# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Fedin, Vladimir' _publ_contact_author_email cluster@che.nsk.su _publ_section_title ; Synthesis, crystal structures, luminescent and thermal properties of two new metal-organic coordination polymers based on zinc(II) carboxylates ; loop_ _publ_author_name V.Fedin S.Sapchenko D.Dybtsev D.Samsonenko # Attachment '- submit.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 769431' #TrackingRef '- submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_structural '(N H2 (C H3)2)2 (Zn3 (C8 H4 O4)4) . (C3 H7 N O) . (H2 O)' _chemical_formula_sum 'C39 H41 N3 O18 Zn3' _chemical_formula_weight 1035.86 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 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.1453(16) _cell_length_b 9.5959(4) _cell_length_c 18.4950(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.467(1) _cell_angle_gamma 90.00 _cell_volume 5882.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9023 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 33.21 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5689 _exptl_absorpt_correction_T_max 0.8834 _exptl_absorpt_process_details 'SADABS (Bruker-AXS, 2004)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius X8Apex CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 25 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 33788 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 35.42 _reflns_number_total 13263 _reflns_number_gt 9279 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2004)' _computing_cell_refinement 'SAINT (Bruker-AXS, 2004)' _computing_data_reduction 'SAINT (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1998)' _computing_molecular_graphics 'SHELXTL (Bruker-AXS, 2004)' _computing_publication_material 'CIFTAB-97 (Sheldrick, 1998)' _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. In order to obtain an appropriate structure model, restraints on atomic displacement parameters and bond distances for disordered carboxyl group, dimethylammonum cation and water molecules were applied during the structure refinement. ; _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^)+(0.1192P)^2^+43.5410P] 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 0 _refine_ls_number_reflns 13263 _refine_ls_number_parameters 349 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.2550 _refine_ls_wR_factor_gt 0.2438 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.079 _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 0.153346(11) 0.71055(4) 0.00432(2) 0.01729(10) Uani 1 1 d . . . Zn2 Zn 0.2500 0.7500 0.0000 0.01428(11) Uani 1 2 d S . . O1 O 0.16089(9) 0.8377(4) 0.08558(15) 0.0297(6) Uani 1 1 d . . . O2 O 0.22866(9) 0.8192(3) 0.09677(14) 0.0254(5) Uani 1 1 d . . . C1 C 0.19440(12) 0.8576(4) 0.11807(19) 0.0235(7) Uani 1 1 d . . . C2 C 0.19242(11) 0.9290(4) 0.1900(2) 0.0243(7) Uani 1 1 d . . . C3 C 0.15608(12) 0.9811(6) 0.2138(2) 0.0348(10) Uani 1 1 d . . . H3 H 0.1325 0.9734 0.1846 0.042 Uiso 1 1 calc R . . C4 C 0.15445(12) 1.0453(6) 0.2817(2) 0.0346(10) Uani 1 1 d . . . H4 H 0.1296 1.0816 0.2985 0.042 Uiso 1 1 calc R . . C5 C 0.18878(11) 1.0564(4) 0.3246(2) 0.0248(7) Uani 1 1 d . . . C6 C 0.22519(12) 1.0020(5) 0.3010(2) 0.0300(8) Uani 1 1 d . . . H6 H 0.2486 1.0076 0.3308 0.036 Uiso 1 1 calc R . . C7 C 0.22699(12) 0.9393(5) 0.2335(2) 0.0302(8) Uani 1 1 d . . . H7 H 0.2519 0.9032 0.2167 0.036 Uiso 1 1 calc R . . C8 C 0.18661(11) 1.1254(4) 0.39731(19) 0.0230(6) Uani 1 1 d . . . O3 O 0.15430(9) 1.1876(4) 0.41167(16) 0.0288(6) Uani 1 1 d . . . O4 O 0.21594(9) 1.1144(3) 0.43925(15) 0.0245(5) Uani 1 1 d . . . O5 O 0.09811(11) 0.6607(5) 0.0230(2) 0.0496(10) Uani 1 1 d . . . O6 O 0.1037(6) 0.5258(18) -0.0721(8) 0.064(3) Uani 0.50 1 d PDU . . O6' O 0.1077(6) 0.492(2) -0.0547(9) 0.074(4) Uani 0.50 1 d PDU . . C9 C 0.08490(16) 0.5672(7) -0.0166(4) 0.0590(17) Uani 1 1 d DU . . C10 C 0.04070(16) 0.5317(7) -0.0080(4) 0.0527(15) Uani 1 1 d . . . C11 C 0.0236(2) 0.4247(9) -0.0461(5) 0.072(2) Uani 1 1 d . . . H11 H 0.0397 0.3737 -0.0792 0.087 Uiso 1 1 calc R . . C12 C 0.0171(2) 0.6115(9) 0.0374(5) 0.068(2) Uani 1 1 d . . . H12 H 0.0283 0.6893 0.0623 0.082 Uiso 1 1 calc R . . O7 O 0.20149(8) 0.5931(3) -0.00612(15) 0.0225(5) Uani 1 1 d . . . O8 O 0.17988(13) 0.4847(4) 0.0922(2) 0.0479(10) Uani 1 1 d . . . C13 C 0.20077(13) 0.4866(4) 0.0385(2) 0.0283(8) Uani 1 1 d . . . C14 C 0.22688(12) 0.3652(4) 0.0176(2) 0.0245(7) Uani 1 1 d . . . C15 C 0.23086(15) 0.2541(5) 0.0670(2) 0.0311(8) Uani 1 1 d . . . H15 H 0.2176 0.2576 0.1123 0.037 Uiso 1 1 calc R . . C16 C 0.24586(13) 0.3600(4) -0.0488(2) 0.0280(7) Uani 1 1 d . . . H16 H 0.2429 0.4350 -0.0820 0.034 Uiso 1 1 calc R . . N1N N 0.1262(3) 0.4483(10) -0.2254(5) 0.094(2) Uani 1 1 d U A 1 C1N C 0.1084(6) 0.390(2) -0.2978(9) 0.077(4) Uani 0.50 1 d PU A 1 H1N1 H 0.1282 0.4006 -0.3364 0.116 Uiso 0.50 1 calc PR A 1 H1N2 H 0.0838 0.4407 -0.3106 0.116 Uiso 0.50 1 calc PR A 1 H1N3 H 0.1020 0.2905 -0.2918 0.116 Uiso 0.50 1 calc PR A 1 C2N C 0.1367(6) 0.5900(18) -0.2346(9) 0.079(4) Uani 0.50 1 d PU A 1 H2N1 H 0.1618 0.5963 -0.2621 0.119 Uiso 0.50 1 calc PR A 1 H2N2 H 0.1405 0.6336 -0.1871 0.119 Uiso 0.50 1 calc PR A 1 H2N3 H 0.1150 0.6381 -0.2610 0.119 Uiso 0.50 1 calc PR A 1 C3N C 0.0918(6) 0.415(2) -0.1875(9) 0.081(4) Uani 0.50 1 d PU A 1 H3N1 H 0.0895 0.3134 -0.1836 0.122 Uiso 0.50 1 calc PR A 1 H3N2 H 0.0681 0.4521 -0.2130 0.122 Uiso 0.50 1 calc PR A 1 H3N3 H 0.0934 0.4557 -0.1390 0.122 Uiso 0.50 1 calc PR A 1 C4N C 0.1638(6) 0.374(2) -0.1968(11) 0.090(4) Uani 0.50 1 d PU A 1 H4N1 H 0.1872 0.4005 -0.2257 0.135 Uiso 0.50 1 calc PR A 1 H4N2 H 0.1598 0.2726 -0.2000 0.135 Uiso 0.50 1 calc PR A 1 H4N3 H 0.1685 0.3999 -0.1462 0.135 Uiso 0.50 1 calc PR A 1 O1D O 0.0727(7) 1.251(2) 0.1473(11) 0.140(8) Uani 0.50 1 d PD B 1 C1D C 0.0993(5) 1.2455(17) 0.0971(9) 0.073(5) Uani 0.50 1 d PD B 1 H1D H 0.1201 1.3135 0.0957 0.087 Uiso 0.50 1 calc PR B 1 N1D N 0.0981(3) 1.1479(12) 0.0481(8) 0.059(3) Uani 0.50 1 d PD B 1 C2D C 0.0705(7) 1.032(2) 0.0491(14) 0.100(7) Uani 0.50 1 d PDU B 1 H2D1 H 0.0746 0.9745 0.0061 0.149 Uiso 0.50 1 calc PR B 1 H2D2 H 