# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Wen-Fu Fu' _publ_contact_author_email 'WF FU@YAHOO.COM.CN' _publ_section_title ; A Flexible 1,8-Naphthyridyl Derivative and Its Zn(II) Complexes: Synthesis, Structures, Spectroscopic Properties and Recognition of Cd(II) ; loop_ _publ_author_name 'Wen-Fu Fu.' 'Shao-Ming Chi.' 'Xin Gan.' 'Jun Wang.' 'Quan-Qing Xu.' ; H.-M.Zhang ; # Attachment 'CIFfile for L and complexes 1-3.cif' ## Crystallographic Data of L data_L _database_code_depnum_ccdc_archive 'CCDC 679373' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H20 N6, 2(Cl O4)' _chemical_formula_sum 'C19 H20 Cl2 N6 O8' _chemical_formula_weight 531.31 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' Cl Cl 0.1484 0.1585 '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 b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 8.1910(5) _cell_length_b 19.3250(12) _cell_length_c 27.8850(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4414.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7263 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 28.0 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.934 _exptl_absorpt_correction_T_max 0.951 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 31220 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3883 _reflns_number_gt 3598 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0498P)^2^+5.3196P] 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 3882 _refine_ls_number_parameters 408 _refine_ls_number_restraints 124 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1339 _refine_ls_wR_factor_gt 0.1306 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.180 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.24246(10) 0.22574(4) 0.56855(3) 0.0360(2) Uani 1 1 d D . . Cl2 Cl 1.00163(9) 0.01682(3) 0.69459(3) 0.0323(2) Uani 1 1 d D . . O1 O 0.1693(6) 0.1730(2) 0.59780(16) 0.0534(14) Uani 0.747(5) 1 d PD A 1 O2 O 0.3894(5) 0.2014(2) 0.5483(2) 0.0758(17) Uani 0.747(5) 1 d PD A 1 O3 O 0.1302(6) 0.2438(2) 0.53084(12) 0.0738(15) Uani 0.747(5) 1 d PD A 1 O4 O 0.2651(6) 0.28664(19) 0.59698(15) 0.0700(14) Uani 0.747(5) 1 d PD A 1 O5 O 0.8509(4) 0.02894(17) 0.67091(14) 0.0664(12) Uani 0.870(6) 1 d PD B 1 O6 O 0.9850(5) -0.03196(14) 0.73264(10) 0.0657(13) Uani 0.870(6) 1 d PD B 1 O7 O 1.1129(3) -0.01123(15) 0.65972(10) 0.0490(10) Uani 0.870(6) 1 d PD B 1 O8 O 1.0661(6) 0.0802(2) 0.7134(2) 0.0444(13) Uani 0.870(6) 1 d PD B 1 O1' O 0.1358(14) 0.1676(5) 0.5766(4) 0.039(3) Uani 0.253(5) 1 d PDU A 2 O2' O 0.3710(11) 0.2233(6) 0.6037(3) 0.062(4) Uani 0.253(5) 1 d PDU A 2 O3' O 0.3135(14) 0.2178(6) 0.5220(3) 0.062(4) Uani 0.253(5) 1 d PDU A 2 O4' O 0.1558(13) 0.2875(4) 0.5708(4) 0.052(3) Uani 0.253(5) 1 d PDU A 2 O5' O 0.8301(12) 0.0031(10) 0.7058(7) 0.053(6) Uani 0.130(6) 1 d PDU B 2 O6' O 1.0870(19) -0.0453(6) 0.7069(7) 0.048(6) Uani 0.130(6) 1 d PDU B 2 O7' O 1.012(3) 0.0307(10) 0.6446(4) 0.062(7) Uani 0.130(6) 1 d PDU B 2 O8' O 1.056(3) 0.0738(10) 0.7228(8) 0.039(10) Uani 0.130(6) 1 d PDU B 2 N1 N 0.1466(3) 0.16498(13) 0.27420(9) 0.0328(6) Uani 1 1 d . . . N2 N 0.1460(3) 0.16453(12) 0.35633(8) 0.0293(6) Uani 1 1 d . . . N3 N 0.1396(3) 0.16601(15) 0.43819(10) 0.0353(6) Uani 1 1 d . . . N6 N 0.3295(3) 0.04505(14) 0.58097(9) 0.0336(6) Uani 1 1 d . . . N5 N 0.2041(3) 0.04253(13) 0.50731(9) 0.0327(6) Uani 1 1 d . . . N4 N 0.0922(4) 0.04231(16) 0.43264(11) 0.0417(7) Uani 1 1 d . . . C2 C 0.1739(4) 0.19127(16) 0.23034(10) 0.0377(8) Uani 1 1 d . . . C3 C 0.2463(5) 0.25570(18) 0.22665(11) 0.0435(9) Uani 1 1 d . . . H3 H 0.2634 0.2759 0.1960 0.052 Uiso 1 1 calc R . . C4 C 0.2935(4) 0.29061(16) 0.26746(11) 0.0390(8) Uani 1 1 d . . . H4 H 0.3453 0.3344 0.2647 0.047 Uiso 1 1 calc R . . C5 C 0.2662(4) 0.26239(14) 0.31277(10) 0.0285(7) Uani 1 1 d . . . C6 C 0.1858(4) 0.19774(14) 0.31595(10) 0.0268(6) Uani 1 1 d . . . C7 C 0.1866(4) 0.19636(15) 0.39716(10) 0.0288(7) Uani 1 1 d . . . C8 C 0.2786(4) 0.25928(15) 0.39855(10) 0.0314(7) Uani 1 1 d . . . H8 H 0.3132 0.2779 0.4284 0.038 Uiso 1 1 calc R . . C9 C 0.3159(4) 0.29193(15) 0.35722(10) 0.0324(7) Uani 1 1 d . . . H9 H 0.3748 0.3343 0.3578 0.039 Uiso 1 1 calc R . . C1 C 0.1243(6) 0.14783(18) 0.18868(12) 0.0518(10) Uani 1 1 d . . . H1A H 0.2123 0.1154 0.1808 0.078 Uiso 1 1 calc R . . H1B H 0.1026 0.1776 0.1610 0.078 Uiso 1 1 calc R . . H1C H 0.0253 0.1219 0.1968 0.078 Uiso 1 1 calc R . . C16 C 0.4320(4) 0.02351(16) 0.61578(11) 0.0360(8) Uani 1 1 d . . . C17 C 0.5112(4) -0.03943(17) 0.60916(12) 0.0402(8) Uani 1 1 d . . . H17 H 0.5862 -0.0556 0.6326 0.048 Uiso 1 1 calc R . . C18 C 0.4812(4) -0.07835(17) 0.56878(12) 0.0398(8) Uani 1 1 d . . . H18 H 0.5322 -0.1222 0.5653 0.048 Uiso 1 1 calc R . . C14 C 0.3773(4) -0.05443(15) 0.53293(12) 0.0357(7) Uani 1 1 d . . . C15 C 0.3015(4) 0.01043(16) 0.53928(11) 0.0316(7) Uani 1 1 d . . . C11 C 0.1802(4) 0.00934(17) 0.46592(11) 0.0368(8) Uani 1 1 d . . . C12 C 0.2463(4) -0.05808(16) 0.45608(12) 0.0424(8) Uani 1 1 d . . . H12 H 0.2221 -0.0808 0.4267 0.051 Uiso 1 1 calc R . . C13 C 0.3428(4) -0.08878(16) 0.48880(12) 0.0411(8) Uani 1 1 d . . . H13 H 0.3878 -0.1332 0.4825 0.049 Uiso 1 1 calc R . . C19 C 0.4554(5) 0.06921(19) 0.65809(11) 0.0446(8) Uani 1 1 d . . . H19A H 0.4863 0.1156 0.6473 0.067 Uiso 1 1 calc R . . H19B H 0.5418 0.0503 0.6785 0.067 Uiso 1 1 calc R . . H19C H 0.3533 0.0718 0.6763 0.067 Uiso 1 1 calc R . . C10 C 0.0224(4) 0.10976(18) 0.43970(12) 0.0431(8) Uani 1 1 d . . . H10A H -0.0336 0.1106 0.4712 0.052 Uiso 1 1 calc R . . H10B H -0.0612 0.1178 0.4147 0.052 Uiso 1 1 calc R . . H3A H 0.163(4) 0.1865(17) 0.4619(12) 0.035(10) Uiso 1 1 d . . . H1 H 0.101(5) 0.124(2) 0.2764(13) 0.055(11) Uiso 1 1 d . . . H4A H 0.081(5) 0.0269(19) 0.4097(13) 0.040(12) Uiso 1 1 d . . . H6 H 0.281(4) 0.0828(18) 0.5853(12) 0.035(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0433(5) 0.0317(4) 0.0331(4) -0.0008(3) 0.0046(4) -0.0003(3) Cl2 0.0360(5) 0.0256(4) 0.0353(4) -0.0012(3) 0.0018(3) -0.0007(3) O1 0.064(3) 0.046(2) 0.050(3) 0.022(2) 0.026(2) 0.016(2) O2 0.055(3) 0.049(2) 0.124(4) -0.011(3) 0.053(3) -0.002(2) O3 0.118(4) 0.059(2) 0.045(2) 0.0033(18) -0.025(2) 0.031(2) O4 0.089(3) 0.052(2) 0.070(3) -0.027(2) 0.002(3) -0.001(2) O5 0.0421(19) 0.063(2) 0.095(3) -0.019(2) -0.0291(19) 0.0139(15) O6 0.126(4) 0.0396(16) 0.0313(15) 0.0050(12) -0.0042(19) -0.0408(19) O7 0.0410(17) 0.0542(18) 0.0519(18) -0.0213(14) 0.0127(14) -0.0075(14) O8 0.055(3) 0.0232(18) 0.055(2) -0.0076(17) -0.002(2) -0.0038(16) O1' 0.036(6) 0.030(5) 0.051(7) 0.002(5) 0.014(5) -0.003(4) O2' 0.049(6) 0.086(7) 0.052(6) 0.031(5) -0.013(5) -0.022(5) O3' 0.056(7) 0.087(7) 0.041(6) -0.020(5) 0.023(5) -0.016(6) O4' 0.063(6) 0.027(4) 0.065(6) 0.007(4) 0.012(5) 0.017(4) O5' 0.030(8) 0.067(9) 0.061(10) 0.003(8) 0.004(7) 0.008(7) O6' 0.046(9) 0.033(8) 0.064(10) 0.003(7) 0.000(8) 0.009(7) O7' 0.085(11) 0.060(10) 0.041(9) -0.003(7) 0.014(8) -0.012(8) O8' 0.053(14) 0.032(13) 0.032(12) -0.010(8) -0.006(8) 0.002(8) N1 0.0448(17) 0.0233(13) 0.0302(14) 0.0000(10) -0.0070(12) -0.0046(12) N2 0.0321(14) 0.0275(12) 0.0283(13) 0.0035(10) -0.0009(11) -0.0027(11) N3 0.0381(16) 0.0419(15) 0.0260(14) 0.0032(12) -0.0004(12) 0.0023(13) N6 0.0353(15) 0.0344(15) 0.0310(14) 0.0103(12) 0.0054(12) 0.0059(13) N5 0.0314(14) 0.0360(14) 0.0306(13) 0.0101(11) 0.0053(11) -0.0023(11) N4 0.0479(19) 0.0467(18) 0.0306(16) 0.0084(14) -0.0024(15) -0.0128(14) C2 0.053(2) 0.0331(16) 0.0266(16) -0.0008(13) -0.0066(15) 0.0011(15) C3 0.064(2) 0.0381(18) 0.0287(16) 0.0063(14) -0.0008(16) -0.0036(17) C4 0.050(2) 0.0317(16) 0.0349(17) 0.0043(13) 0.0017(15) -0.0098(15) C5 0.0341(17) 0.0212(14) 0.0302(15) -0.0004(12) -0.0020(13) -0.0031(12) C6 0.0325(16) 0.0223(13) 0.0257(14) -0.0003(11) -0.0021(13) -0.0012(12) C7 0.0299(16) 0.0301(15) 0.0264(15) 0.0022(12) 0.0012(13) 0.0067(13) C8 0.0359(18) 0.0293(15) 0.0290(15) -0.0066(12) -0.0035(13) 0.0050(13) C9 0.0374(18) 0.0262(15) 0.0335(16) -0.0030(12) -0.0029(14) -0.0018(13) C1 0.083(3) 0.0408(19) 0.0316(18) -0.0052(15) -0.0128(19) -0.0031(19) C16 0.0290(17) 0.0429(18) 0.0362(17) 0.0172(14) 0.0067(14) -0.0019(14) C17 0.0313(18) 0.0449(19) 0.0444(19) 0.0222(16) 0.0056(15) 0.0015(15) C18 0.0337(18) 0.0324(17) 0.053(2) 0.0202(15) 0.0174(16) 0.0026(14) C14 0.0355(18) 0.0285(15) 0.0430(18) 0.0115(14) 0.0150(15) -0.0041(14) C15 0.0287(17) 0.0350(16) 0.0309(16) 0.0104(13) 0.0097(13) -0.0028(13) C11 0.0381(19) 0.0409(18) 0.0314(16) 0.0099(14) 0.0053(15) -0.0138(15) C12 0.052(2) 0.0331(17) 0.0417(19) 0.0006(15) 0.0116(17) -0.0172(16) C13 0.048(2) 0.0273(16) 0.048(2) 0.0061(14) 0.0165(17) -0.0080(15) C19 0.042(2) 0.058(2) 0.0341(17) 0.0121(16) 0.0011(16) -0.0008(17) C10 0.0343(19) 0.061(2) 0.0343(18) 0.0176(16) 0.0030(15) -0.0038(17) _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 Cl1 O4' 1.390(7) . ? Cl1 O2 1.410(4) . ? Cl1 O3' 1.430(7) . ? Cl1 O4 1.431(3) . ? Cl1 O1 1.436(4) . ? Cl1 O2' 1.439(7) . ? Cl1 O3 1.440(3) . ? Cl1 O1' 1.441(8) . ? Cl2 O5 1.420(3) . ? Cl2 O7' 1.423(9) . ? Cl2 O8' 1.424(10) . ? Cl2 O6 1.426(3) . ? Cl2 O6' 1.432(9) . ? Cl2 O8 1.433(3) . ? Cl2 O7 1.439(3) . ? Cl2 O5' 1.464(9) . ? N1 C2 1.343(4) . ? N1 C6 1.364(4) . ? N1 H1 0.88(4) . ? N2 C7 1.336(4) . ? N2 C6 1.336(4) . ? N3 C7 1.342(4) . ? N3 C10 1.451(4) . ? N3 H3A 0.80(3) . ? N6 C16 1.350(4) . ? N6 C15 1.360(4) . ? N6 H6 0.84(3) . ? N5 C11 1.335(4) . ? N5 C15 1.348(4) . ? N4 C11 1.337(4) . ? N4 C10 1.437(5) . ? N4 H4A 0.71(4) . ? C2 C3 1.383(5) . ? C2 C1 1.490(4) . ? C3 C4 1.378(4) . ? C3 H3 0.9500 . ? C4 C5 1.394(4) . ? C4 H4 0.9500 . ? C5 C6 1.415(4) . ? C5 C9 1.424(4) . ? C7 C8 1.431(4) . ? C8 C9 1.349(4) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C16 C17 1.390(5) . ? C16 C19 1.486(5) . ? C17 C18 1.376(5) . ? C17 H17 0.9500 . ? C18 C14 1.392(5) . ? C18 H18 0.9500 . ? C14 C15 1.410(4) . ? C14 C13 1.427(5) . ? C11 C12 1.437(5) . ? C12 C13 1.345(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? 