiso 1 d R . C12 C 0.1662(5) 0.5314(8) -0.2981(5) 0.097(2) Uani 1 d . . H12A H 0.1627(5) 0.4480(8) -0.3251(5) 0.080 Uiso 1 d R . C13 C 0.2487(3) 0.5426(4) 0.0039(3) 0.0392(9) Uani 1 d . . C14 C 0.3185(3) 0.6386(4) 0.0064(3) 0.0425(10) Uani 1 d . . C15 C 0.3833(3) 0.6038(5) -0.0274(3) 0.0525(12) Uani 1 d . . H15A H 0.3805(3) 0.5198(5) -0.0533(3) 0.080 Uiso 1 d R . C16 C 0.4500(4) 0.6896(6) -0.0253(4) 0.072(2) Uani 1 d . . H16A H 0.4956(4) 0.6635(6) -0.0474(4) 0.080 Uiso 1 d R . C17 C 0.4519(4) 0.8095(6) 0.0079(5) 0.078(2) Uani 1 d . . H17A H 0.4988(4) 0.8692(6) 0.0092(5) 0.080 Uiso 1 d R . C18 C 0.3881(5) 0.8464(6) 0.0405(6) 0.105(3) Uani 1 d . . H18A H 0.3905(5) 0.9310(6) 0.0654(6) 0.080 Uiso 1 d R . C19 C 0.3198(4) 0.7599(5) 0.0384(5) 0.074(2) Uani 1 d . . H19A H 0.2729(4) 0.7869(5) 0.0584(5) 0.080 Uiso 1 d R . C20 C 0.2612(3) 0.4244(4) 0.0450(3) 0.0369(9) Uani 1 d . . C21 C 0.3483(3) 0.3669(4) 0.1106(3) 0.0386(9) Uani 1 d . . C22 C 0.3662(3) 0.2368(4) 0.1083(3) 0.0424(10) Uani 1 d . . H22A H 0.3209(3) 0.1818(4) 0.0643(3) 0.080 Uiso 1 d R . C23 C 0.4501(3) 0.1864(5) 0.1694(3) 0.0509(11) Uani 1 d . . H23A H 0.4626(3) 0.0965(5) 0.1672(3) 0.080 Uiso 1 d R . C24 C 0.5155(3) 0.2621(6) 0.2329(4) 0.0584(13) Uani 1 d . . H24A H 0.5731(3) 0.2252(6) 0.2744(4) 0.080 Uiso 1 d R . C25 C 0.4976(4) 0.3904(6) 0.2361(4) 0.0644(14) Uani 1 d . . H25A H 0.5437(4) 0.4433(6) 0.2813(4) 0.080 Uiso 1 d R . C26 C 0.4145(3) 0.4440(5) 0.1765(3) 0.0505(11) Uani 1 d . . H26A H 0.4028(3) 0.5339(5) 0.1799(3) 0.080 Uiso 1 d 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 0.0409(3) 0.0403(3) 0.0458(3) 0.0094(2) 0.0178(2) 0.0004(2) Cl1 0.0690(8) 0.0436(6) 0.0822(9) -0.0045(6) 0.0298(7) 0.0025(6) Cl2 0.0544(7) 0.0827(9) 0.0499(7) 0.0251(6) 0.0238(6) 0.0082(6) N1 0.039(2) 0.053(2) 0.037(2) 0.007(2) 0.014(2) -0.001(2) N2 0.038(2) 0.036(2) 0.040(2) 0.003(2) 0.020(2) 0.0001(15) N3 0.042(2) 0.034(2) 0.057(2) 0.009(2) 0.027(2) 0.0055(15) N4 0.083(3) 0.070(3) 0.058(3) 0.001(2) 0.028(3) 0.007(3) C1 0.050(3) 0.062(3) 0.057(3) 0.005(2) 0.024(2) -0.012(2) C2 0.038(2) 0.078(4) 0.054(3) 0.002(3) 0.013(2) -0.006(2) C3 0.042(3) 0.081(4) 0.047(3) -0.002(3) 0.005(2) 0.009(3) C4 0.047(3) 0.052(3) 0.057(3) 0.011(2) 0.009(2) 0.011(2) C5 0.042(2) 0.046(2) 0.031(2) 0.001(2) 0.018(2) 0.001(2) C6 0.041(2) 0.039(2) 0.030(2) 0.002(2) 0.017(2) 0.000(2) C7 0.053(3) 0.046(3) 0.088(4) 0.025(3) 0.039(3) 0.015(2) C8 0.044(3) 0.052(3) 0.059(3) 0.015(2) 0.014(2) 0.001(2) C9 0.107(5) 0.077(4) 0.063(4) 0.020(3) 0.033(4) -0.014(4) C10 0.155(8) 0.142(8) 0.059(4) 0.022(5) 0.039(5) -0.054(7) C11 0.115(6) 0.195(10) 0.058(4) 0.006(6) 0.046(4) -0.015(7) C12 0.112(6) 0.100(6) 0.076(5) -0.001(4) 0.034(4) 0.016(5) C13 0.039(2) 0.040(2) 0.046(2) 0.003(2) 0.025(2) 0.002(2) C14 0.041(2) 0.037(2) 0.054(3) 0.006(2) 0.024(2) 0.003(2) C15 0.050(3) 0.052(3) 0.064(3) 0.007(2) 0.033(2) 0.000(2) C16 0.060(3) 0.077(4) 0.097(5) 0.022(3) 0.051(3) 0.000(3) C17 0.061(3) 0.073(4) 0.098(5) 0.013(4) 0.031(3) -0.017(3) C18 0.115(6) 0.045(3) 0.179(8) -0.019(4) 0.084(6) -0.023(4) C19 0.082(4) 