# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2014 data_azopy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H45 N11 O13 Zn2' _chemical_formula_sum 'C41 H45 N11 O13 Zn2' _chemical_formula_weight 1030.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 11.0697(6) _cell_length_b 22.2083(11) _cell_length_c 19.5333(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4802.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6329 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details sadabs _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 128645 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.35 _reflns_number_total 11361 _reflns_number_gt 8870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_cell_refinement 'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0901P)^2^+15.9628P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.516(18) _refine_ls_number_reflns 11361 _refine_ls_number_parameters 604 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1906 _refine_ls_wR_factor_gt 0.1738 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.72752(6) 0.63248(3) 0.68133(3) 0.02656(16) Uani 1 1 d . . . Zn2 Zn 0.80492(6) 0.13126(3) 0.49058(3) 0.02707(17) Uani 1 1 d . . . O5 O 0.8272(5) 0.26409(19) 0.4631(3) 0.0356(11) Uani 1 1 d . . . O3 O 0.8228(4) 0.20137(18) 0.5519(2) 0.0333(10) Uani 1 1 d . . . O1 O 0.7526(5) 0.56950(17) 0.6130(3) 0.0386(11) Uani 1 1 d . . . O8 O 0.7582(5) 0.50565(19) 0.7003(2) 0.0347(11) Uani 1 1 d . . . O4 O 0.7905(5) 1.06920(19) 0.5614(3) 0.0448(13) Uani 1 1 d . . . N4 N 0.6511(5) 0.1383(2) 0.4357(3) 0.0315(12) Uani 1 1 d . . . O2 O 0.7013(4) 0.70247(19) 0.6213(3) 0.0340(10) Uani 1 1 d . . . O7 O 0.7028(5) 0.7649(2) 0.7103(3) 0.0372(12) Uani 1 1 d . . . O6 O 0.7692(4) 1.00650(18) 0.4727(2) 0.0348(10) Uani 1 1 d . . . N1 N 0.8807(5) 0.6399(2) 0.7366(3) 0.0292(12) Uani 1 1 d . . . N3 N 0.9534(5) 0.1235(2) 0.4320(3) 0.0278(11) Uani 1 1 d . . . N2 N 0.5780(5) 0.6236(2) 0.7399(3) 0.0271(11) Uani 1 1 d . . . O9 O 0.2736(6) 0.4875(2) 0.4081(3) 0.0535(14) Uani 1 1 d . . . C19 C 0.3914(6) 0.6624(3) 0.7798(4) 0.0314(14) Uani 1 1 d . . . H19 H 0.3353 0.6935 0.7797 0.038 Uiso 1 1 calc R . . C25 C 0.1603(6) 0.1106(3) 0.3507(3) 0.0284(13) Uani 1 1 d . . . N8 N 0.3499(5) 0.1464(2) 0.3073(3) 0.0336(12) Uani 1 1 d . . . C8 C 0.7008(6) 0.8052(3) 0.5979(4) 0.0341(15) Uani 1 1 d . . . H8 H 0.6889 0.7960 0.5519 0.041 Uiso 1 1 calc R . . N7 N 0.2578(5) 0.1025(2) 0.3096(3) 0.0302(12) Uani 1 1 d . . . C30 C 0.4446(6) 0.1428(3) 0.3501(3) 0.0276(13) Uani 1 1 d . . . C15 C 1.0880(5) 0.6441(3) 0.8197(3) 0.0267(13) Uani 1 1 d . . . C16 C 1.0738(5) 0.6005(3) 0.7686(4) 0.0306(14) Uani 1 1 d . . . H16 H 1.1331 0.5715 0.7614 0.037 Uiso 1 1 calc R . . N6 N 1.2716(5) 0.6037(2) 0.8616(3) 0.0330(12) Uani 1 1 d . . . C7 C 0.7012(6) 0.7552(3) 0.6481(4) 0.0281(14) Uani 1 1 d . . . C13 C 0.8954(6) 0.6823(3) 0.7857(4) 0.0332(14) Uani 1 1 d . . . H13 H 0.8344 0.7107 0.7916 0.040 Uiso 1 1 calc R . . N5 N 1.1839(5) 0.6475(2) 0.8623(3) 0.0350(12) Uani 1 1 d . . . C4 C 0.8035(6) 0.3610(3) 0.5580(4) 0.0313(14) Uani 1 1 d . . . H4 H 0.8004 0.3700 0.5115 0.038 Uiso 1 1 calc R . . C28 C 0.6375(6) 0.1809(3) 0.3862(3) 0.0325(14) Uani 1 1 d . . . H28 H 0.6984 0.2095 0.3810 0.039 Uiso 1 1 calc R . . C21 C 0.4593(6) 0.5661(3) 0.8169(4) 0.0325(14) Uani 1 1 d . . . H21 H 0.4493 0.5308 0.8420 0.039 Uiso 1 1 calc R . . C9 C 0.7165(6) 0.8626(3) 0.6154(4) 0.0330(15) Uani 1 1 d . . . H9 H 0.7190 0.8720 0.6618 0.040 Uiso 1 1 calc R . . C23 C 0.0369(6) 0.1670(2) 0.4264(3) 0.0273(13) Uani 1 1 d . . . H23 H 0.0238 0.2024 0.4507 0.033 Uiso 1 1 calc R . . C1 C 0.7619(6) 0.5165(2) 0.6398(3) 0.0293(14) Uani 1 1 d . . . C10 C 0.7298(6) 0.9110(3) 0.5671(4) 0.0350(16) Uani 1 1 d . . . H10 H 0.7195 0.9025 0.5209 0.042 Uiso 1 1 calc R . . C32 C 0.5592(6) 0.0988(3) 0.4423(3) 0.0294(14) Uani 1 1 d . . . H32 H 0.5662 0.0691 0.4756 0.035 Uiso 1 1 calc R . . C14 C 0.9932(6) 0.6860(3) 0.8265(3) 0.0355(15) Uani 1 1 d . . . H14 H 0.9982 0.7163 0.8592 0.043 Uiso 1 1 calc R . . C20 C 0.3714(5) 0.6111(3) 0.8196(3) 0.0287(13) Uani 1 1 d . . . N9 N 0.1295(7) 0.4282(3) 0.4597(4) 0.0544(17) Uani 1 1 d . . . C5 C 0.8179(6) 0.3039(3) 0.5763(4) 0.0332(15) Uani 1 1 d . . . H5 H 0.8251 0.2947 0.6226 0.040 Uiso 1 1 calc R . . C31 C 0.4568(6) 0.0993(2) 0.4034(4) 0.0292(13) Uani 1 1 d . . . H31 H 0.3956 0.0716 0.4116 0.035 Uiso 1 1 calc R . . C27 C -0.0253(6) 0.0723(3) 0.3954(4) 0.0329(14) Uani 1 1 d . . . H27 H -0.0812 0.0411 0.3980 0.039 Uiso 1 1 calc R . . C26 C 0.0746(6) 0.0645(3) 0.3551(4) 0.0360(15) Uani 1 1 d . . . H26 H 0.0853 0.0289 0.3307 0.043 Uiso 1 1 calc R . . O11 O 0.3506(8) -0.0005(3) 0.2470(4) 0.084(2) Uani 1 1 d . . . C17 C 0.9722(6) 0.6011(3) 0.7296(4) 0.0345(14) Uani 1 1 d . . . H17 H 0.9658 0.5722 0.6953 0.041 Uiso 1 1 calc R . . C6 C 0.8230(6) 0.2539(3) 0.5252(4) 0.0284(15) Uani 1 1 d . . . C24 C 0.1386(6) 0.1633(2) 0.3883(3) 0.0298(13) Uani 1 1 d . . . H24 H 0.1931 0.1951 0.3870 0.036 Uiso 1 1 calc R . . C29 C 0.5404(6) 0.1842(3) 0.3441(3) 0.0339(15) Uani 1 1 d . . . H29 H 0.5370 0.2141 0.3108 0.041 Uiso 1 1 calc R . . C12 C 0.7736(7) 1.0160(3) 0.5352(4) 0.0359(15) Uani 1 1 d . . . N10 N 0.3784(9) -0.0984(4) 0.2160(4) 0.077(2) Uani 1 1 d . . . C2 C 0.7794(7) 0.4673(3) 0.5880(4) 0.0355(15) Uani 1 1 d . . . H2 H 0.7814 0.4768 0.5417 0.043 Uiso 1 1 calc R . . C18 C 0.4930(6) 0.6666(3) 0.7412(3) 0.0323(14) Uani 1 1 d . . . H18 H 0.5042 0.7009 0.7146 0.039 Uiso 1 1 calc R . . C22 C 0.5590(6) 0.5738(3) 0.7780(3) 0.0315(14) Uani 1 1 d . . . H22 H 0.6170 0.5435 0.7774 0.038 Uiso 1 1 calc R . . C35 C 0.2324(8) 0.4384(3) 0.4250(4) 0.0481(19) Uani 1 1 d . . . H35 H 0.2771 0.4046 0.4124 0.058 Uiso 1 1 calc R . . C11 C 0.7560(7) 0.9672(3) 0.5849(4) 0.0383(16) Uani 1 1 d . . . H11 H 0.7637 0.9761 0.6312 0.046 Uiso 1 1 calc R . . O12 O 0.3374(9) 0.2846(4) 0.4164(4) 0.094(2) Uani 1 1 d . . . C3 C 0.7921(6) 0.4110(3) 0.6071(4) 0.0314(15) Uani 1 1 d . . . H3 H 0.7940 0.4023 0.6537 0.038 Uiso 1 1 calc R . . N11 N 0.4547(7) 0.2868(3) 0.5125(5) 0.072(2) Uani 1 1 d . . . C37 C 0.4671(11) 0.3513(5) 0.5092(8) 0.101(4) Uani 1 1 d . . . H37A H 0.5172 0.3649 0.5462 0.152 Uiso 1 1 calc R . . H37B H 0.3888 0.3696 0.5128 0.152 Uiso 1 1 calc R . . H37C H 0.5034 0.3623 0.4664 0.152 Uiso 1 1 calc R . . C34 C 0.1010(8) 0.3670(4) 0.4796(5) 0.074(3) Uani 1 1 d . . . H34A H 0.0255 0.3665 0.5039 0.111 Uiso 1 1 calc R . . H34B H 0.1637 0.3517 0.5087 0.111 Uiso 1 1 calc R . . H34C H 0.0947 0.3422 0.4395 0.111 Uiso 1 1 calc R . . C36 C 0.4977(10) 0.2534(7) 0.5766(9) 0.105(4) Uani 1 1 d . . . H36A H 0.5444 0.2802 0.6046 0.158 Uiso 1 1 calc R . . H36B H 0.5467 0.2197 0.5633 0.158 Uiso 1 1 calc R . . H36C H 0.4290 0.2393 0.6020 0.158 Uiso 1 1 calc R . . C33 C 0.0537(8) 0.4742(6) 0.4806(5) 0.087(3) Uani 1 1 d . . . H33A H -0.0143 0.4574 0.5045 0.130 Uiso 1 1 calc R . . H33B H 0.0258 0.4961 0.4413 0.130 Uiso 1 1 calc R . . H33C H 0.0968 0.5008 0.5106 0.130 Uiso 1 1 calc R . . C38 C 0.3871(10) 0.2593(5) 0.4645(6) 0.076(3) Uani 1 1 d . . . H38 H 0.3774 0.2178 0.4681 0.091 Uiso 1 1 calc R . . C41 C 0.3220(12) -0.0512(5) 0.2509(6) 0.077(3) Uani 1 1 d . . . H41 H 0.2571 -0.0606 0.2791 0.093 Uiso 1 1 calc R . . C40 C 0.4721(13) -0.0890(7) 0.1690(6) 0.118(5) Uani 1 1 d . . . H40A H 0.4981 -0.1270 0.1508 0.177 Uiso 1 1 calc R . . H40B H 0.5386 -0.0697 0.1917 0.177 Uiso 1 1 calc R . . H40C H 0.4438 -0.0639 0.1324 0.177 Uiso 1 1 calc R . . C39 C 0.348(2) -0.1606(5) 0.2251(10) 0.176(10) Uani 1 1 d . . . H39A H 0.3983 -0.1849 0.1960 0.264 Uiso 1 1 calc R . . H39B H 0.2649 -0.1669 0.2135 0.264 Uiso 1 1 calc