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 O4' Cl1 O2 137.8(4) . . ? O4' Cl1 O3' 109.9(6) . . ? O2 Cl1 O3' 41.7(5) . . ? O4' Cl1 O4 48.3(4) . . ? O2 Cl1 O4 112.7(3) . . ? O3' Cl1 O4 122.6(5) . . ? O4' Cl1 O1 111.8(5) . . ? O2 Cl1 O1 110.3(3) . . ? O3' Cl1 O1 127.5(5) . . ? O4 Cl1 O1 108.9(3) . . ? O4' Cl1 O2' 111.7(6) . . ? O2 Cl1 O2' 68.8(5) . . ? O3' Cl1 O2' 108.5(6) . . ? O4 Cl1 O2' 63.6(5) . . ? O1 Cl1 O2' 84.0(4) . . ? O4' Cl1 O3 59.9(5) . . ? O2 Cl1 O3 109.5(3) . . ? O3' Cl1 O3 67.9(5) . . ? O4 Cl1 O3 106.7(2) . . ? O1 Cl1 O3 108.7(3) . . ? O2' Cl1 O3 166.5(4) . . ? O4' Cl1 O1' 110.7(6) . . ? O2 Cl1 O1' 108.6(6) . . ? O3' Cl1 O1' 107.7(6) . . ? O4 Cl1 O1' 129.3(5) . . ? O1 Cl1 O1' 26.6(4) . . ? O2' Cl1 O1' 108.2(6) . . ? O3 Cl1 O1' 85.2(5) . . ? O5 Cl2 O7' 64.3(8) . . ? O5 Cl2 O8' 113.6(11) . . ? O7' Cl2 O8' 112.1(10) . . ? O5 Cl2 O6 111.8(2) . . ? O7' Cl2 O6 149.3(8) . . ? O8' Cl2 O6 97.5(11) . . ? O5 Cl2 O6' 132.4(7) . . ? O7' Cl2 O6' 111.3(8) . . ? O8' Cl2 O6' 111.4(10) . . ? O6 Cl2 O6' 46.6(7) . . ? O5 Cl2 O8 110.5(2) . . ? O7' Cl2 O8 100.1(8) . . ? O8' Cl2 O8 12.1(12) . . ? O6 Cl2 O8 109.1(3) . . ? O6' Cl2 O8 116.7(8) . . ? O5 Cl2 O7 107.38(19) . . ? O7' Cl2 O7 50.9(8) . . ? O8' Cl2 O7 117.9(11) . . ? O6 Cl2 O7 108.3(2) . . ? O6' Cl2 O7 62.4(8) . . ? O8 Cl2 O7 109.6(3) . . ? O5 Cl2 O5' 45.2(7) . . ? O7' Cl2 O5' 107.7(8) . . ? O8' Cl2 O5' 108.7(10) . . ? O6 Cl2 O5' 68.2(8) . . ? O6' Cl2 O5' 105.3(8) . . ? O8 Cl2 O5' 115.5(8) . . ? O7 Cl2 O5' 133.2(8) . . ? C2 N1 C6 124.2(3) . . ? C2 N1 H1 118(2) . . ? C6 N1 H1 117(2) . . ? C7 N2 C6 115.9(2) . . ? C7 N3 C10 122.8(3) . . ? C7 N3 H3A 115(2) . . ? C10 N3 H3A 121(2) . . ? C16 N6 C15 124.6(3) . . ? C16 N6 H6 117(2) . . ? C15 N6 H6 118(2) . . ? C11 N5 C15 116.0(3) . . ? C11 N4 C10 123.5(3) . . ? C11 N4 H4A 120(3) . . ? C10 N4 H4A 117(3) . . ? N1 C2 C3 118.7(3) . . ? N1 C2 C1 116.8(3) . . ? C3 C2 C1 124.5(3) . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.8(3) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C4 C5 C6 118.5(3) . . ? C4 C5 C9 125.9(3) . . ? C6 C5 C9 115.6(3) . . ? N2 C6 N1 116.0(2) . . ? N2 C6 C5 126.2(3) . . ? N1 C6 C5 117.8(3) . . ? N2 C7 N3 117.0(3) . . ? N2 C7 C8 123.0(3) . . ? N3 C7 C8 120.0(3) . . ? C9 C8 C7 119.6(3) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C5 119.4(3) . . ? C8 C9 H9 120.3 . . ? C5 C9 H9 120.3 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N6 C16 C17 117.7(3) . . ? N6 C16 C19 117.9(3) . . ? C17 C16 C19 124.4(3) . . ? C18 C17 C16 120.2(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C14 121.0(3) . . ? C17 C18 H18 119.5 . . ? C14 C18 H18 119.5 . . ? C18 C14 C15 118.3(3) . . ? C18 C14 C13 125.9(3) . . ? C15 C14 C13 115.8(3) . . ? N5 C15 N6 116.0(3) . . ? N5 C15 C14 125.9(3) . . ? N6 C15 C14 118.1(3) . . ? N5 C11 N4 116.8(3) . . ? N5 C11 C12 123.1(3) . . ? N4 C11 C12 120.2(3) . . ? C13 C12 C11 119.5(3) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C10 N3 114.4(3) . . ? N4 C10 H10A 108.7 . . ? N3 C10 H10A 108.7 . . ? N4 C10 H10B 108.7 . . ? N3 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? 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 C6 N1 C2 C3 -0.1(5) . . . . ? C6 N1 C2 C1 179.5(3) . . . . ? N1 C2 C3 C4 2.1(5) . . . . ? C1 C2 C3 C4 -177.4(4) . . . . ? C2 C3 C4 C5 -1.4(6) . . . . ? C3 C4 C5 C6 -1.3(5) . . . . ? C3 C4 C5 C9 177.0(3) . . . . ? C7 N2 C6 N1 179.2(3) . . . . ? C7 N2 C6 C5 0.2(4) . . . . ? C2 N1 C6 N2 178.4(3) . . . . ? C2 N1 C6 C5 -2.5(5) . . . . ? C4 C5 C6 N2 -177.9(3) . . . . ? C9 C5 C6 N2 3.7(5) . . . . ? C4 C5 C6 N1 3.1(4) . . . . ? C9 C5 C6 N1 -175.3(3) . . . . ? C6 N2 C7 N3 176.2(3) . . . . ? C6 N2 C7 C8 -4.9(4) . . . . ? C10 N3 C7 N2 -12.6(4) . . . . ? C10 N3 C7 C8 168.5(3) . . . . ? N2 C7 C8 C9 5.7(5) . . . . ? N3 C7 C8 C9 -175.5(3) . . . . ? C7 C8 C9 C5 -1.4(5) . . . . ? C4 C5 C9 C8 178.9(3) . . . . ? C6 C5 C9 C8 -2.8(4) . . . . ? C15 N6 C16 C17 -1.9(4) . . . . ? C15 N6 C16 C19 176.9(3) . . . . ? N6 C16 C17 C18 -1.5(4) . . . . ? C19 C16 C17 C18 179.8(3) . . . . ? C16 C17 C18 C14 2.8(5) . . . . ? C17 C18 C14 C15 -0.8(4) . . . . ? C17 C18 C14 C13 177.1(3) . . . . ? C11 N5 C15 N6 178.3(3) . . . . ? C11 N5 C15 C14 -0.7(4) . . . . ? C16 N6 C15 N5 -175.3(3) . . . . ? C16 N6 C15 C14 3.8(4) . . . . ? C18 C14 C15 N5 176.7(3) . . . . ? C13 C14 C15 N5 -1.5(4) . . . . ? C18 C14 C15 N6 -2.3(4) . . . . ? C13 C14 C15 N6 179.5(3) . . . . ? C15 N5 C11 N4 -176.0(3) . . . . ? C15 N5 C11 C12 3.0(4) . . . . ? C10 N4 C11 N5 -0.9(5) . . . . ? C10 N4 C11 C12 -179.9(3) . . . . ? N5 C11 C12 C13 -2.9(5) . . . . ? N4 C11 C12 C13 176.0(3) . . . . ? C11 C12 C13 C14 0.5(5) . . . . ? C18 C14 C13 C12 -176.5(3) . . . . ? C15 C14 C13 C12 1.5(4) . . . . ? C11 N4 C10 N3 74.2(4) . . . . ? C7 N3 C10 N4 85.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.351 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.056 #===END ## Crystallographic Data of complex 1 data_1 _database_code_depnum_ccdc_archive 'CCDC 690019' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H37 Cl3 N12 O13 Zn2' _chemical_formula_weight 1106.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 17.274(2) _cell_length_b 12.164(2) _cell_length_c 20.729(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.612(2) _cell_angle_gamma 90.00 _cell_volume 4341.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3955 _cell_measurement_theta_min 2.233 _cell_measurement_theta_max 22.216 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 1.370 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.648 _exptl_absorpt_correction_T_max 0.760 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20897 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7668 _reflns_number_gt 4377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0605P)^2^+6.0594P] 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 7657 _refine_ls_number_parameters 682 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 0.18577(4) 0.17594(5) 1.06429(3) 0.0430(2) Uani 1 1 d . . . Zn2 Zn 0.29216(4) 0.27204(5) 0.93859(3) 0.0417(2) Uani 1 1 d . . . Cl1 Cl 0.23967(9) 0.58596(14) 0.05659(8) 0.0581(4) Uani 1 1 d . . . Cl2 Cl 0.58795(9) 0.76450(13) 0.24087(8) 0.0578(4) Uani 1 1 d . . . Cl3 Cl 0.42292(13) 0.15695(18) 0.17604(14) 0.0873(6) Uani 1 1 d . . . N1 N 0.1588(2) 0.2330(4) 1.1594(2) 0.0434(11) Uani 1 1 d . . . N2 N 0.2008(2) 0.0626(4) 1.1409(2) 0.0416(11) Uani 1 1 d . . . N3 N 0.2448(3) -0.1112(4) 1.1175(3) 0.0575(14) Uani 1 1 d . . . H3 H 0.2426 -0.1797 1.1273 0.069 Uiso 1 1 calc R . . N4 N 0.0815(2) 0.1775(4) 1.0020(2) 0.0443(11) Uani 1 1 d . . . N5 N 0.1592(3) 0.0303(4) 0.9973(2) 0.0430(11) Uani 1 1 d . . . N6 N 0.2393(3) -0.1194(4) 1.0007(3) 0.0609(14) Uani 1 1 d . . . H6 H 0.2554 -0.1764 0.9812 0.073 Uiso 1 1 calc R . . N7 N 0.3992(2) 0.3593(3) 0.9363(2) 0.0397(11) Uani 1 1 d . . . N8 N 0.2868(3) 0.4418(3) 0.9030(2) 0.0424(11) Uani 1 1 d . . . N9 N 0.1690(3) 0.5173(4) 0.8647(2) 0.0606(14) Uani 1 1 d . . . H9 H 0.1464 0.5679 0.8412 0.073 Uiso 1 1 calc R . . N10 N 0.2956(3) 0.1155(3) 0.8947(2) 0.0439(11) Uani 1 1 d . . . N11 N 0.1943(3) 0.2270(4) 0.8684(2) 0.0447(11) Uani 1 1 d . . . N12 N 0.0956(3) 0.3502(5) 0.8402(3) 0.0656(15) Uani 1 1 d . . . H12 H 0.0547 0.3650 0.8153 0.079 Uiso 1 1 calc R . . O1 O 0.2623(2) 0.2572(3) 1.02449(17) 0.0479(10) Uani 1 1 d . . . H1 H 0.2924 0.3000 1.0539 0.057 Uiso 1 1 calc R . . O2 O 0.2175(3) 0.6437(4) 0.1119(2) 0.0808(14) Uani 1 1 d . A . O3 O 0.290(2) 0.492(4) 0.079(2) 0.073(5) Uani 0.70(10) 1 d P A 1 O4 O 0.1724(6) 0.538(4) 0.0228(11) 0.076(7) Uani 0.70(10) 1 d P A 1 O5 O 0.281(3) 0.650(2) 0.0144(19) 0.077(7) Uani 0.70(10) 1 d P A 1 O3' O 0.265(6) 0.485(8) 0.070(5) 0.077(15) Uani 0.30(10) 1 d P A 2 O4' O 0.181(3) 0.599(10) 0.009(2) 0.083(19) Uani 0.30(10) 1 d P A 2 O5' O 0.302(4) 0.656(6) 0.038(5) 0.074(12) Uani 0.30(10) 1 d P A 2 O6 O 0.5577(3) 0.6563(4) 0.2356(3) 0.0907(16) Uani 1 1 d . . . O7 O 0.5724(3) 0.8033(4) 0.3026(3) 0.0936(17) Uani 1 1 d . . . O8 O 0.6699(3) 0.7642(5) 0.2360(3) 0.1010(19) Uani 1 1 d . . . O9 O 0.5525(3) 0.8308(4) 0.1921(2) 0.0919(17) Uani 1 1 d . . . O10 O 0.3664(7) 0.2413(9) 0.1598(6) 0.135(5) Uani 0.729(16) 1 d P B 1 O11 O 0.4922(6) 0.1897(9) 0.1525(5) 0.114(4) Uani 0.729(16) 1 d P B 1 O12 O 0.4358(8) 0.1595(11) 0.2457(6) 0.148(5) Uani 0.729(16) 1 d P B 1 O13 O 0.3954(7) 0.0558(9) 0.1564(7) 0.114(4) Uani 0.729(16) 1 d P B 1 O10' O 0.4874(16) 0.108(2) 0.2158(16) 0.120(12) Uani 0.271(16) 1 d P B 2 O11' O 0.3564(15) 0.156(2) 0.2122(15) 0.122(12) Uani 0.271(16) 1 d P B 2 O12' O 0.409(2) 0.096(3) 0.118(2) 0.124(12) Uani 0.271(16) 