0.0427 1.0676 0.0492 0.149 Uiso 0.50 1 calc PR B 1 H2D3 H 0.0752 0.9765 0.0927 0.149 Uiso 0.50 1 calc PR B 1 C3D C 0.1279(6) 1.157(2) -0.0082(11) 0.085(7) Uani 0.50 1 d PD B 1 H3D1 H 0.1241 1.0794 -0.0422 0.128 Uiso 0.50 1 calc PR B 1 H3D2 H 0.1549 1.1515 0.0132 0.128 Uiso 0.50 1 calc PR B 1 H3D3 H 0.1248 1.2454 -0.0340 0.128 Uiso 0.50 1 calc PR B 1 O1W O 0.0895(13) 0.215(5) -0.1455(18) 0.126(13) Uani 0.25 1 d P C 2 O2W O 0.1095(14) 1.162(5) -0.006(3) 0.126(16) Uani 0.25 1 d PU D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01323(16) 0.01990(19) 0.01873(18) -0.00001(13) -0.00018(12) -0.00354(12) Zn2 0.0124(2) 0.0159(2) 0.0145(2) 0.00030(17) -0.00019(16) -0.00079(16) O1 0.0267(13) 0.0416(17) 0.0209(12) -0.0093(12) -0.0018(10) 0.0037(12) O2 0.0252(12) 0.0337(15) 0.0172(11) -0.0053(10) 0.0006(9) 0.0000(10) C1 0.0271(16) 0.0271(17) 0.0164(13) -0.0037(12) 0.0027(12) -0.0041(13) C2 0.0226(15) 0.0312(19) 0.0190(14) -0.0066(13) 0.0011(12) -0.0020(13) C3 0.0208(16) 0.059(3) 0.0249(17) -0.0190(18) -0.0043(13) 0.0033(17) C4 0.0175(15) 0.059(3) 0.0277(18) -0.0196(19) -0.0022(13) 0.0040(16) C5 0.0209(15) 0.0330(19) 0.0204(15) -0.0080(13) -0.0027(12) -0.0002(13) C6 0.0230(16) 0.045(2) 0.0217(16) -0.0117(15) -0.0032(13) 0.0034(15) C7 0.0216(16) 0.049(3) 0.0204(16) -0.0115(16) 0.0001(12) 0.0030(15) C8 0.0244(15) 0.0262(17) 0.0183(14) -0.0056(12) -0.0021(11) 0.0000(12) O3 0.0233(12) 0.0416(17) 0.0214(12) -0.0083(11) -0.0014(10) -0.0009(11) O4 0.0262(12) 0.0258(13) 0.0213(12) -0.0048(10) -0.0050(9) 0.0003(10) O5 0.0265(16) 0.062(3) 0.061(2) 0.005(2) 0.0021(16) -0.0188(17) O6 0.030(5) 0.066(7) 0.097(7) -0.012(5) 0.016(5) -0.008(4) O6' 0.034(5) 0.069(7) 0.119(7) -0.013(6) 0.006(6) -0.002(5) C9 0.025(2) 0.052(3) 0.100(5) -0.006(3) 0.009(3) -0.012(2) C10 0.025(2) 0.059(4) 0.075(4) 0.000(3) 0.005(2) -0.018(2) C11 0.043(3) 0.074(5) 0.101(6) -0.031(5) 0.022(4) -0.018(3) C12 0.037(3) 0.074(5) 0.094(6) -0.027(4) 0.009(3) -0.018(3) O7 0.0199(11) 0.0166(11) 0.0308(13) 0.0012(9) -0.0014(10) -0.0018(8) O8 0.056(2) 0.0315(18) 0.057(2) 0.0089(16) 0.0298(19) 0.0075(16) C13 0.0275(17) 0.0213(17) 0.036(2) 0.0012(14) 0.0040(15) 0.0001(13) C14 0.0269(16) 0.0154(14) 0.0312(18) 0.0025(12) 0.0017(13) -0.0031(12) C15 0.041(2) 0.0242(17) 0.0280(18) 0.0010(15) 0.0093(16) 0.0009(16) C16 0.036(2) 0.0221(17) 0.0257(17) 0.0036(13) 0.0004(14) -0.0015(14) N1N 0.100(5) 0.104(5) 0.078(4) -0.017(4) 0.040(4) -0.006(4) C1N 0.084(8) 0.086(8) 0.062(7) -0.013(7) 0.024(6) -0.011(7) C2N 0.117(9) 0.068(7) 0.055(6) -0.023(6) 0.031(6) -0.017(7) C3N 0.084(8) 0.100(9) 0.059(7) -0.023(7) 0.038(6) -0.020(7) C4N 0.088(8) 0.104(9) 0.078(8) -0.027(8) 0.012(7) 0.011(8) O1D 0.141(17) 0.153(17) 0.126(15) 0.034(13) 0.063(13) 0.000(13) C1D 0.059(9) 0.073(10) 0.086(12) 0.025(9) -0.004(8) 0.006(8) N1D 0.048(6) 0.044(6) 0.085(9) -0.006(6) -0.005(6) -0.003(5) C2D 0.097(8) 0.095(8) 0.107(8) 0.002(5) -0.003(5) -0.001(5) C3D 0.067(11) 0.056(10) 0.13(2) -0.022(10) -0.034(12) 0.003(8) O1W 0.14(3) 0.16(4) 0.08(2) -0.01(2) 0.03(2) 0.00(3) O2W 0.126(17) 0.124(17) 0.128(17) 0.001(5) 0.001(5) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.951(3) . yes Zn1 O3 1.973(3) 6_575 yes Zn1 O5 1.926(3) . yes Zn1 O7 1.964(3) . yes Zn2 O2 2.041(3) . yes Zn2 O2 2.041(3) 7_565 ? Zn2 O4 2.052(3) 4_545 yes Zn2 O4 2.052(3) 6_575 ? Zn2 O7 2.205(3) . yes Zn2 O7 2.205(3) 7_565 ? O1 C1 1.273(5) . ? O2 C1 1.260(5) . ? C1 C2 1.498(5) . ? C2 C3 1.380(6) . ? C2 C7 1.398(5) . ? C3 H3 0.9500 . ? C3 C4 1.400(6) . ? C4 H4 0.9500 . ? C4 C5 1.386(5) . ? C5 C6 1.389(6) . ? C5 C8 1.501(5) . ? C6 H6 0.9500 . ? C6 C7 1.387(5) . ? C7 H7 0.9500 . ? C8 O3 1.256(5) . ? C8 O4 1.243(4) . ? O3 Zn1 1.973(3) 6_576 ? O4 Zn2 2.052(3) 4 ? O5 C9 1.236(8) . ? O6 C9 1.269(9) . ? O6' C9 1.262(9) . ? C9 C10 1.514(7) . ? C10 C11 1.364(10) . ? C10 C12 1.384(10) . ? C11 H11 0.9500 . ? C11 C12 1.405(9) 5_565 ? C12 C11 1.405(9) 5_565 ? C12 H12 0.9500 . ? O7 C13 1.313(5) . ? O8 C13 1.216(6) . ? C13 C14 1.503(6) . ? C14 C15 1.409(6) . ? C14 C16 1.386(6) . ? C15 H15 0.9500 . ? C15 C16 1.383(6) 7 ? C16 C15 1.383(6) 7 ? C16 H16 0.9500 . ? N1N C1N 1.564(19) . ? N1N C2N 1.414(19) . ? N1N C3N 1.381(16) . ? N1N C4N 1.53(2) . ? C1N H1N1 0.9800 . ? C1N H1N2 0.9800 . ? C1N H1N3 0.9800 . ? C2N H2N1 0.9800 . ? C2N H2N2 0.9800 . ? C2N H2N3 0.9800 . ? C3N H3N1 0.9800 . ? C3N H3N2 0.9800 . ? C3N H3N3 0.9800 . ? C4N H4N1 0.9800 . ? C4N H4N2 0.9800 . ? C4N H4N3 0.9800 . ? O1D C1D 1.286(15) . ? C1D H1D 0.9500 . ? C1D N1D 1.304(15) . ? N1D C2D 1.438(16) . ? N1D C3D 1.443(17) . ? C2D H2D1 0.9800 . ? C2D H2D2 0.9800 . ? C2D H2D3 0.9800 . ? C3D H3D1 0.9800 . ? C3D H3D2 0.9800 . ? C3D H3D3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O3 110.87(15) . 6_575 yes O1 Zn1 O7 109.62(12) . . yes O5 Zn1 O1 97.66(17) . . yes O5 Zn1 O3 107.49(16) . 6_575 yes O5 Zn1 O7 130.48(17) . . yes O7 Zn1 O3 100.37(12) . 6_575 yes O2 Zn2 O2 180 . 7_565 yes O2 Zn2 O4 85.37(12) 7_565 6_575 yes O2 Zn2 O4 85.38(12) . 4_545 yes O2 Zn2 O4 94.62(12) 7_565 4_545 ? O2 Zn2 O4 94.63(12) . 6_575 yes O2 Zn2 O7 89.45(11) 7_565 . ? O2 Zn2 O7 89.46(11) . 7_565 yes O2 Zn2 O7 90.54(11) 7_565 7_565 ? O2 Zn2 O7 90.55(11) . . yes O4 Zn2 O4 180 6_575 4_545 yes O4 Zn2 O7 89.58(11) 4_545 . yes O4 Zn2 O7 89.58(11) 6_575 7_565 ? O4 Zn2 O7 90.42(11) 4_545 7_565 ? O4 Zn2 O7 90.42(11) 6_575 . yes O7 Zn2 O7 179.996(1) . 7_565 yes C1 O1 Zn1 124.3(3) . . ? C1 O2 Zn2 133.6(2) . . ? O1 C1 C2 116.3(3) . . ? O2 C1 O1 126.4(3) . . ? O2 C1 C2 117.2(3) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 C7 120.3(3) . . ? C7 C2 C1 120.1(3) . . ? C2 C3 H3 120.5 . . ? C2 C3 C4 119.1(4) . . ? C4 C3 H3 120.5 . . ? C3 C4 H4 119.7 . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 120.2(3) . . ? C4 C5 C8 120.1(3) . . ? C6 C5 C8 119.7(3) . . ? C5 C6 H6 120.3 . . ? C7 C6 C5 119.3(4) . . ? C7 C6 H6 120.3 . . ? C2 C7 H7 119.7 . . ? C6 C7 C2 120.5(4) . . ? C6 C7 H7 119.7 . . ? O3 C8 C5 116.5(3) . . ? O4 C8 C5 118.6(3) . . ? O4 C8 O3 124.9(3) . . ? C8 O3 Zn1 116.0(2) . 6_576 ? C8 O4 Zn2 135.4(3) . 