R . . H39C H 0.3614 -0.1718 0.2720 0.264 Uiso 1 1 calc R . . O1W O 0.0733(9) -0.0698(4) 0.1964(5) 0.110(3) Uani 1 1 d . . . O2W O 0.0880(13) -0.1966(5) 0.1883(5) 0.153(5) 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 0.0368(3) 0.0154(3) 0.0275(4) -0.0006(3) 0.0019(3) 0.0017(2) Zn2 0.0372(3) 0.0135(3) 0.0304(4) 0.0004(3) 0.0026(3) -0.0012(2) O5 0.057(3) 0.017(2) 0.032(3) 0.0001(19) 0.006(2) 0.003(2) O3 0.055(3) 0.017(2) 0.029(2) -0.0016(18) 0.003(2) -0.0010(18) O1 0.068(3) 0.0126(19) 0.036(3) -0.0018(18) 0.003(2) 0.002(2) O8 0.048(3) 0.024(2) 0.032(3) -0.0028(18) 0.009(2) 0.0010(19) O4 0.077(4) 0.015(2) 0.042(3) 0.002(2) 0.011(3) -0.006(2) N4 0.040(3) 0.021(2) 0.033(3) 0.002(2) 0.005(2) -0.002(2) O2 0.050(3) 0.0161(19) 0.036(3) -0.0005(19) -0.002(2) 0.0013(18) O7 0.063(3) 0.020(2) 0.029(3) 0.0024(19) 0.002(2) 0.006(2) O6 0.041(3) 0.022(2) 0.042(3) 0.0076(19) 0.005(2) 0.0012(18) N1 0.038(3) 0.020(3) 0.030(3) -0.004(2) 0.002(2) 0.006(2) N3 0.027(3) 0.018(2) 0.038(3) -0.001(2) 0.001(2) 0.000(2) N2 0.034(3) 0.016(2) 0.031(3) -0.0006(19) 0.002(2) -0.0015(19) O9 0.078(4) 0.031(3) 0.051(3) 0.012(2) 0.007(3) 0.006(2) C19 0.032(3) 0.020(3) 0.042(4) 0.005(3) -0.006(3) 0.004(2) C25 0.039(3) 0.020(3) 0.027(3) 0.008(2) -0.004(3) -0.003(2) N8 0.040(3) 0.023(2) 0.038(3) 0.005(2) 0.001(2) -0.001(2) C8 0.052(4) 0.021(3) 0.029(4) 0.000(3) 0.007(3) -0.006(3) N7 0.027(3) 0.025(3) 0.039(3) 0.000(2) -0.001(2) 0.000(2) C30 0.035(3) 0.021(3) 0.027(3) 0.005(2) 0.008(2) 0.004(2) C15 0.027(3) 0.019(3) 0.033(3) 0.003(2) 0.003(2) 0.002(2) C16 0.026(3) 0.027(3) 0.039(4) -0.011(3) 0.004(3) 0.005(2) N6 0.024(3) 0.028(3) 0.047(4) 0.002(2) 0.003(2) 0.009(2) C7 0.033(3) 0.018(3) 0.034(4) 0.000(2) 0.006(3) 0.000(2) C13 0.038(3) 0.024(3) 0.037(4) -0.007(3) -0.001(3) 0.008(2) N5 0.038(3) 0.027(3) 0.040(3) -0.005(2) 0.002(2) 0.012(2) C4 0.051(4) 0.015(3) 0.027(4) -0.001(3) 0.002(3) -0.001(2) C28 0.042(4) 0.022(3) 0.034(4) 0.004(3) 0.009(3) -0.004(2) C21 0.042(4) 0.015(3) 0.041(4) 0.009(2) 0.003(3) 0.008(2) C9 0.038(4) 0.023(3) 0.038(4) 0.007(3) 0.005(3) -0.004(2) C23 0.035(3) 0.012(2) 0.035(4) 0.003(2) -0.003(2) 0.000(2) C1 0.036(3) 0.013(3) 0.038(4) -0.002(2) 0.004(3) -0.003(2) C10 0.042(4) 0.025(3) 0.038(4) 0.002(3) 0.005(3) -0.001(3) C32 0.032(3) 0.019(3) 0.036(4) 0.008(3) 0.005(3) -0.001(2) C14 0.054(4) 0.022(3) 0.031(4) -0.009(3) -0.001(3) 0.009(3) C20 0.028(3) 0.021(3) 0.036(4) -0.002(3) 0.001(2) 0.000(2) N9 0.061(4) 0.051(4) 0.051(4) 0.008(3) -0.020(3) -0.001(3) C5 0.049(4) 0.016(3) 0.034(4) -0.005(3) 0.003(3) 0.000(3) C31 0.042(4) 0.009(2) 0.036(4) 0.002(2) 0.005(3) 0.000(2) C27 0.040(4) 0.020(3) 0.039(4) -0.008(3) 0.004(3) -0.008(2) C26 0.034(3) 0.023(3) 0.051(4) -0.005(3) 0.004(3) -0.003(2) O11 0.126(6) 0.048(4) 0.079(5) -0.009(3) -0.019(5) 0.024(4) C17 0.039(3) 0.030(4) 0.034(4) -0.009(3) -0.003(3) 0.004(3) C6 0.035(3) 0.013(3) 0.037(4) -0.005(3) 0.001(3) -0.001(2) C24 0.036(3) 0.013(3) 0.041(4) 0.006(2) -0.003(3) 0.000(2) C29 0.041(4) 0.026(3) 0.034(4) 0.009(3) 0.005(3) -0.007(3) C12 0.046(4) 0.017(3) 0.045(4) 0.004(3) 0.006(3) 0.004(3) N10 0.101(7) 0.066(5) 0.063(5) -0.015(4) 0.015(5) 0.006(5) C2 0.054(4) 0.024(3) 0.029(3) -0.001(3) -0.001(3) 0.005(3) C18 0.040(3) 0.019(3) 0.038(4) 0.003(2) -0.005(3) 0.000(2) C22 0.037(3) 0.019(3) 0.039(4) 0.002(3) 0.004(3) 0.007(2) C35 0.061(5) 0.038(4) 0.045(4) 0.011(3) 0.001(4) -0.007(4) C11 0.061(4) 0.017(3) 0.037(4) 0.000(3) 0.013(3) 0.000(3) O12 0.124(7) 0.082(5) 0.076(5) 0.006(4) 0.001(5) 0.005(5) C3 0.048(4) 0.014(3) 0.032(4) -0.008(3) 0.008(3) 0.001(2) N11 0.063(5) 0.052(4) 0.099(6) -0.001(4) 0.022(4) 0.009(4) C37 0.078(7) 0.063(6) 0.162(13) 0.010(7) -0.040(8) -0.014(5) C34 0.067(6) 0.097(7) 0.057(5) 0.028(5) -0.028(4) -0.053(5) C36 0.049(6) 0.125(10) 0.142(11) 0.011(9) -0.007(7) 0.004(6) C33 0.050(5) 0.154(11) 0.057(6) 0.017(7) 0.002(4) 0.024(6) C38 0.083(7) 0.065(6) 0.080(7) -0.020(6) 0.032(6) -0.008(5) C41 0.107(8) 0.064(7) 0.062(6) 0.005(5) -0.011(6) 0.006(6) C40 0.123(11) 0.160(13) 0.073(8) 0.011(8) 0.012(7) 0.076(10) C39 0.32(3) 0.044(7) 0.167(15) -0.006(8) 0.104(18) -0.008(11) O1W 0.118(7) 0.105(7) 0.108(7) 0.009(5) 0.006(6) -0.007(5) O2W 0.219(13) 0.131(9) 0.109(8) 0.008(7) 0.065(9) -0.004(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 O1 1.953(4) . ? Zn1 O2 1.968(5) . ? Zn1 N1 2.016(5) . ? Zn1 N2 2.021(5) . ? Zn2 O4 1.959(5) 1_545 ? Zn2 O3 1.975(4) . ? Zn2 N3 2.010(6) . ? Zn2 N4 2.018(6) . ? O5 C6 1.235(8) . ? O3 C6 1.277(8) . ? O1 C1 1.293(7) . ? O8 C1 1.205(8) . ? O4 C12 1.302(8) . ? O4 Zn2 1.959(5) 1_565 ? N4 C32 1.350(8) . ? N4 C28 1.362(8) . ? O2 C7 1.283(8) . ? O7 C7 1.233(8) . ? O6 C12 1.239(9) . ? N1 C17 1.336(8) . ? N1 C13 1.356(8) . ? N3 C23 1.341(7) 1_655 ? N3 C27 1.364(8) 1_655 ? N2 C18 1.341(8) . ? N2 C22 1.350(8) . ? O9 C35 1.228(8) . ? C19 C18 1.357(10) . ? C19 C20 1.397(9) . ? C25 N7 1.358(9) . ? C25 C26 1.399(9) . ? C25 C24 1.401(9) . ? N8 C30 1.343(9) . ? N8 N7 1.411(8) . ? C8 C9 1.332(9) . ? C8 C7 1.481(9) . ? C30 C29 1.408(9) . ? C30 C31 1.426(9) . ? C15 N5 1.350(9) . ? C15 C16 1.400(9) . ? C15 C14 1.408(8) . ? C16 C17 1.359(10) . ? N6 N5 1.373(7) . ? N6 C20 1.385(9) 1_655 ? C13 C14 1.347(10) . ? C4 C5 1.327(9) . ? C4 C3 1.473(9) . ? C28 C29 1.357(10) . ? C21 C22 1.351(9) . ? C21 C20 1.397(8) . ? C9 C10 1.438(10) . ? C23 N3 1.341(7) 1_455 ? C23 C24 1.353(9) . ? C1 C2 1.502(9) . ? C10 C11 1.328(9) . ? C32 C31 1.365(9) . ? C20 N6 1.385(9) 1_455 ? N9 C35 1.345(11) . ? N9 C33 1.384(12) . ? N9 C34 1.450(10) . ? C5 C6 1.495(9) . ? C27 N3 1.364(8) 1_455 ? C27 C26 1.368(10) . ? O11 C41 1.171(13) . ? C12 C11 1.467(9) . ? N10 C41 1.399(13) . ? N10 C40 1.399(15) . ? N10 C39 1.433(15) . ? C2 C3 1.310(9) . ? O12 C38 1.226(13) . ? N11 C38 1.347(13) . ? N11 C37 1.440(12) . ? N11 C36 1.531(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 100.3(2) . . ? O1 Zn1 N1 107.7(2) . . ? O2 Zn1 N1 112.2(2) . . ? O1 Zn1 N2 115.6(2) . . ? O2 Zn1 N2 107.1(2) . . ? N1 Zn1 N2 113.2(2) . . ? O4 Zn2 O3 97.7(2) 1_545 . ? O4 Zn2 N3 114.1(2) 1_545 . ? O3 Zn2 N3 109.3(2) . . ? O4 Zn2 N4 111.1(2) 1_545 . ? O3 Zn2 N4 110.2(2) . . ? N3 Zn2 N4 113.2(2) . . ? C6 O3 Zn2 118.2(4) . . ? C1 O1 Zn1 112.7(4) . . ? C12 O4 Zn2 111.9(5) . 1_565 ? C32 N4 C28 115.9(6) . . ? C32 N4 Zn2 122.3(4) . . ? C28 N4 Zn2 121.6(5) . . ? C7 O2 Zn1 118.5(5) . . ? C17 N1 C13 115.4(6) . . ? C17 N1 Zn1 122.0(4) . . ? C13 N1 Zn1 122.5(4) . . ? C23 N3 C27 116.0(6) 1_655 1_655 ? C23 N3 Zn2 123.2(4) 1_655 . ? C27 N3 Zn2 120.7(4) 1_655 . ? C18 N2 C22 117.6(5) . . ? C18 N2 Zn1 121.1(4) . . ? C22 N2 Zn1 121.3(4) . . ? C18 C19 C20 119.8(6) . . ? N7 C25 C26 118.6(6) . . ? N7 C25 C24 123.8(6) . . ? C26 C25 C24 117.6(6) . . ? C30 N8 N7 120.3(5) . . ? C9 C8 C7 123.2(7) . . ? C25 N7 N8 120.1(5) . . ? N8 C30 C29 119.8(6) . . ? N8 C30 C31 124.6(6) . . ? C29 C30 C31 115.5(6) . . ? N5 C15 C16 124.4(5) . . ? N5 C15 C14 119.4(6) . . ? C16 C15 C14 116.1(6) . . ? C17 C16 C15 119.1(6) . . ? N5 N6 C20 119.0(5) . 