# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Zhongming Sun' _publ_contact_author_email 'szm@ciac.jl.cn, zhongming.sun@hotmail.com' loop_ _publ_author_name 'Zhongming Sun' 'Min Guo' data_1 _database_code_depnum_ccdc_archive 'CCDC 874148' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 N2 O9 Zn1.50' _chemical_formula_weight 680.60 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6549(12) _cell_length_b 14.5638(16) _cell_length_c 16.0435(17) _cell_angle_alpha 99.783(2) _cell_angle_beta 102.396(2) _cell_angle_gamma 101.834(2) _cell_volume 2319.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 571(2) _cell_measurement_reflns_used 2184 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 20.62 _exptl_crystal_description shuttle-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 0.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6529 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 571(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12256 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.35 _reflns_number_total 8390 _reflns_number_gt 5492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8390 _refine_ls_number_parameters 404 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1274 _refine_ls_R_factor_gt 0.0931 _refine_ls_wR_factor_ref 0.3245 _refine_ls_wR_factor_gt 0.2923 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.155 _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 0.0000 -0.5000 -0.5000 0.0351(3) Uani 1 2 d S . . Zn2 Zn 0.77570(8) 0.62490(5) 0.52481(5) 0.0424(3) Uani 1 1 d . . . O1 O 0.7386(6) 0.5409(4) -0.3985(4) 0.0646(15) Uani 1 1 d . . . O2 O 0.6376(6) 0.5284(5) 0.4011(4) 0.0866(18) Uani 1 1 d U . . O3 O 0.8492(5) 0.5571(3) 0.4263(3) 0.0497(12) Uani 1 1 d . . . O4 O 0.0810(5) -0.3655(3) -0.4189(3) 0.0552(13) Uani 1 1 d . . . O5 O 0.8840(5) 0.4556(4) -0.4187(4) 0.0591(14) Uani 1 1 d . . . O6 O 0.6819(7) 0.2941(5) 0.0443(4) 0.096(2) Uani 1 1 d . . . O7 O 0.5926(6) 0.2483(5) -0.1713(4) 0.0808(18) Uani 1 1 d . . . O8 O 0.4686(6) 0.0095(4) -0.1714(4) 0.087(2) Uani 1 1 d . . . O14 O -0.0631(5) -0.2746(4) -0.4163(4) 0.0640(14) Uani 1 1 d . . . N1 N 0.6448(6) 0.7062(4) 0.5276(4) 0.0530(15) Uani 1 1 d . . . N2 N 0.5408(7) 0.8185(5) 0.5177(5) 0.071(2) Uani 1 1 d . . . C4 C 0.7935(7) 0.4741(5) -0.3874(5) 0.0490(17) Uani 1 1 d . . . C5 C 0.7445(7) 0.4126(5) -0.3280(5) 0.0504(17) Uani 1 1 d . . . C6 C 0.8178(8) 0.3578(6) -0.2893(6) 0.069(2) Uani 1 1 d . . . H6 H 0.9010 0.3581 -0.2988 0.083 Uiso 1 1 calc R . . C8 C 0.6225(8) 0.4111(6) -0.3126(5) 0.064(2) Uani 1 1 d . . . H8 H 0.5722 0.4497 -0.3370 0.077 Uiso 1 1 calc R . . C9 C 0.7388(9) 0.5199(7) 0.3748(5) 0.071(2) Uani 1 1 d U . . C10 C 0.7220(8) 0.4643(5) 0.2868(5) 0.060(2) Uani 1 1 d . . . C11 C 0.8317(8) 0.4556(6) 0.2563(5) 0.063(2) Uani 1 1 d . . . H11 H 0.9162 0.4876 0.2912 0.075 Uiso 1 1 calc R . . C12 C 0.8165(9) 0.3991(6) 0.1734(5) 0.073(2) Uani 1 1 d . . . H12 H 0.8900 0.3941 0.1522 0.087 Uiso 1 1 calc R . . C13 C 0.6879(10) 0.3500(6) 0.1230(5) 0.073(3) Uani 1 1 d . . . C14 C 0.5751(10) 0.3614(7) 0.1508(6) 0.085(3) Uani 1 1 d . . . H14 H 0.4902 0.3337 0.1146 0.102 Uiso 1 1 