0.049(3) 0.115(5) -0.012(3) 0.066(4) -0.009(3) C20 0.037(2) 0.037(2) 0.044(2) -0.001(2) 0.024(2) -0.001(2) C21 0.039(2) 0.041(2) 0.040(2) 0.005(2) 0.021(2) 0.001(2) C22 0.043(2) 0.048(2) 0.036(2) -0.003(2) 0.015(2) -0.003(2) C23 0.051(3) 0.056(3) 0.045(3) 0.013(2) 0.018(2) 0.009(2) C24 0.044(3) 0.079(4) 0.048(3) 0.013(3) 0.016(2) 0.007(3) C25 0.056(3) 0.078(4) 0.047(3) 0.001(3) 0.008(2) -0.011(3) C26 0.055(3) 0.047(3) 0.049(3) -0.006(2) 0.021(2) -0.006(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 N2 2.028(3) . ? Zn1 N1 2.069(4) . ? Zn1 Cl1 2.2055(14) . ? Zn1 Cl2 2.2079(14) . ? N1 C1 1.339(6) . ? N1 C5 1.355(5) . ? N2 C6 1.329(5) . ? N2 C20 1.372(5) . ? N3 C6 1.359(5) . ? N3 C13 1.386(5) . ? N3 C7 1.460(5) . ? N4 C8 1.309(7) . ? N4 C12 1.338(9) . ? C1 C2 1.374(7) . ? C2 C3 1.334(7) . ? C3 C4 1.389(7) . ? C4 C5 1.377(6) . ? C5 C6 1.474(6) . ? C7 C8 1.516(7) . ? C8 C9 1.372(7) . ? C9 C10 1.391(10) . ? C10 C11 1.379(13) . ? C11 C12 1.343(11) . ? C13 C20 1.369(6) . ? C13 C14 1.475(6) . ? C14 C19 1.359(7) . ? C14 C15 1.384(6) . ? C15 C16 1.370(7) . ? C16 C17 1.351(8) . ? C17 C18 1.362(9) . ? C18 C19 1.394(8) . ? C20 C21 1.472(6) . ? C21 C26 1.395(6) . ? C21 C22 1.387(6) . ? C22 C23 1.387(6) . ? C23 C24 1.363(7) . ? C24 C25 1.371(8) . ? C25 C26 1.384(7) . ? 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 N2 Zn1 N1 79.82(14) . . ? N2 Zn1 Cl1 116.44(10) . . ? N1 Zn1 Cl1 111.87(11) . . ? N2 Zn1 Cl2 114.11(10) . . ? N1 Zn1 Cl2 109.93(11) . . ? Cl1 Zn1 Cl2 118.16(6) . . ? C1 N1 C5 119.1(4) . . ? C1 N1 Zn1 125.5(3) . . ? C5 N1 Zn1 115.3(3) . . ? C6 N2 C20 107.4(3) . . ? C6 N2 Zn1 113.4(3) . . ? C20 N2 Zn1 139.1(3) . . ? C6 N3 C13 107.2(3) . . ? C6 N3 C7 130.4(4) . . ? C13 N3 C7 121.5(4) . . ? C8 N4 C12 116.9(6) . . ? N1 C1 C2 122.3(5) . . ? C3 C2 C1 118.6(5) . . ? C2 C3 C4 120.8(5) . . ? C5 C4 C3 118.7(5) . . ? N1 C5 C4 120.4(4) . . ? N1 C5 C6 111.5(3) . . ? C4 C5 C6 128.1(4) . . ? N2 C6 N3 110.1(3) . . ? N2 C6 C5 119.5(4) . . ? N3 C6 C5 130.4(4) . . ? N3 C7 C8 111.8(4) . . ? N4 C8 C9 123.5(5) . . ? N4 C8 C7 116.2(4) . . ? C9 C8 C7 120.3(5) . . ? C8 C9 C10 118.2(7) . . ? C9 C10 C11 118.7(7) . . ? C12 C11 C10 117.7(7) . . ? N4 C12 C11 125.0(8) . . ? C20 C13 N3 106.5(3) . . ? C20 C13 C14 129.5(4) . . ? N3 C13 C14 123.9(4) . . ? C19 C14 C15 119.2(4) . . ? C19 C14 C13 122.5(4) . . ? C15 C14 C13 118.3(4) . . ? C16 C15 C14 120.1(5) . . ? C15 C16 C17 120.4(5) . . ? C18 C17 C16 120.5(5) . . ? C17 C18 C19 119.5(6) . . ? C14 C19 C18 120.2(5) . . ? C13 C20 N2 108.7(4) . . ? C13 C20 C21 127.9(4) . . ? N2 C20 C21 123.4(3) . . ? C26 C21 C22 118.9(4) . . ? C26 C21 C20 119.8(4) . . ? C22 C21 C20 121.3(4) . . ? C23 C22 C21 119.8(4) . . ? C24 C23 C22 121.3(5) . . ? C23 C24 C25 119.0(5) . . ? C24 C25 C26 121.2(5) . . ? C21 C26 C25 119.7(5) . . ? _refine_diff_density_max 0.367 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.076 #===END data_[Zn(L')2](ClO4)2.1/2H2O.1/2CH2Cl2_(2) _database_code_depnum_ccdc_archive 'CCDC 222263' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C52.50 H42 Cl3 N8 O8.50 