1_655 ? O7 C7 O2 124.1(6) . . ? O7 C7 C8 121.4(6) . . ? O2 C7 C8 114.4(6) . . ? C14 C13 N1 123.9(6) . . ? C15 N5 N6 120.7(5) . . ? C5 C4 C3 123.8(7) . . ? C29 C28 N4 123.8(6) . . ? C22 C21 C20 120.0(6) . . ? C8 C9 C10 124.1(7) . . ? N3 C23 C24 125.1(6) 1_455 . ? O8 C1 O1 125.2(6) . . ? O8 C1 C2 121.2(5) . . ? O1 C1 C2 113.6(6) . . ? C11 C10 C9 123.6(7) . . ? N4 C32 C31 124.6(6) . . ? C13 C14 C15 120.2(6) . . ? N6 C20 C19 123.6(6) 1_455 . ? N6 C20 C21 119.6(6) 1_455 . ? C19 C20 C21 116.9(6) . . ? C35 N9 C33 122.6(8) . . ? C35 N9 C34 118.5(8) . . ? C33 N9 C34 118.7(9) . . ? C4 C5 C6 122.4(7) . . ? C32 C31 C30 119.4(5) . . ? N3 C27 C26 123.1(6) 1_455 . ? C27 C26 C25 119.4(6) . . ? N1 C17 C16 125.2(6) . . ? O5 C6 O3 124.7(6) . . ? O5 C6 C5 121.3(6) . . ? O3 C6 C5 114.0(6) . . ? C23 C24 C25 118.8(5) . . ? C28 C29 C30 120.8(6) . . ? O6 C12 O4 123.2(6) . . ? O6 C12 C11 121.4(6) . . ? O4 C12 C11 115.4(6) . . ? C41 N10 C40 122.5(10) . . ? C41 N10 C39 124.0(11) . . ? C40 N10 C39 113.5(11) . . ? C3 C2 C1 121.0(6) . . ? N2 C18 C19 122.9(6) . . ? N2 C22 C21 122.8(6) . . ? O9 C35 N9 126.8(8) . . ? C10 C11 C12 123.3(7) . . ? C2 C3 C4 122.8(7) . . ? C38 N11 C37 118.2(10) . . ? C38 N11 C36 121.5(9) . . ? C37 N11 C36 119.3(11) . . ? O12 C38 N11 125.1(10) . . ? O11 C41 N10 124.6(12) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.269 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.143 _database_code_depnum_ccdc_archive 'CCDC 973248' data_bpee _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H22 N2 O8 Zn' _chemical_formula_sum 'C18 H22 N2 O8 Zn' _chemical_formula_weight 459.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.2190(13) _cell_length_b 5.5243(3) _cell_length_c 18.4719(10) _cell_angle_alpha 90.00 _cell_angle_beta 115.962(2) _cell_angle_gamma 90.00 _cell_volume 2038.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.3 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.252 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4590 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details sadabs _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17871 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 28.32 _reflns_number_total 2548 _reflns_number_gt 2489 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_cell_refinement 'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0295P)^2^+2.0954P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2548 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.03681(3) 0.2500 0.01231(7) Uani 1 2 d S . . C7 C 0.64490(6) 0.6073(2) 0.33038(7) 0.0181(2) Uani 1 1 d . . . H7 H 0.6546 0.7372 0.3052 0.022 Uiso 1 1 calc R . . O1 O 0.49831(4) -0.18198(16) 0.16494(5) 0.01773(17) Uani 1 1 d . . . O2 O 0.56339(6) 0.0993(2) 0.15187(6) 0.0315(2) Uani 1 1 d . . . C4 C 0.61380(6) 0.2205(2) 0.39869(7) 0.0168(2) Uani 1 1 d . . . H4 H 0.6034 0.0878 0.4221 0.020 Uiso 1 1 calc R . . N1 N 0.57894(5) 0.25422(18) 0.31851(6) 0.01460(19) Uani 1 1 d . . . C1 C 0.53356(6) -0.0965(2) 0.13172(7) 0.0172(2) Uani 1 1 d . . . C6 C 0.68058(6) 0.5756(2) 0.41339(7) 0.0162(2) Uani 1 1 d . . . C5 C 0.66403(6) 0.3745(2) 0.44723(7) 0.0185(2) Uani 1 1 d . . . H5 H 0.6869 0.3450 0.5022 0.022 Uiso 1 1 calc R . . C8 C 0.59504(6) 0.4449(2) 0.28554(7) 0.0174(2) Uani 1 1 d . . . H8 H 0.5718 0.4689 0.2303 0.021 Uiso 1 1 calc R . . C3 C 0.49965(7) -0.4330(2) 0.03358(7) 0.0184(2) Uani 1 1 d . . . C2 C 0.53677(7) -0.2373(2) 0.06509(7) 0.0198(2) Uani 1 1 d . . . C9 C 0.73244(6) 0.7518(2) 0.45995(7) 0.0183(2) Uani 1 1 d . . . O1W O 0.76940(8) 0.1752(3) 0.33423(9) 0.0411(3) Uani 1 1 d . . . O2W O 0.68736(7) 0.1841(3) 0.16381(8) 0.0406(3) Uani 1 1 d . . . H1 H 0.5656(8) -0.178(3) 0.0440(10) 0.024(4) Uiso 1 1 d . . . H1A H 0.7425(12) 0.176(4) 0.2873(15) 0.051(7) Uiso 1 1 d . . . H2A H 0.6459(13) 0.171(5) 0.1567(14) 0.061(7) Uiso 1 1 d . . . H2B H 0.6915(13) 0.328(5) 0.1526(15) 0.063(7) Uiso 1 1 d . . . H1B H 0.7861(14) 0.306(6) 0.3395(16) 0.070(9) Uiso 1 1 d . . . H9 H 0.7404(9) 0.875(3) 0.4308(11) 0.028(4) Uiso 1 1 d . . . H3 H 0.4703(9) -0.488(3) 0.0554(10) 0.022(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01416(10) 0.01213(10) 0.00954(10) 0.000 0.00417(7) 0.000 C7 0.0212(6) 0.0147(5) 0.0173(5) -0.0004(4) 0.0074(5) -0.0017(4) O1 0.0235(4) 0.0176(4) 0.0145(4) -0.0015(3) 0.0105(3) 0.0005(3) O2 0.0465(6) 0.0260(5) 0.0307(5) -0.0144(4) 0.0250(5) -0.0162(5) C4 0.0180(5) 0.0181(5) 0.0141(5) 0.0000(4) 0.0069(4) -0.0004(4) N1 0.0152(4) 0.0142(4) 0.0130(4) -0.0015(4) 0.0049(4) 0.0007(4) C1 0.0216(6) 0.0171(5) 0.0130(5) -0.0007(4) 0.0076(5) 0.0015(4) C6 0.0152(5) 0.0168(5) 0.0164(5) -0.0043(4) 0.0067(4) -0.0003(4) C5 0.0185(5) 0.0228(6) 0.0121(5) -0.0012(4) 0.0049(4) -0.0015(5) C8 0.0205(6) 0.0146(5) 0.0137(5) -0.0005(4) 0.0043(5) 0.0007(4) C3 0.0246(6) 0.0186(6) 0.0160(6) -0.0024(5) 0.0126(5) -0.0016(5) C2 0.0269(6) 0.0199(6) 0.0180(6) -0.0036(5) 0.0148(5) -0.0033(5) C9 0.0179(5) 0.0185(5) 0.0183(6) -0.0033(4) 0.0076(5) -0.0025(4) O1W 0.0493(8) 0.0341(7) 0.0403(7) 0.0066(6) 0.0200(6) 0.0082(6) O2W 0.0387(7) 0.0369(7) 0.0502(7) 0.0021(6) 0.0232(6) -0.0049(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.9696(8) 2_655 ? Zn1 O1 1.9696(8) . ? Zn1 N1 2.0437(10) . ? Zn1 N1 2.0437(10) 2_655 ? C7 C8 1.3838(17) . ? C7 C6 1.3950(17) . ? O1 C1 1.2782(15) . ? O2 C1 1.2375(16) . ? C4 N1 1.3505(15) . ? C4 C5 1.3774(17) . ? N1 C8 1.3413(16) . ? C1 C2 1.4839(16) . ? C6 C5 1.4005(17) . ? C6 C9 1.4654(17) . ? C3 C2 1.3296(17) . ? C3 C3 1.450(2) 5_645 ? C9 C9 1.337(2) 7_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 104.29(5) 2_655 . ? O1 Zn1 N1 98.92(4) 2_655 . ? O1 Zn1 N1 124.48(4) . . ? O1 Zn1 N1 124.48(4) 2_655 2_655 ? O1 Zn1 N1 98.92(4) . 2_655 ? N1 Zn1 N1 108.02(6) . 2_655 ? C8 C7 C6 119.84(11) . . ? C1 O1 Zn1 110.76(8) . . ? N1 C4 C5 122.75(11) . . ? C8 N1 C4 117.86(10) . . ? C8 N1 Zn1 120.50(8) . . ? C4 N1 Zn1 121.52(8) . . ? O2 C1 O1 122.59(11) . . ? O2 C1 C2 119.57(11) . . ? O1 C1 C2 117.81(11) . . ? C7 C6 C5 117.14(11) . . ? C7 C6 C9 118.97(11) . . ? C5 C6 C9 123.89(11) . . ? C4 C5 C6 119.72(11) . . ? N1 C8 C7 122.69(11) . . ? C2 C3 C3 123.54(14) . 5_645 ? C3 C2 C1 122.92(11) . . ? C9 C9 C6 124.58(15) 7_666 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.417 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.056 _database_code_depnum_ccdc_archive 'CCDC 973249' data_3bpdh _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 N4 O4 Zn' _chemical_formula_sum 'C20 H18 N4 O4 Zn' _chemical_formula_weight 443.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.000(5) _cell_length_b 5.452(5) _cell_length_c 22.025(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 107.704(5) _cell_angle_gamma 90.000(5) _cell_volume 1830.3(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 28.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 1.379 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5516 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15873 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 28.36 _reflns_number_total 2292 _reflns_number_gt 2248 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_cell_refinement 'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0322P)^2^+1.9480P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2292 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 0.5000 0.09087(3) 0.7500 0.01256(7) Uani 1 2 d S . . C4 C 0.38147(8) -0.3095(2) 0.76446(6) 0.0167(2) Uani 1 1 d . . . H4 H 0.4117 -0.2911 0.8075 0.020 Uiso 1 1 calc R . . O1 O 0.51988(6) 0.31114(18) 0.82178(4) 0.01923(19) Uani 1 1 d . . . O2 O 0.46796(9) 0.0447(2) 0.87783(5) 0.0335(3) Uani 1 1 d . . . C6 C 0.27689(8) -0.5281(2) 0.68155(6) 0.0188(2) Uani 1 1 d . . . H6 H 0.2365 -0.6547 0.6681 0.023 Uiso 1 1 calc R . . N1 N 0.39714(7) -0.1512(2) 0.72253(5) 0.0152(2) Uani 1 1 d . . . C5 C 0.32179(8) -0.4993(3) 0.74563(6) 0.0194(2) Uani 1 1 d . . . H5 H 0.3120 -0.6062 0.7756 0.023 Uiso 1 1 calc R . . N2 N 0.27054(8) -0.2337(2) 0.53266(5) 0.0227(2) Uani 1 1 d . . . C9 C 0.24857(8) -0.3935(2) 0.56777(6) 0.0171(2) Uani 1 1 d . . . C7 C 0.29255(8) -0.3662(2) 0.63733(6) 0.0158(2) Uani 1 1 d . . . C1 C 0.49699(8) 0.2474(2) 0.87087(6) 0.0165(2) Uani 1 1 d . . . C8 C 0.35377(8) -0.1799(2) 0.66040(6) 0.0163(2) Uani 1 1 d . . . H8 H 0.3650 -0.0707 0.6314 0.020 