1 d P B 2 O13' O 0.443(2) 0.266(3) 0.1624(15) 0.139(13) Uani 0.271(16) 1 d P B 2 C1 C 0.1712(3) 0.1314(5) 1.1846(3) 0.0424(14) Uani 1 1 d . . . C2 C 0.2138(3) -0.0408(5) 1.1579(3) 0.0501(16) Uani 1 1 d . . . C3 C 0.1927(4) -0.0810(6) 1.2192(3) 0.0620(19) Uani 1 1 d . . . H3A H 0.1974 -0.1554 1.2292 0.074 Uiso 1 1 calc R . . C4 C 0.1661(4) -0.0108(7) 1.2618(3) 0.067(2) Uani 1 1 d . . . H4 H 0.1548 -0.0365 1.3022 0.081 Uiso 1 1 calc R . . C5 C 0.1550(3) 0.1002(6) 1.2469(3) 0.0528(16) Uani 1 1 d . . . C6 C 0.1270(3) 0.1845(7) 1.2849(3) 0.0646(19) Uani 1 1 d . . . H6A H 0.1146 0.1693 1.3268 0.078 Uiso 1 1 calc R . . C7 C 0.1179(4) 0.2879(6) 1.2610(3) 0.0635(18) Uani 1 1 d . . . H7 H 0.1016 0.3436 1.2874 0.076 Uiso 1 1 calc R . . C8 C 0.1326(3) 0.3117(5) 1.1978(3) 0.0519(16) Uani 1 1 d . . . C9 C 0.1195(4) 0.4236(5) 1.1701(3) 0.072(2) Uani 1 1 d . . . H9A H 0.1379 0.4262 1.1276 0.108 Uiso 1 1 calc R . . H9B H 0.1472 0.4766 1.1974 0.108 Uiso 1 1 calc R . . H9C H 0.0650 0.4402 1.1674 0.108 Uiso 1 1 calc R . . C10 C 0.0935(3) 0.0807(5) 0.9730(3) 0.0438(14) Uani 1 1 d . . . C11 C 0.1754(4) -0.0676(5) 0.9746(3) 0.0501(15) Uani 1 1 d . . . C12 C 0.1269(4) -0.1183(5) 0.9247(3) 0.0597(18) Uani 1 1 d . . . H12A H 0.1398 -0.1871 0.9094 0.072 Uiso 1 1 calc R . . C13 C 0.0636(4) -0.0686(6) 0.9000(3) 0.0644(19) Uani 1 1 d . . . H13 H 0.0326 -0.1017 0.8668 0.077 Uiso 1 1 calc R . . C14 C 0.0430(3) 0.0356(6) 0.9240(3) 0.0539(16) Uani 1 1 d . . . C15 C -0.0214(4) 0.1011(7) 0.9047(3) 0.071(2) Uani 1 1 d . . . H15 H -0.0561 0.0775 0.8709 0.086 Uiso 1 1 calc R . . C16 C -0.0342(4) 0.1979(7) 0.9341(3) 0.069(2) Uani 1 1 d . . . H16 H -0.0781 0.2391 0.9213 0.083 Uiso 1 1 calc R . . C17 C 0.0186(3) 0.2360(5) 0.9838(3) 0.0555(16) Uani 1 1 d . . . C18 C 0.0058(4) 0.3398(6) 1.0194(4) 0.075(2) Uani 1 1 d . . . H18A H -0.0054 0.3230 1.0629 0.112 Uiso 1 1 calc R . . H18B H -0.0371 0.3791 0.9980 0.112 Uiso 1 1 calc R . . H18C H 0.0518 0.3844 1.0202 0.112 Uiso 1 1 calc R . . C19 C 0.2817(3) -0.0844(5) 1.0592(3) 0.0597(18) Uani 1 1 d . . . H19A H 0.2888 -0.0054 1.0575 0.072 Uiso 1 1 calc R . . H19B H 0.3327 -0.1181 1.0617 0.072 Uiso 1 1 calc R . . C20 C 0.3653(3) 0.4517(4) 0.9120(3) 0.0410(13) Uani 1 1 d . . . C21 C 0.2464(4) 0.5252(5) 0.8771(3) 0.0490(15) Uani 1 1 d . . . C22 C 0.2841(4) 0.6258(5) 0.8609(3) 0.0613(18) Uani 1 1 d . . . H22 H 0.2549 0.6844 0.8434 0.074 Uiso 1 1 calc R . . C23 C 0.3609(4) 0.6345(5) 0.8709(3) 0.0591(17) Uani 1 1 d . . . H23 H 0.3850 0.7001 0.8611 0.071 Uiso 1 1 calc R . . C24 C 0.4066(4) 0.5449(5) 0.8963(3) 0.0519(16) Uani 1 1 d . . . C25 C 0.4871(4) 0.5394(5) 0.9051(3) 0.0567(17) Uani 1 1 d . . . H25 H 0.5172 0.5995 0.8952 0.068 Uiso 1 1 calc R . . C26 C 0.5213(4) 0.4460(5) 0.9283(3) 0.0550(16) Uani 1 1 d . . . H26 H 0.5752 0.4415 0.9334 0.066 Uiso 1 1 calc R . . C27 C 0.4759(3) 0.3548(5) 0.9448(3) 0.0485(15) Uani 1 1 d . . . C28 C 0.5129(4) 0.2532(5) 0.9718(3) 0.067(2) Uani 1 1 d . . . H28A H 0.4808 0.2213 1.0025 0.101 Uiso 1 1 calc R . . H28B H 0.5629 0.2707 0.9930 0.101 Uiso 1 1 calc R . . H28C H 0.5191 0.2018 0.9375 0.101 Uiso 1 1 calc R . . C29 C 0.2290(4) 0.1296(5) 0.8566(3) 0.0453(14) Uani 1 1 d . . . C30 C 0.1300(4) 0.2534(5) 0.8317(3) 0.0520(16) Uani 1 1 d . . . C31 C 0.0952(4) 0.1785(6) 0.7860(3) 0.0691(19) Uani 1 1 d . . . H31 H 0.0485 0.1963 0.7629 0.083 Uiso 1 1 calc R . . C32 C 0.1294(4) 0.0817(6) 0.7760(3) 0.0655(19) Uani 1 1 d . . . H32 H 0.1058 0.0321 0.7464 0.079 Uiso 1 1 calc R . . C33 C 0.2010(4) 0.0546(5) 0.8099(3) 0.0564(17) Uani 1 1 d . . . C34 C 0.2456(5) -0.0379(5) 0.8016(3) 0.069(2) Uani 1 1 d . . . H34 H 0.2293 -0.0902 0.7707 0.083 Uiso 1 1 calc R . . C35 C 0.3127(5) -0.0520(5) 0.8385(4) 0.069(2) Uani 1 1 d . . . H35 H 0.3434 -0.1131 0.8319 0.083 Uiso 1 1 calc R . . C36 C 0.3371(4) 0.0248(5) 0.8870(3) 0.0563(17) Uani 1 1 d . . . C37 C 0.4084(4) 0.0071(5) 0.9303(4) 0.076(2) Uani 1 1 d . . . H37A H 0.4524 0.0355 0.9102 0.114 Uiso 1 1 calc R . . H37B H 0.4153 -0.0701 0.9383 0.114 Uiso 1 1 calc R . . H37C H 0.4036 0.0446 0.9706 0.114 Uiso 1 1 calc R . . C38 C 0.1212(3) 0.4319(5) 0.8875(3) 0.0575(17) Uani 1 1 d . . . H38A H 0.0758 0.4654 0.9039 0.069 Uiso 1 1 calc R . . H38B H 0.1499 0.3952 0.9235 0.069 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 0.0427(4) 0.0434(4) 0.0431(4) 0.0040(3) 0.0051(3) -0.0090(3) Zn2 0.0447(4) 0.0369(4) 0.0442(4) 0.0047(3) 0.0072(3) -0.0034(3) Cl1 0.0549(10) 0.0579(11) 0.0615(11) -0.0008(9) 0.0053(8) -0.0028(8) Cl2 0.0484(9) 0.0603(10) 0.0638(11) 0.0163(8) -0.0016(8) -0.0039(8) Cl3 0.0729(16) 0.0736(16) 0.116(2) -0.0096(13) 0.0089(14) -0.0205(12) N1 0.036(3) 0.048(3) 0.046(3) 0.003(2) 0.003(2) -0.008(2) N2 0.038(3) 0.046(3) 0.040(3) 0.007(2) -0.002(2) -0.004(2) N3 0.064(3) 0.042(3) 0.066(4) 0.010(3) 0.001(3) -0.002(3) N4 0.034(3) 0.053(3) 0.046(3) 0.006(2) 0.005(2) -0.007(2) N5 0.048(3) 0.042(3) 0.040(3) -0.003(2) 0.007(2) -0.011(2) N6 0.077(4) 0.045(3) 0.062(4) -0.007(3) 0.012(3) 0.005(3) N7 0.039(3) 0.041(3) 0.039(3) -0.001(2) 0.006(2) -0.002(2) N8 0.050(3) 0.032(3) 0.047(3) 0.004(2) 0.010(2) -0.002(2) N9 0.063(4) 0.055(3) 0.063(4) 0.018(3) 0.002(3) 0.013(3) N10 0.050(3) 0.035(3) 0.049(3) 0.006(2) 0.011(2) -0.002(2) N11 0.046(3) 0.046(3) 0.042(3) 0.004(2) 0.008(2) -0.005(2) N12 0.056(3) 0.074(4) 0.065(4) 0.011(3) -0.007(3) 0.012(3) O1 0.051(2) 0.052(2) 0.042(2) -0.0063(17) 0.0048(18) -0.0235(19) O2 0.107(4) 0.061(3) 0.075(4) -0.014(3) 0.017(3) 0.000(3) O3 0.063(13) 0.054(8) 0.101(12) 0.004(7) -0.015(10) -0.001(10) O4 0.062(5) 0.080(18) 0.083(8) -0.003(9) -0.018(4) -0.011(6) O5 0.085(17) 0.063(6) 0.085(15) 0.020(9) 0.021(10) 0.005(9) O3' 0.08(4) 0.050(16) 0.10(3) -0.003(18) 0.00(3) 0.00(3) O4' 0.070(15) 0.09(5) 0.091(18) 0.00(2) -0.009(14) 0.009(19) O5' 0.06(2) 0.070(15) 0.09(4) 0.02(2) 0.000(17) 0.006(14) O6 0.086(4) 0.062(3) 0.123(5) -0.004(3) 0.003(3) -0.011(3) O7 0.105(4) 0.097(4) 0.079(4) -0.016(3) 0.007(3) -0.033(3) O8 0.054(3) 0.120(5) 0.128(5) 0.049(4) 0.005(3) 0.000(3) O9 0.069(3) 0.112(4) 0.094(4) 0.058(3) 0.006(3) 0.013(3) O10 0.116(9) 0.111(9) 0.173(11) -0.017(7) -0.020(7) 0.016(7) O11 0.090(7) 0.094(8) 0.164(10) -0.009(6) 0.043(6) -0.032(6) O12 0.144(13) 0.157(11) 0.143(11) -0.008(8) 0.006(8) -0.035(9) O13 0.101(7) 0.078(7) 0.159(13) -0.004(7) -0.017(8) -0.047(5) O10' 0.10(2) 0.11(2) 0.15(3) -0.027(18) -0.005(19) -0.004(15) O11' 0.09(2) 0.12(2) 0.15(3) -0.006(19) 0.018(18) -0.028(15) O12' 0.10(2) 0.12(3) 0.15(3) -0.03(2) 0.00(2) -0.019(19) O13' 0.13(3) 0.12(3) 0.17(3) 0.00(2) 0.01(2) -0.03(2) C1 0.033(3) 0.055(4) 0.038(4) 0.001(3) -0.003(3) -0.008(3) C2 0.038(3) 0.053(4) 0.057(4) 0.009(3) -0.015(3) -0.004(3) C3 0.053(4) 0.065(5) 0.065(5) 0.029(4) -0.012(4) -0.010(3) C4 0.050(4) 0.097(6) 0.053(5) 0.025(4) -0.002(3) -0.010(4) C5 0.037(3) 0.083(5) 0.038(4) 0.010(3) -0.001(3) -0.009(3) C6 0.048(4) 0.108(6) 0.039(4) 0.000(4) 0.009(3) -0.005(4) C7 0.051(4) 0.081(5) 0.061(5) -0.015(4) 0.014(3) -0.002(4) C8 0.034(3) 0.065(4) 0.057(4) -0.010(3) 0.008(3) -0.008(3) C9 0.074(5) 0.058(5) 0.085(5) -0.010(4) 0.020(4) -0.001(4) C10 0.040(3) 0.053(4) 0.038(4) 0.002(3) 0.007(3) -0.016(3) C11 0.062(4) 0.045(4) 0.046(4) -0.001(3) 0.020(3) -0.015(3) C12 0.079(5) 0.055(4) 0.047(4) -0.011(3) 0.017(4) -0.027(4) C13 0.065(5) 0.084(5) 0.044(4) -0.012(4) 0.005(3) -0.035(4) C14 0.047(4) 0.072(5) 0.043(4) 0.007(3) 0.005(3) -0.018(3) C15 0.048(4) 0.110(6) 0.055(5) 0.001(4) -0.001(3) -0.022(4) C16 0.040(4) 0.100(6) 0.065(5) 0.020(4) -0.003(3) -0.003(4) C17 0.037(4) 0.067(4) 0.064(4) 0.012(3) 0.012(3) -0.006(3) C18 0.053(4) 0.073(5) 0.100(6) 0.007(4) 0.013(4) 0.010(4) C19 0.043(4) 0.048(4) 0.088(6) -0.002(3) 0.001(4) 0.004(3) C20 0.051(4) 0.033(3) 0.039(3) 0.000(2) 0.005(3) -0.003(3) C21 0.070(4) 0.039(4) 0.039(4) 0.004(3) 0.011(3) 0.004(3) C22 0.093(6) 0.041(4) 0.051(4) 0.013(3) 0.010(4) 0.010(4) C23 0.079(5) 0.043(4) 0.057(4) 0.007(3) 0.019(4) -0.013(3) C24 0.071(5) 0.047(4) 0.039(4) -0.002(3) 0.012(3) -0.011(3) C25 0.069(5) 0.056(4) 0.048(4) -0.010(3) 0.017(3) -0.029(4) C26 0.044(4) 0.065(5) 0.057(4) -0.011(3) 0.013(3) -0.015(3) C27 0.053(4) 0.048(4) 0.045(4) -0.009(3) 0.007(3) 0.001(3) C28 0.046(4) 0.062(5) 0.092(6) 0.001(4) -0.006(4) 0.006(3) C29 0.060(4) 0.041(4) 0.037(4) 0.007(3) 0.013(3) -0.011(3) C30 0.050(4) 0.058(4) 0.049(4) 0.012(3) 0.006(3) -0.003(3) C31 0.071(5) 0.083(5) 0.052(4) 0.013(4) -0.005(3) -0.020(4) C32 0.084(5) 0.062(5) 0.049(4) 0.002(3) -0.001(4) -0.029(4) C33 0.076(5) 0.049(4) 0.046(4) 0.001(3) 0.018(3) -0.020(4) C34 0.104(6) 0.045(4) 0.062(5) -0.007(3) 0.022(4) -0.018(4) C35 0.102(6) 0.032(4) 0.077(5) -0.009(3) 0.025(5) -0.001(4) C36 0.064(4) 0.039(4) 0.068(5) 0.015(3) 0.021(3) -0.002(3) C37 0.072(5) 0.049(4) 0.108(6) 0.016(4) 0.011(4) 0.007(3) C38 0.051(4) 0.059(4) 0.064(5) 0.014(3) 0.016(3) 0.018(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 1.891(3) . ? Zn1 N2 2.103(4) . ? Zn1 N4 2.130(4) . ? Zn1 N1 2.175(5) . ? Zn1 N5 2.275(4) . ? Zn2 O1 1.902(4) . ? Zn2 N10 2.112(4) . ? Zn2 N7 2.136(4) . ? Zn2 N8 2.192(4) . ? Zn2 N11 2.209(5) . ? Cl1 O3' 1.32(10) . ? Cl1 O4' 1.37(3) . ? Cl1 O5 1.41(3) . ? Cl1 O2 1.423(5) . ? Cl1 O4 1.432(17) . ? Cl1 O5' 1.45(7) . ? Cl1 O3 1.48(4) . ? Cl2 O9 1.397(4) . ? Cl2 O7 1.409(5) . ? Cl2 O6 1.417(5) . ? Cl2 O8 1.427(5) . ? Cl3 