data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H60 N10 O24 Zn3' _chemical_formula_weight 1237.07 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 p21/c 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 11.1267(6) _cell_length_b 12.8597(7) _cell_length_c 21.0138(14) _cell_angle_alpha 90.00 _cell_angle_beta 119.836(4) _cell_angle_gamma 90.00 _cell_volume 2608.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2114 _cell_measurement_theta_min 2.9356 _cell_measurement_theta_max 29.2110 _exptl_crystal_description 'Prism' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.459 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.96133 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2312 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10773 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0950 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4540 _reflns_number_gt 2859 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0298P)^2^+1.2262P] 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 4540 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 0.0403(3) Uani 1 2 d S . . Zn2 Zn 0.10534(6) 0.55149(5) 0.37082(4) 0.0422(2) Uani 1 1 d . . . O1 O 0.2206(4) 0.4209(4) 0.4013(3) 0.0847(16) Uani 1 1 d . . . O2 O 0.1420(4) 0.4432(3) 0.4745(2) 0.0602(11) Uani 1 1 d . . . O3 O 0.1689(3) 0.4924(3) 0.6147(2) 0.0518(10) Uani 1 1 d . . . O4 O 0.0848(3) 0.4879(3) 0.69082(19) 0.0546(10) Uani 1 1 d . . . O5 O 0.1414(4) 0.6784(3) 0.4245(2) 0.0558(11) Uani 1 1 d . . . O6 O 0.0662(4) 0.6526(3) 0.5039(2) 0.0520(10) Uani 1 1 d . . . O7 O 0.8188(4) 0.5469(3) 1.0643(3) 0.0987(18) Uani 1 1 d . . . O8 O 0.4487(4) 0.7046(3) 0.8748(2) 0.0870(15) Uani 1 1 d . . . O9 O 0.4781(4) 0.3544(3) 0.8857(2) 0.0584(11) Uani 1 1 d . . . O11 O 0.1319(4) 0.6103(3) 0.2911(2) 0.0632(12) Uani 1 1 d . . . N1 N 0.6485(4) 0.4476(3) 0.9773(2) 0.0384(10) Uani 1 1 d . . . N2 N 0.4571(4) 0.5300(3) 0.8796(2) 0.0390(10) Uani 1 1 d . . . N3 N 0.6336(5) 0.6280(3) 0.9711(3) 0.095(2) Uani 1 1 d . . . N4 N 0.2378(5) 0.6668(4) 0.2309(3) 0.0507(12) Uani 1 1 d . . . C1 C 0.2051(6) 0.3925(4) 0.4523(4) 0.0585(18) Uani 1 1 d . . . C4 C 0.5098(6) 0.6265(4) 0.9057(3) 0.0577(17) Uani 1 1 d . . . C5 C 0.3197(5) 0.5217(4) 0.8136(3) 0.0420(13) Uani 1 1 d . . . H5A H 0.2662 0.5832 0.8101 0.050 Uiso 1 1 calc R . . H5B H 0.2719 0.4620 0.8187 0.050 Uiso 1 1 calc R . . C6 C 0.3248(4) 0.5107(4) 0.7436(3) 0.0408(13) Uani 1 1 d . . . H6A H 0.3823 0.4514 0.7478 0.049 Uiso 1 1 calc R . . H6B H 0.3674 0.5723 0.7366 0.049 Uiso 1 1 calc R . . C7 C 0.1820(5) 0.4961(4) 0.6771(3) 0.0378(12) Uani 1 1 d . . . C8 C 0.5256(5) 0.4381(4) 0.9121(3) 0.0388(12) Uani 1 1 d . . . C9 C 0.7215(5) 0.3519(4) 1.0154(3) 0.0449(14) Uani 1 1 d . . . H9A H 0.6536 0.2994 1.0088 0.054 Uiso 1 1 calc R . . H9B H 0.7766 0.3662 1.0675 0.054 Uiso 1 1 calc R . . C10 C 0.8142(5) 0.3095(4) 0.9889(3) 0.0435(14) Uani 1 1 d . . . H10A H 0.8895 0.3580 1.0014 0.052 Uiso 1 1 calc R . . H10B H 0.7620 0.3032 0.9359 0.052 Uiso 1 1 calc R . . C11 C 0.7090(6) 0.5412(4) 1.0078(3) 0.0643(18) Uani 1 1 d . . . C12 C 0.1257(5) 0.7039(4) 0.4779(3) 0.0390(13) Uani 1 1 d . . . C13 C 0.2375(6) 0.6202(4) 0.2864(3) 0.0522(15) Uani 1 1 d . . . H13 H 0.3204 0.5935 0.3238 0.063 Uiso 1 1 calc R . . C14 C 0.3641(6) 0.6714(5) 0.2262(4) 0.079(2) Uani 1 1 d . . . H14A H 0.4418 0.6518 0.2726 0.118 Uiso 1 1 calc R . . H14B H 0.3772 0.7410 0.2143 0.118 Uiso 1 1 calc R . . H14C H 0.3564 0.6245 0.1888 0.118 Uiso 1 1 calc R . . C15 C 0.1133(6) 0.7147(5) 0.1730(4) 0.0741(19) Uani 1 1 d . . . H15A H 0.0448 0.7193 0.1880 0.111 Uiso 1 1 calc R . . H15B H 0.0779 0.6733 0.1293 0.111 Uiso 1 1 calc R . . H15C H 0.1346 0.7832 0.1633 0.111 Uiso 1 1 calc R . . O12 O 0.7618(8) 0.5503(5) 0.8800(4) 0.154(3) Uani 1 1 d . . . N5 N 0.8292(6) 0.6380(4) 0.8107(4) 0.0759(16) Uani 1 1 d . . . C16 C 0.9262(8) 0.6466(6) 0.7847(4) 0.121(3) Uani 1 1 d . . . H16A H 0.9923 0.5910 0.8047 0.182 Uiso 1 1 calc R . . H16B H 0.9735 0.7121 0.7999 0.182 Uiso 1 1 calc R . . H16C H 0.8775 0.6425 0.7321 0.182 Uiso 1 1 calc R . . C17 C 0.7202(10) 0.7107(8) 0.7875(6) 0.179(5) Uani 1 1 d . . . H17A H 0.7487 0.7669 0.8221 0.268 Uiso 1 1 calc R . . H17B H 0.6405 0.6772 0.7846 0.268 Uiso 1 1 calc R . . H17C H 0.6972 0.7373 0.7401 0.268 Uiso 1 1 calc R . . C18 C 0.8413(9) 0.5648(6) 0.8579(5) 0.096(3) Uani 1 1 d . . . H18 H 0.9178 0.5210 0.8754 0.115 Uiso 1 1 calc R . . O10 O 0.4363(5) 0.4941(5) 0.6184(3) 0.1170(19) Uani 1 1 d . . . H10 H 0.3593 0.4968 0.6145 0.175 Uiso 1 1 d R . . C19 C 0.4583(8) 0.5805(6) 0.5908(6) 0.141(4) Uani 1 1 d . . . H19A H 0.3983 0.6346 0.5902 0.212 Uiso 1 1 calc R . . H19B H 0.4394 0.5675 0.5417 0.212 Uiso 1 1 calc R . . H19C H 0.5530 0.6018 0.6206 0.212 Uiso 1 1 calc R . . C2 C 0.7465(7) 0.7688(7) 0.9914(4) 0.118(4) Uani 1 1 d . . . H2A H 0.6917 0.7796 0.9388 0.142 Uiso 1 1 d R . . H2B H 0.8232 0.7217 1.0039 0.142 Uiso 1 1 d R . . C3 C 0.6757(8) 0.7481(8) 1.0225(4) 0.147(5) Uani 1 1 d . . . H3A H 0.5973 0.7939 1.0089 0.176 Uiso 1 1 d R . . H3B H 0.7302 0.7393 1.0753 0.176 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0417(5) 0.0382(5) 0.0344(6) 0.0048(4) 0.0140(4) -0.0112(4) Zn2 0.0375(4) 0.0414(4) 0.0449(4) -0.0125(3) 0.0183(3) -0.0047(3) O1 0.071(3) 0.128(4) 0.057(3) -0.001(3) 0.033(3) 0.040(3) O2 0.056(3) 0.079(3) 0.052(3) 0.007(2) 0.032(2) -0.006(2) O3 0.043(2) 0.075(3) 0.034(2) 0.005(2) 0.0167(19) -0.005(2) O4 0.035(2) 0.085(3) 0.038(2) -0.007(2) 0.0138(18) -0.012(2) O5 0.095(3) 0.041(2) 0.041(3) -0.0104(19) 0.041(2) -0.023(2) O6 0.064(2) 0.040(2) 0.065(3) -0.006(2) 0.041(2) -0.018(2) O7 0.074(3) 0.051(3) 0.076(4) -0.017(3) -0.034(3) 0.007(2) O8 0.071(3) 0.036(2) 0.085(4) 0.005(2) -0.013(3) 0.017(2) O9 0.066(3) 0.034(2) 0.058(3) -0.008(2) 0.018(2) -0.011(2) O11 0.054(2) 0.088(3) 0.062(3) -0.013(2) 0.040(2) -0.013(2) N1 0.045(2) 0.024(2) 0.033(3) -0.001(2) 0.010(2) 0.009(2) N2 0.035(2) 0.033(2) 0.034(3) -0.007(2) 0.006(2) 0.000(2) N3 0.078(4) 0.025(3) 0.081(4) -0.023(3) -0.037(3) 0.012(3) N4 0.047(3) 0.062(3) 0.043(3) -0.004(3) 0.022(3) 0.001(3) C1 0.048(4) 0.035(3) 0.044(4) -0.005(3) -0.014(3) 0.010(3) C4 0.053(4) 0.032(3) 0.051(4) -0.005(3) -0.002(3) 0.010(3) C5 0.032(3) 0.053(3) 0.033(3) -0.007(3) 0.011(3) -0.002(3) C6 0.028(3) 0.050(3) 0.038(3) 0.001(3) 0.011(3) -0.007(3) C7 0.041(3) 0.031(3) 0.037(4) 0.000(3) 0.016(3) -0.004(3) C8 0.046(3) 0.033(3) 0.035(3) -0.005(3) 0.019(3) -0.001(3) C9 0.053(3) 0.032(3) 0.037(4) 0.007(3) 0.013(3) 0.016(3) C10 0.058(3) 0.036(3) 0.042(4) 0.004(3) 0.029(3) 0.015(3) C11 0.057(4) 0.040(3) 0.048(4) -0.004(3) -0.010(3) 0.007(3) C12 0.044(3) 0.029(3) 0.037(4) 0.002(3) 0.015(3) -0.003(3) C13 0.050(4) 0.059(4) 0.041(4) -0.011(3) 0.017(3) 0.002(3) C14 0.063(4) 0.112(6) 0.074(5) -0.002(4) 0.043(4) -0.008(4) C15 0.071(4) 0.081(5) 0.072(5) 0.004(4) 0.036(4) 0.014(4) O12 0.196(7) 0.131(5) 0.183(8) 0.007(5) 0.130(7) -0.027(5) N5 0.080(4) 0.058(4) 0.084(5) -0.003(3) 0.036(4) -0.003(3) C16 0.143(8) 0.142(8) 0.099(7) -0.051(6) 0.075(7) -0.063(6) C17 0.192(10) 0.157(10) 0.183(12) 0.075(9) 0.090(10) 0.108(9) C18 0.095(6) 0.076(6) 0.099(7) -0.001(5) 0.036(6) -0.001(5) O10 0.073(3) 0.142(5) 0.117(5) 0.025(4) 0.033(3) 0.005(4) C19 0.091(6) 0.109(7) 0.204(12) 0.076(8) 0.058(7) -0.001(6) C2 0.058(4) 0.213(10) 0.100(7) 0.097(7) 0.052(5) 0.046(6) C3 0.092(6) 0.302(14) 0.056(6) 0.035(7) 0.044(5) 0.086(8) _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 O2 2.039(4) 3_566 ? Zn1 O2 2.039(4) . ? Zn1 O6 2.083(3) 3_566 ? Zn1 O6 2.083(3) . ? Zn1 O3 2.201(4) . ? Zn1 O3 2.201(4) 3_566 ? Zn2 O5 1.909(3) . ? Zn2 O4 1.919(3) 3_566 ? Zn2 O11 1.990(4) . ? Zn2 O1 2.015(5) . ? Zn2 O2 2.443(4) . ? O1 C1 1.223(8) . ? O2 C1 1.209(7) . ? O3 C7 1.245(6) . ? O4 C7 1.255(5) . ? O4 Zn2 1.919(3) 3_566 ? O5 C12 1.260(6) . ? O6 C12 1.239(5) . ? O7 C11 1.210(6) . ? O8 C4 1.205(6) . ? O9 C8 1.207(5) . ? O11 C13 1.233(6) . ? N1 C11 1.372(6) . ? N1 C8 1.377(6) . ? N1 C9 1.472(5) . ? N2 C4 1.366(6) . ? N2 C8 1.388(6) . ? N2 C5 1.470(6) . ? N3 C4 1.378(7) . ? N3 C11 1.379(7) . ? N3 C3 1.809(11) . ? N4 C13 1.312(7) . ? N4 C15 1.450(7) . ? N4 C14 1.457(6) . ? C1 C2 1.894(11) 2_646 ? C5 C6 1.508(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.518(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C9 C10 1.498(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C12 1.521(6) 2_646 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C12 C10 1.521(6) 2_656 ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? O12 C18 1.202(9) . ? N5 C18 1.325(9) . ? N5 C17 1.412(8) . ? N5 C16 1.435(8) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18 0.9300 . ? O10 C19 1.331(7) . ? O10 H10 0.8200 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C2 C3 1.278(8) . ? C2 C1 1.894(11) 2_656 ? C2 H2A 0.9701 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9699 . ? 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 O2 Zn1 O2 180.0(2) 3_566 . ? O2 Zn1 O6 92.42(15) 3_566 3_566 ? O2 Zn1 O6 87.58(15) . 3_566 ? O2 Zn1 O6 87.58(15) 3_566 . ? O2 Zn1 O6 92.42(15) . . ? O6 Zn1 O6 180.000(1) 3_566 . ? O2 Zn1 O3 94.54(14) 3_566 . ? O2 Zn1 O3 85.46(14) . . ? O6 Zn1 O3 95.39(14) 3_566 . ? O6 Zn1 O3 84.61(14) . . ? O2 Zn1 O3 85.46(14) 3_566 3_566 ? O2 Zn1 O3 94.54(14) . 3_566 ? O6 Zn1 O3 84.61(14) 3_566 3_566 ? O6 Zn1 O3 95.39(14) . 3_566 ? O3 Zn1 O3 180.000(1) . 3_566 ? O5 Zn2 O4 117.49(17) . 3_566 ? O5 Zn2 O11 95.59(15) . . ? O4 Zn2 O11 96.18(16) 3_566 . ? O5 Zn2 O1 127.67(18) . . ? O4 Zn2 O1 107.92(18) 3_566 . ? O11 Zn2 O1 104.31(18) . . ? O5 Zn2 O2 93.83(15) . . ? O4 Zn2 O2 95.20(14) 3_566 . ? O11 Zn2 O2 159.85(15) . . ? O1 Zn2 O2 56.19(16) . . ? C1 O1 Zn2 100.6(4) . . ? C1 O2 Zn1 165.6(4) . . ? C1 O2 Zn2 80.5(4) . . ? Zn1 O2 Zn2 102.87(17) . . ? C7 O3 Zn1 137.7(3) . . ? C7 O4 Zn2 130.8(4) . 3_566 ? C12 O5 Zn2 131.8(3) . . ? C12 O6 Zn1 137.8(3) . . ? C13 O11 Zn2 130.8(4) . . ? C11 N1 C8 123.8(4) . . ? C11 N1 C9 117.9(4) . . ? C8 N1 C9 118.3(4) . . ? C4 N2 C8 123.7(4) . . ? C4 N2 C5 118.8(4) . . ? C8 N2 C5 117.5(4) . . ? C4 N3 C11 125.1(5) . . ? C4 N3 C3 116.1(4) . . ? C11 N3 C3 116.9(5) . . ? C13 N4 C15 121.0(5) . . ? C13 N4 C14 120.5(5) . . ? C15 N4 C14 118.5(5) . . ? O2 C1 O1 122.6(6) . . ? O2 C1 C2 104.6(6) . 2_646 ? O1 C1 C2 132.7(6) . 2_646 ? O8 C4 N2 121.7(5) . . ? O8 C4 N3 122.8(5) . . ? N2 C4 N3 115.4(5) . . ? N2 C5 C6 113.6(4) . . ? N2 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C5 C6 C7 112.3(4) . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? O3 C7 O4 125.2(5) . . ? O3 C7 C6 119.6(4) . . ? O4 C7 C6 115.2(5) . . ? O9 C8 N1 121.8(5) . . ? O9 C8 N2 121.7(5) . . ? N1 C8 N2 116.4(4) . . ? N1 C9 C10 113.4(4) . . ? N1 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N1 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C9 C10 C12 112.4(4) . 2_646 ? C9 C10 H10A 109.1 . . ? C12 C10 H10A 109.1 2_646 . ? C9 C10 H10B 109.1 . . ? C12 C10 H10B 109.1 2_646 . ? H10A C10 H10B 107.9 . . ? O7 C11 N1 122.3(5) . . ? O7 C11 N3 122.4(5) . . ? N1 C11 N3 115.3(5) . . ? O6 C12 O5 126.5(5) . . ? O6 C12 C10 118.8(5) . 2_656 ? O5 C12 C10 114.7(4) . 2_656 ? O11 C13 N4 122.8(6) . . ? O11 C13 H13 118.6 . . ? N4 C13 H13 118.6 . . ? N4 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N4 C15 H15A 109.5 . . ? N4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 N5 C17 118.6(7) . . ? C18 N5 C16 121.5(7) . . ? C17 N5 C16 119.8(7) . . ? N5 C16 H16A 109.5 . . ? N5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N5 C17 H17A 109.5 . . ? N5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O12 C18 N5 125.4(9) . . ? O12 C18 H18 117.3 . . ? N5 C18 H18 117.3 . . ? C19 O10 H10 109.4 . . ? O10 C19 H19A 109.5 . . ? O10 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O10 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C3 C2 C1 84.9(8) . 2_656 ? C3 C2 H2A 114.5 . . ? C1 C2 H2A 114.4 2_656 . ? C3 C2 H2B 114.6 . . ? C1 C2 H2B 114.6 2_656 . ? H2A C2 H2B 111.6 . . ? C2 C3 N3 85.0(6) . . ? C2 C3 H3A 114.6 . . ? N3 C3 H3A 114.5 . . ? C2 C3 H3B 114.5 . . ? N3 C3 H3B 114.4 . . ? H3A C3 H3B 111.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Zn2 O1 C1 67.7(5) . . . . ? O4 Zn2 O1 C1 -81.9(4) 3_566 . . . ? O11 Zn2 O1 C1 176.6(4) . . . . ? O2 Zn2 O1 C1 2.3(4) . . . . ? O2 Zn1 O2 C1 -98(100) 3_566 . . . ? O6 Zn1 O2 C1 26.8(18) 3_566 . . . ? O6 Zn1 O2 C1 -153.2(18) . . . . ? O3 Zn1 O2 C1 122.4(18) . . . . ? O3 Zn1 O2 C1 -57.6(18) 3_566 . . . ? O2 Zn1 O2 Zn2 4(100) 3_566 . . . ? O6 Zn1 O2 Zn2 128.93(16) 3_566 . . . ? O6 Zn1 O2 Zn2 -51.07(16) . . . . ? O3 Zn1 O2 Zn2 -135.46(16) . . . . ? O3 Zn1 O2 Zn2 44.54(16) 3_566 . . . ? O5 Zn2 O2 C1 -136.1(3) . . . . ? O4 Zn2 O2 C1 105.8(3) 3_566 . . . ? O11 Zn2 O2 C1 -18.3(6) . . . . ? O1 Zn2 O2 C1 -2.3(4) . . . . ? O5 Zn2 O2 Zn1 58.14(18) . . . . ? O4 Zn2 O2 Zn1 -59.94(18) 3_566 . . . ? O11 Zn2 O2 Zn1 175.9(4) . . . . ? O1 Zn2 O2 Zn1 -168.1(3) . . . . ? O2 Zn1 O3 C7 14.8(5) 3_566 . . . ? O2 Zn1 O3 C7 -165.2(5) . . . . ? O6 Zn1 O3 C7 -78.1(5) 3_566 . . . ? O6 Zn1 O3 C7 101.9(5) . . . . ? O3 Zn1 O3 C7 114(100) 3_566 . . . ? O4 Zn2 O5 C12 69.4(5) 3_566 . . . ? O11 Zn2 O5 C12 169.4(5) . . . . ? O1 Zn2 O5 C12 -77.7(5) . . . . ? O2 Zn2 O5 C12 -28.4(5) . . . . ? O2 Zn1 O6 C12 -155.6(5) 3_566 . . . ? O2 Zn1 O6 C12 24.4(5) . . . . ? O6 Zn1 O6 C12 -45(100) 3_566 . . . ? O3 Zn1 O6 C12 109.6(5) . . . . ? O3 Zn1 O6 C12 -70.4(5) 3_566 . . . ? O5 Zn2 O11 C13 87.5(5) . . . . ? O4 Zn2 O11 C13 -154.0(5) 3_566 . . . ? O1 Zn2 O11 C13 -43.7(5) . . . . ? O2 Zn2 O11 C13 -30.0(8) . . . . ? Zn1 O2 C1 O1 108.6(18) . . . . ? Zn2 O2 C1 O1 3.7(6) . . . . ? Zn1 O2 C1 C2 -67.8(19) . . . 2_646 ? Zn2 O2 C1 C2 -172.7(4) . . . 2_646 ? Zn2 O1 C1 O2 -4.5(7) . . . . ? Zn2 O1 C1 C2 170.8(5) . . . 2_646 ? C8 N2 C4 O8 178.1(5) . . . . ? C5 N2 C4 O8 -2.4(9) . . . . ? C8 N2 C4 N3 -4.8(9) . . . . ? C5 N2 C4 N3 174.7(5) . . . . ? C11 N3 C4 O8 -178.5(7) . . . . ? C3 N3 C4 O8 17.7(10) . . . . ? C11 N3 C4 N2 4.3(11) . . . . ? C3 N3 C4 N2 -159.4(5) . . . . ? C4 N2 C5 C6 94.8(6) . . . . ? C8 N2 C5 C6 -85.6(5) . . . . ? N2 C5 C6 C7 176.7(4) . . . . ? Zn1 O3 C7 O4 13.7(9) . . . . ? Zn1 O3 C7 C6 -166.9(3) . . . . ? Zn2 O4 C7 O3 10.0(8) 3_566 . . . ? Zn2 O4 C7 C6 -169.5(3) 3_566 . . . ? C5 C6 C7 O3 175.5(5) . . . . ? C5 C6 C7 O4 -5.0(6) . . . . ? C11 N1 C8 O9 177.2(5) . . . . ? C9 N1 C8 O9 -0.8(7) . . . . ? C11 N1 C8 N2 -4.6(8) . . . . ? C9 N1 C8 N2 177.3(4) . . . . ? C4 N2 C8 O9 -176.9(5) . . . . ? C5 N2 C8 O9 3.6(7) . . . . ? C4 N2 C8 N1 4.9(7) . . . . ? C5 N2 C8 N1 -174.6(4) . . . . ? C11 N1 C9 C10 -92.7(6) . . . . ? C8 N1 C9 C10 85.5(6) . . . . ? N1 C9 C10 C12 -172.8(4) . . . 