Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Syntheses, Structures, and Optical Properties of Novel Zinc(II) Complexes with Multicarboxylate and N-donor Ligands ; _publ_contact_author_name 'Prof. Wei-Yin Sun' _publ_contact_author_email SUNWY@NJU.EDU.CN loop_ _publ_author_name 'Wei-Yin Sun' 'Qian Chu' 'Yong-Qing Huang' 'Guang-Xiang Liu' 'Xiao-Feng Wang' # Attachment 'B707159K .cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 646922' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((Zn2(OA)(bipy)(H2O))-0.5(bipy)) _chemical_melting_point ? _chemical_formula_moiety 'C26 H16 N2 O10 Zn2, C5 H4 N' _chemical_formula_sum 'C31 H20 N3 O10 Zn2' _chemical_formula_weight 725.24 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 'P 21/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 10.9129(11) _cell_length_b 15.0557(15) _cell_length_c 16.4468(17) _cell_angle_alpha 90.00 _cell_angle_beta 91.800(2) _cell_angle_gamma 90.00 _cell_volume 2700.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5679 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.2 _exptl_crystal_description block _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 1.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7089 _exptl_absorpt_correction_T_max 0.7565 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex 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 13226 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4744 _reflns_number_gt 4236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement "SMART'(Bruker, 2000)" _computing_data_reduction 'SAINT (Bruker, 2000)' _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^)+(0.0425P)^2^+2.5729P] 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 4744 _refine_ls_number_parameters 421 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.71397(3) 0.60204(2) 1.032283(19) 0.02555(10) Uani 1 1 d . . . Zn2 Zn 1.10345(3) 0.64863(2) 0.867763(19) 0.03065(11) Uani 1 1 d . . . O1 O 1.2218(2) 0.57892(14) 0.93251(12) 0.0417(6) Uani 1 1 d . . . O1W O 1.2481(2) 0.68170(16) 0.77910(15) 0.0457(6) Uani 1 1 d D . . H1WA H 1.259(4) 0.652(2) 0.7385(17) 0.055 Uiso 1 1 d D . . H1WB H 1.240(4) 0.7330(15) 0.762(2) 0.055 Uiso 1 1 d D . . O2 O 1.26504(19) 0.50113(12) 1.04049(12) 0.0342(5) Uani 1 1 d . . . O3 O 0.97256(19) 0.62403(15) 0.95996(12) 0.0380(5) Uani 1 1 d . . . O4 O 0.86741(18) 0.64731(14) 1.07400(12) 0.0350(5) Uani 1 1 d . . . O5 O 1.1386(2) 0.85158(13) 1.22908(13) 0.0426(6) Uani 1 1 d . . . O6 O 0.91658(19) 1.07847(14) 1.38800(12) 0.0353(5) Uani 1 1 d . . . O7 O 0.8356(2) 1.16882(15) 1.29861(14) 0.0455(6) Uani 1 1 d . . . O8 O 0.8642(3) 1.19765(19) 1.10249(17) 0.0727(9) Uani 1 1 d . . . O9 O 1.0037(2) 1.25213(15) 1.18049(17) 0.0537(7) Uani 1 1 d . . . C1 C 1.2261(2) 0.56987(18) 1.00786(17) 0.0278(6) Uani 1 1 d . . . C2 C 1.1929(3) 0.64546(17) 1.06427(16) 0.0261(6) Uani 1 1 d . . . C3 C 1.2874(3) 0.6767(2) 1.11099(19) 0.0357(7) Uani 1 1 d . . . H3 H 1.3646 0.6511 1.1076 0.043 Uiso 1 1 calc R . . C4 C 1.2695(3) 0.7471(2) 1.16415(19) 0.0381(7) Uani 1 1 d . . . H4 H 1.3356 0.7693 1.1949 0.046 Uiso 1 1 calc R . . C5 C 1.1553(3) 0.78450(19) 1.17192(18) 0.0333(7) Uani 1 1 d . . . C6 C 1.0579(3) 0.75118(19) 1.12968(17) 0.0317(6) Uani 1 1 d . . . H6 H 0.9797 0.7737 1.1372 0.038 Uiso 1 1 calc R . . C7 C 1.0764(2) 0.68207(17) 1.07424(16) 0.0251(6) Uani 1 1 d . . . C8 C 0.9655(3) 0.64781(17) 1.03204(17) 0.0263(6) Uani 1 1 d . . . C9 C 0.9060(3) 1.10866(18) 1.31638(17) 0.0282(6) Uani 1 1 d . . . C10 C 0.9793(3) 1.06200(18) 1.25054(17) 0.0288(6) Uani 1 1 d . . . C11 C 1.0284(3) 0.97914(18) 1.26668(18) 0.0322(6) Uani 1 1 d . . . H11 H 1.0236 0.9552 1.3186 0.039 Uiso 1 1 calc R . . C12 C 1.0856(3) 0.93046(18) 1.20556(18) 0.0330(7) Uani 1 1 d . . . C13 C 1.0933(3) 0.9620(2) 1.12715(19) 0.0387(7) Uani 1 1 d . . . H13 H 1.1289 0.9285 1.0867 0.046 Uiso 1 1 calc R . . C14 C 1.0461(3) 1.0448(2) 1.11126(19) 0.0390(7) Uani 1 1 d . . . H14 H 1.0516 1.0680 1.0591 0.047 Uiso 1 1 calc R . . C15 C 0.9896(3) 1.09587(18) 1.17139(19) 0.0332(7) Uani 1 1 d . . . C16 C 0.9474(3) 1.1874(2) 1.1500(2) 0.0438(8) Uani 1 1 d . . . C17 C 0.9237(3) 0.5292(2) 0.7864(2) 0.0434(8) Uani 1 1 d . . . H17 H 0.8673 0.5685 0.8077 0.052 Uiso 1 1 calc R . . C18 C 0.8831(3) 0.4604(2) 0.7401(2) 0.0442(8) Uani 1 1 d . . . H18 H 0.7993 0.4529 0.7304 0.053 Uiso 1 1 calc R . . C19 C 0.9657(3) 0.39968(18) 0.70635(17) 0.0303(6) Uani 1 1 d . . . C20 C 1.0872(3) 0.4112(2) 0.7253(2) 0.0417(8) Uani 1 1 d . . . H20 H 1.1457 0.3720 0.7064 0.050 Uiso 1 1 calc R . . C21 C 1.1201(3) 0.4817(2) 0.7725(2) 0.0398(8) Uani 1 1 d . . . H21 H 1.2030 0.4892 0.7855 0.048 Uiso 1 1 calc R . . C22 C 0.9268(3) 0.32710(18) 0.65200(17) 0.0299(6) Uani 1 1 d . . . C23 C 0.8052(3) 0.3153(2) 0.6346(2) 0.0498(9) Uani 1 1 d . . . H23 H 0.7471 0.3517 0.6580 0.060 Uiso 1 1 calc R . . C24 C 0.7706(3) 0.2500(2) 0.5830(2) 0.0498(9) Uani 1 1 d . . . H24 H 0.6872 0.2426 0.5715 0.060 Uiso 1 1 calc R . . C25 C 0.9664(3) 0.2030(2) 0.5656(2) 0.0414(8) Uani 1 1 d . . . H25 H 1.0222 0.1639 0.5433 0.050 Uiso 1 1 calc R . . C26 C 1.0078(3) 0.2673(2) 0.6166(2) 0.0439(8) Uani 1 1 d . . . H26 H 1.0914 0.2719 0.6285 0.053 Uiso 1 1 calc R . . C27 C 0.1029(6) 0.6421(4) 0.6107(3) 0.0968(18) Uani 1 1 d . . . H27 H 0.0824 0.6951 0.6359 0.116 Uiso 1 1 calc R . . C28 C 0.0178(6) 0.6009(3) 0.5653(3) 0.0857(16) Uani 1 1 d . . . H28 H -0.0607 0.6247 0.5607 0.103 Uiso 1 1 calc R . . C29 C 0.0439(4) 0.5234(3) 0.5248(2) 0.0602(10) Uani 1 1 d . . . C30 C 0.1631(5) 0.4865(4) 0.5350(3) 0.0827(14) Uani 1 1 d . . . H30 H 0.1852 0.4335 0.5103 0.099 Uiso 1 1 calc R . . C31 C 0.2422(5) 0.5332(4) 0.5827(3) 0.0958(17) Uani 1 1 d . . . H31 H 0.3211 0.5105 0.5893 0.115 Uiso 1 1 calc R . . N1 N 1.0413(2) 0.54156(15) 0.80202(14) 0.0308(5) Uani 1 1 d . . . N2 N 0.8495(2) 0.19448(15) 0.54668(14) 0.0299(5) Uani 1 1 d . . . N3 N 0.2184(5) 0.6102(3) 0.6221(3) 0.0864(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02674(18) 0.02286(17) 0.02702(18) 0.00051(12) 0.00049(13) 0.00273(12) Zn2 0.0349(2) 0.02828(19) 0.02847(19) -0.00289(13) -0.00388(14) 0.00249(14) O1 0.0524(14) 0.0457(13) 0.0264(11) -0.0072(9) -0.0080(10) 0.0248(11) O1W 0.0442(14) 0.0428(14) 0.0501(15) 0.0009(11) -0.0016(11) 0.0017(11) O2 0.0443(12) 0.0239(10) 0.0342(11) -0.0043(9) -0.0027(9) 0.0083(9) O3 0.0333(12) 0.0535(13) 0.0270(11) -0.0069(10) -0.0004(9) -0.0059(10) O4 0.0248(11) 0.0461(13) 0.0341(11) -0.0075(9) 0.0016(9) -0.0019(9) O5 0.0585(15) 0.0298(11) 0.0387(12) -0.0108(9) -0.0107(11) 0.0121(10) O6 0.0341(12) 0.0415(12) 0.0306(11) 0.0005(9) 0.0042(9) 0.0025(9) O7 0.0470(14) 0.0437(13) 0.0465(13) 0.0094(11) 0.0142(11) 0.0165(11) O8 0.094(2) 0.0670(19) 0.0557(17) 0.0089(14) -0.0143(16) 0.0307(17) O9 0.0513(15) 0.0259(12) 0.0851(19) 0.0055(12) 0.0233(13) 0.0045(11) C1 0.0211(14) 0.0285(15) 0.0334(16) -0.0035(12) -0.0033(11) 0.0034(11) C2 0.0294(15) 0.0229(14) 0.0259(14) -0.0005(11) -0.0002(11) 0.0026(11) C3 0.0271(16) 0.0360(16) 0.0438(17) -0.0090(14) -0.0037(13) 0.0083(13) C4 0.0363(17) 0.0353(16) 0.0421(18) -0.0101(14) -0.0072(14) -0.0017(13) C5 0.0435(18) 0.0242(14) 0.0321(15) -0.0058(12) 0.0002(13) 0.0010(13) C6 0.0281(16) 0.0294(15) 0.0376(16) -0.0039(13) 0.0004(12) 0.0073(12) C7 0.0275(14) 0.0213(13) 0.0263(13) 0.0001(11) -0.0006(11) 0.0014(11) C8 0.0265(15) 0.0214(13) 0.0309(15) 0.0019(11) -0.0005(11) 0.0039(11) C9 0.0252(15) 0.0253(14) 0.0344(16) -0.0027(12) 0.0031(12) -0.0068(12) C10 0.0268(15) 0.0245(14) 0.0352(15) -0.0027(12) 0.0027(12) -0.0035(11) C11 0.0379(17) 0.0277(15) 0.0310(15) -0.0018(12) -0.0006(12) -0.0030(12) C12 0.0371(17) 0.0218(14) 0.0396(17) -0.0082(12) -0.0057(13) 0.0007(12) C13 0.0464(19) 0.0307(16) 0.0396(17) -0.0094(13) 0.0095(14) 0.0001(14) C14 0.053(2) 0.0312(16) 0.0333(16) 0.0008(13) 0.0100(14) -0.0016(14) C15 0.0349(17) 0.0251(15) 0.0398(17) 0.0002(12) 0.0059(13) -0.0029(12) C16 0.052(2) 0.0369(19) 0.0434(19) 0.0092(15) 0.0191(16) 0.0083(16) C17 0.0380(19) 0.0440(19) 0.0483(19) -0.0193(15) 0.0028(15) 0.0050(14) C18 0.0328(18) 0.0479(19) 0.052(2) -0.0182(16) -0.0001(15) 0.0009(15) C19 0.0347(16) 0.0246(14) 0.0314(15) -0.0007(12) -0.0033(12) -0.0004(12) C20 0.0378(18) 0.0320(16) 0.054(2) -0.0144(14) -0.0113(15) 0.0091(13) C21 0.0344(17) 0.0339(16) 0.0502(19) -0.0099(14) -0.0135(14) 0.0050(13) C22 0.0339(16) 0.0256(14) 0.0300(15) -0.0012(12) -0.0030(12) -0.0017(12) C23 0.0337(18) 0.048(2) 0.067(2) -0.0302(18) -0.0033(16) 0.0061(15) C24 0.0286(17) 0.053(2) 0.067(2) -0.0281(18) -0.0041(16) -0.0016(15) C25 0.0317(17) 0.0422(18) 0.0500(19) -0.0172(15) -0.0026(14) 0.0078(14) C26 0.0284(17) 0.0474(19) 0.055(2) -0.0185(16) -0.0093(14) 0.0031(14) C27 0.127(5) 0.070(3) 0.091(4) -0.006(3) -0.032(4) 0.011(3) C28 0.106(4) 0.068(3) 0.081(3) -0.008(3) -0.029(3) 0.020(3) C29 0.071(3) 0.066(3) 0.044(2) 0.0066(19) 0.0085(18) 0.002(2) C30 0.075(3) 0.104(4) 0.069(3) -0.023(3) 0.014(2) -0.011(3) C31 0.070(3) 0.125(5) 0.092(4) -0.008(4) 0.004(3) 0.005(3) N1 0.0383(14) 0.0261(12) 0.0277(12) -0.0021(10) -0.0028(10) -0.0015(10) N2 0.0313(13) 0.0240(12) 0.0344(13) -0.0059(10) 0.0007(10) -0.0039(10) N3 0.107(4) 0.085(3) 0.067(3) -0.003(2) -0.006(2) 0.000(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 O4 1.915(2) . ? Zn1 O2 1.9786(19) 3_767 ? Zn1 O6 1.998(2) 2_647 ? Zn1 N2 2.011(2) 2_656 ? Zn2 O1 1.953(2) . ? Zn2 O9 2.042(2) 3_777 ? Zn2 N1 2.045(2) . ? Zn2 O3 2.148(2) . ? Zn2 O1W 2.238(3) . ? Zn2 O8 2.389(3) 3_777 ? Zn2 C16 2.546(3) 3_777 ? O1 C1 1.246(3) . ? O1W H1WA 0.813(18) . ? O1W H1WB 0.826(18) . ? O2 C1 1.235(3) . ? O2 Zn1 1.9786(19) 3_767 ? O3 C8 1.243(3) . ? O4 C8 1.292(3) . ? O5 C12 1.371(4) . ? O5 C5 1.396(3) . ? O6 C9 1.264(3) . ? O6 Zn1 1.998(2) 2_657 ? O7 C9 1.217(3) . ? O8 C16 1.189(5) . ? O8 Zn2 2.389(3) 3_777 ? O9 C16 1.249(4) . ? O9 Zn2 2.042(2) 3_777 ? C1 C2 1.519(4) . ? C2 C3 1.351(4) . ? C2 C7 1.400(4) . ? C3 C4 1.392(4) . ? C3 H3 0.9300 . ? C4 C5 1.377(4) . ? C4 H4 0.9300 . ? C5 C6 1.348(4) . ? C6 C7 1.402(4) . ? C6 H6 0.9300 . ? C7 C8 1.470(4) . ? C9 C10 1.536(4) . ? C10 C11 1.380(4) . ? C10 C15 1.406(4) . ? C11 C12 1.406(4) . ? C11 H11 0.9300 . ? C12 C13 1.379(4) . ? C13 C14 1.370(4) . ? C13 H13 0.9300 . ? C14 C15 1.410(4) . ? C14 H14 0.9300 . ? C15 C16 1.491(4) . ? C16 Zn2 2.546(3) 3_777 ? C17 N1 1.315(4) . ? C17 C18 1.352(4) . ? C17 H17 0.9300 . ? C18 C19 1.410(4) . ? C18 H18 0.9300 . ? C19 C20 1.363(4) . ? C19 C22 1.466(4) . ? C20 C21 1.358(4) . ? C20 H20 0.9300 . ? C21 N1 1.346(4) . ? C21 H21 0.9300 . ? C22 C23 1.361(4) . ? C22 C26 1.401(4) . ? C23 C24 1.346(4) . ? C23 H23 0.9300 . ? C24 N2 1.352(4) . ? C24 H24 0.9300 . ? C25 N2 1.311(4) . ? C25 C26 1.349(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.328(7) . ? C27 N3 1.356(7) . ? C27 H27 0.9300 . ? C28 C29 1.377(6) . ? C28 H28 0.9300 . ? C29 C30 1.420(7) . ? C29 C29 1.424(8) 3_566 ? C30 C31 1.347(7) . ? C30 H30 0.9300 . ? C31 N3 1.358(7) . ? C31 H31 0.9300 . ? N2 Zn1 2.011(2) 2_646 ? 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 Zn1 O2 112.31(9) . 3_767 ? O4 Zn1 O6 117.49(9) . 2_647 ? O2 Zn1 O6 110.85(9) 3_767 2_647 ? O4 Zn1 N2 105.33(9) . 2_656 ? O2 Zn1 N2 101.34(9) 3_767 2_656 ? O6 Zn1 N2 107.97(9) 2_647 2_656 ? O1 Zn2 O9 164.88(10) . 3_777 ? O1 Zn2 N1 93.85(9) . . ? O9 Zn2 N1 101.25(10) 3_777 . ? O1 Zn2 O3 88.01(9) . . ? O9 Zn2 O3 90.87(9) 3_777 . ? N1 Zn2 O3 91.18(9) . . ? O1 Zn2 O1W 90.41(9) . . ? O9 Zn2 O1W 89.48(9) 3_777 . ? N1 Zn2 O1W 93.43(9) . . ? O3 Zn2 O1W 175.22(8) . . ? O1 Zn2 O8 108.55(9) . 3_777 ? O9 Zn2 O8 56.63(10) 3_777 3_777 ? N1 Zn2 O8 156.38(9) . 3_777 ? O3 Zn2 O8 96.87(10) . 3_777 ? O1W Zn2 O8 79.37(10) . 3_777 ? O1 Zn2 C16 136.19(11) . 3_777 ? O9 Zn2 C16 29.04(11) 3_777 3_777 ? N1 Zn2 C16 129.53(11) . 3_777 ? O3 Zn2 C16 95.80(9) . 3_777 ? O1W Zn2 C16 82.25(10) . 3_777 ? O8 Zn2 C16 27.65(11) 3_777 3_777 ? C1 O1 Zn2 127.21(19) . . ? Zn2 O1W H1WA 122(3) . . ? Zn2 O1W H1WB 111(3) . . ? H1WA O1W H1WB 104(4) . . ? C1 O2 Zn1 116.10(18) . 3_767 ? C8 O3 Zn2 133.32(19) . . ? C8 O4 Zn1 122.72(18) . . ? C12 O5 C5 120.0(2) . . ? C9 O6 Zn1 120.07(18) . 2_657 ? C16 O8 Zn2 83.5(2) . 3_777 ? C16 O9 Zn2 98.5(2) . 