# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email a.d.burrows@bath.ac.uk _publ_contact_author_name 'Andrew Burrows' _publ_author_name A.Burrows data_compound1_h09adb12 _database_code_depnum_ccdc_archive 'CCDC 859602' #TrackingRef '- warren-pw.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65.60 H61.50 Cu2 N2 O10.80' _chemical_formula_weight 1177.75 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' Cu Cu 0.3201 1.2651 '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 9.7080(4) _cell_length_b 14.1110(9) _cell_length_c 16.5790(10) _cell_angle_alpha 72.751(2) _cell_angle_beta 87.723(4) _cell_angle_gamma 71.095(3) _cell_volume 2048.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 68637 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description block _exptl_crystal_colour aqua _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.955 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 614 _exptl_absorpt_coefficient_mu 0.564 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25559 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0896 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 25.15 _reflns_number_total 7222 _reflns_number_gt 4798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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. Asymmetric unit = 1/2 of a paddle wheel + 0.9 molecules of benzyl alcohol + a region of diffuse solvent. The oxygen in the benzyl alcohol moiety was disordered equally over 2 proximate sites. The associated hydrogen fraction could not be reliably located, and hence were omitted from the refinement. The diffuse solvent (benzyl alcohol) was treated using PLATON SQUEEZE. Based on the pre-squeeze electron density, allowance was made for an addition 1 full molecule of this solvent in the unit cell, despite additional void space being available. ; _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^)+(0.1292P)^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 7222 _refine_ls_number_parameters 388 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1103 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2095 _refine_ls_wR_factor_gt 0.1955 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Cu1 Cu 0.13284(5) 0.00201(4) 1.00130(3) 0.0299(2) Uani 1 1 d . . . N1 N 0.3573(3) 0.0005(2) 1.00103(19) 0.0246(7) Uani 1 1 d . . . O1 O 0.0844(3) 0.0850(2) 0.88179(19) 0.0407(8) Uani 1 1 d . . . O3 O 0.1787(3) -0.1270(2) 0.9697(2) 0.0411(8) Uani 1 1 d . . . C16 C 0.0449(5) -0.3135(4) 0.9172(3) 0.0423(12) Uani 1 1 d . . . H16 H -0.0570 -0.2771 0.9130 0.051 Uiso 1 1 calc R . . C15 C 0.1410(4) -0.2710(4) 0.9409(3) 0.0380(11) Uani 1 1 d . . . C23 C 0.2622(5) -0.7279(4) 0.8857(3) 0.0487(13) Uani 1 1 d . . . H23 H 0.2016 -0.7707 0.8949 0.058 Uiso 1 1 calc R . . C21 C 0.2980(5) -0.5663(4) 0.8877(3) 0.0391(11) Uani 1 1 d . . . C20 C 0.2910(5) -0.3243(4) 0.9440(3) 0.0438(12) Uani 1 1 d . . . H20 H 0.3588 -0.2955 0.9587 0.053 Uiso 1 1 calc R . . C19 C 0.3406(5) -0.4186(4) 0.9256(3) 0.0435(12) Uani 1 1 d . . . H19 H 0.4426 -0.4538 0.9279 0.052 Uiso 1 1 calc R . . C17 C 0.0953(5) -0.4076(4) 0.8996(3) 0.0441(12) Uani 1 1 d . . . H17 H 0.0272 -0.4356 0.8841 0.053 Uiso 1 1 calc R . . C18 C 0.2444(5) -0.4634(4) 0.9039(3) 0.0376(11) Uani 1 1 d . . . C14 C 0.0866(4) -0.1694(3) 0.9616(3) 0.0356(11) Uani 1 1 d . . . C27 C 0.4540(4) -0.0472(3) 0.9549(3) 0.0340(11) Uani 1 1 d . . . H27 H 0.4238 -0.0822 0.9216 0.041 Uiso 1 1 calc R . . C22 C 0.2148(5) -0.6325(4) 0.9011(3) 0.0427(12) Uani 1 1 d . . . H22 H 0.1208 -0.6108 0.9219 0.051 Uiso 1 1 calc R . . C26 C 0.4368(5) -0.6021(4) 0.8581(3) 0.0474(13) Uani 1 1 d . . . H26 H 0.4971 -0.5590 0.8479 0.057 Uiso 1 1 calc R . . C24 C 0.4006(6) -0.7610(4) 0.8562(3) 0.0537(14) Uani 1 1 d . . . H24 H 0.4350 -0.8266 0.8448 0.064 Uiso 1 1 calc R . . C25 C 0.4878(5) -0.6982(4) 0.8435(4) 0.0579(14) Uani 1 1 d . . . H25 H 0.5831 -0.7214 0.8247 0.069 Uiso 1 1 calc R . . C1 C -0.0374(5) 0.1068(3) 0.8448(3) 0.0363(11) Uani 1 1 d . . . O2 O -0.1427(3) 0.0793(2) 0.87912(19) 0.0426(8) Uani 1 1 d . . . C2 C -0.0644(5) 0.1750(4) 0.7554(3) 0.0378(11) Uani 1 1 d . . . C7 C 0.0336(5) 0.2253(4) 0.7174(3) 0.0464(13) Uani 1 1 d . . . H7 H 0.1208 0.2135 0.7484 0.056 Uiso 1 1 calc R . . C3 C -0.1887(5) 0.1905(4) 0.7069(3) 0.0480(13) Uani 1 1 d . . . H3 H -0.2565 0.1562 0.7314 0.058 Uiso 1 1 calc R . . C4 C -0.2147(5) 0.2537(4) 0.6256(3) 0.0531(14) Uani 1 1 d . . . H4 H -0.3001 0.2620 0.5945 0.064 Uiso 1 1 calc R . . C6 C 0.0073(5) 0.2919(4) 0.6356(3) 0.0560(14) Uani 1 1 d . . . H6 H 0.0741 0.3277 0.6124 0.067 Uiso 1 1 calc R . . C5 C -0.1179(5) 0.3075(4) 0.5859(3) 0.0522(13) Uani 1 1 d . . . C8 C -0.1489(6) 0.3792(5) 0.4996(3) 0.0623(16) Uani 1 1 d . . . C13 C -0.0359(7) 0.3918(6) 0.4474(4) 0.086(2) Uani 1 1 d . . . H13 H 0.0625 0.3537 0.4680 0.103 Uiso 1 1 calc R . . C9 C -0.2888(7) 0.4363(6) 0.4680(4) 0.088(2) Uani 1 1 d . . . H9 H -0.3674 0.4279 0.5022 0.106 Uiso 1 1 calc R . . C12 C -0.0668(9) 0.4602(7) 0.3652(4) 0.104(3) Uani 1 1 d . . . H12 H 0.0115 0.4665 0.3301 0.125 Uiso 1 1 calc R . . C10 C -0.3183(9) 0.5073(6) 0.3862(5) 0.107(3) Uani 1 1 d . . . H10 H -0.4161 0.5484 0.3661 0.128 Uiso 1 1 calc R . . C11 C -0.2040(9) 0.5173(6) 0.3342(4) 0.104(3) Uani 1 1 d . . . H11 H -0.2229 0.5636 0.2780 0.125 Uiso 1 1 calc R . . O4 O -0.0479(3) -0.1323(2) 0.9683(2) 0.0424(8) Uani 1 1 d . . . C28 C 0.4055(4) 0.0482(3) 1.0468(3) 0.0328(10) Uani 1 1 d . . . H28 H 0.3406 0.0833 1.0811 0.039 Uiso 1 1 calc R . . C35 C 0.2280(7) 0.4924(6) 0.1412(5) 0.0611(17) Uani 0.90 1 d P . . H35 H 0.1838 0.5159 0.0855 0.073 Uiso 0.90 1 calc PR . . C34 C 0.2048(7) 0.5590(7) 0.1868(6) 0.080(2) Uani 0.90 1 d P . . H34 H 0.1423 0.6290 0.1624 0.096 Uiso 0.90 1 calc PR . . C30 C 0.3149(7) 0.3905(7) 0.1742(5) 0.070(2) Uani 0.90 1 d P B . C33 C 0.2630(9) 0.5335(7) 0.2627(6) 0.081(2) Uani 0.90 1 d P . . H33 H 0.2420 0.5852 0.2914 0.097 Uiso 0.90 1 calc PR . . C32 C 0.3497(11) 0.4384(9) 0.3006(5) 0.101(3) Uani 0.90 1 d P . . H32 H 0.3918 0.4213 0.3560 0.122 Uiso 0.90 1 calc PR . . C31 C 0.3803(8) 0.3604(7) 0.2573(6) 0.099(3) Uani 0.90 1 d P . . H31 H 0.4423 0.2906 0.2833 0.119 Uiso 0.90 1 calc PR . . C29 C 0.3457(12) 0.3115(11) 0.1308(7) 0.134(4) Uani 0.90 1 d PD . . H29A H 0.3952 0.3355 0.0791 0.161 Uiso 0.45 1 calc PR A 1 H29B H 0.2508 0.3104 0.1119 0.161 