2_646 ? C8 N1 C11 O7 -178.2(6) . . . . ? C9 N1 C11 O7 -0.1(9) . . . . ? C8 N1 C11 N3 4.1(9) . . . . ? C9 N1 C11 N3 -177.8(5) . . . . ? C4 N3 C11 O7 178.3(7) . . . . ? C3 N3 C11 O7 -18.0(11) . . . . ? C4 N3 C11 N1 -4.0(11) . . . . ? C3 N3 C11 N1 159.6(5) . . . . ? Zn1 O6 C12 O5 16.2(9) . . . . ? Zn1 O6 C12 C10 -164.8(4) . . . 2_656 ? Zn2 O5 C12 O6 -8.7(9) . . . . ? Zn2 O5 C12 C10 172.2(3) . . . 2_656 ? Zn2 O11 C13 N4 -175.9(4) . . . . ? C15 N4 C13 O11 3.2(9) . . . . ? C14 N4 C13 O11 -176.7(5) . . . . ? C17 N5 C18 O12 4.8(13) . . . . ? C16 N5 C18 O12 -177.1(8) . . . . ? C1 C2 C3 N3 -178.3(4) 2_656 . . . ? C4 N3 C3 C2 -96.1(7) . . . . ? C11 N3 C3 C2 98.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.505 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.074 #===end data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H58 N6 O27 S4 Zn3' _chemical_formula_weight 1283.19 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' 'S' 'S' 0.1246 0.1234 '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-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.715(2) _cell_length_b 12.993(3) _cell_length_c 20.374(4) _cell_angle_alpha 107.23(3) _cell_angle_beta 91.26(3) _cell_angle_gamma 110.36(3) _cell_volume 2514.9(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4887 _cell_measurement_theta_min 1.7672 _cell_measurement_theta_max 29.1117 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 1.679 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.8144 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724 (4x4 bin mode) ; _diffrn_measurement_method 'dtprofit.ref' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21885 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.1018 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8795 _reflns_number_gt 5807 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0997P)^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 8795 _refine_ls_number_parameters 675 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1987 _refine_ls_wR_factor_gt 0.1686 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.011 _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 0.04439(5) 0.39986(4) 1.27132(3) 0.03123(14) Uani 1 1 d . . . Zn2 Zn 0.44455(5) -0.11940(4) 0.75232(3) 0.03222(14) Uani 1 1 d . . . Zn3 Zn -0.16295(5) 0.11971(4) 1.16489(3) 0.03330(15) Uani 1 1 d . . . C1 C 0.9413(4) 0.2394(4) 0.3293(3) 0.0302(12) Uani 1 1 d . . . C2 C 0.8726(5) 0.1266(4) 0.3435(3) 0.0360(13) Uani 1 1 d . . . H2A H 0.8658 0.0622 0.3026 0.043 Uiso 1 1 calc R . . H2B H 0.7822 0.1196 0.3529 0.043 Uiso 1 1 calc R . . C3 C 0.9488(5) 0.1196(4) 0.4049(2) 0.0361(13) Uani 1 1 d . . . H3A H 1.0375 0.1218 0.3945 0.043 Uiso 1 1 calc R . . H3B H 0.9600 0.1861 0.4453 0.043 Uiso 1 1 calc R . . C4 C 0.8168(5) -0.3014(4) 0.3478(3) 0.0438(14) Uani 1 1 d . . . H4A H 0.8111 -0.3033 0.2999 0.053 Uiso 1 1 calc R . . H4B H 0.7401 -0.3656 0.3517 0.053 Uiso 1 1 calc R . . C5 C 0.9428(5) -0.3167(4) 0.3669(3) 0.0471(16) Uani 1 1 d . . . H5A H 0.9535 -0.3060 0.4161 0.056 Uiso 1 1 calc R . . H5B H 1.0188 -0.2571 0.3582 0.056 Uiso 1 1 calc R . . C6 C 0.9445(5) -0.4348(4) 0.3268(3) 0.0364(13) Uani 1 1 d . . . C7 C 0.6180(4) -0.0922(4) 0.5278(2) 0.0382(13) Uani 1 1 d . . . H7A H 0.5372 -0.1605 0.5074 0.046 Uiso 1 1 calc R . . H7B H 0.5942 -0.0244 0.5355 0.046 Uiso 1 1 calc R . . C8 C 0.6711(5) -0.0944(5) 0.5963(3) 0.0428(14) Uani 1 1 d . . . H8A H 0.7548 -0.0283 0.6150 0.051 Uiso 1 1 calc R . . H8B H 0.6909 -0.1642 0.5884 0.051 Uiso 1 1 calc R . . C9 C 0.5748(5) -0.0913(4) 0.6495(3) 0.0386(14) Uani 1 1 d . . . C10 C 0.7901(5) 0.0146(4) 0.4698(3) 0.0379(13) Uani 1 1 d . . . C11 C 0.7187(5) -0.1951(4) 0.4393(3) 0.0387(14) Uani 1 1 d . . . C12 C 0.8838(4) -0.0909(4) 0.3778(3) 0.0366(12) Uani 1 1 d . . . C13 C 0.4156(5) 0.0757(4) 0.8179(3) 0.0350(12) Uani 1 1 d . . . C14 C 0.3588(4) 0.1689(4) 0.8457(3) 0.0360(13) Uani 1 1 d . . . H14A H 0.3076 0.1730 0.8073 0.043 Uiso 1 1 calc R . . H14B H 0.2969 0.1464 0.8775 0.043 Uiso 1 1 calc R . . C15 C 0.4615(4) 0.2868(4) 0.8823(3) 0.0349(13) Uani 1 1 d . . . H15A H 0.5193 0.2824 0.9178 0.042 Uiso 1 1 calc R . . H15B H 0.5169 0.3145 0.8495 0.042 Uiso 1 1 calc R . . C16 C 0.3749(5) 0.7665(4) 0.8499(3) 0.0346(12) Uani 1 1 d . . . C17 C 0.3931(5) 0.6842(4) 0.8865(3) 0.0428(13) Uani 1 1 d . . . H17A H 0.4697 0.6644 0.8719 0.051 Uiso 1 1 calc R . . H17B H 0.4122 0.7237 0.9362 0.051 Uiso 1 1 calc R . . C18 C 0.2713(4) 0.5750(4) 0.8711(3) 0.0370(13) Uani 1 1 d . . . H18A H 0.1944 0.5940 0.8860 0.044 Uiso 1 1 calc R . . H18B H 0.2519 0.5345 0.8215 0.044 Uiso 1 1 calc R . . C19 C 0.0462(4) 0.3233(4) 1.1243(3) 0.0345(12) Uani 1 1 d . . . C20 C 0.0935(5) 0.3445(4) 1.0595(3) 0.0386(14) Uani 1 1 d . . . H20A H 0.0315 0.3689 1.0384 0.046 Uiso 1 1 calc R . . H20B H 0.0924 0.2724 1.0270 0.046 Uiso 1 1 calc R . . C21 C 0.2324(5) 0.4350(4) 1.0717(2) 0.0379(13) Uani 1 1 d . . . H21A H 0.2305 0.5102 1.0974 0.045 Uiso 1 1 calc R . . H21B H 0.2919 0.4178 1.0998 0.045 Uiso 1 1 calc R . . C22 C 0.2560(4) 0.5098(4) 0.9726(3) 0.0332(12) Uani 1 1 d . . . C23 C 0.3553(4) 0.3688(4) 0.9775(3) 0.0312(12) Uani 1 1 d . . . C24 C 0.3643(4) 0.4310(4) 0.8763(3) 0.0346(13) Uani 1 1 d . . . C25 C -0.2743(9) 0.0998(7) 0.9733(4) 0.107(2) Uani 1 1 d U . . H25A H -0.2627 0.1736 1.0064 0.161 Uiso 1 1 calc R A 1 H25B H -0.3671 0.0493 0.9655 0.161 Uiso 1 1 calc R A 1 H25C H -0.2472 0.1102 0.9303 0.161 Uiso 1 1 calc R A 1 C26 C -0.2176(8) -0.0841(7) 0.9388(4) 0.096(2) Uani 1 1 d U . . H26A H -0.1696 -0.1278 0.9505 0.143 Uiso 1 1 calc R B 1 H26B H -0.1917 -0.0685 0.8969 0.143 Uiso 1 1 calc R B 1 H26C H -0.3125 -0.1280 0.9320 0.143 Uiso 1 1 calc R B 1 C27 C 0.4038(6) 0.5918(4) 1.2883(4) 0.0637(19) Uani 1 1 d . . . H27A H 0.3373 0.6175 1.2739 0.096 Uiso 1 1 calc R . . H27B H 0.4871 0.6269 1.2727 0.096 Uiso 1 1 calc R . . H27C H 0.4170 0.6137 1.3381 0.096 Uiso 1 1 calc R . . C28 C 0.4826(5) 0.4190(5) 1.2917(4) 0.068(2) Uani 1 1 d . . . H28A H 0.4957 0.4566 1.3410 0.102 Uiso 1 1 calc R . . H28B H 0.5635 0.4510 1.2732 0.102 Uiso 1 1 calc R . . H28C H 0.4611 0.3373 1.2821 0.102 Uiso 1 1 calc R . . C31 C 0.1472(6) 0.8664(6) 0.2288(4) 0.071(2) Uani 1 1 d . . . H31A H 0.2021 0.9003 0.1983 0.106 Uiso 1 1 calc R . . H31B H 0.1961 0.8361 0.2530 0.106 Uiso 1 1 calc R . . H31C H 0.1238 0.9245 0.2616 0.106 Uiso 1 1 calc R . . C32 C 0.0749(6) 0.6596(5) 0.1350(4) 0.074(2) Uani 1 1 d . . . H32A H 0.0070 0.5898 0.1047 0.111 Uiso 1 1 calc R . . H32B H 0.1222 0.6407 0.1674 0.111 Uiso 1 1 calc R . . H32C H 0.1370 0.6964 0.1081 0.111 Uiso 1 1 calc R . . N1 N 0.7180(4) -0.0891(3) 0.4792(2) 0.0363(11) Uani 1 1 d . . . N2 N 0.8757(3) 0.0111(3) 0.4205(2) 0.0308(10) Uani 1 1 d . . . N3 N 0.8108(4) -0.1908(3) 0.3927(2) 0.0384(11) Uani 1 1 d . . . N4 N 0.3960(3) 0.3707(3) 0.9151(2) 0.0283(10) Uani 1 1 d . . . N5 N 0.2952(3) 0.4996(3) 0.9078(2) 0.0315(10) Uani 1 1 d . . . N6 N 0.2860(4) 0.4401(3) 1.0061(2) 0.0306(10) Uani 1 1 d . . . O1 O 0.9296(3) 0.2394(2) 0.26568(15) 0.0281(8) Uani 1 1 d . . . O2 O 1.0083(3) 0.3305(3) 0.37549(18) 0.0425(10) Uani 1 1 d . . . O3 O 0.8416(4) -0.5175(3) 0.2977(2) 0.0536(12) Uani 1 1 d . . . O4 O 1.0622(3) -0.4406(3) 0.32547(19) 0.0459(10) Uani 1 1 d . . . O5 O 0.9555(4) -0.0904(3) 0.3337(2) 0.0615(11) Uani 1 1 d . . . O6 O 0.6482(4) -0.2847(3) 0.4459(2) 0.0607(12) Uani 1 1 d . . . O7 O 0.7829(4) 0.1066(3) 0.5045(2) 0.0555(11) Uani 1 1 d . . . O8 O 0.4713(3) -0.0727(3) 0.63966(19) 0.0465(10) Uani 1 1 d . . . O9 O 0.6056(3) -0.1119(3) 0.70425(17) 0.0388(9) Uani 1 1 d . . . O10 O 0.3188(3) -0.2736(3) 0.6835(2) 0.0431(10) Uani 1 1 d . . . H10 H 0.3085 -0.3256 0.7003 0.065 Uiso 1 1 calc R . . O11 O 0.3301(3) -0.0294(2) 0.79155(16) 0.0309(8) Uani 1 1 d . . . O12 O 0.5366(3) 0.0971(3) 0.8189(2) 0.0503(11) Uani 1 1 d . . . O13 O 0.3960(4) 0.4253(3) 0.81925(19) 0.0510(10) Uani 1 1 d . . . O14 O 0.3793(3) 0.3091(3) 1.0089(2) 0.0537(10) Uani 1 1 d . . . O15 O 0.1957(3) 0.5715(3) 0.99828(19) 0.0474(10) Uani 1 1 d . . . O16 O 0.2605(3) 0.7692(3) 0.8428(2) 0.0474(10) Uani 1 1 d . . . O17 O 0.4754(3) 0.8236(3) 0.82845(19) 0.0463(10) Uani 1 1 d . . . O18 O 0.0670(3) 0.4112(3) 1.17691(18) 0.0414(10) Uani 1 1 d . . . O19 O -0.0059(3) 0.2210(3) 1.1231(2) 0.0500(11) Uani 1 1 d . . . O20 O -0.2499(5) 0.0087(4) 1.0660(2) 0.0779(15) Uani 1 1 d . . . O21 O -0.0474(3) 0.0235(3) 1.1745(2) 0.0510(11) Uani 1 1 d . . . H21 H 0.0064 0.0582 1.2103 0.076 Uiso 1 1 calc R C . O22 O 0.2305(3) 0.3949(3) 1.2901(2) 0.0455(10) Uani 1 1 d . . . O24 O -0.0525(4) 0.7964(4) 0.1277(3) 0.0891(16) Uani 1 1 d . . . O25 O 0.8314(4) 0.8464(3) 0.7283(3) 0.0741(15) Uani 1 1 d . . . O26 O 0.7101(5) 0.2223(4) 0.6298(3) 0.107(2) Uani 1 1 d . . . O27 O 0.4354(4) 0.1376(4) 0.6645(3) 0.0827(16) Uani 1 1 d . . . S1 S 0.34945(12) 0.44090(11) 1.25267(8) 0.0421(4) Uani 1 1 d . . . S2A S -0.1810(5) 0.0416(3) 1.00349(19) 0.0891(13) Uani 0.516(3) 1 d PU C 1 S2B S -0.3136(4) -0.0304(3) 0.99334(17) 0.0620(10) Uani 0.484(3) 1 d PU C 2 S4A S 0.2610(4) 0.5181(4) 0.5267(2) 0.0590(13) Uani 0.372(3) 1 d P D 1 S4B S 0.3436(2) 0.5920(2) 0.49515(12) 0.0502(7) Uani 0.628(3) 1 d P D 2 S3 S -0.00016(15) 0.75324(14) 0.17973(10) 0.0639(5) Uani 1 1 d . . . O23 O 0.4080(4) 0.6359(5) 0.5713(3) 0.1068(19) Uani 1 1 d . . . C29 C 0.1889(7) 0.6047(7) 0.4982(5) 0.104(3) Uani 1 1 d . . . H29A H 0.1584 0.6488 0.5365 0.155 Uiso 1 1 calc R D 1 H29B H 0.1143 0.5554 0.4625 0.155 Uiso 1 1 calc R D 1 H29C H 0.2553 0.6568 0.4801 0.155 Uiso 1 1 calc R D 1 C30 C 0.3032(8) 0.4480(7) 0.4688(6) 0.150(4) Uani 1 1 d . . . H30A H 0.3407 0.4009 0.4846 0.226 Uiso 1 1 calc R D 1 H30B H 0.3698 0.4977 0.4496 0.226 Uiso 1 1 calc R D 1 H30C H 0.2271 0.3989 0.4339 0.226 Uiso 1 1 calc R D 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0340(2) 0.0249(2) 0.0363(3) 0.0104(2) 0.0103(2) 0.0120(2) Zn2 0.0358(2) 0.0327(2) 0.0367(3) 0.0157(2) 0.0133(2) 0.0185(2) Zn3 0.0403(3) 0.0273(2) 0.0351(3) 0.0134(2) 0.0104(2) 0.0128(2) C1 0.0259(18) 0.0299(19) 0.042(3) 0.0146(18) 0.0089(19) 0.0163(16) C2 0.037(2) 0.032(2) 0.041(3) 0.016(2) 0.003(2) 0.0119(19) C3 0.048(2) 0.035(2) 0.027(3) 0.0064(19) 0.000(2) 0.0213(19) C4 0.058(3) 0.034(2) 0.041(3) 0.007(2) 0.007(2) 0.022(2) C5 0.045(2) 0.040(2) 0.055(4) 0.009(2) 0.006(3) 0.019(2) C6 0.055(2) 0.0295(19) 0.035(3) 0.0118(19) 0.021(2) 0.0257(19) C7 0.039(2) 0.048(2) 0.037(3) 0.017(2) 0.017(2) 0.023(2) C8 0.046(2) 0.056(3) 0.034(3) 0.018(2) 0.018(2) 0.025(2) C9 0.041(2) 0.033(2) 0.038(3) 0.007(2) 0.015(2) 0.012(2) C10 0.039(2) 0.046(2) 0.036(3) 0.020(2) 0.009(2) 0.018(2) C11 0.044(3) 0.033(2) 0.035(3) 0.014(2) 0.010(2) 0.007(2) C12 0.047(2) 0.041(2) 0.037(3) 0.0232(19) 0.018(2) 0.0254(19) C13 0.045(2) 0.032(2) 0.033(3) 0.0148(19) 0.009(2) 0.0168(19) C14 0.037(2) 0.0268(19) 0.047(3) 0.008(2) 0.009(2) 0.0181(18) C15 0.033(2) 0.0217(19) 0.047(3) 0.004(2) 0.007(2) 0.0112(17) C16 0.045(2) 0.0266(19) 0.035(3) 0.0163(18) 0.002(2) 0.0114(19) C17 0.049(2) 0.039(2) 0.061(3) 0.034(2) 0.012(2) 0.0254(19) C18 0.034(2) 0.039(2) 0.041(3) 0.019(2) 0.006(2) 0.0112(19) C19 0.034(2) 0.034(2) 0.041(3) 0.015(2) 0.010(2) 0.0171(18) C20 0.048(3) 0.032(2) 0.033(3) 0.013(2) 0.013(2) 0.011(2) C21 0.040(2) 0.049(3) 0.026(2) 0.013(2) 0.011(2) 0.017(2) C22 0.042(2) 0.0270(19) 0.033(3) 0.0092(19) 0.009(2) 0.0155(18) C23 0.029(2) 0.0289(19) 0.036(3) 0.0118(19) 0.000(2) 0.0100(17) C24 0.035(2) 0.0216(18) 0.051(3) 0.0193(19) 0.014(2) 0.0078(18) C25 0.145(4) 0.090(3) 0.069(3) 0.017(3) 0.017(3) 0.030(3) C26 0.123(3) 0.089(3) 0.065(3) 0.015(3) 0.028(3) 0.034(3) C27 0.072(3) 0.041(3) 0.090(4) 0.029(3) 0.048(3) 0.027(2) C28 0.043(3) 0.065(3) 0.106(5) 0.038(3) 0.007(3) 0.021(3) C31 0.057(3) 0.067(4) 0.068(5) 0.005(4) 0.009(3) 0.013(3) C32 0.075(3) 0.074(4) 0.082(5) 0.016(4) 0.008(4) 0.045(3) N1 0.049(2) 0.0308(18) 0.032(2) 0.0125(16) 0.0171(18) 0.0148(16) N2 0.0406(18) 0.0294(16) 0.031(2) 0.0165(15) 0.0138(16) 0.0165(15) N3 0.0383(18) 0.0384(18) 0.047(3) 0.0160(18) 0.0119(18) 0.0220(16) N4 0.0368(18) 0.0166(15) 0.030(2) 0.0092(14) 0.0087(16) 0.0068(14) N5 0.0434(18) 0.0314(16) 0.033(2) 0.0167(15) 0.0115(16) 0.0239(14) N6 0.0363(17) 0.0296(16) 0.032(2) 0.0150(15) 0.0122(16) 0.0142(15) O1 0.0338(14) 0.0297(13) 0.0269(16) 0.0155(12) 0.0112(12) 0.0132(12) O2 0.0530(18) 0.0306(15) 0.0366(19) 0.0095(14) 0.0008(16) 0.0084(15) O3 0.057(2) 0.0248(16) 0.064(3) 0.0057(17) -0.0063(19) 0.0046(16) O4 0.0569(18) 0.0352(16) 0.048(2) 0.0091(15) 0.0145(17) 0.0233(15) O5 0.088(2) 0.0503(18) 0.071(2) 0.0348(17) 0.0583(19) 0.0400(16) O6 0.073(2) 0.0420(19) 0.066(3) 0.0198(19) 0.027(2) 0.0167(18) O7 0.091(2) 0.0373(17) 0.045(2) 0.0113(16) 0.0265(19) 0.0316(17) O8 0.0414(16) 0.0541(18) 0.054(2) 0.0222(16) 0.0186(16) 0.0252(14) O9 0.0346(15) 0.0490(17) 0.0364(19) 0.0182(15) 0.0115(14) 0.0156(14) O10 0.0371(16) 0.0304(15) 0.059(2) 0.0117(16) 0.0115(16) 0.0104(14) O11 0.0404(15) 0.0201(13) 0.0309(17) 0.0083(12) 0.0074(14) 0.0097(12) O12 0.0364(16) 0.0396(17) 0.075(3) 0.0127(18) 0.0176(17) 0.0183(14) O13 0.079(2) 0.0539(17) 0.040(2) 0.0243(15) 0.0323(17) 0.0391(16) O14 0.0749(19) 0.0635(17) 0.052(2) 0.0323(16) 0.0161(18) 0.0480(15) O15 0.0679(18) 0.0508(16) 0.049(2) 0.0244(15) 0.0324(16) 0.0441(14) O16 0.0460(17) 0.0420(16) 0.066(2) 0.0322(16) 0.0068(17) 0.0175(14) O17 0.0435(17) 0.0486(16) 0.061(2) 0.0377(15) 0.0136(16) 0.0172(15) O18 0.0474(17) 0.0387(16) 0.039(2) 0.0129(15) 0.0141(15) 0.0170(14) O19 0.0633(19) 0.0359(16) 0.058(2) 0.0206(16) 0.0292(18) 0.0217(15) O20 0.130(3) 0.051(2) 0.037(2) 0.0051(19) -0.016(2) 0.023(2) O21 0.0480(18) 0.0395(16) 0.067(3) 0.0133(17) -0.0016(18) 0.0215(15) O22 0.0340(15) 0.0410(16) 0.067(2) 0.0236(16) 0.0125(16) 0.0144(14) O24 0.104(3) 0.077(2) 0.086(4) -0.003(2) -0.032(3) 0.060(2) O25 0.0468(19) 0.049(2) 0.124(4) 0.028(2) -0.016(2) 0.0163(17) O26 0.097(3) 0.075(3) 0.131(5) 0.003(3) 0.054(3) 0.032(3) O27 0.072(2) 0.066(2) 0.111(4) 0.028(3) -0.013(3) 0.028(2) S1 0.0353(6) 0.0412(6) 0.0505(8) 0.0150(6) 0.0103(6) 0.0147(5) S2A 0.128(3) 0.0607(18) 0.0453(17) 0.0241(14) 0.0028(18) -0.0091(19) S2B 0.0886(19) 0.0667(16) 0.0377(15) 0.0216(13) 0.0151(14) 0.0325(15) S4A 0.057(2) 0.091(3) 0.034(2) 0.0179(19) 0.0089(17) 