O13 1.369(11) . ? Cl3 O11 1.387(9) . ? Cl3 O13' 1.41(3) . ? Cl3 O12' 1.42(4) . ? Cl3 O11' 1.42(3) . ? Cl3 O10 1.438(10) . ? Cl3 O12 1.444(13) . ? Cl3 O10' 1.46(3) . ? N1 C8 1.348(7) . ? N1 C1 1.351(7) . ? N2 C2 1.321(7) . ? N2 C1 1.363(7) . ? N3 C2 1.338(8) . ? N3 C19 1.447(8) . ? N3 H3 0.8600 . ? N4 C17 1.328(7) . ? N4 C10 1.345(7) . ? N5 C11 1.318(7) . ? N5 C10 1.352(7) . ? N6 C11 1.347(7) . ? N6 C19 1.432(8) . ? N6 H6 0.8600 . ? N7 C27 1.324(7) . ? N7 C20 1.347(6) . ? N8 C21 1.320(7) . ? N8 C20 1.360(7) . ? N9 C21 1.344(7) . ? N9 C38 1.431(7) . ? N9 H9 0.8600 . ? N10 C36 1.333(7) . ? N10 C29 1.353(7) . ? N11 C30 1.335(7) . ? N11 C29 1.359(7) . ? N12 C30 1.337(7) . ? N12 C38 1.441(8) . ? N12 H12 0.8600 . ? O1 H1 0.9300 . ? C1 C5 1.396(8) . ? C2 C3 1.436(8) . ? C3 C4 1.335(9) . ? C3 H3A 0.9300 . ? C4 C5 1.396(9) . ? C4 H4 0.9300 . ? C5 C6 1.402(9) . ? C6 C7 1.356(9) . ? C6 H6A 0.9300 . ? C7 C8 1.384(9) . ? C7 H7 0.9300 . ? C8 C9 1.487(9) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C14 1.396(8) . ? C11 C12 1.418(8) . ? C12 C13 1.315(9) . ? C12 H12A 0.9300 . ? C13 C14 1.418(9) . ? C13 H13 0.9300 . ? C14 C15 1.401(9) . ? C15 C16 1.352(9) . ? C15 H15 0.9300 . ? C16 C17 1.399(9) . ? C16 H16 0.9300 . ? C17 C18 1.488(9) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C24 1.392(8) . ? C21 C22 1.438(8) . ? C22 C23 1.331(9) . ? C22 H22 0.9300 . ? C23 C24 1.422(8) . ? C23 H23 0.9300 . ? C24 C25 1.389(8) . ? C25 C26 1.351(8) . ? C25 H25 0.9300 . ? C26 C27 1.416(8) . ? C26 H26 0.9300 . ? C27 C28 1.481(8) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C33 1.389(8) . ? C30 C31 1.413(9) . ? C31 C32 1.340(9) . ? C31 H31 0.9300 . ? C32 C33 1.413(9) . ? C32 H32 0.9300 . ? C33 C34 1.382(9) . ? C34 C35 1.348(9) . ? C34 H34 0.9300 . ? C35 C36 1.411(9) . ? C35 H35 0.9300 . ? C36 C37 1.480(8) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9700 . ? C38 H38B 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 O1 Zn1 N2 128.56(16) . . ? O1 Zn1 N4 108.52(16) . . ? N2 Zn1 N4 120.69(17) . . ? O1 Zn1 N1 115.89(16) . . ? N2 Zn1 N1 63.08(18) . . ? N4 Zn1 N1 108.29(17) . . ? O1 Zn1 N5 104.70(16) . . ? N2 Zn1 N5 87.56(17) . . ? N4 Zn1 N5 61.17(17) . . ? N1 Zn1 N5 138.98(16) . . ? O1 Zn2 N10 109.64(16) . . ? O1 Zn2 N7 111.65(16) . . ? N10 Zn2 N7 112.58(17) . . ? O1 Zn2 N8 113.41(16) . . ? N10 Zn2 N8 134.91(17) . . ? N7 Zn2 N8 62.47(16) . . ? O1 Zn2 N11 109.99(16) . . ? N10 Zn2 N11 62.59(18) . . ? N7 Zn2 N11 136.61(16) . . ? N8 Zn2 N11 90.14(17) . . ? O3' Cl1 O4' 118(3) . . ? O3' Cl1 O5 118(5) . . ? O4' Cl1 O5 83(3) . . ? O3' Cl1 O2 113(5) . . ? O4' Cl1 O2 106.8(14) . . ? O5 Cl1 O2 114.1(13) . . ? O3' Cl1 O4 88(3) . . ? O4' Cl1 O4 34(4) . . ? O5 Cl1 O4 110.9(9) . . ? O2 Cl1 O4 109.6(6) . . ? O3' Cl1 O5' 110(5) . . ? O4' Cl1 O5' 105(3) . . ? O5 Cl1 O5' 23(2) . . ? O2 Cl1 O5' 101(4) . . ? O4 Cl1 O5' 134(2) . . ? O3' Cl1 O3 17(4) . . ? O4' Cl1 O3 134(4) . . ? O5 Cl1 O3 108(2) . . ? O2 Cl1 O3 108.3(19) . . ? O4 Cl1 O3 105.5(15) . . ? O5' Cl1 O3 96(3) . . ? O9 Cl2 O7 111.1(4) . . ? O9 Cl2 O6 110.1(3) . . ? O7 Cl2 O6 106.5(3) . . ? O9 Cl2 O8 109.3(3) . . ? O7 Cl2 O8 109.1(3) . . ? O6 Cl2 O8 110.7(3) . . ? O13 Cl3 O11 116.3(7) . . ? O13 Cl3 O13' 150.9(14) . . ? O11 Cl3 O13' 54.9(14) . . ? O13 Cl3 O12' 41.3(13) . . ? O11 Cl3 O12' 86.7(15) . . ? O13' Cl3 O12' 110(2) . . ? O13 Cl3 O11' 82.5(11) . . ? O11 Cl3 O11' 161.1(11) . . ? O13' Cl3 O11' 109.8(18) . . ? O12' Cl3 O11' 110.7(18) . . ? O13 Cl3 O10 111.0(7) . . ? O11 Cl3 O10 107.5(7) . . ? O13' Cl3 O10 56.7(14) . . ? O12' Cl3 O10 96.1(16) . . ? O11' Cl3 O10 64.5(12) . . ? O13 Cl3 O12 109.8(7) . . ? O11 Cl3 O12 106.2(7) . . ? O13' Cl3 O12 99.2(13) . . ? O12' Cl3 O12 149.8(17) . . ? O11' Cl3 O12 62.5(12) . . ? O10 Cl3 O12 105.4(8) . . ? O13 Cl3 O10' 92.0(11) . . ? O11 Cl3 O10' 71.0(12) . . ? O13' Cl3 O10' 108.0(17) . . ? O12' Cl3 O10' 109.9(19) . . ? O11' Cl3 O10' 108.1(18) . . ? O10 Cl3 O10' 153.7(12) . . ? O12 Cl3 O10' 52.7(11) . . ? C8 N1 C1 118.1(5) . . ? C8 N1 Zn1 150.4(4) . . ? C1 N1 Zn1 91.2(3) . . ? C2 N2 C1 118.2(5) . . ? C2 N2 Zn1 146.5(4) . . ? C1 N2 Zn1 94.0(3) . . ? C2 N3 C19 127.1(5) . . ? C2 N3 H3 116.5 . . ? C19 N3 H3 116.5 . . ? C17 N4 C10 119.5(5) . . ? C17 N4 Zn1 144.1(4) . . ? C10 N4 Zn1 96.3(3) . . ? C11 N5 C10 118.2(5) . . ? C11 N5 Zn1 152.0(4) . . ? C10 N5 Zn1 89.8(3) . . ? C11 N6 C19 123.3(5) . . ? C11 N6 H6 118.4 . . ? C19 N6 H6 118.4 . . ? C27 N7 C20 119.0(5) . . ? C27 N7 Zn2 146.7(4) . . ? C20 N7 Zn2 94.1(3) . . ? C21 N8 C20 118.4(5) . . ? C21 N8 Zn2 150.1(4) . . ? C20 N8 Zn2 91.3(3) . . ? C21 N9 C38 125.4(5) . . ? C21 N9 H9 117.3 . . ? C38 N9 H9 117.3 . . ? C36 N10 C29 118.3(5) . . ? C36 N10 Zn2 146.3(4) . . ? C29 N10 Zn2 94.9(3) . . ? C30 N11 C29 117.7(5) . . ? C30 N11 Zn2 151.0(4) . . ? C29 N11 Zn2 90.6(3) . . ? C30 N12 C38 125.6(5) . . ? C30 N12 H12 117.2 . . ? C38 N12 H12 117.2 . . ? Zn1 O1 Zn2 135.22(19) . . ? Zn1 O1 H1 112.4 . . ? Zn2 O1 H1 112.4 . . ? N1 C1 N2 111.1(5) . . ? N1 C1 C5 124.7(6) . . ? N2 C1 C5 124.2(6) . . ? N2 C2 N3 120.7(6) . . ? N2 C2 C3 120.7(6) . . ? N3 C2 C3 118.6(6) . . ? C4 C3 C2 119.5(7) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 121.4(7) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C1 C5 C4 115.7(6) . . ? C1 C5 C6 115.2(6) . . ? C4 C5 C6 129.1(7) . . ? C7 C6 C5 120.5(6) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C8 121.0(6) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? N1 C8 C7 120.4(6) . . ? N1 C8 C9 118.0(6) . . ? C7 C8 C9 121.6(6) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 C10 N5 112.6(5) . . ? N4 C10 C14 124.0(6) . . ? N5 C10 C14 123.3(6) . . ? N5 C11 N6 118.0(6) . . ? N5 C11 C12 121.6(6) . . ? N6 C11 C12 120.4(6) . . ? C13 C12 C11 120.5(6) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C12 C13 C14 119.8(6) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C10 C14 C15 114.8(6) . . ? C10 C14 C13 116.6(6) . . ? C15 C14 C13 128.6(6) . . ? C16 C15 C14 121.4(6) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C17 120.0(7) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? N4 C17 C16 120.2(6) . . ? N4 C17 C18 117.6(6) . . ? C16 C17 C18 122.2(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 . . ? N6 C19 N3 114.3(5) . . ? N6 C19 H19A 108.7 . . ? N3 C19 H19A 108.7 . . ? N6 C19 H19B 108.7 . . ? N3 C19 H19B 108.7 . . ? H19A C19 H19B 107.6 . . ? N7 C20 N8 112.1(5) . . ? N7 C20 C24 123.5(5) . . ? N8 C20 C24 124.4(5) . . ? N8 C21 N9 120.5(5) . . ? N8 C21 C22 121.0(6) . . ? N9 C21 C22 118.5(6) . . ? C23 C22 C21 119.7(6) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.9(6) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C20 117.2(6) . . ? C25 C24 C23 127.3(6) . . ? C20 C24 C23 115.5(6) . . ? C26 C25 C24 119.5(6) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 120.6(6) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? N7 C27 C26 120.3(5) . . ? N7 C27 C28 118.8(5) . . ? C26 C27 C28 120.9(6) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N10 C29 N11 111.8(5) . . ? N10 C29 C33 123.8(6) . . ? N11 C29 C33 124.4(6) . . ? N11 C30 N12 119.6(6) . . ? N11 C30 C31 121.2(6) . . ? N12 C30 C31 119.1(6) . . ? C32 C31 C30 120.1(7) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.5(6) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C29 117.1(7) . . ? C34 C33 C32 127.1(7) . . ? C29 C33 C32 115.8(6) . . ? C35 C34 C33 119.7(7) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 120.9(6) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? N10 C36 C35 120.1(6) . . ? N10 C36 C37 118.5(6) . . ? C35 C36 C37 121.5(6) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N9 C38 N12 115.5(5) . . ? N9 C38 H38A 108.4 . . ? N12 C38 H38A 108.4 . . ? N9 C38 H38B 108.4 . . ? N12 C38 H38B 108.4 . . ? H38A C38 H38B 107.5 . . ? 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 O1 Zn1 N1 C8 61.3(8) . . . . ? N2 Zn1 N1 C8 -176.6(8) . . . . ? N4 Zn1 N1 C8 -60.8(8) . . . . ? N5 Zn1 N1 C8 -127.6(7) . . . . ? O1 Zn1 N1 C1 -127.1(3) . . . . ? N2 Zn1 N1 C1 -5.0(3) . . . . ? N4 Zn1 N1 C1 110.8(3) . . . . ? N5 Zn1 N1 C1 43.9(4) . . . . ? O1 Zn1 N2 C2 -88.0(7) . . . . ? N4 Zn1 N2 C2 73.0(7) . . . . ? N1 Zn1 N2 C2 169.2(7) . . . . ? N5 Zn1 N2 C2 18.9(7) . . . . ? O1 Zn1 N2 C1 107.8(3) . . . . ? N4 Zn1 N2 C1 -91.2(3) . . . . ? N1 Zn1 N2 C1 5.0(3) . . . . ? N5 Zn1 N2 C1 -145.3(3) . . . . ? O1 Zn1 N4 C17 -82.0(7) . . . . ? N2 Zn1 N4 C17 113.6(6) . . . . ? N1 Zn1 N4 C17 44.6(7) . . . . ? N5 Zn1 N4 C17 -178.9(7) . . . . ? O1 Zn1 N4 C10 95.4(3) . . . . ? N2 Zn1 N4 C10 -69.0(4) . . . . ? N1 Zn1 N4 C10 -138.0(3) . . . . ? N5 Zn1 N4 C10 -1.6(3) . . . . ? O1 Zn1 N5 C11 79.4(8) . . . . ? N2 Zn1 N5 C11 -49.9(8) . . . . ? N4 Zn1 N5 C11 -177.2(9) . . . . ? N1 Zn1 N5 C11 -92.2(8) . . . . ? O1 Zn1 N5 C10 -101.8(3) . . . . ? N2 Zn1 N5 C10 128.9(3) . . . . ? N4 Zn1 N5 C10 1.6(3) . . . . ? N1 Zn1 N5 C10 86.6(4) . . . . ? O1 Zn2 N7 C27 79.6(7) . . . . ? N10 Zn2 N7 C27 -44.2(7) . . . . ? N8 Zn2 N7 C27 -174.4(7) . . . . ? N11 Zn2 N7 C27 -117.6(7) . . . . ? O1 Zn2 N7 C20 -106.3(3) . . . . ? N10 Zn2 N7 C20 129.8(3) . . . . ? N8 Zn2 N7 C20 -0.4(3) . . . . ? N11 Zn2 N7 C20 56.5(4) . . . . ? O1 Zn2 N8 C21 -81.8(8) . . . . ? N10 Zn2 N8 C21 79.7(8) . . . . ? N7 Zn2 N8 C21 175.0(8) . . . . ? N11 Zn2 N8 C21 