Zn' _chemical_formula_weight 1092.66 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' 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' 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 tetragonal _symmetry_space_group_name_H-M P41212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' 'y, x, -z' '-y, -x, -z+1/2' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' _cell_length_a 16.513(18) _cell_length_b 16.513(18) _cell_length_c 39.02(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10640(20) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4496 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2 intervals, counting time 5 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25096 _diffrn_reflns_av_R_equivalents 0.1285 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 20.91 _reflns_number_total 5426 _reflns_number_gt 4806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 w=1/[\s^2^(Fo^2^)+(0.0162P)^2^+129.6492P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(5) _refine_ls_number_reflns 5426 _refine_ls_number_parameters 341 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1336 _refine_ls_R_factor_gt 0.1177 _refine_ls_wR_factor_ref 0.2402 _refine_ls_wR_factor_gt 0.2299 _refine_ls_goodness_of_fit_ref 1.243 _refine_ls_restrained_S_all 1.250 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.21563(10) 0.84227(10) 0.09700(4) 0.0287(4) Uani 1 d . . . N11 N 0.2617(7) 0.7622(7) 0.0592(3) 0.039(3) Uiso 1 d . . . C12 C 0.3419(10) 0.7553(9) 0.0514(4) 0.040(4) Uiso 1 d . . . H12 H 0.3806 0.7823 0.0644 0.048 Uiso 1 calc R . . C13 C 0.3655(10) 0.7068(10) 0.0234(4) 0.046(4) Uiso 1 d . . . H13 H 0.4196 0.7048 0.0169 0.055 Uiso 1 calc R . . C14 C 0.3097(10) 0.6634(11) 0.0060(4) 0.051(5) Uiso 1 d . . . H14 H 0.3254 0.6275 -0.0111 0.061 Uiso 1 calc R . . C15 C 0.2273(10) 0.6732(9) 0.0142(4) 0.042(4) Uiso 1 d . . . H15 H 0.1883 0.6456 0.0016 0.051 Uiso 1 calc R . . C16 C 0.2034(8) 0.7235(8) 0.0410(3) 0.027(3) Uiso 1 d . . . N23 N 0.0480(7) 0.7170(7) 0.0396(3) 0.032(3) Uiso 1 d . . . C24 C -0.0091(10) 0.7562(10) 0.0574(4) 0.042(4) Uiso 1 d . . . C25 C 0.0286(9) 0.8074(9) 0.0797(4) 0.033(4) Uiso 1 d . . . C26 C 0.1211(10) 0.7431(10) 0.0519(4) 0.039(4) Uiso 1 d . . . N21 N 0.1087(7) 0.7985(8) 0.0763(3) 0.040(3) Uiso 1 d . . . C31 C -0.1028(11) 0.7461(11) 0.0522(5) 0.059(5) Uiso 1 d . . . C32 C -0.1484(11) 0.8123(11) 0.0437(4) 0.058(5) Uiso 1 d . . . H32 H -0.1225 0.8617 0.0404 0.069 Uiso 1 calc R . . C33 C -0.2348(12) 0.8085(13) 0.0397(5) 0.073(6) Uiso 1 d . . . H33 H -0.2663 0.8538 0.0349 0.088 Uiso 1 calc R . . C34 C -0.2677(15) 0.7310(14) 0.0436(5) 0.087(7) Uiso 1 d . . . H34 H -0.3230 0.7250 0.0400 0.104 Uiso 1 calc R . . C35 C -0.2269(14) 0.6668(15) 0.0519(5) 0.088(7) Uiso 1 d . . . H35 H -0.2534 0.6179 0.0556 0.105 Uiso 1 calc R . . C36 C -0.1402(12) 0.6720(12) 0.0553(5) 0.067(6) Uiso 1 d . . . H36 H -0.1098 0.6256 0.0595 0.080 Uiso 1 calc R . . C41 C -0.0144(10) 0.8663(9) 0.1042(4) 0.041(4) Uiso 1 d . . . C42 C -0.0017(11) 0.9474(11) 0.1012(5) 0.062(5) Uiso 1 d . . . H42 H 0.0336 