calc R . . C15 C 0.5948(9) 0.4160(7) 0.2349(5) 0.071(2) Uani 1 1 d . . . H15 H 0.5217 0.4203 0.2569 0.085 Uiso 1 1 calc R . . C16 C 0.4477(12) 1.0506(7) 0.5563(7) 0.101(4) Uani 1 1 d . . . H16 H 0.4105 1.0842 0.5950 0.122 Uiso 1 1 calc R . . C17 C 0.4711(13) 0.9616(8) 0.5671(8) 0.112(4) Uani 1 1 d . . . H17 H 0.4521 0.9364 0.6138 0.134 Uiso 1 1 calc R . . C18 C 0.5212(10) 0.9135(6) 0.5088(6) 0.075(3) Uani 1 1 d . . . C19 C 0.4564(10) 0.7447(7) 0.5333(6) 0.078(3) Uani 1 1 d . . . H19 H 0.3712 0.7428 0.5395 0.094 Uiso 1 1 calc R . . C20 C 0.6537(9) 0.7906(6) 0.5156(6) 0.071(2) Uani 1 1 d . . . H20 H 0.7287 0.8288 0.5065 0.085 Uiso 1 1 calc R . . C21 C 0.5197(9) 0.6752(6) 0.5381(6) 0.067(2) Uani 1 1 d . . . H21 H 0.4846 0.6149 0.5471 0.080 Uiso 1 1 calc R . . C23 C 0.5738(8) 0.3538(7) -0.2618(6) 0.070(2) Uani 1 1 d . . . H23 H 0.4889 0.3508 -0.2546 0.084 Uiso 1 1 calc R . . C24 C 0.3611(8) -0.0579(5) -0.2236(5) 0.061(2) Uani 1 1 d . . . C25 C 0.2402(10) -0.0448(6) -0.2532(7) 0.084(3) Uani 1 1 d . . . H25 H 0.2235 0.0145 -0.2348 0.100 Uiso 1 1 calc R . . C26 C 0.3827(9) -0.1491(6) -0.2477(6) 0.073(2) Uani 1 1 d . . . H26 H 0.4650 -0.1602 -0.2254 0.088 Uiso 1 1 calc R . . C27 C 0.0526(7) -0.2902(5) -0.3950(4) 0.0463(16) Uani 1 1 d . . . C28 C 0.1614(7) -0.2088(5) -0.3354(5) 0.0503(17) Uani 1 1 d . . . C29 C 0.1406(9) -0.1175(6) -0.3102(6) 0.078(3) Uani 1 1 d . . . H29 H 0.0585 -0.1061 -0.3322 0.093 Uiso 1 1 calc R . . C30 C 0.2831(8) -0.2222(5) -0.3042(5) 0.062(2) Uani 1 1 d . . . H30 H 0.2994 -0.2819 -0.3214 0.074 Uiso 1 1 calc R . . C36 C 0.4514(9) 0.0900(6) -0.1237(5) 0.071(3) Uani 1 1 d . . . H36A H 0.3945 0.0726 -0.0862 0.086 Uiso 1 1 calc R . . H36B H 0.4094 0.1256 -0.1625 0.086 Uiso 1 1 calc R . . C37 C 0.5864(9) 0.1522(6) -0.0683(5) 0.066(2) Uani 1 1 d . . . C39 C 0.6644(9) 0.1933(6) -0.1264(5) 0.061(2) Uani 1 1 d . . . H39A H 0.7504 0.2333 -0.0917 0.074 Uiso 1 1 calc R . . H39B H 0.6783 0.1419 -0.1677 0.074 Uiso 1 1 calc R . . C41 C 0.6480(8) 0.3019(6) -0.2223(5) 0.061(2) Uani 1 1 d . . . C42 C 0.7710(9) 0.3025(6) -0.2366(6) 0.076(3) Uani 1 1 d . . . H42 H 0.8220 0.2653 -0.2105 0.091 Uiso 1 1 calc R . . C46 C 0.5553(10) 0.2317(7) -0.0040(5) 0.079(3) Uani 1 1 d . . . H46A H 0.5009 0.2668 -0.0358 0.095 Uiso 1 1 calc R . . H46B H 0.5088 0.2038 0.0351 0.095 Uiso 1 1 calc R . . C48 C 0.6696(12) 0.0941(7) -0.0145(7) 0.105(4) Uani 1 1 d . . . H48A H 0.6675 0.0347 -0.0521 0.158 Uiso 1 1 calc R . . H48B H 0.6323 0.0806 0.0329 0.158 Uiso 1 1 calc R . . H48C H 0.7598 0.1316 0.0087 0.158 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 0.0376(6) 0.0279(5) 0.0403(6) 0.0065(4) 0.0090(4) 0.0109(4) Zn2 0.0464(5) 0.0321(5) 0.0540(5) 0.0114(3) 0.0134(4) 0.0192(3) O1 0.073(4) 0.062(3) 0.082(4) 0.041(3) 0.033(3) 0.033(3) O2 0.075(4) 0.105(4) 0.068(3) -0.014(3) -0.006(3) 0.048(3) O3 0.058(3) 0.044(3) 0.041(2) 0.006(2) -0.001(2) 0.017(2) O4 0.065(3) 0.035(3) 0.057(3) 0.000(2) -0.001(2) 0.017(2) O5 0.063(3) 0.059(3) 0.081(4) 0.038(3) 0.041(3) 0.029(3) O6 0.107(5) 0.083(4) 0.060(3) -0.021(3) 0.024(3) -0.032(4) O7 0.077(4) 0.098(5) 0.089(4) 0.056(4) 0.037(3) 0.024(4) O8 0.081(4) 0.054(4) 