Uiso 0.45 1 calc PR A 1 H29C H 0.4494 0.2946 0.1173 0.161 Uiso 0.45 1 calc PR A 2 H29D H 0.2867 0.3435 0.0763 0.161 Uiso 0.45 1 calc PR A 2 O5 O 0.3200(16) 0.2117(9) 0.1731(8) 0.107(4) Uani 0.45 1 d PD B 2 O5A O 0.4338(15) 0.2020(8) 0.1750(8) 0.109(4) Uani 0.45 1 d PD B 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 Cu1 0.0248(3) 0.0313(4) 0.0317(3) -0.0056(2) 0.0002(2) -0.0101(2) N1 0.0289(18) 0.0157(17) 0.0227(17) 0.0012(14) -0.0006(14) -0.0046(14) O1 0.0308(17) 0.046(2) 0.0396(18) 0.0007(16) -0.0066(14) -0.0158(14) O3 0.0266(15) 0.0403(19) 0.060(2) -0.0193(17) 0.0013(14) -0.0113(14) C16 0.025(2) 0.038(3) 0.062(3) -0.015(3) -0.001(2) -0.006(2) C15 0.033(2) 0.040(3) 0.040(3) -0.007(2) -0.0005(19) -0.014(2) C23 0.057(3) 0.035(3) 0.051(3) -0.002(3) -0.005(2) -0.020(2) C21 0.035(3) 0.037(3) 0.041(3) -0.009(2) -0.003(2) -0.009(2) C20 0.029(2) 0.044(3) 0.062(3) -0.020(3) -0.002(2) -0.013(2) C19 0.027(2) 0.042(3) 0.061(3) -0.018(3) 0.000(2) -0.006(2) C17 0.029(2) 0.046(3) 0.060(3) -0.019(3) -0.002(2) -0.013(2) C18 0.036(3) 0.039(3) 0.040(3) -0.014(2) 0.004(2) -0.014(2) C14 0.028(3) 0.039(3) 0.034(3) -0.004(2) -0.0024(19) -0.010(2) C27 0.032(2) 0.035(3) 0.037(3) -0.011(2) 0.003(2) -0.014(2) C22 0.040(3) 0.036(3) 0.052(3) -0.010(2) 0.004(2) -0.015(2) C26 0.043(3) 0.040(3) 0.058(3) -0.014(3) 0.005(2) -0.012(2) C24 0.066(4) 0.029(3) 0.058(3) -0.006(3) -0.006(3) -0.010(3) C25 0.044(3) 0.053(4) 0.070(4) -0.019(3) 0.011(3) -0.007(3) C1 0.038(3) 0.028(3) 0.044(3) -0.011(2) 0.003(2) -0.011(2) O2 0.0330(17) 0.050(2) 0.0359(18) 0.0036(16) -0.0020(13) -0.0165(15) C2 0.038(3) 0.040(3) 0.035(3) -0.008(2) -0.001(2) -0.014(2) C7 0.039(3) 0.056(3) 0.041(3) -0.003(3) -0.006(2) -0.021(2) C3 0.043(3) 0.058(4) 0.040(3) -0.003(3) 0.002(2) -0.023(2) C4 0.049(3) 0.064(4) 0.042(3) 0.003(3) -0.011(2) -0.029(3) C6 0.054(3) 0.070(4) 0.039(3) 0.003(3) 0.000(2) -0.031(3) C5 0.055(3) 0.059(4) 0.036(3) -0.002(3) 0.001(2) -0.021(3) C8 0.071(4) 0.080(4) 0.033(3) 0.005(3) -0.012(3) -0.040(3) C13 0.081(4) 0.121(6) 0.045(4) 0.013(4) -0.009(3) -0.052(4) C9 0.074(4) 0.109(6) 0.049(4) 0.015(4) -0.004(3) -0.021(4) C12 0.099(5) 0.140(7) 0.058(4) 0.033(4) -0.008(4) -0.075(5) C10 0.099(5) 0.113(7) 0.071(5) 0.034(5) -0.023(4) -0.036(5) C11 0.122(6) 0.113(7) 0.060(4) 0.034(4) -0.033(4) -0.065(5) O4 0.0286(17) 0.042(2) 0.061(2) -0.0226(17) 0.0038(14) -0.0105(14) C28 0.031(2) 0.031(3) 0.035(3) -0.012(2) 0.0043(19) -0.0055(19) C35 0.052(4) 0.067(5) 0.070(5) -0.016(4) 0.015(3) -0.032(4) C34 0.051(4) 0.091(6) 0.092(6) -0.012(5) 0.018(4) -0.033(4) C30 0.061(4) 0.094(6) 0.085(5) -0.056(5) 0.033(4) -0.042(4) C33 0.087(5) 0.087(7) 0.078(6) -0.034(5) 0.022(5) -0.032(5) C32 0.129(7) 0.118(8) 0.066(5) -0.029(6) -0.007(5) -0.049(7) C31 0.080(5) 0.069(6) 0.120(8) -0.003(6) -0.021(5) -0.006(4) C29 0.109(8) 0.208(13) 0.144(10) -0.091(10) 0.034(7) -0.097(9) O5 0.121(10) 0.132(12) 0.114(10) -0.069(9) 0.045(8) -0.074(9) O5A 0.133(11) 0.090(10) 0.120(11) -0.058(9) 0.043(9) -0.038(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 Cu1 O3 1.952(3) . ? Cu1 O4 1.961(3) 2_557 ? Cu1 O2 1.962(3) 2_557 ? Cu1 O1 1.965(3) . ? Cu1 N1 2.172(3) . ? Cu1 Cu1 2.6005(9) 