Uiso 1 1 calc R . . C3 C 0.49326(8) 0.4066(2) 0.97569(6) 0.0166(2) Uani 1 1 d . . . C2 C 0.51006(8) 0.4417(2) 0.92045(6) 0.0169(2) Uani 1 1 d . . . C10 C 0.18518(10) -0.5999(3) 0.54569(7) 0.0238(3) Uani 1 1 d . . . H10A H 0.1618 -0.5959 0.5001 0.036 Uiso 1 1 calc R . . H10B H 0.1382 -0.5834 0.5641 0.036 Uiso 1 1 calc R . . H10C H 0.2148 -0.7531 0.5588 0.036 Uiso 1 1 calc R . . H1 H 0.5297(13) 0.592(3) 0.9105(10) 0.029(5) Uiso 1 1 d . . . H2 H 0.4727(11) 0.253(4) 0.9849(8) 0.025(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01600(11) 0.01342(11) 0.00757(10) 0.000 0.00256(7) 0.000 C4 0.0191(5) 0.0181(6) 0.0121(5) 0.0005(4) 0.0035(4) 0.0016(5) O1 0.0269(5) 0.0205(4) 0.0114(4) -0.0036(3) 0.0074(3) -0.0017(4) O2 0.0595(8) 0.0231(5) 0.0249(5) -0.0096(4) 0.0232(5) -0.0141(5) C6 0.0197(6) 0.0187(6) 0.0178(6) -0.0012(5) 0.0054(5) -0.0037(5) N1 0.0158(5) 0.0162(5) 0.0124(5) -0.0004(4) 0.0027(4) 0.0000(4) C5 0.0233(6) 0.0198(6) 0.0157(6) 0.0025(5) 0.0068(5) -0.0022(5) N2 0.0271(6) 0.0254(6) 0.0112(5) -0.0012(4) -0.0009(4) -0.0077(5) C9 0.0158(5) 0.0195(6) 0.0143(5) -0.0026(4) 0.0022(4) -0.0012(4) C7 0.0154(5) 0.0184(5) 0.0128(5) -0.0015(4) 0.0031(4) -0.0002(4) C1 0.0198(5) 0.0182(6) 0.0109(5) -0.0025(4) 0.0038(4) 0.0022(4) C8 0.0180(5) 0.0181(6) 0.0119(5) 0.0004(4) 0.0033(4) -0.0011(4) C3 0.0207(6) 0.0162(6) 0.0126(5) -0.0019(4) 0.0044(4) 0.0008(4) C2 0.0227(6) 0.0156(5) 0.0122(5) -0.0020(4) 0.0050(4) 0.0002(4) C10 0.0268(6) 0.0272(7) 0.0161(6) -0.0040(5) 0.0044(5) -0.0111(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.9332(12) . ? Zn1 O1 1.9332(12) 2_656 ? Zn1 N1 2.0521(14) . ? Zn1 N1 2.0521(14) 2_656 ? C4 N1 1.3422(17) . ? C4 C5 1.383(2) . ? O1 C1 1.2901(15) . ? O2 C1 1.2262(19) . ? C6 C5 1.3841(17) . ? C6 C7 1.3923(18) . ? N1 C8 1.3421(15) . ? N2 C9 1.2832(18) . ? N2 N2 1.400(2) 7_546 ? C9 C7 1.4863(17) . ? C9 C10 1.4937(19) . ? C7 C8 1.3953(18) . ? C1 C2 1.4898(18) . ? C3 C2 1.3373(17) . ? C3 C3 1.446(2) 5_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 103.19(8) . 2_656 ? O1 Zn1 N1 123.95(5) . . ? O1 Zn1 N1 103.93(5) 2_656 . ? O1 Zn1 N1 103.93(5) . 2_656 ? O1 Zn1 N1 123.95(5) 2_656 2_656 ? N1 Zn1 N1 99.95(8) . 2_656 ? N1 C4 C5 122.08(11) . . ? C1 O1 Zn1 120.00(9) . . ? C5 C6 C7 119.55(12) . . ? C8 N1 C4 118.67(11) . . ? C8 N1 Zn1 119.69(9) . . ? C4 N1 Zn1 120.77(9) . . ? C4 C5 C6 119.18(12) . . ? C9 N2 N2 113.83(14) . 7_546 ? N2 C9 C7 114.99(11) . . ? N2 C9 C10 126.79(12) . . ? C7 C9 C10 118.21(11) . . ? C6 C7 C8 117.55(12) . . ? C6 C7 C9 121.88(12) . . ? C8 C7 C9 120.54(11) . . ? O2 C1 O1 124.21(11) . . ? O2 C1 C2 121.55(12) . . ? O1 C1 C2 114.23(12) . . ? N1 C8 C7 122.97(11) . . ? C2 C3 C3 123.15(15) . 5_667 ? C3 C2 C1 122.87(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.429 _refine_diff_density_min -0.179 _refine_diff_density_rms 0.063 _database_code_depnum_ccdc_archive 'CCDC 973250' data_4bpdh _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H86 N20 O18 Zn4' _chemical_formula_sum 'C94 H86 N20 O18 Zn4' _chemical_formula_weight 2045.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7575(4) _cell_length_b 15.3180(6) _cell_length_c 29.3906(13) _cell_angle_alpha 81.1120(10) _cell_angle_beta 87.7110(10) _cell_angle_gamma 84.5360(10) _cell_volume 4761.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 28.4 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2108 _exptl_absorpt_coefficient_mu 1.073 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6669 _exptl_absorpt_correction_T_max 0.7448 _exptl_absorpt_process_details sadabs _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 135441 _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.42 _reflns_number_total 23865 _reflns_number_gt 15835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2010)' _computing_cell_refinement 'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0563P)^2^+3.2314P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23865 _refine_ls_number_parameters 1242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1147 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 0.27361(3) 0.64965(2) 0.691799(12) 0.01594(9) Uani 1 1 d . . . Zn4 Zn 0.30113(3) 0.87076(2) 0.179057(12) 0.01609(9) Uani 1 1 d . . . Zn3 Zn 0.20491(3) 1.14310(2) 0.190246(12) 0.01651(9) Uani 1 1 d . . . Zn2 Zn 0.23574(3) 0.39167(2) 0.683583(12) 0.01633(9) Uani 1 1 d . . . N5 N 0.1901(2) 1.09368(16) 0.26199(9) 0.0208(6) Uani 1 1 d . . . N1 N 0.2456(2) 0.60058(17) 0.76373(9) 0.0219(6) Uani 1 1 d . . . N2 N 0.2872(2) 0.70377(16) 0.61896(9) 0.0197(6) Uani 1 1 d . . . N8 N 0.2761(2) 0.81712(16) 0.25016(9) 0.0182(5) Uani 1 1 d . . . N3 N 0.2169(2) 0.33340(16) 0.75476(9) 0.0183(6) Uani 1 1 d . . . N4 N 0.2600(2) 0.44175(18) 0.61158(9) 0.0231(6) Uani 1 1 d . . . O9 O 0.3099(2) 1.26608(16) 0.20332(9) 0.0338(6) Uani 1 1 d . . . O1 O 0.1899(2) 0.79567(15) 0.69770(8) 0.0283(5) Uani 1 1 d . . . O16 O 0.4108(2) 0.75120(14) 0.16935(8) 0.0262(5) Uani 1 1 d . . . O6 O 0.41003(19) 0.41831(14) 0.69598(7) 0.0208(5) Uani 1 1 d . . . N13 N 0.2563(3) 0.10749(18) 0.95382(9) 0.0262(6) Uani 1 1 d . . . O12 O 0.3672(2) 1.06957(15) 0.18156(8) 0.0307(6) Uani 1 1 d . . . O11 O 0.05136(19) 1.08478(14) 0.17797(8) 0.0221(5) Uani 1 1 d . . . O7 O 0.1480(2) 0.28671(14) 0.66787(8) 0.0252(5) Uani 1 1 d . . . O4 O 0.42351(19) 0.56508(14) 0.68172(8) 0.0243(5) Uani 1 1 d . . . O15 O 0.2090(2) 0.74303(15) 0.16594(8) 0.0270(5) Uani 1 1 d . . . O8 O 0.3481(2) 1.24194(15) 0.67309(9) 0.0328(6) Uani 1 1 d . . . O5 O 0.0814(2) 0.47568(14) 0.69245(8) 0.0242(5) Uani 1 1 d . . . O10 O 0.1072(2) 1.26647(14) 0.19679(8) 0.0263(5) Uani 1 1 d . . . O3 O 0.09825(19) 0.62212(14) 0.68110(8) 0.0246(5) Uani 1 1 d . . . O14 O 0.1314(2) 0.94335(15) 0.18750(8) 0.0272(5) Uani 1 1 d . . . N14 N 0.2677(3) 0.14849(18) 0.90886(9) 0.0263(6) Uani 1 1 d . . . N6 N 0.2322(2) 0.19785(17) 1.11788(9) 0.0208(6) Uani 1 1 d . . . N7 N 0.2987(2) 0.92099(17) 0.10685(9) 0.0227(6) Uani 1 1 d . . . N16 N 0.2867(3) 0.61496(19) 0.45531(9) 0.0263(6) Uani 1 1 d . . . N11 N 0.2148(3) 0.8768(2) 0.46307(10) 0.0337(7) Uani 1 1 d . . . C89 C 0.6877(4) 0.8600(3) 0.54295(16) 0.0544(12) Uani 1 1 d . . . C54 C 0.1847(3) 0.2392(2) 0.84347(10) 0.0183(6) Uani 1 1 d . . . C41 C 0.3041(3) 0.7836(2) 0.52647(11) 0.0245(7) Uani 1 1 d . . . N15 N 0.3085(3) 0.64938(18) 0.40952(9) 0.0255(6) Uani 1 1 d . . . O2 O 0.3879(2) 0.74778(14) 0.70463(8) 0.0314(6) Uani 1 1 d . . . C48 C 0.1567(3) 1.0190(2) 0.35455(11) 0.0227(7) Uani 1 1 d . . . O1W O 0.5595(3) 1.2876(2) 0.19214(10) 0.0561(8) Uani 1 1 d . . . O13 O 0.45327(19) 0.93063(14) 0.19170(8) 0.0241(5) Uani 1 1 d . . . C27 C 0.1842(3) 0.5281(2) 0.85444(11) 0.0227(7) Uani 1 1 d . . . C55 C 0.3028(3) 0.2460(2) 0.82284(11) 0.0207(7) Uani 1 1 d . . . H55 H 0.3732 0.2187 0.8384 0.025 Uiso 1 1 calc R . . C67 C 0.1389(3) 0.7567(2) 0.31031(11) 0.0236(7) Uani 1 1 d . . . H67 H 0.0582 0.7438 0.3197 0.028 Uiso 1 1 calc R . . C57 C 0.1686(3) 0.1883(2) 0.89007(11) 0.0235(7) Uani 1 1 d . . . C66 C 0.1632(3) 0.7959(2) 0.26614(11) 0.0233(7) Uani 1 1 d . . . H66 H 0.0971 0.8085 0.2460 0.028 Uiso 1 1 calc R . . O2W O 0.6408(3) 0.7678(2) 0.69388(11) 0.0573(8) Uani 1 1 d . . . C18 C 0.3179(3) 0.7070(2) 0.16803(11) 0.0229(7) Uani 1 1 d . . . C68 C 0.2368(3) 0.7363(2) 0.34121(11) 0.0209(7) Uani 1 1 d . . . N10 N 0.1921(3) 0.3755(2) 0.96110(10) 0.0373(8) Uani 1 1 d . . . N12 N 0.2281(3) 0.9169(2) 0.41711(10) 0.0345(7) Uani 1 1 d . . . C44 C 0.3128(3) 0.8273(2) 0.47765(12) 0.0267(8) Uani 1 1 d . . . C22 C -0.1884(3) 1.0243(2) 0.19312(11) 0.0203(7) Uani 1 1 d . . . H22 H -0.1817 1.0842 0.1938 0.024 Uiso 1 1 calc R . . C71 C 0.2144(3) 