3_777 ? O2 C1 O1 121.7(3) . . ? O2 C1 C2 116.6(2) . . ? O1 C1 C2 121.5(2) . . ? C3 C2 C7 118.4(3) . . ? C3 C2 C1 114.6(2) . . ? C7 C2 C1 127.0(2) . . ? C2 C3 C4 120.2(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 121.0(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 120.1(3) . . ? C6 C5 O5 119.9(3) . . ? C4 C5 O5 119.8(3) . . ? C5 C6 C7 118.9(3) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C2 C7 C6 121.2(3) . . ? C2 C7 C8 122.9(2) . . ? C6 C7 C8 115.7(2) . . ? O3 C8 O4 125.8(3) . . ? O3 C8 C7 118.5(3) . . ? O4 C8 C7 115.7(2) . . ? O7 C9 O6 122.0(3) . . ? O7 C9 C10 120.6(3) . . ? O6 C9 C10 117.2(2) . . ? C11 C10 C15 117.6(3) . . ? C11 C10 C9 119.0(3) . . ? C15 C10 C9 123.1(3) . . ? C10 C11 C12 120.8(3) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? O5 C12 C13 121.7(3) . . ? O5 C12 C11 116.3(3) . . ? C13 C12 C11 122.0(3) . . ? C14 C13 C12 117.3(3) . . ? C14 C13 H13 121.4 . . ? C12 C13 H13 121.4 . . ? C13 C14 C15 122.1(3) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C10 C15 C14 120.1(3) . . ? C10 C15 C16 121.4(3) . . ? C14 C15 C16 118.5(3) . . ? O8 C16 O9 121.2(3) . . ? O8 C16 C15 119.9(3) . . ? O9 C16 C15 118.8(3) . . ? O8 C16 Zn2 68.8(2) . 3_777 ? O9 C16 Zn2 52.51(17) . 3_777 ? C15 C16 Zn2 171.0(3) . 3_777 ? N1 C17 C18 121.3(3) . . ? N1 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C19 121.1(3) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 117.2(3) . . ? C20 C19 C22 119.7(3) . . ? C18 C19 C22 123.1(3) . . ? C21 C20 C19 117.9(3) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? N1 C21 C20 124.7(3) . . ? N1 C21 H21 117.6 . . ? C20 C21 H21 117.6 . . ? C23 C22 C26 116.9(3) . . ? C23 C22 C19 119.1(3) . . ? C26 C22 C19 123.9(3) . . ? C24 C23 C22 118.7(3) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 N2 124.1(3) . . ? C23 C24 H24 118.0 . . ? N2 C24 H24 118.0 . . ? N2 C25 C26 121.5(3) . . ? N2 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C25 C26 C22 121.1(3) . . ? C25 C26 H26 119.5 . . ? C22 C26 H26 119.5 . . ? C28 C27 N3 122.9(5) . . ? C28 C27 H27 118.5 . . ? N3 C27 H27 118.5 . . ? C27 C28 C29 121.1(5) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C28 C29 C30 118.4(4) . . ? C28 C29 C29 123.4(5) . 3_566 ? C30 C29 C29 118.1(5) . 3_566 ? C31 C30 C29 115.6(5) . . ? C31 C30 H30 122.2 . . ? C29 C30 H30 122.2 . . ? C30 C31 N3 126.6(6) . . ? C30 C31 H31 116.7 . . ? N3 C31 H31 116.7 . . ? C17 N1 C21 117.7(3) . . ? C17 N1 Zn2 121.4(2) . . ? C21 N1 Zn2 120.9(2) . . ? C25 N2 C24 117.6(3) . . ? C25 N2 Zn1 122.3(2) . 2_646 ? C24 N2 Zn1 120.1(2) . 2_646 ? C27 N3 C31 115.3(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 O9 Zn2 O1 C1 56.7(5) 3_777 . . . ? N1 Zn2 O1 C1 -120.3(3) . . . . ? O3 Zn2 O1 C1 -29.2(3) . . . . ? O1W Zn2 O1 C1 146.3(3) . . . . ? O8 Zn2 O1 C1 67.3(3) 3_777 . . . ? C16 Zn2 O1 C1 67.1(3) 3_777 . . . ? O1 Zn2 O3 C8 67.2(3) . . . . ? O9 Zn2 O3 C8 -97.7(3) 3_777 . . . ? N1 Zn2 O3 C8 161.0(3) . . . . ? O8 Zn2 O3 C8 -41.2(3) 3_777 . . . ? C16 Zn2 O3 C8 -69.0(3) 3_777 . . . ? O2 Zn1 O4 C8 35.0(2) 3_767 . . . ? O6 Zn1 O4 C8 165.34(19) 2_647 . . . ? N2 Zn1 O4 C8 -74.4(2) 2_656 . . . ? Zn1 O2 C1 O1 -12.7(4) 3_767 . . . ? Zn1 O2 C1 C2 171.83(18) 3_767 . . . ? Zn2 O1 C1 O2 149.2(2) . . . . ? Zn2 O1 C1 C2 -35.6(4) . . . . ? O2 C1 C2 C3 61.5(4) . . . . ? O1 C1 C2 C3 -113.9(3) . . . . ? O2 C1 C2 C7 -115.8(3) . . . . ? O1 C1 C2 C7 68.7(4) . . . . ? C7 C2 C3 C4 -3.6(4) . . . . ? C1 C2 C3 C4 178.8(3) . . . . ? C2 C3 C4 C5 1.8(5) . . . . ? C3 C4 C5 C6 2.2(5) . . . . ? C3 C4 C5 O5 176.3(3) . . . . ? C12 O5 C5 C6 -58.7(4) . . . . ? C12 O5 C5 C4 127.2(3) . . . . ? C4 C5 C6 C7 -4.1(5) . . . . ? O5 C5 C6 C7 -178.2(3) . . . . ? C3 C2 C7 C6 1.7(4) . . . . ? C1 C2 C7 C6 178.9(3) . . . . ? C3 C2 C7 C8 -174.4(3) . . . . ? C1 C2 C7 C8 2.9(4) . . . . ? C5 C6 C7 C2 2.2(4) . . . . ? C5 C6 C7 C8 178.5(3) . . . . ? Zn2 O3 C8 O4 160.9(2) . . . . ? Zn2 O3 C8 C7 -17.4(4) . . . . ? Zn1 O4 C8 O3 3.7(4) . . . . ? Zn1 O4 C8 C7 -177.96(17) . . . . ? C2 C7 C8 O3 -39.6(4) . . . . ? C6 C7 C8 O3 144.1(3) . . . . ? C2 C7 C8 O4 141.9(3) . . . . ? C6 C7 C8 O4 -34.3(3) . . . . ? Zn1 O6 C9 O7 18.1(4) 2_657 . . . ? Zn1 O6 C9 C10 -157.76(18) 2_657 . . . ? O7 C9 C10 C11 -160.7(3) . . . . ? O6 C9 C10 C11 15.3(4) . . . . ? O7 C9 C10 C15 13.3(4) . . . . ? O6 C9 C10 C15 -170.8(3) . . . . ? C15 C10 C11 C12 -0.6(4) . . . . ? C9 C10 C11 C12 173.7(3) . . . . ? C5 O5 C12 C13 -27.2(4) . . . . ? C5 O5 C12 C11 155.7(3) . . . . ? C10 C11 C12 O5 175.8(3) . . . . ? C10 C11 C12 C13 -1.2(5) . . . . ? O5 C12 C13 C14 -174.8(3) . . . . ? C11 C12 C13 C14 2.1(5) . . . . ? C12 C13 C14 C15 -1.2(5) . . . . ? C11 C10 C15 C14 1.4(4) . . . . ? C9 C10 C15 C14 -172.6(3) . . . . ? C11 C10 C15 C16 -175.5(3) . . . . ? C9 C10 C15 C16 10.5(4) . . . . ? C13 C14 C15 C10 -0.5(5) . . . . ? C13 C14 C15 C16 176.5(3) . . . . ? Zn2 O8 C16 O9 -4.6(3) 3_777 . . . ? Zn2 O8 C16 C15 178.1(3) 3_777 . . . ? Zn2 O9 C16 O8 5.4(4) 3_777 . . . ? Zn2 O9 C16 C15 -177.3(2) 3_777 . . . ? C10 C15 C16 O8 -115.2(4) . . . . ? C14 C15 C16 O8 67.9(4) . . . . ? C10 C15 C16 O9 67.5(4) . . . . ? C14 C15 C16 O9 -109.5(4) . . . . ? N1 C17 C18 C19 -0.5(5) . . . . ? C17 C18 C19 C20 2.7(5) . . . . ? C17 C18 C19 C22 -176.4(3) . . . . ? C18 C19 C20 C21 -2.3(5) . . . . ? C22 C19 C20 C21 176.8(3) . . . . ? C19 C20 C21 N1 -0.3(5) . . . . ? C20 C19 C22 C23 178.9(3) . . . . ? C18 C19 C22 C23 -2.0(5) . . . . ? C20 C19 C22 C26 -0.4(5) . . . . ? C18 C19 C22 C26 178.7(3) . . . . ? C26 C22 C23 C24 -2.4(5) . . . . ? C19 C22 C23 C24 178.2(3) . . . . ? C22 C23 C24 N2 0.1(6) . . . . ? N2 C25 C26 C22 0.5(5) . . . . ? C23 C22 C26 C25 2.2(5) . . . . ? C19 C22 C26 C25 -178.5(3) . . . . ? N3 C27 C28 C29 -1.8(9) . . . . ? C27 C28 C29 C30 2.2(8) . . . . ? C27 C28 C29 C29 -180.0(5) . . . 3_566 ? C28 C29 C30 C31 -1.8(7) . . . . ? C29 C29 C30 C31 -179.7(5) 3_566 . . . ? C29 C30 C31 N3 1.0(8) . . . . ? C18 C17 N1 C21 -2.1(5) . . . . ? C18 C17 N1 Zn2 177.2(3) . . . . ? C20 C21 N1 C17 2.6(5) . . . . ? C20 C21 N1 Zn2 -176.8(3) . . . . ? O1 Zn2 N1 C17 136.7(3) . . . . ? O9 Zn2 N1 C17 -42.5(3) 3_777 . . . ? O3 Zn2 N1 C17 48.6(3) . . . . ? O1W Zn2 N1 C17 -132.7(2) . . . . ? O8 Zn2 N1 C17 -61.6(4) 3_777 . . . ? C16 Zn2 N1 C17 -49.9(3) 3_777 . . . ? O1 Zn2 N1 C21 -44.0(2) . . . . ? O9 Zn2 N1 C21 136.8(2) 3_777 . . . ? O3 Zn2 N1 C21 -132.1(2) . . . . ? O1W Zn2 N1 C21 46.7(2) . . . . ? O8 Zn2 N1 C21 117.7(3) 3_777 . . . ? C16 Zn2 N1 C21 129.4(2) 3_777 . . . ? C26 C25 N2 C24 -2.8(5) . . . . ? C26 C25 N2 Zn1 177.8(3) . . . 2_646 ? C23 C24 N2 C25 2.6(6) . . . . ? C23 C24 N2 Zn1 -178.0(3) . . . 2_646 ? C28 C27 N3 C31 0.9(8) . . . . ? C30 C31 N3 C27 -0.5(9) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.462 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.069 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 646923' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H18 N4 O10 Zn2, H2 O' _chemical_formula_sum 'C28 H20 N4 O11 Zn2' _chemical_formula_weight 719.22 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4425(17) _cell_length_b 15.209(2) _cell_length_c 16.019(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.143(3) _cell_angle_gamma 90.00 _cell_volume 2663.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2557 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.41 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.793 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 1.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7054 _exptl_absorpt_correction_T_max 0.8062 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex 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 14155 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0930 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5211 _reflns_number_gt 3542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0400P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5211 _refine_ls_number_parameters 413 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1099 _refine_ls_wR_factor_gt 0.1035 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.17887(5) 1.09806(3) 0.17300(3) 0.02578(15) Uani 1 1 d . . . Zn2 Zn 0.79124(5) 0.94608(3) 0.12670(3) 0.03489(17) Uani 1 1 d . . . O1W O 0.5004(5) 0.9481(4) 0.8877(4) 0.142(2) Uani 1 1 d . . . O1 O 0.3464(3) 1.3155(2) 0.3150(2) 0.0522(10) Uani 1 1 d . . . O2W O 0.6231(5) 0.9236(5) 0.0441(4) 0.138(2) Uani 1 1 d D . . H2WA H 0.601(7) 0.886(4) 0.075(4) 0.165 Uiso 1 1 d D . . H2WB H 0.577(6) 0.927(5) -0.007(2) 0.165 Uiso 1 1 d D . . O2 O 0.2806(3) 1.4478(2) 0.2713(2) 0.0603(11) Uani 1 1 d . . . O3 O 0.4156(4) 1.1478(3) 0.2189(3) 0.0877(14) Uani 1 1 d . . . O4 O 0.2426(3) 1.2109(2) 0.1498(2) 0.0465(9) Uani 1 1 d . . . O5 O 0.7882(3) 1.01954(18) -0.13792(19) 0.0386(8) Uani 1 1 d . . . O6 O 0.8258(3) 0.9735(2) -0.00193(19) 0.0494(10) Uani 1 1 d . . . O7 O 0.8921(3) 1.05354(18) 0.16590(18) 0.0353(8) Uani 1 1 d . . . O8 O 1.0088(3) 1.13697(19) 0.11066(18) 0.0320(7) Uani 1 1 d . . . O9 O 0.6207(3) 1.35503(18) 0.0309(2) 0.0384(8) Uani 1 1 d . . . N1 N 1.1990(3) 1.0786(2) 0.2992(2) 0.0268(8) Uani 1 1 d . . . N2 N 1.1711(3) 1.0158(2) 0.4149(2) 0.0249(8) Uani 1 1 d . . . N3 N 1.0086(3) 0.7657(2) 0.6108(2) 0.0269(8) Uani 1 1 d . . . N4 N 0.9073(3) 0.6548(2) 0.6428(2) 0.0320(9) Uani 1 1 d . . . C1 C 0.3374(4) 1.3796(3) 0.2649(3) 0.0341(11) Uani 1 1 d . . . C2 C 0.4047(4) 1.3735(3) 0.1978(3) 0.0288(10) Uani 1 1 d . . . C3 C 0.4632(4) 1.4453(3) 0.1766(3) 0.0301(11) Uani 1 1 d . . . H3 H 0.4541 1.4999 0.2002 0.036 Uiso 1 1 calc R . . C4 C 0.5353(4) 1.4385(3) 0.1213(3) 0.0302(11) Uani 1 1 d . . . H4 H 0.5728 1.4880 0.1067 0.036 Uiso 1 1 calc R . . C5 C 0.5505(4) 1.3575(3) 0.0882(3) 0.0282(10) Uani 1 1 d . . . C6 C 0.4935(4) 1.2847(3) 0.1079(3) 0.0327(11) Uani 1 1 d . . . H6 H 0.5039 1.2303 0.0846 0.039 Uiso 1 1 calc R . . C7 C 0.4203(4) 1.2925(3) 0.1628(3) 0.0309(11) Uani 1 1 d . . . C8 C 0.3545(5) 1.2119(3) 0.1774(3) 0.0401(12) Uani 1 1 d . . . C9 C 0.6147(4) 1.2426(3) -0.0736(3) 0.0362(11) Uani 1 1 d . . . H9 H 0.5536 1.2732 -0.1144 0.043 Uiso 1 1 calc R . . C10 C 0.6604(4) 1.1652(3) -0.0958(3) 0.0384(12) Uani 1 1 d . . . H10 H 0.6299 1.1441 -0.1526 0.046 Uiso 1 1 calc R . . C11 C 0.7501(4) 1.1182(3) -0.0361(3) 0.0297(11) Uani 1 1 d . . . C12 C 0.7925(4) 1.0304(3) -0.0591(3) 0.0325(11) Uani 1 1 d . . . C13 C 0.9078(4) 1.1093(3) 0.1124(3) 0.0254(10) Uani 1 1 d . . . C14 C 0.7988(4) 1.1519(3) 0.0485(3) 0.0224(10) Uani 1 1 d . . . C15 C 0.7543(4) 1.2303(3) 0.0706(3) 0.0286(10) Uani 1 1 d . . . H15 H 0.7874 1.2537 0.1262 0.034 Uiso 1 1 calc R . . C16 C 0.6614(4) 1.2738(3) 0.0106(3) 0.0294(11) Uani 1 1 d . . . C17 C 1.1489(4) 1.0120(3) 0.3279(3) 0.0291(10) Uani 1 1 d . . . H17 H 1.1039 0.9679 0.2926 0.035 Uiso 1 1 calc R . . C18 C 1.2407(4) 1.0894(3) 0.4429(3) 0.0304(11) Uani 1 1 d . . . H18 H 1.2707 1.1090 0.5002 0.036 Uiso 1 1 calc R . . C19 C 1.2571(4) 1.1275(3) 0.3717(3) 0.0281(10) Uani 1 1 d . . . H19 H 1.3010 1.1789 0.3715 0.034 Uiso 1 1 calc R . . C20 C 1.1280(4) 0.9529(2) 0.4659(3) 0.0249(10) Uani 1 1 d . . . C21 C 1.0240(4) 0.9065(3) 0.4275(3) 0.0297(11) Uani 1 1 d . . . H21 H 0.9790 0.9182 0.3700 0.036 Uiso 1 1 calc R . . C22 C 0.9855(4) 0.8418(3) 0.4744(3) 0.0304(11) Uani 1 1 d . . . H22 H 0.9167 0.8081 0.4483 0.036 Uiso 1 1 calc R . . C23 C 1.0512(4) 0.8286(3) 0.5607(3) 0.0270(10) Uani 1 1 d . . . C24 C 1.1527(4) 0.8777(3) 0.5996(3) 0.0324(11) Uani 1 1 d . . . H24 H 1.1944 0.8692 0.6583 0.039 Uiso 1 1 calc R . . C25 C 1.1931(4) 0.9400(3) 0.5516(3) 0.0322(11) Uani 1 1 d . . . H25 H 1.2634 0.9725 0.5771 0.039 Uiso 1 1 calc R . . C26 C 0.9446(4) 0.6920(3) 0.5815(3) 0.0328(11) Uani 1 1 d . . . H26 H 0.9290 0.6703 0.5250 0.039 Uiso 1 1 calc R . . C27 C 0.9487(4) 0.7085(3) 0.7152(3) 0.0335(11) Uani 1 1 d . . . H27 H 0.9353 0.6989 0.7690 0.040 Uiso 1 1 calc R . . C28 C 1.0106(4) 0.7759(3) 0.6964(3) 0.0310(11) Uani 1 1 d . . . H28 H 1.0480 0.8211 0.7339 0.037 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 0.0338(3) 0.0223(3) 0.0236(3) 0.0014(2) 0.0121(2) -0.0006(2) Zn2 0.0414(4) 0.0242(3) 0.0437(4) 0.0002(2) 0.0197(3) 0.0009(3) O1W 0.165(6) 0.139(5) 0.123(5) 0.014(4) 0.044(4) 0.053(4) O1 0.072(3) 0.042(2) 0.052(2) 0.0074(18) 0.034(2) 0.0042(19) O2W 0.078(4) 0.224(7) 0.093(4) 0.064(4) -0.004(3) -0.048(4) O2 0.077(3) 0.043(2) 0.087(3) 0.023(2) 0.065(2) 0.024(2) O3 0.075(3) 0.049(3) 0.157(4) 0.027(3) 0.061(3) 0.009(2) O4 0.039(2) 0.038(2) 0.057(2) 0.0093(16) 0.0056(18) -0.0154(17) O5 0.055(2) 0.0286(17) 0.0324(19) -0.0049(14) 0.0136(17) 0.0043(16) O6 0.082(3) 0.0312(19) 0.033(2) 0.0019(16) 0.0141(19) 0.0214(19) O7 0.043(2) 0.0327(18) 0.0285(17) 0.0043(14) 0.0075(15) -0.0108(15) O8 0.0259(19) 0.0365(18) 0.0337(18) 0.0076(14) 0.0087(15) -0.0009(15) O9 0.043(2) 0.0227(17) 0.063(2) 0.0027(15) 0.0370(18) 0.0041(15) N1 0.034(2) 0.024(2) 0.0229(19) 0.0015(15) 0.0092(17) -0.0017(17) N2 0.032(2) 0.0223(19) 0.022(2) 0.0000(15) 0.0105(17) -0.0042(17) N3 0.037(2) 0.023(2) 0.024(2) -0.0021(15) 0.0132(17) -0.0046(17) N4 0.043(3) 0.024(2) 0.036(2) -0.0028(17) 0.023(2) -0.0066(18) C1 0.032(3) 0.032(3) 0.042(3) -0.004(2) 0.018(2) -0.002(2) C2 0.024(3) 0.030(3) 0.034(3) 0.003(2) 0.011(2) 0.004(2) C3 0.029(3) 