0.0339(19) S4B 0.0552(12) 0.0485(12) 0.0395(13) 0.0100(10) 0.0116(10) 0.0137(10) S3 0.0565(8) 0.0525(8) 0.0730(12) 0.0051(8) 0.0137(8) 0.0212(7) O23 0.102(3) 0.133(3) 0.057(3) -0.046(3) -0.030(2) 0.077(3) C29 0.089(4) 0.114(5) 0.113(7) 0.017(5) -0.001(5) 0.061(4) C30 0.128(5) 0.068(4) 0.208(10) -0.037(5) -0.101(6) 0.055(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 O4 1.978(3) 1_466 ? Zn1 O1 1.985(3) 1_456 ? Zn1 O18 1.986(4) . ? Zn1 O22 2.049(3) . ? Zn2 O17 1.973(4) 1_545 ? Zn2 O9 1.990(3) . ? Zn2 O11 1.999(3) . ? Zn2 O10 2.041(3) . ? Zn3 O20 2.066(4) . ? Zn3 O21 2.085(4) . ? Zn3 O16 2.093(4) 2_567 ? Zn3 O19 2.115(4) . ? Zn3 O11 2.144(3) 2_557 ? Zn3 O1 2.136(3) 1_456 ? C1 O2 1.234(5) . ? C1 O1 1.298(6) . ? C1 C2 1.512(6) . ? C2 C3 1.521(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.486(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.482(6) . ? C4 C5 1.490(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.517(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 O3 1.220(5) . ? C6 O4 1.290(6) . ? C7 N1 1.473(6) . ? C7 C8 1.509(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.515(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O8 1.238(6) . ? C9 O9 1.283(7) . ? C10 O7 1.225(6) . ? C10 N1 1.373(6) . ? C10 N2 1.375(6) . ? C11 O6 1.196(6) . ? C11 N3 1.382(6) . ? C11 N1 1.379(6) . ? C12 O5 1.195(6) . ? C12 N2 1.386(6) . ? C12 N3 1.388(6) . ? C13 O12 1.225(5) . ? C13 O11 1.290(5) . ? C13 C14 1.510(7) . ? C14 C15 1.493(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N4 1.499(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 O16 1.245(6) . ? C16 O17 1.248(6) . ? C16 C17 1.533(7) . ? C17 C18 1.498(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N5 1.478(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O19 1.243(6) . ? C19 O18 1.261(5) . ? C19 C20 1.491(7) . ? C20 C21 1.501(6) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N6 1.477(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 O15 1.208(6) . ? C22 N5 1.378(6) . ? C22 N6 1.396(7) . ? C23 O14 1.225(6) . ? C23 N4 1.357(6) . ? C23 N6 1.388(6) . ? C24 O13 1.206(6) . ? C24 N4 1.377(7) . ? C24 N5 1.375(6) . ? C25 S2A 1.650(11) . ? C25 S2B 1.769(10) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 S2B 1.693(9) . ? C26 S2A 1.678(8) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 S1 1.747(5) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 S1 1.766(6) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C31 S3 1.760(6) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 S3 1.736(7) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? O1 Zn1 1.985(3) 1_654 ? O1 Zn3 2.136(3) 1_654 ? O4 Zn1 1.978(3) 1_644 ? O10 H10 0.8200 . ? O11 Zn3 2.144(3) 2_557 ? O16 Zn3 2.093(4) 2_567 ? O17 Zn2 1.973(4) 1_565 ? O20 S2B 1.478(5) . ? O20 S2A 1.579(6) . ? O21 H21 0.8200 . ? O22 S1 1.532(4) . ? O24 S3 1.516(5) . ? S4A C30 1.449(10) . ? S4A O23 1.756(6) . ? S4A C29 1.781(10) . ? S4B O23 1.537(5) . ? S4B C30 1.675(8) . ? S4B C29 1.723(8) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O1 137.09(14) 1_466 1_456 ? O4 Zn1 O18 102.06(16) 1_466 . ? O1 Zn1 O18 110.49(13) 1_456 . ? O4 Zn1 O22 104.70(14) 1_466 . ? O1 Zn1 O22 99.82(13) 1_456 . ? O18 Zn1 O22 94.67(15) . . ? O17 Zn2 O9 103.23(15) 1_545 . ? O17 Zn2 O11 101.81(15) 1_545 . ? O9 Zn2 O11 143.21(14) . . ? O17 Zn2 O10 98.33(15) 1_545 . ? O9 Zn2 O10 95.89(14) . . ? O11 Zn2 O10 106.67(13) . . ? O20 Zn3 O21 91.76(18) . . ? O20 Zn3 O16 91.40(18) . 2_567 ? O21 Zn3 O16 174.16(13) . 2_567 ? O20 Zn3 O19 90.01(17) . . ? O21 Zn3 O19 89.21(15) . . ? O16 Zn3 O19 85.88(15) 2_567 . ? O20 Zn3 O11 91.15(16) . 2_557 ? O21 Zn3 O11 96.05(14) . 2_557 ? O16 Zn3 O11 88.80(13) 2_567 2_557 ? O19 Zn3 O11 174.58(14) . 2_557 ? O20 Zn3 O1 177.99(16) . 1_456 ? O21 Zn3 O1 89.26(14) . 1_456 ? O16 Zn3 O1 87.43(13) 2_567 1_456 ? O19 Zn3 O1 88.27(13) . 1_456 ? O11 Zn3 O1 90.46(11) 2_557 1_456 ? O2 C1 O1 119.2(4) . . ? O2 C1 C2 122.5(5) . . ? O1 C1 C2 118.3(4) . . ? C1 C2 C3 111.8(4) . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? N2 C3 C2 111.0(3) . . ? N2 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? N2 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? N3 C4 C5 112.2(4) . . ? N3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? N3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 C6 113.1(4) . . ? C4 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? C4 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? O3 C6 O4 123.0(4) . . ? O3 C6 C5 122.1(4) . . ? O4 C6 C5 115.0(4) . . ? N1 C7 C8 111.5(4) . . ? N1 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N1 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? C7 C8 C9 113.7(4) . . ? C7 C8 H8A 108.8 . . ? C9 C8 H8A 108.8 . . ? C7 C8 H8B 108.8 . . ? C9 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? O8 C9 O9 122.5(5) . . ? O8 C9 C8 121.7(5) . . ? O9 C9 C8 115.8(5) . . ? O7 C10 N1 122.4(5) . . ? O7 C10 N2 121.1(5) . . ? N1 C10 N2 116.4(4) . . ? O6 C11 N3 121.9(5) . . ? O6 C11 N1 122.7(5) . . ? N3 C11 N1 115.4(4) . . ? O5 C12 N2 121.3(4) . . ? O5 C12 N3 122.9(4) . . ? N2 C12 N3 115.7(4) . . ? O12 C13 O11 120.7(4) . . ? O12 C13 C14 122.6(4) . . ? O11 C13 C14 116.8(4) . . ? C15 C14 C13 114.7(4) . . ? C15 C14 H14A 108.6 . . ? C13 C14 H14A 108.6 . . ? C15 C14 H14B 108.6 . . ? C13 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? N4 C15 C14 111.1(3) . . ? N4 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? N4 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? O16 C16 O17 125.4(5) . . ? O16 C16 C17 117.3(4) . . ? O17 C16 C17 117.3(4) . . ? C18 C17 C16 112.4(4) . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17B 109.1 . . ? C16 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? N5 C18 C17 109.8(4) . . ? N5 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? N5 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? O19 C19 O18 125.0(5) . . ? O19 C19 C20 117.8(4) . . ? O18 C19 C20 117.1(4) . . ? C19 C20 C21 113.1(4) . . ? C19 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? C19 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? N6 C21 C20 112.0(4) . . ? N6 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? N6 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? O15 C22 N5 123.0(5) . . ? O15 C22 N6 121.7(5) . . ? N5 C22 N6 115.3(4) . . ? O14 C23 N4 122.8(4) . . ? O14 C23 N6 120.2(5) . . ? N4 C23 N6 117.0(4) . . ? O13 C24 N4 122.5(4) . . ? O13 C24 N5 122.4(5) . . ? N4 C24 N5 115.0(4) . . ? S2A C25 S2B 47.2(3) . . ? S2A C25 H25A 109.5 . . ? S2B C25 H25A 124.4 . . ? S2A C25 H25B 109.5 . . ? S2B C25 H25B 62.3 . . ? H25A C25 H25B 109.5 . . ? S2A C25 H25C 109.5 . . ? S2B C25 H25C 125.4 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S2B C26 S2A 48.0(3) . . ? S2B C26 H26A 121.8 . . ? S2A C26 H26A 109.5 . . ? S2B C26 H26B 128.1 . . ? S2A C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S2B C26 H26C 61.6 . . ? S2A C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? S1 C27 H27A 109.5 . . ? S1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S3 C32 H32A 109.5 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C10 N1 C11 124.3(4) . . ? C10 N1 C7 118.9(4) . . ? C11 N1 C7 116.2(4) . . ? C12 N2 C10 123.5(4) . . ? C12 N2 C3 117.4(4) . . ? C10 N2 C3 118.5(4) . . ? C11 N3 C12 123.8(4) . . ? C11 N3 C4 118.4(4) . . ? C12 N3 C4 117.1(4) . . ? C23 N4 C24 124.5(4) . . ? C23 N4 C15 116.5(4) . . ? C24 N4 C15 118.2(4) . . ? C22 N5 C24 125.3(4) . . ? C22 N5 C18 117.7(4) . . ? C24 N5 C18 116.8(4) . . ? C23 N6 C22 122.6(4) . . ? C23 N6 C21 118.7(4) . . ? C22 N6 C21 118.5(4) . . ? C1 O1 Zn1 104.0(2) . 1_654 ? C1 O1 Zn3 138.8(3) . 1_654 ? Zn1 O1 Zn3 117.12(16) 1_654 1_654 ? C6 O4 Zn1 109.2(3) . 1_644 ? C9 O9 Zn2 102.3(3) . . ? Zn2 O10 H10 109.5 . . ? C13 O11 Zn2 103.5(3) . . ? C13 O11 Zn3 128.2(3) . 2_557 ? Zn2 O11 Zn3 114.67(14) . 2_557 ? C16 O16 Zn3 141.5(3) . 2_567 ? C16 O17 Zn2 117.8(3) . 1_565 ? C19 O18 Zn1 122.4(3) . . ? C19 O19 Zn3 138.6(3) . . ? S2B O20 S2A 53.2(3) . . ? S2B O20 Zn3 158.9(3) . . ? S2A O20 Zn3 117.1(3) . . ? Zn3 O21 H21 109.5 . . ? S1 O22 Zn1 124.2(2) . . ? O22 S1 C27 104.6(3) . . ? O22 S1 C28 104.3(3) . . ? C27 S1 C28 99.3(3) . . ? O20 S2A C25 104.9(5) . . ? O20 S2A C26 106.0(4) . . ? C25 S2A C26 101.1(5) . . ? O20 S2B C26 110.0(4) . . ? O20 S2B C25 103.8(4) . . ? C26 S2B C25 95.8(5) . . ? C30 S4A O23 105.5(4) . . ? C30 S4A C29 110.1(6) . . ? O23 S4A C29 94.3(4) . . ? O23 S4B C30 105.6(5) . . ? O23 S4B C29 105.2(4) . . ? C30 S4B C29 102.8(4) . . ? O24 S3 C32 107.3(3) . . ? O24 S3 C31 107.4(3) . . ? C32 S3 C31 97.5(3) . . ? S4B O23 S4A 49.2(2) . . ? S4B C29 S4A 46.5(3) . . ? S4B C29 H29A 127.8 . . ? S4A C29 H29A 109.5 . . ? S4B C29 H29B 121.9 . . ? S4A C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? S4B C29 H29C 63.1 . . ? S4A C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? S4A C30 S4B 52.0(3) . . ? S4A C30 H30A 109.5 . . ? S4B C30 H30A 131.0 . . ? S4A C30 H30B 109.5 . . ? S4B C30 H30B 57.9 . . ? H30A C30 H30B 109.5 . . ? S4A C30 H30C 109.5 . . ? S4B C30 H30C 119.4 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.232 _refine_diff_density_min -0.910 _refine_diff_density_rms 0.104 #===end data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18 N3 Na O12 Zn' _chemical_formula_weight 484.65 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' 'Na' 'Na' 0.0362 0.0249 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 11.875(2) _cell_length_b 5.0074(10) _cell_length_c 30.424(8) _cell_angle_alpha 90.00 _cell_angle_beta 111.91(3) _cell_angle_gamma 90.00 _cell_volume 1678.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4130 _cell_measurement_theta_min 1.8729 _cell_measurement_theta_max 27.8605 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 1.567 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.8080 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724 (4x4 bin mode) ; _diffrn_measurement_method 'dtprofit.ref' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11043 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2944 _reflns_number_gt 2666 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1418P)^2^+1.2690P] 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 2944 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.2085 _refine_ls_wR_factor_gt 0.1882 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.008 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 0.39568(5) 0.80040(13) 0.90552(2) 0.0262(3) Uani 1 1 d . . . Na1 Na 0.5227(2) 1.2525(4) 0.87042(8) 0.0260(5) Uani 1 1 d . . . O1 O 0.3633(4) 0.9120(8) 0.83792(14) 0.0360(10) Uani 1 1 d . . . O2 O 0.4335(4) 0.5485(10) 0.81439(14) 0.0421(12) Uani 1 1 d . . . O3 O 0.3564(4) 0.5466(9) 0.5734(2) 0.0508(13) Uani 1 1 d . . . O4 O 0.4357(3) 0.9313(8) 0.56413(15) 0.0300(9) Uani 1 1 d . . . O5 O -0.3663(3) 0.4109(7) 0.59798(13) 0.0235(8) Uani 1 1 d . . . O6 O -0.2673(3) 0.0507(7) 0.59090(15) 0.0268(9) Uani 1 1 d . . . O7 O 0.1357(4) 0.3368(10) 0.69176(16) 0.0426(12) Uani 1 1 d . . . O8 O 0.3264(3) 1.0225(8) 0.64984(13) 0.0301(9) Uani 1 1 d . . . O9 O -0.0210(4) 0.6716(9) 0.54285(14) 0.0314(10) Uani 1 1 d . . . O10 O 0.4204(5) 0.7172(10) 0.98850(18) 0.0487(13) Uani 1 1 d . . . N1 N 0.2347(4) 0.6783(9) 0.67199(16) 0.0242(11) Uani 1 1 d . . . N2 N 0.1532(4) 0.8534(9) 0.59543(15) 0.0197(9) Uani 1 1 d . . . N3 N 0.0535(4) 0.5002(9) 0.61702(15) 0.0219(10) Uani 1 1 d . . . C1 C 0.3733(6) 0.7520(13) 0.8065(2) 0.0301(13) Uani 1 1 d . . . C2 C 0.3012(7) 0.8338(13) 0.7550(2) 0.0402(16) Uani 1 1 d . . . H2A H 0.2152 0.8181 0.7486 0.048 Uiso 1 1 calc R . . H2B H 0.3181 1.0196 0.7508 0.048 Uiso 1 1 calc R . . C3 C 0.3316(5) 0.6659(13) 0.7198(2) 0.0304(14) Uani 1 1 d . . . H3A H 0.4072 0.7279 0.7181 0.036 Uiso 1 1 calc R . . H3B H 0.3428 0.4819 0.7306 0.036 Uiso 1 1 calc R . . C4 C 0.1413(5) 0.4945(12) 0.66266(19) 0.0250(12) Uani 1 1 d . . . C5 C 0.2440(4) 0.8624(11) 0.64003(19) 0.0206(11) Uani 1 1 d . . . C6 C 0.1635(5) 1.0252(11) 0.55781(19) 0.0233(11) Uani 1 1 d . . . H6A H 0.2130 1.1796 0.5720 0.028 Uiso 1 1 calc R . . H6B H 0.0835 1.0884 0.5378 0.028 Uiso 1 1 calc R . . C7 C 0.2204(5) 0.8742(13) 0.52731(19) 0.0275(12) Uani 1 1 d . . . H7A H 0.1684 0.7259 0.5116 0.033 Uiso 1 1 calc R . . H7B H 0.2262 0.9930 0.5030 0.033 Uiso 1 1 calc R . . C8 C 0.3450(5) 0.7700(12) 0.55663(19) 0.0244(12) Uani 1 1 d . . . C9 C 0.0561(5) 0.6733(11) 0.58209(19) 0.0218(12) Uani 1 1 d . . . C10 C -0.0509(5) 0.3160(10) 0.6053(2) 0.0244(12) Uani 1 1 d . . . H10A H -0.0333 0.1785 0.6294 0.029 Uiso 1 1 calc R . . H10B H -0.0645 0.2299 0.5752 0.029 Uiso 1 1 calc R . . C11 C -0.1646(5) 0.4674(12) 0.6023(3) 0.0346(15) Uani 1 1 d . . . H11A H -0.1457 0.5736 0.6308 0.042 Uiso 1 1 calc R . . H11B H -0.1861 0.5899 0.5757 0.042 Uiso 1 1 calc R . . C12 C -0.2726(5) 0.2970(10) 0.59670(19) 0.0203(12) Uani 1 1 d . . . O11 O 0.1429(10) 0.288(2) 0.7909(4) 0.129(4) Uani 1 1 d . . . O12 O 0.0262(15) 0.818(3) 0.7977(7) 0.247(9) 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 0.0183(4) 0.0166(5) 0.0423(5) -0.0012(3) 0.0099(3) 0.0006(2) Na1 0.0260(12) 0.0192(10) 0.0311(12) 0.0008(9) 0.0089(10) 0.0015(9) O1 0.049(3) 0.025(2) 0.030(2) -0.0067(18) 0.010(2) -0.004(2) O2 0.053(3) 0.045(3) 0.027(2) 0.013(2) 0.012(2) 0.021(2) O3 0.035(2) 0.030(3) 0.079(4) 0.016(3) 0.012(2) 0.002(2) O4 0.0192(19) 0.023(2) 0.045(2) -0.0003(18) 0.0093(17) -0.0058(16) O5 0.0209(19) 0.017(2) 0.036(2) 0.0024(16) 0.0140(16) -0.0012(16) O6 0.0239(19) 0.015(2) 0.046(2) -0.0043(17) 0.0181(17) -0.0014(15) O7 0.036(3) 0.053(3) 0.033(2) 0.019(2) 0.006(2) -0.008(2) O8 0.027(2) 0.033(2) 0.026(2) 0.0008(18) 0.0056(17) -0.0142(18) O9 0.020(2) 0.044(3) 0.024(2) 0.0054(18) 0.0020(17) -0.0078(18) O10 0.057(3) 0.046(3) 0.039(3) 0.005(2) 0.013(2) 0.021(2) N1 0.018(2) 0.031(3) 0.020(2) 0.0065(19) 0.0026(19) -0.0029(19) N2 0.017(2) 0.022(2) 0.020(2) 0.0020(18) 0.0059(18) -0.0034(18) N3 0.015(2) 0.025(2) 0.024(2) 0.0035(19) 0.0055(18) -0.0029(19) C1 0.026(3) 0.031(3) 0.029(3) 0.002(3) 0.005(3) 0.000(3) C2 0.045(4) 0.037(4) 0.027(3) 0.002(3) 0.001(3) 0.009(3) C3 0.018(3) 0.048(4) 0.019(3) 0.005(3) -0.001(2) -0.001(3) C4 0.024(3) 0.026(3) 0.027(3) 0.005(2) 0.011(2) 0.000(2) C5 0.014(2) 0.020(3) 0.030(3) -0.002(2) 0.011(2) 0.000(2) C6 0.018(2) 0.020(3) 0.031(3) 0.007(2) 0.008(2) 0.002(2) C7 0.023(3) 0.036(3) 0.020(3) 0.007(2) 0.005(2) -0.001(3) C8 0.026(3) 0.027(3) 0.021(3) -0.003(2) 0.008(2) 0.001(2) C9 0.019(3) 0.024(3) 0.024(3) -0.001(2) 0.010(2) 0.001(2) C10 0.019(3) 0.018(3) 0.036(3) 0.000(2) 0.011(2) -0.003(2) C11 0.018(3) 0.023(3) 0.067(4) -0.001(3) 0.020(3) -0.003(2) C12 0.019(3) 0.018(3) 0.025(3) 0.002(2) 0.010(2) 0.000(2) O11 0.126(8) 0.165(10) 0.100(7) -0.014(6) 0.046(6) 0.017(7) O12 0.181(16) 0.28(2) 0.27(2) 0.013(14) 0.068(16) 0.045(13) _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 O5 1.977(4) 2_556 ? Zn1 O4 1.977(4) 2_656 ? Zn1 O6 2.008(4) 2_566 ? Zn1 O1 2.025(4) . ? Zn1 O10 2.466(5) . ? Zn1 Na1 3.485(2) 1_545 ? Na1 O2 2.208(5) 1_565 ? Na1 O3 2.307(5) 2_666 ? Na1 O8 2.396(4) 2_656 ? Na1 O4 2.462(5) 2_656 ? Na1 O1 2.464(5) . ? Na1 O5 2.517(4) 2_566 ? Na1 Zn1 3.485(2) 1_565 ? O1 C1 1.287(8) . ? O2 C1 1.216(8) . ? O2 Na1 2.208(5) 1_545 ? O3 C8 1.216(7) . ? O3 Na1 2.307(5) 2_646 ? O4 C8 1.297(7) . ? O4 Zn1 1.977(4) 2_656 ? O4 Na1 2.462(5) 2_656 ? O5 C12 1.264(7) . ? O5 Zn1 1.977(4) 2_556 ? O5 Na1 2.517(4) 2_546 ? O6 C12 1.251(7) . ? O6 Zn1 2.008(4) 2_546 ? O7 C4 1.207(7) . ? O8 C5 1.214(6) . ? O8 Na1 2.396(4) 2_656 ? O9 C9 1.203(7) . ? N1 C5 1.374(7) . ? N1 C4 1.386(7) . ? N1 C3 1.482(7) . ? N2 C5 1.384(7) . ? N2 C9 1.399(7) . ? N2 C6 1.473(7) . ? N3 C9 1.381(7) . ? N3 C4 1.391(7) . ? N3 C10 1.478(7) . ? C1 C2 1.534(9) . ? C2 C3 1.506(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C6 C7 1.536(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.507(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C10 C11 1.521(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.496(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O4 118.66(16) 2_556 2_656 ? O5 Zn1 O6 119.78(15) 2_556 2_566 ? O4 Zn1 O6 115.12(16) 2_656 2_566 ? O5 Zn1 O1 104.75(16) 2_556 . ? O4 Zn1 O1 99.09(18) 2_656 . ? O6 Zn1 O1 91.30(18) 2_566 . ? O5 Zn1 O10 80.78(17) 2_556 . ? O4 Zn1 O10 82.23(19) 2_656 . ? O6 Zn1 O10 81.54(17) 2_566 . ? O1 Zn1 O10 172.55(17) . . ? O5 Zn1 Na1 45.15(11) 2_556 1_545 ? O4 Zn1 Na1 85.73(12) 2_656 1_545 ? O6 Zn1 Na1 158.81(13) 2_566 1_545 ? O1 Zn1 Na1 81.12(13) . 