4 ? C9 O5 Zn1 114.0(4) . . ? O5 C9 O6 122.2(11) . . ? O5 C9 O6' 122.3(12) . . ? O5 C9 C10 116.1(5) . . ? O6 C9 C10 119.7(11) . . ? O6' C9 O6 21.5(14) . . ? O6' C9 C10 120.9(12) . . ? C11 C10 C9 120.8(6) . . ? C11 C10 C12 119.7(5) . . ? C12 C10 C9 119.4(6) . . ? C10 C11 H11 119.3 . . ? C10 C11 C12 121.5(7) . 5_565 ? C12 C11 H11 119.3 5_565 . ? C10 C12 C11 118.7(6) . 5_565 ? C10 C12 H12 120.6 . . ? C11 C12 H12 120.6 5_565 . ? Zn1 O7 Zn2 101.28(12) . . ? C13 O7 Zn1 111.4(2) . . ? C13 O7 Zn2 121.1(2) . . ? O7 C13 C14 115.4(4) . . ? O8 C13 O7 122.6(4) . . ? O8 C13 C14 122.0(4) . . ? C15 C14 C13 118.1(4) . . ? C16 C14 C13 121.5(4) . . ? C16 C14 C15 120.4(4) . . ? C14 C15 H15 120.3 . . ? C16 C15 C14 119.4(4) 7 . ? C16 C15 H15 120.3 7 . ? C14 C16 H16 119.9 . . ? C15 C16 C14 120.2(4) 7 . ? C15 C16 H16 119.9 7 . ? C2N N1N C1N 109.6(12) . . ? C2N N1N C4N 106.9(14) . . ? C3N N1N C1N 92.5(11) . . ? C3N N1N C2N 119.3(13) . . ? C3N N1N C4N 113.0(15) . . ? C4N N1N C1N 115.3(12) . . ? N1N C1N H1N1 109.5 . . ? N1N C1N H1N2 109.5 . . ? N1N C1N H1N3 109.5 . . ? H1N1 C1N H1N2 109.5 . . ? H1N1 C1N H1N3 109.5 . . ? H1N2 C1N H1N3 109.5 . . ? N1N C2N H2N1 109.5 . . ? N1N C2N H2N2 109.5 . . ? N1N C2N H2N3 109.5 . . ? H2N1 C2N H2N2 109.5 . . ? H2N1 C2N H2N3 109.5 . . ? H2N2 C2N H2N3 109.5 . . ? N1N C3N H3N1 109.5 . . ? N1N C3N H3N2 109.5 . . ? N1N C3N H3N3 109.5 . . ? H3N1 C3N H3N2 109.5 . . ? H3N1 C3N H3N3 109.5 . . ? H3N2 C3N H3N3 109.5 . . ? N1N C4N H4N1 109.5 . . ? N1N C4N H4N2 109.5 . . ? N1N C4N H4N3 109.5 . . ? H4N1 C4N H4N2 109.5 . . ? H4N1 C4N H4N3 109.5 . . ? H4N2 C4N H4N3 109.5 . . ? O1D C1D H1D 119.4 . . ? O1D C1D N1D 121.1(19) . . ? N1D C1D H1D 119.4 . . ? C1D N1D C2D 124.0(16) . . ? C1D N1D C3D 116.3(13) . . ? C2D N1D C3D 119.6(15) . . ? N1D C2D H2D1 109.5 . . ? N1D C2D H2D2 109.5 . . ? N1D C2D H2D3 109.5 . . ? H2D1 C2D H2D2 109.5 . . ? H2D1 C2D H2D3 109.5 . . ? H2D2 C2D H2D3 109.5 . . ? N1D C3D H3D1 109.5 . . ? N1D C3D H3D2 109.5 . . ? N1D C3D H3D3 109.5 . . ? H3D1 C3D H3D2 109.5 . . ? H3D1 C3D H3D3 109.5 . . ? H3D2 C3D H3D3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.984 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.190 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 769432' #TrackingRef '- submit.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_structural '(C2 H8 N)2 (Zn3 (C14 H8 O4)4) . 5(C3 H7 N O)' _chemical_formula_sum 'C75 H83 N7 O21 Zn3' _chemical_formula_weight 1614.59 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 Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 24.6744(5) _cell_length_b 14.5575(5) _cell_length_c 22.4021(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8046.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9877 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.28 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3360 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7000 _exptl_absorpt_correction_T_max 0.8615 _exptl_absorpt_process_details 'SADABS (Bruker-AXS, 2004)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius X8Apex CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean 25 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 62979 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.34 _reflns_number_total 19099 _reflns_number_gt 16199 _reflns_threshold_expression >2\s(I) _computing_data_collection 'APEX2 (Bruker-AXS, 2004)' _computing_cell_refinement 'SAINT (Bruker-AXS, 2004)' _computing_data_reduction 'SAINT (Bruker-AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1998)' _computing_molecular_graphics 'SHELXTL (Bruker-AXS, 2004)' _computing_publication_material 'CIFTAB-97 (Sheldrick, 1998)' _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. In order to obtain an appropriate structure model, restraints on atomic displacement parameters for DMF of solvation were applied. ; _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^)+(0.0715P)^2^+1.2502P] 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 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.514(8) _refine_ls_number_reflns 19099 _refine_ls_number_parameters 956 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.656167(12) 0.04083(2) 0.613224(13) 0.01652(8) Uani 1 1 d . . . Zn2 Zn 0.655975(10) 0.00357(2) 0.770978(18) 0.01165(6) Uani 1 1 d . . . Zn3 Zn 0.660277(12) -0.03922(2) 0.935175(13) 0.01779(8) Uani 1 1 d . . . O101 O 0.65132(10) 0.03415(18) 0.52673(12) 0.0328(6) Uani 1 1 d . . . O102 O 0.73147(10) 0.10132(17) 0.51110(10) 0.0356(5) Uani 1 1 d . . . C101 C 0.69009(13) 0.0617(2) 0.49399(14) 0.0260(6) Uani 1 1 d . . . C102 C 0.68285(13) 0.0407(2) 0.42810(14) 0.0269(7) Uani 1 1 d . . . C103 C 0.64082(14) -0.0140(3) 0.40892(16) 0.0327(7) Uani 1 1 d . . . H103 H 0.6154 -0.0371 0.4370 0.039 Uiso 1 1 calc R . . C104 C 0.63534(15) -0.0356(3) 0.34942(15) 0.0359(8) Uani 1 1 d . . . H104 H 0.6060 -0.0733 0.3370 0.043 Uiso 1 1 calc R . . C105 C 0.67192(17) -0.0033(3) 0.30694(16) 0.0326(8) Uani 1 1 d . . . C106 C 0.71524(15) 0.0506(3) 0.32674(16) 0.0361(8) Uani 1 1 d . . . H106 H 0.7412 0.0723 0.2988 0.043 Uiso 1 1 calc R . . C107 C 0.72088(14) 0.0732(3) 0.38709(15) 0.0324(7) Uani 1 1 d . . . H107 H 0.7503 0.1102 0.4001 0.039 Uiso 1 1 calc R . . C108 C 0.66523(16) -0.0247(3) 0.24238(17) 0.0339(8) Uani 1 1 d . . . C109 C 0.61371(15) -0.0437(3) 0.21928(16) 0.0356(8) Uani 1 1 d . . . H109 H 0.5835 -0.0456 0.2455 0.043 Uiso 1 1 calc R . . C110 C 0.60607(14) -0.0598(3) 0.15933(15) 0.0338(7) Uani 1 1 d . . . H110 H 0.5710 -0.0748 0.1448 0.041 Uiso 1 1 calc R . . C111 C 0.64918(14) -0.0543(2) 0.12011(17) 0.0322(7) Uani 1 1 d . . . C112 C 0.70067(15) -0.0390(3) 0.14272(17) 0.0395(9) Uani 1 1 d . . . H112 H 0.7309 -0.0377 0.1164 0.047 Uiso 1 1 calc R . . C113 C 0.70850(15) -0.0254(3) 0.20383(15) 0.0390(9) Uani 1 1 d . . . H113 H 0.7441 -0.0166 0.2189 0.047 Uiso 1 1 calc R . . C114 C 0.63907(14) -0.0633(3) 0.05411(15) 0.0307(7) Uani 1 1 d . . . O103 O 0.59489(11) -0.0911(2) 0.03601(11) 0.0465(7) Uani 1 1 d . . . O104 O 0.67835(11) -0.04154(18) 0.02030(10) 0.0340(6) Uani 1 1 d . . . O201 O 0.59150(9) -0.03112(17) 0.62985(11) 0.0286(5) Uani 1 1 d . . . O202 O 0.58202(9) -0.00190(16) 0.72784(11) 0.0301(5) Uani 1 1 d . . . C201 C 0.56765(12) -0.0374(2) 0.67993(14) 0.0250(6) Uani 1 