0.025(2) 0.037(3) -0.004(2) 0.010(2) 0.001(2) C4 0.027(3) 0.023(2) 0.042(3) 0.000(2) 0.013(2) -0.005(2) C5 0.021(2) 0.027(2) 0.038(3) 0.002(2) 0.012(2) 0.003(2) C6 0.033(3) 0.022(2) 0.047(3) -0.001(2) 0.017(2) 0.000(2) C7 0.027(3) 0.026(2) 0.042(3) 0.007(2) 0.015(2) 0.003(2) C8 0.038(3) 0.030(3) 0.060(3) 0.006(2) 0.026(3) 0.004(3) C9 0.027(3) 0.032(3) 0.045(3) 0.005(2) 0.004(2) 0.007(2) C10 0.041(3) 0.033(3) 0.034(3) -0.007(2) 0.000(2) -0.004(2) C11 0.029(3) 0.025(2) 0.035(3) -0.005(2) 0.008(2) -0.002(2) C12 0.031(3) 0.029(3) 0.033(3) -0.008(2) 0.003(2) 0.002(2) C13 0.036(3) 0.019(2) 0.024(2) -0.0061(18) 0.013(2) -0.005(2) C14 0.022(2) 0.021(2) 0.027(2) 0.0005(18) 0.013(2) -0.0005(19) C15 0.034(3) 0.029(3) 0.027(2) -0.005(2) 0.015(2) -0.005(2) C16 0.029(3) 0.020(2) 0.046(3) 0.000(2) 0.024(2) -0.002(2) C17 0.038(3) 0.027(2) 0.023(2) -0.0014(19) 0.010(2) -0.003(2) C18 0.035(3) 0.029(3) 0.029(2) -0.008(2) 0.012(2) -0.005(2) C19 0.029(3) 0.024(2) 0.033(3) -0.001(2) 0.011(2) -0.005(2) C20 0.030(3) 0.020(2) 0.029(2) -0.0025(18) 0.016(2) 0.000(2) C21 0.041(3) 0.028(2) 0.020(2) -0.0016(19) 0.010(2) -0.002(2) C22 0.037(3) 0.030(3) 0.027(3) -0.0087(19) 0.014(2) -0.007(2) C23 0.035(3) 0.022(2) 0.030(3) -0.0019(19) 0.020(2) -0.001(2) C24 0.036(3) 0.038(3) 0.024(2) 0.003(2) 0.009(2) -0.004(2) C25 0.033(3) 0.034(3) 0.030(3) 0.000(2) 0.010(2) -0.009(2) C26 0.045(3) 0.030(3) 0.028(3) -0.006(2) 0.019(2) -0.010(2) C27 0.048(3) 0.032(3) 0.025(2) 0.003(2) 0.018(2) -0.001(2) C28 0.042(3) 0.031(3) 0.022(2) -0.0038(19) 0.012(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.943(3) 1_655 ? Zn1 O5 1.945(3) 3_775 ? Zn1 N1 1.987(3) . ? Zn1 O8 1.998(3) . ? Zn2 O7 1.993(3) . ? Zn2 N4 1.996(3) 4_575 ? Zn2 O2W 2.017(5) . ? Zn2 O2 2.034(3) 2_645 ? Zn2 O6 2.249(3) . ? O1 C1 1.247(5) . ? O2W H2WA 0.84(6) . ? O2W H2WB 0.83(2) . ? O2 C1 1.245(5) . ? O2 Zn2 2.034(3) 2_655 ? O3 C8 1.268(6) . ? O4 C8 1.225(5) . ? O4 Zn1 1.943(3) 1_455 ? O5 C12 1.259(5) . ? O5 Zn1 1.945(3) 3_775 ? O6 C12 1.236(5) . ? O7 C13 1.256(5) . ? O8 C13 1.237(5) . ? O9 C5 1.387(5) . ? O9 C16 1.393(5) . ? N1 C17 1.312(5) . ? N1 C19 1.375(5) . ? N2 C17 1.341(5) . ? N2 C18 1.370(5) . ? N2 C20 1.436(5) . ? N3 C26 1.345(5) . ? N3 C28 1.374(5) . ? N3 C23 1.423(5) . ? N4 C26 1.309(5) . ? N4 C27 1.384(5) . ? N4 Zn2 1.996(3) 4_576 ? C1 C2 1.498(6) . ? C2 C3 1.375(6) . ? C2 C7 1.386(6) . ? C3 C4 1.381(6) . ? C3 H3 0.9300 . ? C4 C5 1.372(5) . ? C4 H4 0.9300 . ? C5 C6 1.368(6) . ? C6 C7 1.388(6) . ? C6 H6 0.9300 . ? C7 C8 1.492(6) . ? C9 C10 1.377(6) . ? C9 C16 1.379(6) . ? C9 H9 0.9300 . ? C10 C11 1.379(6) . ? C10 H10 0.9300 . ? C11 C14 1.402(5) . ? C11 C12 1.504(6) . ? C13 C14 1.507(6) . ? C14 C15 1.383(5) . ? C15 C16 1.375(6) . ? C15 H15 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.341(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.365(5) . ? C20 C25 1.370(6) . ? C21 C22 1.387(5) . ? C21 H21 0.9300 . ? C22 C23 1.379(5) . ? C22 H22 0.9300 . ? C23 C24 1.367(6) . ? C24 C25 1.382(6) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.330(6) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? 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 Zn1 O5 129.92(15) 1_655 3_775 ? O4 Zn1 N1 112.84(14) 1_655 . ? O5 Zn1 N1 100.54(13) 3_775 . ? O4 Zn1 O8 90.47(13) 1_655 . ? O5 Zn1 O8 111.78(13) 3_775 . ? N1 Zn1 O8 110.85(13) . . ? O7 Zn2 N4 106.76(14) . 4_575 ? O7 Zn2 O2W 134.2(2) . . ? N4 Zn2 O2W 115.1(3) 4_575 . ? O7 Zn2 O2 94.03(13) . 2_645 ? N4 Zn2 O2 108.51(15) 4_575 2_645 ? O2W Zn2 O2 89.8(2) . 2_645 ? O7 Zn2 O6 83.95(12) . . ? N4 Zn2 O6 88.32(13) 4_575 . ? O2W Zn2 O6 79.71(18) . . ? O2 Zn2 O6 162.84(14) 2_645 . ? Zn2 O2W H2WA 97(5) . . ? Zn2 O2W H2WB 147(5) . . ? H2WA O2W H2WB 114(4) . . ? C1 O2 Zn2 113.6(3) . 2_655 ? C8 O4 Zn1 110.7(3) . 1_455 ? C12 O5 Zn1 117.2(3) . 3_775 ? C12 O6 Zn2 135.3(3) . . ? C13 O7 Zn2 121.7(3) . . ? C13 O8 Zn1 131.8(3) . . ? C5 O9 C16 118.5(3) . . ? C17 N1 C19 105.8(3) . . ? C17 N1 Zn1 122.7(3) . . ? C19 N1 Zn1 131.4(3) . . ? C17 N2 C18 106.8(3) . . ? C17 N2 C20 124.8(3) . . ? C18 N2 C20 128.4(3) . . ? C26 N3 C28 106.8(3) . . ? C26 N3 C23 127.2(3) . . ? C28 N3 C23 125.4(3) . . ? C26 N4 C27 105.5(4) . . ? C26 N4 Zn2 126.0(3) . 4_576 ? C27 N4 Zn2 127.8(3) . 4_576 ? O2 C1 O1 122.9(4) . . ? O2 C1 C2 120.1(4) . . ? O1 C1 C2 116.9(4) . . ? C3 C2 C7 118.5(4) . . ? C3 C2 C1 121.2(4) . . ? C7 C2 C1 119.9(4) . . ? C2 C3 C4 121.6(4) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 118.9(4) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C6 C5 C4 121.0(4) . . ? C6 C5 O9 122.6(4) . . ? C4 C5 O9 116.4(4) . . ? C5 C6 C7 119.7(4) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C2 C7 C6 120.3(4) . . ? C2 C7 C8 122.4(4) . . ? C6 C7 C8 117.1(4) . . ? O4 C8 O3 122.4(5) . . ? O4 C8 C7 118.4(4) . . ? O3 C8 C7 119.2(5) . . ? C10 C9 C16 118.7(4) . . ? C10 C9 H9 120.7 . . ? C16 C9 H9 120.7 . . ? C9 C10 C11 121.7(4) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C14 118.9(4) . . ? C10 C11 C12 121.2(4) . . ? C14 C11 C12 119.8(4) . . ? O6 C12 O5 124.3(4) . . ? O6 C12 C11 119.4(4) . . ? O5 C12 C11 116.3(4) . . ? O8 C13 O7 124.5(4) . . ? O8 C13 C14 115.5(4) . . ? O7 C13 C14 119.8(4) . . ? C15 C14 C11 119.5(4) . . ? C15 C14 C13 119.4(4) . . ? C11 C14 C13 120.8(4) . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C9 121.0(4) . . ? C15 C16 O9 120.4(4) . . ? C9 C16 O9 118.3(4) . . ? N1 C17 N2 111.3(4) . . ? N1 C17 H17 124.4 . . ? N2 C17 H17 124.4 . . ? C19 C18 N2 106.8(4) . . ? C19 C18 H18 126.6 . . ? N2 C18 H18 126.6 . . ? C18 C19 N1 109.3(4) . . ? C18 C19 H19 125.3 . . ? N1 C19 H19 125.3 . . ? C21 C20 C25 121.5(4) . . ? C21 C20 N2 119.2(4) . . ? C25 C20 N2 119.3(4) . . ? C20 C21 C22 119.8(4) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 118.7(4) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C24 C23 C22 121.1(4) . . ? C24 C23 N3 119.7(4) . . ? C22 C23 N3 119.1(4) . . ? C23 C24 C25 120.0(4) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C20 C25 C24 118.9(4) . . ? C20 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? N4 C26 N3 111.3(4) . . ? N4 C26 H26 124.4 . . ? N3 C26 H26 124.4 . . ? C28 C27 N4 109.8(4) . . ? C28 C27 H27 125.1 . . ? N4 C27 H27 125.1 . . ? C27 C28 N3 106.6(4) . . ? C27 C28 H28 126.7 . . ? N3 C28 H28 126.7 . . ? 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 O7 Zn2 O6 C12 -69.7(4) . . . . ? N4 Zn2 O6 C12 -176.8(5) 4_575 . . . ? O2W Zn2 O6 C12 67.3(5) . . . . ? O2 Zn2 O6 C12 14.3(7) 2_645 . . . ? N4 Zn2 O7 C13 106.6(3) 4_575 . . . ? O2W Zn2 O7 C13 -49.1(5) . . . . ? O2 Zn2 O7 C13 -142.7(3) 2_645 . . . ? O6 Zn2 O7 C13 20.2(3) . . . . ? O4 Zn1 O8 C13 -161.0(4) 1_655 . . . ? O5 Zn1 O8 C13 65.0(4) 3_775 . . . ? N1 Zn1 O8 C13 -46.3(4) . . . . ? O4 Zn1 N1 C17 171.3(3) 1_655 . . . ? O5 Zn1 N1 C17 -46.8(4) 3_775 . . . ? O8 Zn1 N1 C17 71.5(4) . . . . ? O4 Zn1 N1 C19 -5.5(4) 1_655 . . . ? O5 Zn1 N1 C19 136.4(4) 3_775 . . . ? O8 Zn1 N1 C19 -105.3(4) . . . . ? Zn2 O2 C1 O1 1.8(6) 2_655 . . . ? Zn2 O2 C1 C2 -174.9(3) 2_655 . . . ? O2 C1 C2 C3 36.0(7) . . . . ? O1 C1 C2 C3 -140.8(4) . . . . ? O2 C1 C2 C7 -151.1(5) . . . . ? O1 C1 C2 C7 32.0(6) . . . . ? C7 C2 C3 C4 0.7(7) . . . . ? C1 C2 C3 C4 173.6(4) . . . . ? C2 C3 C4 C5 -1.4(7) . . . . ? C3 C4 C5 C6 1.4(7) . . . . ? C3 C4 C5 O9 178.1(4) . . . . ? C16 O9 C5 C6 -17.2(6) . . . . ? C16 O9 C5 C4 166.1(4) . . . . ? C4 C5 C6 C7 -0.7(7) . . . . ? O9 C5 C6 C7 -177.2(4) . . . . ? C3 C2 C7 C6 0.0(6) . . . . ? C1 C2 C7 C6 -173.0(4) . . . . ? C3 C2 C7 C8 -176.1(4) . . . . ? C1 C2 C7 C8 10.9(7) . . . . ? C5 C6 C7 C2 0.0(7) . . . . ? C5 C6 C7 C8 176.3(4) . . . . ? Zn1 O4 C8 O3 -3.3(6) 1_455 . . . ? Zn1 O4 C8 C7 178.0(3) 1_455 . . . ? C2 C7 C8 O4 62.4(7) . . . . ? C6 C7 C8 O4 -113.8(5) . . . . ? C2 C7 C8 O3 -116.4(5) . . . . ? C6 C7 C8 O3 67.4(6) . . . . ? C16 C9 C10 C11 0.6(7) . . . . ? C9 C10 C11 C14 -2.3(7) . . . . ? C9 C10 C11 C12 175.3(4) . . . . ? Zn2 O6 C12 O5 -155.3(3) . . . . ? Zn2 O6 C12 C11 22.7(7) . . . . ? Zn1 O5 C12 O6 6.2(6) 3_775 . . . ? Zn1 O5 C12 C11 -171.9(3) 3_775 . . . ? C10 C11 C12 O6 -147.2(5) . . . . ? C14 C11 C12 O6 30.4(6) . . . . ? C10 C11 C12 O5 30.9(6) . . . . ? C14 C11 C12 O5 -151.5(4) . . . . ? Zn1 O8 C13 O7 9.7(6) . . . . ? Zn1 O8 C13 C14 -174.5(2) . . . . ? Zn2 O7 C13 O8 -128.1(4) . . . . ? Zn2 O7 C13 C14 56.4(5) . . . . ? C10 C11 C14 C15 1.3(6) . . . . ? C12 C11 C14 C15 -176.4(4) . . . . ? C10 C11 C14 C13 -172.0(4) . . . . ? C12 C11 C14 C13 10.3(6) . . . . ? O8 C13 C14 C15 -84.0(5) . . . . ? O7 C13 C14 C15 92.0(5) . . . . ? O8 C13 C14 C11 89.3(5) . . . . ? O7 C13 C14 C11 -94.8(5) . . . . ? C11 C14 C15 C16 1.3(6) . . . . ? C13 C14 C15 C16 174.7(4) . . . . ? C14 C15 C16 C9 -3.1(6) . . . . ? C14 C15 C16 O9 -176.6(3) . . . . ? C10 C9 C16 C15 2.1(7) . . . . ? C10 C9 C16 O9 175.7(4) . . . . ? C5 O9 C16 C15 -73.8(5) . . . . ? C5 O9 C16 C9 112.6(4) . . . . ? C19 N1 C17 N2 0.4(5) . . . . ? Zn1 N1 C17 N2 -177.1(3) . . . . ? C18 N2 C17 N1 -0.6(5) . . . . ? C20 N2 C17 N1 179.5(4) . . . . ? C17 N2 C18 C19 0.4(5) . . . . ? C20 N2 C18 C19 -179.6(4) . . . . ? N2 C18 C19 N1 -0.2(5) . . . . ? C17 N1 C19 C18 -0.2(5) . . . . ? Zn1 N1 C19 C18 177.0(3) . . . . ? C17 N2 C20 C21 -26.4(6) . . . . ? C18 N2 C20 C21 153.6(4) . . . . ? C17 N2 C20 C25 152.6(4) . . . . ? C18 N2 C20 C25 -27.4(6) . . . . ? C25 C20 C21 C22 -2.9(6) . . . . ? N2 C20 C21 C22 176.0(4) . . . . ? C20 C21 C22 C23 2.7(6) . . . . ? C21 C22 C23 C24 -0.2(6) . . . . ? C21 C22 C23 N3 176.5(4) . . . . ? C26 N3 C23 C24 -153.0(4) . . . . ? C28 N3 C23 C24 36.8(6) . . . . ? C26 N3 C23 C22 30.2(6) . . . . ? C28 N3 C23 C22 -140.0(4) . . . . ? C22 C23 C24 C25 -2.1(7) . . . . ? N3 C23 C24 C25 -178.8(4) . . . . ? C21 C20 C25 C24 0.6(7) . . . . ? N2 C20 C25 C24 -178.3(4) . . . . ? C23 C24 C25 C20 1.9(7) . . . . ? C27 N4 C26 N3 0.7(5) . . . . ? Zn2 N4 C26 N3 171.3(3) 4_576 . . . ? C28 N3 C26 N4 -0.5(5) . . . . ? C23 N3 C26 N4 -172.2(4) . . . . ? C26 N4 C27 C28 -0.6(5) . . . . ? Zn2 N4 C27 C28 -171.0(3) 4_576 . . . ? N4 C27 C28 N3 0.3(5) . . . . ? C26 N3 C28 C27 0.1(5) . . . . ? C23 N3 C28 C27 172.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.066 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.090 #====END data_3 _database_code_depnum_ccdc_archive 'CCDC 646924' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H40 N8 O12 Zn2' _chemical_formula_sum 'C36 H40 N8 O12 Zn2' _chemical_formula_weight 907.50 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 'p 21/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 10.8373(14) _cell_length_b 24.482(3) _cell_length_c 14.6610(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.565(2) _cell_angle_gamma 90.00 _cell_volume 3871.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3256 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 23.22 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.313 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7435 _exptl_absorpt_correction_T_max 0.8479 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex 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 20441 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7577 _reflns_number_gt 5481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0717P)^2^+5.1886P] 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 7577 _refine_ls_number_parameters 536 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 1.49585(5) 0.18827(2) -0.53111(4) 0.03420(16) Uani 1 1 d . . . Zn2 Zn 1.27092(5) 0.42519(2) -0.34970(3) 0.03711(17) Uani 1 1 d . . . O1 O 1.3671(3) 0.43141(13) -0.4559(2) 0.0446(8) Uani 1 1 d . . . O1W O 0.9035(4) 0.47477(16) -0.9195(3) 0.0707(12) Uani 1 1 d . . . O2 O 1.4798(4) 0.35697(14) -0.4230(2) 0.0515(9) Uani 1 1 d . . . O2W O 1.7075(6) 0.2756(4) -0.4056(4) 0.176(4) Uani 1 1 d . . . O3 O 1.5468(3) 0.25988(13) -0.5757(2) 0.0455(8) Uani 1 1 d . . . O3W O 1.2047(8) 0.3078(3) -0.7594(6) 0.187(4) Uani 1 1 d . . . O4 O 1.3490(3) 0.28385(14) -0.5859(3) 0.0496(9) Uani 1 1 d . . . O5 O 1.6031(3) 0.41085(14) -0.8285(2) 0.0401(8) Uani 1 1 d . . . O6 O 1.1658(3) 0.34049(13) -1.0150(2) 0.0416(8) Uani 1 1 d . . . O7 O 1.1165(3) 0.42436(14) -0.9736(2) 0.0465(9) Uani 1 1 d . . . O8 O 1.3731(3) 0.42216(14) -1.2344(2) 0.0437(8) Uani 1 1 d . . . O9 O 1.1943(3) 0.41970(15) -1.1730(2) 0.0477(9) Uani 1 1 d . . . N1 N 1.1732(4) 0.49492(17) -0.3624(3) 0.0426(10) Uani 1 1 d . . . N2 N 1.0343(4) 0.55658(17) -0.3363(3) 0.0440(10) Uani 1 1 d . . . N3 N 0.7992(4) 0.42724(16) -0.1886(3) 0.0408(10) Uani 1 1 d . . . N4 N 0.8851(4) 0.35523(15) -0.1213(3) 0.0367(9) Uani 1 1 d . . . N5 N 1.4206(4) 0.19513(15) -0.4126(3) 0.0354(9) Uani 1 1 d . A . N6 N 1.3567(4) 0.22919(17) -0.2877(3) 