0.9686 0.0849 0.075 Uiso 1 calc R . . C43 C -0.0463(14) 0.9990(15) 0.1247(6) 0.091(7) Uiso 1 d . . . H43 H -0.0408 1.0550 0.1236 0.109 Uiso 1 calc R . . C44 C -0.0930(14) 0.9667(15) 0.1470(6) 0.093(7) Uiso 1 d . . . H44 H -0.1203 1.0020 0.1615 0.111 Uiso 1 calc R . . C45 C -0.1071(15) 0.8880(15) 0.1517(7) 0.102(8) Uiso 1 d . . . H45 H -0.1412 0.8691 0.1688 0.122 Uiso 1 calc R . . C46 C -0.0661(11) 0.8343(13) 0.1286(5) 0.067(6) Uiso 1 d . . . H46 H -0.0743 0.7786 0.1300 0.081 Uiso 1 calc R . . C51 C 0.0337(11) 0.6579(11) 0.0120(4) 0.056(5) Uiso 1 d . . . H51A H 0.0697 0.6121 0.0151 0.068 Uiso 1 calc R . . H51B H -0.0216 0.6382 0.0135 0.068 Uiso 1 calc R . . C52 C 0.0466(12) 0.6922(12) -0.0215(5) 0.065(5) Uiso 1 d . . . N53 N 0.0624(12) 0.6323(12) -0.0459(5) 0.101(6) Uiso 1 d . . . C54 C 0.0767(17) 0.661(2) -0.0775(8) 0.135(10) Uiso 1 d . . . H54 H 0.0909 0.6244 -0.0945 0.162 Uiso 1 calc R . . C55 C 0.0716(18) 0.7418(19) -0.0863(8) 0.139(11) Uiso 1 d . . . H55 H 0.0755 0.7573 -0.1091 0.166 Uiso 1 calc R . . C56 C 0.0610(17) 0.7978(19) -0.0619(7) 0.126(10) Uiso 1 d . . . H56 H 0.0619 0.8528 -0.0670 0.151 Uiso 1 calc R . . C57 C 0.0491(13) 0.7713(14) -0.0300(6) 0.082(6) Uiso 1 d . . . H57 H 0.0421 0.8095 -0.0127 0.098 Uiso 1 calc R . . N101 N 0.3273(7) 0.4142(7) 0.1122(3) 0.029(3) Uiso 1 d . . . C102 C 0.3133(8) 0.4968(8) 0.1147(3) 0.022(3) Uiso 1 d . . . C103 C 0.3471(10) 0.5527(10) 0.0932(4) 0.050(4) Uiso 1 d . . . H103 H 0.3384 0.6080 0.0958 0.060 Uiso 1 calc R . . C104 C 0.3948(9) 0.5218(10) 0.0673(4) 0.040(4) Uiso 1 d . . . H104 H 0.4199 0.5580 0.0524 0.049 Uiso 1 calc R . . C105 C 0.4070(10) 0.4419(10) 0.0625(4) 0.047(5) Uiso 1 d . . . H105 H 0.4371 0.4224 0.0441 0.057 Uiso 1 calc R . . C106 C 0.3727(8) 0.3908(8) 0.0861(3) 0.025(4) Uiso 1 d . . . H106 H 0.3821 0.3356 0.0836 0.030 Uiso 1 calc R . . N81 N 0.3001(7) 0.7901(7) 0.1341(3) 0.031(3) Uiso 1 d . . . C82 C 0.2978(8) 0.7152(8) 0.1484(3) 0.030(4) Uiso 1 d . . . C83 C 0.3550(10) 0.6931(10) 0.1717(4) 0.051(5) Uiso 1 d . . . H83 H 0.3519 0.6426 0.1822 0.061 Uiso 1 calc R . . C84 C 0.4182(12) 0.7457(12) 0.1801(5) 0.071(6) Uiso 1 d . . . H84 H 0.4592 0.7300 0.1950 0.085 Uiso 1 calc R . . C85 C 0.4177(11) 0.8232(11) 0.1653(4) 0.057(5) Uiso 1 d . . . H85 H 0.4578 0.8607 0.1707 0.068 Uiso 1 calc R . . C86 C 0.3580(11) 0.8421(12) 0.1431(4) 0.059(5) Uiso 1 d . . . H86 H 0.3572 0.8939 0.1337 0.071 Uiso 1 calc R . . N91 N 0.2498(7) 0.4554(7) 0.1692(3) 0.027(3) Uiso 1 d . . . C92 C 0.2651(8) 0.5130(8) 0.1456(3) 0.030(4) Uiso 1 d . . . N93 N 0.2261(7) 0.5849(7) 0.1552(3) 0.034(3) Uiso 1 d . . . C94 C 0.1888(9) 0.5712(9) 0.1862(3) 0.032(4) Uiso 1 d . . . C95 C 0.2023(9) 0.4914(9) 0.1942(4) 0.035(4) Uiso 1 d . . . C87 C 0.2264(9) 0.6619(9) 0.1383(4) 0.033(4) Uiso 1 d . . . H87A H 0.1765 0.6901 0.1438 0.040 Uiso 1 calc R . . H87B H 0.2275 0.6532 0.1138 0.040 Uiso 1 calc R . . C111 C 0.1765(9) 0.4469(10) 0.2261(4) 0.041(4) Uiso 1 d . . . C112 C 0.2336(11) 0.4095(10) 0.2461(4) 0.047(4) Uiso 1 d . . . H112 H 0.2880 0.4101 0.2398 0.056 Uiso 1 calc R . . C113 C 0.2083(14) 