0.092(4) -0.018(3) 0.006(4) -0.009(3) O14 0.056(3) 0.041(3) 0.084(4) -0.004(3) 0.013(3) 0.010(2) N1 0.053(4) 0.042(3) 0.070(4) 0.015(3) 0.015(3) 0.022(3) N2 0.082(5) 0.072(5) 0.096(5) 0.047(4) 0.042(4) 0.059(4) C4 0.050(4) 0.045(4) 0.052(4) 0.018(3) 0.010(3) 0.010(3) C5 0.052(4) 0.048(4) 0.057(4) 0.020(3) 0.018(3) 0.015(3) C6 0.059(5) 0.077(6) 0.101(6) 0.061(5) 0.037(5) 0.030(4) C8 0.049(4) 0.084(6) 0.077(5) 0.039(5) 0.025(4) 0.027(4) C9 0.067(4) 0.086(4) 0.054(4) -0.005(3) -0.007(3) 0.048(4) C10 0.068(5) 0.052(4) 0.053(4) 0.007(4) -0.004(4) 0.023(4) C11 0.060(5) 0.058(5) 0.057(4) 0.009(4) 0.005(4) -0.001(4) C12 0.071(6) 0.078(6) 0.053(5) -0.007(4) 0.013(4) 0.003(5) C13 0.090(7) 0.058(5) 0.055(5) -0.003(4) 0.018(5) -0.004(5) C14 0.073(6) 0.086(7) 0.069(6) -0.018(5) 0.000(5) 0.010(5) C15 0.062(5) 0.082(6) 0.056(5) -0.004(4) -0.003(4) 0.027(5) C16 0.165(11) 0.087(7) 0.117(8) 0.059(7) 0.083(8) 0.096(8) C17 0.165(12) 0.109(9) 0.129(9) 0.069(8) 0.083(9) 0.099(9) C18 0.103(7) 0.069(6) 0.095(6) 0.042(5) 0.049(5) 0.068(5) C19 0.068(6) 0.086(7) 0.098(7) 0.031(6) 0.029(5) 0.043(5) C20 0.079(6) 0.059(5) 0.110(7) 0.042(5) 0.051(5) 0.049(5) C21 0.070(5) 0.047(5) 0.093(6) 0.018(4) 0.022(5) 0.031(4) C23 0.055(5) 0.097(7) 0.077(6) 0.042(5) 0.031(4) 0.026(5) C24 0.063(5) 0.046(4) 0.057(4) 0.002(4) 0.006(4) -0.004(4) C25 0.084(7) 0.038(4) 0.108(7) -0.017(5) 0.012(6) 0.010(4) C26 0.062(5) 0.058(5) 0.088(6) 0.010(5) 0.000(5) 0.013(4) C27 0.052(4) 0.034(4) 0.048(4) 0.007(3) 0.011(3) 0.007(3) C28 0.055(4) 0.035(4) 0.053(4) 0.004(3) 0.008(3) 0.006(3) C29 0.067(6) 0.048(5) 0.103(7) -0.009(5) 0.006(5) 0.020(4) C30 0.063(5) 0.037(4) 0.073(5) 0.002(4) 0.003(4) 0.011(4) C36 0.092(7) 0.047(5) 0.063(5) 0.011(4) 0.021(5) -0.008(4) C37 0.085(6) 0.047(4) 0.048(4) 0.011(3) 0.005(4) -0.012(4) C39 0.077(6) 0.049(4) 0.052(4) 0.013(3) 0.007(4) 0.013(4) C41 0.060(5) 0.064(5) 0.063(5) 0.030(4) 0.020(4) 0.012(4) C42 0.075(6) 0.075(6) 0.100(7) 0.050(5) 0.028(5) 0.038(5) C46 0.085(6) 0.073(6) 0.057(5) -0.003(4) 0.018(5) -0.017(5) C48 0.130(10) 0.076(7) 0.089(7) 0.045(6) -0.005(7) -0.003(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 2.057(4) . ? Zn1 O4 2.057(4) 2_544 ? Zn1 O5 2.074(5) 2_654 ? Zn1 O5 2.074(5) 1_445 ? Zn1 O3 2.177(4) 2_655 ? Zn1 O3 2.177(4) 1_444 ? Zn2 O1 1.921(5) 1_556 ? Zn2 O14 1.946(5) 1_666 ? Zn2 N1 2.008(6) . ? Zn2 O3 2.098(5) . ? Zn2 O2 2.242(6) . ? Zn2 C9 2.526(8) . ? O1 C4 1.251(9) . ? O1 Zn2 1.921(5) 1_554 ? O2 C9 1.261(11) . ? O3 C9 1.237(9) . ? O3 Zn1 2.177(4) 1_666 ? O4 C27 1.219(8) . ? O5 C4 1.233(9) . ? O5 Zn1 2.074(5) 1_665 ? O6 C13 1.363(10) . ? O6 C46 1.433(9) . ? O7 C41 1.363(9) . ? O7 C39 1.399(9) . ? O8 C24 1.351(9) . ? O8 C36 1.356(10) . ? O14 C27 1.285(9) . ? O14 Zn2 1.946(5) 1_444 ? N1 C20 1.264(9) . ? N1 C21 1.372(11) . ? N2 C19 1.349(12) . ? N2 C20 1.352(10) . ? N2 C18 1.466(9) . ? C4 C5 1.516(9) . ? C5 C6 1.360(10) . ? C5 C8 1.371(10) . ? C6 C42 1.363(11) . ? C8 C23 1.366(11) . ? C9 C10 1.457(11) . ? C10 C11 1.381(12) . ? C10 C15 1.397(11) . ? C11 C12 1.397(11) . ? C12 C13 1.403(12) . ? C13 C14 1.400(14) . ? C14 C15 1.392(12) . ? C16 C18 1.318(12) 2_676 ? C16 C17 1.400(12) . ? C17 C18 1.340(14) . ? C18 C16 1.318(12) 2_676 ? C19 C21 1.330(12) . ? C23 C41 1.338(11) . ? C24 C25 1.339(12) . ? C24 C26 1.398(12) . ? C25 C29 1.370(11) . ? C26 C30 1.370(10) . ? C27 C28 1.496(9) . ? C28 C30 1.352(11) . ? C28 C29 1.398(10) . ? C36 C37 1.523(11) . ? C37 C39 1.496(11) . ? C37 C46 1.554(13) . ? C37 C48 1.573(13) . ? C41 C42 1.377(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O4 180.00(17) . 