0.6931(2) 0.38896(11) 0.0235(7) Uani 1 1 d . . . C23 C -0.0845(3) 0.9713(2) 0.19096(11) 0.0230(7) Uani 1 1 d . . . H23 H -0.0917 0.9108 0.1930 0.028 Uiso 1 1 calc R . . C70 C 0.3706(3) 0.79775(19) 0.27955(10) 0.0172(6) Uani 1 1 d . . . H70 H 0.4501 0.8117 0.2691 0.021 Uiso 1 1 calc R . . C10 C 0.6852(3) 0.5315(2) 0.69163(11) 0.0192(7) Uani 1 1 d . . . C9 C -0.1801(3) 0.5125(2) 0.69236(11) 0.0199(7) Uani 1 1 d . . . H9 H -0.1479 0.4536 0.6937 0.024 Uiso 1 1 calc R . . C56 C 0.3148(3) 0.2933(2) 0.77937(11) 0.0189(7) Uani 1 1 d . . . H56 H 0.3946 0.2978 0.7663 0.023 Uiso 1 1 calc R . . C2 C 0.3368(3) 0.9024(2) 0.69681(12) 0.0268(8) Uani 1 1 d . . . H2 H 0.4195 0.9106 0.7018 0.032 Uiso 1 1 calc R . . N9 N 0.2183(3) 0.4152(2) 0.91632(10) 0.0397(8) Uani 1 1 d . . . C20 C 0.5827(3) 1.0466(2) 0.19139(11) 0.0199(7) Uani 1 1 d . . . H20 H 0.5864 1.1070 0.1911 0.024 Uiso 1 1 calc R . . C32 C 0.2846(3) 0.3228(2) 0.97832(11) 0.0257(7) Uani 1 1 d . . . C69 C 0.3550(3) 0.75790(19) 0.32472(11) 0.0194(7) Uani 1 1 d . . . H69 H 0.4230 0.7456 0.3440 0.023 Uiso 1 1 calc R . . N20 N 0.5520(3) 0.9688(3) 0.50066(13) 0.0511(10) Uani 1 1 d . . . C33 C 0.4056(3) 0.3047(2) 0.95345(12) 0.0329(8) Uani 1 1 d . . . H33A H 0.3917 0.3106 0.9210 0.049 Uiso 1 1 calc R . . H33B H 0.4406 0.2456 0.9644 0.049 Uiso 1 1 calc R . . H33C H 0.4625 0.3464 0.9589 0.049 Uiso 1 1 calc R . . C30 C 0.1525(3) 0.4870(2) 0.90219(12) 0.0286(8) Uani 1 1 d . . . C53 C 0.0826(3) 0.2817(2) 0.81818(11) 0.0229(7) Uani 1 1 d . . . H53 H 0.0018 0.2793 0.8306 0.028 Uiso 1 1 calc R . . C1 C 0.3008(3) 0.8107(2) 0.70023(11) 0.0259(8) Uani 1 1 d . . . C46 C 0.1406(3) 0.9771(2) 0.40309(11) 0.0271(8) Uani 1 1 d . . . C37 C 0.3459(3) 0.2081(2) 1.09906(12) 0.0294(8) Uani 1 1 d . . . H37 H 0.4149 0.1886 1.1172 0.035 Uiso 1 1 calc R . . C94 C 0.1034(3) 0.3267(2) 0.77488(11) 0.0232(7) Uani 1 1 d . . . H94 H 0.0346 0.3543 0.7585 0.028 Uiso 1 1 calc R . . C21 C 0.6882(3) 0.9940(2) 0.19451(11) 0.0208(7) Uani 1 1 d . . . H21 H 0.6823 0.9331 0.1978 0.025 Uiso 1 1 calc R . . C34 C 0.2655(3) 0.2788(2) 1.02624(11) 0.0245(7) Uani 1 1 d . . . C49 C 0.0765(3) 1.0882(2) 0.33355(11) 0.0282(8) Uani 1 1 d . . . H49 H 0.0091 1.1112 0.3502 0.034 Uiso 1 1 calc R . . C28 C 0.2745(4) 0.4866(2) 0.82856(12) 0.0314(8) Uani 1 1 d . . . H28 H 0.3164 0.4330 0.8411 0.038 Uiso 1 1 calc R . . C8 C -0.0999(3) 0.5736(2) 0.69118(11) 0.0204(7) Uani 1 1 d . . . H8 H -0.1322 0.6318 0.6920 0.025 Uiso 1 1 calc R . . C24 C 0.0426(3) 1.0017(2) 0.18548(10) 0.0181(6) Uani 1 1 d . . . C13 C 0.2030(3) 1.3063(2) 0.19910(11) 0.0250(7) Uani 1 1 d . . . C11 C 0.6074(3) 0.4687(2) 0.69246(11) 0.0193(7) Uani 1 1 d . . . C3 C 0.2568(3) 0.9730(2) 0.68702(12) 0.0274(8) Uani 1 1 d . . . H3 H 0.1742 0.9635 0.6829 0.033 Uiso 1 1 calc R . . C81 C 0.2755(5) 0.6766(5) 0.99252(19) 0.086(2) Uani 1 1 d . . . H81 H 0.2925 0.6448 1.0215 0.103 Uiso 1 1 calc R . . C61 C 0.3045(3) -0.0102(2) 1.01242(12) 0.0295(8) Uani 1 1 d . . . C76 C 0.2065(4) 0.5424(2) 0.54349(12) 0.0381(10) Uani 1 1 d . . . H76 H 0.1574 0.5923 0.5301 0.046 Uiso 1 1 calc R . . C29 C 0.3026(4) 0.5240(2) 0.78443(12) 0.0322(9) Uani 1 1 d . . . H29 H 0.3644 0.4946 0.7679 0.039 Uiso 1 1 calc R . . C7 C 0.0373(3) 0.5551(2) 0.68861(10) 0.0175(6) Uani 1 1 d . . . C75 C 0.2930(4) 0.4997(2) 0.51708(12) 0.0309(8) Uani 1 1 d . . . C73 C 0.3107(4) 0.5319(2) 0.46731(12) 0.0352(9) Uani 1 1 d . . . C38 C 0.3662(3) 0.2461(2) 1.05419(12) 0.0304(8) Uani 1 1 d . . . H38 H 0.4474 0.2500 1.0425 0.036 Uiso 1 1 calc R . . C36 C 0.1351(3) 0.2280(2) 1.09088(11) 0.0258(7) Uani 1 1 d . . . H36 H 0.0550 0.2212 1.1032 0.031 Uiso 1 1 calc R . . C6 C 0.2371(3) 1.2264(2) 0.67032(12) 0.0243(7) Uani 1 1 d . . . C42 C 0.4082(3) 0.7410(2) 0.54997(12) 0.0277(8) Uani 1 1 d . . . H42 H 0.4860 0.7381 0.5350 0.033 Uiso 1 1 calc R . . C40 C 0.1916(3) 0.7842(2) 0.55093(12) 0.0290(8) Uani 1 1 d . . . H40 H 0.1193 0.8120 0.5368 0.035 Uiso 1 1 calc R . . C12 C 0.4689(3) 0.4862(2) 0.68973(10) 0.0167(6) Uani 1 1 d . . . C62 C 0.2288(4) 0.0286(2) 1.04372(13) 0.0359(9) Uani 1 1 d . . . H62 H 0.1766 0.0794 1.0338 0.043 Uiso 1 1 calc R . . C4 C 0.2873(3) 1.0639(2) 0.68221(12) 0.0281(8) Uani 1 1 d . . . H4 H 0.3700 1.0739 0.6859 0.034 Uiso 1 1 calc R . . C50 C 0.0966(3) 1.1233(2) 0.28782(11) 0.0260(7) Uani 1 1 d . . . H50 H 0.0416 1.1700 0.2746 0.031 Uiso 1 1 calc R . . C39 C 0.1864(3) 0.7440(2) 0.59597(11) 0.0262(8) Uani 1 1 d . . . H39 H 0.1093 0.7446 0.6114 0.031 Uiso 1 1 calc R . . C19 C 0.4587(3) 1.0128(2) 0.18828(10) 0.0184(6) Uani 1 1 d . . . C16 C 0.2574(3) 1.5540(2) 0.17994(12) 0.0302(8) Uani 1 1 d . . . H16 H 0.1751 1.5786 0.1812 0.036 Uiso 1 1 calc R . . C43 C 0.3956(3) 0.7031(2) 0.59548(11) 0.0249(7) Uani 1 1 d . . . H43 H 0.4666 0.6756 0.6105 0.030 Uiso 1 1 calc R . . C45 C 0.4314(3) 0.8118(2) 0.45039(12) 0.0300(8) Uani 1 1 d . . . H45A H 0.4168 0.8314 0.4183 0.045 Uiso 1 1 calc R . . H45B H 0.4588 0.7496 0.4551 0.045 Uiso 1 1 calc R . . H45C H 0.4946 0.8443 0.4603 0.045 Uiso 1 1 calc R . . C35 C 0.1474(3) 0.2685(2) 1.04601(12) 0.0283(8) Uani 1 1 d . . . H35 H 0.0768 0.2890 1.0289 0.034 Uiso 1 1 calc R . . C72 C 0.0856(3) 0.7028(3) 0.41014(13) 0.0464(11) Uani 1 1 d . . . H72A H 0.0370 0.6586 0.4017 0.070 Uiso 1 1 calc R . . H72B H 0.0463 0.7608 0.3993 0.070 Uiso 1 1 calc R . . H72C H 0.0909 0.6951 0.4431 0.070 Uiso 1 1 calc R . . C15 C 0.2773(3) 1.4578(2) 0.18673(12) 0.0283(8) Uani 1 1 d . . . H15 H 0.3590 1.4320 0.1855 0.034 Uiso 1 1 calc R . . C59 C 0.3087(4) 0.0291(2) 0.96310(12) 0.0337(9) Uani 1 1 d . . . C26 C 0.1274(3) 0.6080(2) 0.83328(12) 0.0292(8) Uani 1 1 d . . . H26 H 0.0672 0.6397 0.8494 0.035 Uiso 1 1 calc R . . C14 C 0.1870(3) 1.4051(2) 0.19446(12) 0.0297(8) Uani 1 1 d . . . H14 H 0.1062 1.4316 0.1973 0.036 Uiso 1 1 calc R . . C17 C 0.3441(3) 0.6092(2) 0.17226(13) 0.0317(8) Uani 1 1 d . . . H17 H 0.4265 0.5860 0.1693 0.038 Uiso 1 1 calc R . . N19 N 0.4534(4) 0.5358(3) 0.99845(15) 0.0686(13) Uani 1 1 d . . . C25 C 0.1591(3) 0.6410(2) 0.78866(12) 0.0292(8) Uani 1 1 d . . . H25 H 0.1180 0.6944 0.7752 0.035 Uiso 1 1 calc R . . C52 C 0.2552(4) 0.9886(2) 0.32751(12) 0.0331(9) Uani 1 1 d . . . H52 H 0.3122 0.9424 0.3399 0.040 Uiso 1 1 calc R . . C51 C 0.2684(3) 1.0268(2) 0.28254(12) 0.0299(8) Uani 1 1 d . . . H51 H 0.3353 1.0053 0.2652 0.036 Uiso 1 1 calc R . . C31 C 0.0538(4) 0.5315(3) 0.92972(15) 0.0599(14) Uani 1 1 d . . . H31A H 0.0791 0.5875 0.9349 0.090 Uiso 1 1 calc R . . H31B H 0.0413 0.4948 0.9588 0.090 Uiso 1 1 calc R . . H31C H -0.0228 0.5411 0.9133 0.090 Uiso 1 1 calc R . . C82 C 0.3379(5) 0.6518(4) 0.95372(17) 0.0660(16) Uani 1 1 d . . . C65 C 0.2294(4) 0.9934(2) 0.08950(12) 0.0332(9) Uani 1 1 d . . . H65 H 0.1777 1.0223 0.1097 0.040 Uiso 1 1 calc R . . C58 C 0.0421(4) 0.1862(4) 0.91242(14) 0.0616(15) Uani 1 1 d . . . H58A H -0.0051 0.1471 0.8989 0.092 Uiso 1 1 calc R . . H58B H -0.0001 0.2449 0.9080 0.092 Uiso 1 1 calc R . . H58C H 0.0498 0.1654 0.9448 0.092 Uiso 1 1 calc R . . C5 C 0.2055(3) 1.1334(2) 0.67288(13) 0.0287(8) Uani 1 1 d . . . H5 H 0.1236 1.1238 0.6676 0.034 Uiso 1 1 calc R . . C77 C 0.1921(4) 0.5116(2) 0.58963(12) 0.0375(9) Uani 1 1 d . . . H77 H 0.1314 0.5413 0.6065 0.045 Uiso 1 1 calc R . . N17 N 0.1563(5) 0.7987(4) 0.9472(2) 0.1037(19) Uani 1 1 d . . . C64 C 0.3717(5) 0.8823(3) 0.07702(14) 0.0663(17) Uani 1 1 d . . . H64 H 0.4225 0.8315 0.0880 0.080 Uiso 1 1 calc R . . C47 C 0.0323(4) 1.0077(3) 0.43133(14) 0.0560(13) Uani 1 1 d . . . H47A H 0.0402 1.0675 0.4361 0.084 Uiso 1 1 calc R . . H47B H 0.0304 0.9698 0.4606 0.084 Uiso 1 1 calc R . . H47C H -0.0436 1.0056 0.4156 0.084 Uiso 1 1 calc R . . C74 