1 d . . . C202 C 0.51619(12) -0.0940(2) 0.67999(14) 0.0276(7) Uani 1 1 d . . . C203 C 0.49105(14) -0.1165(3) 0.62651(15) 0.0354(8) Uani 1 1 d . . . H203 H 0.5063 -0.0965 0.5898 0.042 Uiso 1 1 calc R . . C204 C 0.44416(14) -0.1677(3) 0.62630(16) 0.0387(9) Uani 1 1 d . . . H204 H 0.4268 -0.1815 0.5895 0.046 Uiso 1 1 calc R . . C205 C 0.42181(13) -0.1997(2) 0.67999(15) 0.0337(8) Uani 1 1 d . . . C206 C 0.44787(15) -0.1779(3) 0.73331(15) 0.0364(8) Uani 1 1 d . . . H206 H 0.4338 -0.1999 0.7701 0.044 Uiso 1 1 calc R . . C207 C 0.49419(14) -0.1242(3) 0.73288(15) 0.0342(8) Uani 1 1 d . . . H207 H 0.5110 -0.1081 0.7696 0.041 Uiso 1 1 calc R . . C208 C 0.37198(13) -0.2575(2) 0.67905(15) 0.0309(7) Uani 1 1 d . . . C209 C 0.36275(14) -0.3179(2) 0.63102(15) 0.0316(7) Uani 1 1 d . . . H209 H 0.3882 -0.3216 0.5993 0.038 Uiso 1 1 calc R . . C210 C 0.31667(13) -0.3721(2) 0.62996(14) 0.0275(7) Uani 1 1 d . . . H210 H 0.3110 -0.4131 0.5976 0.033 Uiso 1 1 calc R . . C211 C 0.27870(12) -0.3672(2) 0.67538(14) 0.0254(6) Uani 1 1 d . . . C212 C 0.28737(13) -0.3071(2) 0.72297(15) 0.0323(7) Uani 1 1 d . . . H212 H 0.2616 -0.3035 0.7543 0.039 Uiso 1 1 calc R . . C213 C 0.33384(14) -0.2521(3) 0.72473(17) 0.0349(8) Uani 1 1 d . . . H213 H 0.3394 -0.2111 0.7571 0.042 Uiso 1 1 calc R . . C214 C 0.22839(11) -0.4247(2) 0.67267(13) 0.0209(6) Uani 1 1 d . . . O203 O 0.22595(9) -0.48304(16) 0.63025(10) 0.0247(5) Uani 1 1 d . . . O204 O 0.19221(8) -0.41125(13) 0.71039(9) 0.0226(4) Uani 1 1 d . . . O301 O 0.64380(10) 0.16820(15) 0.63659(11) 0.0319(5) Uani 1 1 d . . . O302 O 0.68059(9) 0.12252(14) 0.72257(10) 0.0293(5) Uani 1 1 d . . . C301 C 0.65856(12) 0.1818(2) 0.69070(16) 0.0245(7) Uani 1 1 d . . . C302 C 0.65152(14) 0.2772(2) 0.71488(16) 0.0280(7) Uani 1 1 d . . . C303 C 0.62846(16) 0.3462(2) 0.67993(17) 0.0370(9) Uani 1 1 d . . . H303 H 0.6162 0.3329 0.6407 0.044 Uiso 1 1 calc R . . C304 C 0.62350(16) 0.4339(2) 0.70266(17) 0.0347(8) Uani 1 1 d . . . H304 H 0.6083 0.4809 0.6785 0.042 Uiso 1 1 calc R . . C305 C 0.64043(14) 0.45476(19) 0.76042(15) 0.0257(7) Uani 1 1 d . . . C306 C 0.66324(17) 0.3849(2) 0.79543(18) 0.0395(9) Uani 1 1 d . . . H306 H 0.6753 0.3976 0.8349 0.047 Uiso 1 1 calc R . . C307 C 0.66806(16) 0.2971(2) 0.77197(17) 0.0358(8) Uani 1 1 d . . . H307 H 0.6831 0.2497 0.7959 0.043 Uiso 1 1 calc R . . C308 C 0.63644(14) 0.5502(2) 0.78454(16) 0.0279(7) Uani 1 1 d . . . C309 C 0.63928(17) 0.6252(2) 0.74741(16) 0.0342(8) Uani 1 1 d . . . H309 H 0.6416 0.6154 0.7056 0.041 Uiso 1 1 calc R . . C310 C 0.63883(15) 0.7148(2) 0.76872(16) 0.0322(7) Uani 1 1 d . . . H310 H 0.6396 0.7654 0.7420 0.039 Uiso 1 1 calc R . . C311 C 0.63722(13) 0.7288(2) 0.83038(14) 0.0242(6) Uani 1 1 d . . . C312 C 0.63428(16) 0.6544(2) 0.86821(16) 0.0319(8) Uani 1 1 d . . . H312 H 0.6332 0.6640 0.9101 0.038 Uiso 1 1 calc R . . C313 C 0.63290(18) 0.5657(2) 0.84598(17) 0.0372(8) Uani 1 1 d . . . H313 H 0.6295 0.5152 0.8726 0.045 Uiso 1 1 calc R . . C314 C 0.63964(12) 0.8242(2) 0.85455(15) 0.0234(6) Uani 1 1 d . . . O303 O 0.62917(10) 0.88950(15) 0.82003(11) 0.0337(5) Uani 1 1 d . . . O304 O 0.65149(9) 0.83349(16) 0.90893(12) 0.0304(5) Uani 1 1 d . . . O401 O 0.73119(9) 0.00993(17) 0.80991(11) 0.0330(5) Uani 1 1 d . . . O402 O 0.72770(9) 0.01906(17) 0.90990(11) 0.0300(5) Uani 1 1 d . . . C401 C 0.74865(12) 0.0349(2) 0.85947(14) 0.0249(6) Uani 1 1 d . . . C402 C 0.79978(12) 0.0902(2) 0.86135(15) 0.0276(7) Uani 1 1 d . . . C403 C 0.81427(13) 0.1441(2) 0.81244(15) 0.0304(7) Uani 1 1 d . . . H403 H 0.7925 0.1441 0.7775 0.036 Uiso 1 1 calc R . . C404 C 0.86088(14) 0.1978(3) 0.81524(16) 0.0347(8) Uani 1 1 d . . . H404 H 0.8705 0.2354 0.7822 0.042 Uiso 1 1 calc R . . C405 C 0.89361(13) 0.1972(2) 0.86585(15) 0.0302(7) Uani 1 1 d . . . C406 C 0.87887(13) 0.1421(3) 0.91361(16) 0.0346(8) Uani 1 1 d . . . H406 H 0.9013 0.1402 0.9480 0.041 Uiso 1 1 calc R . . C407 C 0.83249(12) 0.0904(2) 0.91213(16) 0.0299(7) Uani 1 1 d . . . H407 H 0.8226 0.0545 0.9458 0.036 Uiso 1 1 calc R . . C408 C 0.94379(13) 0.2525(2) 0.86813(15) 0.0288(7) Uani 1 1 d . . . C409 C 0.97539(14) 0.2684(2) 0.81721(16) 0.0343(7) Uani 1 1 d . . . H409 H 0.9639 0.2440 0.7800 0.041 Uiso 1 1 calc R . . C410 C 1.02299(13) 0.3189(2) 0.81977(15) 0.0309(7) Uani 1 1 d . . . H410 H 1.0446 0.3265 0.7851 0.037 Uiso 1 1 calc R . . C411 C 1.03900(12) 0.3589(2) 0.87439(15) 0.0260(6) Uani 1 1 d . . . C412 C 1.00759(13) 0.3451(2) 0.92453(15) 0.0281(7) Uani 1 1 d U . . H412 H 1.0182 0.3719 0.9614 0.034 Uiso 1 1 calc R . . C413 C 0.96083(13) 0.2928(2) 0.92208(15) 0.0295(7) Uani 1 1 d . . . H413 H 0.9399 0.2840 0.9572 0.035 Uiso 1 1 calc R . . C414 C 1.09007(11) 0.41488(19) 0.87653(14) 0.0221(6) Uani 1 1 d . . . O403 O 1.12255(8) 0.40765(14) 0.83425(10) 0.0255(4) Uani 1 1 d . . . O404 O 1.09628(9) 0.46312(15) 0.92298(10) 0.0259(5) Uani 1 1 d . . . N1 N 0.81304(12) 0.1353(2) 0.59180(14) 0.0374(7) Uani 1 1 d . . . H1A H 0.7846 0.1054 0.5736 0.045 Uiso 1 1 calc R . . H1B H 0.8316 0.0927 0.6142 0.045 Uiso 1 1 calc R . . C11 C 0.79097(18) 0.2044(3) 0.6318(2) 0.0555(11) Uani 1 1 d . . . H11A H 0.7676 0.1747 0.6614 0.083 Uiso 1 1 calc R . . H11B H 0.7698 0.2490 0.6088 0.083 Uiso 1 1 calc R . . H11C H 0.8207 0.2361 0.6523 0.083 Uiso 1 1 calc R . . C12 C 0.84934(18) 0.1698(4) 0.5455(2) 0.0579(12) Uani 1 1 d . . . H12A H 0.8622 0.1184 0.5210 0.087 Uiso 1 1 calc R . . H12B H 0.8804 0.2005 0.5641 0.087 Uiso 1 1 calc R . . H12C H 0.8298 0.2137 0.5202 0.087 Uiso 1 1 calc R . . N2 N 0.51243(13) 0.8586(3) 0.96493(16) 0.0497(9) Uani 1 1 d . . . H2A H 0.5451 0.8842 0.9758 0.060 Uiso 1 1 calc R . . H2B H 0.5154 0.7959 0.9691 0.060 Uiso 1 1 calc R . . C21 C 0.50151(18) 0.8804(4) 0.9018(2) 0.0611(13) Uani 1 1 d . . . H21A H 0.5307 0.8558 0.8769 0.092 Uiso 1 1 calc R . . H21B H 0.4995 0.9472 0.8968 0.092 Uiso 1 1 calc R . . H21C H 0.4670 0.8527 0.8898 0.092 Uiso 1 1 calc R . . C22 C 0.4698(2) 0.8924(4) 1.0055(2) 0.0715(15) Uani 1 1 d . . . H22A H 0.4789 0.8754 1.0467 0.107 Uiso 1 1 calc R . . H22B H 0.4350 0.8649 0.9945 0.107 Uiso 1 1 calc R . . H22C H 0.4673 0.9594 1.0024 0.107 Uiso 1 1 calc R . . O1D O 0.64427(15) 0.4359(3) 0.98987(17) 0.0656(9) Uani 