2_557 ? N1 C27 1.326(5) . ? N1 C28 1.335(5) . ? O1 C1 1.256(5) . ? O3 C14 1.256(5) . ? C16 C17 1.374(6) . ? C16 C15 1.385(6) . ? C16 H16 0.9500 . ? C15 C20 1.401(6) . ? C15 C14 1.496(6) . ? C23 C22 1.372(6) . ? C23 C24 1.393(7) . ? C23 H23 0.9500 . ? C21 C22 1.388(6) . ? C21 C26 1.402(6) . ? C21 C18 1.478(6) . ? C20 C19 1.381(6) . ? C20 H20 0.9500 . ? C19 C18 1.395(6) . ? C19 H19 0.9500 . ? C17 C18 1.398(6) . ? C17 H17 0.9500 . ? C14 O4 1.254(5) . ? C27 C28 1.358(6) 2_657 ? C27 H27 0.9500 . ? C22 H22 0.9500 . ? C26 C25 1.375(7) . ? C26 H26 0.9500 . ? C24 C25 1.381(7) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C1 O2 1.265(5) . ? C1 C2 1.488(6) . ? O2 Cu1 1.962(3) 2_557 ? C2 C7 1.389(6) . ? C2 C3 1.397(6) . ? C7 C6 1.379(6) . ? C7 H7 0.9500 . ? C3 C4 1.358(6) . ? C3 H3 0.9500 . ? C4 C5 1.418(7) . ? C4 H4 0.9500 . ? C6 C5 1.416(7) . ? C6 H6 0.9500 . ? C5 C8 1.463(7) . ? C8 C9 1.365(8) . ? C8 C13 1.394(8) . ? C13 C12 1.394(8) . ? C13 H13 0.9500 . ? C9 C10 1.402(9) . ? C9 H9 0.9500 . ? C12 C11 1.342(10) . ? C12 H12 0.9500 . ? C10 C11 1.395(10) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? O4 Cu1 1.961(3) 2_557 ? C28 C27 1.358(6) 2_657 ? C28 H28 0.9500 . ? C35 C34 1.333(9) . ? C35 C30 1.365(9) . ? C35 H35 0.9500 . ? C34 C33 1.299(10) . ? C34 H34 0.9500 . ? C30 C31 1.425(11) . ? C30 C29 1.446(12) . ? C33 C32 1.310(11) . ? C33 H33 0.9500 . ? C32 C31 1.434(11) . ? C32 H32 0.9500 . ? C31 H31 0.9500 . ? C29 O5 1.472(13) . ? C29 O5A 1.475(13) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 H29C 0.9900 . ? C29 H29D 0.9900 . ? 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 Cu1 O4 169.00(11) . 2_557 ? O3 Cu1 O2 89.80(14) . 2_557 ? O4 Cu1 O2 89.69(14) 2_557 2_557 ? O3 Cu1 O1 89.93(13) . . ? O4 Cu1 O1 88.53(13) 2_557 . ? O2 Cu1 O1 169.26(11) 2_557 . ? O3 Cu1 N1 94.28(12) . . ? O4 Cu1 N1 96.70(12) 2_557 . ? O2 Cu1 N1 95.73(11) 2_557 . ? O1 Cu1 N1 94.99(11) . . ? O3 Cu1 Cu1 83.49(8) . 2_557 ? O4 Cu1 Cu1 85.52(8) 2_557 2_557 ? O2 Cu1 Cu1 84.74(8) 2_557 2_557 ? O1 Cu1 Cu1 84.56(8) . 2_557 ? N1 Cu1 Cu1 177.73(9) . 2_557 ? C27 N1 C28 116.2(3) . . ? C27 N1 Cu1 121.9(3) . . ? C28 N1 Cu1 121.9(3) . . ? C1 O1 Cu1 123.1(3) . . ? C14 O3 Cu1 124.3(3) . . ? C17 C16 C15 120.7(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C15 C20 118.6(4) . . ? C16 C15 C14 121.0(4) . . ? C20 C15 C14 120.4(4) . . ? C22 C23 C24 119.0(4) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C22 C21 C26 116.6(4) . . ? C22 C21 C18 122.1(4) . . ? C26 C21 C18 121.2(4) . . ? C19 C20 C15 120.1(4) . . ? C19 C20 H20 119.9 . . ? C15 C20 H20 119.9 . . ? C20 C19 C18 121.6(4) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C16 C17 C18 121.7(4) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C19 C18 C17 117.2(4) . . ? C19 C18 C21 121.3(4) . . ? C17 C18 C21 121.6(4) . . ? O4 C14 O3 125.0(4) . . ? O4 C14 C15 117.4(4) . . ? O3 C14 C15 117.6(4) . . ? N1 C27 C28 122.8(4) . 2_657 ? N1 C27 H27 118.6 . . ? C28 C27 H27 118.6 2_657 . ? C23 C22 C21 122.9(4) . . ? C23 C22 H22 118.5 . . ? C21 C22 H22 118.5 . . ? C25 C26 C21 121.5(4) . . ? C25 C26 H26 119.2 . . ? C21 C26 H26 119.2 . . ? C25 C24 C23 119.8(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 120.1(5) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? O1 C1 O2 124.8(4) . . ? O1 C1 C2 118.3(4) . . ? O2 C1 C2 116.8(4) . . ? C1 O2 Cu1 122.8(3) . 