C 0.3532(6) 0.4690(3) 0.43490(15) 0.084(2) Uani 1 1 d . . . H74A H 0.2839 0.4388 0.4278 0.127 Uiso 1 1 calc R . . H74B H 0.4171 0.4264 0.4489 0.127 Uiso 1 1 calc R . . H74C H 0.3861 0.5011 0.4071 0.127 Uiso 1 1 calc R . . C88 C 0.5800(4) 0.9283(3) 0.54112(15) 0.0503(12) Uani 1 1 d . . . C85 C 0.4342(5) 0.5760(4) 0.95750(17) 0.0649(15) Uani 1 1 d . . . C93 C 0.7282(5) 0.8085(4) 0.58360(18) 0.0648(15) Uani 1 1 d . . . H93 H 0.6885 0.8167 0.6115 0.078 Uiso 1 1 calc R . . C60 C 0.3736(5) -0.0217(3) 0.92798(14) 0.0690(17) Uani 1 1 d . . . H60A H 0.3191 -0.0624 0.9196 0.103 Uiso 1 1 calc R . . H60B H 0.4482 -0.0541 0.9407 0.103 Uiso 1 1 calc R . . H60C H 0.3950 0.0188 0.9012 0.103 Uiso 1 1 calc R . . C83 C 0.3068(5) 0.7029(4) 0.91167(19) 0.0726(17) Uani 1 1 d . . . H83 H 0.3468 0.6900 0.8845 0.087 Uiso 1 1 calc R . . C63 C 0.3761(5) -0.0863(3) 1.03045(15) 0.0732(18) Uani 1 1 d . . . H63 H 0.4279 -0.1168 1.0110 0.088 Uiso 1 1 calc R . . C86 C 0.5037(5) 0.5528(4) 0.91450(16) 0.0770(17) Uani 1 1 d . . . H86A H 0.5628 0.5023 0.9226 0.115 Uiso 1 1 calc R . . H86B H 0.5472 0.6024 0.9003 0.115 Uiso 1 1 calc R . . H86C H 0.4454 0.5392 0.8933 0.115 Uiso 1 1 calc R . . C92 C 0.8268(6) 0.7456(4) 0.5824(2) 0.0822(18) Uani 1 1 d . . . H92 H 0.8523 0.7128 0.6103 0.099 Uiso 1 1 calc R . . C79 C 0.3641(5) 0.4273(3) 0.54006(14) 0.0651(16) Uani 1 1 d . . . H79 H 0.4249 0.3960 0.5240 0.078 Uiso 1 1 calc R . . C87 C 0.5113(5) 0.9433(3) 0.58523(15) 0.0633(14) Uani 1 1 d . . . H87A H 0.4816 0.8887 0.6001 0.095 Uiso 1 1 calc R . . H87B H 0.4417 0.9870 0.5785 0.095 Uiso 1 1 calc R . . H87C H 0.5668 0.9640 0.6052 0.095 Uiso 1 1 calc R . . C78 C 0.3448(4) 0.4016(3) 0.58655(14) 0.0548(13) Uani 1 1 d . . . H78 H 0.3945 0.3531 0.6011 0.066 Uiso 1 1 calc R . . C80 C 0.1875(5) 0.7493(6) 0.9875(2) 0.111(3) Uani 1 1 d . . . H80 H 0.1471 0.7650 1.0140 0.133 Uiso 1 1 calc R . . C91 C 0.8501(5) 0.7781(5) 0.5059(2) 0.100(2) Uani 1 1 d . . . H91 H 0.8923 0.7682 0.4787 0.120 Uiso 1 1 calc R . . N18 N 0.8887(5) 0.7277(4) 0.5447(2) 0.0942(17) Uani 1 1 d . . . C90 C 0.7521(5) 0.8440(4) 0.50286(18) 0.0779(18) Uani 1 1 d . . . H90 H 0.7300 0.8767 0.4745 0.094 Uiso 1 1 calc R . . C84 C 0.2172(6) 0.7720(5) 0.9107(2) 0.087(2) Uani 1 1 d . . . H84 H 0.1965 0.8036 0.8820 0.104 Uiso 1 1 calc R . . H10 H 0.655(3) 0.594(2) 0.6912(10) 0.019(8) Uiso 1 1 d . . . H11 H 0.638(4) 0.406(3) 0.6945(13) 0.048(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01556(18) 0.01440(17) 0.01687(19) 0.00223(14) -0.00143(14) -0.00329(13) Zn4 0.01493(18) 0.01608(17) 0.01571(19) 0.00318(14) -0.00048(14) -0.00246(13) Zn3 0.01739(18) 0.01355(17) 0.01718(19) 0.00276(14) -0.00094(14) -0.00227(14) Zn2 0.01531(18) 0.01634(18) 0.01646(19) 0.00337(14) -0.00164(14) -0.00599(14) N5 0.0257(15) 0.0160(13) 0.0194(15) 0.0025(11) -0.0009(12) -0.0031(11) N1 0.0256(15) 0.0206(14) 0.0191(15) 0.0007(11) -0.0018(12) -0.0055(11) N2 0.0205(14) 0.0191(13) 0.0176(14) 0.0030(11) -0.0011(11) -0.0013(11) N8 0.0167(13) 0.0182(13) 0.0181(14) 0.0030(11) -0.0011(11) -0.0028(10) N3 0.0145(13) 0.0191(13) 0.0199(14) 0.0024(11) -0.0025(11) -0.0031(10) N4 0.0236(15) 0.0256(15) 0.0185(15) 0.0035(12) -0.0005(12) -0.0053(12) O9 0.0315(14) 0.0280(13) 0.0411(16) -0.0027(12) -0.0060(12) -0.0005(11) O1 0.0294(13) 0.0224(12) 0.0338(14) -0.0029(10) 0.0035(11) -0.0102(10) O16 0.0227(12) 0.0240(12) 0.0311(14) -0.0002(10) 0.0001(10) -0.0050(10) O6 0.0150(11) 0.0245(12) 0.0221(12) 0.0025(9) -0.0022(9) -0.0076(9) N13 0.0322(16) 0.0274(15) 0.0146(14) 0.0065(12) 0.0004(12) 0.0032(13) O12 0.0183(12) 0.0321(13) 0.0342(15) 0.0118(11) 0.0046(10) 0.0073(10) O11 0.0167(11) 0.0209(11) 0.0280(13) 0.0024(10) -0.0037(9) -0.0064(9) O7 0.0262(13) 0.0171(11) 0.0316(14) -0.0006(10) 0.0000(10) -0.0044(10) O4 0.0174(11) 0.0173(11) 0.0355(14) 0.0022(10) 0.0023(10) 0.0012(9) O15 0.0186(12) 0.0253(12) 0.0358(15) -0.0010(11) -0.0009(10) -0.0021(10) O8 0.0272(13) 0.0242(13) 0.0475(17) -0.0019(11) -0.0038(12) -0.0093(10) O5 0.0173(11) 0.0215(12) 0.0300(14) 0.0050(10) 0.0033(10) 0.0020(9) O10 0.0296(13) 0.0183(11) 0.0301(14) 0.0001(10) 0.0013(11) -0.0054(10) O3 0.0169(11) 0.0257(12) 0.0296(13) 0.0049(10) -0.0012(10) -0.0083(9) O14 0.0177(12) 0.0301(13) 0.0281(14) 0.0075(10) 0.0034(10) 0.0051(10) N14 0.0315(16) 0.0299(16) 0.0135(14) 0.0067(12) 0.0011(12) 0.0009(13) N6 0.0223(14) 0.0206(14) 0.0181(14) 0.0022(11) 0.0001(11) -0.0030(11) N7 0.0258(15) 0.0235(14) 0.0160(14) 0.0025(11) -0.0009(11) 0.0028(12) N16 0.0328(16) 0.0304(16) 0.0126(14) 0.0051(12) 0.0006(12) -0.0017(13) N11 0.0423(19) 0.0335(17) 0.0196(16) 0.0073(13) 0.0006(14) 0.0064(14) C89 0.049(3) 0.077(3) 0.041(3) -0.006(2) -0.001(2) -0.031(3) C54 0.0191(16) 0.0203(15) 0.0142(16) 0.0024(13) 0.0000(12) -0.0033(12) C41 0.0296(18) 0.0221(17) 0.0195(18) 0.0031(14) -0.0001(14) -0.0009(14) N15 0.0311(16) 0.0272(15) 0.0146(14) 0.0050(12) 0.0023(12) 0.0010(12) O2 0.0407(15) 0.0169(12) 0.0359(15) -0.0001(10) -0.0094(12) -0.0018(11) C48 0.0295(18) 0.0206(16) 0.0167(17) 0.0006(13) -0.0012(14) -0.0008(14) O1W 0.0461(18) 0.072(2) 0.051(2) -0.0047(17) 0.0016(15) -0.0182(16) O13 0.0172(11) 0.0247(12) 0.0285(13) 0.0048(10) -0.0046(10) -0.0056(9) C27 0.0299(18) 0.0227(17) 0.0147(16) 0.0007(13) -0.0039(14) -0.0026(14) C55 0.0150(15) 0.0226(16) 0.0219(17) 0.0035(13) -0.0030(13) 0.0006(12) C67 0.0154(16) 0.0314(18) 0.0219(18) 0.0034(14) 0.0026(13) -0.0049(13) C57 0.0238(17) 0.0264(17) 0.0182(17) 0.0031(14) 0.0010(14) -0.0023(14) C66 0.0167(16) 0.0287(18) 0.0222(18) 0.0051(14) -0.0027(13) -0.0037(13) O2W 0.0516(19) 0.064(2) 0.056(2) -0.0058(17) 0.0043(16) -0.0118(16) C18 0.0241(17) 0.0196(16) 0.0240(18) -0.0012(14) -0.0012(14) -0.0001(13) C68 0.0258(17) 0.0190(16) 0.0162(17) 0.0002(13) 0.0024(13) 0.0014(13) N10 0.044(2) 0.0383(18) 0.0210(17) 0.0106(14) 0.0068(14) 0.0102(15) N12 0.0440(19) 0.0366(18) 0.0168(16) 0.0081(13) 0.0026(14) 0.0058(15) C44 0.036(2) 0.0203(17) 0.0224(19) 0.0011(14) 0.0009(15) -0.0023(15) C22 0.0180(16) 0.0203(16) 0.0228(18) -0.0005(13) -0.0023(13) -0.0075(13) C71 0.0253(17) 0.0265(17) 0.0171(17) 0.0004(14) 0.0025(14) -0.0013(14) C23 0.0173(16) 0.0190(16) 0.032(2) -0.0003(14) -0.0013(14) -0.0033(13) C70 0.0171(15) 0.0154(14) 0.0182(16) 0.0002(12) -0.0024(12) -0.0003(12) C10 0.0183(16) 0.0177(16) 0.0215(17) -0.0014(13) 0.0022(13) -0.0052(12) C9 0.0176(16) 0.0178(15) 0.0238(18) -0.0004(13) 0.0000(13) -0.0030(12) C56 0.0128(15) 0.0225(16) 0.0201(17) 0.0018(13) 0.0004(12) -0.0038(12) C2 0.0327(19) 0.0209(17) 0.028(2) -0.0049(15) -0.0007(15) -0.0083(14) N9 0.053(2) 0.0383(19) 0.0193(17) 0.0117(14) 0.0073(15) 0.0113(16) C20 0.0192(16) 0.0177(15) 0.0226(18) -0.0025(13) 0.0002(13) -0.0018(12) C32 0.036(2) 0.0202(17) 0.0196(18) 0.0014(14) 0.0023(15) -0.0027(14) C69 0.0183(16) 0.0169(15) 0.0226(17) -0.0028(13) -0.0019(13) 0.0011(12) N20 0.051(2) 0.073(3) 0.035(2) -0.012(2) 0.0010(19) -0.0267(19) C33 0.036(2) 0.034(2) 0.025(2) 0.0023(16) 0.0053(16) -0.0005(16) C30 0.035(2) 0.0290(19) 0.0194(18) 0.0030(15) 0.0017(15) -0.0021(16) C53 0.0158(16) 0.0293(18) 0.0208(18) 0.0058(14) -0.0001(13) -0.0032(13) C1 0.042(2) 0.0185(16) 0.0184(18) -0.0038(13) 0.0003(15) -0.0064(15) C46 0.034(2) 0.0269(18) 0.0181(18) 0.0029(14) -0.0012(15) 0.0002(15) C37 0.0220(18) 0.034(2) 0.028(2) 0.0083(16) -0.0056(15) -0.0043(15) C94 0.0152(15) 0.0272(17) 0.0240(18) 0.0070(14) -0.0027(13) -0.0018(13) C21 0.0151(15) 0.0220(16) 0.0257(18) -0.0031(14) 0.0019(13) -0.0050(13) C34 0.0294(18) 0.0231(17) 0.0185(18) 0.0033(14) 0.0013(14) -0.0018(14) C49 0.0279(19) 0.0337(19) 0.0198(18) 0.0011(15) 0.0023(14) 0.0035(15) C28 0.050(2) 0.0196(17) 0.0200(18) 0.0036(14) 