30.1(8) . . . . ? O1 Zn2 N8 C20 103.5(3) . . . . ? N10 Zn2 N8 C20 -94.9(4) . . . . ? N7 Zn2 N8 C20 0.4(3) . . . . ? N11 Zn2 N8 C20 -144.5(3) . . . . ? O1 Zn2 N10 C36 -83.8(7) . . . . ? N7 Zn2 N10 C36 41.1(7) . . . . ? N8 Zn2 N10 C36 114.1(7) . . . . ? N11 Zn2 N10 C36 173.3(8) . . . . ? O1 Zn2 N10 C29 105.3(3) . . . . ? N7 Zn2 N10 C29 -129.8(3) . . . . ? N8 Zn2 N10 C29 -56.8(4) . . . . ? N11 Zn2 N10 C29 2.4(3) . . . . ? O1 Zn2 N11 C30 87.8(8) . . . . ? N10 Zn2 N11 C30 -169.9(8) . . . . ? N7 Zn2 N11 C30 -75.2(8) . . . . ? N8 Zn2 N11 C30 -27.3(8) . . . . ? O1 Zn2 N11 C29 -104.7(3) . . . . ? N10 Zn2 N11 C29 -2.3(3) . . . . ? N7 Zn2 N11 C29 92.3(4) . . . . ? N8 Zn2 N11 C29 140.2(3) . . . . ? N2 Zn1 O1 Zn2 123.0(3) . . . . ? N4 Zn1 O1 Zn2 -39.8(3) . . . . ? N1 Zn1 O1 Zn2 -161.8(3) . . . . ? N5 Zn1 O1 Zn2 24.2(3) . . . . ? N10 Zn2 O1 Zn1 -44.0(3) . . . . ? N7 Zn2 O1 Zn1 -169.5(3) . . . . ? N8 Zn2 O1 Zn1 122.2(3) . . . . ? N11 Zn2 O1 Zn1 23.0(3) . . . . ? C8 N1 C1 N2 -177.3(4) . . . . ? Zn1 N1 C1 N2 7.4(4) . . . . ? C8 N1 C1 C5 3.6(8) . . . . ? Zn1 N1 C1 C5 -171.7(5) . . . . ? C2 N2 C1 N1 -177.9(4) . . . . ? Zn1 N2 C1 N1 -7.7(4) . . . . ? C2 N2 C1 C5 1.3(8) . . . . ? Zn1 N2 C1 C5 171.4(5) . . . . ? C1 N2 C2 N3 -178.1(5) . . . . ? Zn1 N2 C2 N3 19.8(10) . . . . ? C1 N2 C2 C3 3.8(7) . . . . ? Zn1 N2 C2 C3 -158.2(5) . . . . ? C19 N3 C2 N2 13.2(9) . . . . ? C19 N3 C2 C3 -168.7(5) . . . . ? N2 C2 C3 C4 -6.0(9) . . . . ? N3 C2 C3 C4 175.9(6) . . . . ? C2 C3 C4 C5 3.0(9) . . . . ? N1 C1 C5 C4 175.0(5) . . . . ? N2 C1 C5 C4 -4.1(8) . . . . ? N1 C1 C5 C6 -2.9(8) . . . . ? N2 C1 C5 C6 178.1(5) . . . . ? C3 C4 C5 C1 1.7(9) . . . . ? C3 C4 C5 C6 179.2(6) . . . . ? C1 C5 C6 C7 -0.5(8) . . . . ? C4 C5 C6 C7 -177.9(6) . . . . ? C5 C6 C7 C8 2.9(9) . . . . ? C1 N1 C8 C7 -1.0(8) . . . . ? Zn1 N1 C8 C7 169.5(5) . . . . ? C1 N1 C8 C9 179.6(5) . . . . ? Zn1 N1 C8 C9 -10.0(10) . . . . ? C6 C7 C8 N1 -2.2(9) . . . . ? C6 C7 C8 C9 177.2(6) . . . . ? C17 N4 C10 N5 -179.3(5) . . . . ? Zn1 N4 C10 N5 2.5(5) . . . . ? C17 N4 C10 C14 -0.5(8) . . . . ? Zn1 N4 C10 C14 -178.7(5) . . . . ? C11 N5 C10 N4 177.0(5) . . . . ? Zn1 N5 C10 N4 -2.3(4) . . . . ? C11 N5 C10 C14 -1.7(8) . . . . ? Zn1 N5 C10 C14 178.9(5) . . . . ? C10 N5 C11 N6 -177.4(5) . . . . ? Zn1 N5 C11 N6 1.2(11) . . . . ? C10 N5 C11 C12 1.9(8) . . . . ? Zn1 N5 C11 C12 -179.5(5) . . . . ? C19 N6 C11 N5 12.5(9) . . . . ? C19 N6 C11 C12 -166.7(6) . . . . ? N5 C11 C12 C13 -0.5(9) . . . . ? N6 C11 C12 C13 178.8(6) . . . . ? C11 C12 C13 C14 -1.1(10) . . . . ? N4 C10 C14 C15 2.3(8) . . . . ? N5 C10 C14 C15 -179.0(5) . . . . ? N4 C10 C14 C13 -178.4(5) . . . . ? N5 C10 C14 C13 0.2(8) . . . . ? C12 C13 C14 C10 1.2(9) . . . . ? C12 C13 C14 C15 -179.7(6) . . . . ? C10 C14 C15 C16 -2.9(9) . . . . ? C13 C14 C15 C16 177.9(6) . . . . ? C14 C15 C16 C17 1.8(11) . . . . ? C10 N4 C17 C16 -0.8(8) . . . . ? Zn1 N4 C17 C16 176.1(5) . . . . ? C10 N4 C17 C18 177.2(5) . . . . ? Zn1 N4 C17 C18 -5.8(10) . . . . ? C15 C16 C17 N4 0.2(10) . . . . ? C15 C16 C17 C18 -177.7(6) . . . . ? C11 N6 C19 N3 75.8(7) . . . . ? C2 N3 C19 N6 -111.7(7) . . . . ? C27 N7 C20 N8 176.8(5) . . . . ? Zn2 N7 C20 N8 0.6(5) . . . . ? C27 N7 C20 C24 -1.4(8) . . . . ? Zn2 N7 C20 C24 -177.7(5) . . . . ? C21 N8 C20 N7 -177.5(5) . . . . ? Zn2 N8 C20 N7 -0.5(4) . . . . ? C21 N8 C20 C24 0.7(8) . . . . ? Zn2 N8 C20 C24 177.7(5) . . . . ? C20 N8 C21 N9 177.1(5) . . . . ? Zn2 N8 C21 N9 3.2(12) . . . . ? C20 N8 C21 C22 -2.2(8) . . . . ? Zn2 N8 C21 C22 -176.2(5) . . . . ? C38 N9 C21 N8 11.8(9) . . . . ? C38 N9 C21 C22 -168.8(6) . . . . ? N8 C21 C22 C23 1.3(9) . . . . ? N9 C21 C22 C23 -178.1(6) . . . . ? C21 C22 C23 C24 1.2(9) . . . . ? N7 C20 C24 C25 1.6(8) . . . . ? N8 C20 C24 C25 -176.4(5) . . . . ? N7 C20 C24 C23 179.7(5) . . . . ? N8 C20 C24 C23 1.7(8) . . . . ? C22 C23 C24 C25 175.3(6) . . . . ? C22 C23 C24 C20 -2.6(9) . . . . ? C20 C24 C25 C26 -0.2(9) . . . . ? C23 C24 C25 C26 -178.1(6) . . . . ? C24 C25 C26 C27 -1.3(9) . . . . ? C20 N7 C27 C26 -0.1(8) . . . . ? Zn2 N7 C27 C26 173.1(5) . . . . ? C20 N7 C27 C28 179.7(5) . . . . ? Zn2 N7 C27 C28 -7.1(10) . . . . ? C25 C26 C27 N7 1.5(9) . . . . ? C25 C26 C27 C28 -178.4(6) . . . . ? C36 N10 C29 N11 -178.0(5) . . . . ? Zn2 N10 C29 N11 -3.7(5) . . . . ? C36 N10 C29 C33 0.3(8) . . . . ? Zn2 N10 C29 C33 174.5(5) . . . . ? C30 N11 C29 N10 176.7(5) . . . . ? Zn2 N11 C29 N10 3.5(4) . . . . ? C30 N11 C29 C33 -1.5(8) . . . . ? Zn2 N11 C29 C33 -174.7(5) . . . . ? C29 N11 C30 N12 -177.7(5) . . . . ? Zn2 N11 C30 N12 -11.8(12) . . . . ? C29 N11 C30 C31 5.6(8) . . . . ? Zn2 N11 C30 C31 171.4(6) . . . . ? C38 N12 C30 N11 -0.9(9) . . . . ? C38 N12 C30 C31 175.9(6) . . . . ? N11 C30 C31 C32 -4.4(10) . . . . ? N12 C30 C31 C32 178.9(6) . . . . ? C30 C31 C32 C33 -1.1(10) . . . . ? N10 C29 C33 C34 -1.6(9) . . . . ? N11 C29 C33 C34 176.4(5) . . . . ? N10 C29 C33 C32 178.4(5) . . . . ? N11 C29 C33 C32 -3.6(9) . . . . ? C31 C32 C33 C34 -175.2(6) . . . . ? C31 C32 C33 C29 4.9(9) . . . . ? C29 C33 C34 C35 0.4(9) . . . . ? C32 C33 C34 C35 -179.5(6) . . . . ? C33 C34 C35 C36 2.0(10) . . . . ? C29 N10 C36 C35 2.1(8) . . . . ? Zn2 N10 C36 C35 -167.5(5) . . . . ? C29 N10 C36 C37 -177.7(5) . . . . ? Zn2 N10 C36 C37 12.6(10) . . . . ? C34 C35 C36 N10 -3.3(10) . . . . ? C34 C35 C36 C37 176.5(6) . . . . ? C21 N9 C38 N12 -103.8(7) . . . . ? C30 N12 C38 N9 95.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.621 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.080 #===END ## Crystallographic Data of complex 2 data_2 _database_code_depnum_ccdc_archive 'CCDC 690020' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H52 N12 O14 Zn4, C H2 Cl2' _chemical_formula_sum 'C51 H54 Cl2 N12 O14 Zn4' _chemical_formula_weight 1391.52 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 monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall -P2yn 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 18.411(2) _cell_length_b 8.6379(8) _cell_length_c 19.976(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.311(2) _cell_angle_gamma 90.00 _cell_volume 2998.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3097 _cell_measurement_theta_min 2.595 _cell_measurement_theta_max 25.25 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 1.742 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.708 _exptl_absorpt_correction_T_max 0.840 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14847 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5293 _reflns_number_gt 2786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0622P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5225 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.105 _refine_ls_shift/su_mean 0.003 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 0.34512(3) 0.39270(7) 0.12676(3) 0.0543(2) Uani 1 1 d . . . Zn2 Zn 0.26042(4) 0.60514(10) -0.02503(3) 0.0764(3) Uani 1 1 d . . . N1 N 0.3337(3) 0.1607(5) 0.1379(2) 0.0638(12) Uani 1 1 d . . . N2 N 0.4416(3) 0.1727(5) 0.1042(2) 0.0622(12) Uani 1 1 d . . . N3 N 0.5481(3) 0.1891(7) 0.0707(3) 0.0768(14) Uani 1 1 d . . . N4 N 0.1991(3) 0.4951(6) -0.1211(3) 0.0731(14) Uani 1 1 d . . . N5 N 0.3229(3) 0.5175(5) -0.1204(2) 0.0642(12) Uani 1 1 d . . . N6 N 0.4504(3) 0.5486(6) -0.1151(3) 0.0763(14) Uani 1 1 d . . . O1 O 0.3374(2) 0.4665(5) 0.03363(18) 0.0738(11) Uani 1 1 d . . . H1 H 0.3746 0.4317 0.0151 0.089 Uiso 1 1 calc R . . O2 O 0.2550(2) 0.5076(5) 0.1364(2) 0.0728(11) Uani 1 1 d . . . O3 O 0.1914(3) 0.6152(7) 0.0337(3) 0.1171(19) Uani 1 1 d . . . O4 O 0.4392(2) 0.4854(4) 0.19636(19) 0.0650(10) Uani 1 1 d . . . O5 O 0.3912(3) 0.3832(6) 0.2732(3) 0.1165(18) Uani 1 1 d . . . O6 O 0.3039(3) 0.8164(7) -0.0360(3) 0.1040(15) Uani 1 1 d . . . O7 O 0.1825(10) 0.8469(15) -0.0778(7) 0.154(6) Uani 0.65(2) 1 d P A 1 Cl1 Cl 0.0381(3) 0.1390(5) 0.00707(18) 0.261(2) Uani 1 1 d . . . C1 C 0.3933(4) 0.0842(6) 0.1271(3) 0.0616(15) Uani 1 1 d . . . C2 C 0.4996(4) 0.1017(8) 0.0924(3) 0.0692(15) Uani 1 1 d . . . C3 C 0.5137(5) -0.0626(8) 0.1017(4) 0.089(2) Uani 1 1 d . . . H3 H 0.5553 -0.1086 0.0928 0.107 Uiso 1 1 calc R . . C4 C 0.4642(5) -0.1469(8) 0.1239(4) 0.103(2) Uani 1 1 d . . . H4 H 0.4721 -0.2529 0.1306 0.123 Uiso 1 1 calc R . . C5 C 0.4016(4) -0.0798(7) 0.1370(3) 0.0823(19) Uani 1 1 d . . . C6 C 0.3471(5) -0.1536(8) 0.1604(4) 0.103(2) Uani 1 1 d . . . H6 H 0.3509 -0.2598 0.1683 0.124 Uiso 1 1 calc R . . C7 C 0.2887(5) -0.0750(8) 0.1719(4) 0.098(2) Uani 1 1 d . . . H7 H 0.2525 -0.1274 0.1866 0.117 Uiso 1 1 calc R . . C8 C 0.2832(4) 0.0823(7) 0.1617(3) 0.0761(18) Uani 1 1 d . . . C9 C 0.2207(4) 0.1690(9) 0.1754(4) 0.104(2) Uani 1 1 d . . . H9A H 0.1768 0.1025 0.1677 0.155 Uiso 1 1 calc R . . H9B H 0.2066 0.2560 0.1438 0.155 Uiso 1 1 calc R . . H9C H 0.2377 0.2049 0.2236 0.155 Uiso 1 1 calc R . . C10 C 0.2518(4) 0.4634(7) -0.1546(3) 0.0654(15) Uani 1 1 d . . . C11 C 0.3788(4) 0.4911(7) -0.1491(3) 0.0691(17) Uani 1 1 d . . . C12 C 0.3639(5) 0.4099(9) -0.2123(4) 0.097(2) Uani 1 1 d . . . H12 H 0.4037 0.3905 -0.2302 0.116 Uiso 1 1 calc R . . C13 C 0.2933(7) 0.3595(9) -0.2475(4) 0.108(3) Uani 1 1 d . . . H13 H 0.2837 0.3083 -0.2905 0.130 Uiso 1 1 calc R . . C14 C 0.2317(5) 0.3837(8) -0.2195(4) 0.091(2) Uani 1 1 d . . . C15 C 0.1561(7) 0.3408(11) -0.2484(5) 