0.0428(10) Uani 1 1 d . . . N7 N 1.5773(4) 0.2128(2) 0.0595(3) 0.0573(12) Uani 1 1 d . . . N8 N 1.6572(4) 0.13823(18) 0.1216(3) 0.0474(11) Uani 1 1 d . . . C1 C 1.4410(4) 0.39358(18) -0.4751(3) 0.0329(10) Uani 1 1 d . . . C2 C 1.4814(4) 0.39702(18) -0.5700(3) 0.0289(9) Uani 1 1 d . . . C3 C 1.4951(4) 0.34999(17) -0.6225(3) 0.0284(9) Uani 1 1 d . . . C4 C 1.5329(4) 0.35534(18) -0.7094(3) 0.0332(10) Uani 1 1 d . . . H4A H 1.5420 0.3243 -0.7447 0.040 Uiso 1 1 calc R . . C5 C 1.5571(4) 0.40567(19) -0.7440(3) 0.0324(10) Uani 1 1 d . . . C6 C 1.5419(4) 0.45215(19) -0.6935(3) 0.0353(10) Uani 1 1 d . . . H6A H 1.5566 0.4864 -0.7177 0.042 Uiso 1 1 calc R . . C7 C 1.5045(4) 0.44731(18) -0.6069(3) 0.0360(11) Uani 1 1 d . . . H7A H 1.4947 0.4787 -0.5725 0.043 Uiso 1 1 calc R . . C8 C 1.4600(5) 0.29422(18) -0.5911(3) 0.0360(11) Uani 1 1 d . . . C9 C 1.5234(4) 0.41383(17) -0.9071(3) 0.0289(9) Uani 1 1 d . . . C10 C 1.3984(4) 0.40241(17) -0.9109(3) 0.0288(9) Uani 1 1 d . . . H10A H 1.3627 0.3930 -0.8579 0.035 Uiso 1 1 calc R . . C11 C 1.3260(4) 0.40507(17) -0.9947(3) 0.0275(9) Uani 1 1 d . . . C12 C 1.3809(4) 0.41952(17) -1.0732(3) 0.0304(10) Uani 1 1 d . . . C13 C 1.5064(4) 0.43173(19) -1.0664(3) 0.0371(11) Uani 1 1 d . . . H13A H 1.5427 0.4416 -1.1189 0.045 Uiso 1 1 calc R . . C14 C 1.5784(4) 0.42964(19) -0.9842(3) 0.0370(11) Uani 1 1 d . . . H14A H 1.6621 0.4386 -0.9805 0.044 Uiso 1 1 calc R . . C15 C 1.1910(4) 0.38985(18) -0.9954(3) 0.0297(10) Uani 1 1 d . . . C16 C 1.3075(5) 0.42055(18) -1.1655(3) 0.0359(11) Uani 1 1 d . . . C17 C 1.1002(5) 0.5137(2) -0.3034(3) 0.0425(12) Uani 1 1 d . . . H17A H 1.0951 0.4990 -0.2454 0.051 Uiso 1 1 calc R . . C18 C 1.0682(6) 0.5659(2) -0.4227(4) 0.0585(15) Uani 1 1 d . . . H18A H 1.0373 0.5930 -0.4632 0.070 Uiso 1 1 calc R . . C19 C 1.1537(5) 0.5287(2) -0.4375(4) 0.0565(15) Uani 1 1 d . . . H19A H 1.1941 0.5259 -0.4905 0.068 Uiso 1 1 calc R . . C20 C 0.9323(5) 0.5819(2) -0.2935(4) 0.0498(13) Uani 1 1 d . . . H20A H 0.9317 0.6208 -0.3058 0.060 Uiso 1 1 calc R . . H20B H 0.9455 0.5769 -0.2276 0.060 Uiso 1 1 calc R . . C21 C 0.8082(5) 0.5579(2) -0.3285(4) 0.0489(13) Uani 1 1 d . . . H21A H 0.7439 0.5773 -0.3001 0.059 Uiso 1 1 calc R . . H21B H 0.7948 0.5643 -0.3940 0.059 Uiso 1 1 calc R . . C22 C 0.7943(5) 0.4976(2) -0.3109(3) 0.0466(12) Uani 1 1 d . . . H22A H 0.7227 0.4840 -0.3489 0.056 Uiso 1 1 calc R . . H22B H 0.8668 0.4787 -0.3287 0.056 Uiso 1 1 calc R . . C23 C 0.7794(6) 0.4849(2) -0.2122(3) 0.0500(13) Uani 1 1 d . . . H23A H 0.8377 0.5068 -0.1735 0.060 Uiso 1 1 calc R . . H23B H 0.6964 0.4952 -0.1993 0.060 Uiso 1 1 calc R . . C24 C 0.8930(5) 0.4082(2) -0.1326(3) 0.0415(12) Uani 1 1 d . . . H24A H 0.9565 0.4298 -0.1047 0.050 Uiso 1 1 calc R . . C25 C 0.7810(5) 0.3394(2) -0.1753(4) 0.0502(13) Uani 1 1 d . . . H25A H 0.7518 0.3038 -0.1819 0.060 Uiso 1 1 calc R . . C26 C 0.7274(5) 0.3835(2) -0.2171(4) 0.0551(14) Uani 1 1 d . . . H26A H 0.6558 0.3841 -0.2575 0.066 Uiso 1 1 calc R . . C27 C 1.4139(5) 0.2388(2) -0.3621(3) 0.0427(12) Uani 1 1 d . A . H27A H 1.4455 0.2726 -0.3766 0.051 Uiso 1 1 calc R . . C28 C 1.3248(5) 0.1754(2) -0.2899(4) 0.0502(13) Uani 1 1 d . A . H28A H 1.2840 0.1565 -0.2467 0.060 Uiso 1 1 calc R . . C29 C 1.3642(5) 0.1551(2) -0.3670(4) 0.0473(13) Uani 1 1 d . . . H29A H 1.3544 0.1190 -0.3864 0.057 Uiso 1 1 calc R A . C30 C 1.3253(7) 0.2693(3) -0.2185(4) 0.078(2) Uani 0.82(8) 1 d PDU A 1 H30A H 1.2992 0.3029 -0.2497 0.094 Uiso 0.82(8) 1 calc PR A 1 H30B H 1.2553 0.2555 -0.1890 0.094 Uiso 0.82(8) 1 calc PR A 1 C30' C 1.3253(7) 0.2693(3) -0.2185(4) 0.078(2) Uani 0.18(8) 1 d P A 2 H30C H 1.2397 0.2793 -0.2364 0.094 Uiso 0.18(8) 1 calc PR A 2 H30D H 1.3741 0.3015 -0.2295 0.094 Uiso 0.18(8) 1 calc PR A 2 C31 C 1.4252(11) 0.2820(4) -0.1480(7) 0.104(5) Uani 0.830(17) 1 d PDU A 1 H31A H 1.4961 0.2947 -0.1776 0.125 Uiso 0.830(17) 1 calc PR A 1 H31B H 1.3986 0.3119 -0.1110 0.125 Uiso 0.830(17) 1 calc PR A 1 C31' C 1.335(3) 0.2631(19) -0.1111(15) 0.146(18) Uani 0.170(17) 1 d PDU A 2 H31C H 1.3272 0.2981 -0.0812 0.175 Uiso 0.170(17) 1 calc PR A 2 H31D H 1.2718 0.2385 -0.0922 0.175 Uiso 0.170(17) 1 calc PR A 2 C32 C 1.4624(11) 0.2396(4) -0.0911(6) 0.123(4) Uani 0.50(12) 1 d PDU A 1 H32A H 1.5034 0.2123 -0.1254 0.147 Uiso 0.50(12) 1 calc PR A 1 H32B H 1.3902 0.2228 -0.0687 0.147 Uiso 0.50(12) 1 calc PR A 1 C32' C 1.4624(11) 0.2396(4) -0.0911(6) 0.123(4) Uani 0.50(12) 1 d P A 2 H32C H 1.5050 0.2452 -0.1455 0.147 Uiso 0.50(12) 1 calc PR A 2 H32D H 1.4525 0.2005 -0.0846 0.147 Uiso 0.50(12) 1 calc PR A 2 C33 C 1.5580(7) 0.2599(3) -0.0030(5) 0.090(2) Uani 0.50 1 d PD A 1 H33A H 1.6363 0.2716 -0.0235 0.108 Uiso 0.50 1 calc PR A 1 H33B H 1.5224 0.2903 0.0280 0.108 Uiso 0.50 1 calc PR A 1 C33' C 1.5580(7) 0.2599(3) -0.0030(5) 0.090(2) Uani 0.50 1 d P A 2 H33C H 1.6363 0.2716 -0.0235 0.108 Uiso 0.50 1 calc PR A 2 H33D H 1.5224 0.2903 0.0280 0.108 Uiso 0.50 1 calc PR A 2 C34 C 1.6671(5) 0.1755(2) 0.0589(3) 0.0451(12) Uani 1 1 d . A . H34A H 1.7287 0.1759 0.0190 0.054 Uiso 1 1 calc R . . C35 C 1.5548(6) 0.1524(3) 0.1640(5) 0.075(2) Uani 1 1 d . A . H35A H 1.5241 0.1332 0.2117 0.090 Uiso 1 1 calc R . . C36 C 1.5061(6) 0.1977(3) 0.1269(5) 0.082(2) Uani 1 1 d . A . H36A H 1.4363 0.2158 0.1436 0.098 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 0.0337(3) 0.0337(3) 0.0355(3) -0.0019(2) 0.0049(2) 0.0029(2) Zn2 0.0374(3) 0.0481(3) 0.0264(3) -0.0001(2) 0.0056(2) 0.0003(3) O1 0.061(2) 0.046(2) 0.0296(17) 0.0012(14) 0.0180(16) 0.0074(17) O1W 0.077(3) 0.059(3) 0.082(3) 0.006(2) 0.035(2) 0.010(2) O2 0.078(3) 0.050(2) 0.0283(18) 0.0120(16) 0.0127(17) 0.0080(19) O2W 0.104(5) 0.319(11) 0.104(5) -0.050(6) 0.001(4) -0.094(6) O3 0.046(2) 0.0312(18) 0.060(2) 0.0047(16) 0.0090(17) 0.0049(16) O3W 0.181(8) 0.135(6) 0.221(9) -0.037(6) -0.098(7) 0.059(5) O4 0.042(2) 0.043(2) 0.065(2) 0.0053(17) 0.0140(18) -0.0064(16) O5 0.0288(17) 0.068(2) 0.0243(16) 0.0056(15) 0.0077(13) -0.0011(15) O6 0.0329(18) 0.0363(19) 0.055(2) 0.0007(15) -0.0001(15) -0.0104(15) O7 0.0328(19) 0.059(2) 0.049(2) -0.0070(17) 0.0077(16) 0.0090(17) O8 0.047(2) 0.060(2) 0.0240(16) 0.0042(15) 0.0061(15) -0.0009(17) O9 0.035(2) 0.074(3) 0.0336(18) 0.0045(17) -0.0002(15) -0.0057(17) N1 0.043(2) 0.049(3) 0.036(2) 0.0040(19) 0.0050(19) 0.0031(19) N2 0.041(2) 0.044(2) 0.047(3) 0.0039(19) 0.0020(19) 0.0044(19) N3 0.044(2) 0.041(2) 0.038(2) 0.0062(18) 0.0026(18) 0.0033(19) N4 0.035(2) 0.038(2) 0.036(2) 0.0032(17) 0.0009(17) 0.0004(17) N5 0.040(2) 0.033(2) 0.034(2) 0.0020(16) 0.0081(17) 0.0048(17) N6 0.047(3) 0.046(3) 0.037(2) -0.0044(18) 0.0104(19) 0.007(2) N7 0.055(3) 0.070(3) 0.047(3) 0.008(2) 0.001(2) 0.019(2) N8 0.041(3) 0.058(3) 0.044(2) 0.004(2) 0.009(2) 0.007(2) C1 0.039(3) 0.035(3) 0.025(2) -0.0015(19) 0.0055(19) -0.012(2) C2 0.026(2) 0.036(2) 0.025(2) 0.0017(18) 0.0018(17) -0.0038(19) C3 0.023(2) 0.030(2) 0.032(2) -0.0023(18) -0.0007(17) 0.0006(17) C4 0.031(2) 0.038(3) 0.031(2) -0.0072(19) 0.0043(19) 0.001(2) C5 0.023(2) 0.050(3) 0.024(2) 0.0015(19) 0.0016(18) -0.0031(19) C6 0.037(3) 0.038(3) 0.030(2) 0.006(2) 0.0018(19) -0.009(2) C7 0.042(3) 0.030(2) 0.036(3) -0.0012(19) 0.005(2) -0.004(2) C8 0.050(3) 0.033(3) 0.026(2) -0.0023(18) 0.006(2) 0.003(2) C9 0.027(2) 0.034(2) 0.026(2) 0.0004(17) 0.0051(18) 0.0029(18) C10 0.030(2) 0.034(2) 0.024(2) 0.0024(17) 0.0095(18) 0.0008(18) C11 0.029(2) 0.026(2) 0.028(2) 0.0005(17) 0.0042(18) 0.0036(17) C12 0.036(3) 0.031(2) 0.025(2) 0.0010(17) 0.0056(18) 0.0042(19) C13 0.038(3) 0.050(3) 0.025(2) 0.007(2) 0.013(2) -0.003(2) C14 0.030(3) 0.048(3) 0.033(2) 0.002(2) 0.007(2) -0.004(2) C15 0.029(2) 0.039(3) 0.022(2) 0.0038(18) 0.0027(17) -0.004(2) C16 0.048(3) 0.032(3) 0.028(2) 0.0035(19) 0.006(2) 0.001(2) C17 0.041(3) 0.050(3) 0.037(3) 0.006(2) 0.005(2) 0.006(2) C18 0.058(4) 0.063(4) 0.054(4) 0.024(3) 0.004(3) 0.005(3) C19 0.060(4) 0.072(4) 0.039(3) 0.013(3) 0.013(3) 0.010(3) C20 0.046(3) 0.043(3) 0.062(4) 0.001(2) 0.010(3) 0.006(2) C21 0.048(3) 0.049(3) 0.048(3) 0.008(2) -0.002(2) 0.009(2) C22 0.041(3) 0.052(3) 0.046(3) 0.000(2) 0.001(2) 0.005(2) C23 0.060(4) 0.043(3) 0.047(3) 0.004(2) 0.008(3) 0.012(3) C24 0.043(3) 0.039(3) 0.042(3) 0.004(2) 0.000(2) -0.006(2) C25 0.046(3) 0.043(3) 0.060(3) 0.000(3) -0.006(3) -0.005(3) C26 0.043(3) 0.059(4) 0.059(4) 0.003(3) -0.012(3) -0.003(3) C27 0.056(3) 0.034(3) 0.040(3) 0.002(2) 0.007(2) -0.004(2) C28 0.045(3) 0.055(3) 0.052(3) 0.004(3) 0.013(3) -0.009(3) C29 0.050(3) 0.042(3) 0.051(3) -0.001(2) 0.013(3) -0.007(2) C30 0.115(6) 0.071(4) 0.051(4) -0.016(3) 0.019(4) 0.007(4) C30' 0.115(6) 0.071(4) 0.051(4) -0.016(3) 0.019(4) 0.007(4) C31 0.134(10) 0.092(8) 0.086(7) -0.014(6) 0.004(7) 0.044(7) C31' 0.20(3) 0.11(3) 0.13(3) 0.05(2) -0.01(3) -0.10(3) C32 0.150(9) 0.099(7) 0.108(7) -0.006(5) -0.040(6) 0.061(6) C32' 0.150(9) 0.099(7) 0.108(7) -0.006(5) -0.040(6) 0.061(6) C33 0.105(6) 0.094(6) 0.072(5) 0.017(4) 0.016(4) 0.044(5) C33' 0.105(6) 0.094(6) 0.072(5) 0.017(4) 0.016(4) 0.044(5) C34 0.035(3) 0.058(3) 0.041(3) -0.001(2) 0.002(2) 0.007(2) C35 0.059(4) 0.100(5) 0.072(4) 0.019(4) 0.033(3) 0.023(4) C36 0.060(4) 0.111(6) 0.078(5) 0.021(4) 0.025(4) 0.042(4) _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 O6 1.965(3) 4_666 ? Zn1 O3 1.969(3) . ? Zn1 N5 1.996(4) . ? Zn1 N4 2.004(4) 4_665 ? Zn2 O8 1.931(3) 1_556 ? Zn2 O1 1.961(3) . ? Zn2 N8 2.001(4) 4_565 ? Zn2 N1 2.008(4) . ? O1 C1 1.274(5) . ? O2 C1 1.225(5) . ? O3 C8 1.265(5) . ? O4 C8 1.238(6) . ? O5 C9 1.373(5) . ? O5 C5 1.385(5) . ? O6 C15 1.266(5) . ? O6 Zn1 1.965(3) 4_565 ? O7 C15 1.231(5) . ? O8 C16 1.291(5) . ? O8 Zn2 1.931(3) 1_554 ? O9 C16 1.221(6) . ? N1 C17 1.312(6) . ? N1 C19 1.376(6) . ? N2 C17 1.333(6) . ? N2 C18 1.372(7) . ? N2 C20 1.462(6) . ? N3 C24 1.328(6) . ? N3 C26 1.364(7) . ? N3 C23 1.463(6) . ? N4 C24 1.311(6) . ? N4 C25 1.370(6) . ? N4 Zn1 2.004(4) 4_566 ? N5 C27 1.306(6) . ? N5 C29 1.365(6) . ? N6 C27 1.326(6) . ? N6 C28 1.361(6) . ? N6 C30 1.476(7) . ? N7 C34 1.334(6) . ? N7 C36 1.363(8) . ? N7 C33 1.476(8) . ? N8 C34 1.306(6) . ? N8 C35 1.370(7) . ? N8 Zn2 2.001(4) 4_666 ? C1 C2 1.501(6) . ? C2 C7 1.378(6) . ? C2 C3 1.401(6) . ? C3 C4 1.381(6) . ? C3 C8 1.502(6) . ? C4 C5 1.368(6) . ? C4 H4A 0.9300 . ? C5 C6 1.376(6) . ? C6 C7 1.375(6) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C9 C10 1.379(6) . ? C9 C14 1.384(6) . ? C10 C11 1.394(6) . ? C10 H10A 0.9300 . ? C11 C12 1.392(6) . ? C11 C15 1.509(6) . ? C12 C13 1.387(6) . ? C12 C16 1.502(6) . ? C13 C14 1.371(6) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.334(8) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.510(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.509(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.504(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9300 . ? C25 C26 1.346(7) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C29 1.341(7) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 C31 1.457(10) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.368(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31' H31C 0.9700 . ? C31' H31D 0.9700 . ? C32 C33 1.652(10) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9300 . ? C35 C36 1.322(9) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? 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 O6 Zn1 O3 93.98(14) 4_666 . ? O6 Zn1 N5 112.50(15) 4_666 . ? O3 Zn1 N5 111.43(15) . . ? O6 Zn1 N4 112.53(15) 4_666 4_665 ? O3 Zn1 N4 115.06(15) . 4_665 ? N5 Zn1 N4 110.47(16) . 4_665 ? O8 Zn2 O1 113.21(15) 1_556 . ? O8 Zn2 N8 116.32(16) 1_556 4_565 ? O1 Zn2 N8 104.91(16) . 4_565 ? O8 Zn2 N1 111.51(15) 1_556 . ? O1 Zn2 N1 100.14(15) . . ? N8 Zn2 N1 109.37(18) 4_565 . ? C1 O1 Zn2 120.8(3) . . ? C8 O3 Zn1 115.0(3) . . ? C9 O5 C5 120.2(3) . . ? C15 O6 Zn1 123.3(3) . 4_565 ? C16 O8 Zn2 111.9(3) . 1_554 ? C17 N1 C19 105.2(4) . . ? C17 N1 Zn2 125.7(3) . . ? C19 N1 Zn2 128.6(4) . . ? C17 N2 C18 106.5(4) . . ? C17 N2 C20 125.4(4) . . ? C18 N2 C20 127.4(5) . . ? C24 N3 C26 107.1(4) . . ? C24 N3 C23 124.8(4) . . ? C26 N3 C23 128.1(5) . . ? C24 N4 C25 105.5(4) . . ? C24 N4 Zn1 124.5(3) . 4_566 ? C25 N4 Zn1 129.6(3) . 4_566 ? C27 N5 C29 104.9(4) . . ? C27 N5 Zn1 127.8(3) . . ? C29 N5 Zn1 127.4(3) . . ? C27 N6 C28 106.8(4) . . ? C27 N6 C30 127.2(5) . . ? C28 N6 C30 125.9(5) . . ? C34 N7 C36 106.5(5) . . ? C34 N7 C33 126.2(5) . . ? C36 N7 C33 127.3(5) . . ? C34 N8 C35 105.5(5) . . ? C34 N8 Zn2 126.8(4) . 4_666 ? C35 N8 Zn2 127.7(4) . 