2_544 ? O4 Zn1 O5 87.2(2) . 2_654 ? O4 Zn1 O5 92.8(2) 2_544 2_654 ? O4 Zn1 O5 92.8(2) . 1_445 ? O4 Zn1 O5 87.2(2) 2_544 1_445 ? O5 Zn1 O5 180.000(1) 2_654 1_445 ? O4 Zn1 O3 91.03(18) . 2_655 ? O4 Zn1 O3 88.97(18) 2_544 2_655 ? O5 Zn1 O3 93.48(19) 2_654 2_655 ? O5 Zn1 O3 86.52(19) 1_445 2_655 ? O4 Zn1 O3 88.97(18) . 1_444 ? O4 Zn1 O3 91.03(18) 2_544 1_444 ? O5 Zn1 O3 86.52(19) 2_654 1_444 ? O5 Zn1 O3 93.48(19) 1_445 1_444 ? O3 Zn1 O3 180.000(1) 2_655 1_444 ? O1 Zn2 O14 109.4(3) 1_556 1_666 ? O1 Zn2 N1 104.4(3) 1_556 . ? O14 Zn2 N1 98.1(2) 1_666 . ? O1 Zn2 O3 110.2(2) 1_556 . ? O14 Zn2 O3 97.1(2) 1_666 . ? N1 Zn2 O3 134.6(2) . . ? O1 Zn2 O2 97.0(3) 1_556 . ? O14 Zn2 O2 149.8(3) 1_666 . ? N1 Zn2 O2 88.9(2) . . ? O3 Zn2 O2 59.0(2) . . ? O1 Zn2 C9 107.2(3) 1_556 . ? O14 Zn2 C9 123.6(3) 1_666 . ? N1 Zn2 C9 112.4(3) . . ? O3 Zn2 C9 29.2(2) . . ? O2 Zn2 C9 29.9(3) . . ? C4 O1 Zn2 124.0(5) . 1_554 ? C9 O2 Zn2 87.6(5) . . ? C9 O3 Zn2 94.9(5) . . ? C9 O3 Zn1 133.8(5) . 1_666 ? Zn2 O3 Zn1 102.55(18) . 1_666 ? C27 O4 Zn1 141.3(5) . . ? C4 O5 Zn1 141.8(5) . 1_665 ? C13 O6 C46 117.1(8) . . ? C41 O7 C39 119.9(7) . . ? C24 O8 C36 119.2(8) . . ? C27 O14 Zn2 123.9(5) . 1_444 ? C20 N1 C21 105.9(7) . . ? C20 N1 Zn2 129.5(6) . . ? C21 N1 Zn2 124.5(5) . . ? C19 N2 C20 106.6(7) . . ? C19 N2 C18 128.4(8) . . ? C20 N2 C18 124.9(8) . . ? O5 C4 O1 126.3(7) . . ? O5 C4 C5 118.0(6) . . ? O1 C4 C5 115.7(7) . . ? C6 C5 C8 118.4(7) . . ? C6 C5 C4 122.0(7) . . ? C8 C5 C4 119.6(7) . . ? C5 C6 C42 120.8(8) . . ? C23 C8 C5 120.9(8) . . ? O3 C9 O2 118.1(7) . . ? O3 C9 C10 122.5(8) . . ? O2 C9 C10 119.4(8) . . ? O3 C9 Zn2 55.8(4) . . ? O2 C9 Zn2 62.5(4) . . ? C10 C9 Zn2 176.6(8) . . ? C11 C10 C15 119.9(7) . . ? C11 C10 C9 120.2(7) . . ? C15 C10 C9 119.8(9) . . ? C10 C11 C12 120.5(8) . . ? C11 C12 C13 118.5(9) . . ? O6 C13 C14 123.1(8) . . ? O6 C13 C12 114.9(9) . . ? C14 C13 C12 121.9(8) . . ? C15 C14 C13 117.5(9) . . ? C14 C15 C10 121.4(9) . . ? C18 C16 C17 119.7(10) 2_676 . ? C18 C17 C16 118.8(10) . . ? C16 C18 C17 121.5(8) 2_676 . ? C16 C18 N2 119.5(8) 2_676 . ? C17 C18 N2 119.0(8) . . ? C21 C19 N2 106.1(8) . . ? N1 C20 N2 111.7(8) . . ? C19 C21 N1 109.6(8) . . ? C41 C23 C8 120.2(8) . . ? C25 C24 O8 126.3(8) . . ? C25 C24 C26 118.9(7) . . ? O8 C24 C26 114.8(8) . . ? C24 C25 C29 121.0(8) . . ? C30 C26 C24 120.2(8) . . ? O4 C27 O14 125.6(6) . . ? O4 C27 C28 117.5(7) . . ? O14 C27 C28 116.9(6) . . ? C30 C28 C29 118.3(7) . . ? C30 C28 C27 120.3(7) . . ? C29 C28 C27 121.4(7) . . ? C25 C29 C28 120.5(8) . . ? C28 C30 C26 121.1(8) . . ? O8 C36 C37 108.9(8) . . ? C39 C37 C36 109.5(6) . . ? C39 C37 C46 112.0(7) . . ? C36 C37 C46 105.2(8) . . ? C39 C37 C48 108.3(8) . . ? C36 C37 C48 112.6(7) . . ? C46 C37 C48 109.2(7) . . ? O7 C39 C37 108.1(7) . . ? C23 C41 O7 116.3(8) . . ? C23 C41 C42 119.7(7) . . ? O7 C41 C42 124.0(8) . . ? C6 C42 C41 119.8(8) . . ? O6 C46 C37 105.4(8) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.447 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.209 # Attachment '- 2.