0.131(3) Uani 1 1 d . . . H15 H 0.1406 0.2849 -0.2906 0.157 Uiso 1 1 calc R . . C16 C 0.1038(6) 0.3771(12) -0.2176(5) 0.129(4) Uani 1 1 d . . . H16 H 0.0523 0.3514 -0.2397 0.155 Uiso 1 1 calc R . . C17 C 0.1268(4) 0.4545(10) -0.1517(4) 0.103(2) Uani 1 1 d . . . C18 C 0.0712(4) 0.4938(13) -0.1138(5) 0.148(4) Uani 1 1 d . . . H18A H 0.0772 0.4216 -0.0758 0.222 Uiso 1 1 calc R . . H18B H 0.0196 0.4883 -0.1464 0.222 Uiso 1 1 calc R . . H18C H 0.0814 0.5967 -0.0948 0.222 Uiso 1 1 calc R . . C19 C 0.1972(4) 0.5662(9) 0.0937(4) 0.0813(19) Uani 1 1 d . . . C20 C 0.1269(4) 0.5885(11) 0.1174(4) 0.130(3) Uani 1 1 d . . . H20A H 0.1124 0.4908 0.1321 0.195 Uiso 1 1 calc R . . H20B H 0.0850 0.6287 0.0786 0.195 Uiso 1 1 calc R . . H20C H 0.1393 0.6600 0.1564 0.195 Uiso 1 1 calc R . . C21 C 0.4382(3) 0.4616(8) 0.2579(3) 0.0684(16) Uani 1 1 d . . . C22 C 0.4985(5) 0.5357(14) 0.3173(4) 0.166(5) Uani 1 1 d . . . H22A H 0.4849 0.5281 0.3596 0.248 Uiso 1 1 calc R . . H22B H 0.5029 0.6428 0.3063 0.248 Uiso 1 1 calc R . . H22C H 0.5467 0.4846 0.3245 0.248 Uiso 1 1 calc R . . C23 C 0.247(3) 0.899(5) -0.0587(11) 0.068(13) Uani 0.48(12) 1 d P A 1 C24 C 0.2558(18) 1.072(2) -0.0699(11) 0.152(13) Uani 0.64(4) 1 d P A 1 H24A H 0.3048 1.1065 -0.0387 0.228 Uiso 0.64(4) 1 calc PR A 1 H24B H 0.2155 1.1276 -0.0598 0.228 Uiso 0.64(4) 1 calc PR A 1 H24C H 0.2525 1.0901 -0.1182 0.228 Uiso 0.64(4) 1 calc PR A 1 C34 C 0.5341(3) 0.3495(8) 0.0546(3) 0.0706(17) Uani 1 1 d . . . H34A H 0.4806 0.3621 0.0254 0.085 Uiso 1 1 calc R . . H34B H 0.5654 0.3822 0.0265 0.085 Uiso 1 1 calc R . . C25 C 0.0698(14) -0.061(2) 0.0248(12) 0.163(8) Uani 0.50 1 d P . . H25A H 0.0973 -0.0816 0.0745 0.195 Uiso 0.50 1 calc PR . . H25B H 0.0991 -0.0975 -0.0045 0.195 Uiso 0.50 1 calc PR . . O8 O 0.3343(11) 1.061(3) -0.0504(11) 0.115(9) Uani 0.35(2) 1 d P A 2 C27 C 0.2139(15) 1.002(4) -0.0398(17) 0.103(14) Uani 0.36(4) 1 d P A 2 H27A H 0.2108 1.1122 -0.0375 0.155 Uiso 0.36(4) 1 calc PR A 2 H27B H 0.2083 0.9569 0.0022 0.155 Uiso 0.36(4) 1 calc PR A 2 H27C H 0.1735 0.9643 -0.0807 0.155 Uiso 0.36(4) 1 calc PR A 2 C26 C 0.289(5) 0.957(6) -0.0452(19) 0.09(2) Uani 0.52(12) 1 d P A 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 0.0606(4) 0.0487(4) 0.0545(4) 0.0052(3) 0.0201(3) -0.0050(3) Zn2 0.0682(5) 0.1003(6) 0.0547(4) 0.0138(4) 0.0124(3) 0.0132(4) N1 0.089(3) 0.046(3) 0.062(3) -0.008(2) 0.031(3) -0.011(3) N2 0.073(3) 0.054(3) 0.062(3) -0.005(2) 0.027(2) 0.012(3) N3 0.072(3) 0.087(4) 0.067(3) 0.001(3) 0.019(3) 0.023(3) N4 0.045(3) 0.092(4) 0.068(3) 0.006(3) 0.000(2) 0.001(3) N5 0.066(3) 0.073(3) 0.054(3) 0.006(2) 0.021(2) 0.004(3) N6 0.071(4) 0.077(4) 0.091(4) 0.005(3) 0.041(3) 0.009(3) O1 0.054(2) 0.114(3) 0.058(2) 0.030(2) 0.0249(19) 0.022(2) O2 0.067(3) 0.081(3) 0.081(3) 0.001(2) 0.039(2) 0.003(2) O3 0.068(3) 0.188(6) 0.098(4) 0.024(4) 0.031(3) 0.047(3) O4 0.069(3) 0.069(2) 0.058(2) -0.006(2) 0.022(2) 0.004(2) O5 0.140(5) 0.114(4) 0.108(4) 0.002(3) 0.058(4) -0.032(4) O6 0.089(4) 0.119(5) 0.104(4) -0.002(3) 0.032(3) 0.025(3) O7 0.145(13) 0.135(11) 0.196(12) 0.003(8) 0.075(10) 0.004(8) Cl1 0.402(7) 0.232(5) 0.119(2) 0.017(3) 0.042(3) -0.019(4) C1 0.083(4) 0.041(3) 0.054(3) -0.008(3) 0.014(3) -0.009(3) C2 0.077(4) 0.068(4) 0.059(3) -0.008(3) 0.019(3) 0.003(4) C3 0.096(5) 0.079(5) 0.087(5) -0.017(4) 0.021(4) 0.034(4) C4 0.132(7) 0.065(5) 0.104(6) -0.013(4) 0.029(5) 0.015(5) C5 0.104(5) 0.056(4) 0.085(4) -0.012(3) 0.027(4) 0.002(4) C6 0.135(7) 0.044(4) 0.122(6) 0.006(4) 0.031(6) -0.027(5) C7 0.118(7) 0.066(5) 0.106(6) 0.011(4) 0.033(5) -0.025(4) C8 0.092(5) 0.060(4) 0.079(4) 0.000(3) 0.031(4) -0.027(4) C9 0.105(6) 0.101(5) 0.127(6) -0.002(5) 0.068(5) -0.026(5) C10 0.073(4) 0.064(4) 0.052(3) 0.010(3) 0.012(3) 0.003(3) C11 0.100(5) 0.062(4) 0.057(3) 0.013(3) 0.041(4) 0.021(4) C12 0.120(7) 0.090(5) 0.090(5) 0.007(5) 0.048(5) 0.021(5) C13 0.182(9) 0.083(6) 0.063(4) -0.007(4) 0.048(6) 0.015(6) C14 0.109(6) 0.080(5) 0.063(4) 0.001(4) -0.002(4) -0.005(5) C15 0.152(10) 0.107(7) 0.092(6) -0.016(5) -0.016(7) -0.002(7) C16 0.105(7) 0.124(8) 0.101(7) 0.017(6) -0.045(6) -0.029(6) C17 0.064(5) 0.123(6) 0.102(6) 0.040(5) 0.001(4) -0.003(4) C18 0.046(4) 0.221(11) 0.155(8) 0.057(8) 0.003(5) -0.016(6) C19 0.064(4) 0.098(5) 0.091(5) -0.016(4) 0.039(4) -0.004(4) C20 0.065(5) 0.211(10) 0.129(6) -0.029(6) 0.054(5) 0.006(5) C21 0.061(4) 0.077(4) 0.071(4) -0.008(3) 0.027(3) 0.001(3) C22 0.133(7) 0.289(14) 0.082(5) -0.067(7) 0.045(5) -0.093(8) C23 0.05(2) 0.087(17) 0.063(10) -0.014(12) 0.018(10) 0.011(18) C24 0.21(3) 0.095(14) 0.116(13) 0.003(10) -0.001(16) -0.026(15) C34 0.056(4) 0.097(5) 0.067(4) 0.019(3) 0.031(3) 0.002(3) C25 0.21(2) 0.113(15) 0.154(17) -0.019(13) 0.046(16) -0.067(15) O8 0.074(13) 0.139(18) 0.140(15) -0.013(12) 0.049(11) -0.019(11) C27 0.084(18) 0.10(3) 0.12(2) -0.002(18) 0.022(15) 0.026(16) C26 0.11(5) 0.08(3) 0.087(13) 0.026(13) 0.02(2) 0.03(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 1.927(3) . ? Zn1 O4 1.996(4) . ? Zn1 O2 1.996(4) . ? Zn1 N1 2.035(4) . ? Zn2 O1 1.928(4) . ? Zn2 O3 1.996(5) . ? Zn2 O6 2.034(7) . ? Zn2 N4 2.105(5) . ? N1 C8 1.358(7) . ? N1 C1 1.359(7) . ? N2 C2 1.319(7) . ? N2 C1 1.359(7) . ? N3 C2 1.346(7) . ? N3 C34 1.427(8) . ? N4 C17 1.317(8) . ? N4 C10 1.375(7) . ? N5 C10 1.345(7) . ? N5 C11 1.353(7) . ? N6 C11 1.361(8) . ? N6 C34 1.445(8) 3_665 ? O1 H1 0.9300 . ? O2 C19 1.231(8) . ? O3 C19 1.242(8) . ? O4 C21 1.252(7) . ? O5 C21 1.215(7) . ? O6 C23 1.22(2) . ? O6 C26 1.25(4) . ? O7 C23 1.21(7) . ? Cl1 C25 1.82(2) . ? Cl1 C25 1.99(2) 3 ? C1 C5 1.431(8) . ? C2 C3 1.444(9) . ? C3 C4 1.352(10) . ? C3 H3 0.9300 . ? C4 C5 1.390(10) . ? C4 H4 0.9300 . ? C5 C6 1.393(10) . ? C6 C7 1.353(10) . ? C6 H6 0.9300 . ? C7 C8 1.373(9) . ? C7 H7 0.9300 . ? C8 C9 1.473(9) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C14 1.404(9) . ? C11 C12 1.390(9) . ? C12 C13 1.331(11) . ? C12 H12 0.9300 . ? C13 C14 1.437(11) . ? C13 H13 0.9300 . ? C14 C15 1.370(12) . ? C15 C16 1.340(12) . ? C15 H15 0.9300 . ? C16 C17 1.410(12) . ? C16 H16 0.9300 . ? C17 C18 1.500(12) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.530(8) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.475(9) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.53(5) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C34 N6 1.445(8) 3_665 ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C25 Cl1 1.99(2) 3 ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? O8 C26 1.25(9) . ? C27 C26 1.48(6) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? 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 108.03(16) . . ? O1 Zn1 O2 97.47(16) . . ? O4 Zn1 O2 106.92(16) . . ? O1 Zn1 N1 117.01(18) . . ? O4 Zn1 N1 114.60(18) . . ? O2 Zn1 N1 111.12(19) . . ? O1 Zn2 O3 98.79(18) . . ? O1 Zn2 O6 112.72(19) . . ? O3 Zn2 O6 112.0(2) . . ? O1 Zn2 N4 109.79(19) . . ? O3 Zn2 N4 107.6(2) . . ? O6 Zn2 N4 114.7(2) . . ? C8 N1 C1 119.8(5) . . ? C8 N1 Zn1 129.6(4) . . ? C1 N1 Zn1 110.1(4) . . ? C2 N2 C1 117.2(5) . . ? C2 N3 C34 121.9(5) . . ? C17 N4 C10 119.3(6) . . ? C17 N4 Zn2 134.3(6) . . ? C10 N4 Zn2 106.4(4) . . ? C10 N5 C11 118.3(5) . . ? C11 N6 C34 122.1(5) . 3_665 ? Zn1 O1 Zn2 126.64(19) . . ? Zn1 O1 H1 116.7 . . ? Zn2 O1 H1 116.7 . . ? C19 O2 Zn1 134.0(4) . . ? C19 O3 Zn2 133.2(4) . . ? C21 O4 Zn1 109.1(4) . . ? C23 O6 C26 42.2(16) . . ? C23 O6 Zn2 104(3) . . ? C26 O6 Zn2 145(4) . . ? C25 Cl1 C25 87.9(11) . 3 ? N1 C1 N2 115.6(5) . . ? N1 C1 C5 120.9(6) . . ? N2 C1 C5 123.5(6) . . ? N2 C2 N3 117.4(6) . . ? N2 C2 C3 123.8(6) . . ? N3 C2 C3 118.9(6) . . ? C4 C3 C2 117.3(7) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C5 121.9(7) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C4 C5 C6 127.3(7) . . ? C4 C5 C1 116.3(7) . . ? C6 C5 C1 116.4(7) . . ? C7 C6 C5 121.9(7) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C8 119.7(7) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? N1 C8 C7 121.3(7) . . ? N1 C8 C9 118.7(6) . . ? C7 C8 C9 120.0(7) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 N4 114.1(5) . . ? N5 C10 C14 123.7(6) . . ? N4 C10 C14 122.2(6) . . ? N5 C11 N6 118.2(5) . . ? N5 C11 C12 121.4(7) . . ? N6 C11 C12 120.4(6) . . ? C13 C12 C11 120.6(7) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.4(7) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C10 116.3(8) . . ? C15 C14 C13 128.2(9) . . ? C10 C14 C13 115.4(7) . . ? C16 C15 C14 121.8(9) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 120.0(8) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? N4 C17 C16 120.3(8) . . ? N4 C17 C18 117.3(8) . . ? C16 C17 C18 122.4(8) . . ? 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 . . ? O2 C19 O3 125.9(6) . . ? O2 C19 C20 117.6(7) . . ? O3 C19 C20 116.4(7) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 O4 125.5(6) . . ? O5 C21 C22 116.6(6) . . ? O4 C21 C22 117.9(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O7 C23 O6 122(4) . . ? O7 C23 C24 117(2) . . ? O6 C23 C24 120(4) . . ? N3 C34 N6 115.6(5) . 3_665 ? N3 C34 H34A 108.4 . . ? N6 C34 H34A 108.4 3_665 . ? N3 C34 H34B 108.4 . . ? N6 C34 H34B 108.4 3_665 . ? H34A C34 H34B 107.4 . . ? Cl1 C25 Cl1 92.1(11) . 