4_666 ? O2 C1 O1 125.4(4) . . ? O2 C1 C2 120.3(4) . . ? O1 C1 C2 114.2(4) . . ? C7 C2 C3 119.0(4) . . ? C7 C2 C1 119.7(4) . . ? C3 C2 C1 121.3(4) . . ? C4 C3 C2 119.1(4) . . ? C4 C3 C8 118.4(4) . . ? C2 C3 C8 122.3(4) . . ? C5 C4 C3 120.8(4) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 120.6(4) . . ? C4 C5 O5 120.9(4) . . ? C6 C5 O5 118.5(4) . . ? C7 C6 C5 119.1(4) . . ? C7 C6 H6A 120.4 . . ? C5 C6 H6A 120.4 . . ? C6 C7 C2 121.4(4) . . ? C6 C7 H7A 119.3 . . ? C2 C7 H7A 119.3 . . ? O4 C8 O3 124.2(4) . . ? O4 C8 C3 118.8(4) . . ? O3 C8 C3 116.9(4) . . ? O5 C9 C10 123.9(4) . . ? O5 C9 C14 114.6(4) . . ? C10 C9 C14 121.5(4) . . ? C9 C10 C11 119.6(4) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C12 C11 C10 119.4(4) . . ? C12 C11 C15 123.3(4) . . ? C10 C11 C15 117.2(4) . . ? C13 C12 C11 119.3(4) . . ? C13 C12 C16 119.4(4) . . ? C11 C12 C16 121.2(4) . . ? C14 C13 C12 121.7(4) . . ? C14 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? C13 C14 C9 118.4(4) . . ? C13 C14 H14A 120.8 . . ? C9 C14 H14A 120.8 . . ? O7 C15 O6 125.6(4) . . ? O7 C15 C11 119.2(4) . . ? O6 C15 C11 115.1(4) . . ? O9 C16 O8 123.8(4) . . ? O9 C16 C12 121.3(4) . . ? O8 C16 C12 114.9(4) . . ? N1 C17 N2 111.9(4) . . ? N1 C17 H17A 124.1 . . ? N2 C17 H17A 124.1 . . ? C19 C18 N2 106.8(5) . . ? C19 C18 H18A 126.6 . . ? N2 C18 H18A 126.6 . . ? C18 C19 N1 109.6(5) . . ? C18 C19 H19A 125.2 . . ? N1 C19 H19A 125.2 . . ? N2 C20 C21 112.0(4) . . ? N2 C20 H20A 109.2 . . ? C21 C20 H20A 109.2 . . ? N2 C20 H20B 109.2 . . ? C21 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C22 C21 C20 115.0(4) . . ? C22 C21 H21A 108.5 . . ? C20 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? C20 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C21 112.9(4) . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22B 109.0 . . ? C21 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? N3 C23 C22 113.7(4) . . ? N3 C23 H23A 108.8 . . ? C22 C23 H23A 108.8 . . ? N3 C23 H23B 108.8 . . ? C22 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N4 C24 N3 111.7(4) . . ? N4 C24 H24A 124.1 . . ? N3 C24 H24A 124.1 . . ? C26 C25 N4 109.3(5) . . ? C26 C25 H25A 125.3 . . ? N4 C25 H25A 125.3 . . ? C25 C26 N3 106.4(5) . . ? C25 C26 H26A 126.8 . . ? N3 C26 H26A 126.8 . . ? N5 C27 N6 112.2(4) . . ? N5 C27 H27A 123.9 . . ? N6 C27 H27A 123.9 . . ? C29 C28 N6 106.2(5) . . ? C29 C28 H28A 126.9 . . ? N6 C28 H28A 126.9 . . ? C28 C29 N5 109.9(5) . . ? C28 C29 H29A 125.0 . . ? N5 C29 H29A 125.0 . . ? C31 C30 N6 115.2(7) . . ? C31 C30 H30A 108.5 . . ? N6 C30 H30A 108.5 . . ? C31 C30 H30B 108.5 . . ? N6 C30 H30B 108.5 . . ? H30A C30 H30B 107.5 . . ? C32 C31 C30 115.2(10) . . ? C32 C31 H31A 108.5 . . ? C30 C31 H31A 108.5 . . ? C32 C31 H31B 108.5 . . ? C30 C31 H31B 108.5 . . ? H31A C31 H31B 107.5 . . ? H31C C31' H31D 109.3 . . ? C31 C32 C33 111.9(8) . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32B 109.2 . . ? C33 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? N7 C33 C32 106.8(6) . . ? N7 C33 H33A 110.4 . . ? C32 C33 H33A 110.4 . . ? N7 C33 H33B 110.4 . . ? C32 C33 H33B 110.4 . . ? H33A C33 H33B 108.6 . . ? N8 C34 N7 111.4(5) . . ? N8 C34 H34A 124.3 . . ? N7 C34 H34A 124.3 . . ? C36 C35 N8 109.6(6) . . ? C36 C35 H35A 125.2 . . ? N8 C35 H35A 125.2 . . ? C35 C36 N7 107.1(5) . . ? C35 C36 H36A 126.4 . . ? N7 C36 H36A 126.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.999 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.085 #====END data_4 _database_code_depnum_ccdc_archive 'CCDC 646925' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Zn2(OA)(phen)2(H2O) ; _chemical_name_common Zn2(OA)(phen)2(H2O) _chemical_melting_point ? _chemical_formula_moiety 'C40 H24 N4 O10 Zn2' _chemical_formula_sum 'C40 H24 N4 O10 Zn2' _chemical_formula_weight 851.37 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 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 14.3155(16) _cell_length_b 13.1762(15) _cell_length_c 17.355(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.976(2) _cell_angle_gamma 90.00 _cell_volume 3271.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3117 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 22.24 _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 1.540 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7088 _exptl_absorpt_correction_T_max 0.9133 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex 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 16537 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6062 _reflns_number_gt 4851 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0445P)^2^+2.8824P] 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 6062 _refine_ls_number_parameters 513 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.004 _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 0.08518(3) 0.80057(3) 0.13960(2) 0.03068(14) Uani 1 1 d . . . Zn2 Zn 0.01878(3) 0.42449(3) 0.21129(3) 0.03463(14) Uani 1 1 d . . . N1 N 0.1295(2) 0.9479(2) 0.11610(17) 0.0327(7) Uani 1 1 d . . . N2 N -0.0436(2) 0.8704(2) 0.11479(17) 0.0339(8) Uani 1 1 d . . . N3 N -0.1011(2) 0.3321(3) 0.21033(19) 0.0367(8) Uani 1 1 d . . . N4 N 0.0742(2) 0.2777(2) 0.24876(18) 0.0349(8) Uani 1 1 d . . . O1 O 0.11027(18) 0.7904(2) 0.25303(15) 0.0374(7) Uani 1 1 d . . . O2 O -0.02082(19) 0.7044(2) 0.23500(15) 0.0398(7) Uani 1 1 d . . . O3 O 0.03958(18) 0.5101(2) 0.30268(16) 0.0402(7) Uani 1 1 d . . . O4 O -0.1055(2) 0.5050(3) 0.3440(2) 0.0639(10) Uani 1 1 d . . . O5 O 0.2715(2) 1.2588(2) 0.42136(19) 0.0559(8) Uani 1 1 d . . . O6 O 0.3974(2) 1.1669(2) 0.41328(16) 0.0445(7) Uani 1 1 d . . . O7 O 0.3686(2) 0.9581(3) 0.3469(2) 0.0709(11) Uani 1 1 d . . . O8 O 0.4410(3) 0.9168(3) 0.4563(3) 0.1077(17) Uani 1 1 d . . . O9 O 0.0930(2) 0.8574(2) 0.54466(15) 0.0480(8) Uani 1 1 d . . . O1W O -0.0624(2) 0.5372(3) 0.1442(2) 0.0462(7) Uani 1 1 d D . . C1 C 0.1624(3) 0.2490(3) 0.2584(2) 0.0446(11) Uani 1 1 d . . . H1 H 0.2092 0.2966 0.2511 0.054 Uiso 1 1 calc R . . C2 C 0.1882(3) 0.1503(4) 0.2790(2) 0.0514(12) Uani 1 1 d . . . H2 H 0.2510 0.1327 0.2850 0.062 Uiso 1 1 calc R . . C3 C 0.1210(4) 0.0806(4) 0.2902(2) 0.0535(13) Uani 1 1 d . . . H3 H 0.1374 0.0147 0.3043 0.064 Uiso 1 1 calc R . . C4 C 0.0261(4) 0.1071(3) 0.2806(2) 0.0441(11) Uani 1 1 d . . . C5 C -0.0502(4) 0.0387(4) 0.2876(3) 0.0573(14) Uani 1 1 d . . . H5 H -0.0384 -0.0281 0.3024 0.069 Uiso 1 1 calc R . . C6 C -0.1381(4) 0.0681(4) 0.2734(3) 0.0581(15) Uani 1 1 d . . . H6 H -0.1863 0.0221 0.2806 0.070 Uiso 1 1 calc R . . C7 C -0.1606(3) 0.1683(4) 0.2473(2) 0.0456(12) Uani 1 1 d . . . C8 C -0.2506(3) 0.2001(4) 0.2245(3) 0.0571(14) Uani 1 1 d . . . H8 H -0.3014 0.1570 0.2301 0.069 Uiso 1 1 calc R . . C9 C -0.2635(3) 0.2947(4) 0.1940(3) 0.0606(14) Uani 1 1 d . . . H9 H -0.3228 0.3163 0.1779 0.073 Uiso 1 1 calc R . . C10 C -0.1866(3) 0.3584(4) 0.1873(3) 0.0492(12) Uani 1 1 d . . . H10 H -0.1959 0.4224 0.1656 0.059 Uiso 1 1 calc R . . C11 C -0.0874(3) 0.2382(3) 0.2399(2) 0.0352(10) Uani 1 1 d . . . C12 C 0.0064(3) 0.2081(3) 0.2583(2) 0.0351(9) Uani 1 1 d . . . C13 C -0.1288(3) 0.8319(4) 0.1174(2) 0.0458(11) Uani 1 1 d . . . H13 H -0.1354 0.7632 0.1281 0.055 Uiso 1 1 calc R . . C14 C -0.2093(3) 0.8902(4) 0.1047(3) 0.0556(13) Uani 1 1 d . . . H14 H -0.2683 0.8613 0.1083 0.067 Uiso 1 1 calc R . . C15 C -0.1997(3) 0.9910(4) 0.0867(2) 0.0537(13) Uani 1 1 d . . . H15 H -0.2524 1.0308 0.0772 0.064 Uiso 1 1 calc R . . C16 C -0.1116(3) 1.0335(3) 0.0825(2) 0.0430(11) Uani 1 1 d . . . C17 C -0.0948(4) 1.1388(4) 0.0650(2) 0.0532(14) Uani 1 1 d . . . H17 H -0.1454 1.1813 0.0537 0.064 Uiso 1 1 calc R . . C18 C -0.0077(4) 1.1772(3) 0.0645(2) 0.0546(13) Uani 1 1 d . . . H18 H 0.0008 1.2451 0.0521 0.065 Uiso 1 1 calc R . . C19 C 0.0718(4) 1.1152(3) 0.0827(2) 0.0430(11) Uani 1 1 d . . . C20 C 0.1640(4) 1.1501(4) 0.0856(2) 0.0553(13) Uani 1 1 d . . . H20 H 0.1765 1.2181 0.0760 0.066 Uiso 1 1 calc R . . C21 C 0.2353(4) 1.0853(4) 0.1022(3) 0.0577(13) Uani 1 1 d . . . H21 H 0.2966 1.1086 0.1038 0.069 Uiso 1 1 calc R . . C22 C 0.2163(3) 0.9840(3) 0.1170(2) 0.0447(11) Uani 1 1 d . . . H22 H 0.2658 0.9400 0.1278 0.054 Uiso 1 1 calc R . . C23 C 0.0580(3) 1.0118(3) 0.0990(2) 0.0325(9) Uani 1 1 d . . . C24 C -0.0346(3) 0.9704(3) 0.0988(2) 0.0341(9) Uani 1 1 d . . . C25 C 0.0430(3) 0.7371(3) 0.2779(2) 0.0301(9) Uani 1 1 d . . . C26 C 0.0392(2) 0.7199(3) 0.3634(2) 0.0281(8) Uani 1 1 d . . . C27 C 0.0719(3) 0.7950(3) 0.4129(2) 0.0313(9) Uani 1 1 d . . . H27 H 0.1002 0.8525 0.3932 0.038 Uiso 1 1 calc R . . C28 C 0.0629(3) 0.7853(3) 0.4910(2) 0.0333(9) Uani 1 1 d . . . C29 C 0.0180(3) 0.7020(3) 0.5209(2) 0.0408(10) Uani 1 1 d . . . H29 H 0.0104 0.6961 0.5737 0.049 Uiso 1 1 calc R . . C30 C -0.0155(3) 0.6275(3) 0.4708(2) 0.0368(10) Uani 1 1 d . . . H30 H -0.0473 0.5723 0.4905 0.044 Uiso 1 1 calc R . . C31 C -0.0029(2) 0.6329(3) 0.3927(2) 0.0304(9) Uani 1 1 d . . . C32 C -0.0277(3) 0.5424(3) 0.3424(2) 0.0334(9) Uani 1 1 d . . . C33 C 0.3131(3) 1.1779(3) 0.4312(2) 0.0366(10) Uani 1 1 d . . . C34 C 0.2610(3) 1.0900(3) 0.4647(2) 0.0308(9) Uani 1 1 d . . . C35 C 0.1773(3) 1.1095(3) 0.4990(2) 0.0392(10) Uani 1 1 d . . . H35 H 0.1579 1.1764 0.5043 0.047 Uiso 1 1 calc R . . C36 C 0.1217(3) 1.0327(3) 0.5255(2) 0.0408(10) Uani 1 1 d . . . H36 H 0.0648 1.0475 0.5471 0.049 Uiso 1 1 calc R . . C37 C 0.1511(3) 0.9343(3) 0.5196(2) 0.0373(10) Uani 1 1 d . . . C38 C 0.2359(3) 0.9133(3) 0.4895(2) 0.0394(10) Uani 1 1 d . . . H38 H 0.2572 0.8466 0.4891 0.047 Uiso 1 1 calc R . . C39 C 0.2909(3) 0.9897(3) 0.4596(2) 0.0367(9) Uani 1 1 d . . . C40 C 0.3754(3) 0.9532(3) 0.4189(3) 0.0522(13) Uani 1 1 d . . . H1WA H -0.049(4) 0.547(5) 0.0991(16) 0.11(3) Uiso 1 1 d D . . H1WB H -0.044(5) 0.587(4) 0.168(4) 0.13(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0342(3) 0.0232(2) 0.0346(3) 0.00394(19) 0.00089(19) 0.00490(19) Zn2 0.0321(3) 0.0246(3) 0.0475(3) -0.0050(2) 0.0069(2) -0.00331(19) N1 0.042(2) 0.0257(18) 0.0305(17) 0.0004(14) 0.0065(14) 0.0015(15) N2 0.0346(19) 0.034(2) 0.0327(18) 0.0063(15) 0.0012(14) 0.0078(15) N3 0.0342(19) 0.0312(19) 0.045(2) -0.0123(16) 0.0091(15) -0.0056(15) N4 0.039(2) 0.0299(19) 0.0358(18) -0.0059(14) 0.0006(15) -0.0016(15) O1 0.0370(16) 0.0396(17) 0.0359(14) 0.0077(13) 0.0048(12) -0.0075(13) O2 0.0421(17) 0.0358(17) 0.0411(16) 0.0031(13) -0.0051(13) -0.0015(13) O3 0.0333(16) 0.0309(16) 0.0564(18) -0.0134(13) 0.0015(13) 0.0033(12) O4 0.051(2) 0.064(2) 0.079(2) -0.0261(19) 0.0225(17) -0.0312(18) O5 0.063(2) 0.0278(17) 0.076(2) 0.0073(16) -0.0053(17) -0.0047(16) O6 0.0495(19) 0.0357(17) 0.0486(17) 0.0048(14) 0.0041(14) -0.0142(14) O7 0.049(2) 0.084(3) 0.082(3) -0.045(2) 0.0320(19) -0.0278(19) O8 0.067(3) 0.090(3) 0.168(5) 0.060(3) 0.040(3) 0.045(2) O9 0.068(2) 0.0404(18) 0.0363(16) -0.0080(13) 0.0173(14) -0.0218(16) O1W 0.0410(18) 0.0397(19) 0.058(2) -0.0022(17) -0.0024(16) -0.0033(15) C1 0.049(3) 0.040(3) 0.044(3) -0.009(2) -0.004(2) -0.001(2) C2 0.062(3) 0.048(3) 0.043(3) -0.009(2) -0.017(2) 0.013(3) C3 0.090(4) 0.033(3) 0.036(2) -0.001(2) -0.014(2) 0.010(3) C4 0.078(3) 0.031(2) 0.023(2) -0.0022(18) 0.001(2) -0.009(2) C5 0.098(4) 0.038(3) 0.036(3) 0.003(2) 0.006(3) -0.018(3) C6 0.092(4) 0.045(3) 0.039(3) -0.003(2) 0.018(3) -0.040(3) C7 0.056(3) 0.048(3) 0.034(2) -0.014(2) 0.017(2) -0.022(2) C8 0.051(3) 0.062(4) 0.060(3) -0.024(3) 0.028(2) -0.030(3) C9 0.037(3) 0.065(4) 0.080(4) -0.026(3) 0.008(2) -0.007(3) C10 0.035(3) 0.043(3) 0.070(3) -0.014(2) 0.010(2) 0.000(2) C11 0.049(3) 0.030(2) 0.028(2) -0.0108(17) 0.0146(18) -0.0120(19) C12 0.049(3) 0.033(2) 0.0236(19) -0.0067(17) 0.0051(17) -0.0068(19) C13 0.043(3) 0.053(3) 0.041(2) 0.007(2) 0.001(2) 0.002(2) C14 0.038(3) 0.079(4) 0.051(3) 0.008(3) 0.003(2) 0.009(3) C15 0.050(3) 0.074(4) 0.037(2) 0.002(2) 0.001(2) 0.031(3) C16 0.058(3) 0.048(3) 0.023(2) -0.0011(19) 0.0025(19) 0.028(2) C17 0.096(4) 0.041(3) 0.023(2) 0.0025(19) 0.006(2) 0.042(3) C18 0.103(4) 0.029(2) 0.031(2) 0.0028(19) 0.006(3) 0.020(3) C19 0.083(4) 0.026(2) 0.020(2) -0.0010(17) 0.008(2) 0.010(2) C20 0.095(4) 0.032(3) 0.040(3) -0.002(2) 0.009(3) -0.017(3) C21 0.070(4) 0.047(3) 0.056(3) -0.004(2) 0.004(3) -0.017(3) C22 0.047(3) 0.044(3) 0.043(2) -0.001(2) 0.007(2) -0.005(2) C23 0.052(3) 0.024(2) 0.0220(19) -0.0009(15) 0.0065(17) 0.0054(19) C24 0.050(3) 0.031(2) 0.0213(18) 0.0005(16) 0.0055(17) 0.0148(19) C25 0.032(2) 0.020(2) 0.038(2) 0.0006(17) 0.0006(18) 0.0073(17) C26 0.025(2) 0.025(2) 0.034(2) 0.0026(16) 0.0032(16) 0.0027(15) C27 0.034(2) 0.023(2) 0.037(2) 0.0021(17) 0.0104(17) -0.0009(17) C28 0.040(2) 0.024(2) 0.036(2) -0.0056(17) 0.0076(17) -0.0017(17) C29 0.054(3) 0.032(2) 0.037(2) -0.0006(19) 0.0137(19) -0.003(2) C30 0.043(2) 0.021(2) 0.047(2) 0.0060(18) 0.0104(19) -0.0024(18) C31 0.026(2) 0.026(2) 0.039(2) 0.0014(17) 0.0044(16) 0.0028(16) C32 0.040(2) 0.021(2) 0.039(2) 0.0026(17) 0.0015(18) -0.0019(18) C33 0.051(3) 0.030(2) 