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 874149' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 N2 O9 Zn1.50' _chemical_formula_weight 680.60 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9810(5) _cell_length_b 12.2471(7) _cell_length_c 15.8888(9) _cell_angle_alpha 76.8270(10) _cell_angle_beta 75.9530(10) _cell_angle_gamma 79.3840(10) _cell_volume 1635.31(16) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 3142 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 25.93 _exptl_crystal_description shuttle-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 1.163 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6734 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9139 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 26.09 _reflns_number_total 6389 _reflns_number_gt 5172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1337P)^2^+3.0307P] 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 6389 _refine_ls_number_parameters 403 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.2114 _refine_ls_wR_factor_gt 0.1955 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.5000 0.5000 0.0235(2) Uani 1 2 d S . . N1 N -0.7228(5) 0.8943(4) 0.5523(3) 0.0414(11) Uani 1 1 d . . . O1 O 0.5012(5) 0.9951(3) -0.1882(3) 0.0437(10) Uani 1 1 d . . . C1 C 0.3558(7) 0.8719(4) -0.0700(3) 0.0359(12) Uani 1 1 d . . . Zn2 Zn -0.34011(6) 0.64668(4) 0.55962(3) 0.02239(19) Uani 1 1 d . . . N2 N -0.5218(5) 0.7681(4) 0.5741(3) 0.0367(10) Uani 1 1 d . . . O2 O 0.1669(5) 0.8464(3) -0.1457(3) 0.0424(9) Uani 1 1 d . . . C2 C 0.3662(7) 0.9936(5) -0.1190(4) 0.0388(12) Uani 1 1 d . . . H2A H 0.2727 1.0242 -0.1440 0.047 Uiso 1 1 calc R . . H2B H 0.3721 1.0414 -0.0777 0.047 Uiso 1 1 calc R . . C13 C 0.0991(8) 0.7621(5) 0.1378(3) 0.0428(13) Uani 1 1 d . . . C7 C -0.0421(7) 0.8296(5) -0.2017(4) 0.0417(13) Uani 1 1 d . . . H7A H -0.1002 0.8876 -0.1717 0.050 Uiso 1 1 calc R . . O7 O -0.2328(4) 0.6917(3) -0.3613(2) 0.0345(8) Uani 1 1 d . . . O4 O 0.6000(5) 1.5008(3) -0.3778(3) 0.0501(11) Uani 1 1 d . . . C4 C 0.2280(8) 0.8811(5) 0.0116(3) 0.0407(13) Uani 1 1 d . . . H4A H 0.2598 0.9209 0.0507 0.049 Uiso 1 1 calc R . . H4B H 0.1325 0.9251 -0.0060 0.049 Uiso 1 1 calc R . . C15 C -0.0153(8) 0.6390(5) 0.2671(4) 0.0486(15) Uani 1 1 d . . . H15A H -0.0291 0.5645 0.2988 0.058 Uiso 1 1 calc R . . O6 O -0.0041(4) 0.5894(3) -0.4042(2) 0.0317(8) Uani 1 1 d . . . C6 C 0.1107(6) 0.7915(4) -0.1945(3) 0.0339(11) Uani 1 1 d . . . C9 C -0.0251(6) 0.6980(4) -0.2965(3) 0.0275(10) Uani 1 1 d . . . O9 O -0.1827(4) 0.6230(3) 0.4490(2) 0.0351(8) Uani 1 1 d . . . C8 C -0.1100(6) 0.7838(5) -0.2522(4) 0.0358(12) Uani 1 1 d . . . H8A H -0.2144 0.8104 -0.2571 0.043 Uiso 1 1 calc R . . O8 O -0.2843(6) 0.7972(4) 0.4180(3) 0.0586(12) Uani 1 1 d U . . C22 C 0.4953(7) 1.3013(5) -0.2713(4) 0.0503(16) Uani 1 1 d . . . H22 H 0.4289 1.3706 -0.2667 0.060 Uiso 1 1 calc R . . C21 C 0.4453(7) 1.2008(5) -0.2227(4) 0.0473(14) Uani 1 1 d . . . H21A H 0.3468 1.2013 -0.1835 0.057 Uiso 1 1 calc R . . C20 C 0.5399(7) 1.0997(4) -0.2318(3) 0.0365(12) Uani 1 1 d . . . C19 C -0.1929(6) 0.7154(5) 0.3945(4) 0.0353(11) Uani 1 1 d U . . O3 O 0.1991(6) 0.7701(3) 0.0572(3) 0.0510(11) Uani 1 1 d . . . C3 C 0.5097(7) 0.8145(5) -0.0430(4) 0.0465(14) Uani 1 1 d . . . H3A H 0.4992 0.7365 -0.0120 0.070 Uiso 1 1 calc R . . H3B H 0.5349 0.8564 -0.0038 0.070 Uiso 1 1 calc R . . H3C H 0.5927 0.8141 -0.0960 0.070 Uiso 1 1 calc R . . O5 O 0.8312(4) 1.4045(3) -0.4237(2) 0.0341(8) Uani 1 1 d . . . C5 C 0.3178(6) 0.8016(4) -0.1274(3) 0.0337(11) Uani 1 1 d . . . H5A H 0.3963 0.8043 -0.1833 0.040 Uiso 1 1 calc R . . H5B H 0.3189 0.7217 -0.0962 0.040 Uiso 1 1 calc R . . C26 C 0.6956(6) 1.4103(4) -0.3794(3) 0.0319(11) Uani 1 1 d . . . C11 C 0.1943(6) 0.7049(4) -0.2354(4) 0.0348(11) Uani 1 1 d . . . H11A H 0.2971 0.6763 -0.2281 0.042 Uiso 1 1 calc R . . C25 C 0.6844(7) 1.0995(4) -0.2878(4) 0.0378(12) Uani 1 1 d . . . H25A H 0.7484 1.0299 -0.2952 0.045 Uiso 1 1 calc R . . C24 C 0.7348(6) 1.2004(4) -0.3327(3) 0.0346(11) Uani 1 1 d . . . H24A H 0.8362 1.2003 -0.3687 0.041 Uiso 1 1 calc R . . C23 C 0.6398(6) 1.3026(4) -0.3264(3) 0.0332(11) Uani 1 1 d . . . C28 C -0.6415(7) 0.9378(4) 0.5968(4) 0.0438(14) Uani 1 1 d . . . H28A H -0.6670 1.0090 0.6147 0.053 Uiso 1 1 calc R . . C32 C -0.9651(6) 0.8832(5) 0.5144(4) 0.0434(14) Uani 1 1 d . . . H32 H -0.9411 0.8031 0.5241 0.052 Uiso 1 1 calc R . . C30 C -0.8645(6) 0.9472(5) 0.5247(3) 0.0392(13) Uani 1 1 d . . . C29 C -0.6455(6) 0.7907(5) 0.5398(3) 0.0403(13) Uani 1 1 d . . . H29A H -0.6766 0.7420 0.5106 0.048 Uiso 1 1 calc R . . C12 C -0.0921(5) 0.6553(4) -0.3579(3) 0.0269(10) Uani 1 1 d . . . C18 C 0.0222(7) 0.8553(5) 0.1743(4) 0.0438(13) Uani 1 1 d . . . H18A H 0.0349 0.9298 0.1423 0.053 Uiso 1 1 calc R . . C17 C -0.0719(7) 0.8389(5) 0.2565(4) 0.0427(13) Uani 1 1 d . . . H17A H -0.1253 0.9023 0.2816 0.051 Uiso 1 1 calc R . . C16 C -0.0901(7) 0.7298(5) 0.3039(3) 0.0397(13) Uani 1 1 d . . . C27 C -0.5180(6) 0.8594(4) 0.6101(4) 0.0405(13) Uani 1 1 d . . . H27A H -0.4410 0.8662 0.6396 0.049 Uiso 1 1 calc R . . C10 C 0.1273(6) 0.6599(4) -0.2874(3) 0.0293(10) Uani 1 1 d . . . H10A H 0.1862 0.6020 -0.3173 0.035 Uiso 1 1 calc R . . C31 C -0.8973(7) 1.0649(5) 0.5104(4) 0.0439(14) Uani 1 1 d . . . H31 H -0.8262 1.1090 0.5176 0.053 Uiso 1 1 calc R . . C14 C 0.0805(9) 0.6546(5) 0.1839(4) 0.0545(17) Uani 1 1 d . . . H14A H 0.1333 0.5910 0.1589 0.065 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 0.0239(4) 0.0180(4) 0.0214(4) -0.0001(3) 0.0020(3) 0.0019(3) N1 0.034(2) 0.035(2) 0.041(3) 0.004(2) -0.005(2) 0.0139(19) O1 0.053(2) 0.032(2) 0.043(2) 0.0044(16) -0.0016(18) -0.0220(18) C1 0.049(3) 0.035(3) 0.028(3) 0.003(2) -0.011(2) -0.022(2) Zn2 0.0186(3) 0.0193(3) 0.0267(3) -0.0041(2) -0.0025(2) 0.0002(2) N2 0.036(2) 0.029(2) 0.038(2) -0.0017(18) -0.0085(19) 0.0108(18) O2 0.046(2) 0.040(2) 0.052(2) -0.0153(18) -0.0189(18) -0.0115(17) C2 0.051(3) 0.035(3) 0.034(3) 0.000(2) -0.008(2) -0.023(2) C13 0.062(4) 0.037(3) 0.025(3) 