0.3699(12) 0.2767(5) 0.076(6) Uiso 1 d . . . H113 H 0.2455 0.3444 0.2910 0.091 Uiso 1 calc R . . C114 C 0.1311(14) 0.3704(13) 0.2841(6) 0.081(7) Uiso 1 d . . . H114 H 0.1169 0.3455 0.3046 0.097 Uiso 1 calc R . . C115 C 0.0699(15) 0.4018(13) 0.2662(6) 0.088(7) Uiso 1 d . . . H115 H 0.0159 0.3957 0.2725 0.105 Uiso 1 calc R . . C116 C 0.0963(11) 0.4487(11) 0.2344(4) 0.059(5) Uiso 1 d . . . H116 H 0.0592 0.4773 0.2212 0.071 Uiso 1 calc R . . C121 C 0.1426(10) 0.6344(9) 0.2062(4) 0.041(4) Uiso 1 d . . . C122 C 0.0706(10) 0.6638(10) 0.1956(4) 0.050(5) Uiso 1 d . . . H122 H 0.0497 0.6458 0.1749 0.060 Uiso 1 calc R . . C123 C 0.0266(11) 0.7193(11) 0.2142(4) 0.056(5) Uiso 1 d . . . H123 H -0.0234 0.7378 0.2065 0.067 Uiso 1 calc R . . C124 C 0.0579(12) 0.7456(12) 0.2436(5) 0.067(6) Uiso 1 d . . . H124 H 0.0301 0.7844 0.2563 0.081 Uiso 1 calc R . . C125 C 0.1296(13) 0.7168(14) 0.2554(6) 0.091(7) Uiso 1 d . . . H125 H 0.1476 0.7337 0.2769 0.109 Uiso 1 calc R . . C126 C 0.1784(12) 0.6619(12) 0.2364(5) 0.068(6) Uiso 1 d . . . H126 H 0.2297 0.6457 0.2434 0.081 Uiso 1 calc R . . Cl1 Cl 0.5591(3) 0.5591(3) 0.0000 0.062(2) Uani 1 d S . . O11 O 0.4760(12) 0.5609(12) -0.0119(5) 0.136(7) Uiso 1 d . . . O12 O 0.6132(11) 0.5652(11) -0.0267(4) 0.113(6) Uiso 1 d . . . Cl2 Cl 0.0461(3) 0.5487(3) 0.10356(12) 0.0589(13) Uani 1 d . . . O21 O 0.0564(8) 0.5022(8) 0.1339(3) 0.071(4) Uiso 1 d . . . O22 O 0.1215(9) 0.5486(8) 0.0844(3) 0.082(4) Uiso 1 d . . . O23 O 0.0287(8) 0.6309(8) 0.1114(3) 0.081(4) Uiso 1 d . . . O24 O -0.0165(10) 0.5150(10) 0.0840(4) 0.101(5) Uiso 1 d . . . Cl3 Cl 0.0433(4) 0.0433(4) 0.0000 0.099(3) Uani 1 d SD . . O31 O -0.0065(16) 0.0808(17) 0.0277(6) 0.115(11) Uiso 0.50 d PD . . O33 O 0.019(2) 0.082(2) -0.0316(6) 0.181(19) Uiso 0.50 d PD . . O34 O 0.1271(12) 0.069(2) 0.0081(9) 0.19(2) Uiso 0.50 d PD . . O32 O 0.035(2) -0.0412(10) 0.0008(9) 0.19(2) Uiso 0.50 d PD . . C71 C -0.104(2) 0.3709(15) 0.1444(8) 0.107(17) Uiso 0.50 d PD . . Cl71 Cl -0.047(2) 0.330(3) 0.1779(9) 0.069(10) Uiso 0.17 d PD A 1 Cl72 Cl -0.147(3) 0.284(3) 0.1233(10) 0.115(15) Uiso 0.17 d PD A 1 Cl73 Cl -0.056(2) 0.361(2) 0.1859(7) 0.075(13) Uiso 0.17 d PD A 1 Cl74 Cl -0.099(4) 0.268(2) 0.1292(11) 0.134(18) Uiso 0.17 d PD A 1 Cl75 Cl -0.1870(19) 0.328(3) 0.1237(9) 0.093(12) Uiso 0.17 d PD A 1 Cl76 Cl -0.045(2) 0.292(3) 0.1604(16) 0.15(2) Uiso 0.17 d PD A 1 O100 O -0.049(2) 0.241(2) 0.1474(9) 0.102(11) Uiso 0.50 d P A 1 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 0.0341(11) 0.0212(9) 0.0309(8) -0.0011(8) 0.0013(8) -0.0004(9) Cl1 0.065(3) 0.065(3) 0.055(4) -0.029(3) 0.029(3) -0.005(4) Cl2 0.082(4) 0.034(3) 0.061(3) -0.012(2) -0.018(3) 0.005(2) Cl3 0.097(4) 0.097(4) 0.102(7) 0.002(4) -0.002(4) 0.019(6) _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 N91 2.053(11) 7 ? Zn1 N21 2.072(12) . ? Zn1 N101 2.110(11) 7 ? Zn1 N11 2.121(12) . ? Zn1 N81 2.186(11) . ? N11 C16 1.356(17) . ? N11 C12 1.364(19) . ? C12 C13 1.41(2) . ? C13 C14 1.35(2) . ? C14 C15 1.41(2) . ? C15 C16 1.391(19) . ? C16 C26 1.46(2) . ? N23 C24 1.339(19) . ? N23 