0.0003(16) 0.0086(16) C8 0.0173(16) 0.0170(15) 0.0262(18) -0.0006(13) -0.0013(13) -0.0018(12) C24 0.0152(15) 0.0231(16) 0.0150(16) 0.0009(13) -0.0012(12) -0.0029(13) C13 0.033(2) 0.0219(17) 0.0187(18) -0.0006(14) 0.0006(15) -0.0024(15) C11 0.0160(15) 0.0169(15) 0.0244(18) -0.0020(13) -0.0020(13) 0.0002(12) C3 0.0298(19) 0.0207(17) 0.033(2) -0.0038(15) -0.0034(16) -0.0077(14) C81 0.044(3) 0.170(7) 0.047(3) -0.016(4) 0.001(3) -0.023(4) C61 0.041(2) 0.0269(18) 0.0175(18) 0.0022(14) -0.0007(15) 0.0063(16) C76 0.056(3) 0.028(2) 0.024(2) 0.0053(16) 0.0017(18) 0.0130(18) C29 0.050(2) 0.0206(17) 0.0226(19) 0.0007(15) 0.0055(17) 0.0078(16) C7 0.0184(16) 0.0202(16) 0.0124(16) 0.0029(12) -0.0011(12) -0.0034(12) C75 0.043(2) 0.0267(18) 0.0197(19) 0.0029(15) 0.0019(16) 0.0024(16) C73 0.048(2) 0.032(2) 0.0212(19) 0.0044(16) 0.0056(17) 0.0045(17) C38 0.0244(18) 0.037(2) 0.026(2) 0.0093(16) 0.0024(15) -0.0069(15) C36 0.0202(17) 0.0308(19) 0.0234(19) 0.0022(15) 0.0014(14) 0.0015(14) C6 0.0300(19) 0.0190(16) 0.0245(19) -0.0016(14) -0.0005(15) -0.0083(14) C42 0.0258(18) 0.0319(19) 0.0221(19) 0.0045(15) 0.0041(15) -0.0015(15) C40 0.0268(19) 0.034(2) 0.0213(19) 0.0052(15) -0.0022(15) 0.0063(15) C12 0.0165(15) 0.0206(16) 0.0126(15) 0.0000(12) 0.0019(12) -0.0038(12) C62 0.047(2) 0.0256(19) 0.028(2) 0.0057(16) 0.0016(18) 0.0128(17) C4 0.0252(18) 0.0219(17) 0.038(2) -0.0026(15) 0.0002(16) -0.0077(14) C50 0.0226(17) 0.0267(18) 0.0243(19) 0.0077(14) -0.0034(14) 0.0025(14) C39 0.0219(17) 0.0308(18) 0.0218(18) 0.0050(15) 0.0011(14) 0.0031(14) C19 0.0147(15) 0.0272(17) 0.0106(15) 0.0058(13) -0.0011(12) -0.0018(13) C16 0.032(2) 0.0251(18) 0.034(2) -0.0041(16) 0.0033(16) -0.0039(15) C43 0.0214(17) 0.0291(18) 0.0211(18) 0.0054(14) 0.0004(14) -0.0014(14) C45 0.039(2) 0.0285(19) 0.0209(19) 0.0012(15) 0.0045(16) -0.0042(16) C35 0.0257(18) 0.035(2) 0.0197(18) 0.0065(15) -0.0039(14) 0.0025(15) C72 0.029(2) 0.075(3) 0.027(2) 0.011(2) 0.0075(17) 0.004(2) C15 0.0308(19) 0.0224(17) 0.032(2) -0.0046(15) 0.0007(16) -0.0022(14) C59 0.049(2) 0.032(2) 0.0167(18) 0.0008(15) -0.0006(16) 0.0052(17) C26 0.0279(19) 0.0321(19) 0.0227(19) 0.0028(15) 0.0043(15) 0.0092(15) C14 0.036(2) 0.0209(17) 0.032(2) -0.0039(15) 0.0015(16) -0.0018(15) C17 0.0268(19) 0.0223(18) 0.045(2) -0.0056(16) 0.0018(17) 0.0004(14) N19 0.065(3) 0.110(4) 0.039(2) -0.020(3) 0.001(2) -0.036(2) C25 0.0283(19) 0.0276(18) 0.026(2) 0.0078(15) 0.0002(15) 0.0072(15) C52 0.047(2) 0.0241(18) 0.0220(19) 0.0055(15) -0.0016(17) 0.0153(16) C51 0.040(2) 0.0252(18) 0.0200(18) 0.0013(15) 0.0048(16) 0.0103(16) C31 0.066(3) 0.062(3) 0.037(3) 0.018(2) 0.021(2) 0.022(3) C82 0.053(3) 0.113(5) 0.040(3) -0.015(3) 0.003(2) -0.045(3) C65 0.048(2) 0.0274(19) 0.0196(19) 0.0030(15) 0.0093(17) 0.0069(17) C58 0.031(2) 0.102(4) 0.035(3) 0.034(3) 0.0071(19) 0.002(2) C5 0.0256(18) 0.0177(16) 0.044(2) -0.0047(15) -0.0055(16) -0.0060(14) C77 0.057(3) 0.030(2) 0.021(2) 0.0017(16) 0.0059(18) 0.0088(18) N17 0.053(3) 0.174(6) 0.081(4) -0.004(4) -0.001(3) -0.021(3) C64 0.089(4) 0.064(3) 0.026(2) 0.017(2) 0.015(2) 0.053(3) C47 0.054(3) 0.070(3) 0.030(2) 0.017(2) 0.015(2) 0.021(2) C74 0.181(6) 0.036(3) 0.024(2) 0.004(2) 0.031(3) 0.024(3) C88 0.057(3) 0.065(3) 0.035(3) -0.007(2) 0.001(2) -0.037(2) C85 0.060(3) 0.104(4) 0.041(3) -0.023(3) 0.003(2) -0.046(3) C93 0.069(4) 0.082(4) 0.047(3) -0.002(3) -0.004(3) -0.037(3) C60 0.124(5) 0.051(3) 0.022(2) 0.001(2) 0.016(3) 0.030(3) C83 0.061(4) 0.115(5) 0.050(3) -0.017(3) 0.006(3) -0.048(4) C63 0.111(4) 0.064(3) 0.025(2) 0.011(2) 0.020(3) 0.059(3) C86 0.099(5) 0.098(4) 0.041(3) -0.018(3) 0.013(3) -0.037(4) C92 0.066(4) 0.102(5) 0.075(4) 0.011(4) -0.010(3) -0.028(4) C79 0.082(4) 0.063(3) 0.030(2) 0.018(2) 0.025(2) 0.045(3) C87 0.089(4) 0.070(3) 0.034(3) -0.005(2) 0.006(3) -0.026(3) C78 0.064(3) 0.056(3) 0.028(2) 0.020(2) 0.011(2) 0.033(2) C80 0.043(3) 0.219(9) 0.071(5) -0.024(5) 0.010(3) -0.008(5) C91 0.046(3) 0.170(7) 0.076(5) -0.006(5) 0.009(3) 0.006(4) N18 0.054(3) 0.125(5) 0.095(4) 0.012(4) -0.008(3) -0.009(3) C90 0.045(3) 0.133(5) 0.050(3) 0.000(3) 0.000(3) -0.004(3) C84 0.065(4) 0.134(6) 0.065(4) -0.006(4) 0.003(3) -0.045(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 2.012(2) . ? Zn1 O3 2.019(2) . ? Zn1 O2 2.116(2) . ? Zn1 N1 2.151(3) . ? Zn1 N2 2.177(3) . ? Zn1 O1 2.360(2) . ? Zn1 C1 2.563(3) . ? Zn4 O13 2.024(2) . ? Zn4 O14 2.072(2) . ? Zn4 O16 2.133(2) . ? Zn4 N8 2.140(3) . ? Zn4 N7 2.143(3) . ? Zn4 O15 2.365(2) . ? Zn4 C18 2.567(3) . ? Zn3 O12 2.015(2) . ? Zn3 O11 2.021(2) . ? Zn3 O10 2.105(2) . ? Zn3 N5 2.133(3) . ? Zn3 N6 2.182(3) 1_564 ? Zn3 O9 2.374(2) . ? Zn3 C13 2.551(3) . ? Zn2 O6 2.015(2) . ? Zn2 O5 2.036(2) . ? Zn2 O7 2.060(2) . ? Zn2 N4 2.151(3) . ? Zn2 N3 2.154(3) . ? N5 C50 1.323(4) . ? N5 C51 1.345(4) . ? N1 C25 1.328(4) . ? N1 C29 1.340(4) . ? N2 C43 1.331(4) . ? N2 C39 1.347(4) . ? N8 C66 1.335(4) . ? N8 C70 1.343(4) . ? N3 C94 1.340(4) . ? N3 C56 1.345(4) . ? N4 C78 1.316(5) . ? N4 C77 1.331(4) . ? O9 C13 1.253(4) . ? O1 C1 1.243(4) . ? O16 C18 1.264(4) . ? O6 C12 1.254(3) . ? N13 C59 1.271(4) . ? N13 N14 1.379(4) . ? O12 C19 1.250(4) . ? O11 C24 1.269(4) . ? O7 C6 1.262(4) 1_545 ? O4 C12 1.250(4) . ? O15 C18 1.246(4) . ? O8 C6 1.248(4) . ? O5 C7 1.252(4) . ? O10 C13 1.256(4) . ? O3 C7 1.257(3) . ? O14 C24 1.242(4) . ? N14 C57 1.278(4) . ? N6 C37 1.335(4) . ? N6 C36 1.340(4) . ? N6 Zn3 2.182(3) 1_546 ? N7 C65 1.321(4) . ? N7 C64 1.323(5) . ? N16 C73 1.271(4) . ? N16 N15 1.387(4) . ? N11 C44 1.286(4) . ? N11 N12 1.403(4) . ? C89 C90 1.386(7) . ? C89 C93 1.387(6) . ? C89 C88 1.481(7) . ? C54 C55 1.391(4) . ? C54 C53 1.401(4) . ? C54 C57 1.481(4) . ? C41 C40 1.383(5) . ? C41 C42 1.392(5) . ? C41 C44 1.490(4) . ? N15 C71 1.278(4) . ? O2 C1 1.275(4) . ? C48 C49 1.384(4) . ? C48 C52 1.387(5) . ? C48 C46 1.482(4) . ? O13 C19 1.254(4) . ? C27 C28 1.378(5) . ? C27 C26 1.382(4) . ? C27 C30 1.488(4) . ? C55 C56 1.376(4) . ? C67 C66 1.370(4) . ? C67 C68 1.399(4) . ? C57 C58 1.488(5) . ? C18 C17 1.485(4) . ? C68 C69 1.394(4) . ? C68 C71 1.477(4) . ? N10 C32 1.288(4) . ? N10 N9 1.392(4) . ? N12 C46 1.286(4) . ? C44 C45 1.498(5) . ? C22 C23 1.323(4) . ? C22 C21 1.445(4) 1_455 ? C71 C72 1.500(5) . ? C23 C24 1.480(4) . ? C70 C69 1.384(4) . ? C10 C11 1.330(4) . ? C10 C9 1.451(4) 1_655 ? C9 C8 1.328(4) . ? C9 C10 1.451(4) 1_455 ? C2 C3 1.319(5) . ? C2 C1 1.479(4) . ? N9 C30 1.271(4) . ? C20 C21 1.325(4) . ? C20 C19 1.487(4) . ? C32 C34 1.480(4) . ? C32 C33 1.491(5) . ? N20 C88 1.286(5) . ? N20 N20 1.398(7) 2_676 ? C30 C31 1.487(5) . ? C53 C94 1.372(4) . ? C46 C47 1.485(5) . ? C37 C38 1.375(5) . ? C21 C22 1.445(4) 1_655 ? C34 C35 1.388(5) . ? C34 C38 1.393(5) . ? C49 C50 1.385(4) . ? C28 C29 1.369(5) . ? C8 C7 1.477(4) . ? C13 C14 1.493(4) . ? C11 C12 1.492(4) . ? C3 C4 1.445(4) . ? C81 C82 1.385(7) . ? C81 C80 1.386(9) . ? C61 C62 1.372(5) . ? C61 C63 1.379(5) . ? C61 C59 1.482(5) . ? C76 C75 1.371(5) . ? C76 C77 1.373(5) . ? C75 C79 1.385(5) . ? C75 C73 1.481(5) . ? C73 C74 1.487(5) . ? C36 C35 1.375(4) . ? C6 O7 1.262(4) 1_565 ? C6 C5 1.485(4) . ? C42 C43 1.380(4) . ? C40 C39 1.372(4) . ? C62 C65 1.370(5) 1_546 ? C4 C5 1.317(5) . ? C16 C17 1.308(5) 1_565 ? C16 C15 1.453(5) . ? C15 C14 1.312(5) . ? C59 C60 1.499(5) . ? C26 C25 1.373(5) . ? C17 C16 1.308(5) 1_545 ? N19 C85 1.279(6) . ? N19 N19 1.408(9) 2_667 ? C52 C51 1.368(5) . ? C82 C83 1.392(7) . ? C82 C85 1.474(8) . ? C65 C62 1.370(5) 1_564 ? N17 C84 1.330(8) . ? N17 C80 1.339(8) . ? C64 C63 1.379(5) 1_564 ? C88 C87 1.504(6) . ? C85 C86 1.515(6) . ? C93 C92 1.367(8) . ? C83 C84 1.360(8) . ? C63 C64 1.379(5) 1_546 ? C92 N18 1.323(7) . ? C79 C78 1.376(5) . ? C91 N18 1.331(7) . ? C91 C90 1.384(8) . ? 