0.000(2) -0.002(2) -0.010(3) C7 0.042(3) 0.041(3) 0.048(3) -0.023(3) -0.013(3) 0.001(2) O7 0.0272(18) 0.038(2) 0.043(2) -0.0147(16) -0.0113(15) -0.0007(15) O4 0.040(2) 0.0259(19) 0.068(3) -0.0022(18) 0.014(2) -0.0064(17) C4 0.067(4) 0.032(3) 0.027(3) -0.001(2) -0.007(2) -0.026(3) C15 0.071(4) 0.033(3) 0.038(3) 0.001(2) -0.006(3) -0.014(3) O6 0.0299(18) 0.0350(19) 0.0295(18) -0.0088(15) -0.0062(14) 0.0010(15) C6 0.040(3) 0.033(3) 0.034(3) -0.008(2) -0.013(2) -0.009(2) C9 0.029(2) 0.026(2) 0.028(2) -0.0024(19) -0.0076(19) -0.0041(19) O9 0.0271(18) 0.036(2) 0.0272(17) 0.0074(15) 0.0035(14) 0.0051(14) C8 0.031(3) 0.036(3) 0.045(3) -0.015(2) -0.015(2) 0.001(2) O8 0.060(3) 0.041(2) 0.057(3) -0.005(2) 0.007(2) 0.006(2) C22 0.047(3) 0.031(3) 0.062(4) -0.004(3) 0.011(3) -0.014(3) C21 0.044(3) 0.039(3) 0.051(3) -0.003(3) 0.009(3) -0.018(3) C20 0.049(3) 0.028(3) 0.034(3) 0.003(2) -0.009(2) -0.018(2) C19 0.036(3) 0.035(3) 0.038(3) -0.009(2) -0.011(2) -0.004(2) O3 0.080(3) 0.034(2) 0.029(2) -0.0011(16) 0.0086(19) -0.016(2) C3 0.058(4) 0.046(3) 0.043(3) 0.003(3) -0.025(3) -0.022(3) O5 0.0314(19) 0.0267(18) 0.0337(19) 0.0043(14) 0.0042(15) -0.0049(14) C5 0.039(3) 0.031(3) 0.034(3) -0.001(2) -0.012(2) -0.015(2) C26 0.038(3) 0.021(2) 0.033(3) -0.0039(19) 0.003(2) -0.008(2) C11 0.032(3) 0.034(3) 0.043(3) -0.006(2) -0.014(2) -0.008(2) C25 0.045(3) 0.023(2) 0.041(3) 0.002(2) -0.006(2) -0.006(2) C24 0.037(3) 0.029(3) 0.033(3) 0.000(2) -0.003(2) -0.007(2) C23 0.039(3) 0.022(2) 0.035(3) -0.001(2) 0.001(2) -0.011(2) C28 0.039(3) 0.022(3) 0.057(4) 0.000(2) -0.002(3) 0.007(2) C32 0.036(3) 0.037(3) 0.037(3) 0.011(2) 0.001(2) 0.012(2) C30 0.029(3) 0.037(3) 0.032(3) 0.010(2) 0.001(2) 0.015(2) C29 0.040(3) 0.039(3) 0.033(3) -0.005(2) -0.012(2) 0.019(2) C12 0.027(2) 0.022(2) 0.029(2) 0.0027(18) -0.0064(19) -0.0048(18) C18 0.061(4) 0.036(3) 0.035(3) -0.004(2) -0.007(3) -0.015(3) C17 0.054(4) 0.034(3) 0.040(3) -0.007(2) -0.008(3) -0.008(3) C16 0.048(3) 0.042(3) 0.026(3) -0.005(2) -0.014(2) 0.007(2) C27 0.035(3) 0.028(3) 0.050(3) -0.001(2) -0.003(2) 0.000(2) C10 0.029(2) 0.028(2) 0.031(2) -0.0063(19) -0.007(2) -0.0048(19) C31 0.035(3) 0.038(3) 0.040(3) 0.010(2) -0.002(2) 0.011(2) C14 0.076(5) 0.038(3) 0.040(3) -0.007(3) 0.005(3) -0.007(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 2.058(3) 2_565 ? Zn1 O6 2.058(3) 1_556 ? Zn1 O5 2.062(3) 1_446 ? Zn1 O5 2.062(3) 2_675 ? Zn1 O9 2.190(3) . ? Zn1 O9 2.190(3) 2_566 ? N1 C29 1.362(7) . ? N1 C28 1.372(8) . ? N1 C30 1.438(6) . ? O1 C20 1.373(6) . ? O1 C2 1.425(7) . ? C1 C5 1.518(7) . ? C1 C4 1.519(8) . ? C1 C2 1.524(7) . ? C1 C3 1.543(8) . ? Zn2 O4 1.938(4) 1_446 ? Zn2 O7 1.977(3) 1_556 ? Zn2 N2 2.002(4) . ? Zn2 O9 2.012(3) . ? N2 C29 1.310(7) . ? N2 C27 1.376(7) . ? O2 C6 1.364(6) . ? O2 C5 1.438(6) . ? C13 O3 1.368(7) . ? C13 C14 1.372(8) . ? C13 C18 1.390(8) . ? C7 C8 1.378(7) . ? C7 C6 1.390(8) . ? O7 C12 1.270(6) . ? O7 Zn2 1.977(3) 1_554 ? O4 C26 1.272(6) . ? O4 Zn2 1.938(4) 1_664 ? C4 O3 1.425(6) . ? C15 C16 1.364(8) . ? C15 C14 1.385(8) . ? O6 C12 1.253(6) . ? O6 Zn1 2.058(3) 1_554 ? C6 C11 1.376(8) . ? C9 C10 1.393(7) . ? C9 C8 1.399(7) . ? C9 C12 1.491(7) . ? O9 C19 1.262(6) . ? O8 C19 1.239(7) . ? C22 C23 1.379(8) . ? C22 C21 1.383(8) . ? C21 C20 1.382(8) . ? C20 C25 1.385(8) . ? C19 C16 1.501(8) . ? O5 C26 1.248(6) . ? O5 Zn1 2.062(3) 1_664 ? C26 C23 1.494(6) . ? C11 C10 1.385(7) . ? C25 C24 1.375(7) . ? C24 C23 1.388(7) . ? C28 C27 1.351(7) . ? C32 C30 1.360(9) . ? C32 C31 1.385(8) 2_376 ? C30 C31 1.394(8) . ? C18 C17 1.367(8) . ? C17 C16 1.393(8) . ? C31 C32 1.385(8) 2_376 ? 