1 1 d . . . C11D C 0.6867(2) 0.4096(3) 0.97261(18) 0.0482(10) Uani 1 1 d . . . H11D H 0.7157 0.4526 0.9727 0.058 Uiso 1 1 calc R . . N1D N 0.69776(16) 0.3258(2) 0.95305(17) 0.0540(9) Uani 1 1 d . . . C12D C 0.6564(3) 0.2568(4) 0.9490(3) 0.094(2) Uani 1 1 d . . . H12D H 0.6722 0.1996 0.9338 0.140 Uiso 1 1 calc R . . H12E H 0.6279 0.2776 0.9217 0.140 Uiso 1 1 calc R . . H12F H 0.6408 0.2460 0.9886 0.140 Uiso 1 1 calc R . . C13D C 0.7512(3) 0.3017(4) 0.9297(3) 0.0883(19) Uani 1 1 d . . . H13A H 0.7513 0.2370 0.9176 0.133 Uiso 1 1 calc R . . H13B H 0.7786 0.3115 0.9608 0.133 Uiso 1 1 calc R . . H13C H 0.7595 0.3404 0.8951 0.133 Uiso 1 1 calc R . . O2D O 0.88881(15) 0.0634(3) 0.66870(19) 0.0770(11) Uani 1 1 d . . . C21D C 0.8888(2) 0.0180(4) 0.7146(2) 0.0610(12) Uani 1 1 d . . . H21D H 0.8542 -0.0008 0.7287 0.073 Uiso 1 1 calc R . . N2D N 0.9301(2) -0.0080(3) 0.7466(2) 0.0705(12) Uani 1 1 d . . . C22D C 0.9840(3) 0.0217(7) 0.7303(4) 0.124(3) Uani 1 1 d . . . H22D H 1.0104 -0.0042 0.7584 0.186 Uiso 1 1 calc R . . H22E H 0.9858 0.0889 0.7317 0.186 Uiso 1 1 calc R . . H22F H 0.9924 0.0005 0.6898 0.186 Uiso 1 1 calc R . . C23D C 0.9238(4) -0.0627(4) 0.7992(3) 0.102(2) Uani 1 1 d . . . H23A H 0.9595 -0.0753 0.8166 0.153 Uiso 1 1 calc R . . H23B H 0.9061 -0.1208 0.7889 0.153 Uiso 1 1 calc R . . H23C H 0.9015 -0.0294 0.8283 0.153 Uiso 1 1 calc R . . O3D O 0.6111(3) 0.5668(3) 0.5635(2) 0.1099(14) Uani 1 1 d U . . C31D C 0.6574(4) 0.5866(6) 0.5664(4) 0.1068(13) Uani 1 1 d U . . H31D H 0.6822 0.5379 0.5592 0.128 Uiso 1 1 calc R . . N3D N 0.6791(3) 0.6661(4) 0.5782(2) 0.1077(13) Uani 1 1 d U . . C32D C 0.6484(4) 0.7499(5) 0.5884(4) 0.1153(18) Uani 1 1 d U . . H32A H 0.6735 0.8006 0.5965 0.173 Uiso 1 1 calc R . . H32B H 0.6242 0.7415 0.6226 0.173 Uiso 1 1 calc R . . H32C H 0.6269 0.7642 0.5528 0.173 Uiso 1 1 calc R . . C33D C 0.7401(4) 0.6739(5) 0.5798(3) 0.1176(17) Uani 1 1 d U . . H33A H 0.7503 0.7373 0.5892 0.176 Uiso 1 1 calc R . . H33B H 0.7550 0.6570 0.5407 0.176 Uiso 1 1 calc R . . H33C H 0.7546 0.6326 0.6104 0.176 Uiso 1 1 calc R . . O4D O 0.40846(18) 0.7247(4) 0.8916(2) 0.1052(12) Uani 1 1 d U . . C41D C 0.3573(3) 0.7146(5) 0.9011(3) 0.0870(10) Uani 1 1 d U . . H41D H 0.3330 0.7284 0.8695 0.104 Uiso 1 1 calc R . . N4D N 0.33711(19) 0.6868(4) 0.9509(3) 0.0828(10) Uani 1 1 d U . . C42D C 0.3741(3) 0.6789(5) 1.0019(3) 0.0958(15) Uani 1 1 d U . . H42A H 0.3543 0.6547 1.0364 0.144 Uiso 1 1 calc R . . H42B H 0.3888 0.7396 1.0116 0.144 Uiso 1 1 calc R . . H42C H 0.4038 0.6372 0.9917 0.144 Uiso 1 1 calc R . . C43D C 0.2828(2) 0.6765(5) 0.9643(3) 0.0920(14) Uani 1 1 d U . . H43A H 0.2790 0.6523 1.0049 0.138 Uiso 1 1 calc R . . H43B H 0.2663 0.6336 0.9359 0.138 Uiso 1 1 calc R . . H43C H 0.2647 0.7362 0.9615 0.138 Uiso 1 1 calc R . . O5D O 0.52288(18) 0.6784(4) 0.9913(3) 0.1186(15) Uani 1 1 d U . . C51D C 0.5177(3) 0.6057(6) 0.9627(5) 0.1277(15) Uani 1 1 d U . . H51D H 0.5137 0.6080 0.9206 0.153 Uiso 1 1 calc R . . N5D N 0.5178(2) 0.5236(5) 0.9907(5) 0.1294(15) Uani 1 1 d U . . C52D C 0.5248(4) 0.5110(7) 1.0533(5) 0.142(2) Uani 1 1 d U . . H52A H 0.5232 0.4453 1.0627 0.213 Uiso 1 1 calc R . . H52B H 0.4960 0.5434 1.0748 0.213 Uiso 1 1 calc R . . H52C H 0.5602 0.5356 1.0653 0.213 Uiso 1 1 calc R . . C53D C 0.5163(3) 0.4452(6) 0.9482(5) 0.141(2) Uani 1 1 d U . . H53A H 0.5163 0.3873 0.9706 0.211 Uiso 1 1 calc R . . H53B H 0.5482 0.4476 0.9222 0.211 Uiso 1 1 calc R . . H53C H 0.4833 0.4489 0.9239 0.211 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 0.01616(16) 0.01721(16) 0.01619(17) -0.00219(13) 0.00061(12) -0.00004(11) Zn2 0.01120(11) 0.01092(12) 0.01284(12) -0.00196(9) -0.00001(12) -0.00054(11) Zn3 0.01718(15) 0.01850(17) 0.01768(18) -0.00214(13) -0.00007(12) -0.00046(12) O101 0.0288(13) 0.0510(15) 0.0186(12) -0.0045(10) -0.0003(9) -0.0018(10) O102 0.0391(13) 0.0408(14) 0.0268(12) -0.0015(10) -0.0019(10) -0.0092(11) C101 0.0318(16) 0.0270(15) 0.0191(15) -0.0021(12) -0.0022(12) 0.0031(13) C102 0.0299(16) 0.0317(16) 0.0190(16) -0.0029(12) 0.0016(13) 0.0018(13) C103 0.0276(16) 0.048(2) 0.0227(16) -0.0036(15) 0.0035(13) -0.0085(15) C104 0.0354(19) 0.050(2) 0.0225(17) -0.0022(15) 0.0026(14) -0.0125(16) C105 0.0359(18) 0.043(2) 0.0192(17) -0.0025(14) -0.0008(14) -0.0039(15) C106 0.0364(19) 0.051(2) 0.0206(17) 0.0041(15) 0.0032(14) -0.0107(16) C107 0.0289(16) 0.0426(19) 0.0256(17) -0.0021(14) -0.0004(13) -0.0084(14) C108 0.0385(19) 0.046(2) 0.0174(16) -0.0001(15) -0.0037(14) -0.0017(16) C109 0.0314(18) 0.052(2) 0.0234(17) -0.0036(15) 0.0056(13) 0.0002(15) C110 0.0252(16) 0.049(2) 0.0275(17) -0.0030(15) -0.0027(13) 0.0024(14) C111 0.0346(17) 0.0382(18) 0.0237(17) 0.0007(14) -0.0029(14) 0.0027(14) C112 0.0291(18) 0.065(3) 0.0241(18) -0.0078(16) 0.0036(14) -0.0001(17) C113 0.0301(17) 0.066(2) 0.0209(18) -0.0041(17) -0.0022(13) -0.0051(17) C114 0.0317(16) 0.0383(18) 0.0222(16) -0.0020(13) -0.0042(13) 0.0068(14) O103 0.0429(15) 0.076(2) 0.0202(12) -0.0037(12) -0.0042(10) -0.0105(14) O104 0.0359(14) 0.0476(15) 0.0186(12) -0.0046(10) 0.0006(10) 0.0045(11) O201 0.0240(11) 0.0350(12) 0.0267(13) -0.0029(9) 0.0039(9) -0.0131(9) O202 0.0192(10) 0.0375(13) 0.0335(13) -0.0111(10) -0.0019(9) -0.0044(9) C201 0.0168(13) 0.0274(16) 0.0308(17) -0.0032(12) -0.0032(12) -0.0020(12) C202 0.0213(14) 0.0371(18) 0.0246(16) -0.0019(13) -0.0012(11) -0.0097(13) C203 0.0339(17) 0.050(2) 0.0224(16) -0.0005(15) -0.0032(13) -0.0201(16) C204 0.0334(18) 0.054(2) 0.0288(18) -0.0020(16) -0.0006(14) -0.0225(17) C205 0.0303(16) 0.0361(19) 0.0346(19) 0.0001(14) -0.0019(14) -0.0154(14) C206 0.0387(18) 0.046(2) 0.0245(17) 0.0009(14) 0.0039(14) -0.0192(16) C207 0.0334(17) 0.046(2) 0.0237(16) -0.0014(15) -0.0070(13) -0.0135(15) C208 0.0285(16) 0.0345(18) 0.0296(17) -0.0032(14) 0.0008(13) -0.0165(14) C209 0.0285(16) 0.0413(19) 0.0251(17) -0.0055(14) 0.0088(13) -0.0111(15) C210 0.0259(15) 0.0318(17) 0.0249(16) -0.0060(13) 0.0032(12) -0.0077(13) C211 0.0231(14) 0.0259(15) 0.0270(16) -0.0004(12) 0.0021(12) -0.0062(12) C212 0.0278(16) 0.0379(18) 0.0311(18) -0.0070(14) 0.0096(13) -0.0124(14) C213 0.0306(17) 0.0386(19) 0.0355(19) -0.0108(15) 0.0039(14) -0.0158(15) C214 