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 O3 121.96(9) . . ? O4 Zn1 O2 91.77(9) . . ? O3 Zn1 O2 145.80(9) . . ? O4 Zn1 N1 96.17(10) . . ? O3 Zn1 N1 88.54(9) . . ? O2 Zn1 N1 93.62(10) . . ? O4 Zn1 N2 87.97(9) . . ? O3 Zn1 N2 88.01(9) . . ? O2 Zn1 N2 87.71(9) . . ? N1 Zn1 N2 175.60(10) . . ? O4 Zn1 O1 148.81(8) . . ? O3 Zn1 O1 87.44(9) . . ? O2 Zn1 O1 58.36(8) . . ? N1 Zn1 O1 94.64(9) . . ? N2 Zn1 O1 82.48(9) . . ? O4 Zn1 C1 120.36(11) . . ? O3 Zn1 C1 116.19(11) . . ? O2 Zn1 C1 29.70(10) . . ? N1 Zn1 C1 97.42(10) . . ? N2 Zn1 C1 81.68(10) . . ? O1 Zn1 C1 28.88(9) . . ? O13 Zn4 O14 115.03(9) . . ? O13 Zn4 O16 92.43(9) . . ? O14 Zn4 O16 152.05(9) . . ? O13 Zn4 N8 92.49(9) . . ? O14 Zn4 N8 85.03(9) . . ? O16 Zn4 N8 88.85(9) . . ? O13 Zn4 N7 95.33(10) . . ? O14 Zn4 N7 89.24(9) . . ? O16 Zn4 N7 93.47(9) . . ? N8 Zn4 N7 171.74(10) . . ? O13 Zn4 O15 150.31(8) . . ? O14 Zn4 O15 94.08(9) . . ? O16 Zn4 O15 58.12(8) . . ? N8 Zn4 O15 83.93(9) . . ? N7 Zn4 O15 90.56(9) . . ? O13 Zn4 C18 121.42(10) . . ? O14 Zn4 C18 122.65(10) . . ? O16 Zn4 C18 29.40(9) . . ? N8 Zn4 C18 83.36(10) . . ? N7 Zn4 C18 94.78(10) . . ? O15 Zn4 C18 28.91(9) . . ? O12 Zn3 O11 114.16(10) . . ? O12 Zn3 O10 149.90(9) . . ? O11 Zn3 O10 94.83(9) . . ? O12 Zn3 N5 93.48(10) . . ? O11 Zn3 N5 90.99(9) . . ? O10 Zn3 N5 93.92(9) . . ? O12 Zn3 N6 84.71(10) . 1_564 ? O11 Zn3 N6 93.14(9) . 1_564 ? O10 Zn3 N6 85.86(9) . 1_564 ? N5 Zn3 N6 175.87(10) . 1_564 ? O12 Zn3 O9 92.18(9) . . ? O11 Zn3 O9 153.11(9) . . ? O10 Zn3 O9 58.36(8) . . ? N5 Zn3 O9 92.76(9) . . ? N6 Zn3 O9 83.61(9) 1_564 . ? O12 Zn3 C13 120.71(11) . . ? O11 Zn3 C13 123.92(10) . . ? O10 Zn3 C13 29.35(10) . . ? N5 Zn3 C13 96.29(10) . . ? N6 Zn3 C13 81.50(10) 1_564 . ? O9 Zn3 C13 29.20(9) . . ? O6 Zn2 O5 123.17(9) . . ? O6 Zn2 O7 138.03(9) . . ? O5 Zn2 O7 98.49(9) . . ? O6 Zn2 N4 90.87(9) . . ? O5 Zn2 N4 94.38(10) . . ? O7 Zn2 N4 90.85(10) . . ? O6 Zn2 N3 88.87(9) . . ? O5 Zn2 N3 88.84(9) . . ? O7 Zn2 N3 86.89(9) . . ? N4 Zn2 N3 176.31(10) . . ? C50 N5 C51 116.5(3) . . ? C50 N5 Zn3 121.0(2) . . ? C51 N5 Zn3 122.3(2) . . ? C25 N1 C29 116.4(3) . . ? C25 N1 Zn1 120.3(2) . . ? C29 N1 Zn1 122.9(2) . . ? C43 N2 C39 116.5(3) . . ? C43 N2 Zn1 122.1(2) . . ? C39 N2 Zn1 121.2(2) . . ? C66 N8 C70 117.1(3) . . ? C66 N8 Zn4 119.5(2) . . ? C70 N8 Zn4 123.2(2) . . ? C94 N3 C56 116.8(3) . . ? C94 N3 Zn2 120.4(2) . . ? C56 N3 Zn2 122.4(2) . . ? C78 N4 C77 116.3(3) . . ? C78 N4 Zn2 119.7(2) . . ? C77 N4 Zn2 123.9(2) . . ? C13 O9 Zn3 83.2(2) . . ? C1 O1 Zn1 84.67(19) . . ? C18 O16 Zn4 94.66(19) . . ? C12 O6 Zn2 135.3(2) . . ? C59 N13 N14 116.5(3) . . ? C19 O12 Zn3 162.3(2) . . ? C24 O11 Zn3 124.4(2) . . ? C6 O7 Zn2 101.35(19) 1_545 . ? C12 O4 Zn1 144.8(2) . . ? C18 O15 Zn4 84.56(19) . . ? C7 O5 Zn2 145.5(2) . . ? C13 O10 Zn3 95.4(2) . . ? C7 O3 Zn1 136.4(2) . . ? C24 O14 Zn4 165.1(2) . . ? C57 N14 N13 117.0(3) . . ? C37 N6 C36 116.7(3) . . ? C37 N6 Zn3 121.8(2) . 1_546 ? C36 N6 Zn3 121.4(2) . 1_546 ? C65 N7 C64 115.9(3) . . ? C65 N7 Zn4 122.9(2) . . ? C64 N7 Zn4 121.2(2) . . ? C73 N16 N15 117.6(3) . . ? C44 N11 N12 112.7(3) . . ? C90 C89 C93 116.7(5) . . ? C90 C89 C88 120.3(5) . . ? C93 C89 C88 123.1(5) . . ? C55 C54 C53 117.3(3) . . ? C55 C54 C57 121.0(3) . . ? C53 C54 C57 121.7(3) . . ? C40 C41 C42 116.6(3) . . ? C40 C41 C44 121.3(3) . . ? C42 C41 C44 122.1(3) . . ? C71 N15 N16 115.2(3) . . ? C1 O2 Zn1 94.9(2) . . ? C49 C48 C52 116.5(3) . . ? C49 C48 C46 123.3(3) . . ? C52 C48 C46 120.2(3) . . ? C19 O13 Zn4 125.3(2) . . ? C28 C27 C26 116.1(3) . . ? C28 C27 C30 120.3(3) . . ? C26 C27 C30 123.6(3) . . ? C56 C55 C54 119.7(3) . . ? C66 C67 C68 119.3(3) . . ? N14 C57 C54 116.2(3) . . ? N14 C57 C58 123.9(3) . . ? C54 C57 C58 119.9(3) . . ? N8 C66 C67 124.0(3) . . ? O15 C18 O16 121.8(3) . . ? O15 C18 C17 121.4(3) . . ? O16 C18 C17 116.7(3) . . ? O15 C18 Zn4 66.53(17) . . ? O16 C18 Zn4 55.94(16) . . ? C17 C18 Zn4 166.1(3) . . ? C69 C68 C67 117.0(3) . . ? C69 C68 C71 122.2(3) . . ? C67 C68 C71 120.8(3) . . ? C32 N10 N9 112.1(3) . . ? C46 N12 N11 115.0(3) . . ? N11 C44 C41 115.0(3) . . ? N11 C44 C45 126.0(3) . . ? C41 C44 C45 119.0(3) . . ? C23 C22 C21 123.4(3) . 1_455 ? N15 C71 C68 116.5(3) . . ? N15 C71 C72 124.3(3) . . ? C68 C71 C72 119.1(3) . . ? C22 C23 C24 124.5(3) . . ? N8 C70 C69 122.9(3) . . ? C11 C10 C9 122.7(3) . 1_655 ? C8 C9 C10 124.3(3) . 1_455 ? N3 C56 C55 123.3(3) . . ? C3 C2 C1 122.8(3) . . ? C30 N9 N10 115.9(3) . . ? C21 C20 C19 122.7(3) . . ? N10 C32 C34 115.7(3) . . ? N10 C32 C33 124.6(3) . . ? C34 C32 C33 119.7(3) . . ? C70 C69 C68 119.6(3) . . ? C88 N20 N20 114.9(5) . 2_676 ? N9 C30 C31 125.5(3) . . ? N9 C30 C27 114.4(3) . . ? C31 C30 C27 120.0(3) . . ? C94 C53 C54 119.0(3) . . ? O1 C1 O2 121.1(3) . . ? O1 C1 C2 121.3(3) . . ? O2 C1 C2 117.6(3) . . ? O1 C1 Zn1 66.45(17) . . ? O2 C1 Zn1 55.35(16) . . ? C2 C1 Zn1 167.5(3) . . ? N12 C46 C48 114.2(3) . . ? N12 C46 C47 125.9(3) . . ? C48 C46 C47 119.9(3) . . ? N6 C37 C38 123.3(3) . . ? N3 C94 C53 124.0(3) . . ? C20 C21 C22 124.8(3) . 1_655 ? C35 C34 C38 116.3(3) . . ? C35 C34 C32 122.3(3) . . ? C38 C34 C32 121.3(3) . . ? C48 C49 C50 120.0(3) . . ? C29 C28 C27 120.3(3) . . ? C9 C8 C7 124.3(3) . . ? O14 C24 O11 125.6(3) . . ? O14 C24 C23 116.9(3) . . ? O11 C24 C23 117.5(3) . . ? O9 C13 O10 122.2(3) . . ? O9 C13 C14 120.0(3) . . ? O10 C13 C14 117.7(3) . . ? O9 C13 Zn3 67.56(18) . . ? O10 C13 Zn3 55.25(16) . . ? C14 C13 Zn3 167.3(2) . . ? C10 C11 C12 124.2(3) . . ? C2 C3 C4 125.2(3) . . ? C82 C81 C80 119.1(6) . . ? C62 C61 C63 115.2(3) . . ? C62 C61 C59 121.3(3) . . ? C63 C61 C59 123.5(3) . . ? C75 C76 C77 120.2(3) . . ? N1 C29 C28 123.5(3) . . ? O5 C7 O3 126.4(3) . . ? O5 C7 C8 117.9(3) . . ? O3 C7 C8 115.6(3) . . ? C76 C75 C79 116.0(3) . . ? C76 C75 C73 121.2(3) . . ? C79 C75 C73 122.8(3) . . ? N16 C73 C75 115.3(3) . . ? N16 C73 C74 124.2(3) . . ? C75 C73 C74 120.6(3) . . ? C37 C38 C34 120.2(3) . . ? N6 C36 C35 123.6(3) . . ? O8 C6 O7 122.4(3) . 1_565 ? O8 C6 C5 119.8(3) . . ? O7 C6 C5 117.7(3) 1_565 . ? C43 C42 C41 119.9(3) . . ? C39 C40 C41 120.1(3) . . ? O4 C12 O6 126.9(3) . . ? O4 C12 C11 118.0(3) . . ? O6 C12 C11 115.1(3) . . ? C65 C62 C61 120.6(3) 1_546 . ? C5 C4 C3 124.2(3) . . ? N5 C50 C49 123.3(3) . . ? N2 C39 C40 123.5(3) . . ? O12 C19 O13 124.8(3) . . ? O12 C19 C20 116.8(3) . . ? O13 C19 C20 118.4(3) . . ? C17 C16 C15 126.2(4) 1_565 . ? N2 C43 C42 123.5(3) . . ? C36 C35 C34 119.9(3) . . ? C14 C15 C16 123.9(3) . . ? N13 C59 C61 115.3(3) . . ? N13 C59 C60 124.1(3) . . ? C61 C59 C60 120.6(3) . . ? C25 C26 C27 120.5(3) . . ? C15 C14 C13 125.5(3) . . ? C16 C17 C18 123.6(3) 1_545 . ? C85 N19 N19 114.5(5) . 2_667 ? N1 C25 C26 123.3(3) . . ? C51 C52 C48 119.8(3) . . ? N5 C51 C52 123.8(3) . . ? C81 C82 C83 116.7(6) . . ? C81 C82 C85 121.0(5) . . ? C83 C82 C85 122.3(5) . . ? N7 C65 C62 124.2(3) . 1_564 ? C4 C5 C6 123.5(3) . . ? N4 C77 C76 123.7(3) . . ? C84 N17 C80 114.3(7) . . ? N7 C64 C63 123.3(4) . 1_564 ? N20 C88 C89 115.5(4) . . ? N20 C88 C87 125.5(5) . . ? C89 C88 C87 118.9(4) . . ? N19 C85 C82 115.2(5) . . ? N19 C85 C86 125.3(6) . . ? C82 C85 C86 119.5(5) . . ? C92 C93 C89 119.7(5) . . ? C84 C83 C82 119.2(6) . . ? C64 C63 C61 120.8(4) 1_546 . ? N18 C92 C93 125.0(6) . . ? C78 C79 C75 120.1(4) . . ? N4 C78 C79 123.7(4) . . ? N17 C80 C81 124.8(6) . . ? N18 C91 C90 125.3(6) . . ? C92 N18 C91 114.9(6) . . ? C91 C90 C89 118.5(5) . . ? N17 C84 C83 126.0(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.323 _refine_diff_density_min -0.536 _refine_diff_density_rms 0.147 _database_code_depnum_ccdc_archive 'CCDC 973251'