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 O6 180.00(10) 2_565 1_556 ? O6 Zn1 O5 85.26(14) 2_565 1_446 ? O6 Zn1 O5 94.74(14) 1_556 1_446 ? O6 Zn1 O5 94.74(14) 2_565 2_675 ? O6 Zn1 O5 85.26(14) 1_556 2_675 ? O5 Zn1 O5 180.00(16) 1_446 2_675 ? O6 Zn1 O9 88.18(14) 2_565 . ? O6 Zn1 O9 91.82(14) 1_556 . ? O5 Zn1 O9 88.44(13) 1_446 . ? O5 Zn1 O9 91.56(13) 2_675 . ? O6 Zn1 O9 91.82(14) 2_565 2_566 ? O6 Zn1 O9 88.18(14) 1_556 2_566 ? O5 Zn1 O9 91.56(13) 1_446 2_566 ? O5 Zn1 O9 88.44(13) 2_675 2_566 ? O9 Zn1 O9 180.00(17) . 2_566 ? C29 N1 C28 107.3(4) . . ? C29 N1 C30 126.1(5) . . ? C28 N1 C30 126.6(5) . . ? C20 O1 C2 116.5(4) . . ? C5 C1 C4 111.4(4) . . ? C5 C1 C2 111.0(4) . . ? C4 C1 C2 104.9(5) . . ? C5 C1 C3 107.7(5) . . ? C4 C1 C3 110.3(4) . . ? C2 C1 C3 111.6(4) . . ? O4 Zn2 O7 104.28(19) 1_446 1_556 ? O4 Zn2 N2 110.22(18) 1_446 . ? O7 Zn2 N2 95.16(17) 1_556 . ? O4 Zn2 O9 108.03(16) 1_446 . ? O7 Zn2 O9 107.49(16) 1_556 . ? N2 Zn2 O9 128.44(16) . . ? C29 N2 C27 107.0(4) . . ? C29 N2 Zn2 130.3(4) . . ? C27 N2 Zn2 121.5(4) . . ? C6 O2 C5 117.2(4) . . ? O1 C2 C1 108.7(5) . . ? O3 C13 C14 116.1(5) . . ? O3 C13 C18 123.7(5) . . ? C14 C13 C18 120.2(5) . . ? C8 C7 C6 120.5(5) . . ? C12 O7 Zn2 123.0(3) . 1_554 ? C26 O4 Zn2 121.6(3) . 1_664 ? O3 C4 C1 108.9(5) . . ? C16 C15 C14 120.4(5) . . ? C12 O6 Zn1 142.0(3) . 1_554 ? O2 C6 C11 124.7(5) . . ? O2 C6 C7 115.1(5) . . ? C11 C6 C7 120.2(5) . . ? C10 C9 C8 118.7(4) . . ? C10 C9 C12 120.6(4) . . ? C8 C9 C12 120.5(4) . . ? C19 O9 Zn2 106.3(3) . . ? C19 O9 Zn1 137.8(3) . . ? Zn2 O9 Zn1 102.85(14) . . ? C7 C8 C9 120.0(5) . . ? C23 C22 C21 121.2(6) . . ? C20 C21 C22 119.4(5) . . ? O1 C20 C21 124.4(5) . . ? O1 C20 C25 115.5(5) . . ? C21 C20 C25 120.1(5) . . ? O8 C19 O9 119.1(5) . . ? O8 C19 C16 119.6(5) . . ? O9 C19 C16 121.3(5) . . ? C13 O3 C4 116.6(4) . . ? C26 O5 Zn1 143.7(3) . 1_664 ? O2 C5 C1 108.8(4) . . ? O5 C26 O4 124.8(4) . . ? O5 C26 C23 117.7(4) . . ? O4 C26 C23 117.5(4) . . ? C6 C11 C10 119.5(5) . . ? C24 C25 C20 119.7(5) . . ? C25 C24 C23 121.0(5) . . ? C22 C23 C24 118.6(5) . . ? C22 C23 C26 121.9(5) . . ? C24 C23 C26 119.5(5) . . ? C27 C28 N1 106.5(5) . . ? C30 C32 C31 119.9(5) . 2_376 ? C32 C30 C31 121.0(5) . . ? C32 C30 N1 120.4(5) . . ? C31 C30 N1 118.6(6) . . ? N2 C29 N1 110.2(5) . . ? O6 C12 O7 125.1(4) . . ? O6 C12 C9 117.6(4) . . ? O7 C12 C9 117.3(4) . . ? C17 C18 C13 119.5(5) . . ? C18 C17 C16 120.4(6) . . ? C15 C16 C17 119.6(5) . . ? C15 C16 C19 121.6(5) . . ? C17 C16 C19 118.8(5) . . ? C28 C27 N2 109.1(5) . . ? C11 C10 C9 121.1(5) . . ? C32 C31 C30 119.2(6) 2_376 . ? C13 C14 C15 119.8(6) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.869 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.221