0.0184(13) 0.0208(13) 0.0236(14) 0.0032(11) -0.0006(11) -0.0023(11) O203 0.0172(10) 0.0281(10) 0.0287(13) -0.0042(9) 0.0022(9) -0.0052(9) O204 0.0193(10) 0.0210(10) 0.0274(11) 0.0018(8) 0.0065(8) -0.0022(8) O301 0.0454(13) 0.0185(11) 0.0318(14) -0.0065(10) 0.0013(11) 0.0044(10) O302 0.0330(12) 0.0192(10) 0.0357(13) 0.0021(9) 0.0094(10) 0.0012(9) C301 0.0276(16) 0.0177(15) 0.0280(16) -0.0032(12) 0.0084(12) -0.0011(12) C302 0.0386(18) 0.0148(14) 0.0307(18) -0.0024(12) 0.0045(13) 0.0038(12) C303 0.056(2) 0.0243(17) 0.031(2) -0.0018(14) -0.0042(17) 0.0102(16) C304 0.050(2) 0.0223(16) 0.0317(19) 0.0005(14) -0.0056(16) 0.0077(15) C305 0.0388(17) 0.0132(13) 0.0250(16) -0.0013(12) 0.0052(14) 0.0010(12) C306 0.064(3) 0.0247(17) 0.0295(19) -0.0062(15) -0.0079(17) 0.0053(16) C307 0.059(2) 0.0208(14) 0.0277(18) 0.0030(14) -0.0035(17) 0.0090(14) C308 0.0341(18) 0.0205(14) 0.0293(17) -0.0046(13) -0.0008(14) -0.0002(13) C309 0.057(2) 0.0239(16) 0.0221(16) -0.0005(13) 0.0051(15) 0.0033(16) C310 0.051(2) 0.0185(13) 0.0276(16) 0.0031(13) 0.0023(17) 0.0025(13) C311 0.0295(16) 0.0186(14) 0.0245(16) -0.0020(12) 0.0030(13) 0.0016(12) C312 0.050(2) 0.0218(16) 0.0237(17) -0.0035(13) 0.0010(15) 0.0043(15) C313 0.066(2) 0.0154(15) 0.0298(19) 0.0032(13) 0.0036(18) 0.0021(16) C314 0.0224(14) 0.0149(13) 0.0330(17) -0.0002(12) 0.0077(12) -0.0010(12) O303 0.0491(15) 0.0193(10) 0.0328(13) 0.0017(9) 0.0106(11) 0.0005(10) O304 0.0413(13) 0.0195(11) 0.0303(13) -0.0053(10) -0.0060(10) 0.0004(9) O401 0.0185(11) 0.0458(14) 0.0349(13) -0.0123(11) -0.0002(9) -0.0038(10) O402 0.0202(11) 0.0388(12) 0.0310(13) 0.0057(11) -0.0037(10) -0.0104(10) C401 0.0169(13) 0.0274(16) 0.0306(17) -0.0012(13) -0.0037(12) -0.0018(12) C402 0.0204(14) 0.0304(16) 0.0321(17) 0.0017(13) -0.0023(12) -0.0080(13) C403 0.0216(15) 0.0423(19) 0.0273(16) 0.0001(14) -0.0033(12) -0.0102(14) C404 0.0305(17) 0.0395(19) 0.0342(19) 0.0099(15) -0.0014(14) -0.0102(15) C405 0.0225(15) 0.0349(18) 0.0331(18) 0.0010(14) -0.0004(13) -0.0093(13) C406 0.0244(16) 0.045(2) 0.0346(18) 0.0056(16) -0.0094(14) -0.0134(14) C407 0.0226(14) 0.0376(18) 0.0294(17) 0.0071(14) -0.0042(12) -0.0108(13) C408 0.0220(15) 0.0322(16) 0.0323(17) 0.0001(14) -0.0009(12) -0.0077(13) C409 0.0330(17) 0.0411(19) 0.0289(17) -0.0069(14) -0.0002(14) -0.0132(15) C410 0.0266(15) 0.0388(18) 0.0272(16) -0.0027(13) 0.0075(13) -0.0097(14) C411 0.0209(14) 0.0242(15) 0.0327(17) 0.0008(12) 0.0016(12) -0.0062(12) C412 0.0281(15) 0.0308(16) 0.0254(16) 0.0009(12) 0.0000(12) -0.0084(13) C413 0.0247(15) 0.0349(17) 0.0290(17) 0.0001(13) 0.0048(12) -0.0083(13) C414 0.0185(13) 0.0195(13) 0.0282(16) 0.0062(11) 0.0019(11) -0.0052(11) O403 0.0242(10) 0.0198(10) 0.0323(12) 0.0033(9) 0.0052(9) -0.0037(8) O404 0.0221(10) 0.0267(11) 0.0289(13) -0.0008(9) 0.0046(9) -0.0072(9) N1 0.0319(15) 0.0433(17) 0.0369(16) 0.0018(14) -0.0047(13) -0.0073(13) C11 0.046(2) 0.071(3) 0.050(3) -0.013(2) 0.0030(19) -0.004(2) C12 0.044(2) 0.087(4) 0.042(2) 0.000(2) 0.0075(18) -0.013(2) N2 0.0299(16) 0.068(2) 0.051(2) -0.0130(18) -0.0040(14) -0.0036(15) C21 0.040(2) 0.092(4) 0.051(3) -0.006(2) -0.012(2) -0.019(2) C22 0.048(3) 0.103(4) 0.063(3) -0.026(3) 0.005(2) 0.016(3) O1D 0.065(2) 0.079(2) 0.053(2) 0.0078(19) -0.0006(17) 0.0121(18) C11D 0.066(3) 0.044(2) 0.034(2) 0.0002(17) -0.0044(19) -0.008(2) N1D 0.064(2) 0.0433(18) 0.055(2) -0.0090(17) -0.0067(18) -0.0149(17) C12D 0.119(5) 0.073(4) 0.090(5) -0.017(4) -0.008(4) -0.050(4) C13D 0.092(4) 0.066(4) 0.106(5) -0.027(3) 0.028(4) 0.001(3) O2D 0.067(2) 0.080(2) 0.084(3) 0.026(2) -0.0243(19) -0.0074(19) C21D 0.062(3) 0.061(3) 0.060(3) -0.003(2) -0.009(2) -0.005(2) N2D 0.076(3) 0.065(3) 0.070(3) 0.001(2) -0.018(2) 0.006(2) C22D 0.050(4) 0.181(8) 0.140(7) 0.038(7) -0.019(4) 0.009(4) C23D 0.162(7) 0.072(4) 0.072(4) 0.000(3) -0.036(4) 0.015(4) O3D 0.158(4) 0.091(2) 0.081(2) 0.006(2) -0.016(3) -0.045(3) C31D 0.172(4) 0.082(2) 0.067(2) -0.0012(18) -0.016(2) -0.045(2) N3D 0.173(4) 0.082(2) 0.068(2) -0.0018(18) -0.016(2) -0.044(2) C32D 0.179(4) 0.094(3) 0.072(3) -0.003(3) -0.011(3) -0.029(3) C33D 0.180(4) 0.087(3) 0.086(3) 0.000(3) -0.021(3) -0.040(3) O4D 0.087(2) 0.113(3) 0.116(3) -0.029(2) 0.036(2) -0.036(2) C41D 0.0749(19) 0.088(2) 0.098(2) -0.0212(19) 0.0236(17) -0.0220(17) N4D 0.0698(19) 0.083(2) 0.095(2) -0.0216(19) 0.0234(16) -0.0226(17) C42D 0.086(3) 0.095(3) 0.107(3) -0.013(3) 0.004(3) -0.022(3) C43D 0.074(3) 0.084(3) 0.119(3) -0.024(3) 0.027(3) -0.024(2) O5D 0.072(2) 0.091(3) 0.193(4) -0.005(3) -0.038(3) 0.005(2) C51D 0.071(2) 0.101(3) 0.211(4) -0.014(3) -0.047(3) 0.001(2) N5D 0.072(2) 0.102(3) 0.214(4) -0.015(3) -0.048(3) 0.000(2) C52D 0.088(3) 0.118(3) 0.221(5) -0.003(4) -0.036(4) -0.001(3) C53D 0.085(3) 0.109(3) 0.229(5) -0.023(4) -0.047(3) 0.002(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 O101 1.944(3) . yes Zn1 O201 1.945(2) . yes Zn1 O203 1.954(2) 4_545 yes Zn1 O301 1.951(2) . yes Zn2 O202 2.067(2) . yes Zn2 O204 2.109(2) 4_545 yes Zn2 O302 2.131(2) . yes Zn2 O303 2.098(2) 1_545 yes Zn2 O401 2.053(2) . yes Zn2 O403 2.088(2) 4_455 yes Zn3 O104 1.959(2) 1_556 yes Zn3 O304 1.956(2) 1_545 yes Zn3 O402 1.951(2) . yes Zn3 O404 1.948(2) 4_455 yes O101 C101 1.271(4) . ? O102 C101 1.234(4) . ? C101 C102 1.518(4) . ? C102 C103 1.377(5) . ? C102 C107 1.396(5) . ? C103 H103 0.9500 . ? C103 C104 1.376(5) . ? C104 H104 0.9500 . ? C104 C105 1.393(5) . ? C105 C106 1.398(5) . ? C105 C108 1.489(5) . ? C106 H106 0.9500 . ? C106 C107 1.398(5) . ? C107 H107 0.9500 . ? C108 C109 1.400(5) . ? C108 C113 1.373(5) . ? C109 H109 0.9500 . ? C109 C110 1.376(5) . ? C110 H110 0.9500 . ? C110 C111 1.382(5) . ? C111 C112 1.386(5) . ? C111 C114 1.505(5) . ? C112 H112 0.9500 . ? C112 C113 1.396(5) . ? C113 H113 0.9500 . ? C114 O103 1.231(4) . ? C114 O104 1.270(4) . ? O104 Zn3 1.959(2) 1_554 ? O201 C201 1.270(4) . ? O202 C201 1.243(4) . ? C201 C202 1.513(4) . ? C202 C203 1.389(4) . ? C202 C207 1.376(5) . ? C203 H203 0.9500 . ? C203 C204 1.376(4) . ? C204 H204 0.9500 . ? C204 C205 1.403(5) . ? C205 C206 1.393(5) . ? C205 C208 1.490(4) . ? C206 H206 0.9500 . ? C206 C207 1.384(5) . ? C207 H207 0.9500 . ? C208 C209 1.409(5) . ? C208 