1_545 ? O10 Zn1 Na1 106.31(12) . 1_545 ? O2 Na1 O3 97.5(2) 1_565 2_666 ? O2 Na1 O8 108.27(18) 1_565 2_656 ? O3 Na1 O8 100.33(18) 2_666 2_656 ? O2 Na1 O4 163.00(19) 1_565 2_656 ? O3 Na1 O4 86.33(19) 2_666 2_656 ? O8 Na1 O4 87.17(15) 2_656 2_656 ? O2 Na1 O1 94.54(19) 1_565 . ? O3 Na1 O1 155.7(2) 2_666 . ? O8 Na1 O1 95.75(17) 2_656 . ? O4 Na1 O1 76.39(16) 2_656 . ? O2 Na1 O5 82.74(16) 1_565 2_566 ? O3 Na1 O5 81.92(17) 2_666 2_566 ? O8 Na1 O5 168.21(17) 2_656 2_566 ? O4 Na1 O5 81.42(14) 2_656 2_566 ? O1 Na1 O5 78.80(15) . 2_566 ? O2 Na1 Zn1 64.56(13) 1_565 1_565 ? O3 Na1 Zn1 59.41(13) 2_666 1_565 ? O8 Na1 Zn1 155.23(14) 2_656 1_565 ? O4 Na1 Zn1 104.21(12) 2_656 1_565 ? O1 Na1 Zn1 108.21(13) . 1_565 ? O5 Na1 Zn1 33.84(9) 2_566 1_565 ? C1 O1 Zn1 123.2(4) . . ? C1 O1 Na1 117.4(4) . . ? Zn1 O1 Na1 87.55(16) . . ? C1 O2 Na1 142.4(4) . 1_545 ? C8 O3 Na1 147.1(4) . 2_646 ? C8 O4 Zn1 120.4(4) . 2_656 ? C8 O4 Na1 116.9(3) . 2_656 ? Zn1 O4 Na1 88.65(16) 2_656 2_656 ? C12 O5 Zn1 125.7(3) . 2_556 ? C12 O5 Na1 130.8(3) . 2_546 ? Zn1 O5 Na1 101.01(15) 2_556 2_546 ? C12 O6 Zn1 121.9(3) . 2_546 ? C5 O8 Na1 150.1(4) . 2_656 ? C5 N1 C4 124.7(5) . . ? C5 N1 C3 119.0(5) . . ? C4 N1 C3 116.2(4) . . ? C5 N2 C9 124.2(4) . . ? C5 N2 C6 118.9(4) . . ? C9 N2 C6 116.7(4) . . ? C9 N3 C4 123.9(5) . . ? C9 N3 C10 117.6(4) . . ? C4 N3 C10 118.5(4) . . ? O2 C1 O1 125.8(6) . . ? O2 C1 C2 119.3(6) . . ? O1 C1 C2 115.0(5) . . ? C3 C2 C1 112.7(5) . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N1 C3 C2 111.7(5) . . ? N1 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? O7 C4 N1 122.9(5) . . ? O7 C4 N3 121.3(5) . . ? N1 C4 N3 115.8(5) . . ? O8 C5 N1 122.7(5) . . ? O8 C5 N2 121.7(5) . . ? N1 C5 N2 115.7(5) . . ? N2 C6 C7 111.4(4) . . ? N2 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? N2 C6 H6B 109.4 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C8 C7 C6 111.7(5) . . ? C8 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? C8 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? O3 C8 O4 122.9(5) . . ? O3 C8 C7 119.9(5) . . ? O4 C8 C7 117.1(5) . . ? O9 C9 N3 122.1(5) . . ? O9 C9 N2 122.1(5) . . ? N3 C9 N2 115.7(5) . . ? N3 C10 C11 110.4(4) . . ? N3 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N3 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C12 C11 C10 115.2(5) . . ? C12 C11 H11A 108.5 . . ? C10 C11 H11A 108.5 . . ? C12 C11 H11B 108.5 . . ? C10 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? O6 C12 O5 122.7(5) . . ? O6 C12 C11 119.5(5) . . ? O5 C12 C11 117.8(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 O5 Zn1 O1 C1 -25.4(5) 2_556 . . . ? O4 Zn1 O1 C1 97.6(5) 2_656 . . . ? O6 Zn1 O1 C1 -146.7(5) 2_566 . . . ? O10 Zn1 O1 C1 -162.8(13) . . . . ? Na1 Zn1 O1 C1 13.4(5) 1_545 . . . ? O5 Zn1 O1 Na1 -146.85(14) 2_556 . . . ? O4 Zn1 O1 Na1 -23.86(17) 2_656 . . . ? O6 Zn1 O1 Na1 91.84(16) 2_566 . . . ? O10 Zn1 O1 Na1 75.7(14) . . . . ? Na1 Zn1 O1 Na1 -108.05(13) 1_545 . . . ? O2 Na1 O1 C1 87.3(4) 1_565 . . . ? O3 Na1 O1 C1 -153.0(5) 2_666 . . . ? O8 Na1 O1 C1 -21.6(4) 2_656 . . . ? O4 Na1 O1 C1 -107.3(4) 2_656 . . . ? O5 Na1 O1 C1 168.9(4) 2_566 . . . ? Zn1 Na1 O1 C1 152.0(4) 1_565 . . . ? O2 Na1 O1 Zn1 -146.15(18) 1_565 . . . ? O3 Na1 O1 Zn1 -26.5(5) 2_666 . . . ? O8 Na1 O1 Zn1 104.95(16) 2_656 . . . ? O4 Na1 O1 Zn1 19.28(14) 2_656 . . . ? O5 Na1 O1 Zn1 -64.49(15) 2_566 . . . ? Zn1 Na1 O1 Zn1 -81.46(14) 1_565 . . . ? Na1 O2 C1 O1 18.7(12) 1_545 . . . ? Na1 O2 C1 C2 -161.4(6) 1_545 . . . ? Zn1 O1 C1 O2 -22.3(9) . . . . ? Na1 O1 C1 O2 84.0(8) . . . . ? Zn1 O1 C1 C2 157.7(5) . . . . ? Na1 O1 C1 C2 -95.9(6) . . . . ? O2 C1 C2 C3 -9.2(10) . . . . ? O1 C1 C2 C3 170.8(6) . . . . ? C5 N1 C3 C2 93.7(7) . . . . ? C4 N1 C3 C2 -87.8(6) . . . . ? C1 C2 C3 N1 159.7(5) . . . . ? C5 N1 C4 O7 -179.4(6) . . . . ? C3 N1 C4 O7 2.1(8) . . . . ? C5 N1 C4 N3 1.1(8) . . . . ? C3 N1 C4 N3 -177.4(5) . . . . ? C9 N3 C4 O7 -179.0(6) . . . . ? C10 N3 C4 O7 2.7(8) . . . . ? C9 N3 C4 N1 0.4(8) . . . . ? C10 N3 C4 N1 -177.8(5) . . . . ? Na1 O8 C5 N1 136.0(6) 2_656 . . . ? Na1 O8 C5 N2 -43.6(10) 2_656 . . . ? C4 N1 C5 O8 179.0(5) . . . . ? C3 N1 C5 O8 -2.6(8) . . . . ? C4 N1 C5 N2 -1.4(8) . . . . ? C3 N1 C5 N2 177.0(5) . . . . ? C9 N2 C5 O8 179.9(5) . . . . ? C6 N2 C5 O8 5.8(8) . . . . ? C9 N2 C5 N1 0.3(7) . . . . ? C6 N2 C5 N1 -173.8(5) . . . . ? C5 N2 C6 C7 95.3(6) . . . . ? C9 N2 C6 C7 -79.2(6) . . . . ? N2 C6 C7 C8 -58.7(6) . . . . ? Na1 O3 C8 O4 17.3(13) 2_646 . . . ? Na1 O3 C8 C7 -160.2(6) 2_646 . . . ? Zn1 O4 C8 O3 10.9(8) 2_656 . . . ? Na1 O4 C8 O3 -94.6(6) 2_656 . . . ? Zn1 O4 C8 C7 -171.6(4) 2_656 . . . ? Na1 O4 C8 C7 83.0(5) 2_656 . . . ? C6 C7 C8 O3 91.5(7) . . . . ? C6 C7 C8 O4 -86.1(6) . . . . ? C4 N3 C9 O9 179.5(5) . . . . ? C10 N3 C9 O9 -2.3(8) . . . . ? C4 N3 C9 N2 -1.4(7) . . . . ? C10 N3 C9 N2 176.9(5) . . . . ? C5 N2 C9 O9 -179.8(5) . . . . ? C6 N2 C9 O9 -5.7(8) . . . . ? C5 N2 C9 N3 1.0(7) . . . . ? C6 N2 C9 N3 175.2(4) . . . . ? C9 N3 C10 C11 -72.8(6) . . . . ? C4 N3 C10 C11 105.5(6) . . . . ? N3 C10 C11 C12 -172.6(5) . . . . ? Zn1 O6 C12 O5 -11.1(7) 2_546 . . . ? Zn1 O6 C12 C11 169.1(4) 2_546 . . . ? Zn1 O5 C12 O6 -167.4(4) 2_556 . . . ? Na1 O5 C12 O6 34.2(8) 2_546 . . . ? Zn1 O5 C12 C11 12.5(7) 2_556 . . . ? Na1 O5 C12 C11 -145.9(4) 2_546 . . . ? C10 C11 C12 O6 -5.8(8) . . . . ? C10 C11 C12 O5 174.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.892 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.141 #===end data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H36 N6 O26 Zn5' _chemical_formula_weight 1151.44 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 P21/c 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 5.5807(11) _cell_length_b 13.793(3) _cell_length_c 24.064(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.91(3) _cell_angle_gamma 90.00 _cell_volume 1842.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5845 _cell_measurement_theta_min 2.2529 _cell_measurement_theta_max 29.2406 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 3.317 _exptl_absorpt_correction_type 'None' _exptl_absorpt_correction_T_min 0.0000 _exptl_absorpt_correction_T_max 0.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724 (4x4 bin mode) ; _diffrn_measurement_method 'dtprofit.ref' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16302 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 29.25 _reflns_number_total 4854 _reflns_number_gt 4082 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0763P)^2^+4.4033P] 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 4854 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1580 _refine_ls_wR_factor_gt 0.1338 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 1.00171(9) 0.42378(4) 0.44983(2) 0.02220(16) Uani 1 1 d . . . Zn2 Zn 0.5000 0.5000 0.5000 0.02153(19) Uani 1 2 d S . . Zn3 Zn 1.30894(10) 0.24723(4) 0.50589(2) 0.02420(16) Uani 1 1 d . . . O1 O 0.7152(8) 0.4701(3) 0.20905(16) 0.0404(10) Uani 1 1 d . . . O2 O 0.3624(7) 0.3357(3) 0.35258(15) 0.0349(9) Uani 1 1 d . . . O3 O 0.9207(7) 0.1655(3) 0.26715(17) 0.0380(9) Uani 1 1 d . . . O4 O 0.8674(6) 0.2799(3) 0.42519(15) 0.0289(7) Uani 1 1 d . . . O5 O 1.1451(7) 0.1647(3) 0.44599(15) 0.0308(8) Uani 1 1 d . . . O6 O 0.8680(7) 0.4806(3) 0.37895(14) 0.0315(8) Uani 1 1 d . . . O7 O 1.1698(5) 0.5597(2) 0.48370(13) 0.0205(6) Uani 1 1 d . . . O8 O 1.3384(5) 0.3713(2) 0.46607(13) 0.0199(6) Uani 1 1 d . . . O9 O 1.6182(6) 0.1771(3) 0.51744(15) 0.0319(8) Uani 1 1 d . . . O10 O 1.0590(7) 0.2438(3) 0.05716(15) 0.0317(8) Uani 1 1 d . . . O11 O 0.5701(7) 0.5534(3) 0.41881(14) 0.0319(8) Uani 1 1 d . . . O16 O 1.3310(7) 0.3058(4) 0.12072(18) 0.0508(12) Uani 1 1 d . . . N1 N 0.6397(8) 0.2467(3) 0.31110(16) 0.0233(8) Uani 1 1 d . . . N2 N 0.8385(8) 0.3203(3) 0.24095(16) 0.0262(8) Uani 1 1 d . . . N3 N 0.5398(7) 0.4058(3) 0.28164(16) 0.0241(8) Uani 1 1 d . . . C1 C 0.5081(9) 0.3299(4) 0.31839(19) 0.0244(9) Uani 1 1 d . . . C2 C 0.8088(9) 0.2390(3) 0.2731(2) 0.0258(10) Uani 1 1 d . . . C3 C 0.6999(9) 0.4033(4) 0.24155(19) 0.0277(10) Uani 1 1 d . . . C4 C 0.4152(10) 0.4987(4) 0.2904(2) 0.0302(11) Uani 1 1 d . . . H4A H 0.2804 0.4868 0.3119 0.036 Uiso 1 1 calc R . . H4B H 0.3522 0.5251 0.2545 0.036 Uiso 1 1 calc R . . C5 C 0.5842(9) 0.5721(3) 0.32097(19) 0.0263(10) Uani 1 1 d . . . H5A H 0.4983 0.6323 0.3254 0.032 Uiso 1 1 calc R . . H5B H 0.7171 0.5855 0.2991 0.032 Uiso 1 1 calc R . . C6 C 0.6810(9) 0.5338(3) 0.3778(2) 0.0242(9) Uani 1 1 d . . . C7 C 0.5974(9) 0.1617(4) 0.3462(2) 0.0270(10) Uani 1 1 d . . . H7A H 0.5310 0.1098 0.3221 0.032 Uiso 1 1 calc R . . H7B H 0.4773 0.1789 0.3709 0.032 Uiso 1 1 calc R . . C8 C 0.8182(10) 0.1239(4) 0.3812(2) 0.0311(11) Uani 1 1 d . . . H8A H 0.7701 0.0699 0.4034 0.037 Uiso 1 1 calc R . . H8B H 0.9295 0.0989 0.3563 0.037 Uiso 1 1 calc R . . C9 C 0.9504(9) 0.1968(3) 0.42000(19) 0.0236(9) Uani 1 1 d . . . C10 C 1.0268(9) 0.3168(4) 0.2023(2) 0.0299(11) Uani 1 1 d . . . H10A H 1.1660 0.2827 0.2202 0.036 Uiso 1 1 calc R . . H10B H 1.0764 0.3824 0.1945 0.036 Uiso 1 1 calc R . . C11 C 1.1294(9) 0.2747(4) 0.1073(2) 0.0280(10) Uani 1 1 d . . . C13 C 0.9425(9) 0.2672(4) 0.1483(2) 0.0286(10) Uani 1 1 d . . . H13A H 0.7935 0.2968 0.1322 0.034 Uiso 1 1 calc R . . H13B H 0.9106 0.1995 0.1554 0.034 Uiso 1 1 calc R . . O15 O 0.6680(10) 0.4806(3) 0.0818(2) 0.0575(13) 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 0.0193(3) 0.0258(3) 0.0214(3) -0.0029(2) 0.0018(2) 0.0020(2) Zn2 0.0166(4) 0.0229(4) 0.0254(4) -0.0030(3) 0.0036(3) -0.0011(3) Zn3 0.0237(3) 0.0257(3) 0.0237(3) 0.0030(2) 0.0046(2) 0.0001(2) O1 0.059(3) 0.036(2) 0.0285(19) 0.0098(16) 0.0153(18) 0.0056(19) O2 0.040(2) 0.035(2) 0.0319(19) 0.0016(15) 0.0148(17) 0.0078(17) O3 0.048(2) 0.0309(19) 0.037(2) -0.0036(16) 0.0141(18) 0.0069(17) O4 0.0297(19) 0.0241(17) 0.0323(19) -0.0059(14) 0.0008(15) -0.0019(14) O5 0.033(2) 0.0277(18) 0.0298(19) -0.0040(14) -0.0040(15) 0.0026(15) O6 0.035(2) 0.0350(19) 0.0237(17) -0.0015(14) -0.0004(15) 0.0106(16) O7 0.0167(15) 0.0233(15) 0.0222(15) -0.0020(12) 0.0053(12) -0.0007(12) O8 0.0209(15) 0.0184(14) 0.0206(15) -0.0009(11) 0.0039(12) -0.0023(12) O9 0.0243(18) 0.038(2) 0.0335(19) 0.0081(16) 0.0023(15) 0.0033(15) O10 0.0318(19) 0.043(2) 0.0213(17) -0.0034(14) 0.0083(14) 0.0030(16) O11 0.034(2) 0.042(2) 0.0214(17) 0.0054(15) 0.0090(15) 0.0060(16) O16 0.030(2) 0.084(3) 0.040(2) -0.015(2) 0.0131(18) -0.013(2) N1 0.028(2) 0.0214(18) 0.0206(18) -0.0001(14) 0.0051(16) -0.0014(15) N2 0.032(2) 0.029(2) 0.0190(18) -0.0014(16) 0.0052(16) 0.0004(17) N3 0.030(2) 0.026(2) 0.0166(18) 0.0023(15) 0.0013(16) 0.0030(16) C1 0.024(2) 0.029(2) 0.019(2) -0.0028(18) -0.0026(18) -0.0002(19) C2 0.026(2) 0.028(2) 0.024(2) -0.0011(18) 0.0019(19) 0.0017(19) C3 0.035(3) 0.030(2) 0.019(2) -0.0025(18) 0.003(2) 0.001(2) C4 0.033(3) 0.032(3) 0.025(2) 0.0051(19) -0.001(2) 0.008(2) C5 0.034(3) 0.026(2) 0.019(2) 0.0027(17) 0.0033(19) 0.004(2) C6 0.026(2) 0.020(2) 0.026(2) -0.0005(17) 0.0011(19) -0.0013(18) C7 0.031(3) 0.026(2) 0.023(2) 0.0001(18) 0.0000(19) -0.006(2) C8 0.047(3) 0.022(2) 0.023(2) -0.0002(18) 0.000(2) -0.002(2) C9 0.026(2) 0.024(2) 0.021(2) 0.0029(17) 0.0059(18) -0.0018(18) C10 0.030(3) 0.036(3) 0.024(2) -0.004(2) 0.005(2) -0.004(2) C11 0.029(3) 0.032(2) 0.025(2) 0.0016(19) 0.009(2) 0.002(2) C13 0.025(2) 0.038(3) 0.023(2) -0.003(2) 0.0064(19) -0.001(2) O15 0.081(4) 0.036(2) 0.056(3) -0.008(2) 0.013(3) -0.014(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 O7 1.960(3) 3_766 ? Zn1 O6 1.954(4) . ? Zn1 O8 2.014(3) . ? Zn1 O4 2.181(3) . ? Zn1 O7 2.214(3) . ? Zn1 Zn2 3.0991(9) 1_655 ? Zn2 O7 2.020(3) 1_455 ? Zn2 O7 2.020(3) 3_766 ? Zn2 O8 2.117(3) 1_455 ? Zn2 O8 2.117(3) 3_766 ? Zn2 O11 2.161(3) . ? Zn2 O11 2.161(3) 3_666 ? Zn2 Zn1 3.0991(9) 1_455 ? Zn2 Zn1 3.0991(9) 3_766 ? Zn3 O10 1.959(4) 4_566 ? Zn3 O8 1.976(3) . ? Zn3 O9 1.973(4) . ? Zn3 O5 1.985(4) . ? O1 C3 1.218(6) . ? O2 C1 1.217(6) . ? O3 C2 1.208(6) . ? O4 C9 1.248(6) . ? O5 C9 1.276(6) . ? O6 C6 1.273(6) . ? O7 Zn1 1.960(3) 3_766 ? O7 Zn2 2.020(3) 1_655 ? O8 Zn2 2.117(3) 1_655 ? O10 C11 1.303(6) . ? O10 Zn3 1.959(3) 4_565 ? O11 C6 1.248(6) . ? O16 C11 1.216(7) . ? N1 C2 1.385(6) . ? N1 C1 1.383(6) . ? N1 C7 1.478(6) . ? N2 C3 1.381(6) . ? N2 C2 1.382(6) . ? N2 C10 1.474(6) . ? N3 C3 1.381(6) . ? N3 C1 1.394(6) . ? N3 C4 1.483(6) . ? C4 C5 1.521(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.513(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C7 C8 1.512(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.512(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 C13 1.502(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C13 1.510(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Zn1 O6 119.42(14) 3_766 . ? O7 Zn1 O8 114.05(13) 3_766 . ? O6 Zn1 O8 125.33(14) . . ? O7 Zn1 O4 98.30(13) 3_766 . ? O6 Zn1 O4 92.19(15) . . ? O8 Zn1 O4 90.76(13) . . ? O7 Zn1 O7 79.93(13) 3_766 . ? O6 Zn1 O7 95.20(14) . . ? O8 Zn1 O7 83.21(12) . . ? O4 Zn1 O7 172.30(13) . . ? O7 Zn1 Zn2 97.85(10) 3_766 1_655 ? O6 Zn1 Zn2 116.78(12) . 