3 ? Cl1 C25 H25A 113.3 . . ? Cl1 C25 H25A 113.3 3 . ? Cl1 C25 H25B 113.3 . . ? Cl1 C25 H25B 113.3 3 . ? H25A C25 H25B 110.6 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O8 C26 O6 126(5) . . ? O8 C26 C27 119(3) . . ? O6 C26 C27 114(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 O1 Zn1 N1 C8 -123.0(5) . . . . ? O4 Zn1 N1 C8 109.0(5) . . . . ? O2 Zn1 N1 C8 -12.3(5) . . . . ? O1 Zn1 N1 C1 65.8(4) . . . . ? O4 Zn1 N1 C1 -62.2(4) . . . . ? O2 Zn1 N1 C1 176.5(3) . . . . ? O1 Zn2 N4 C17 117.2(6) . . . . ? O3 Zn2 N4 C17 10.7(7) . . . . ? O6 Zn2 N4 C17 -114.6(6) . . . . ? O1 Zn2 N4 C10 -62.4(4) . . . . ? O3 Zn2 N4 C10 -168.9(4) . . . . ? O6 Zn2 N4 C10 65.7(4) . . . . ? O4 Zn1 O1 Zn2 -111.8(3) . . . . ? O2 Zn1 O1 Zn2 -1.3(3) . . . . ? N1 Zn1 O1 Zn2 117.1(3) . . . . ? O3 Zn2 O1 Zn1 -7.4(3) . . . . ? O6 Zn2 O1 Zn1 111.0(3) . . . . ? N4 Zn2 O1 Zn1 -119.8(3) . . . . ? O1 Zn1 O2 C19 21.3(6) . . . . ? O4 Zn1 O2 C19 132.8(6) . . . . ? N1 Zn1 O2 C19 -101.5(6) . . . . ? O1 Zn2 O3 C19 7.9(8) . . . . ? O6 Zn2 O3 C19 -111.0(7) . . . . ? N4 Zn2 O3 C19 122.0(7) . . . . ? O1 Zn1 O4 C21 168.5(4) . . . . ? O2 Zn1 O4 C21 64.5(4) . . . . ? N1 Zn1 O4 C21 -59.1(4) . . . . ? O1 Zn2 O6 C23 -164.1(10) . . . . ? O3 Zn2 O6 C23 -53.7(10) . . . . ? N4 Zn2 O6 C23 69.3(10) . . . . ? O1 Zn2 O6 C26 -150(3) . . . . ? O3 Zn2 O6 C26 -40(3) . . . . ? N4 Zn2 O6 C26 83(3) . . . . ? C8 N1 C1 N2 -179.1(5) . . . . ? Zn1 N1 C1 N2 -6.8(6) . . . . ? C8 N1 C1 C5 3.2(8) . . . . ? Zn1 N1 C1 C5 175.4(4) . . . . ? C2 N2 C1 N1 -179.3(5) . . . . ? C2 N2 C1 C5 -1.5(8) . . . . ? C1 N2 C2 N3 -179.1(5) . . . . ? C1 N2 C2 C3 0.6(8) . . . . ? C34 N3 C2 N2 -5.7(8) . . . . ? C34 N3 C2 C3 174.5(5) . . . . ? N2 C2 C3 C4 -0.1(10) . . . . ? N3 C2 C3 C4 179.7(6) . . . . ? C2 C3 C4 C5 0.4(11) . . . . ? C3 C4 C5 C6 -179.5(7) . . . . ? C3 C4 C5 C1 -1.1(11) . . . . ? N1 C1 C5 C4 179.4(6) . . . . ? N2 C1 C5 C4 1.8(9) . . . . ? N1 C1 C5 C6 -2.1(9) . . . . ? N2 C1 C5 C6 -179.7(6) . . . . ? C4 C5 C6 C7 179.5(8) . . . . ? C1 C5 C6 C7 1.1(11) . . . . ? C5 C6 C7 C8 -1.2(12) . . . . ? C1 N1 C8 C7 -3.3(9) . . . . ? Zn1 N1 C8 C7 -173.8(5) . . . . ? C1 N1 C8 C9 177.9(6) . . . . ? Zn1 N1 C8 C9 7.4(8) . . . . ? C6 C7 C8 N1 2.3(11) . . . . ? C6 C7 C8 C9 -178.9(7) . . . . ? C11 N5 C10 N4 179.6(5) . . . . ? C11 N5 C10 C14 -1.4(8) . . . . ? C17 N4 C10 N5 176.6(5) . . . . ? Zn2 N4 C10 N5 -3.8(6) . . . . ? C17 N4 C10 C14 -2.4(9) . . . . ? Zn2 N4 C10 C14 177.3(5) . . . . ? C10 N5 C11 N6 178.8(5) . . . . ? C10 N5 C11 C12 -0.2(8) . . . . ? C34 N6 C11 N5 -7.2(8) 3_665 . . . ? C34 N6 C11 C12 171.8(6) 3_665 . . . ? N5 C11 C12 C13 2.0(10) . . . . ? N6 C11 C12 C13 -176.9(7) . . . . ? C11 C12 C13 C14 -2.1(11) . . . . ? N5 C10 C14 C15 -178.0(7) . . . . ? N4 C10 C14 C15 0.9(10) . . . . ? N5 C10 C14 C13 1.2(9) . . . . ? N4 C10 C14 C13 -179.9(6) . . . . ? C12 C13 C14 C15 179.7(8) . . . . ? C12 C13 C14 C10 0.6(11) . . . . ? C10 C14 C15 C16 2.0(13) . . . . ? C13 C14 C15 C16 -177.0(9) . . . . ? C14 C15 C16 C17 -3.5(15) . . . . ? C10 N4 C17 C16 1.0(10) . . . . ? Zn2 N4 C17 C16 -178.6(6) . . . . ? C10 N4 C17 C18 -179.0(6) . . . . ? Zn2 N4 C17 C18 1.4(10) . . . . ? C15 C16 C17 N4 1.9(13) . . . . ? C15 C16 C17 C18 -178.1(9) . . . . ? Zn1 O2 C19 O3 -26.6(11) . . . . ? Zn1 O2 C19 C20 156.5(5) . . . . ? Zn2 O3 C19 O2 7.7(12) . . . . ? Zn2 O3 C19 C20 -175.4(5) . . . . ? Zn1 O4 C21 O5 5.9(8) . . . . ? Zn1 O4 C21 C22 -173.4(6) . . . . ? C26 O6 C23 O7 -177(3) . . . . ? Zn2 O6 C23 O7 -9.2(18) . . . . ? C26 O6 C23 C24 8(2) . . . . ? Zn2 O6 C23 C24 176.2(16) . . . . ? C2 N3 C34 N6 75.9(7) . . . 3_665 ? C25 Cl1 C25 Cl1 0.0 3 . . 3 ? C23 O6 C26 O8 -158(5) . . . . ? Zn2 O6 C26 O8 -179.1(14) . . . . ? C23 O6 C26 C27 30(3) . . . . ? Zn2 O6 C26 C27 9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.516 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.063 #===END ## Crystallographic Data of complex 3 data_3 _database_code_depnum_ccdc_archive 'CCDC 690021' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H60 N12 O20 Zn5, 4(O)' _chemical_formula_sum 'C58 H74 N12 O24 Zn5' _chemical_formula_weight 1650.14 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc ' 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 23.643(3) _cell_length_b 8.9890(18) _cell_length_c 36.249(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.896(2) _cell_angle_gamma 90.00 _cell_volume 7565.0(19) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3028 _cell_measurement_theta_min 2.286 _cell_measurement_theta_max 25.319 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 1.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.849 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18925 _diffrn_reflns_av_R_equivalents 0.1045 _diffrn_reflns_av_sigmaI/netI 0.1220 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6666 _reflns_number_gt 3451 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0941P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6600 _refine_ls_number_parameters 440 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1527 _refine_ls_R_factor_gt 0.0783 _refine_ls_wR_factor_ref 0.1962 _refine_ls_wR_factor_gt 0.1667 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.976 _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 0.5000 0.5000 0.0000 0.0382(3) Uani 1 2 d S . . Zn2 Zn 0.61667(4) 0.28543(10) 0.02110(3) 0.0480(3) Uani 1 1 d . . . Zn3 Zn 0.57968(5) 0.54536(12) 0.23507(3) 0.0598(4) Uani 1 1 d . . . N1 N 0.6879(3) 0.1665(7) 0.04441(17) 0.0441(16) Uani 1 1 d . . . N2 N 0.6573(3) 0.2698(7) 0.09462(17) 0.0464(16) Uani 1 1 d . . . N3 N 0.6233(4) 0.3716(8) 0.14527(19) 0.062(2) Uani 1 1 d . . . H3 H 0.6292 0.3887 0.1690 0.074 Uiso 1 1 calc R . . N4 N 0.5781(3) 0.7695(8) 0.22665(18) 0.0553(19) Uani 1 1 d . . . N5 N 0.5779(3) 0.6796(7) 0.16822(16) 0.0447(16) Uani 1 1 d . . . N6 N 0.5779(3) 0.5827(8) 0.10936(18) 0.0560(19) Uani 1 1 d . . . H6 H 0.5823 0.5968 0.0866 0.067 Uiso 1 1 calc R . . O1 O 0.5361(2) 0.3085(5) 0.03030(13) 0.0422(13) Uani 1 1 d . . . O2 O 0.5588(3) 0.0738(7) 0.03824(17) 0.0663(17) Uani 1 1 d . . . O3 O 0.5712(3) 0.6215(5) 0.02709(14) 0.0455(13) Uani 1 1 d . . . O4 O 0.6505(2) 0.4905(6) 0.02442(16) 0.0570(15) Uani 1 1 d . . . O5 O 0.5389(2) 0.4453(6) -0.04642(14) 0.0508(14) Uani 1 1 d . . . O6 O 0.6021(3) 0.2599(7) -0.03421(16) 0.0637(17) Uani 1 1 d . . . O7 O 0.6489(3) 0.4291(7) 0.22724(16) 0.0700(18) Uani 1 1 d . . . O8 O 0.6811(4) 0.5910(9) 0.2718(2) 0.101(3) Uani 1 1 d . . . O9 O 0.5206(4) 0.4112(7) 0.20373(17) 0.076(2) Uani 1 1 d . . . C1 C 0.6969(3) 0.1831(8) 0.0828(2) 0.0423(19) Uani 1 1 d . . . C2 C 0.6637(4) 0.2898(9) 0.1316(2) 0.053(2) Uani 1 1 d . . . C3 C 0.7088(5) 0.2239(11) 0.1579(3) 0.068(3) Uani 1 1 d . . . H3A H 0.7109 0.2396 0.1835 0.081 Uiso 1 1 calc R . . C4 C 0.7481(5) 0.1395(11) 0.1459(3) 0.069(3) Uani 1 1 d . . . H4A H 0.7780 0.0973 0.1630 0.083 Uiso 1 1 calc R . . C5 C 0.7437(4) 0.1142(9) 0.1063(2) 0.055(2) Uani 1 1 d . . . C6 C 0.7804(4) 0.0283(10) 0.0898(3) 0.068(3) Uani 1 1 d . . . H6A H 0.8114 -0.0196 0.1047 0.082 Uiso 1 1 calc R . . C7 C 0.7718(4) 0.0130(10) 0.0518(3) 0.061(2) Uani 1 1 d . . . H7 H 0.7971 -0.0442 0.0410 0.074 Uiso 1 1 calc R . . C8 C 0.7256(3) 0.0821(9) 0.0293(2) 0.046(2) Uani 1 1 d . . . C9 C 0.7137(4) 0.0644(10) -0.0119(2) 0.054(2) Uani 1 1 d . . . H9A H 0.6846 -0.0103 -0.0189 0.081 Uiso 1 1 calc R . . H9B H 0.7483 0.0347 -0.0201 0.081 Uiso 1 1 calc R . . H9C H 0.7004 0.1572 -0.0235 0.081 Uiso 1 1 calc R . . C10 C 0.5777(4) 0.8027(9) 0.1899(2) 0.050(2) Uani 1 1 d . . . C11 C 0.5772(4) 0.7005(10) 0.1320(2) 0.054(2) Uani 1 1 d . . . C12 C 0.5749(4) 0.8483(12) 0.1158(3) 0.069(3) Uani 1 1 d . . . H12 H 0.5730 0.8595 0.0901 0.083 Uiso 1 1 calc R . . C13 C 0.5754(5) 0.9655(12) 0.1370(3) 0.076(3) Uani 1 1 d . . . H13 H 0.5745 1.0600 0.1264 0.091 Uiso 1 1 calc R . . C14 C 0.5775(4) 0.9496(10) 0.1760(3) 0.063(3) Uani 1 1 d . . . C15 C 0.5792(5) 1.0607(13) 0.2024(4) 0.092(4) Uani 1 1 d . . . H15 H 0.5795 1.1595 0.1948 0.110 Uiso 1 1 calc R . . C16 C 0.5806(6) 1.0309(14) 0.2382(4) 0.097(4) Uani 1 1 d . . . H16 H 0.5816 1.1094 0.2551 0.117 Uiso 1 1 calc R . . C17 C 0.5806(4) 0.8838(13) 0.2518(3) 0.071(3) Uani 1 1 d . . . C18 C 0.5839(6) 0.8457(14) 0.2922(3) 0.107(4) Uani 1 1 d . . . H18A H 0.5458 0.8442 0.2978 0.161 Uiso 1 1 calc R . . H18B H 0.6067 0.9189 0.3076 0.161 Uiso 1 1 calc R . . H18C H 0.6013 0.7495 0.2972 0.161 Uiso 1 1 calc R . . C19 C 0.5715(4) 0.4314(10) 0.1223(2) 0.057(2) Uani 1 1 d . . . H19A H 0.5408 0.4299 0.1368 0.068 Uiso 1 1 calc R . . H19B H 0.5599 0.3674 0.1007 0.068 Uiso 1 1 calc R . . C20 C 0.5225(4) 0.1746(10) 0.0376(2) 0.047(2) Uani 1 1 d . . . C21 C 0.4643(4) 0.1457(12) 0.0458(3) 0.074(3) Uani 1 1 d . . . H21A H 0.4393 0.1115 0.0234 0.111 Uiso 1 1 calc R . . H21B H 0.4491 0.2358 0.0543 0.111 Uiso 1 1 calc R . . H21C H 0.4669 0.0711 0.0650 0.111 Uiso 1 1 calc R . . C22 C 0.6242(4) 0.6102(9) 0.0286(2) 0.045(2) Uani 1 1 d . . . C23 C 0.6604(4) 0.7450(11) 0.0358(3) 0.077(3) Uani 1 1 d . . . H23A H 0.6822 0.7569 0.0162 0.115 Uiso 1 1 calc R . . H23B H 0.6862 0.7353 0.0596 0.115 Uiso 1 1 calc R . . H23C H 0.6362 0.8305 0.0364 0.115 Uiso 1 1 calc R . . C24 C 0.5692(4) 0.3485(10) -0.0556(2) 0.049(2) Uani 1 1 d . . . C25 C 0.5695(4) 0.3251(13) -0.0977(2) 0.073(3) Uani 1 1 d . . . H25A H 0.5354 0.2723 -0.1091 0.110 Uiso 1 1 calc R . . H25B H 0.6029 0.2683 -0.1004 0.110 Uiso 1 1 calc R . . H25C H 0.5706 0.4199 -0.1097 0.110 Uiso 1 1 calc R . . C26 C 0.6914(5) 0.4906(14) 0.2510(3) 0.082(3) Uani 1 1 d D . . C27 C 0.7526(6) 0.4378(19) 0.2509(4) 0.136(6) Uani 1 1 d D . . OW1 O 0.7465(3) 0.6743(7) 0.14746(13) 0.228(7) Uani 1 1 d . . . OW2 O 0.8259(3) 0.5630(7) 0.10885(13) 0.230(8) Uani 1 1 d R . . O10 O 0.4485(3) 0.5211(7) 0.21795(13) 0.170(6) Uani 1 1 d R . . C29 C 0.4412(3) 0.3054(7) 0.17205(13) 0.142(6) Uani 1 1 d RD . . H29A H 0.4009 0.3207 0.1627 0.212 Uiso 1 1 calc R . . H29B H 0.4471 0.2082 0.1831 0.212 Uiso 1 1 calc R . . H29C H 0.4618 0.3135 0.1517 0.212 Uiso 1 1 calc R . . C28 C 0.4628(3) 0.4208(7) 0.20115(13) 0.078(3) Uani 1 1 d RD . . 