C213 1.392(5) . ? C209 H209 0.9500 . ? C209 C210 1.384(4) . ? C210 H210 0.9500 . ? C210 C211 1.385(4) . ? C211 C212 1.396(4) . ? C211 C214 1.499(4) . ? C212 H212 0.9500 . ? C212 C213 1.399(4) . ? C213 H213 0.9500 . ? C214 O203 1.276(4) . ? C214 O204 1.245(4) . ? O203 Zn1 1.954(2) 4_445 ? O204 Zn2 2.109(2) 4_445 ? O301 C301 1.281(4) . ? O302 C301 1.245(4) . ? C301 C302 1.500(4) . ? C302 C303 1.395(5) . ? C302 C307 1.373(5) . ? C303 H303 0.9500 . ? C303 C304 1.380(5) . ? C304 H304 0.9500 . ? C304 C305 1.393(5) . ? C305 C306 1.402(5) . ? C305 C308 1.494(4) . ? C306 H306 0.9500 . ? C306 C307 1.388(5) . ? C307 H307 0.9500 . ? C308 C309 1.375(5) . ? C308 C313 1.397(5) . ? C309 H309 0.9500 . ? C309 C310 1.389(4) . ? C310 H310 0.9500 . ? C310 C311 1.397(5) . ? C311 C312 1.377(5) . ? C311 C314 1.493(4) . ? C312 H312 0.9500 . ? C312 C313 1.384(5) . ? C313 H313 0.9500 . ? C314 O303 1.252(4) . ? C314 O304 1.260(4) . ? O303 Zn2 2.098(2) 1_565 ? O304 Zn3 1.956(2) 1_565 ? O401 C401 1.245(4) . ? O402 C401 1.263(4) . ? C401 C402 1.497(4) . ? C402 C403 1.394(5) . ? C402 C407 1.395(5) . ? C403 H403 0.9500 . ? C403 C404 1.393(5) . ? C404 H404 0.9500 . ? C404 C405 1.392(5) . ? C405 C406 1.386(5) . ? C405 C408 1.478(4) . ? C406 H406 0.9500 . ? C406 C407 1.370(4) . ? C407 H407 0.9500 . ? C408 C409 1.401(5) . ? C408 C413 1.408(5) . ? C409 H409 0.9500 . ? C409 C410 1.387(4) . ? C410 H410 0.9500 . ? C410 C411 1.411(5) . ? C411 C412 1.379(4) . ? C411 C414 1.502(4) . ? C412 H412 0.9500 . ? C412 C413 1.383(4) . ? C413 H413 0.9500 . ? C414 O403 1.245(4) . ? C414 O404 1.265(4) . ? O403 Zn2 2.088(2) 4 ? O404 Zn3 1.948(2) 4 ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N1 C11 1.453(5) . ? N1 C12 1.460(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N2 C21 1.474(6) . ? N2 C22 1.474(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O1D C11D 1.180(6) . ? C11D H11D 0.9500 . ? C11D N1D 1.325(6) . ? N1D C12D 1.435(6) . ? N1D C13D 1.460(7) . ? C12D H12D 0.9800 . ? C12D H12E 0.9800 . ? C12D H12F 0.9800 . ? C13D H13A 0.9800 . ? C13D H13B 0.9800 . ? C13D H13C 0.9800 . ? O2D C21D 1.222(6) . ? C21D H21D 0.9500 . ? C21D N2D 1.304(6) . ? N2D C22D 1.444(8) . ? N2D C23D 1.431(8) . ? C22D H22D 0.9800 . ? C22D H22E 0.9800 . ? C22D H22F 0.9800 . ? C23D H23A 0.9800 . ? C23D H23B 0.9800 . ? C23D H23C 0.9800 . ? O3D C31D 1.178(9) . ? C31D H31D 0.9500 . ? C31D N3D 1.302(9) . ? N3D C32D 1.454(10) . ? N3D C33D 1.511(11) . ? C32D H32A 0.9800 . ? C32D H32B 0.9800 . ? C32D H32C 0.9800 . ? C33D H33A 0.9800 . ? C33D H33B 0.9800 . ? C33D H33C 0.9800 . ? O4D C41D 1.289(7) . ? C41D H41D 0.9500 . ? C41D N4D 1.287(9) . ? N4D C42D 1.465(9) . ? N4D C43D 1.381(7) . ? C42D H42A 0.9800 . ? C42D H42B 0.9800 . ? C42D H42C 0.9800 . ? C43D H43A 0.9800 . ? C43D H43B 0.9800 . ? C43D H43C 0.9800 . ? O5D C51D 1.243(9) . ? C51D H51D 0.9500 . ? C51D N5D 1.349(11) . ? N5D C52D 1.425(13) . ? N5D C53D 1.486(11) . ? C52D H52A 0.9800 . ? C52D H52B 0.9800 . ? C52D H52C 0.9800 . ? C53D H53A 0.9800 . ? C53D H53B 0.9800 . ? C53D H53C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O101 Zn1 O201 96.52(10) . . yes O101 Zn1 O203 103.14(10) . 4_545 yes O101 Zn1 O301 107.79(11) . . yes O201 Zn1 O203 116.98(11) . 4_545 yes O201 Zn1 O301 109.40(11) . . yes O301 Zn1 O203 119.65(11) . 4_545 yes O202 Zn2 O204 92.80(9) . 4_545 yes O202 Zn2 O302 92.58(10) . . yes O202 Zn2 O303 86.33(10) . 1_545 yes O202 Zn2 O403 89.57(9) . 4_455 yes O204 Zn2 O302 93.99(8) 4_545 . yes O303 Zn2 O204 88.07(8) 1_545 4_545 yes O303 Zn2 O302 177.72(9) 1_545 . yes O401 Zn2 O202 177.24(10) . . yes O401 Zn2 O204 85.35(9) . 4_545 yes O401 Zn2 O302 85.52(10) . . yes O401 Zn2 O303 95.63(10) . 1_545 yes O401 Zn2 O403 92.34(9) . 4_455 yes O403 Zn2 O204 177.19(9) 4_455 4_545 yes O403 Zn2 O302 87.43(8) 4_455 . yes O403 Zn2 O303 90.56(9) 4_455 1_545 yes O304 Zn3 O104 107.55(11) 1_545 1_556 yes O402 Zn3 O104 95.51(11) . 1_556 yes O402 Zn3 O304 114.78(11) . 1_545 yes O404 Zn3 O104 109.32(10) 4_455 1_556 yes O404 Zn3 O304 114.00(10) 4_455 1_545 yes O404 Zn3 O402 113.77(10) 4_455 . yes C101 O101 Zn1 120.9(2) . . ? O101 C101 C102 114.2(3) . . ? O102 C101 O101 126.3(3) . . ? O102 C101 C102 119.6(3) . . ? C103 C102 C101 120.6(3) . . ? C103 C102 C107 119.8(3) . . ? C107 C102 C101 119.5(3) . . ? C102 C103 H103 119.7 . . ? C104 C103 C102 120.5(3) . . ? C104 C103 H103 119.7 . . ? C103 C104 H104 119.3 . . ? C103 C104 C105 121.4(3) . . ? C105 C104 H104 119.3 . . ? C104 C105 C106 117.9(3) . . ? C104 C105 C108 121.4(3) . . ? C106 C105 C108 120.7(3) . . ? C105 C106 H106 119.5 . . ? C107 C106 C105 121.0(3) . . ? C107 C106 H106 119.5 . . ? C102 C107 C106 119.4(3) . . ? C102 C107 H107 120.3 . . ? C106 C107 H107 120.3 . . ? C109 C108 C105 120.1(4) . . ? C113 C108 C105 121.8(4) . . ? C113 C108 C109 118.2(3) . . ? C108 C109 H109 119.4 . . ? C110 C109 C108 121.2(3) . . ? C110 C109 H109 119.4 . . ? C109 C110 H110 119.8 . . ? C109 C110 C111 120.3(3) . . ? C111 C110 H110 119.8 . . ? C110 C111 C112 118.9(3) . . ? C110 C111 C114 119.5(3) . . ? C112 C111 C114 121.7(3) . . ? C111 C112 H112 119.7 . . ? C111 C112 C113 120.5(3) . . ? C113 C112 H112 119.7 . . ? C108 C113 C112 120.7(3) . . ? C108 C113 H113 119.7 . . ? C112 C113 H113 119.7 . . ? O103 C114 C111 119.9(3) . . ? O103 C114 O104 124.1(3) . . ? O104 C114 C111 116.0(3) . . ? C114 O104 Zn3 114.3(2) . 1_554 ? C201 O201 Zn1 126.0(2) . . ? C201 O202 Zn2 132.2(2) . . ? O201 C201 C202 115.4(3) . . ? O202 C201 O201 126.9(3) . . ? O202 C201 C202 117.7(3) . . ? C203 C202 C201 120.2(3) . . ? C207 C202 C201 120.4(3) . . ? C207 C202 C203 119.4(3) . . ? C202 C203 H203 119.8 . . ? C204 C203 C202 120.4(3) . . ? C204 C203 H203 119.8 . . ? C203 C204 H204 119.8 . . ? C203 C204 C205 120.5(3) . . ? C205 C204 H204 119.8 . . ? C204 C205 C208 120.0(3) . . ? C206 C205 C204 118.6(3) . . ? C206 C205 C208 121.4(3) . . ? C205 C206 H206 119.9 . . ? C207 C206 C205 120.2(3) . . ? C207 C206 H206 119.9 . . ? C202 C207 C206 120.8(3) . . ? C202 C207 H207 119.6 . . ? C206 C207 H207 119.6 . . ? C209 C208 C205 119.8(3) . . ? C213 C208 C205 121.1(3) . . ? C213 C208 C209 119.1(3) . . ? C208 C209 H209 119.9 . . ? C210 C209 C208 120.1(3) . . ? C210 C209 H209 119.9 . . ? C209 C210 H210 119.5 . . ? C209 C210 C211 120.9(3) . . ? C211 C210 H210 119.5 . . ? C210 C211 C212 119.3(3) . . ? C210 C211 C214 120.1(3) . . ? C212 C211 C214 120.5(3) . . ? C211 C212 H212 119.8 . . ? C211 C212 C213 120.4(3) . . ? C213 C212 H212 119.8 . . ? C208 C213 C212 120.1(3) . . ? C208 C213 H213 120.0 . . ? C212 C213 H213 120.0 . . ? O203 C214 C211 116.2(3) . . ? O204 C214 C211 118.6(3) . . ? O204 C214 O203 125.2(3) . . ? C214 O203 Zn1 118.26(19) . 