1_655 ? O8 Zn1 Zn2 42.66(9) . 1_655 ? O4 Zn1 Zn2 133.14(10) . 1_655 ? O7 Zn1 Zn2 40.56(8) . 1_655 ? O7 Zn2 O7 180.000(1) 1_455 3_766 ? O7 Zn2 O8 85.61(12) 1_455 1_455 ? O7 Zn2 O8 94.39(12) 3_766 1_455 ? O7 Zn2 O8 94.39(12) 1_455 3_766 ? O7 Zn2 O8 85.61(12) 3_766 3_766 ? O8 Zn2 O8 180.00(16) 1_455 3_766 ? O7 Zn2 O11 86.10(13) 1_455 . ? O7 Zn2 O11 93.90(13) 3_766 . ? O8 Zn2 O11 92.67(13) 1_455 . ? O8 Zn2 O11 87.33(13) 3_766 . ? O7 Zn2 O11 93.90(13) 1_455 3_666 ? O7 Zn2 O11 86.10(13) 3_766 3_666 ? O8 Zn2 O11 87.33(13) 1_455 3_666 ? O8 Zn2 O11 92.67(13) 3_766 3_666 ? O11 Zn2 O11 180.000(1) . 3_666 ? O7 Zn2 Zn1 45.46(9) 1_455 1_455 ? O7 Zn2 Zn1 134.54(9) 3_766 1_455 ? O8 Zn2 Zn1 40.15(8) 1_455 1_455 ? O8 Zn2 Zn1 139.85(8) 3_766 1_455 ? O11 Zn2 Zn1 90.12(11) . 1_455 ? O11 Zn2 Zn1 89.88(11) 3_666 1_455 ? O7 Zn2 Zn1 134.54(9) 1_455 3_766 ? O7 Zn2 Zn1 45.46(9) 3_766 3_766 ? O8 Zn2 Zn1 139.85(8) 1_455 3_766 ? O8 Zn2 Zn1 40.15(8) 3_766 3_766 ? O11 Zn2 Zn1 89.88(11) . 3_766 ? O11 Zn2 Zn1 90.12(11) 3_666 3_766 ? Zn1 Zn2 Zn1 180.00(2) 1_455 3_766 ? O10 Zn3 O8 110.56(14) 4_566 . ? O10 Zn3 O9 127.69(16) 4_566 . ? O8 Zn3 O9 112.18(14) . . ? O10 Zn3 O5 100.88(16) 4_566 . ? O8 Zn3 O5 101.53(14) . . ? O9 Zn3 O5 98.74(16) . . ? C9 O4 Zn1 138.0(3) . . ? C9 O5 Zn3 117.5(3) . . ? C6 O6 Zn1 119.3(3) . . ? Zn1 O7 Zn2 113.65(16) 3_766 1_655 ? Zn1 O7 Zn1 100.07(13) 3_766 . ? Zn2 O7 Zn1 93.98(13) 1_655 . ? Zn3 O8 Zn1 106.43(14) . . ? Zn3 O8 Zn2 126.34(16) . 1_655 ? Zn1 O8 Zn2 97.19(13) . 1_655 ? C11 O10 Zn3 113.4(3) . 4_565 ? C6 O11 Zn2 142.4(3) . . ? C2 N1 C1 123.7(4) . . ? C2 N1 C7 118.5(4) . . ? C1 N1 C7 117.9(4) . . ? C3 N2 C2 124.5(4) . . ? C3 N2 C10 118.1(4) . . ? C2 N2 C10 117.4(4) . . ? C3 N3 C1 123.9(4) . . ? C3 N3 C4 117.9(4) . . ? C1 N3 C4 117.8(4) . . ? O2 C1 N3 121.1(4) . . ? O2 C1 N1 122.8(4) . . ? N3 C1 N1 116.0(4) . . ? O3 C2 N1 122.6(5) . . ? O3 C2 N2 121.5(5) . . ? N1 C2 N2 115.9(4) . . ? O1 C3 N2 122.9(5) . . ? O1 C3 N3 121.5(5) . . ? N2 C3 N3 115.6(4) . . ? N3 C4 C5 111.6(4) . . ? N3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? N3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 110.5(4) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? O11 C6 O6 125.4(5) . . ? O11 C6 C5 118.7(4) . . ? O6 C6 C5 115.9(4) . . ? N1 C7 C8 115.0(4) . . ? N1 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? N1 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C9 C8 C7 115.6(4) . . ? C9 C8 H8A 108.4 . . ? C7 C8 H8A 108.4 . . ? C9 C8 H8B 108.4 . . ? C7 C8 H8B 108.4 . . ? H8A C8 H8B 107.4 . . ? O4 C9 O5 125.2(4) . . ? O4 C9 C8 120.7(4) . . ? O5 C9 C8 114.1(4) . . ? N2 C10 C13 112.4(4) . . ? N2 C10 H10A 109.1 . . ? C13 C10 H10A 109.1 . . ? N2 C10 H10B 109.1 . . ? C13 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? O16 C11 O10 122.9(5) . . ? O16 C11 C13 122.3(5) . . ? O10 C11 C13 114.8(4) . . ? C10 C13 C11 111.0(4) . . ? C10 C13 H13A 109.4 . . ? C11 C13 H13A 109.4 . . ? C10 C13 H13B 109.4 . . ? C11 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? 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 Zn1 O4 C9 -116.8(5) 3_766 . . . ? O6 Zn1 O4 C9 123.1(5) . . . . ? O8 Zn1 O4 C9 -2.3(5) . . . . ? O7 Zn1 O4 C9 -40.6(12) . . . . ? Zn2 Zn1 O4 C9 -7.7(5) 1_655 . . . ? O10 Zn3 O5 C9 60.7(4) 4_566 . . . ? O8 Zn3 O5 C9 -53.1(4) . . . . ? O9 Zn3 O5 C9 -168.0(3) . . . . ? O7 Zn1 O6 C6 5.2(4) 3_766 . . . ? O8 Zn1 O6 C6 -161.5(3) . . . . ? O4 Zn1 O6 C6 106.0(4) . . . . ? O7 Zn1 O6 C6 -76.1(4) . . . . ? Zn2 Zn1 O6 C6 -112.2(4) 1_655 . . . ? O7 Zn1 O7 Zn1 0.0 3_766 . . 3_766 ? O6 Zn1 O7 Zn1 119.00(15) . . . 3_766 ? O8 Zn1 O7 Zn1 -115.97(15) . . . 3_766 ? O4 Zn1 O7 Zn1 -77.4(9) . . . 3_766 ? Zn2 Zn1 O7 Zn1 -114.89(18) 1_655 . . 3_766 ? O7 Zn1 O7 Zn2 114.89(18) 3_766 . . 1_655 ? O6 Zn1 O7 Zn2 -126.12(14) . . . 1_655 ? O8 Zn1 O7 Zn2 -1.09(12) . . . 1_655 ? O4 Zn1 O7 Zn2 37.5(9) . . . 1_655 ? O10 Zn3 O8 Zn1 -37.72(19) 4_566 . . . ? O9 Zn3 O8 Zn1 173.18(14) . . . . ? O5 Zn3 O8 Zn1 68.67(17) . . . . ? O10 Zn3 O8 Zn2 74.5(2) 4_566 . . 1_655 ? O9 Zn3 O8 Zn2 -74.6(2) . . . 1_655 ? O5 Zn3 O8 Zn2 -179.07(18) . . . 1_655 ? O7 Zn1 O8 Zn3 56.57(18) 3_766 . . . ? O6 Zn1 O8 Zn3 -136.10(16) . . . . ? O4 Zn1 O8 Zn3 -42.88(15) . . . . ? O7 Zn1 O8 Zn3 132.33(15) . . . . ? Zn2 Zn1 O8 Zn3 131.29(19) 1_655 . . . ? O7 Zn1 O8 Zn2 -74.72(15) 3_766 . . 1_655 ? O6 Zn1 O8 Zn2 92.61(18) . . . 1_655 ? O4 Zn1 O8 Zn2 -174.17(13) . . . 1_655 ? O7 Zn1 O8 Zn2 1.04(11) . . . 1_655 ? O7 Zn2 O11 C6 -146.2(6) 1_455 . . . ? O7 Zn2 O11 C6 33.8(6) 3_766 . . . ? O8 Zn2 O11 C6 -60.8(6) 1_455 . . . ? O8 Zn2 O11 C6 119.2(6) 3_766 . . . ? O11 Zn2 O11 C6 76.7(14) 3_666 . . . ? Zn1 Zn2 O11 C6 -100.8(6) 1_455 . . . ? Zn1 Zn2 O11 C6 79.2(6) 3_766 . . . ? C3 N3 C1 O2 -179.3(5) . . . . ? C4 N3 C1 O2 8.1(7) . . . . ? C3 N3 C1 N1 -3.2(7) . . . . ? C4 N3 C1 N1 -175.9(4) . . . . ? C2 N1 C1 O2 -179.0(5) . . . . ? C7 N1 C1 O2 0.7(7) . . . . ? C2 N1 C1 N3 5.0(7) . . . . ? C7 N1 C1 N3 -175.3(4) . . . . ? C1 N1 C2 O3 -179.5(5) . . . . ? C7 N1 C2 O3 0.8(7) . . . . ? C1 N1 C2 N2 -1.1(7) . . . . ? C7 N1 C2 N2 179.2(4) . . . . ? C3 N2 C2 O3 173.2(5) . . . . ? C10 N2 C2 O3 -5.0(7) . . . . ? C3 N2 C2 N1 -5.3(7) . . . . ? C10 N2 C2 N1 176.5(4) . . . . ? C2 N2 C3 O1 -172.9(5) . . . . ? C10 N2 C3 O1 5.3(7) . . . . ? C2 N2 C3 N3 6.9(7) . . . . ? C10 N2 C3 N3 -174.9(4) . . . . ? C1 N3 C3 O1 177.4(5) . . . . ? C4 N3 C3 O1 -9.9(7) . . . . ? C1 N3 C3 N2 -2.4(7) . . . . ? C4 N3 C3 N2 170.3(4) . . . . ? C3 N3 C4 C5 -73.7(5) . . . . ? C1 N3 C4 C5 99.4(5) . . . . ? N3 C4 C5 C6 -60.3(5) . . . . ? Zn2 O11 C6 O6 -24.9(9) . . . . ? Zn2 O11 C6 C5 152.6(4) . . . . ? Zn1 O6 C6 O11 -0.4(7) . . . . ? Zn1 O6 C6 C5 -178.0(3) . . . . ? C4 C5 C6 O11 -91.8(5) . . . . ? C4 C5 C6 O6 85.9(5) . . . . ? C2 N1 C7 C8 57.2(6) . . . . ? C1 N1 C7 C8 -122.5(5) . . . . ? N1 C7 C8 C9 56.2(6) . . . . ? Zn1 O4 C9 O5 24.9(8) . . . . ? Zn1 O4 C9 C8 -155.9(4) . . . . ? Zn3 O5 C9 O4 7.7(6) . . . . ? Zn3 O5 C9 C8 -171.5(3) . . . . ? C7 C8 C9 O4 5.5(7) . . . . ? C7 C8 C9 O5 -175.3(4) . . . . ? C3 N2 C10 C13 -95.7(5) . . . . ? C2 N2 C10 C13 82.6(6) . . . . ? Zn3 O10 C11 O16 -0.1(7) 4_565 . . . ? Zn3 O10 C11 C13 -178.9(3) 4_565 . . . ? N2 C10 C13 C11 173.7(4) . . . . ? O16 C11 C13 C10 9.1(8) . . . . ? O10 C11 C13 C10 -172.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 29.25 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.913 _refine_diff_density_min -1.153 _refine_diff_density_rms 0.293 #===end data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 N10 O24 Zn3' _chemical_formula_weight 1349.11 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 P21/c 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 25.826(5) _cell_length_b 7.7641(16) _cell_length_c 36.021(11) _cell_angle_alpha 90.00 _cell_angle_beta 132.767(18) _cell_angle_gamma 90.00 _cell_volume 5302(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9863 _cell_measurement_theta_min 1.7207 _cell_measurement_theta_max 27.8764 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 1.444 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.6425 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724 (4x4 bin mode) ; _diffrn_measurement_method 'dtprofit.ref' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 35093 _diffrn_reflns_av_R_equivalents 0.0953 _diffrn_reflns_av_sigmaI/netI 0.1015 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9264 _reflns_number_gt 6721 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.2310P)^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 9264 _refine_ls_number_parameters 768 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1474 _refine_ls_R_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.3553 _refine_ls_wR_factor_gt 0.2892 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.35289(5) 0.72635(14) 0.84587(4) 0.0301(3) Uani 1 1 d . . . Zn2 Zn 0.26216(5) 0.35219(13) 0.77647(4) 0.0315(4) Uani 1 1 d . . . Zn3 Zn 0.88089(6) 0.68731(15) 1.02207(4) 0.0385(4) Uani 1 1 d . . . O1 O 0.7471(4) 0.3469(12) 0.8932(3) 0.057(2) Uani 1 1 d . . . O2 O 0.5195(4) 0.5027(13) 0.7634(3) 0.065(2) Uani 1 1 d . . . O3 O 0.5821(4) 0.2219(12) 0.8991(3) 0.058(2) Uani 1 1 d . . . O4 O 0.8567(4) 0.4417(10) 1.0236(3) 0.055(2) Uani 1 1 d . . . O5 O 0.7619(5) 0.6042(12) 0.9775(4) 0.073(3) Uani 1 1 d . . . O6 O 0.0633(4) 1.1631(10) 0.6728(3) 0.0457(18) Uani 1 1 d . . . O7 O -0.1460(4) 1.1634(9) 0.6305(3) 0.0476(19) Uani 1 1 d . . . O8 O 0.0270(4) 0.8037(10) 0.7522(3) 0.055(2) Uani 1 1 d . . . O9 O 0.2482(3) 0.7635(8) 0.7996(2) 0.0327(15) Uani 1 1 d . . . O10 O 0.2116(3) 0.5725(8) 0.7392(2) 0.0359(15) Uani 1 1 d . . . O11 O 0.1965(3) 0.2120(9) 0.7103(2) 0.0379(16) Uani 1 1 d . . . H11 H 0.1585 0.1970 0.7022 0.057 Uiso 1 1 calc R . . O12 O 0.3189(4) 0.1353(9) 0.8223(3) 0.0490(19) Uani 1 1 d . . . H12 H 0.3084 0.1141 0.8388 0.073 Uiso 1 1 calc R . . O13 O 0.3661(3) 0.4869(9) 0.8330(3) 0.0388(16) Uani 1 1 d . . . O14 O 0.3391(3) 0.3594(10) 0.7685(2) 0.0429(17) Uani 1 1 d . . . O15 O -0.2527(4) 0.6376(9) 0.6452(3) 0.0465(18) Uani 1 1 d . . . O16 O -0.2064(4) 0.8513(9) 0.7014(3) 0.0439(17) Uani 1 1 d . . . O17 O 0.6345(5) 0.3363(12) 0.6989(3) 0.063(2) Uani 1 1 d . . . O18 O 0.7355(5) 0.4322(10) 0.7738(3) 0.059(2) Uani 1 1 d . . . O19 O -0.1152(4) 1.5980(10) 0.5530(3) 0.054(2) Uani 1 1 d . . . O20 O -0.0497(5) 1.7805(10) 0.6167(3) 0.070(3) Uani 1 1 d . . . N1 N -0.0402(4) 1.1754(9) 0.6529(3) 0.0287(16) Uani 1 1 d . . . N2 N -0.0595(4) 0.9843(10) 0.6925(3) 0.0298(16) Uani 1 1 d . . . N3 N 0.0503(4) 0.9869(9) 0.7165(3) 0.0283(16) Uani 1 1 d . . . N4 N 0.3592(4) 0.6651(10) 0.9075(3) 0.0322(17) Uani 1 1 d . . . N5 N 0.4533(4) 0.8229(10) 0.9097(3) 0.0355(18) Uani 1 1 d . . . N6 N 0.5487(4) 0.3618(11) 0.8311(3) 0.0338(19) Uani 1 1 d . . . N7 N 0.6342(4) 0.4316(11) 0.8286(3) 0.0395(19) Uani 1 1 d . . . N8 N 0.6672(4) 0.2857(11) 0.8989(3) 0.0361(19) Uani 1 1 d . . . N9 N 0.8454(5) 0.7802(11) 0.9537(3) 0.042(2) Uani 1 1 d . . . N10 N 0.9750(5) 0.6707(10) 1.0379(3) 0.0367(19) Uani 1 1 d . . . C1 C 0.7816(6) 0.8308(16) 0.9118(4) 0.055(3) Uani 1 1 d . . . H1 H 0.7439 0.8193 0.9098 0.066 Uiso 1 1 calc R . . C2 C 0.7693(7) 0.9006(16) 0.8708(4) 0.058(3) Uani 1 1 d . . . H2 H 0.7238 0.9318 0.8417 0.069 Uiso 1 1 calc R . . C3 C 0.8227(7) 0.9229(16) 0.8729(4) 0.062(4) Uani 1 1 d . . . H3 H 0.8145 0.9742 0.8460 0.075 Uiso 1 1 calc R . . C4 C 0.8913(6) 0.8687(13) 0.9159(4) 0.045(3) Uani 1 1 d . . . C5 C 0.9006(6) 0.7953(12) 0.9559(4) 0.037(2) Uani 1 1 d . . . C6 C 0.9533(9) 0.8813(16) 0.9218(6) 0.064(4) Uani 1 1 d . . . H6 H 0.9485 0.9280 0.8959 0.077 Uiso 1 1 calc R . . C7 C 1.0156(8) 0.8273(15) 0.9635(6) 0.062(4) Uani 1 1 d . . . H7 H 1.0538 0.8394 0.9661 0.075 Uiso 1 1 calc R . . C8 C 1.0275(6) 0.7520(13) 1.0045(4) 0.044(3) Uani 1 1 d . . . C9 C 0.9686(5) 0.7366(12) 1.0011(4) 0.036(2) Uani 1 1 d . . . C10 C 1.0902(6) 0.6939(16) 1.0475(5) 0.057(3) Uani 1 1 d . . . H10 H 1.1296 0.7008 1.0514 0.069 Uiso 1 1 calc R . . C11 C 1.0968(6) 0.6252(14) 1.0855(5) 0.057(3) Uani 1 1 d . . . H11A H 1.1401 0.5841 1.1148 0.068 Uiso 1 1 calc R . . C12 C 1.0377(6) 0.6177(15) 1.0795(4) 0.051(3) Uani 1 1 d . . . H12A H 1.0426 0.5738 1.1057 0.061 Uiso 1 1 calc R . . C13 C 0.7927(6) 0.4649(15) 0.9988(4) 0.045(3) Uani 1 1 d . . . C14 C 0.7499(6) 0.3094(18) 0.9933(4) 0.056(3) Uani 1 1 d . . . H14A H 0.7804 0.2390 1.0236 0.067 Uiso 1 1 calc R . . H14B H 0.7117 0.3515 0.9901 0.067 Uiso 1 1 calc R . . C15 C 0.7193(6) 0.1977(15) 0.9467(4) 0.047(3) Uani 1 1 d . . . H15A H 0.7576 0.1604 0.9494 0.057 Uiso 1 1 calc R . . H15B H 0.6979 0.0955 0.9470 0.057 Uiso 1 1 calc R . . C16 C 0.6873(5) 0.3518(13) 0.8755(4) 0.038(2) Uani 1 1 d . . . C17 C 0.5655(6) 0.4373(16) 0.8054(4) 0.047(3) Uani 1 1 d . . . C18 C 0.5980(6) 0.2845(13) 0.8781(4) 0.042(3) Uani 1 1 d . . . C19 C 0.4739(6) 0.3477(15) 0.8065(4) 0.045(3) Uani 1 1 d . . . H19A H 0.4642 0.2304 0.8095 0.054 Uiso 1 1 calc R . . H19B H 0.4434 0.3743 0.7708 0.054 Uiso 1 1 calc R . . C20 C 0.4576(5) 0.4690(13) 0.8302(4) 0.038(2) Uani 1 1 d . . . H20A H 0.4617 0.5872 0.8238 0.045 Uiso 1 1 calc R . . H20B H 0.4912 0.4514 0.8665 0.045 Uiso 1 1 calc R . . C21 C 0.3827(5) 0.4360(12) 0.8079(4) 0.036(2) Uani 1 1 d . . . C22 C -0.2086(5) 0.7567(12) 0.6720(3) 0.031(2) Uani 1 1 d . . . C23 C -0.1552(5) 0.7889(13) 0.6682(4) 0.040(2) Uani 1 1 d . . . H23A H -0.1795 0.8172 0.6335 0.048 Uiso 1 1 calc R . . H23B H -0.1285 0.6841 0.6770 0.048 Uiso 1 1 calc R . . C24 C 0.2005(5) 0.6964(12) 0.7562(3) 0.031(2) Uani 1 1 d . . . C25 C 0.1298(6) 0.7757(13) 0.7243(4) 0.043(2) Uani 1 1 d . . . H25A H 0.1168 0.8164 0.6934 0.051 Uiso 1 1 calc R . . H25B H 0.0964 0.6868 0.7148 0.051 Uiso 1 1 calc R . . C26 C 0.1222(4) 0.9198(12) 0.7468(3) 0.030(2) Uani 1 1 d . . . H26A H 0.1394 0.8825 0.7792 0.037 Uiso 1 1 calc R . . H26B H 0.1523 1.0133 0.7532 0.037 Uiso 1 1 calc R . . C27 C 0.0269(5) 1.1126(12) 0.6804(3) 0.031(2) Uani 1 1 d . . . C28 C -0.0858(4) 1.1125(11) 0.6569(3) 0.0261(18) Uani 1 1 d . . . C29 C 0.0061(5) 0.9137(11) 0.7214(3) 0.031(2) Uani 1 1 d . . . C30 C 0.3105(5) 0.5921(12) 0.9050(4) 0.036(2) Uani 1 1 d . . . H30 H 0.2653 0.5761 0.8736 0.044 Uiso 1 1 calc R . . C31 C 0.3256(6) 0.5386(16) 0.9485(4) 0.052(3) Uani 1 1 d . . . H31 H 0.2909 0.4834 0.9454 0.063 Uiso 1 1 calc R . . C32 C 0.3892(7) 0.5656(15) 0.9946(5) 0.051(3) Uani 1 1 d . . . H32 H 0.3986 0.5304 1.0234 0.062 Uiso 1 1 calc R . . C33 C 0.4416(6) 0.6478(13) 0.9989(4) 0.044(3) Uani 1 1 d . . . C34 C 0.4230(5) 0.6959(11) 0.9525(3) 0.029(2) Uani 1 1 d . . . C35 C 0.4734(5) 0.7809(12) 0.9544(3) 0.033(2) Uani 1 1 d . . . C36 C 0.4977(6) 0.9097(13) 0.9101(4) 0.042(2) Uani 1 1 d . . . H36 H 0.4824 