2_557 ? C7 C2 C3 117.8(4) . . ? C7 C2 C1 121.0(4) . . ? C3 C2 C1 121.2(4) . . ? C6 C7 C2 121.6(4) . . ? C6 C7 H7 119.2 . . ? C2 C7 H7 119.2 . . ? C4 C3 C2 121.5(4) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 121.8(4) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C7 C6 C5 120.9(4) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C5 C4 116.4(4) . . ? C6 C5 C8 121.7(4) . . ? C4 C5 C8 121.9(4) . . ? C9 C8 C13 118.1(5) . . ? C9 C8 C5 121.2(5) . . ? C13 C8 C5 120.7(5) . . ? C8 C13 C12 120.2(6) . . ? C8 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C8 C9 C10 121.2(6) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C12 C13 121.9(7) . . ? C11 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C11 C10 C9 120.0(7) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 118.6(6) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C14 O4 Cu1 121.6(3) . 2_557 ? N1 C28 C27 121.0(4) . 2_657 ? N1 C28 H28 119.5 . . ? C27 C28 H28 119.5 2_657 . ? C34 C35 C30 120.2(7) . . ? C34 C35 H35 119.9 . . ? C30 C35 H35 119.9 . . ? C33 C34 C35 123.7(8) . . ? C33 C34 H34 118.2 . . ? C35 C34 H34 118.2 . . ? C35 C30 C31 117.3(7) . . ? C35 C30 C29 124.8(9) . . ? C31 C30 C29 117.9(9) . . ? C34 C33 C32 121.7(9) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C33 C32 C31 119.0(8) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C30 C31 C32 118.1(7) . . ? C30 C31 H31 120.9 . . ? C32 C31 H31 120.9 . . ? C30 C29 O5 118.9(9) . . ? C30 C29 O5A 119.9(10) . . ? O5 C29 O5A 42.6(7) . . ? C30 C29 H29A 107.4 . . ? O5 C29 H29A 133.1 . . ? O5A C29 H29A 107.4 . . ? C30 C29 H29B 107.4 . . ? O5 C29 H29B 67.5 . . ? O5A C29 H29B 107.4 . . ? H29A C29 H29B 106.9 . . ? C30 C29 H29C 107.6 . . ? O5 C29 H29C 107.6 . . ? O5A C29 H29C 67.1 . . ? H29A C29 H29C 47.0 . . ? H29B C29 H29C 141.7 . . ? C30 C29 H29D 107.6 . . ? O5 C29 H29D 107.6 . . ? O5A C29 H29D 131.9 . . ? H29A C29 H29D 62.2 . . ? H29B C29 H29D 46.6 . . ? H29C C29 H29D 107.0 . . ? 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 O3 Cu1 N1 C27 25.4(3) . . . . ? O4 Cu1 N1 C27 -154.0(3) 2_557 . . . ? O2 Cu1 N1 C27 115.6(3) 2_557 . . . ? O1 Cu1 N1 C27 -64.9(3) . . . . ? Cu1 Cu1 N1 C27 14(2) 2_557 . . . ? O3 Cu1 N1 C28 -155.1(3) . . . . ? O4 Cu1 N1 C28 25.5(3) 2_557 . . . ? O2 Cu1 N1 C28 -64.9(3) 2_557 . . . ? O1 Cu1 N1 C28 114.6(3) . . . . ? Cu1 Cu1 N1 C28 -167(2) 2_557 . . . ? O3 Cu1 O1 C1 82.4(3) . . . . ? O4 Cu1 O1 C1 -86.7(3) 2_557 . . . ? O2 Cu1 O1 C1 -6.2(9) 2_557 . . . ? N1 Cu1 O1 C1 176.7(3) . . . . ? Cu1 Cu1 O1 C1 -1.1(3) 2_557 . . . ? O4 Cu1 O3 C14 -4.8(9) 2_557 . . . ? O2 Cu1 O3 C14 82.5(3) 2_557 . . . ? O1 Cu1 O3 C14 -86.7(3) . . . . ? N1 Cu1 O3 C14 178.3(3) . . . . ? Cu1 Cu1 O3 C14 -2.2(3) 2_557 . . . ? C17 C16 C15 C20 2.1(7) . . . . ? C17 C16 C15 C14 -179.0(4) . . . . ? C16 C15 C20 C19 -1.7(7) . . . . ? C14 C15 C20 C19 179.4(4) . . . . ? C15 C20 C19 C18 -0.1(7) . . . . ? C15 C16 C17 C18 -0.8(8) . . . . ? C20 C19 C18 C17 1.4(7) . . . . ? C20 C19 C18 C21 -177.5(4) . . . . ? C16 C17 C18 C19 -0.9(7) . . . . ? C16 C17 C18 C21 177.9(4) . . . . ? C22 C21 C18 C19 152.2(5) . . . . ? C26 C21 C18 C19 -27.6(7) . . . . ? C22 C21 C18 C17 -26.6(7) . . . . ? C26 C21 C18 C17 153.6(5) . . . . ? Cu1 O3 C14 O4 3.8(6) . . . . ? Cu1 O3 C14 C15 -177.2(3) . . . . ? C16 C15 C14 O4 9.9(6) . . . . ? C20 C15 C14 O4 -171.1(4) . . . . ? C16 C15 C14 O3 -169.1(4) . . . . ? C20 C15 C14 O3 9.8(6) . . . . ? C28 N1 C27 C28 -0.2(7) . . . 