C26 1.369(18) . ? N23 C51 1.472(19) . ? C24 C25 1.36(2) . ? C24 C31 1.57(2) . ? C25 N21 1.338(18) . ? C25 C41 1.54(2) . ? C26 N21 1.336(18) . ? C31 C32 1.37(2) . ? C31 C36 1.38(3) . ? C32 C33 1.44(3) . ? C33 C34 1.40(3) . ? C34 C35 1.30(3) . ? C35 C36 1.44(3) . ? C41 C42 1.36(2) . ? C41 C46 1.38(2) . ? C42 C43 1.45(3) . ? C43 C44 1.28(3) . ? C44 C45 1.33(3) . ? C45 C46 1.43(3) . ? C51 C52 1.44(2) . ? C52 C57 1.35(3) . ? C52 N53 1.40(2) . ? N53 C54 1.34(3) . ? C54 C55 1.38(4) . ? C55 C56 1.34(3) . ? C56 C57 1.33(3) . ? N101 C106 1.321(16) . ? N101 C102 1.388(17) . ? N101 Zn1 2.110(11) 7_545 ? C102 C103 1.37(2) . ? C102 C92 1.469(19) . ? C103 C104 1.38(2) . ? C104 C105 1.35(2) . ? C105 C106 1.37(2) . ? N81 C86 1.33(2) . ? N81 C82 1.356(17) . ? C82 C83 1.362(19) . ? C82 C87 1.523(19) . ? C83 C84 1.40(2) . ? C84 C85 1.40(2) . ? C85 C86 1.35(2) . ? N91 C92 1.346(17) . ? N91 C95 1.387(18) . ? N91 Zn1 2.053(11) 7_545 ? C92 N93 1.402(18) . ? N93 C94 1.377(17) . ? N93 C87 1.431(18) . ? C94 C95 1.37(2) . ? C94 C121 1.51(2) . ? C95 C111 1.51(2) . ? C111 C116 1.36(2) . ? C111 C112 1.37(2) . ? C112 C113 1.42(2) . ? C113 C114 1.31(3) . ? C114 C115 1.33(3) . ? C115 C116 1.52(3) . ? C121 C122 1.35(2) . ? C121 C126 1.39(2) . ? C122 C123 1.38(2) . ? C123 C124 1.33(2) . ? C124 C125 1.36(3) . ? C125 C126 1.42(3) . ? Cl1 O12 1.376(17) . ? Cl1 O12 1.376(17) 5 ? Cl1 O11 1.450(19) 5 ? Cl1 O11 1.450(19) . ? Cl2 O24 1.401(17) . ? Cl2 O21 1.423(13) . ? Cl2 O23 1.421(14) . ? Cl2 O22 1.452(14) . ? Cl3 O32 1.401(16) 5 ? Cl3 O32 1.401(16) . ? Cl3 O33 1.440(16) . ? Cl3 O33 1.441(16) 5 ? Cl3 O34 1.479(16) 5 ? Cl3 O34 1.479(16) . ? Cl3 O31 1.494(15) . ? Cl3 O31 1.494(15) 5 ? O31 O32 1.46(4) 5 ? O31 O33 1.78(3) 5 ? O33 O34 1.44(5) 5 ? O33 O32 1.74(4) 5 ? O33 O31 1.78(3) 5 ? O34 O33 1.44(5) 5 ? O34 O34 1.50(6) 5 ? O32 O31 1.46(4) 5 ? O32 O33 1.74(4) 5 ? O32 O32 1.79(6) 5 ? C71 Cl76 1.740(19) . ? C71 Cl75 1.737(19) . ? C71 Cl72 1.793(19) . ? C71 Cl74 1.80(2) . ? C71 Cl71 1.746(19) . ? C71 Cl73 1.810(19) . ? Cl71 Cl76 0.92(6) . ? Cl71 Cl73 0.62(5) . ? Cl71 O100 1.89(5) . ? Cl71 Cl74 2.31(4) . ? Cl72 Cl75 0.99(5) . ? Cl72 Cl74 0.87(6) . ? Cl72 Cl76 2.22(4) . ? Cl73 Cl76 1.52(6) . ? Cl74 O100 1.18(5) . ? Cl74 Cl76 1.56(6) . ? Cl74 Cl75 1.77(6) . ? Cl76 O100 0.99(6) . ? 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 N91 Zn1 N21 115.7(5) 7 . ? N91 Zn1 N101 79.2(4) 7 7 ? N21 Zn1 N101 101.8(5) . 7 ? N91 Zn1 N11 104.7(5) 7 . ? N21 Zn1 N11 79.4(5) . . ? N101 Zn1 N11 174.9(5) 7 . ? N91 Zn1 N81 112.7(4) 7 . ? N21 Zn1 N81 131.6(5) . . ? N101 Zn1 N81 86.4(4) 7 . ? N11 Zn1 N81 89.2(4) . . ? C16 N11 C12 122.1(12) . . ? C16 N11 Zn1 113.8(9) . . ? C12 N11 Zn1 123.8(10) . . ? N11 C12 C13 119.3(15) . . ? C14 C13 C12 120.2(16) . . ? C13 C14 C15 118.9(16) . . ? C16 C15 C14 120.9(15) . . ? N11 C16 C15 118.3(13) . . ? N11 C16 C26 113.8(12) . . ? C15 C16 C26 127.9(13) . . ? C24 N23 C26 106.7(12) . . ? C24 N23 C51 126.0(13) . . ? C26 N23 C51 127.3(13) . . ? N23 C24 C25 108.0(14) . . ? N23 C24 C31 125.1(14) . . ? C25 C24 C31 126.9(15) . . ? N21 C25 C24 