0.9430 0.8792 0.050 Uiso 1 1 calc R . . C37 C 0.5649(7) 0.9537(16) 0.9533(5) 0.058(3) Uani 1 1 d . . . H37 H 0.5947 1.0120 0.9516 0.070 Uiso 1 1 calc R . . C38 C 0.5870(5) 0.9091(15) 0.9992(4) 0.052(3) Uani 1 1 d . . . H38 H 0.6322 0.9378 1.0291 0.062 Uiso 1 1 calc R . . C39 C 0.5412(6) 0.8206(13) 1.0008(5) 0.045(3) Uani 1 1 d . . . C40 C 0.5583(6) 0.7692(13) 1.0471(4) 0.046(3) Uani 1 1 d . . . H40 H 0.6027 0.7944 1.0783 0.055 Uiso 1 1 calc R . . C41 C 0.5122(7) 0.6880(15) 1.0455(4) 0.051(3) Uani 1 1 d . . . H41 H 0.5258 0.6549 1.0758 0.062 Uiso 1 1 calc R . . C42 C 0.6739(6) 0.3729(13) 0.7444(4) 0.039(2) Uani 1 1 d . . . C43 C 0.6539(5) 0.4894(14) 0.8005(4) 0.042(2) Uani 1 1 d . . . H43A H 0.7023 0.5298 0.8240 0.051 Uiso 1 1 calc R . . H43B H 0.6236 0.5839 0.7782 0.051 Uiso 1 1 calc R . . C44 C 0.6459(7) 0.3391(15) 0.7696(5) 0.055(3) Uani 1 1 d . . . H44A H 0.6703 0.2399 0.7916 0.065 Uiso 1 1 calc R . . H44B H 0.5962 0.3098 0.7436 0.065 Uiso 1 1 calc R . . C45 C -0.0650(5) 1.3132(11) 0.6157(3) 0.034(2) Uani 1 1 d . . . H45A H -0.1150 1.2984 0.5869 0.041 Uiso 1 1 calc R . . H45B H -0.0409 1.3022 0.6038 0.041 Uiso 1 1 calc R . . C46 C -0.1042(5) 0.9338(13) 0.7025(4) 0.038(2) Uani 1 1 d . . . H46A H -0.1309 1.0332 0.6977 0.046 Uiso 1 1 calc R . . H46B H -0.0743 0.8974 0.7374 0.046 Uiso 1 1 calc R . . C47 C -0.0731(6) 1.6320(12) 0.6004(4) 0.043(3) Uani 1 1 d . . . C48 C -0.0523(6) 1.4903(13) 0.6371(4) 0.045(3) Uani 1 1 d . . . H48A H -0.0026 1.5023 0.6672 0.054 Uiso 1 1 calc R . . H48B H -0.0788 1.5035 0.6470 0.054 Uiso 1 1 calc R . . O21 O 0.2738(7) 0.165(2) 0.9825(6) 0.138(6) Uani 1 1 d . . . O22 O 0.6102(6) 0.574(2) 0.3394(5) 0.143(6) Uani 1 1 d . . . O23 O 0.6223(6) 0.8025(17) 0.4099(5) 0.113(4) Uani 1 1 d . . . O24 O 0.2411(5) 0.9432(12) 0.9126(3) 0.071(3) 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 0.0282(6) 0.0332(6) 0.0301(6) 0.0000(4) 0.0202(5) 0.0016(4) Zn2 0.0275(6) 0.0289(6) 0.0439(7) 0.0004(4) 0.0265(6) 0.0011(4) Zn3 0.0405(7) 0.0359(7) 0.0458(8) -0.0074(5) 0.0319(6) -0.0040(5) O1 0.032(4) 0.096(6) 0.053(5) 0.015(4) 0.032(4) 0.011(4) O2 0.041(4) 0.096(7) 0.056(5) 0.022(5) 0.032(4) 0.018(5) O3 0.043(5) 0.085(6) 0.054(5) 0.013(4) 0.036(4) -0.006(4) O4 0.032(4) 0.051(5) 0.059(5) 0.010(4) 0.022(4) -0.006(3) O5 0.070(6) 0.064(6) 0.097(7) 0.015(5) 0.061(6) 0.016(5) O6 0.031(4) 0.060(5) 0.052(4) 0.011(4) 0.031(4) -0.003(3) O7 0.037(4) 0.037(4) 0.068(5) 0.011(3) 0.035(4) 0.009(3) O8 0.058(5) 0.048(4) 0.070(5) 0.027(4) 0.048(5) 0.020(4) O9 0.029(3) 0.043(4) 0.024(3) 0.002(3) 0.018(3) 0.007(3) O10 0.042(4) 0.030(3) 0.043(4) -0.004(3) 0.032(3) 0.002(3) O11 0.027(4) 0.047(4) 0.036(4) -0.008(3) 0.020(3) -0.007(3) O12 0.054(5) 0.041(4) 0.061(5) 0.009(3) 0.042(4) 0.007(3) O13 0.039(4) 0.039(4) 0.055(4) -0.005(3) 0.038(4) 0.003(3) O14 0.020(3) 0.066(5) 0.028(4) -0.009(3) 0.010(3) -0.008(3) O15 0.054(5) 0.037(4) 0.064(5) -0.012(3) 0.046(4) -0.016(3) O16 0.050(4) 0.039(4) 0.066(5) 0.001(3) 0.049(4) -0.003(3) O17 0.058(5) 0.093(7) 0.042(5) -0.006(4) 0.036(4) 0.013(5) O18 0.074(6) 0.040(4) 0.092(6) -0.020(4) 0.068(5) -0.021(4) O19 0.052(5) 0.057(5) 0.040(4) 0.001(4) 0.026(4) -0.006(4) O20 0.098(8) 0.030(4) 0.076(6) -0.003(4) 0.057(6) -0.015(4) N1 0.026(4) 0.028(4) 0.031(4) 0.004(3) 0.019(3) 0.002(3) N2 0.026(4) 0.034(4) 0.029(4) -0.003(3) 0.019(3) -0.001(3) N3 0.025(4) 0.026(4) 0.032(4) 0.005(3) 0.019(3) 0.000(3) N4 0.026(4) 0.040(4) 0.032(4) -0.002(3) 0.020(4) 0.001(3) N5 0.028(4) 0.038(4) 0.037(5) -0.003(3) 0.021(4) -0.002(3) N6 0.012(3) 0.064(5) 0.023(4) -0.003(4) 0.012(3) -0.001(3) N7 0.029(4) 0.050(5) 0.039(5) -0.004(4) 0.023(4) -0.002(4) N8 0.022(4) 0.053(5) 0.029(4) -0.004(4) 0.016(4) -0.006(4) N9 0.038(5) 0.045(5) 0.039(5) -0.011(4) 0.025(4) -0.001(4) N10 0.041(5) 0.026(4) 0.044(5) -0.006(3) 0.030(4) 0.001(3) C1 0.039(7) 0.069(8) 0.031(6) 0.006(5) 0.014(5) 0.007(6) C2 0.063(8) 0.052(7) 0.043(6) -0.005(5) 0.030(6) 0.006(6) C3 0.079(10) 0.053(7) 0.033(6) 0.010(5) 0.029(7) 0.012(7) C4 0.058(7) 0.031(5) 0.041(6) -0.004(4) 0.032(6) 0.002(5) C5 0.060(7) 0.027(5) 0.042(6) -0.003(4) 0.042(6) 0.001(4) C6 0.107(12) 0.053(7) 0.096(10) 0.007(7) 0.094(11) 0.012(7) C7 0.083(10) 0.050(7) 0.103(11) -0.005(7) 0.083(10) -0.010(7) C8 0.045(6) 0.042(6) 0.060(7) -0.012(5) 0.042(6) -0.007(5) C9 0.033(5) 0.031(5) 0.042(6) -0.011(4) 0.024(5) -0.005(4) C10 0.036(6) 0.066(8) 0.074(9) -0.007(6) 0.039(7) 0.002(5) C11 0.033(6) 0.043(6) 0.070(8) -0.017(6) 0.025(6) -0.005(5) C12 0.036(6) 0.054(7) 0.051(7) 0.005(5) 0.025(6) 0.009(5) C13 0.051(7) 0.057(7) 0.034(5) -0.004(5) 0.031(5) -0.011(5) C14 0.031(6) 0.098(10) 0.037(6) -0.001(6) 0.022(5) -0.012(6) C15 0.035(6) 0.056(7) 0.051(7) 0.009(5) 0.029(6) -0.002(5) C16 0.029(5) 0.047(6) 0.040(6) -0.006(4) 0.024(5) -0.006(4) C17 0.041(6) 0.067(7) 0.043(6) 0.001(5) 0.032(5) 0.005(5) C18 0.042(6) 0.038(5) 0.062(7) 0.012(5) 0.041(6) 0.005(4) C19 0.038(6) 0.058(7) 0.052(6) -0.013(5) 0.035(5) -0.007(5) C20 0.021(5) 0.041(5) 0.041(5) 0.004(4) 0.017(4) 0.001(4) C21 0.027(5) 0.031(5) 0.054(6) 0.010(5) 0.029(5) 0.002(4) C22 0.034(5) 0.034(5) 0.025(5) 0.010(4) 0.020(4) 0.008(4) C23 0.034(5) 0.038(5) 0.047(6) 0.003(5) 0.028(5) 0.006(4) C24 0.023(5) 0.037(5) 0.034(5) 0.003(4) 0.019(4) 0.002(4) C25 0.036(6) 0.032(5) 0.050(6) -0.001(5) 0.026(5) 0.003(4) C26 0.014(4) 0.041(5) 0.027(4) 0.002(4) 0.010(4) 0.006(4) C27 0.023(4) 0.039(5) 0.028(5) -0.008(4) 0.016(4) -0.004(4) C28 0.016(4) 0.028(4) 0.027(4) -0.002(4) 0.012(4) 0.003(3) C29 0.033(5) 0.028(5) 0.030(5) 0.006(4) 0.021(4) 0.005(4) C30 0.023(5) 0.042(5) 0.035(5) -0.005(4) 0.016(4) -0.002(4) C31 0.053(7) 0.067(8) 0.049(7) -0.007(6) 0.039(6) -0.016(6) C32 0.073(8) 0.055(7) 0.068(8) 0.002(6) 0.065(7) 0.004(6) C33 0.040(6) 0.036(5) 0.060(7) -0.005(5) 0.036(6) 0.005(4) C34 0.029(5) 0.029(4) 0.036(5) -0.001(4) 0.025(5) 0.003(4) C35 0.025(5) 0.032(5) 0.030(5) -0.004(4) 0.015(4) -0.004(4) C36 0.055(7) 0.036(5) 0.057(6) 0.002(5) 0.046(6) -0.005(5) C37 0.056(8) 0.051(7) 0.084(9) -0.001(6) 0.055(8) -0.011(6) C38 0.021(5) 0.054(7) 0.046(6) -0.011(5) 0.009(5) -0.004(5) C39 0.052(7) 0.030(5) 0.070(8) -0.004(5) 0.048(6) 0.003(5) C40 0.033(5) 0.043(6) 0.039(6) -0.009(5) 0.015(5) -0.001(5) C41 0.053(7) 0.060(7) 0.039(6) -0.006(5) 0.031(6) 0.004(6) C42 0.050(6) 0.042(6) 0.041(6) -0.010(5) 0.037(5) -0.008(5) C43 0.031(5) 0.048(6) 0.056(6) 0.005(5) 0.033(5) 0.000(4) C44 0.078(9) 0.058(7) 0.057(7) -0.021(6) 0.058(7) -0.033(6) C45 0.027(5) 0.031(5) 0.029(5) 0.007(4) 0.013(4) 0.005(4) C46 0.037(5) 0.046(6) 0.047(6) -0.005(5) 0.035(5) -0.003(4) C47 0.040(6) 0.027(5) 0.050(7) 0.008(4) 0.025(5) 0.005(4) C48 0.045(6) 0.033(5) 0.043(6) 0.004(4) 0.024(5) -0.001(5) O21 0.094(10) 0.183(15) 0.160(12) -0.084(11) 0.095(10) -0.026(9) O22 0.064(8) 0.167(14) 0.126(11) 0.051(10) 0.036(8) 0.015(9) O23 0.067(7) 0.110(9) 0.112(9) 0.029(7) 0.041(7) -0.002(7) O24 0.085(7) 0.069(6) 0.063(5) -0.010(4) 0.052(5) -0.023(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 O13 2.001(7) . ? Zn1 O9 2.013(6) . ? Zn1 O17 2.037(8) 2_656 ? Zn1 N5 2.115(8) . ? Zn1 N4 2.165(8) . ? Zn2 O10 2.013(6) . ? Zn2 O11 2.062(6) . ? Zn2 O16 2.067(7) 2_546 ? Zn2 O12 2.104(7) . ? Zn2 O14 2.192(7) . ? Zn2 O13 2.242(7) . ? Zn3 O19 1.969(8) 4_686 ? Zn3 O4 2.019(8) . ? Zn3 N9 2.086(9) . ? Zn3 N10 2.090(9) . ? Zn3 O5 2.396(10) . ? O1 C16 1.207(12) . ? O2 C17 1.232(13) . ? O3 C18 1.184(12) . ? O4 C13 1.248(13) . ? O5 C13 1.250(14) . ? O6 C27 1.209(11) . ? O7 C28 1.212(11) . ? O8 C29 1.199(11) . ? O9 C24 1.273(11) . ? O10 C24 1.272(11) . ? O11 H11 0.8200 . ? O12 H12 0.8200 . ? O13 C21 1.295(11) . ? O14 C21 1.211(12) . ? O15 C22 1.261(12) . ? O16 C22 1.259(11) . ? O16 Zn2 2.067(7) 2_556 ? O17 C42 1.239(12) . ? O17 Zn1 2.037(8) 2_646 ? O18 C42 1.255(13) . ? O19 C47 1.285(13) . ? O19 Zn3 1.969(8) 4_485 ? O20 C47 1.248(13) . ? N1 C28 1.368(11) . ? N1 C27 1.375(12) . ? N1 C45 1.479(11) . ? N2 C29 1.363(12) . ? N2 C28 1.384(11) . ? N2 C46 1.477(11) . ? N3 C29 1.391(12) . ? N3 C27 1.393(12) . ? N3 C26 1.470(10) . ? N4 C30 1.326(12) . ? N4 C34 1.332(12) . ? N5 C36 1.321(13) . ? N5 C35 1.352(12) . ? N6 C18 1.384(13) . ? N6 C17 1.393(13) . ? N6 C19 1.484(12) . ? N7 C17 1.356(13) . ? N7 C16 1.405(13) . ? N7 C43 1.475(12) . ? N8 C16 1.357(13) . ? N8 C18 1.390(13) . ? N8 C15 1.447(13) . ? N9 C1 1.330(14) . ? N9 C5 1.380(14) . ? N10 C12 1.319(14) . ? N10 C9 1.323(13) . ? C1 C2 1.395(17) . ? C1 H1 0.9300 . ? C2 C3 1.339(19) . ? C2 H2 0.9300 . ? C3 C4 1.410(17) . ? C3 H3 0.9300 . ? C4 C5 1.410(14) . ? C4 C6 1.468(17) . ? C5 C9 1.434(15) . ? C6 C7 1.32(2) . ? C6 H6 0.9300 . ? C7 C8 1.416(17) . ? C7 H7 0.9300 . ? C8 C10 1.349(17) . ? C8 C9 1.445(14) . ? C10 C11 1.364(18) . ? C10 H10 0.9300 . ? C11 C12 1.390(16) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.555(16) . ? C14 C15 1.547(17) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C19 C20 1.510(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.531(12) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C22 C23 1.496(13) . ? C23 C46 1.521(14) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.477(13) . ? C25 C26 1.473(13) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C30 C31 1.396(15) . ? C30 H30 0.9300 . ? C31 C32 1.342(17) . ? C31 H31 0.9300 . ? C32 C33 1.406(16) . ? C32 H32 0.9300 . ? C33 C41 1.443(16) . ? C33 C34 1.441(14) . ? C34 C35 1.419(13) . ? C35 C39 1.408(15) . ? C36 C37 1.372(16) . ? C36 H36 0.9300 . ? C37 C38 1.378(17) . ? C37 H37 0.9300 . ? C38 C39 1.402(16) . ? C38 H38 0.9300 . ? C39 C40 1.460(16) . ? C40 C41 1.313(17) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C44 1.519(13) . ? C43 C44 1.528(15) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 C48 1.500(13) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.509(14) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Zn1 O9 106.6(3) . . ? O13 Zn1 O17 93.5(3) . 2_656 ? O9 Zn1 O17 97.5(3) . 2_656 ? O13 Zn1 N5 107.8(3) . . ? O9 Zn1 N5 144.6(3) . . ? O17 Zn1 N5 88.6(3) 2_656 . ? O13 Zn1 N4 97.3(3) . . ? O9 Zn1 N4 90.2(3) . . ? O17 Zn1 N4 164.3(3) 2_656 . ? N5 Zn1 N4 77.3(3) . . ? O10 Zn2 O11 91.5(3) . . ? O10 Zn2 O16 87.3(3) . 2_546 ? O11 Zn2 O16 101.6(3) . 2_546 ? O10 Zn2 O12 174.0(3) . . ? O11 Zn2 O12 94.2(3) . . ? O16 Zn2 O12 89.5(3) 2_546 . ? O10 Zn2 O14 97.3(3) . . ? O11 Zn2 O14 88.3(3) . . ? O16 Zn2 O14 169.0(3) 2_546 . ? O12 Zn2 O14 85.0(3) . . ? O10 Zn2 O13 92.5(3) . . ? O11 Zn2 O13 146.5(3) . . ? O16 Zn2 O13 111.7(3) 2_546 . ? O12 Zn2 O13 83.9(3) . . ? O14 Zn2 O13 58.2(2) . . ? O19 Zn3 O4 133.0(4) 4_686 . ? O19 Zn3 N9 100.8(3) 4_686 . ? O4 Zn3 N9 117.6(3) . . ? O19 Zn3 N10 107.1(3) 4_686 . ? O4 Zn3 N10 105.0(3) . . ? N9 Zn3 N10 80.9(3) . . ? O19 Zn3 O5 99.0(3) 4_686 . ? O4 Zn3 O5 58.9(3) . . ? N9 Zn3 O5 88.1(3) . . ? N10 Zn3 O5 153.1(3) . . ? C13 O4 Zn3 97.4(7) . . ? C13 O5 Zn3 80.2(7) . . ? C24 O9 Zn1 126.5(6) . . ? C24 O10 Zn2 125.3(6) . . ? Zn2 O11 H11 109.5 . . ? Zn2 O12 H12 109.5 . . ? C21 O13 Zn1 129.4(6) . . ? C21 O13 Zn2 89.0(5) . . ? Zn1 O13 Zn2 110.9(3) . . ? C21 O14 Zn2 93.6(6) . . ? C22 O16 Zn2 133.0(6) . 2_556 ? C42 O17 Zn1 135.6(8) . 2_646 ? C47 O19 Zn3 104.5(6) . 4_485 ? C28 N1 C27 123.4(7) . . ? C28 N1 C45 118.7(7) . . ? C27 N1 C45 117.8(8) . . ? C29 N2 C28 124.8(8) . . ? C29 N2 C46 118.6(8) . . ? C28 N2 C46 116.4(8) . . ? C29 N3 C27 122.2(7) . . ? C29 N3 C26 119.5(7) . . ? C27 N3 C26 118.1(7) . . ? C30 N4 C34 119.5(8) . . ? C30 N4 Zn1 128.1(6) . . ? C34 N4 Zn1 112.2(6) . . ? C36 N5 C35 118.7(9) . . ? C36 N5 Zn1 127.3(7) . . ? C35 N5 Zn1 113.9(6) . . ? C18 N6 C17 123.4(8) . . ? C18 N6 C19 116.4(8) . . ? C17 N6 C19 120.0(8) . . ? C17 N7 C16 123.7(9) . . ? C17 N7 C43 118.9(8) . . ? C16 N7 C43 116.8(8) . . ? C16 N8 C18 124.0(8) . . ? C16 N8 C15 118.6(8) . . ? C18 N8 C15 117.1(8) . . ? C1 N9 C5 118.4(10) . . ? C1 N9 Zn3 130.9(8) . . ? C5 N9 Zn3 110.7(7) . . ? C12 N10 C9 118.8(10) . . ? C12 N10 Zn3 129.3(8) . . ? C9 N10 Zn3 111.8(7) . . ? N9 C1 C2 122.2(12) . . ? N9 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 120.4(12) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 120.0(11) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 117.4(11) . . ? C5 C4 C6 117.7(11) . . ? C3 C4 C6 124.9(11) . . ? N9 C5 C4 121.6(10) . . ? N9 C5 C9 117.3(9) . . ? C4 C5 C9 121.1(10) . . ? C7 C6 C4 120.9(11) . . ? C7 C6 H6 119.6 . . ? C4 C6 H6 119.6 . . ? C6 C7 C8 123.4(12) . . ? C6 C7 H7 118.3 . . ? C8 C7 H7 118.3 . . ? C10 C8 C7 125.3(12) . . ? C10 C8 C9 116.3(10) . . ? C7 C8 C9 118.4(11) . . ? N10 C9 C5 119.0(9) . . ? N10 C9 C8 122.5(9) . . ? C5 C9 C8 118.5(9) . . ? C8 C10 C11 121.2(11) . . ? C8 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 118.9(11) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? N10 C12 C11 122.3(12) . . ? N10 C12 H12A 118.8 . . ? C11 C12 H12A 118.8 . . ? O4 C13 O5 123.1(11) . . ? O4 C13 C14 117.4(10) . . ? O5 C13 C14 119.6(11) . . ? C15 C14 C13 111.7(9) . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? N8 C15 C14 113.8(10) . . ? N8 C15 H15A 108.8 . . ? C14 C15 H15A 108.8 . . ? N8 C15 H15B 108.8 . . ? C14 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? O1 C16 N8 123.5(10) . . ? O1 C16 N7 120.2(9) . . ? N8 C16 N7 116.3(8) . . ? O2 C17 N7 122.5(10) . . ? O2 C17 N6 121.0(10) . . ? N7 C17 N6 116.5(9) . . ? O3 C18 N6 121.8(10) . . ? O3 C18 N8 122.2(10) . . ? N6 C18 N8 115.9(8) . . ? N6 C19 C20 111.4(8) . . ? N6 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? N6 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C19 C20 C21 109.7(8) . . ? C19 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 . . ? C19 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? O14 C21 O13 118.8(8) . . ? O14 C21 C20 122.3(9) . . ? O13 C21 C20 118.8(9) . . ? O16 C22 O15 125.0(9) . . ? O16 C22 C23 117.4(9) . . ? O15 C22 C23 117.6(8) . . ? C22 C23 C46 113.2(8) . . ? C22 C23 H23A 108.9 . . ? C46 C23 H23A 108.9 . . ? C22 C23 H23B 108.9 . . ? C46 C23 H23B 108.9 . . ? H23A C23 H23B 107.8 . . ? O10 C24 O9 123.7(8) . . ? O10 C24 C25 120.2(9) . . ? O9 C24 C25 116.1(8) . . ? C26 C25 C24 116.4(9) . . ? C26 C25 H25A 108.2 . . ? C24 C25 H25A 108.2 . . ? C26 C25 H25B 108.2 . . ? C24 C25 H25B 108.2 . . ? H25A C25 H25B 107.3 . . ? N3 C26 C25 115.8(8) . . ? N3 C26 H26A 108.3 . . ? C25 C26 H26A 108.3 . . ? N3 C26 H26B 108.3 . . ? C25 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? O6 C27 N1 121.1(9) . . ? O6 C27 N3 121.8(9) . . ? N1 C27 N3 117.2(8) . . ? O7 C28 N1 122.6(8) . . ? O7 C28 N2 121.4(8) . . ? N1 C28 N2 116.0(7) . . ? O8 C29 N2 122.6(9) . . ? O8 C29 N3 121.1(9) . . ? N2 C29 N3 116.0(7) . . ? N4 C30 C31 121.5(9) . . ? N4 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C32 C31 C30 121.2(10) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C33 119.0(10) . . ? C31 C32 H32 120.5 . . ? C33 C32 H32 120.5 . . ? C32 C33 C41 126.0(11) . . ? C32 C33 C34 116.9(10) . . ? C41 C33 C34 117.1(10) . . ? N4 C34 C35 118.6(8) . . ? N4 C34 C33 121.9(9) . . ? C35 C34 C33 119.5(9) . . ? N5 C35 C39 121.6(9) . . ? N5 C35 C34 117.1(8) . . ? C39 C35 C34 121.2(9) . . ? N5 C36 C37 124.1(10) . . ? N5 C36 H36 118.0 . . ? C37 C36 H36 118.0 . . ? C36 C37 C38 118.2(10) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? C37 C38 C39 119.9(10) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C35 117.5(10) . . ? C38 C39 C40 124.8(11) . . ? C35 C39 C40 117.7(10) . . ? C41 C40 C39 121.2(10) . . ? C41 C40 H40 119.4 . . ? C39 C40 H40 119.4 . . ? C40 C41 C33 123.2(11) . . ? C40 C41 H41 118.4 . . ? C33 C41 H41 118.4 . . ? O17 C42 O18 129.2(10) . . ? O17 C42 C44 117.0(10) . . ? O18 C42 C44 113.8(9) . . ? N7 C43 C44 109.2(8) . . ? N7 C43 H43A 109.8 . . ? C44 C43 H43A 109.8 . . ? N7 C43 H43B 109.8 . . ? C44 C43 H43B 109.8 . . ? H43A C43 H43B 108.3 . . ? C42 C44 C43 114.9(9) . . ? C42 C44 H44A 108.6 . . ? C43 C44 H44A 108.6 . . ? C42 C44 H44B 108.6 . . ? C43 C44 H44B 108.6 . . ? H44A C44 H44B 107.5 . . ? N1 C45 C48 112.9(8) . . ? N1 C45 H45A 109.0 . . ? C48 C45 H45A 109.0 . . ? N1 C45 H45B 109.0 . . ? C48 C45 H45B 109.0 . . ? H45A C45 H45B 107.8 . . ? N2 C46 C23 112.8(8) . . ? N2 C46 H46A 109.0 . . ? C23 C46 H46A 109.0 . . ? N2 C46 H46B 109.0 . . ? C23 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? O20 C47 O19 121.1(10) . . ? O20 C47 C48 119.5(10) . . ? O19 C47 C48 119.4(9) . . ? C45 C48 C47 113.3(9) . . ? C45 C48 H48A 108.9 . . ? C47 C48 H48A 108.9 . . ? C45 C48 H48B 108.9 . . ? C47 C48 H48B 108.9 . . ? H48A C48 H48B 107.7 . . ? 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 O19 Zn3 O4 C13 68.1(8) 4_686 . . . ? N9 Zn3 O4 C13 -72.7(7) . . . . ? N10 Zn3 O4 C13 -160.1(6) . . . . ? O5 Zn3 O4 C13 -3.7(6) . . . . ? O19 Zn3 O5 C13 -131.6(7) 4_686 . . . ? O4 Zn3 O5 C13 3.7(6) . . . . ? N9 Zn3 O5 C13 127.8(7) . . . . ? N10 Zn3 O5 C13 62.4(10) . . . . ? O13 Zn1 O9 C24 -31.0(8) . . . . ? O17 Zn1 O9 C24 64.9(8) 2_656 . . . ? N5 Zn1 O9 C24 163.2(7) . . . . ? N4 Zn1 O9 C24 -128.8(7) . . . . ? O11 Zn2 O10 C24 144.3(7) . . . . ? O16 Zn2 O10 C24 42.7(7) 2_546 . . . ? O12 Zn2 O10 C24 -15(3) . . . . ? O14 Zn2 O10 C24 -127.2(7) . . . . ? O13 Zn2 O10 C24 -68.9(7) . . . . ? O9 Zn1 O13 C21 104.0(8) . . . . ? O17 Zn1 O13 C21 5.0(8) 2_656 . . . ? N5 Zn1 O13 C21 -84.6(8) . . . . ? N4 Zn1 O13 C21 -163.6(8) . . . . ? O9 Zn1 O13 Zn2 -2.9(4) . . . . ? O17 Zn1 O13 Zn2 -101.8(4) 2_656 . . . ? N5 Zn1 O13 Zn2 168.5(3) . . . . ? N4 Zn1 O13 Zn2 89.6(3) . . . . ? O10 Zn2 O13 C21 -99.7(5) . . . . ? O11 Zn2 O13 C21 -3.2(8) . . . . ? O16 Zn2 O13 C21 172.2(5) 2_546 . . . ? O12 Zn2 O13 C21 85.2(5) . . . . ? O14 Zn2 O13 C21 -2.6(5) . . . . ? O10 Zn2 O13 Zn1 32.6(3) . . . . ? O11 Zn2 O13 Zn1 129.1(4) . . . . ? O16 Zn2 O13 Zn1 -55.5(4) 2_546 . . . ? O12 Zn2 O13 Zn1 -142.5(4) . . . . ? O14 Zn2 O13 Zn1 129.6(4) . . . . ? O10 Zn2 O14 C21 91.3(6) . . . . ? O11 Zn2 O14 C21 -177.4(6) . . . . ? O16 Zn2 O14 C21 -22.9(18) 2_546 . . . ? O12 Zn2 O14 C21 -83.1(6) . . . . ? O13 Zn2 O14 C21 2.8(5) . . . . ? O13 Zn1 N4 C30 -76.0(8) . . . . ? O9 Zn1 N4 C30 30.8(8) . . . . ? O17 Zn1 N4 C30 150.6(12) 2_656 . . . ? N5 Zn1 N4 C30 177.3(9) . . . . ? O13 Zn1 N4 C34 98.5(6) . . . . ? O9 Zn1 N4 C34 -154.7(6) . . . . ? O17 Zn1 N4 C34 -34.9(16) 2_656 . . . ? N5 Zn1 N4 C34 -8.2(6) . . . . ? O13 Zn1 N5 C36 90.6(8) . . . . ? O9 Zn1 N5 C36 -103.8(9) . . . . ? O17 Zn1 N5 C36 -2.7(9) 2_656 . . . ? N4 Zn1 N5 C36 -175.7(9) . . . . ? O13 Zn1 N5 C35 -86.0(7) . . . . ? O9 Zn1 N5 C35 79.6(8) . . . . ? O17 Zn1 N5 C35 -179.3(7) 2_656 . . . ? N4 Zn1 N5 C35 7.7(6) . . . . ? O19 Zn3 N9 C1 -75.8(10) 4_686 . . . ? O4 Zn3 N9 C1 76.1(10) . . . . ? N10 Zn3 N9 C1 178.4(10) . . . . ? O5 Zn3 N9 C1 23.0(10) . . . . ? O19 Zn3 N9 C5 101.0(7) 4_686 . . . ? O4 Zn3 N9 C5 -107.0(7) . . . . ? N10 Zn3 N9 C5 -4.8(6) . . . . ? O5 Zn3 N9 C5 -160.2(7) . . . . ? O19 Zn3 N10 C12 81.0(9) 4_686 . . . ? O4 Zn3 N10 C12 -64.2(9) . . . . ? N9 Zn3 N10 C12 179.5(9) . . . . ? O5 Zn3 N10 C12 -113.5(10) . . . . ? O19 Zn3 N10 C9 -93.5(7) 4_686 . . . ? O4 Zn3 N10 C9 121.3(6) . . . . ? N9 Zn3 N10 C9 5.1(6) . . . . ? O5 Zn3 N10 C9 72.1(10) . . . . ? C5 N9 C1 C2 -1.1(16) . . . . ? Zn3 N9 C1 C2 175.6(9) . . . . ? N9 C1 C2 C3 -1.7(19) . . . . ? C1 C2 C3 C4 2.8(19) . . . . ? C2 C3 C4 C5 -1.3(17) . . . . ? C2 C3 C4 C6 177.9(12) . . . . ? C1 N9 C5 C4 2.5(14) . . . . ? Zn3 N9 C5 C4 -174.7(7) . . . . ? C1 N9 C5 C9 -178.7(9) . . . . ? Zn3 N9 C5 C9 4.0(10) . . . . ? C3 C4 C5 N9 -1.4(14) . . . . ? C6 C4 C5 N9 179.3(9) . . . . ? C3 C4 C5 C9 180.0(9) . . . . ? C6 C4 C5 C9 0.6(14) . . . . ? C5 C4 C6 C7 -0.7(17) . . . . ? C3 C4 C6 C7 180.0(12) . . . . ? C4 C6 C7 C8 1(2) . . . . ? C6 C7 C8 C10 179.4(13) . . . . ? C6 C7 C8 C9 -1.4(18) . . . . ? C12 N10 C9 C5 -179.7(9) . . . . ? Zn3 N10 C9 C5 -4.6(10) . . . . ? C12 N10 C9 C8 0.3(14) . . . . ? Zn3 N10 C9 C8 175.4(7) . . . . ? N9 C5 C9 N10 0.4(13) . . . . ? C4 C5 C9 N10 179.1(9) . . . . ? N9 C5 C9 C8 -179.6(8) . . . . ? C4 C5 C9 C8 -0.9(14) . . . . ? C10 C8 C9 N10 0.5(15) . . . . ? C7 C8 C9 N10 -178.8(10) . . . . ? C10 C8 C9 C5 -179.5(10) . . . . ? C7 C8 C9 C5 1.2(14) . . . . ? C7 C8 C10 C11 179.0(11) . . . . ? C9 C8 C10 C11 -0.2(17) . . . . ? C8 C10 C11 C12 -0.9(18) . . . . ? C9 N10 C12 C11 -1.4(16) . . . . ? Zn3 N10 C12 C11 -175.6(8) . . . . ? C10 C11 C12 N10 1.7(18) . . . . ? Zn3 O4 C13 O5 7.3(12) . . . . ? Zn3 O4 C13 C14 -174.7(7) . . . . ? Zn3 O5 C13 O4 -6.2(10) . . . . ? Zn3 O5 C13 C14 175.8(9) . . . . ? O4 C13 C14 C15 -88.6(12) . . . . ? O5 C13 C14 C15 89.5(13) . . . . ? C16 N8 C15 C14 100.1(11) . . . . ? C18 N8 C15 C14 -85.1(12) . . . . ? C13 C14 C15 N8 -65.1(13) . . . . ? C18 N8 C16 O1 -177.4(10) . . . . ? C15 N8 C16 O1 -2.9(16) . . . . ? C18 N8 C16 N7 3.7(15) . . . . ? C15 N8 C16 N7 178.2(9) . . . . ? C17 N7 C16 O1 177.7(11) . . . . ? C43 N7 C16 O1 6.7(15) . . . . ? C17 N7 C16 N8 -3.4(15) . . . . ? C43 N7 C16 N8 -174.4(9) . . . . ? C16 N7 C17 O2 -177.3(11) . . . . ? C43 N7 C17 O2 -6.4(17) . . . . ? C16 N7 C17 N6 1.5(16) . . . . ? C43 N7 C17 N6 172.3(9) . . . . ? C18 N6 C17 O2 179.1(11) . . . . ? C19 N6 C17 O2 4.5(16) . . . . ? C18 N6 C17 N7 0.3(16) . . . . ? C19 N6 C17 N7 -174.3(9) . . . . ? C17 N6 C18 O3 179.7(11) . . . . ? C19 N6 C18 O3 -5.5(16) . . . . ? C17 N6 C18 N8 0.0(15) . . . . ? C19 N6 C18 N8 174.8(9) . . . . ? C16 N8 C18 O3 178.1(11) . . . . ? C15 N8 C18 O3 3.5(16) . . . . ? C16 N8 C18 N6 -2.1(15) . . . . ? C15 N8 C18 N6 -176.7(9) . . . . ? C18 N6 C19 C20 75.9(12) . . . . ? C17 N6 C19 C20 -109.1(11) . . . . ? N6 C19 C20 C21 -173.5(8) . . . . ? Zn2 O14 C21 O13 -4.8(9) . . . . ? Zn2 O14 C21 C20 172.9(8) . . . . ? Zn1 O13 C21 O14 -111.9(9) . . . . ? Zn2 O13 C21 O14 4.7(9) . . . . ? Zn1 O13 C21 C20 70.3(11) . . . . ? Zn2 O13 C21 C20 -173.1(7) . . . . ? C19 C20 C21 O14 -18.3(13) . . . . ? C19 C20 C21 O13 159.4(9) . . . . ? Zn2 O16 C22 O15 4.8(15) 2_556 . . . ? Zn2 O16 C22 C23 -175.6(7) 2_556 . . . ? O16 C22 C23 C46 1.0(12) . . . . ? O15 C22 C23 C46 -179.4(9) . . . . ? Zn2 O10 C24 O9 49.6(12) . . . . ? Zn2 O10 C24 C25 -133.1(8) . . . . ? Zn1 O9 C24 O10 12.4(13) . . . . ? Zn1 O9 C24 C25 -165.0(7) . . . . ? O10 C24 C25 C26 -179.2(9) . . . . ? O9 C24 C25 C26 -1.7(14) . . . . ? C29 N3 C26 C25 88.2(11) . . . . ? C27 N3 C26 C25 -86.3(11) . . . . ? C24 C25 C26 N3 -174.6(8) . . . . ? C28 N1 C27 O6 174.2(8) . . . . ? C45 N1 C27 O6 -3.2(13) . . . . ? C28 N1 C27 N3 -4.6(13) . . . . ? C45 N1 C27 N3 177.9(7) . . . . ? C29 N3 C27 O6 -172.3(9) . . . . ? C26 N3 C27 O6 2.0(13) . . . . ? C29 N3 C27 N1 6.5(12) . . . . ? C26 N3 C27 N1 -179.2(7) . . . . ? C27 N1 C28 O7 -176.2(9) . . . . ? C45 N1 C28 O7 1.3(13) . . . . ? C27 N1 C28 N2 2.8(12) . . . . ? C45 N1 C28 N2 -179.8(7) . . . . ? C29 N2 C28 O7 176.1(9) . . . . ? C46 N2 C28 O7 -9.8(12) . . . . ? C29 N2 C28 N1 -2.9(13) . . . . ? C46 N2 C28 N1 171.2(7) . . . . ? C28 N2 C29 O8 179.3(9) . . . . ? C46 N2 C29 O8 5.3(14) . . . . ? C28 N2 C29 N3 4.7(13) . . . . ? C46 N2 C29 N3 -169.3(8) . . . . ? C27 N3 C29 O8 178.8(9) . . . . ? C26 N3 C29 O8 4.6(13) . . . . ? C27 N3 C29 N2 -6.5(12) . . . . ? C26 N3 C29 N2 179.3(8) . . . . ? C34 N4 C30 C31 -3.3(15) . . . . ? Zn1 N4 C30 C31 170.9(8) . . . . ? N4 C30 C31 C32 2.7(18) . . . . ? C30 C31 C32 C33 -0.6(18) . . . . ? C31 C32 C33 C41 179.3(11) . . . . ? C31 C32 C33 C34 -0.8(16) . . . . ? C30 N4 C34 C35 -177.3(8) . . . . ? Zn1 N4 C34 C35 7.6(10) . . . . ? C30 N4 C34 C33 1.8(14) . . . . ? Zn1 N4 C34 C33 -173.3(7) . . . . ? C32 C33 C34 N4 0.3(14) . . . . ? C41 C33 C34 N4 -179.8(9) . . . . ? C32 C33 C34 C35 179.4(9) . . . . ? C41 C33 C34 C35 -0.7(13) . . . . ? C36 N5 C35 C39 -2.8(14) . . . . ? Zn1 N5 C35 C39 174.1(7) . . . . ? C36 N5 C35 C34 176.7(9) . . . . ? Zn1 N5 C35 C34 -6.4(11) . . . . ? N4 C34 C35 N5 -1.0(13) . . . . ? C33 C34 C35 N5 179.9(8) . . . . ? N4 C34 C35 C39 178.5(9) . . . . ? C33 C34 C35 C39 -0.6(14) . . . . ? C35 N5 C36 C37 3.2(15) . . . . ? Zn1 N5 C36 C37 -173.3(9) . . . . ? N5 C36 C37 C38 -1.9(18) . . . . ? C36 C37 C38 C39 0.3(17) . . . . ? C37 C38 C39 C35 0.0(16) . . . . ? C37 C38 C39 C40 -179.0(11) . . . . ? N5 C35 C39 C38 1.3(14) . . . . ? C34 C35 C39 C38 -178.2(9) . . . . ? N5 C35 C39 C40 -179.7(9) . . . . ? C34 C35 C39 C40 0.9(14) . . . . ? C38 C39 C40 C41 179.2(11) . . . . ? C35 C39 C40 C41 0.3(15) . . . . ? C39 C40 C41 C33 -1.7(17) . . . . ? C32 C33 C41 C40 -178.2(11) . . . . ? C34 C33 C41 C40 1.9(16) . . . . ? Zn1 O17 C42 O18 39.2(19) 2_646 . . . ? Zn1 O17 C42 C44 -139.4(10) 2_646 . . . ? C17 N7 C43 C44 -86.2(12) . . . . ? C16 N7 C43 C44 85.3(11) . . . . ? O17 C42 C44 C43 -131.1(11) . . . . ? O18 C42 C44 C43 50.1(15) . . . . ? N7 C43 C44 C42 -172.0(10) . . . . ? C28 N1 C45 C48 89.3(10) . . . . ? C27 N1 C45 C48 -93.2(10) . . . . ? C29 N2 C46 C23 -95.6(10) . . . . ? C28 N2 C46 C23 89.9(10) . . . . ? C22 C23 C46 N2 -170.4(8) . . . . ? Zn3 O19 C47 O20 6.0(13) 4_485 . . . ? Zn3 O19 C47 C48 -174.7(9) 4_485 . . . ? N1 C45 C48 C47 176.4(9) . . . . ? O20 C47 C48 C45 -162.0(11) . . . . ? O19 C47 C48 C45 18.6(15) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.046 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.208 #===end data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H64 N18 O26 Zn3' _chemical_formula_weight 1505.28 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 12.618(3) _cell_length_b 12.927(3) _cell_length_c 13.012(3) _cell_angle_alpha 78.30(3) _cell_angle_beta 62.22(3) _cell_angle_gamma 62.07(3) _cell_volume 1658.8(7) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5291 _cell_measurement_theta_min 2.0222 _cell_measurement_theta_max 29.0986 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 1.168 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.8876 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Saturn724 (4x4 bin mode) ; _diffrn_measurement_method 'dtprofit.ref' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14385 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5829 _reflns_number_gt 5082 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1530P)^2^+3.2863P] 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 5829 _refine_ls_number_parameters 430 _refine_ls_number_restraints 612 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2417 _refine_ls_wR_factor_gt 0.2311 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.101 _refine_ls_shift/su_mean 0.002 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 0.34177(3) 0.85875(3) 0.60613(3) 0.03268(11) Uani 1 1 d U . . Zn2 Zn 0.0000 0.0000 1.0000 0.04282(15) Uani 1 2 d SU . . O1 O 0.3185(3) 0.7401(4) 0.5490(3) 0.0867(10) Uani 1 1 d U . . O2 O 0.1420(4) 0.8156(3) 0.7030(3) 0.0902(10) Uani 1 1 d U . . O3 O -0.5138(3) 0.7729(2) 0.6523(3) 0.0592(8) Uani 1 1 d U . . O4 O -0.6167(3) 0.6815(4) 0.7886(4) 0.1001(16) Uani 1 1 d U . . O5 O 0.1511(2) 0.0055(2) 0.8349(2) 0.0446(7) Uani 1 1 d U . . O6 O 0.2408(2) 0.0268(2) 0.6459(2) 0.0415(7) Uani 1 1 d U . . O7 O 0.1758(2) 0.4171(2) 0.7055(3) 0.0537(8) Uani 1 1 d U . . O8 O -0.1099(2) 0.3680(2) 0.6239(3) 0.0574(8) Uani 1 1 d U . . O9 O -0.1722(3) 0.7341(2) 0.6687(3) 0.0585(9) Uani 1 1 d U . . O10 O -0.0503(3) 0.1678(3) 1.0560(3) 0.0723(10) Uani 1 1 d U . . H10 H -0.1123 0.1833 1.1210 0.108 Uiso 1 1 d R . . N1 N 0.0379(3) 0.3894(2) 0.6592(3) 0.0362(7) Uani 1 1 d U . . N2 N -0.1445(3) 0.5529(2) 0.6460(3) 0.0389(8) Uani 1 1 d U . . N3 N 0.0036(3) 0.5788(2) 0.6864(3) 0.0433(8) Uani 1 1 d U . . N7 N 0.4537(3) 0.8912(3) 0.4361(3) 0.0412(8) Uani 1 1 d U . . N8 N 0.6028(4) 0.8518(4) 0.2534(3) 0.0598(11) Uani 1 1 d U . . H7 H 0.6717 0.8114 0.1848 0.072 Uiso 1 1 d R . . N9 N 0.5307(3) 0.9682(3) 0.2718(3) 0.0464(8) Uani 1 1 d U . . N10 N 0.1364(3) -0.0779(3) 1.0739(3) 0.0479(9) Uani 1 1 d U . . N11 N 0.2990(4) -0.2136(4) 1.1166(4) 0.0676(12) Uani 1 1 d U . . H5 H 0.3756 -0.2798 1.1124 0.081 Uiso 1 1 d R . . N12 N 0.2142(3) -0.1324(3) 1.2021(3) 0.0539(10) Uani 1 1 d U . . C1 C 0.0092(4) -0.0987(4) 1.4674(4) 0.0566(10) Uani 1 1 d U . . H1 H 0.0150 -0.1661 1.4456 0.068 Uiso 1 1 calc R . . C2 C 0.1138(4) -0.0673(4) 1.4053(3) 0.0503(10) Uani 1 1 d U . . C3 C 0.1006(4) 0.0333(4) 1.4413(4) 0.0547(11) Uani 1 1 d U . . H3 H 0.1690 0.0564 1.4017 0.066 Uiso 1 1 calc R . . C4 C 0.2356(4) -0.1410(5) 1.3067(4) 0.0709(15) Uani 1 1 d U . . H4A H 0.3050 -0.1171 1.2874 0.085 Uiso 1 1 calc R . . H4B H 0.2658 -0.2220 1.3302 0.085 Uiso 1 1 calc R . . C5 C 0.2498(4) -0.1795(4) 1.0410(4) 0.0602(13) Uani 1 1 d U . . C6 C 0.1167(4) -0.0504(4) 1.1764(3) 0.0490(10) Uani 1 1 d U . . H6 H 0.0468 0.0151 1.2222 0.059 Uiso 1 1 calc R . . C7 C 0.5524(4) 0.8076(4) 0.3554(4) 0.0520(12) Uani 1 1 d U . . C8 C 0.4434(4) 0.9900(3) 0.3807(3) 0.0451(9) Uani 1 1 d U . . H8 H 0.3832 1.0643 0.4139 0.054 Uiso 1 1 calc R . . C9 C 0.5521(4) 1.0489(4) 0.1749(3) 0.0622(11) Uani 1 1 d U . . H9A H 0.6428 1.0393 0.1417 0.075 Uiso 1 1 calc R . . H9B H 0.4932 1.1291 0.2032 0.075 Uiso 1 1 calc R . . C10 C 0.5253(3) 1.0240(3) 0.0833(3) 0.0459(9) Uani 1 1 d U . . C11 C 0.6273(4) 0.9531(4) -0.0118(4) 0.0601(13) Uani 1 1 d U . . H11 H 0.7142 0.9210 -0.0203 0.072 Uiso 1 1 calc R . . C12 C 0.3980(4) 1.0706(4) 0.0943(4) 0.0552(12) Uani 1 1 d U . . H12 H 0.3282 1.1186 0.1580 0.066 Uiso 1 1 calc R . . C13 C 0.1628(3) 0.0672(3) 0.7476(3) 0.0349(8) Uani 1 1 d U . . C14 C 0.0827(4) 0.1987(3) 0.7611(3) 0.0447(11) Uani 1 1 d U . . H14A H 0.0945 0.2269 0.8169 0.054 Uiso 1 1 calc R . . H14B H -0.0107 0.2171 0.7920 0.054 Uiso 1 1 calc R . . C15 C 0.1220(3) 0.2624(3) 0.6474(3) 0.0376(9) Uani 1 1 d U . . H15A H 0.2137 0.2483 0.6192 0.045 Uiso 1 1 calc R . . H15B H 0.1161 0.2303 0.5900 0.045 Uiso 1 1 calc R . . C16 C 0.0779(3) 0.4592(3) 0.6871(3) 0.0390(9) Uani 1 1 d U . . C17 C -0.0732(3) 0.4315(3) 0.6419(3) 0.0394(9) Uani 1 1 d U . . C18 C -0.1082(3) 0.6287(3) 0.6680(3) 0.0416(10) Uani 1 1 d U . . C19 C 0.0475(4) 0.6551(3) 0.7114(4) 0.0517(11) Uani 1 1 d U . . H19A H 0.0657 0.6269 0.7790 0.062 Uiso 1 1 calc R . . H19B H -0.0230 0.7341 0.7288 0.062 Uiso 1 1 calc R . . C20 C 0.1700(4) 0.6567(4) 0.6098(4) 0.0530(10) Uani 1 1 d U . . H20A H 0.1550 0.6752 0.5403 0.064 Uiso 1 1 calc R . . H20B H 0.2430 0.5793 0.5986 0.064 Uiso 1 1 calc R . . C21 C 0.2080(4) 0.7449(4) 0.6264(4) 0.0607(11) Uani 1 1 d U . . C22 C -0.2642(4) 0.6017(4) 0.6263(3) 0.0458(10) Uani 1 1 d U . . H22A H -0.2522 0.5504 0.5729 0.055 Uiso 1 1 calc R . . H22B H -0.2759 0.6773 0.5901 0.055 Uiso 1 1 calc R . . C23 C -0.3878(4) 0.6165(4) 0.7366(4) 0.0494(11) Uani 1 1 d U . . H23A H -0.3883 0.6511 0.7965 0.059 Uiso 1 1 calc R . . H23B H -0.3857 0.5400 0.7625 0.059 Uiso 1 1 calc R . . C24 C -0.5147(4) 0.6929(4) 0.7219(4) 0.0547(12) Uani 1 1 d U . . O12 O 0.2047(16) 0.4242(18) 0.0504(16) 0.454(8) Uani 1 1 d U . . O13 O 0.1371(12) 0.3079(15) 0.9667(8) 0.374(12) Uani 1 1 d U . . O11 O 0.4987(14) 0.5581(12) 0.3523(19) 0.401(13) Uani 1 1 d U . . 