2_657 ? Cu1 N1 C27 C28 179.3(3) . . . 2_657 ? C24 C23 C22 C21 0.8(7) . . . . ? C26 C21 C22 C23 -0.9(7) . . . . ? C18 C21 C22 C23 179.4(4) . . . . ? C22 C21 C26 C25 -0.3(7) . . . . ? C18 C21 C26 C25 179.5(5) . . . . ? C22 C23 C24 C25 0.4(8) . . . . ? C21 C26 C25 C24 1.4(8) . . . . ? C23 C24 C25 C26 -1.5(8) . . . . ? Cu1 O1 C1 O2 0.5(6) . . . . ? Cu1 O1 C1 C2 176.8(3) . . . . ? O1 C1 O2 Cu1 0.8(6) . . . 2_557 ? C2 C1 O2 Cu1 -175.5(3) . . . 2_557 ? O1 C1 C2 C7 -8.8(6) . . . . ? O2 C1 C2 C7 167.8(4) . . . . ? O1 C1 C2 C3 171.0(4) . . . . ? O2 C1 C2 C3 -12.4(6) . . . . ? C3 C2 C7 C6 2.6(8) . . . . ? C1 C2 C7 C6 -177.5(5) . . . . ? C7 C2 C3 C4 -0.9(8) . . . . ? C1 C2 C3 C4 179.3(5) . . . . ? C2 C3 C4 C5 -0.4(8) . . . . ? C2 C7 C6 C5 -3.1(8) . . . . ? C7 C6 C5 C4 1.7(8) . . . . ? C7 C6 C5 C8 178.9(5) . . . . ? C3 C4 C5 C6 0.0(8) . . . . ? C3 C4 C5 C8 -177.2(5) . . . . ? C6 C5 C8 C9 -145.4(6) . . . . ? C4 C5 C8 C9 31.7(9) . . . . ? C6 C5 C8 C13 34.1(9) . . . . ? C4 C5 C8 C13 -148.9(6) . . . . ? C9 C8 C13 C12 -0.7(10) . . . . ? C5 C8 C13 C12 179.8(6) . . . . ? C13 C8 C9 C10 -1.3(11) . . . . ? C5 C8 C9 C10 178.2(7) . . . . ? C8 C13 C12 C11 1.5(12) . . . . ? C8 C9 C10 C11 2.6(12) . . . . ? C13 C12 C11 C10 -0.2(13) . . . . ? C9 C10 C11 C12 -1.8(13) . . . . ? O3 C14 O4 Cu1 -3.0(6) . . . 2_557 ? C15 C14 O4 Cu1 178.0(3) . . . 2_557 ? C27 N1 C28 C27 0.2(6) . . . 2_657 ? Cu1 N1 C28 C27 -179.3(3) . . . 2_657 ? C30 C35 C34 C33 1.2(10) . . . . ? C34 C35 C30 C31 -1.2(9) . . . . ? C34 C35 C30 C29 179.1(6) . . . . ? C35 C34 C33 C32 -0.3(12) . . . . ? C34 C33 C32 C31 -0.5(13) . . . . ? C35 C30 C31 C32 0.4(10) . . . . ? C29 C30 C31 C32 -179.8(7) . . . . ? C33 C32 C31 C30 0.4(12) . . . . ? C35 C30 C29 O5 -126.9(12) . . . . ? C31 C30 C29 O5 53.4(14) . . . . ? C35 C30 C29 O5A -176.1(9) . . . . ? C31 C30 C29 O5A 4.2(13) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.15 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.900 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.105 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.053 0.000 0.500 719 136 ' ' _platon_squeeze_details ; ; #===end data_compound2_bath820 _database_code_depnum_ccdc_archive 'CCDC 859603' #TrackingRef '- warren-pw.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.50 H29 Cu N O4.50' _chemical_formula_weight 569.11 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' Cu Cu 0.3201 1.2651 '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 23.320(3) _cell_length_b 9.5701(14) _cell_length_c 26.478(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.799(2) _cell_angle_gamma 90.00 _cell_volume 5738.7(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3619 _cell_measurement_theta_min 2.258 _cell_measurement_theta_max 25.164 _exptl_crystal_description Block _exptl_crystal_colour ? _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.7848 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker APEXII diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22246 _diffrn_reflns_av_R_equivalents 0.0727 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5395 _reflns_number_gt 3400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. The asymmetric unit consists of two copper atoms (1/2 occupancy by virtue of location on a crystallographic 2-fold rotation axis), two carboxylate ligands, one 1/2 occupancy dabco ligand (nitrogen atoms located on the same axis as the copper atoms) and a fragment of very disordered solvent. This solvent was treated with the PLATON SQUEEZE function and thus determined to approximate to half a benzyl alcohol per asymmetric unit. ; _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^)+(0.1352P)^2^+8.3797P] 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 SHELXL _refine_ls_extinction_coef 0.0070(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5395 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1143 _refine_ls_R_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.2340 _refine_ls_wR_factor_gt 0.2140 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 Cu1 Cu 0.0000 0.86702(8) 0.2500 0.0476(4) Uani 1 2 d S . . Cu2 Cu 0.0000 0.59344(8) 0.2500 0.0519(4) Uani 1 2 d S . . O1 O 0.04176(17) 0.8404(3) 0.19387(16) 0.0533(10) Uani 1 1 d . A 1 O2 O 0.01952(18) 0.6118(3) 0.18230(16) 0.0562(11) Uani 1 1 d . A 1 O3 O 0.07582(16) 0.8479(3) 0.30229(15) 0.0504(10) Uani 1 1 d . A . O4 O 0.08483(17) 0.6212(3) 0.28445(17) 0.0570(11) Uani 1 1 d . . . N1 N 0.0000 1.0955(5) 0.2500 0.0446(16) Uani 1 2 d S . . N2 N 0.0000 1.3645(5) 0.2500 0.0464(16) Uani 1 2 d S . . C1 C 0.0404(2) 0.7255(5) 0.1693(2) 0.0520(15) Uani 1 1 d . A 1 C2 C 0.0648(3) 0.7205(5) 0.1230(2) 0.0541(15) Uani 1 1 d . A 1 C3 C 0.0888(3) 0.8392(6) 0.1050(3) 0.0549(15) Uani 1 1 d . A 1 H3 H 0.0896 0.9248 0.1233 0.066 Uiso 1 1 calc R A 1 C4 C 0.1109(3) 0.8349(6) 0.0624(3) 0.0600(17) Uani 1 1 d . A 1 H4 H 0.1263 0.9182 0.0512 0.072 Uiso 1 1 calc R A 1 C5 C 0.1118(3) 0.7110(6) 0.0337(3) 0.0600(17) Uani 1 1 d . A 1 C6 C 0.0900(4) 0.5918(6) 0.0531(3) 0.076(2) Uani 1 1 d . A 1 H6 H 0.0919 0.5045 0.0366 0.091 Uiso 1 1 calc R A 1 C7 C 0.0663(4) 0.5975(6) 0.0947(3) 0.070(2) Uani 1 1 d . A 1 H7 H 0.0499 0.5148 0.1053 0.084 Uiso 1 1 calc R A 1 C8 C 0.1343(3) 0.7052(6) -0.0142(3) 0.0646(18) Uani 1 1 d . A 1 C9 C 0.1131(4) 0.6105(7) -0.0528(3) 0.082(2) Uani 1 1 d . A 1 H9 H 0.0824 0.5484 -0.0495 0.098 Uiso 1 1 calc R A 1 C10 C 0.1360(5) 0.6037(9) -0.0971(4) 0.099(3) Uani 1 1 d . A 1 H10 H 0.1209 0.5350 -0.1227 0.119 Uiso 1 1 calc R A 1 C12 C 0.1981(5) 0.7891(9) -0.0691(4) 0.118(4) Uani 1 1 d . A 1 H12 H 0.2267 0.8542 -0.0748 0.142 Uiso 1 1 calc R A 1 C13 C 0.1772(5) 0.7968(9) -0.0240(4) 0.108(3) Uani 1 1 d . A 1 H13 H 0.1926 0.8669 0.0009 0.129 Uiso 1 1 calc R A 1 C14 C 0.1040(2) 0.7341(5) 0.3062(2) 0.0497(14) Uani 1 1 d . A . C15 C 0.1647(2) 0.7335(5) 0.3400(2) 0.0462(13) Uani 1 1 d . . . C16 C 0.1833(3) 0.8353(6) 