108.8(14) . . ? N21 C25 C41 125.9(13) . . ? C24 C25 C41 125.3(14) . . ? N21 C26 N23 109.3(13) . . ? N21 C26 C16 120.1(13) . . ? N23 C26 C16 130.5(14) . . ? C25 N21 C26 107.2(13) . . ? C25 N21 Zn1 140.0(11) . . ? C26 N21 Zn1 112.8(10) . . ? C32 C31 C36 119.0(18) . . ? C32 C31 C24 119.3(16) . . ? C36 C31 C24 121.8(16) . . ? C31 C32 C33 122.5(18) . . ? C34 C33 C32 114(2) . . ? C35 C34 C33 125(2) . . ? C34 C35 C36 119(2) . . ? C31 C36 C35 119(2) . . ? C42 C41 C46 122.1(17) . . ? C42 C41 C25 119.8(15) . . ? C46 C41 C25 118.1(15) . . ? C41 C42 C43 116.3(18) . . ? C44 C43 C42 119(2) . . ? C43 C44 C45 127(3) . . ? C44 C45 C46 116(2) . . ? C41 C46 C45 119(2) . . ? C52 C51 N23 112.3(15) . . ? C57 C52 N53 120.8(19) . . ? C57 C52 C51 127.5(19) . . ? N53 C52 C51 111.6(17) . . ? C54 N53 C52 114(2) . . ? N53 C54 C55 124(3) . . ? C56 C55 C54 120(3) . . ? C57 C56 C55 117(3) . . ? C56 C57 C52 123(2) . . ? C106 N101 C102 116.0(11) . . ? C106 N101 Zn1 127.4(9) . 7_545 ? C102 N101 Zn1 116.3(9) . 7_545 ? C103 C102 N101 123.5(13) . . ? C103 C102 C92 127.1(13) . . ? N101 C102 C92 109.2(11) . . ? C102 C103 C104 115.7(15) . . ? C105 C104 C103 123.4(16) . . ? C104 C105 C106 116.6(15) . . ? N101 C106 C105 124.8(14) . . ? C86 N81 C82 119.9(13) . . ? C86 N81 Zn1 112.2(11) . . ? C82 N81 Zn1 127.9(9) . . ? N81 C82 C83 120.0(13) . . ? N81 C82 C87 116.3(12) . . ? C83 C82 C87 123.6(13) . . ? C82 C83 C84 120.5(16) . . ? C85 C84 C83 117.8(18) . . ? C86 C85 C84 118.7(19) . . ? N81 C86 C85 123.0(18) . . ? C92 N91 C95 106.5(11) . . ? C92 N91 Zn1 112.4(9) . 7_545 ? C95 N91 Zn1 139.8(9) . 7_545 ? N91 C92 N93 109.2(11) . . ? N91 C92 C102 122.2(12) . . ? N93 C92 C102 128.5(12) . . ? C94 N93 C92 107.5(11) . . ? C94 N93 C87 123.5(12) . . ? C92 N93 C87 128.9(12) . . ? C95 C94 N93 106.5(13) . . ? C95 C94 C121 129.0(13) . . ? N93 C94 C121 124.5(13) . . ? C94 C95 N91 110.1(12) . . ? C94 C95 C111 127.5(14) . . ? N91 C95 C111 122.2(13) . . ? N93 C87 C82 113.5(12) . . ? C116 C111 C112 122.9(16) . . ? C116 C111 C95 117.4(14) . . ? C112 C111 C95 119.7(14) . . ? C111 C112 C113 118.8(17) . . ? C114 C113 C112 118(2) . . ? C113 C114 C115 129(2) . . ? C114 C115 C116 114(2) . . ? C111 C116 C115 117.4(18) . . ? C122 C121 C126 121.0(16) . . ? C122 C121 C94 122.5(14) . . ? C126 C121 C94 116.5(15) . . ? C121 C122 C123 123.0(17) . . ? C124 C123 C122 117.8(19) . . ? C123 C124 C125 121(2) . . ? C124 C125 C126 123(2) . . ? C121 C126 C125 114.1(19) . . ? O12 Cl1 O12 118.5(15) . 5 ? O12 Cl1 O11 107.4(11) . 5 ? O12 Cl1 O11 111.7(10) 5 5 ? O12 Cl1 O11 111.7(11) . . ? O12 Cl1 O11 107.4(11) 5 . ? O11 Cl1 O11 98.2(16) 5 . ? O24 Cl2 O21 109.1(9) . . ? O24 Cl2 O23 110.4(9) . . ? O21 Cl2 O23 111.1(8) . . ? O24 Cl2 O22 110.5(9) . . ? O21 Cl2 O22 109.0(8) . . ? O23 Cl2 O22 106.7(8) . . ? O32 Cl3 O32 79(3) 5 . ? O32 Cl3 O33 76(2) 5 . ? O32 Cl3 O33 115.6(15) . . ? O32 Cl3 O33 115.6(15) 5 5 ? O32 Cl3 O33 76(2) . 5 ? O33 Cl3 O33 166(3) . 5 ? O32 Cl3 O34 111.4(14) 5 5 ? O32 Cl3 O34 164(2) . 5 ? O33 Cl3 O34 59(2) . 