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 0.03404(15) 0.02762(17) 0.03800(18) 0.00137(14) -0.01754(14) -0.01272(13) Zn2 0.0619(3) 0.0451(3) 0.0334(3) 0.0107(2) -0.0226(2) -0.0338(2) O1 0.1051(15) 0.1106(19) 0.0809(19) 0.0116(16) -0.0431(15) -0.0747(14) O2 0.1380(17) 0.0522(16) 0.121(2) -0.0075(15) -0.0927(15) -0.0313(15) O3 0.0696(12) 0.0385(13) 0.0865(16) 0.0111(12) -0.0561(12) -0.0174(11) O4 0.0588(16) 0.131(3) 0.099(3) 0.038(2) -0.0365(17) -0.0433(18) O5 0.0496(11) 0.0383(12) 0.0394(12) 0.0121(10) -0.0158(10) -0.0218(9) O6 0.0490(11) 0.0245(10) 0.0380(12) 0.0000(9) -0.0137(10) -0.0108(9) O7 0.0546(11) 0.0389(12) 0.0812(16) 0.0084(12) -0.0419(11) -0.0205(10) O8 0.0558(11) 0.0402(13) 0.0894(17) -0.0076(12) -0.0430(12) -0.0154(10) O9 0.0512(13) 0.0252(12) 0.0805(19) -0.0009(12) -0.0235(13) -0.0064(11) O10 0.1189(18) 0.0613(14) 0.0546(16) 0.0050(12) -0.0331(15) -0.0580(13) N1 0.0353(11) 0.0248(12) 0.0458(14) 0.0051(11) -0.0168(11) -0.0134(10) N2 0.0338(11) 0.0274(13) 0.0490(15) 0.0028(11) -0.0185(11) -0.0082(10) N3 0.0433(12) 0.0297(12) 0.0588(17) 0.0005(12) -0.0196(12) -0.0193(10) N7 0.0398(12) 0.0452(15) 0.0361(14) 0.0014(12) -0.0143(11) -0.0186(11) N8 0.0524(17) 0.068(2) 0.0381(17) -0.0056(15) -0.0065(15) -0.0210(16) N9 0.0648(13) 0.0536(15) 0.0407(14) 0.0098(12) -0.0280(11) -0.0387(12) N10 0.0560(13) 0.0572(16) 0.0394(15) 0.0074(13) -0.0211(12) -0.0331(12) N11 0.0564(17) 0.065(2) 0.070(2) -0.0112(18) -0.0278(16) -0.0122(17) N12 0.0525(14) 0.0547(18) 0.0546(17) -0.0030(14) -0.0261(13) -0.0186(14) C1 0.0771(17) 0.0403(17) 0.077(2) 0.0013(16) -0.0485(16) -0.0282(15) C2 0.0630(16) 0.0469(19) 0.0553(18) 0.0062(15) -0.0416(14) -0.0202(15) C3 0.0641(16) 0.053(2) 0.065(2) 0.0112(17) -0.0378(16) -0.0327(15) C4 0.066(2) 0.079(3) 0.070(2) 0.000(2) -0.0453(18) -0.016(2) C5 0.0570(19) 0.064(2) 0.057(2) -0.0024(19) -0.0197(18) -0.0278(18) C6 0.0602(16) 0.0507(19) 0.0449(18) 0.0055(15) -0.0293(14) -0.0258(15) C7 0.0435(17) 0.055(2) 0.0434(19) 0.0016(17) -0.0153(15) -0.0138(16) C8 0.0606(15) 0.0456(17) 0.0410(16) 0.0058(14) -0.0274(14) -0.0280(14) C9 0.1033(19) 0.079(2) 0.0456(18) 0.0247(16) -0.0443(16) -0.0674(17) C10 0.0693(15) 0.0581(17) 0.0351(15) 0.0135(13) -0.0276(13) -0.0458(13) C11 0.0490(16) 0.086(3) 0.051(2) 0.0077(19) -0.0242(16) -0.0327(18) C12 0.0605(19) 0.061(2) 0.0386(18) -0.0069(17) -0.0188(16) -0.0219(18) C13 0.0345(12) 0.0308(14) 0.0415(16) 0.0050(12) -0.0168(12) -0.0169(11) C14 0.0457(17) 0.0277(16) 0.0407(19) 0.0035(14) -0.0074(15) -0.0129(14) C15 0.0354(14) 0.0284(15) 0.0401(17) 0.0003(13) -0.0127(13) -0.0103(12) C16 0.0416(14) 0.0296(15) 0.0468(18) 0.0057(13) -0.0190(13) -0.0180(12) C17 0.0384(14) 0.0325(16) 0.0426(17) -0.0011(13) -0.0157(13) -0.0128(13) C18 0.0376(15) 0.0281(16) 0.0461(19) 0.0061(14) -0.0127(14) -0.0118(13) C19 0.0636(18) 0.0381(17) 0.056(2) -0.0045(15) -0.0219(17) -0.0259(15) C20 0.0672(16) 0.0495(18) 0.060(2) 0.0061(16) -0.0307(16) -0.0368(14) C21 0.0827(17) 0.068(2) 0.0615(18) 0.0252(16) -0.0508(15) -0.0449(16) C22 0.0462(15) 0.0416(19) 0.0437(17) 0.0073(15) -0.0245(14) -0.0118(15) C23 0.0411(15) 0.048(2) 0.053(2) 0.0127(16) -0.0254(14) -0.0144(15) C24 0.0454(16) 0.055(2) 0.064(2) 0.0036(18) -0.0278(16) -0.0191(16) O12 0.586(11) 0.651(17) 0.385(15) -0.033(13) -0.210(12) -0.444(12) O13 0.209(9) 0.48(2) 0.111(6) 0.052(9) -0.034(6) 0.038(12) O11 0.280(11) 0.260(12) 0.60(3) 0.131(14) -0.153(16) -0.149(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.941(3) 1_655 ? Zn1 O6 1.965(2) 1_565 ? Zn1 O1 2.020(5) . ? Zn1 N7 2.082(3) . ? Zn2 N10 2.104(4) . ? Zn2 N10 2.104(4) 2_557 ? Zn2 O5 2.122(3) 2_557 ? Zn2 O5 2.122(3) . ? Zn2 O10 2.135(3) 2_557 ? Zn2 O10 2.135(3) . ? O1 C21 1.264(5) . ? O2 C21 1.185(6) . ? O3 C24 1.229(6) . ? O3 Zn1 1.941(3) 1_455 ? O4 C24 1.231(6) . ? O5 C13 1.239(4) . ? O6 C13 1.256(4) . ? O6 Zn1 1.965(2) 1_545 ? O7 C16 1.214(5) . ? O8 C17 1.217(5) . ? O9 C18 1.215(4) . ? O10 H10 0.8201 . ? N1 C17 1.357(5) . ? N1 C16 1.389(6) . ? N1 C15 1.471(4) . ? N2 C18 1.380(6) . ? N2 C17 1.393(4) . ? N2 C22 1.466(5) . ? N3 C18 1.366(5) . ? N3 C16 1.384(4) . ? N3 C19 1.481(6) . ? N7 C8 1.313(5) . ? N7 C7 1.342(5) . ? N8 C7 1.318(6) . ? N8 N9 1.345(5) . ? N8 H7 0.9300 . ? N9 C8 1.311(5) . ? N9 C9 1.471(5) . ? N10 C6 1.330(6) . ? N10 C5 1.360(5) . ? N11 C5 1.299(7) . ? N11 N12 1.340(5) . ? N11 H5 0.9300 . ? N12 C6 1.329(5) . ? N12 C4 1.479(7) . ? C1 C3 1.350(5) 2_558 ? C1 C2 1.391(6) . ? C1 H1 0.9300 . ? C2 C3 1.383(7) . ? C2 C4 1.484(6) . ? C3 C1 1.350(5) 2_558 ? C3 H3 0.9300 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C6 H6 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.507(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C12 1.371(6) . ? C10 C11 1.377(5) . ? C11 C12 1.376(7) 2_675 ? C11 H11 0.9300 . ? C12 C11 1.376(7) 2_675 ? C12 H12 0.9300 . ? C13 C14 1.512(5) . ? C14 C15 1.523(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C19 C20 1.500(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.512(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C22 C23 1.508(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.518(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O6 116.04(14) 1_655 1_565 ? O3 Zn1 O1 107.34(15) 1_655 . ? O6 Zn1 O1 135.81(14) 1_565 . ? O3 Zn1 N7 97.59(13) 1_655 . ? O6 Zn1 N7 91.70(12) 1_565 . ? O1 Zn1 N7 90.65(15) . . ? N10 Zn2 N10 180.000(1) . 2_557 ? N10 Zn2 O5 88.55(12) . 2_557 ? N10 Zn2 O5 91.45(12) 2_557 2_557 ? N10 Zn2 O5 91.45(12) . . ? N10 Zn2 O5 88.55(12) 2_557 . ? O5 Zn2 O5 180.0 2_557 . ? N10 Zn2 O10 90.57(15) . 2_557 ? N10 Zn2 O10 89.43(15) 2_557 2_557 ? O5 Zn2 O10 94.52(12) 2_557 2_557 ? O5 Zn2 O10 85.48(12) . 2_557 ? N10 Zn2 O10 89.43(15) . . ? N10 Zn2 O10 90.57(15) 2_557 . ? O5 Zn2 O10 85.48(12) 2_557 . ? O5 Zn2 O10 94.52(12) . . ? O10 Zn2 O10 180.000(1) 2_557 . ? C21 O1 Zn1 103.2(3) . . ? C24 O3 Zn1 121.0(3) . 1_455 ? C13 O5 Zn2 138.7(2) . . ? C13 O6 Zn1 123.9(2) . 1_545 ? Zn2 O10 H10 109.4 . . ? C17 N1 C16 123.9(3) . . ? C17 N1 C15 118.5(3) . . ? C16 N1 C15 117.6(3) . . ? C18 N2 C17 123.4(3) . . ? C18 N2 C22 118.8(3) . . ? C17 N2 C22 117.8(4) . . ? C18 N3 C16 123.8(4) . . ? C18 N3 C19 119.3(3) . . ? C16 N3 C19 116.9(3) . . ? C8 N7 C7 104.6(3) . . ? C8 N7 Zn1 130.9(2) . . ? C7 N7 Zn1 124.4(3) . . ? C7 N8 N9 103.8(3) . . ? C7 N8 H7 127.8 . . ? N9 N8 H7 128.4 . . ? C8 N9 N8 109.6(3) . . ? C8 N9 C9 130.0(3) . . ? N8 N9 C9 120.3(3) . . ? C6 N10 C5 104.4(4) . . ? C6 N10 Zn2 126.3(2) . . ? C5 N10 Zn2 128.2(3) . . ? C5 N11 N12 104.5(4) . . ? C5 N11 H5 127.6 . . ? N12 N11 H5 127.9 . . ? C6 N12 N11 110.3(4) . . ? C6 N12 C4 128.7(4) . . ? N11 N12 C4 121.0(4) . . ? C3 C1 C2 121.2(4) 2_558 . ? C3 C1 H1 119.4 2_558 . ? C2 C1 H1 119.4 . . ? C3 C2 C1 117.2(3) . . ? C3 C2 C4 121.7(4) . . ? C1 C2 C4 121.1(4) . . ? C1 C3 C2 121.6(4) 2_558 . ? C1 C3 H3 119.2 2_558 . ? C2 C3 H3 119.2 . . ? N12 C4 C2 112.6(4) . . ? N12 C4 H4A 109.1 . . ? C2 C4 H4A 109.1 . . ? N12 C4 H4B 109.1 . . ? C2 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? N11 C5 N10 112.6(4) . . ? N10 C6 N12 108.3(3) . . ? N10 C6 H6 125.9 . . ? N12 C6 H6 125.9 . . ? N8 C7 N7 112.2(4) . . ? N9 C8 N7 109.8(3) . . ? N9 C8 H8 125.1 . . ? N7 C8 H8 125.1 . . ? N9 C9 C10 109.7(4) . . ? N9 C9 H9A 109.7 . . ? C10 C9 H9A 109.7 . . ? N9 C9 H9B 109.7 . . ? C10 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C12 C10 C11 118.8(4) . . ? C12 C10 C9 120.2(3) . . ? C11 C10 C9 121.0(4) . . ? C12 C11 C10 120.7(4) 2_675 . ? C12 C11 H11 119.7 2_675 . ? C10 C11 H11 119.7 . . ? C10 C12 C11 120.5(4) . 2_675 ? C10 C12 H12 119.7 . . ? C11 C12 H12 119.7 2_675 . ? O5 C13 O6 123.4(3) . . ? O5 C13 C14 119.8(3) . . ? O6 C13 C14 116.8(3) . . ? C13 C14 C15 113.0(3) . . ? C13 C14 H14A 109.0 . . ? C15 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C15 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? N1 C15 C14 112.9(3) . . ? N1 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? N1 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? O7 C16 N3 122.4(4) . . ? O7 C16 N1 121.6(3) . . ? N3 C16 N1 115.9(3) . . ? O8 C17 N1 122.6(3) . . ? O8 C17 N2 121.1(4) . . ? N1 C17 N2 116.3(4) . . ? O9 C18 N3 122.4(4) . . ? O9 C18 N2 121.1(4) . . ? N3 C18 N2 116.5(3) . . ? N3 C19 C20 111.0(3) . . ? N3 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? N3 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C19 C20 C21 112.4(4) . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? O2 C21 O1 120.6(5) . . ? O2 C21 C20 125.0(4) . . ? O1 C21 C20 114.4(4) . . ? N2 C22 C23 113.0(3) . . ? N2 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? N2 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C22 C23 C24 113.0(4) . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? O3 C24 O4 122.8(4) . . ? O3 C24 C23 117.4(4) . . ? O4 C24 C23 119.2(4) . . ? 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 O3 Zn1 O1 C21 110.9(3) 1_655 . . . ? O6 Zn1 O1 C21 -57.8(4) 1_565 . . . ? N7 Zn1 O1 C21 -150.9(3) . . . . ? N10 Zn2 O5 C13 -149.1(4) . . . . ? N10 Zn2 O5 C13 30.9(4) 2_557 . . . ? O5 Zn2 O5 C13 -33.6(4) 2_557 . . . ? O10 Zn2 O5 C13 120.5(4) 2_557 . . . ? O10 Zn2 O5 C13 -59.5(4) . . . . ? O3 Zn1 N7 C8 -122.9(4) 1_655 . . . ? O6 Zn1 N7 C8 -6.4(4) 1_565 . . . ? O1 Zn1 N7 C8 129.5(4) . . . . ? O3 Zn1 N7 C7 61.3(4) 1_655 . . . ? O6 Zn1 N7 C7 177.9(4) 1_565 . . . ? O1 Zn1 N7 C7 -46.3(4) . . . . ? C7 N8 N9 C8 0.8(5) . . . . ? C7 N8 N9 C9 -176.2(4) . . . . ? N10 Zn2 N10 C6 49(100) 2_557 . . . ? O5 Zn2 N10 C6 -43.0(4) 2_557 . . . ? O5 Zn2 N10 C6 137.0(4) . . . . ? O10 Zn2 N10 C6 -137.5(4) 2_557 . . . ? O10 Zn2 N10 C6 42.5(4) . . . . ? N10 Zn2 N10 C5 -145(100) 2_557 . . . ? O5 Zn2 N10 C5 122.8(4) 2_557 . . . ? O5 Zn2 N10 C5 -57.2(4) . . . . ? O10 Zn2 N10 C5 28.3(4) 2_557 . . . ? O10 Zn2 N10 C5 -151.7(4) . . . . ? C5 N11 N12 C6 -0.8(6) . . . . ? C5 N11 N12 C4 179.5(5) . . . . ? C3 C1 C2 C3 0.2(7) 2_558 . . . ? C3 C1 C2 C4 178.5(4) 2_558 . . . ? C1 C2 C3 C1 -0.2(7) . . . 2_558 ? C4 C2 C3 C1 -178.5(4) . . . 2_558 ? C6 N12 C4 C2 18.4(8) . . . . ? N11 N12 C4 C2 -161.9(5) . . . . ? C3 C2 C4 N12 -108.5(5) . . . . ? C1 C2 C4 N12 73.2(6) . . . . ? N12 N11 C5 N10 0.7(6) . . . . ? C6 N10 C5 N11 -0.3(6) . . . . ? Zn2 N10 C5 N11 -168.5(3) . . . . ? C5 N10 C6 N12 -0.2(5) . . . . ? Zn2 N10 C6 N12 168.3(3) . . . . ? N11 N12 C6 N10 0.6(5) . . . . ? C4 N12 C6 N10 -179.7(5) . . . . ? N9 N8 C7 N7 -0.7(6) . . . . ? C8 N7 C7 N8 0.3(6) . . . . ? Zn1 N7 C7 N8 176.9(3) . . . . ? N8 N9 C8 N7 -0.7(5) . . . . ? C9 N9 C8 N7 176.0(4) . . . . ? C7 N7 C8 N9 0.3(5) . . . . ? Zn1 N7 C8 N9 -176.1(3) . . . . ? C8 N9 C9 C10 -116.3(5) . . . . ? N8 N9 C9 C10 60.1(5) . . . . ? N9 C9 C10 C12 83.0(5) . . . . ? N9 C9 C10 C11 -96.0(5) . . . . ? C12 C10 C11 C12 0.0(8) . . . 2_675 ? C9 C10 C11 C12 179.1(4) . . . 2_675 ? C11 C10 C12 C11 0.0(8) . . . 2_675 ? C9 C10 C12 C11 -179.1(4) . . . 2_675 ? Zn2 O5 C13 O6 -144.3(3) . . . . ? Zn2 O5 C13 C14 37.1(6) . . . . ? Zn1 O6 C13 O5 7.4(6) 1_545 . . . ? Zn1 O6 C13 C14 -173.9(3) 1_545 . . . ? O5 C13 C14 C15 172.4(4) . . . . ? O6 C13 C14 C15 -6.3(6) . . . . ? C17 N1 C15 C14 -90.1(4) . . . . ? C16 N1 C15 C14 90.1(4) . . . . ? C13 C14 C15 N1 176.1(4) . . . . ? C18 N3 C16 O7 -178.9(4) . . . . ? C19 N3 C16 O7 -1.0(5) . . . . ? C18 N3 C16 N1 4.5(5) . . . . ? C19 N3 C16 N1 -177.6(3) . . . . ? C17 N1 C16 O7 177.5(3) . . . . ? C15 N1 C16 O7 -2.7(5) . . . . ? C17 N1 C16 N3 -5.8(5) . . . . ? C15 N1 C16 N3 174.0(3) . . . . ? C16 N1 C17 O8 -175.8(3) . . . . ? C15 N1 C17 O8 4.4(5) . . . . ? C16 N1 C17 N2 4.1(5) . . . . ? C15 N1 C17 N2 -175.7(3) . . . . ? C18 N2 C17 O8 179.0(3) . . . . ? C22 N2 C17 O8 -0.8(5) . . . . ? C18 N2 C17 N1 -1.0(5) . . . . ? C22 N2 C17 N1 179.2(3) . . . . ? C16 N3 C18 O9 179.4(4) . . . . ? C19 N3 C18 O9 1.6(6) . . . . ? C16 N3 C18 N2 -1.7(5) . . . . ? C19 N3 C18 N2 -179.5(3) . . . . ? C17 N2 C18 O9 178.7(3) . . . . ? C22 N2 C18 O9 -1.5(5) . . . . ? C17 N2 C18 N3 -0.2(5) . . . . ? C22 N2 C18 N3 179.6(3) . . . . ? C18 N3 C19 C20 -108.0(4) . . . . ? C16 N3 C19 C20 74.1(4) . . . . ? N3 C19 C20 C21 173.0(3) . . . . ? Zn1 O1 C21 O2 5.6(6) . . . . ? Zn1 O1 C21 C20 -175.6(3) . . . . ? C19 C20 C21 O2 -8.8(7) . . . . ? C19 C20 C21 O1 172.5(4) . . . . ? C18 N2 C22 C23 -90.2(4) . . . . ? C17 N2 C22 C23 89.6(4) . . . . ? N2 C22 C23 C24 166.1(4) . . . . ? Zn1 O3 C24 O4 -19.6(7) 1_455 . . . ? Zn1 O3 C24 C23 169.2(3) 1_455 . . . ? C22 C23 C24 O3 -32.6(6) . . . . ? C22 C23 C24 O4 155.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.840 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.199