0.028(2) 0.0001(17) -0.0101(19) -0.012(2) C34 0.039(2) 0.026(2) 0.0272(19) -0.0041(16) -0.0017(16) -0.0057(17) C35 0.050(3) 0.030(2) 0.038(2) -0.0044(18) 0.0047(19) 0.0023(19) C36 0.042(2) 0.041(3) 0.040(2) -0.008(2) 0.0103(19) -0.005(2) C37 0.047(3) 0.034(2) 0.031(2) -0.0036(18) 0.0063(18) -0.0103(19) C38 0.052(3) 0.023(2) 0.044(2) -0.0010(18) 0.009(2) -0.0018(19) C39 0.037(2) 0.032(2) 0.041(2) -0.0027(18) 0.0028(18) -0.0035(18) C40 0.049(3) 0.023(2) 0.086(4) 0.000(2) 0.026(3) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.993(3) . ? Zn1 O6 2.006(3) 2_545 ? Zn1 N1 2.087(3) . ? Zn1 N2 2.092(3) . ? Zn1 O5 2.405(3) 2_545 ? Zn1 C33 2.523(4) 2_545 ? Zn2 O3 1.960(3) . ? Zn2 O7 1.981(3) 2_545 ? Zn2 N3 2.104(3) . ? Zn2 N4 2.182(3) . ? Zn2 O1W 2.195(3) . ? N1 C22 1.330(5) . ? N1 C23 1.350(5) . ? N2 C13 1.324(5) . ? N2 C24 1.353(5) . ? N3 C10 1.321(5) . ? N3 C11 1.352(5) . ? N4 C1 1.323(5) . ? N4 C12 1.349(5) . ? O1 C25 1.279(4) . ? O2 C25 1.237(4) . ? O3 C32 1.276(5) . ? O4 C32 1.219(5) . ? O5 C33 1.231(5) . ? O5 Zn1 2.405(3) 2 ? O6 C33 1.265(5) . ? O6 Zn1 2.006(3) 2 ? O7 C40 1.253(6) . ? O7 Zn2 1.981(3) 2 ? O8 C40 1.222(6) . ? O9 C28 1.388(4) . ? O9 C37 1.390(5) . ? O1W H1WA 0.82(2) . ? O1W H1WB 0.82(2) . ? C1 C2 1.396(6) . ? C1 H1 0.9300 . ? C2 C3 1.349(7) . ? C2 H2 0.9300 . ? C3 C4 1.406(7) . ? C3 H3 0.9300 . ? C4 C12 1.412(6) . ? C4 C5 1.425(7) . ? C5 C6 1.332(7) . ? C5 H5 0.9300 . ? C6 C7 1.429(7) . ? C6 H6 0.9300 . ? C7 C8 1.399(7) . ? C7 C11 1.404(6) . ? C8 C9 1.364(7) . ? C8 H8 0.9300 . ? C9 C10 1.393(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.426(6) . ? C13 C14 1.395(6) . ? C13 H13 0.9300 . ? C14 C15 1.372(7) . ? C14 H14 0.9300 . ? C15 C16 1.383(7) . ? C15 H15 0.9300 . ? C16 C24 1.402(5) . ? C16 C17 1.443(7) . ? C17 C18 1.346(7) . ? C17 H17 0.9300 . ? C18 C19 1.427(6) . ? C18 H18 0.9300 . ? C19 C20 1.397(7) . ? C19 C23 1.407(5) . ? C20 C21 1.353(7) . ? C20 H20 0.9300 . ? C21 C22 1.388(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.434(6) . ? C25 C26 1.503(5) . ? C26 C27 1.382(5) . ? C26 C31 1.399(5) . ? C27 C28 1.373(5) . ? C27 H27 0.9300 . ? C28 C29 1.382(5) . ? C29 C30 1.387(5) . ? C29 H29 0.9300 . ? C30 C31 1.375(5) . ? C30 H30 0.9300 . ? C31 C32 1.513(5) . ? C33 C34 1.505(5) . ? C33 Zn1 2.523(4) 2 ? C34 C35 1.380(5) . ? C34 C39 1.393(5) . ? C35 C36 1.377(6) . ? C35 H35 0.9300 . ? C36 C37 1.367(6) . ? C36 H36 0.9300 . ? C37 C38 1.366(6) . ? C38 C39 1.390(5) . ? C38 H38 0.9300 . ? C39 C40 1.500(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O6 111.84(11) . 2_545 ? O1 Zn1 N1 102.10(12) . . ? O6 Zn1 N1 133.18(12) 2_545 . ? O1 Zn1 N2 111.12(11) . . ? O6 Zn1 N2 114.49(13) 2_545 . ? N1 Zn1 N2 79.76(13) . . ? O1 Zn1 O5 106.96(11) . 2_545 ? O6 Zn1 O5 58.42(11) 2_545 2_545 ? N1 Zn1 O5 81.80(11) . 2_545 ? N2 Zn1 O5 140.30(12) . 2_545 ? O1 Zn1 C33 110.54(12) . 2_545 ? O6 Zn1 C33 29.73(13) 2_545 2_545 ? N1 Zn1 C33 108.45(13) . 2_545 ? N2 Zn1 C33 134.48(12) . 2_545 ? O5 Zn1 C33 28.79(12) 2_545 2_545 ? O3 Zn2 O7 100.38(15) . 2_545 ? O3 Zn2 N3 116.12(12) . . ? O7 Zn2 N3 143.43(16) 2_545 . ? O3 Zn2 N4 103.02(12) . . ? O7 Zn2 N4 93.21(13) 2_545 . ? N3 Zn2 N4 77.15(13) . . ? O3 Zn2 O1W 95.93(13) . . ? O7 Zn2 O1W 90.21(13) 2_545 . ? N3 Zn2 O1W 88.30(13) . . ? N4 Zn2 O1W 159.79(13) . . ? C22 N1 C23 118.7(4) . . ? C22 N1 Zn1 128.4(3) . . ? C23 N1 Zn1 112.9(3) . . ? C13 N2 C24 118.3(3) . . ? C13 N2 Zn1 129.2(3) . . ? C24 N2 Zn1 112.4(3) . . ? C10 N3 C11 118.5(4) . . ? C10 N3 Zn2 126.7(3) . . ? C11 N3 Zn2 114.8(3) . . ? C1 N4 C12 118.6(4) . . ? C1 N4 Zn2 128.8(3) . . ? C12 N4 Zn2 112.5(3) . . ? C25 O1 Zn1 105.0(2) . . ? C32 O3 Zn2 122.2(2) . . ? C33 O5 Zn1 80.9(3) . 2 ? C33 O6 Zn1 98.4(3) . 2 ? C40 O7 Zn2 117.5(3) . 2 ? C28 O9 C37 117.7(3) . . ? Zn2 O1W H1WA 118(5) . . ? Zn2 O1W H1WB 97(5) . . ? H1WA O1W H1WB 106(7) . . ? N4 C1 C2 122.8(4) . . ? N4 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.2(5) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 120.3(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C12 116.7(4) . . ? C3 C4 C5 125.0(5) . . ? C12 C4 C5 118.2(5) . . ? C6 C5 C4 121.5(5) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 121.9(4) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C11 117.5(4) . . ? C8 C7 C6 124.2(4) . . ? C11 C7 C6 118.3(5) . . ? C9 C8 C7 119.6(4) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 119.2(5) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N3 C10 C9 122.9(5) . . ? N3 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N3 C11 C7 122.4(4) . . ? N3 C11 C12 117.6(3) . . ? C7 C11 C12 119.9(4) . . ? N4 C12 C4 122.4(4) . . ? N4 C12 C11 117.4(4) . . ? C4 C12 C11 120.1(4) . . ? N2 C13 C14 122.7(5) . . ? N2 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C15 C14 C13 118.7(5) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C24 117.5(4) . . ? C15 C16 C17 124.0(4) . . ? C24 C16 C17 118.5(4) . . ? C18 C17 C16 121.5(4) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 121.1(4) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C23 116.8(4) . . ? C20 C19 C18 124.4(4) . . ? C23 C19 C18 118.8(4) . . ? C21 C20 C19 120.3(4) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 119.7(5) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? N1 C22 C21 122.1(4) . . ? N1 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? N1 C23 C19 122.5(4) . . ? N1 C23 C24 117.2(3) . . ? C19 C23 C24 120.3(4) . . ? N2 C24 C16 122.6(4) . . ? N2 C24 C23 117.7(3) . . ? C16 C24 C23 119.7(4) . . ? O2 C25 O1 122.5(4) . . ? O2 C25 C26 119.3(3) . . ? O1 C25 C26 118.0(3) . . ? C27 C26 C31 120.1(3) . . ? C27 C26 C25 118.9(3) . . ? C31 C26 C25 120.9(3) . . ? C28 C27 C26 120.4(3) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.4(4) . . ? C27 C28 O9 124.1(3) . . ? C29 C28 O9 115.4(3) . . ? C28 C29 C30 118.8(4) . . ? C28 C29 H29 120.6 . . ? C30 C29 H29 120.6 . . ? C31 C30 C29 121.9(4) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C26 118.2(4) . . ? C30 C31 C32 119.5(3) . . ? C26 C31 C32 122.1(3) . . ? O4 C32 O3 125.8(4) . . ? O4 C32 C31 120.0(4) . . ? O3 C32 C31 114.1(3) . . ? O5 C33 O6 121.8(4) . . ? O5 C33 C34 118.4(4) . . ? O6 C33 C34 119.8(4) . . ? O5 C33 Zn1 70.3(2) . 2 ? O6 C33 Zn1 51.85(19) . 2 ? C34 C33 Zn1 169.4(3) . 2 ? C35 C34 C39 118.5(4) . . ? C35 C34 C33 118.2(4) . . ? C39 C34 C33 123.2(4) . . ? C36 C35 C34 121.8(4) . . ? C36 C35 H35 119.1 . . ? C34 C35 H35 119.1 . . ? C37 C36 C35 119.3(4) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C38 C37 C36 120.0(4) . . ? C38 C37 O9 121.4(4) . . ? C36 C37 O9 118.6(4) . . ? C37 C38 C39 121.2(4) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C38 C39 C34 118.9(4) . . ? C38 C39 C40 114.9(4) . . ? C34 C39 C40 126.1(4) . . ? O8 C40 O7 125.6(5) . . ? O8 C40 C39 119.6(5) . . ? O7 C40 C39 114.7(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.612 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.081 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 646926' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H30 N4 O19 Zn4, 2(H2 O)' _chemical_formula_sum 'C52 H34 N4 O21 Zn4' _chemical_formula_weight 1312.31 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' 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 'C 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' _cell_length_a 14.3048(14) _cell_length_b 23.8232(14) _cell_length_c 14.5836(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.253(2) _cell_angle_gamma 90.00 _cell_volume 4890.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9419 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.66 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 2.030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3755 _exptl_absorpt_correction_T_max 0.8545 _exptl_absorpt_process_details 'SADABS(Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Aepex 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 17938 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.50 _reflns_number_total 8847 _reflns_number_gt 8248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0950P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.152(11) _refine_ls_number_reflns 8847 _refine_ls_number_parameters 731 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.78172(4) 0.42112(3) 0.66948(4) 0.02553(15) Uani 1 1 d . . . Zn2 Zn 0.67257(4) 0.43507(2) 0.42995(4) 0.02477(14) Uani 1 1 d . . . Zn3 Zn 1.05610(4) 0.35308(3) 0.83038(4) 0.02742(15) Uani 1 1 d . . . Zn4 Zn 0.41368(4) 0.39254(3) 0.27673(4) 0.03355(17) Uani 1 1 d . . . N1 N 0.3544(4) 0.4680(2) 0.2346(4) 0.0427(13) Uani 1 1 d . . . N2 N 0.2834(4) 0.3657(2) 0.2063(4) 0.0408(12) Uani 1 1 d . . . N3 N 1.1034(3) 0.4356(2) 0.8594(4) 0.0329(11) Uani 1 1 d . . . N4 N 1.1953(4) 0.3402(2) 0.8980(3) 0.0343(11) Uani 1 1 d . . . O1 O 0.4421(3) 0.32596(19) 0.3788(3) 0.0416(10) Uani 1 1 d . . . O2 O 0.3988(3) 0.40729(19) 0.4208(3) 0.0399(10) Uani 1 1 d . . . O3 O 0.5954(3) 0.40062(17) 0.5157(3) 0.0338(9) Uani 1 1 d . . . O4 O 0.6724(3) 0.37276(17) 0.6542(3) 0.0359(9) Uani 1 1 d . . . O5 O 0.2748(3) 0.26439(16) 0.6681(4) 0.0397(10) Uani 1 1 d . . . O6 O 0.2916(3) 0.00043(17) 0.6688(4) 0.0428(10) Uani 1 1 d . . . O7 O 0.0838(3) 0.08721(18) 0.8155(3) 0.0320(9) Uani 1 1 d . . . O8 O 0.0057(3) 0.12900(19) 0.6931(3) 0.0364(9) Uani 1 1 d . . . O9 O 0.1406(3) 0.01074(19) 0.6782(4) 0.0489(12) Uani 1 1 d . . . O10 O 0.8748(3) 0.39488(18) 0.7765(3) 0.0325(9) Uani 1 1 d . . . O11 O 0.9498(3) 0.35767(17) 0.9051(3) 0.0349(9) Uani 1 1 d . . . O12 O 0.8139(3) 0.47528(19) 0.9114(4) 0.0514(12) Uani 1 1 d . . . O13 O 0.6659(3) 0.48572(16) 0.9349(3) 0.0421(10) Uani 1 1 d . . . O14 O 0.6677(3) 0.22293(16) 0.8893(3) 0.0333(9) Uani 1 1 d . . . O15 O 0.5533(3) 0.14560(16) 1.1944(3) 0.0304(8) Uani 1 1 d . . . O16 O 0.4402(3) 0.2101(2) 1.1558(3) 0.0456(11) Uani 1 1 d . . . O17 O 0.3582(3) 0.09891(18) 1.0737(3) 0.0363(9) Uani 1 1 d . . . O18 O 0.2789(3) 0.11455(17) 0.9304(3) 0.0353(9) Uani 1 1 d . . . O1W O 1.0330(3) 0.26390(18) 0.8207(3) 0.0435(10) Uani 1 1 d . . . H1WA H 0.9766 0.2563 0.7761 0.065 Uiso 1 1 d R . . H1WB H 1.0254 0.2497 0.8806 0.065 Uiso 1 1 d R . . O2W O 0.9638(4) 1.0063(3) 0.5445(5) 0.087(2) Uani 1 1 d . . . H2WA H 1.0164 1.0082 0.5822 0.104 Uiso 1 1 d R . . H2WB H 0.9476 0.9720 0.5381 0.104 Uiso 1 1 d R . . O3W O 0.9763(5) 0.4923(4) 0.0541(6) 0.088(2) Uani 1 1 d D . . H3WA H 0.929(6) 0.486(5) 0.013(6) 0.105 Uiso 1 1 d D . . H3WB H 0.955(8) 0.510(5) 0.095(6) 0.105 Uiso 1 1 d D . . C1 C 0.6010(4) 0.3749(2) 0.5907(4) 0.0256(11) Uani 1 1 d . . . C2 C 0.5148(4) 0.3435(2) 0.6076(4) 0.0251(11) Uani 1 1 d . . . C3 C 0.5148(4) 0.3205(2) 0.6949(4) 0.0339(13) Uani 1 1 d . . . H3 H 0.5691 0.3235 0.7405 0.041 Uiso 1 1 calc R . . C4 C 0.4354(4) 0.2932(3) 0.7156(4) 0.0357(13) Uani 1 1 d . . . H4 H 0.4350 0.2791 0.7749 0.043 Uiso 1 1 calc R . . C5 C 0.3582(4) 0.2876(2) 0.6470(4) 0.0295(11) Uani 1 1 d . . . C6 C 0.3555(4) 0.3092(2) 0.5595(4) 0.0304(12) Uani 1 1 d . . . H6 H 0.3012 0.3052 0.5143 0.037 Uiso 1 1 calc R . . C7 C 0.4348(4) 0.3372(2) 0.5386(4) 0.0250(11) Uani 1 1 d . . . C8 C 0.4267(4) 0.3591(2) 0.4412(4) 0.0283(11) Uani 1 1 d . . . C9 C 0.0836(4) 0.1126(2) 0.7402(4) 0.0263(11) Uani 1 1 d . . . C10 C 0.1720(4) 0.1294(2) 0.7051(4) 0.0255(11) Uani 1 1 d . . . C11 C 0.1874(4) 0.1868(2) 0.7023(4) 0.0273(11) Uani 1 1 d . . . H11 H 0.1452 0.2117 0.7223 0.033 Uiso 1 1 calc R . . C12 C 0.2668(4) 0.2067(2) 0.6689(4) 0.0266(11) Uani 1 1 d . . . C13 C 0.3287(4) 0.1707(2) 0.6387(4) 0.0308(12) Uani 1 1 d . . . H13 H 0.3806 0.1844 0.6151 0.037 Uiso 1 1 calc R . . C14 C 0.3134(4) 0.1132(2) 0.6434(4) 0.0309(12) Uani 1 1 d . . . H14 H 0.3563 0.0885 0.6241 0.037 Uiso 1 1 calc R . . C15 C 0.2184(4) 0.0298(2) 0.6743(4) 0.0313(12) Uani 1 1 d . . . C16 C 0.2348(4) 0.0920(2) 0.6764(4) 0.0279(11) Uani 1 1 d . . . C17 C 0.8740(4) 0.3733(2) 0.8542(4) 0.0261(11) Uani 1 1 d . . . C18 C 0.7827(4) 0.3576(2) 0.8848(3) 0.0222(10) Uani 1 1 d . . . C19 C 0.7648(4) 0.3003(2) 0.8803(4) 0.0256(11) Uani 1 1 d . . . H19 H 0.8087 0.2757 0.8623 0.031 Uiso 1 1 calc R . . C20 C 0.6807(4) 0.2801(2) 0.9029(4) 0.0257(11) Uani 1 1 d . . . C21 C 0.6159(4) 0.3159(2) 0.9314(4) 0.0289(11) Uani 1 1 d . . . H21 H 0.5599 0.3022 0.9471 0.035 Uiso 1 1 calc R . . C22 C 0.6353(4) 0.3724(2) 0.9363(4) 0.0299(12) Uani 1 1 d . . . H22 H 0.5923 0.3966 0.9567 0.036 Uiso 1 1 calc R . . C23 C 0.7175(4) 0.3946(2) 0.9116(4) 0.0278(11) Uani 1 1 d . . . C24 C 0.7359(4) 0.4563(2) 0.9193(4) 0.0294(12) Uani 1 1 d . . . C25 C 0.3500(4) 0.1179(2) 0.9942(4) 0.0261(11) Uani 1 1 d . . . C26 C 0.4348(4) 0.1469(2) 0.9677(4) 0.0243(10) Uani 1 1 d . . . C27 C 0.4426(4) 0.1506(2) 0.8751(4) 0.0296(12) Uani 