5 ? O33 Cl3 O34 108.2(14) 5 5 ? O32 Cl3 O34 164(2) 5 . ? O32 Cl3 O34 111.4(14) . . ? O33 Cl3 O34 108.2(14) . . ? O33 Cl3 O34 59(2) 5 . ? O34 Cl3 O34 61(3) 5 . ? O32 Cl3 O31 60.5(18) 5 . ? O32 Cl3 O31 110.1(14) . . ? O33 Cl3 O31 106.6(13) . . ? O33 Cl3 O31 74.7(13) 5 . ? O34 Cl3 O31 86(2) 5 . ? O34 Cl3 O31 104.1(13) . . ? O32 Cl3 O31 110.1(14) 5 5 ? O32 Cl3 O31 60.5(18) . 5 ? O33 Cl3 O31 74.7(13) . 5 ? O33 Cl3 O31 106.6(13) 5 5 ? O34 Cl3 O31 104.1(13) 5 5 ? O34 Cl3 O31 86(2) . 5 ? O31 Cl3 O31 169(2) . 5 ? O32 O31 Cl3 56.6(12) 5 . ? O32 O31 O33 95.3(19) 5 5 ? Cl3 O31 O33 51.3(9) . 5 ? O34 O33 Cl3 61.9(15) 5 . ? O34 O33 O32 96.6(18) 5 5 ? Cl3 O33 O32 51.2(13) . 5 ? O34 O33 O31 93(2) 5 5 ? Cl3 O33 O31 54.0(9) . 5 ? O32 O33 O31 84.7(17) 5 5 ? O33 O34 Cl3 59.2(11) 5 . ? O33 O34 O34 107(2) 5 5 ? Cl3 O34 O34 59.5(13) . 5 ? Cl3 O32 O31 62.9(12) . 5 ? Cl3 O32 O33 53.2(11) . 5 ? O31 O32 O33 94.2(19) 5 5 ? Cl3 O32 O32 50.4(14) . 5 ? O31 O32 O32 93(2) 5 5 ? O33 O32 O32 86.0(18) 5 5 ? Cl76 C71 Cl75 107.9(15) . . ? Cl76 C71 Cl72 77.9(19) . . ? Cl75 C71 Cl72 32.4(17) . . ? Cl76 C71 Cl74 52(2) . . ? Cl75 C71 Cl74 60(2) . . ? Cl72 C71 Cl74 27.9(19) . . ? Cl76 C71 Cl71 30.6(19) . . ? Cl75 C71 Cl71 128(2) . . ? Cl72 C71 Cl71 104.1(14) . . ? Cl74 C71 Cl71 81.6(17) . . ? Cl76 C71 Cl73 51(2) . . ? Cl75 C71 Cl73 136(3) . . ? Cl72 C71 Cl73 120.5(19) . . ? Cl74 C71 Cl73 100.7(13) . . ? Cl71 C71 Cl73 19.9(15) . . ? Cl76 Cl71 Cl73 160(4) . . ? Cl76 Cl71 C71 74.3(17) . . ? Cl73 Cl71 C71 86(3) . . ? Cl76 Cl71 O100 9(4) . . ? Cl73 Cl71 O100 164(4) . . ? C71 Cl71 O100 79.9(18) . . ? Cl76 Cl71 Cl74 28(2) . . ? Cl73 Cl71 Cl74 134(3) . . ? C71 Cl71 Cl74 50.1(11) . . ? O100 Cl71 Cl74 30.5(15) . . ? Cl75 Cl72 Cl74 147(3) . . ? Cl75 Cl72 C71 70.7(17) . . ? Cl74 Cl72 C71 76.3(18) . . ? Cl75 Cl72 Cl76 117(2) . . ? Cl74 Cl72 Cl76 32(3) . . ? C71 Cl72 Cl76 50.0(11) . . ? Cl71 Cl73 Cl76 12(2) . . ? Cl71 Cl73 C71 74(2) . . ? Cl76 Cl73 C71 62.4(12) . . ? Cl72 Cl74 O100 157(7) . . ? Cl72 Cl74 C71 76(2) . . ? O100 Cl74 C71 102(3) . . ? Cl72 Cl74 Cl76 131(4) . . ? O100 Cl74 Cl76 40(2) . . ? C71 Cl74 Cl76 62.0(13) . . ? Cl72 Cl74 Cl75 17.6(17) . . ? O100 Cl74 Cl75 150(4) . . ? C71 Cl74 Cl75 58.2(14) . . ? Cl76 Cl74 Cl75 115(2) . . ? Cl72 Cl74 Cl71 115(3) . . ? O100 Cl74 Cl71 55(2) . . ? C71 Cl74 Cl71 48.3(9) . . ? Cl76 Cl74 Cl71 15.9(16) . . ? Cl75 Cl74 Cl71 99.0(18) . . ? Cl72 Cl75 C71 76.9(16) . . ? Cl72 Cl75 Cl74 15.4(15) . . ? C71 Cl75 Cl74 61.5(12) . . ? Cl71 Cl76 O100 162(8) . . ? Cl71 Cl76 C71 75(2) . . ? O100 Cl76 C71 115(4) . . ? Cl71 Cl76 Cl73 7.9(16) . . ? O100 Cl76 Cl73 165(6) . . ? C71 Cl76 Cl73 67.1(17) . . ? Cl71 Cl76 Cl74 137(3) . . ? O100 Cl76 Cl74 49(3) . . ? C71 Cl76 Cl74 65.7(14) . . ? Cl73 Cl76 Cl74 129(2) . . ? Cl71 Cl76 Cl72 119(3) . . ? O100 Cl76 Cl72 64(3) . . ? C71 Cl76 Cl72 52.1(11) . . ? Cl73 Cl76 Cl72 112(2) . . ? Cl74 Cl76 Cl72 17.2(19) . . ? Cl74 O100 Cl76 91(4) . . ? Cl74 O100 Cl71 95(3) . . ? Cl76 O100 Cl71 9(4) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 20.91 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.618 _refine_diff_density_min -0.512 _refine_diff_density_rms 0.113