4_445 ? C214 O204 Zn2 129.84(19) . 4_445 ? C301 O301 Zn1 110.9(2) . . ? C301 O302 Zn2 136.9(2) . . ? O301 C301 C302 116.9(3) . . ? O302 C301 O301 124.0(3) . . ? O302 C301 C302 119.0(3) . . ? C303 C302 C301 120.7(3) . . ? C307 C302 C301 119.8(3) . . ? C307 C302 C303 119.5(3) . . ? C302 C303 H303 120.2 . . ? C304 C303 C302 119.7(3) . . ? C304 C303 H303 120.2 . . ? C303 C304 H304 119.4 . . ? C303 C304 C305 121.2(3) . . ? C305 C304 H304 119.4 . . ? C304 C305 C306 118.8(3) . . ? C304 C305 C308 121.3(3) . . ? C306 C305 C308 119.9(3) . . ? C305 C306 H306 120.3 . . ? C307 C306 C305 119.4(3) . . ? C307 C306 H306 120.3 . . ? C302 C307 C306 121.4(3) . . ? C302 C307 H307 119.3 . . ? C306 C307 H307 119.3 . . ? C309 C308 C305 121.1(3) . . ? C309 C308 C313 118.1(3) . . ? C313 C308 C305 120.7(3) . . ? C308 C309 H309 118.7 . . ? C308 C309 C310 122.5(3) . . ? C310 C309 H309 118.7 . . ? C309 C310 H310 120.8 . . ? C309 C310 C311 118.5(3) . . ? C311 C310 H310 120.8 . . ? C310 C311 C314 119.5(3) . . ? C312 C311 C310 119.7(3) . . ? C312 C311 C314 120.7(3) . . ? C311 C312 H312 119.6 . . ? C311 C312 C313 120.9(3) . . ? C313 C312 H312 119.6 . . ? C308 C313 H313 119.9 . . ? C312 C313 C308 120.2(3) . . ? C312 C313 H313 119.9 . . ? O303 C314 C311 118.3(3) . . ? O303 C314 O304 124.3(3) . . ? O304 C314 C311 117.4(3) . . ? C314 O303 Zn2 149.2(2) . 1_565 ? C314 O304 Zn3 114.7(2) . 1_565 ? C401 O401 Zn2 134.8(2) . . ? C401 O402 Zn3 133.4(2) . . ? O401 C401 O402 127.0(3) . . ? O401 C401 C402 118.3(3) . . ? O402 C401 C402 114.7(3) . . ? C403 C402 C401 119.8(3) . . ? C403 C402 C407 119.4(3) . . ? C407 C402 C401 120.8(3) . . ? C402 C403 H403 120.2 . . ? C404 C403 C402 119.5(3) . . ? C404 C403 H403 120.2 . . ? C403 C404 H404 119.6 . . ? C405 C404 C403 120.8(3) . . ? C405 C404 H404 119.6 . . ? C404 C405 C408 120.7(3) . . ? C406 C405 C404 118.7(3) . . ? C406 C405 C408 120.6(3) . . ? C405 C406 H406 119.4 . . ? C407 C406 C405 121.2(3) . . ? C407 C406 H406 119.4 . . ? C402 C407 H407 119.9 . . ? C406 C407 C402 120.3(3) . . ? C406 C407 H407 119.9 . . ? C409 C408 C405 121.9(3) . . ? C409 C408 C413 117.6(3) . . ? C413 C408 C405 120.5(3) . . ? C408 C409 H409 119.2 . . ? C410 C409 C408 121.7(3) . . ? C410 C409 H409 119.2 . . ? C409 C410 H410 120.3 . . ? C409 C410 C411 119.4(3) . . ? C411 C410 H410 120.3 . . ? C410 C411 C414 119.1(3) . . ? C412 C411 C410 119.3(3) . . ? C412 C411 C414 121.6(3) . . ? C411 C412 H412 119.5 . . ? C411 C412 C413 121.1(3) . . ? C413 C412 H412 119.5 . . ? C408 C413 H413 119.6 . . ? C412 C413 C408 120.8(3) . . ? C412 C413 H413 119.6 . . ? O403 C414 C411 118.0(3) . . ? O403 C414 O404 126.5(3) . . ? O404 C414 C411 115.4(3) . . ? C414 O403 Zn2 135.91(19) . 4 ? C414 O404 Zn3 121.96(19) . 4 ? H1A N1 H1B 107.5 . . ? C11 N1 H1A 108.4 . . ? C11 N1 H1B 108.4 . . ? C11 N1 C12 115.5(4) . . ? C12 N1 H1A 108.4 . . ? C12 N1 H1B 108.4 . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? H2A N2 H2B 107.8 . . ? C21 N2 H2A 109.0 . . ? C21 N2 H2B 109.0 . . ? C21 N2 C22 112.9(4) . . ? C22 N2 H2A 109.0 . . ? C22 N2 H2B 109.0 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1D C11D H11D 116.9 . . ? O1D C11D N1D 126.2(5) . . ? N1D C11D H11D 116.9 . . ? C11D N1D C12D 121.3(5) . . ? C11D N1D C13D 121.7(4) . . ? C12D N1D C13D 116.8(5) . . ? N1D C12D H12D 109.5 . . ? N1D C12D H12E 109.5 . . ? N1D C12D H12F 109.5 . . ? H12D C12D H12E 109.5 . . ? H12D C12D H12F 109.5 . . ? H12E C12D H12F 109.5 . . ? N1D C13D H13A 109.5 . . ? N1D C13D H13B 109.5 . . ? N1D C13D H13C 109.5 . . ? H13A C13D H13B 109.5 . . ? H13A C13D H13C 109.5 . . ? H13B C13D H13C 109.5 . . ? O2D C21D H21D 115.8 . . ? O2D C21D N2D 128.3(6) . . ? N2D C21D H21D 115.8 . . ? C21D N2D C22D 119.6(5) . . ? C21D N2D C23D 122.0(6) . . ? C23D N2D C22D 118.3(6) . . ? N2D C22D H22D 109.5 . . ? N2D C22D H22E 109.5 . . ? N2D C22D H22F 109.5 . . ? H22D C22D H22E 109.5 . . ? H22D C22D H22F 109.5 . . ? H22E C22D H22F 109.5 . . ? N2D C23D H23A 109.5 . . ? N2D C23D H23B 109.5 . . ? N2D C23D H23C 109.5 . . ? H23A C23D H23B 109.5 . . ? H23A C23D H23C 109.5 . . ? H23B C23D H23C 109.5 . . ? O3D C31D H31D 115.6 . . ? O3D C31D N3D 128.8(10) . . ? N3D C31D H31D 115.6 . . ? C31D N3D C32D 124.3(8) . . ? C31D N3D C33D 118.8(8) . . ? C32D N3D C33D 116.8(6) . . ? N3D C32D H32A 109.5 . . ? N3D C32D H32B 109.5 . . ? N3D C32D H32C 109.5 . . ? H32A C32D H32B 109.5 . . ? H32A C32D H32C 109.5 . . ? H32B C32D H32C 109.5 . . ? N3D C33D H33A 109.5 . . ? N3D C33D H33B 109.5 . . ? N3D C33D H33C 109.5 . . ? H33A C33D H33B 109.5 . . ? H33A C33D H33C 109.5 . . ? H33B C33D H33C 109.5 . . ? O4D C41D H41D 118.0 . . ? N4D C41D O4D 124.0(8) . . ? N4D C41D H41D 118.0 . . ? C41D N4D C42D 117.3(6) . . ? C41D N4D C43D 126.7(7) . . ? C43D N4D C42D 115.3(6) . . ? N4D C42D H42A 109.5 . . ? N4D C42D H42B 109.5 . . ? N4D C42D H42C 109.5 . . ? H42A C42D H42B 109.5 . . ? H42A C42D H42C 109.5 . . ? H42B C42D H42C 109.5 . . ? N4D C43D H43A 109.5 . . ? N4D C43D H43B 109.5 . . ? N4D C43D H43C 109.5 . . ? H43A C43D H43B 109.5 . . ? H43A C43D H43C 109.5 . . ? H43B C43D H43C 109.5 . . ? O5D C51D H51D 119.5 . . ? O5D C51D N5D 120.9(11) . . ? N5D C51D H51D 119.5 . . ? C51D N5D C52D 124.8(9) . . ? C51D N5D C53D 112.5(10) . . ? C52D N5D C53D 122.2(9) . . ? N5D C52D H52A 109.5 . . ? N5D C52D H52B 109.5 . . ? N5D C52D H52C 109.5 . . ? H52A C52D H52B 109.5 . . ? H52A C52D H52C 109.5 . . ? H52B C52D H52C 109.5 . . ? N5D C53D H53A 109.5 . . ? N5D C53D H53B 109.5 . . ? N5D C53D H53C 109.5 . . ? H53A C53D H53B 109.5 . . ? H53A C53D H53C 109.5 . . ? H53B C53D H53C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.381 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.215