1 1 d . . . H27 H 0.3953 0.1354 0.8300 0.036 Uiso 1 1 calc R . . C28 C 0.5194(4) 0.1767(2) 0.8483(4) 0.0306(12) Uani 1 1 d . . . H28 H 0.5241 0.1797 0.7857 0.037 Uiso 1 1 calc R . . C29 C 0.5892(4) 0.1982(2) 0.9167(4) 0.0268(11) Uani 1 1 d . . . C30 C 0.5837(4) 0.1945(2) 1.0099(4) 0.0304(12) Uani 1 1 d . . . H30 H 0.6321 0.2091 1.0547 0.036 Uiso 1 1 calc R . . C31 C 0.5060(4) 0.1691(2) 1.0365(4) 0.0262(11) Uani 1 1 d . . . C32 C 0.4966(4) 0.1746(2) 1.1369(4) 0.0284(11) Uani 1 1 d . . . C33 C 0.2557(6) 0.3131(4) 0.1895(5) 0.058(2) Uani 1 1 d . . . H33 H 0.2973 0.2844 0.2124 0.070 Uiso 1 1 calc R . . C34 C 0.1675(6) 0.2991(5) 0.1391(6) 0.072(3) Uani 1 1 d . . . H34 H 0.1499 0.2618 0.1284 0.087 Uiso 1 1 calc R . . C35 C 0.1085(6) 0.3405(6) 0.1064(6) 0.078(3) Uani 1 1 d . . . H35 H 0.0489 0.3321 0.0723 0.094 Uiso 1 1 calc R . . C36 C 0.1344(6) 0.3949(5) 0.1221(5) 0.066(3) Uani 1 1 d . . . H36 H 0.0924 0.4235 0.0995 0.079 Uiso 1 1 calc R . . C37 C 0.2250(4) 0.4079(3) 0.1725(4) 0.0450(17) Uani 1 1 d . . . C38 C 0.2628(5) 0.4649(3) 0.1897(5) 0.0462(18) Uani 1 1 d . . . C39 C 0.2107(7) 0.5126(4) 0.1640(6) 0.069(3) Uani 1 1 d . . . H39 H 0.1481 0.5100 0.1330 0.083 Uiso 1 1 calc R . . C40 C 0.2516(8) 0.5637(4) 0.1841(7) 0.083(3) Uani 1 1 d . . . H40 H 0.2169 0.5964 0.1682 0.100 Uiso 1 1 calc R . . C41 C 0.3447(9) 0.5667(4) 0.2282(8) 0.085(3) Uani 1 1 d . . . H41 H 0.3739 0.6014 0.2411 0.102 Uiso 1 1 calc R . . C42 C 0.3944(6) 0.5176(3) 0.2530(6) 0.059(2) Uani 1 1 d . . . H42 H 0.4572 0.5196 0.2833 0.071 Uiso 1 1 calc R . . C43 C 1.0529(5) 0.4815(3) 0.8342(6) 0.0465(16) Uani 1 1 d . . . H43 H 0.9909 0.4779 0.8020 0.056 Uiso 1 1 calc R . . C44 C 1.0896(6) 0.5342(3) 0.8546(7) 0.061(2) Uani 1 1 d . . . H44 H 1.0529 0.5659 0.8369 0.073 Uiso 1 1 calc R . . C45 C 1.1811(6) 0.5394(3) 0.9014(6) 0.063(2) Uani 1 1 d . . . H45 H 1.2071 0.5748 0.9152 0.075 Uiso 1 1 calc R . . C46 C 1.2344(5) 0.4925(3) 0.9280(5) 0.0508(18) Uani 1 1 d . . . H46 H 1.2963 0.4954 0.9606 0.061 Uiso 1 1 calc R . . C47 C 1.1929(4) 0.4399(3) 0.9049(4) 0.0327(13) Uani 1 1 d . . . C48 C 1.2433(4) 0.3865(3) 0.9284(4) 0.0342(13) Uani 1 1 d . . . C49 C 1.3350(5) 0.3834(3) 0.9806(5) 0.0470(17) Uani 1 1 d . . . H49 H 1.3680 0.4160 1.0010 0.056 Uiso 1 1 calc R . . C50 C 1.3754(5) 0.3325(3) 1.0012(5) 0.049 Uani 1 1 d . . . H50 H 1.4353 0.3298 1.0381 0.059 Uiso 1 1 calc R . . C51 C 1.3274(6) 0.2853(4) 0.9676(5) 0.059(2) Uani 1 1 d . . . H51 H 1.3552 0.2502 0.9792 0.071 Uiso 1 1 calc R . . C52 C 1.2370(5) 0.2903(3) 0.9160(5) 0.0486(17) Uani 1 1 d . . . H52 H 1.2043 0.2580 0.8933 0.058 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 0.0207(3) 0.0268(3) 0.0303(3) -0.0029(2) 0.0078(2) -0.0034(2) Zn2 0.0202(3) 0.0237(3) 0.0318(3) 0.0030(2) 0.0085(2) 0.0021(2) Zn3 0.0240(3) 0.0291(3) 0.0297(3) -0.0014(3) 0.0064(2) -0.0033(2) Zn4 0.0251(3) 0.0436(4) 0.0333(3) 0.0074(3) 0.0088(3) 0.0089(3) N1 0.042(3) 0.046(3) 0.045(3) 0.016(2) 0.022(2) 0.014(2) N2 0.033(3) 0.053(3) 0.038(3) 0.010(2) 0.009(2) 0.000(3) N3 0.031(3) 0.026(2) 0.044(3) -0.004(2) 0.015(2) -0.004(2) N4 0.033(3) 0.037(3) 0.033(3) -0.002(2) 0.005(2) 0.003(2) O1 0.049(3) 0.045(2) 0.032(2) -0.0039(18) 0.0097(18) 0.005(2) O2 0.044(2) 0.038(2) 0.038(2) 0.0074(18) 0.0076(18) 0.0088(19) O3 0.027(2) 0.042(2) 0.034(2) 0.0116(17) 0.0084(16) -0.0054(16) O4 0.0240(19) 0.037(2) 0.043(2) 0.0088(18) -0.0032(17) -0.0107(17) O5 0.026(2) 0.025(2) 0.073(3) 0.010(2) 0.023(2) -0.0020(17) O6 0.044(3) 0.0227(19) 0.066(3) -0.003(2) 0.023(2) 0.0016(19) O7 0.026(2) 0.043(2) 0.027(2) 0.0065(17) 0.0050(16) -0.0067(16) O8 0.026(2) 0.047(2) 0.036(2) 0.0095(19) 0.0058(17) -0.0008(18) O9 0.042(3) 0.036(3) 0.071(3) -0.007(2) 0.017(2) -0.015(2) O10 0.0203(18) 0.049(2) 0.028(2) 0.0066(17) 0.0031(15) -0.0067(16) O11 0.0205(19) 0.045(2) 0.039(2) 0.0085(18) 0.0055(17) 0.0016(17) O12 0.045(3) 0.034(2) 0.081(3) -0.009(2) 0.026(2) -0.010(2) O13 0.047(3) 0.022(2) 0.064(3) -0.002(2) 0.028(2) 0.0024(19) O14 0.028(2) 0.0238(19) 0.053(2) -0.0022(17) 0.0207(18) -0.0059(15) O15 0.032(2) 0.035(2) 0.0246(18) 0.0017(16) 0.0078(16) 0.0058(16) O16 0.045(3) 0.051(3) 0.040(2) -0.001(2) 0.0063(19) 0.021(2) O17 0.033(2) 0.045(2) 0.034(2) 0.0088(18) 0.0138(17) -0.0046(17) O18 0.026(2) 0.041(2) 0.038(2) 0.0023(17) 0.0030(17) -0.0134(17) O1W 0.054(3) 0.033(2) 0.043(2) 0.0026(19) 0.008(2) -0.0112(19) O2W 0.056(4) 0.071(4) 0.119(6) -0.029(4) -0.022(4) 0.024(3) O3W 0.058(4) 0.108(6) 0.092(5) -0.005(4) -0.001(3) 0.037(4) C1 0.021(3) 0.022(2) 0.034(3) 0.000(2) 0.007(2) 0.002(2) C2 0.023(3) 0.022(3) 0.032(3) 0.004(2) 0.009(2) 0.0011(19) C3 0.028(3) 0.036(3) 0.035(3) 0.007(2) 0.000(2) -0.004(2) C4 0.038(3) 0.034(3) 0.037(3) 0.014(3) 0.013(3) 0.001(2) C5 0.025(3) 0.021(3) 0.045(3) 0.004(2) 0.014(2) -0.001(2) C6 0.022(3) 0.027(3) 0.042(3) 0.001(2) 0.005(2) -0.001(2) C7 0.023(3) 0.019(2) 0.033(3) 0.000(2) 0.008(2) 0.001(2) C8 0.020(3) 0.033(3) 0.032(3) 0.000(2) 0.006(2) -0.003(2) C9 0.027(3) 0.024(3) 0.028(3) -0.003(2) 0.008(2) -0.004(2) C10 0.023(3) 0.028(3) 0.025(3) 0.002(2) 0.003(2) -0.003(2) C11 0.021(3) 0.029(3) 0.034(3) 0.001(2) 0.011(2) 0.000(2) C12 0.026(3) 0.024(3) 0.029(3) 0.004(2) 0.003(2) -0.004(2) C13 0.022(3) 0.032(3) 0.040(3) 0.003(2) 0.011(2) -0.006(2) C14 0.030(3) 0.033(3) 0.032(3) -0.004(2) 0.012(2) 0.002(2) C15 0.041(3) 0.027(3) 0.027(3) -0.001(2) 0.009(2) 0.000(2) C16 0.026(3) 0.031(3) 0.028(3) -0.002(2) 0.007(2) -0.002(2) C17 0.023(3) 0.023(3) 0.031(3) -0.005(2) 0.005(2) -0.002(2) C18 0.019(2) 0.024(3) 0.024(2) 0.0015(19) 0.005(2) 0.0013(19) C19 0.020(2) 0.027(3) 0.030(3) 0.000(2) 0.007(2) 0.000(2) C20 0.027(3) 0.023(3) 0.027(3) 0.003(2) 0.004(2) -0.003(2) C21 0.020(3) 0.033(3) 0.036(3) 0.003(2) 0.012(2) -0.003(2) C22 0.025(3) 0.028(3) 0.039(3) 0.001(2) 0.013(2) 0.006(2) C23 0.028(3) 0.029(3) 0.027(3) 0.000(2) 0.006(2) 0.001(2) C24 0.033(3) 0.027(3) 0.030(3) -0.001(2) 0.010(2) 0.000(2) C25 0.023(3) 0.021(2) 0.036(3) 0.000(2) 0.009(2) 0.001(2) C26 0.021(2) 0.024(3) 0.028(3) 0.001(2) 0.004(2) -0.0024(19) C27 0.028(3) 0.032(3) 0.028(3) 0.002(2) 0.004(2) -0.004(2) C28 0.035(3) 0.033(3) 0.025(3) 0.004(2) 0.009(2) 0.000(2) C29 0.022(3) 0.024(3) 0.035(3) 0.002(2) 0.008(2) -0.0012(19) C30 0.022(3) 0.032(3) 0.037(3) -0.001(2) 0.002(2) -0.004(2) C31 0.024(3) 0.024(3) 0.031(3) 0.004(2) 0.006(2) 0.002(2) C32 0.026(3) 0.028(3) 0.030(3) 0.000(2) 0.005(2) -0.003(2) C33 0.055(5) 0.074(6) 0.049(4) 0.003(4) 0.014(3) -0.018(4) C34 0.058(5) 0.103(7) 0.059(5) -0.009(5) 0.018(4) -0.031(5) C35 0.042(5) 0.144(10) 0.050(5) -0.013(6) 0.011(4) -0.032(6) C36 0.038(4) 0.121(8) 0.041(4) 0.013(4) 0.010(3) 0.018(5) C37 0.028(3) 0.080(5) 0.029(3) 0.009(3) 0.012(3) 0.014(3) C38 0.040(4) 0.067(5) 0.035(3) 0.021(3) 0.017(3) 0.029(3) C39 0.071(6) 0.083(7) 0.059(5) 0.024(4) 0.028(4) 0.039(5) C40 0.103(9) 0.070(7) 0.090(7) 0.032(5) 0.054(6) 0.045(6) C41 0.105(9) 0.044(5) 0.122(9) 0.017(5) 0.061(7) 0.012(5) C42 0.056(5) 0.052(5) 0.075(5) 0.008(4) 0.026(4) 0.001(4) C43 0.032(3) 0.039(3) 0.070(5) -0.002(3) 0.014(3) -0.002(3) C44 0.053(5) 0.033(4) 0.105(7) 0.004(4) 0.033(4) 0.004(3) C45 0.063(5) 0.038(4) 0.094(6) -0.020(4) 0.032(4) -0.024(4) C46 0.049(4) 0.043(4) 0.064(4) -0.018(3) 0.020(3) -0.018(3) C47 0.028(3) 0.039(3) 0.034(3) -0.010(2) 0.015(2) -0.010(2) C48 0.029(3) 0.045(3) 0.030(3) -0.008(2) 0.008(2) -0.007(2) C49 0.029(3) 0.070(5) 0.041(4) -0.013(3) 0.005(3) -0.009(3) C50 0.029 0.069 0.044 -0.009 -0.003 0.013 C51 0.056(5) 0.063(5) 0.055(4) 0.000(4) -0.001(4) 0.026(4) C52 0.045(4) 0.043(4) 0.053(4) -0.006(3) -0.005(3) 0.009(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 O6 1.895(4) 3 ? Zn1 O4 1.923(4) . ? Zn1 O10 1.964(4) . ? Zn1 O17 1.980(4) 4_554 ? Zn2 O13 1.891(4) 2_564 ? Zn2 O18 1.926(4) 4_554 ? Zn2 O7 1.982(4) 4_554 ? Zn2 O3 1.986(4) . ? Zn3 O15 1.977(4) 4_554 ? Zn3 O11 2.026(4) . ? Zn3 N4 2.082(5) . ? Zn3 N3 2.097(5) . ? Zn3 O1W 2.151(4) . ? Zn4 O8 2.014(4) 4_554 ? Zn4 N1 2.036(5) . ? Zn4 N2 2.063(6) . ? Zn4 O1 2.164(4) . ? Zn4 O2 2.178(4) . ? Zn4 O7 2.447(4) 4_554 ? Zn4 C9 2.582(5) 4_554 ? N1 C42 1.319(10) . ? N1 C38 1.359(9) . ? N2 C33 1.323(10) . ? N2 C37 1.344(9) . ? N3 C43 1.326(9) . ? N3 C47 1.338(8) . ? N4 C48 1.332(8) . ? N4 C52 1.335(9) . ? O1 C8 1.253(7) . ? O2 C8 1.235(7) . ? O3 C1 1.244(7) . ? O4 C1 1.252(7) . ? O5 C12 1.379(7) . ? O5 C5 1.398(7) . ? O6 C15 1.273(7) . ? O6 Zn1 1.895(4) 3_445 ? O7 C9 1.253(7) . ? O7 Zn2 1.982(4) 4_455 ? O7 Zn4 2.447(4) 4_455 ? O8 C9 1.262(7) . ? O8 Zn4 2.014(4) 4_455 ? O9 C15 1.213(8) . ? O10 C17 1.246(7) . ? O11 C17 1.256(7) . ? O12 C24 1.228(7) . ? O13 C24 1.276(7) . ? O13 Zn2 1.891(4) 2_565 ? O14 C20 1.383(7) . ? O14 C29 1.389(6) . ? O15 C32 1.264(7) . ? O15 Zn3 1.977(4) 4_455 ? O16 C32 1.232(7) . ? O17 C25 1.230(7) . ? O17 Zn1 1.980(4) 4_455 ? O18 C25 1.252(7) . ? O18 Zn2 1.926(4) 4_455 ? O1W H1WA 0.9599 . ? O1W H1WB 0.9601 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.84(5) . ? O3W H3WB 0.83(5) . ? C1 C2 1.500(7) . ? C2 C3 1.387(8) . ? C2 C7 1.391(8) . ? C3 C4 1.389(8) . ? C3 H3 0.9300 . ? C4 C5 1.358(8) . ? C4 H4 0.9300 . ? C5 C6 1.370(8) . ? C6 C7 1.395(8) . ? C6 H6 0.9300 . ? C7 C8 1.497(8) . ? C9 C10 1.501(7) . ? C9 Zn4 2.582(5) 4_455 ? C10 C16 1.382(8) . ? C10 C11 1.385(8) . ? C11 C12 1.397(8) . ? C11 H11 0.9300 . ? C12 C13 1.361(8) . ? C13 C14 1.390(8) . ? C13 H13 0.9300 . ? C14 C16 1.395(8) . ? C14 H14 0.9300 . ? C15 C16 1.499(8) . ? C17 C18 1.501(7) . ? C18 C19 1.387(8) . ? C18 C23 1.390(8) . ? C19 C20 1.390(8) . ? C19 H19 0.9300 . ? C20 C21 1.379(8) . ? C21 C22 1.374(8) . ? C21 H21 0.9300 . ? C22 C23 1.393(8) . ? C22 H22 0.9300 . ? C23 C24 1.493(8) . ? C25 C26 1.505(7) . ? C26 C27 1.378(7) . ? C26 C31 1.400(8) . ? C27 C28 1.378(8) . ? C27 H27 0.9300 . ? C28 C29 1.378(8) . ? C28 H28 0.9300 . ? C29 C30 1.379(8) . ? C30 C31 1.380(8) . ? C30 H30 0.9300 . ? C31 C32 1.501(7) . ? C33 C34 1.383(12) . ? C33 H33 0.9300 . ? C34 C35 1.330(15) . ? C34 H34 0.9300 . ? C35 C36 1.356(14) . ? C35 H35 0.9300 . ? C36 C37 1.407(11) . ? C36 H36 0.9300 . ? C37 C38 1.465(11) . ? C38 C39 1.376(10) . ? C39 C40 1.360(15) . ? C39 H39 0.9300 . ? C40 C41 1.372(16) . ? C40 H40 0.9300 . ? C41 C42 1.383(12) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.374(10) . ? C43 H43 0.9300 . ? C44 C45 1.369(12) . ? C44 H44 0.9300 . ? C45 C46 1.369(12) . ? C45 H45 0.9300 . ? C46 C47 1.402(9) . ? C46 H46 0.9300 . ? C47 C48 1.472(9) . ? C48 C49 1.397(9) . ? C49 C50 1.353(11) . ? C49 H49 0.9300 . ? C50 C51 1.363(12) . ? C50 H50 0.9300 . ? C51 C52 1.380(10) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? 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 O6 Zn1 O4 131.0(2) 3 . ? O6 Zn1 O10 106.3(2) 3 . ? O4 Zn1 O10 108.86(16) . . ? O6 Zn1 O17 100.71(19) 3 4_554 ? O4 Zn1 O17 108.28(19) . 4_554 ? O10 Zn1 O17 95.90(17) . 4_554 ? O13 Zn2 O18 131.11(19) 2_564 4_554 ? O13 Zn2 O7 105.7(2) 2_564 4_554 ? O18 Zn2 O7 103.05(17) 4_554 4_554 ? O13 Zn2 O3 110.53(18) 2_564 . ? O18 Zn2 O3 105.73(18) 4_554 . ? O7 Zn2 O3 94.32(17) 4_554 . ? O15 Zn3 O11 130.98(16) 4_554 . ? O15 Zn3 N4 108.94(18) 4_554 . ? O11 Zn3 N4 119.98(18) . . ? O15 Zn3 N3 97.78(18) 4_554 . ? O11 Zn3 N3 95.00(18) . . ? N4 Zn3 N3 78.2(2) . . ? O15 Zn3 O1W 88.55(16) 4_554 . ? O11 Zn3 O1W 88.12(18) . . ? N4 Zn3 O1W 90.49(19) . . ? N3 Zn3 O1W 168.32(19) . . ? O8 Zn4 N1 108.91(19) 4_554 . ? O8 Zn4 N2 104.44(19) 4_554 . ? N1 Zn4 N2 80.4(2) . . ? O8 Zn4 O1 99.61(17) 4_554 . ? N1 Zn4 O1 150.73(18) . . ? N2 Zn4 O1 99.1(2) . . ? O8 Zn4 O2 144.31(16) 4_554 . ? N1 Zn4 O2 92.38(19) . . ? N2 Zn4 O2 107.20(19) . . ? O1 Zn4 O2 59.55(16) . . ? O8 Zn4 O7 57.28(14) 4_554 4_554 ? N1 Zn4 O7 103.8(2) . 4_554 ? N2 Zn4 O7 161.71(18) . 4_554 ? O1 Zn4 O7 85.89(16) . 4_554 ? O2 Zn4 O7 90.54(15) . 4_554 ? O8 Zn4 C9 28.61(16) 4_554 4_554 ? N1 Zn4 C9 109.64(19) . 4_554 ? N2 Zn4 C9 133.04(19) . 4_554 ? O1 Zn4 C9 92.22(17) . 4_554 ? O2 Zn4 C9 117.65(17) . 4_554 ? O7 Zn4 C9 28.70(15) 4_554 4_554 ? C42 N1 C38 119.5(6) . . ? C42 N1 Zn4 126.0(5) . . ? C38 N1 Zn4 114.2(5) . . ? C33 N2 C37 119.7(7) . . ? C33 N2 Zn4 126.9(5) . . ? C37 N2 Zn4 113.4(5) . . ? C43 N3 C47 120.1(5) . . ? C43 N3 Zn3 125.2(4) . . ? C47 N3 Zn3 114.7(4) . . ? C48 N4 C52 119.1(6) . . ? C48 N4 Zn3 115.4(4) . . ? C52 N4 Zn3 125.5(5) . . ? C8 O1 Zn4 90.1(4) . . ? C8 O2 Zn4 90.0(4) . . ? C1 O3 Zn2 143.3(4) . . ? C1 O4 Zn1 126.9(4) . . ? C12 O5 C5 118.1(4) . . ? C15 O6 Zn1 119.0(4) . 3_445 ? C9 O7 Zn2 140.3(4) . 4_455 ? C9 O7 Zn4 81.7(3) . 4_455 ? Zn2 O7 Zn4 135.16(19) 4_455 4_455 ? C9 O8 Zn4 101.6(3) . 4_455 ? C17 O10 Zn1 137.7(4) . . ? C17 O11 Zn3 110.5(3) . . ? C24 O13 Zn2 119.7(4) . 2_565 ? C20 O14 C29 118.0(4) . . ? C32 O15 Zn3 123.6(4) . 