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 0.0384(8) 0.0332(7) 0.0423(7) 0.0027(5) 0.0057(5) 0.0031(6) Zn2 0.0435(6) 0.0452(6) 0.0545(6) 0.0016(4) 0.0074(4) 0.0064(5) Zn3 0.0744(8) 0.0561(7) 0.0520(6) -0.0047(5) 0.0196(5) -0.0069(6) N1 0.046(4) 0.041(4) 0.044(4) 0.003(3) 0.007(3) -0.005(3) N2 0.051(4) 0.046(4) 0.041(4) -0.002(3) 0.007(3) 0.001(3) N3 0.085(6) 0.057(5) 0.042(4) -0.012(4) 0.009(4) -0.005(4) N4 0.060(5) 0.057(5) 0.049(4) -0.021(3) 0.010(3) -0.001(4) N5 0.056(5) 0.041(4) 0.038(4) 0.000(3) 0.010(3) -0.005(3) N6 0.067(5) 0.066(5) 0.036(4) 0.001(3) 0.011(3) 0.000(4) O1 0.041(3) 0.038(3) 0.048(3) 0.005(2) 0.008(2) -0.001(2) O2 0.066(5) 0.046(4) 0.086(5) 0.010(3) 0.013(3) 0.008(3) O3 0.045(4) 0.040(3) 0.051(3) -0.001(2) 0.008(3) -0.002(3) O4 0.048(4) 0.047(4) 0.080(4) 0.002(3) 0.020(3) 0.001(3) O5 0.057(4) 0.060(4) 0.040(3) 0.003(3) 0.019(3) 0.016(3) O6 0.065(4) 0.072(4) 0.056(4) -0.007(3) 0.015(3) 0.026(3) O7 0.072(5) 0.080(4) 0.054(4) -0.011(3) -0.001(3) -0.003(4) O8 0.115(7) 0.109(6) 0.068(5) -0.034(4) -0.011(4) 0.028(5) O9 0.120(6) 0.054(4) 0.058(4) -0.009(3) 0.029(4) -0.023(4) C1 0.039(5) 0.036(4) 0.051(5) 0.003(4) 0.005(4) -0.003(4) C2 0.072(7) 0.041(5) 0.045(5) -0.003(4) 0.009(4) -0.002(5) C3 0.085(8) 0.066(6) 0.047(5) 0.010(5) -0.001(5) -0.018(6) C4 0.078(8) 0.068(6) 0.055(6) 0.005(5) -0.008(5) -0.002(6) C5 0.049(6) 0.046(5) 0.062(6) 0.003(4) -0.008(4) 0.004(4) C6 0.047(6) 0.052(6) 0.098(8) 0.014(5) -0.008(5) 0.007(5) C7 0.040(6) 0.061(6) 0.081(7) -0.004(5) 0.006(5) 0.014(5) C8 0.033(5) 0.036(5) 0.074(6) 0.000(4) 0.020(4) -0.005(4) C9 0.058(6) 0.056(5) 0.057(5) 0.003(4) 0.030(4) 0.005(5) C10 0.052(6) 0.046(5) 0.049(5) -0.005(4) 0.004(4) -0.001(4) C11 0.051(6) 0.060(6) 0.049(5) -0.001(4) 0.007(4) -0.005(5) C12 0.072(7) 0.070(7) 0.067(6) 0.032(6) 0.015(5) 0.011(6) C13 0.083(8) 0.047(6) 0.097(9) 0.025(6) 0.017(6) 0.004(5) C14 0.065(7) 0.035(5) 0.088(7) -0.004(5) 0.012(5) -0.001(4) C15 0.090(9) 0.053(7) 0.138(12) -0.008(8) 0.034(8) 0.005(6) C16 0.111(11) 0.064(8) 0.119(11) -0.037(8) 0.026(8) -0.005(7) C17 0.069(7) 0.096(9) 0.049(6) -0.028(5) 0.015(5) 0.004(6) C18 0.133(11) 0.121(10) 0.062(7) -0.040(7) 0.004(7) 0.019(9) C19 0.067(7) 0.055(6) 0.052(5) -0.011(4) 0.019(5) -0.006(5) C20 0.054(6) 0.046(5) 0.039(5) 0.003(4) 0.003(4) -0.002(5) C21 0.068(7) 0.075(7) 0.081(7) 0.025(5) 0.017(5) -0.008(6) C22 0.048(6) 0.044(5) 0.042(5) 0.002(4) 0.006(4) -0.001(4) C23 0.061(7) 0.058(6) 0.111(8) -0.005(5) 0.012(6) -0.016(5) C24 0.039(5) 0.054(5) 0.058(5) -0.008(4) 0.017(4) 0.002(4) C25 0.057(6) 0.116(9) 0.048(6) -0.001(5) 0.013(4) 0.020(6) C26 0.082(9) 0.103(9) 0.053(6) -0.009(6) -0.011(6) -0.005(7) C27 0.064(9) 0.163(15) 0.167(13) -0.068(11) -0.017(8) 0.020(9) OW1 0.207(14) 0.253(17) 0.210(13) 0.085(12) 0.004(10) -0.091(13) OW2 0.322(18) 0.215(13) 0.106(8) -0.090(8) -0.082(10) 0.059(12) O10 0.243(14) 0.185(11) 0.099(7) 0.014(7) 0.075(7) 0.129(10) C29 0.130(13) 0.150(14) 0.125(11) 0.037(10) -0.029(9) -0.067(11) C28 0.107(10) 0.070(7) 0.050(6) 0.022(5) -0.007(6) -0.013(7) _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 O3 2.090(5) 5_665 ? Zn1 O3 2.090(5) . ? Zn1 O5 2.122(5) 5_665 ? Zn1 O5 2.122(5) . ? Zn1 O1 2.132(5) . ? Zn1 O1 2.132(5) 5_665 ? Zn2 O6 1.983(6) . ? Zn2 O4 2.004(6) . ? Zn2 O2 2.492(6) . ? Zn2 O1 2.006(5) . ? Zn2 N1 2.039(6) . ? Zn2 O2 2.489(6) . ? Zn3 O10 1.955(6) 2_655 ? Zn3 O7 2.006(7) . ? Zn3 O8 2.546(8) . ? Zn3 O9 2.024(7) . ? Zn3 N4 2.037(7) . ? N1 C8 1.362(10) . ? N1 C1 1.375(9) . ? N2 C2 1.333(9) . ? N2 C1 1.348(10) . ? N3 C2 1.370(11) . ? N3 C19 1.449(11) . ? N3 H3 0.8600 . ? N4 C10 1.364(10) . ? N4 C17 1.367(11) . ? N5 C11 1.324(9) . ? N5 C10 1.359(10) . ? N6 C11 1.341(11) . ? N6 C19 1.456(11) . ? N6 H6 0.8600 . ? O1 C20 1.285(9) . ? O2 C20 1.246(10) . ? O3 C22 1.248(9) . ? O4 C22 1.266(9) . ? O5 C24 1.213(9) . ? O6 C24 1.270(10) . ? O7 C26 1.316(11) . ? O8 C26 1.228(12) . ? O9 C28 1.354(9) . ? C1 C5 1.407(11) . ? C2 C3 1.418(12) . ? C3 C4 1.335(14) . ? C3 H3A 0.9300 . ? C4 C5 1.438(12) . ? C4 H4A 0.9300 . ? C5 C6 1.381(13) . ? C6 C7 1.358(12) . ? C6 H6A 0.9300 . ? C7 C8 1.383(12) . ? C7 H7 0.9300 . ? C8 C9 1.475(11) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C14 1.413(12) . ? C11 C12 1.449(13) . ? C12 C13 1.302(13) . ? C12 H12 0.9300 . ? C13 C14 1.414(13) . ? C13 H13 0.9300 . ? C14 C15 1.379(14) . ? C15 C16 1.319(15) . ? C15 H15 0.9300 . ? C16 C17 1.411(16) . ? C16 H16 0.9300 . ? C17 C18 1.493(14) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.485(12) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.478(12) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.540(11) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.523(13) . ? O10 C28 1.1730 . ? O10 Zn3 1.955(6) 2_655 ? C29 C28 1.4986 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? 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 O3 Zn1 O3 180.0(4) 5_665 . ? O3 Zn1 O5 93.6(2) 5_665 5_665 ? O3 Zn1 O5 86.4(2) . 5_665 ? O3 Zn1 O5 86.4(2) 5_665 . ? O3 Zn1 O5 93.6(2) . . ? O5 Zn1 O5 180.0(3) 5_665 . ? O3 Zn1 O1 91.64(19) 5_665 . ? O3 Zn1 O1 88.36(19) . . ? O5 Zn1 O1 88.3(2) 5_665 . ? O5 Zn1 O1 91.7(2) . . ? O3 Zn1 O1 88.36(19) 5_665 5_665 ? O3 Zn1 O1 91.64(19) . 5_665 ? O5 Zn1 O1 91.7(2) 5_665 5_665 ? O5 Zn1 O1 88.3(2) . 5_665 ? O1 Zn1 O1 180.0(2) . 5_665 ? O6 Zn2 O4 99.1(3) . . ? O6 Zn2 O1 101.0(2) . . ? O4 Zn2 O1 106.0(2) . . ? O6 Zn2 N1 109.3(2) . . ? O4 Zn2 N1 99.7(2) . . ? O1 Zn2 N1 136.2(2) . . ? O6 Zn2 O2 99.5(2) . . ? O4 Zn2 O2 156.9(2) . . ? O1 Zn2 O2 56.9(2) . . ? N1 Zn2 O2 86.9(2) . . ? O10 Zn3 O7 119.1(3) 2_655 . ? O10 Zn3 O9 96.3(2) 2_655 . ? O7 Zn3 O9 96.0(3) . . ? O10 Zn3 N4 103.9(3) 2_655 . ? O7 Zn3 N4 119.1(3) . . ? O9 Zn3 N4 120.9(3) . . ? O10 Zn3 O8 88.9(4) 2_655 . ? O9 Zn3 O8 149.9(3) . . ? O7 Zn3 O8 56.5(2) . . ? N4 Zn3 O8 84.6(3) . . ? C8 N1 C1 118.8(7) . . ? C8 N1 Zn2 132.6(5) . . ? C1 N1 Zn2 108.6(5) . . ? C2 N2 C1 116.4(7) . . ? C2 N3 C19 124.3(7) . . ? C2 N3 H3 117.8 . . ? C19 N3 H3 117.8 . . ? C10 N4 C17 118.5(8) . . ? C10 N4 Zn3 111.1(5) . . ? C17 N4 Zn3 130.3(7) . . ? C11 N5 C10 117.2(7) . . ? C11 N6 C19 121.7(7) . . ? C11 N6 H6 119.2 . . ? C19 N6 H6 119.2 . . ? C20 O1 Zn2 102.7(5) . . ? C20 O1 Zn1 140.4(5) . . ? Zn2 O1 Zn1 107.3(2) . . ? C20 O2 Zn2 81.3(5) . . ? C22 O3 Zn1 133.7(5) . . ? C22 O4 Zn2 126.1(5) . . ? C24 O5 Zn1 138.7(6) . . ? C24 O6 Zn2 121.0(5) . . ? C26 O7 Zn3 103.4(7) . . ? C28 O9 Zn3 125.5(5) . . ? N2 C1 N1 113.7(7) . . ? N2 C1 C5 125.1(8) . . ? N1 C1 C5 121.2(8) . . ? N2 C2 N3 118.8(8) . . ? N2 C2 C3 123.2(9) . . ? N3 C2 C3 117.9(8) . . ? C4 C3 C2 119.9(9) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 119.5(9) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C6 C5 C1 118.1(8) . . ? C6 C5 C4 126.1(9) . . ? C1 C5 C4 115.8(9) . . ? C7 C6 C5 120.6(8) . . ? C7 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? C6 C7 C8 120.3(9) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? N1 C8 C7 121.0(8) . . ? N1 C8 C9 117.0(7) . . ? C7 C8 C9 121.9(8) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N5 C10 N4 112.7(7) . . ? N5 C10 C14 123.8(8) . . ? N4 C10 C14 123.5(8) . . ? N5 C11 N6 119.7(8) . . ? N5 C11 C12 121.6(8) . . ? N6 C11 C12 118.7(8) . . ? C13 C12 C11 120.6(9) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 120.1(9) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C10 115.6(10) . . ? C15 C14 C13 127.8(10) . . ? C10 C14 C13 116.7(8) . . ? C16 C15 C14 121.9(11) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 122.1(11) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? N4 C17 C16 118.4(9) . . ? N4 C17 C18 118.0(10) . . ? C16 C17 C18 123.6(10) . . ? 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 N6 113.7(7) . . ? N3 C19 H19A 108.8 . . ? N6 C19 H19A 108.8 . . ? N3 C19 H19B 108.8 . . ? N6 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? O2 C20 O1 119.1(8) . . ? O2 C20 C21 122.0(8) . . ? O1 C20 C21 118.8(8) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O3 C22 O4 125.1(7) . . ? O3 C22 C23 118.9(8) . . ? O4 C22 C23 116.0(8) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O5 C24 O6 127.3(8) . . ? O5 C24 C25 119.0(8) . . ? O6 C24 C25 113.7(8) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O8 C26 O7 119.6(10) . . ? O8 C26 C27 122.0(10) . . ? O7 C26 C27 118.4(10) . . ? C28 O10 Zn3 135.82(17) . 2_655 ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O10 C28 O9 113.5(4) . . ? O10 C28 C29 143.5 . . ? O9 C28 C29 102.1(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.831 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.105