4_455 ? C25 O17 Zn1 141.4(4) . 4_455 ? C25 O18 Zn2 125.3(4) . 4_455 ? Zn3 O1W H1WA 109.4 . . ? Zn3 O1W H1WB 109.2 . . ? H1WA O1W H1WB 109.5 . . ? H2WA O2W H2WB 108.4 . . ? H3WA O3W H3WB 105(10) . . ? O3 C1 O4 125.9(5) . . ? O3 C1 C2 117.6(5) . . ? O4 C1 C2 116.5(5) . . ? C3 C2 C7 119.2(5) . . ? C3 C2 C1 118.8(5) . . ? C7 C2 C1 122.0(5) . . ? C2 C3 C4 121.1(5) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 118.5(5) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C4 C5 C6 122.2(5) . . ? C4 C5 O5 119.4(5) . . ? C6 C5 O5 118.1(5) . . ? C5 C6 C7 119.6(5) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C2 C7 C6 119.3(5) . . ? C2 C7 C8 124.3(5) . . ? C6 C7 C8 116.4(5) . . ? O2 C8 O1 120.1(5) . . ? O2 C8 C7 121.3(5) . . ? O1 C8 C7 118.4(5) . . ? O7 C9 O8 119.4(5) . . ? O7 C9 C10 123.8(5) . . ? O8 C9 C10 116.6(5) . . ? O7 C9 Zn4 69.6(3) . 4_455 ? O8 C9 Zn4 49.8(3) . 4_455 ? C10 C9 Zn4 164.7(4) . 4_455 ? C16 C10 C11 120.8(5) . . ? C16 C10 C9 124.3(5) . . ? C11 C10 C9 114.9(5) . . ? C10 C11 C12 119.3(5) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 O5 124.5(5) . . ? C13 C12 C11 121.0(5) . . ? O5 C12 C11 114.5(5) . . ? C12 C13 C14 119.2(5) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C16 121.2(5) . . ? C13 C14 H14 119.4 . . ? C16 C14 H14 119.4 . . ? O9 C15 O6 124.7(5) . . ? O9 C15 C16 120.7(5) . . ? O6 C15 C16 114.6(5) . . ? C10 C16 C14 118.5(5) . . ? C10 C16 C15 122.4(5) . . ? C14 C16 C15 119.0(5) . . ? O10 C17 O11 120.9(5) . . ? O10 C17 C18 121.5(5) . . ? O11 C17 C18 117.1(5) . . ? C19 C18 C23 120.7(5) . . ? C19 C18 C17 113.3(5) . . ? C23 C18 C17 126.0(5) . . ? C18 C19 C20 119.3(5) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C21 C20 O14 125.0(5) . . ? C21 C20 C19 120.9(5) . . ? O14 C20 C19 114.0(5) . . ? C22 C21 C20 118.8(5) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C23 122.0(5) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C18 C23 C22 118.1(5) . . ? C18 C23 C24 121.9(5) . . ? C22 C23 C24 119.9(5) . . ? O12 C24 O13 124.6(5) . . ? O12 C24 C23 120.4(5) . . ? O13 C24 C23 114.9(5) . . ? O17 C25 O18 127.2(5) . . ? O17 C25 C26 117.7(5) . . ? O18 C25 C26 115.1(5) . . ? C27 C26 C31 120.1(5) . . ? C27 C26 C25 119.4(5) . . ? C31 C26 C25 120.5(5) . . ? C28 C27 C26 121.0(5) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C29 C28 C27 118.3(5) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C28 C29 C30 122.0(5) . . ? C28 C29 O14 117.9(5) . . ? C30 C29 O14 120.1(5) . . ? C29 C30 C31 119.7(5) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C30 C31 C26 119.0(5) . . ? C30 C31 C32 116.9(5) . . ? C26 C31 C32 123.5(5) . . ? O16 C32 O15 126.5(5) . . ? O16 C32 C31 117.0(5) . . ? O15 C32 C31 116.1(5) . . ? N2 C33 C34 122.8(9) . . ? N2 C33 H33 118.6 . . ? C34 C33 H33 118.6 . . ? C35 C34 C33 118.1(10) . . ? C35 C34 H34 120.9 . . ? C33 C34 H34 120.9 . . ? C34 C35 C36 120.8(8) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C35 C36 C37 119.8(8) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? N2 C37 C36 118.7(8) . . ? N2 C37 C38 116.4(6) . . ? C36 C37 C38 124.9(7) . . ? N1 C38 C39 121.0(8) . . ? N1 C38 C37 115.4(5) . . ? C39 C38 C37 123.6(7) . . ? C40 C39 C38 119.3(9) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 119.5(9) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C40 C41 C42 119.3(10) . . ? C40 C41 H41 120.4 . . ? C42 C41 H41 120.4 . . ? N1 C42 C41 121.4(9) . . ? N1 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? N3 C43 C44 121.7(7) . . ? N3 C43 H43 119.1 . . ? C44 C43 H43 119.1 . . ? C45 C44 C43 119.0(7) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C46 C45 C44 120.1(7) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 118.1(7) . . ? C45 C46 H46 120.9 . . ? C47 C46 H46 120.9 . . ? N3 C47 C46 121.0(6) . . ? N3 C47 C48 115.8(5) . . ? C46 C47 C48 123.2(6) . . ? N4 C48 C49 121.1(6) . . ? N4 C48 C47 115.8(5) . . ? C49 C48 C47 123.1(6) . . ? C50 C49 C48 119.4(7) . . ? C50 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? C49 C50 C51 119.5(6) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C50 C51 C52 119.2(7) . . ? C50 C51 H51 120.4 . . ? C52 C51 H51 120.4 . . ? N4 C52 C51 121.7(7) . . ? N4 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? 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 O8 Zn4 N1 C42 -79.1(6) 4_554 . . . ? N2 Zn4 N1 C42 178.9(6) . . . . ? O1 Zn4 N1 C42 87.4(7) . . . . ? O2 Zn4 N1 C42 71.8(6) . . . . ? O7 Zn4 N1 C42 -19.3(6) 4_554 . . . ? C9 Zn4 N1 C42 -48.7(6) 4_554 . . . ? O8 Zn4 N1 C38 106.1(4) 4_554 . . . ? N2 Zn4 N1 C38 4.0(4) . . . . ? O1 Zn4 N1 C38 -87.4(6) . . . . ? O2 Zn4 N1 C38 -103.0(4) . . . . ? O7 Zn4 N1 C38 165.8(4) 4_554 . . . ? C9 Zn4 N1 C38 136.5(4) 4_554 . . . ? O8 Zn4 N2 C33 67.5(6) 4_554 . . . ? N1 Zn4 N2 C33 174.7(6) . . . . ? O1 Zn4 N2 C33 -35.0(6) . . . . ? O2 Zn4 N2 C33 -95.8(6) . . . . ? O7 Zn4 N2 C33 69.6(9) 4_554 . . . ? C9 Zn4 N2 C33 66.7(6) 4_554 . . . ? O8 Zn4 N2 C37 -109.7(4) 4_554 . . . ? N1 Zn4 N2 C37 -2.5(4) . . . . ? O1 Zn4 N2 C37 147.8(4) . . . . ? O2 Zn4 N2 C37 87.0(4) . . . . ? O7 Zn4 N2 C37 -107.6(7) 4_554 . . . ? C9 Zn4 N2 C37 -110.5(4) 4_554 . . . ? O15 Zn3 N3 C43 69.7(6) 4_554 . . . ? O11 Zn3 N3 C43 -62.9(6) . . . . ? N4 Zn3 N3 C43 177.5(6) . . . . ? O1W Zn3 N3 C43 -168.0(8) . . . . ? O15 Zn3 N3 C47 -108.6(4) 4_554 . . . ? O11 Zn3 N3 C47 118.8(4) . . . . ? N4 Zn3 N3 C47 -0.8(4) . . . . ? O1W Zn3 N3 C47 13.7(12) . . . . ? O15 Zn3 N4 C48 96.6(4) 4_554 . . . ? O11 Zn3 N4 C48 -86.6(5) . . . . ? N3 Zn3 N4 C48 2.4(4) . . . . ? O1W Zn3 N4 C48 -174.7(4) . . . . ? O15 Zn3 N4 C52 -86.4(6) 4_554 . . . ? O11 Zn3 N4 C52 90.3(6) . . . . ? N3 Zn3 N4 C52 179.3(6) . . . . ? O1W Zn3 N4 C52 2.2(6) . . . . ? O8 Zn4 O1 C8 146.1(3) 4_554 . . . ? N1 Zn4 O1 C8 -20.9(6) . . . . ? N2 Zn4 O1 C8 -107.4(3) . . . . ? O2 Zn4 O1 C8 -2.7(3) . . . . ? O7 Zn4 O1 C8 90.3(3) 4_554 . . . ? C9 Zn4 O1 C8 118.3(3) 4_554 . . . ? O8 Zn4 O2 C8 -58.1(5) 4_554 . . . ? N1 Zn4 O2 C8 174.0(4) . . . . ? N2 Zn4 O2 C8 93.3(4) . . . . ? O1 Zn4 O2 C8 2.8(3) . . . . ? O7 Zn4 O2 C8 -82.1(3) 4_554 . . . ? C9 Zn4 O2 C8 -72.3(4) 4_554 . . . ? O13 Zn2 O3 C1 -107.9(7) 2_564 . . . ? O18 Zn2 O3 C1 38.7(7) 4_554 . . . ? O7 Zn2 O3 C1 143.6(7) 4_554 . . . ? O6 Zn1 O4 C1 50.0(6) 3 . . . ? O10 Zn1 O4 C1 -176.3(5) . . . . ? O17 Zn1 O4 C1 -73.2(5) 4_554 . . . ? O6 Zn1 O10 C17 109.9(6) 3 . . . ? O4 Zn1 O10 C17 -35.5(6) . . . . ? O17 Zn1 O10 C17 -147.1(6) 4_554 . . . ? O15 Zn3 O11 C17 -13.4(5) 4_554 . . . ? N4 Zn3 O11 C17 170.7(4) . . . . ? N3 Zn3 O11 C17 91.4(4) . . . . ? O1W Zn3 O11 C17 -99.8(4) . . . . ? Zn2 O3 C1 O4 18.4(10) . . . . ? Zn2 O3 C1 C2 -161.5(4) . . . . ? Zn1 O4 C1 O3 16.1(9) . . . . ? Zn1 O4 C1 C2 -163.9(4) . . . . ? O3 C1 C2 C3 -171.9(5) . . . . ? O4 C1 C2 C3 8.1(8) . . . . ? O3 C1 C2 C7 7.6(8) . . . . ? O4 C1 C2 C7 -172.4(5) . . . . ? C7 C2 C3 C4 -2.4(8) . . . . ? C1 C2 C3 C4 177.1(5) . . . . ? C2 C3 C4 C5 2.4(9) . . . . ? C3 C4 C5 C6 -1.7(9) . . . . ? C3 C4 C5 O5 -174.8(5) . . . . ? C12 O5 C5 C4 -83.9(7) . . . . ? C12 O5 C5 C6 102.7(6) . . . . ? C4 C5 C6 C7 1.1(9) . . . . ? O5 C5 C6 C7 174.2(5) . . . . ? C3 C2 C7 C6 1.7(8) . . . . ? C1 C2 C7 C6 -177.8(5) . . . . ? C3 C2 C7 C8 -178.8(5) . . . . ? C1 C2 C7 C8 1.7(8) . . . . ? C5 C6 C7 C2 -1.0(8) . . . . ? C5 C6 C7 C8 179.4(5) . . . . ? Zn4 O2 C8 O1 -4.8(5) . . . . ? Zn4 O2 C8 C7 -179.5(4) . . . . ? Zn4 O1 C8 O2 4.8(5) . . . . ? Zn4 O1 C8 C7 179.7(4) . . . . ? C2 C7 C8 O2 -87.5(7) . . . . ? C6 C7 C8 O2 92.0(7) . . . . ? C2 C7 C8 O1 97.6(6) . . . . ? C6 C7 C8 O1 -82.8(6) . . . . ? Zn2 O7 C9 O8 -163.9(4) 4_455 . . . ? Zn4 O7 C9 O8 -3.0(5) 4_455 . . . ? Zn2 O7 C9 C10 10.8(9) 4_455 . . . ? Zn4 O7 C9 C10 171.7(5) 4_455 . . . ? Zn2 O7 C9 Zn4 -160.9(6) 4_455 . . 4_455 ? Zn4 O8 C9 O7 3.7(6) 4_455 . . . ? Zn4 O8 C9 C10 -171.4(4) 4_455 . . . ? O7 C9 C10 C16 67.7(8) . . . . ? O8 C9 C10 C16 -117.5(6) . . . . ? Zn4 C9 C10 C16 -143.2(12) 4_455 . . . ? O7 C9 C10 C11 -112.8(6) . . . . ? O8 C9 C10 C11 62.0(7) . . . . ? Zn4 C9 C10 C11 36.3(16) 4_455 . . . ? C16 C10 C11 C12 0.7(8) . . . . ? C9 C10 C11 C12 -178.7(5) . . . . ? C5 O5 C12 C13 -9.1(8) . . . . ? C5 O5 C12 C11 172.1(5) . . . . ? C10 C11 C12 C13 0.5(8) . . . . ? C10 C11 C12 O5 179.3(5) . . . . ? O5 C12 C13 C14 179.7(5) . . . . ? C11 C12 C13 C14 -1.6(8) . . . . ? C12 C13 C14 C16 1.5(9) . . . . ? Zn1 O6 C15 O9 -1.5(9) 3_445 . . . ? Zn1 O6 C15 C16 178.0(4) 3_445 . . . ? C11 C10 C16 C14 -0.8(8) . . . . ? C9 C10 C16 C14 178.6(5) . . . . ? C11 C10 C16 C15 -177.1(5) . . . . ? C9 C10 C16 C15 2.3(8) . . . . ? C13 C14 C16 C10 -0.3(8) . . . . ? C13 C14 C16 C15 176.1(5) . . . . ? O9 C15 C16 C10 16.1(9) . . . . ? O6 C15 C16 C10 -163.5(5) . . . . ? O9 C15 C16 C14 -160.2(6) . . . . ? O6 C15 C16 C14 20.3(8) . . . . ? Zn1 O10 C17 O11 175.0(4) . . . . ? Zn1 O10 C17 C18 3.9(9) . . . . ? Zn3 O11 C17 O10 -15.2(6) . . . . ? Zn3 O11 C17 C18 156.2(4) . . . . ? O10 C17 C18 C19 103.8(6) . . . . ? O11 C17 C18 C19 -67.6(6) . . . . ? O10 C17 C18 C23 -73.4(7) . . . . ? O11 C17 C18 C23 115.2(6) . . . . ? C23 C18 C19 C20 0.0(8) . . . . ? C17 C18 C19 C20 -177.3(5) . . . . ? C29 O14 C20 C21 -8.2(8) . . . . ? C29 O14 C20 C19 175.2(5) . . . . ? C18 C19 C20 C21 -1.3(8) . . . . ? C18 C19 C20 O14 175.5(5) . . . . ? O14 C20 C21 C22 -175.8(5) . . . . ? C19 C20 C21 C22 0.6(8) . . . . ? C20 C21 C22 C23 1.3(8) . . . . ? C19 C18 C23 C22 1.8(8) . . . . ? C17 C18 C23 C22 178.8(5) . . . . ? C19 C18 C23 C24 178.5(5) . . . . ? C17 C18 C23 C24 -4.5(8) . . . . ? C21 C22 C23 C18 -2.5(8) . . . . ? C21 C22 C23 C24 -179.2(5) . . . . ? Zn2 O13 C24 O12 8.8(9) 2_565 . . . ? Zn2 O13 C24 C23 -171.6(4) 2_565 . . . ? C18 C23 C24 O12 -7.6(8) . . . . ? C22 C23 C24 O12 169.1(6) . . . . ? C18 C23 C24 O13 172.8(5) . . . . ? C22 C23 C24 O13 -10.5(8) . . . . ? Zn1 O17 C25 O18 -27.3(10) 4_455 . . . ? Zn1 O17 C25 C26 155.0(4) 4_455 . . . ? Zn2 O18 C25 O17 -14.4(8) 4_455 . . . ? Zn2 O18 C25 C26 163.4(3) 4_455 . . . ? O17 C25 C26 C27 156.8(5) . . . . ? O18 C25 C26 C27 -21.2(7) . . . . ? O17 C25 C26 C31 -22.3(8) . . . . ? O18 C25 C26 C31 159.7(5) . . . . ? C31 C26 C27 C28 -0.7(8) . . . . ? C25 C26 C27 C28 -179.8(5) . . . . ? C26 C27 C28 C29 1.0(8) . . . . ? C27 C28 C29 C30 -0.3(8) . . . . ? C27 C28 C29 O14 178.1(5) . . . . ? C20 O14 C29 C28 113.5(6) . . . . ? C20 O14 C29 C30 -68.0(7) . . . . ? C28 C29 C30 C31 -0.6(8) . . . . ? O14 C29 C30 C31 -179.0(5) . . . . ? C29 C30 C31 C26 0.8(8) . . . . ? C29 C30 C31 C32 -170.3(5) . . . . ? C27 C26 C31 C30 -0.2(8) . . . . ? C25 C26 C31 C30 178.9(5) . . . . ? C27 C26 C31 C32 170.4(5) . . . . ? C25 C26 C31 C32 -10.5(8) . . . . ? Zn3 O15 C32 O16 5.2(8) 4_455 . . . ? Zn3 O15 C32 C31 178.8(3) 4_455 . . . ? C30 C31 C32 O16 100.6(6) . . . . ? C26 C31 C32 O16 -70.1(7) . . . . ? C30 C31 C32 O15 -73.6(6) . . . . ? C26 C31 C32 O15 115.7(6) . . . . ? C37 N2 C33 C34 -1.1(11) . . . . ? Zn4 N2 C33 C34 -178.1(6) . . . . ? N2 C33 C34 C35 0.1(13) . . . . ? C33 C34 C35 C36 0.0(13) . . . . ? C34 C35 C36 C37 0.8(13) . . . . ? C33 N2 C37 C36 1.8(9) . . . . ? Zn4 N2 C37 C36 179.2(5) . . . . ? C33 N2 C37 C38 -176.7(6) . . . . ? Zn4 N2 C37 C38 0.7(7) . . . . ? C35 C36 C37 N2 -1.7(11) . . . . ? C35 C36 C37 C38 176.7(7) . . . . ? C42 N1 C38 C39 -0.6(10) . . . . ? Zn4 N1 C38 C39 174.6(5) . . . . ? C42 N1 C38 C37 180.0(6) . . . . ? Zn4 N1 C38 C37 -4.8(7) . . . . ? N2 C37 C38 N1 2.7(8) . . . . ? C36 C37 C38 N1 -175.7(6) . . . . ? N2 C37 C38 C39 -176.6(6) . . . . ? C36 C37 C38 C39 5.0(10) . . . . ? N1 C38 C39 C40 -0.2(11) . . . . ? C37 C38 C39 C40 179.1(7) . . . . ? C38 C39 C40 C41 1.3(13) . . . . ? C39 C40 C41 C42 -1.4(14) . . . . ? C38 N1 C42 C41 0.5(11) . . . . ? Zn4 N1 C42 C41 -174.1(6) . . . . ? C40 C41 C42 N1 0.6(14) . . . . ? C47 N3 C43 C44 -0.7(11) . . . . ? Zn3 N3 C43 C44 -178.9(6) . . . . ? N3 C43 C44 C45 0.5(13) . . . . ? C43 C44 C45 C46 -0.6(13) . . . . ? C44 C45 C46 C47 0.8(12) . . . . ? C43 N3 C47 C46 1.0(9) . . . . ? Zn3 N3 C47 C46 179.3(5) . . . . ? C43 N3 C47 C48 -179.1(6) . . . . ? Zn3 N3 C47 C48 -0.8(6) . . . . ? C45 C46 C47 N3 -1.0(10) . . . . ? C45 C46 C47 C48 179.1(6) . . . . ? C52 N4 C48 C49 -1.7(9) . . . . ? Zn3 N4 C48 C49 175.4(5) . . . . ? C52 N4 C48 C47 179.4(6) . . . . ? Zn3 N4 C48 C47 -3.5(7) . . . . ? N3 C47 C48 N4 2.8(8) . . . . ? C46 C47 C48 N4 -177.3(6) . . . . ? N3 C47 C48 C49 -176.1(6) . . . . ? C46 C47 C48 C49 3.9(10) . . . . ? N4 C48 C49 C50 -0.5(10) . . . . ? C47 C48 C49 C50 178.3(6) . . . . ? C48 C49 C50 C51 2.6(11) . . . . ? C49 C50 C51 C52 -2.5(12) . . . . ? C48 N4 C52 C51 1.9(11) . . . . ? Zn3 N4 C52 C51 -174.9(6) . . . . ? C50 C51 C52 N4 0.2(12) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.017 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.083 #====END