0.3777(3) 0.0618(17) Uani 1 1 d . A . H16 H 0.1570 0.9082 0.3816 0.074 Uiso 1 1 calc R . . C17 C 0.2388(3) 0.8313(6) 0.4091(3) 0.0602(17) Uani 1 1 d . . . H17 H 0.2502 0.9002 0.4355 0.072 Uiso 1 1 calc R A . C18 C 0.2793(2) 0.7280(5) 0.4035(2) 0.0465(13) Uani 1 1 d . A . C19 C 0.2603(2) 0.6279(5) 0.3658(2) 0.0491(14) Uani 1 1 d . . . H19 H 0.2869 0.5565 0.3611 0.059 Uiso 1 1 calc R A . C20 C 0.2037(2) 0.6291(5) 0.3348(2) 0.0471(13) Uani 1 1 d . A . H20 H 0.1914 0.5575 0.3097 0.056 Uiso 1 1 calc R . . C21 C 0.3399(3) 0.7239(5) 0.4367(2) 0.0505(14) Uani 1 1 d . . . C22 C 0.3506(3) 0.7333(7) 0.4906(3) 0.0699(18) Uani 1 1 d . A . H22 H 0.3184 0.7464 0.5064 0.084 Uiso 1 1 calc R . . C23 C 0.4068(3) 0.7240(8) 0.5212(3) 0.078(2) Uani 1 1 d . . . H23 H 0.4133 0.7294 0.5580 0.094 Uiso 1 1 calc R A . C24 C 0.4545(3) 0.7066(7) 0.4989(3) 0.078(2) Uani 1 1 d . A . H24 H 0.4934 0.6991 0.5202 0.094 Uiso 1 1 calc R . . C25 C 0.4451(3) 0.7004(6) 0.4463(3) 0.0665(18) Uani 1 1 d . . . H25 H 0.4776 0.6904 0.4307 0.080 Uiso 1 1 calc R A . C26 C 0.3883(3) 0.7086(6) 0.4151(3) 0.0568(15) Uani 1 1 d . A . H26 H 0.3823 0.7036 0.3784 0.068 Uiso 1 1 calc R . . C27 C 0.0135(6) 1.1451(9) 0.1986(4) 0.049(3) Uani 0.50 1 d P B -1 H27A H 0.0524 1.1087 0.1960 0.058 Uiso 0.50 1 calc PR B -1 H27B H -0.0169 1.1088 0.1688 0.058 Uiso 0.50 1 calc PR B -1 C28 C 0.0139(5) 1.3054(9) 0.1972(4) 0.043(2) Uani 0.50 1 d P B -1 H28A H -0.0163 1.3392 0.1667 0.052 Uiso 1 1 calc R B -1 H28B H 0.0530 1.3391 0.1939 0.052 Uiso 1 1 calc R B -1 C29 C -0.0562(5) 1.1492(9) 0.2515(6) 0.056(3) Uani 0.50 1 d P B -1 H29A H -0.0670 1.1151 0.2833 0.067 Uiso 0.50 1 calc PR B -1 H29B H -0.0860 1.1140 0.2210 0.067 Uiso 0.50 1 calc PR B -1 C30 C -0.0570(4) 1.3123(10) 0.2511(5) 0.041(3) Uani 0.50 1 d P B -1 H30A H -0.0866 1.3461 0.2202 0.050 Uiso 0.50 1 calc PR B -1 H30B H -0.0684 1.3471 0.2826 0.050 Uiso 0.50 1 calc PR B -1 C31 C 0.0470(6) 1.1532(9) 0.2923(5) 0.051(3) Uani 0.50 1 d P B -1 H31A H 0.0858 1.1181 0.2888 0.061 Uiso 0.50 1 calc PR B -1 H31B H 0.0410 1.1213 0.3262 0.061 Uiso 0.50 1 calc PR B -1 C32 C 0.0468(5) 1.3122(9) 0.2907(6) 0.055(3) Uani 0.50 1 d P B -1 H32A H 0.0423 1.3489 0.3245 0.066 Uiso 0.50 1 calc PR B -1 H32B H 0.0851 1.3456 0.2853 0.066 Uiso 0.50 1 calc PR B -1 C33 C 0.1775(4) 0.6887(9) -0.1046(4) 0.093(3) Uani 1 1 d . A 1 H11 H 0.1929 0.6795 -0.1346 0.111 Uiso 1 1 calc R A 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 Cu1 0.0498(6) 0.0116(4) 0.0708(7) 0.000 -0.0067(5) 0.000 Cu2 0.0529(6) 0.0112(4) 0.0783(8) 0.000 -0.0107(5) 0.000 O1 0.059(2) 0.0198(17) 0.074(3) -0.0054(17) 0.001(2) 0.0008(15) O2 0.066(3) 0.0172(17) 0.076(3) -0.0029(16) -0.002(2) 0.0030(16) O3 0.051(2) 0.0220(17) 0.068(3) 0.0031(16) -0.0063(18) -0.0034(15) O4 0.053(2) 0.0202(17) 0.083(3) 0.0000(17) -0.013(2) -0.0038(15) N1 0.048(4) 0.015(3) 0.063(4) 0.000 -0.001(3) 0.000 N2 0.054(4) 0.014(3) 0.063(4) 0.000 -0.001(3) 0.000 C1 0.052(3) 0.021(2) 0.074(4) 0.004(2) -0.003(3) 0.005(2) C2 0.063(4) 0.022(2) 0.067(4) -0.002(2) -0.005(3) 0.007(2) C3 0.056(3) 0.035(3) 0.069(4) -0.012(3) 0.006(3) -0.004(2) C4 0.057(4) 0.039(3) 0.079(5) -0.013(3) 0.006(3) 0.000(3) C5 0.062(4) 0.035(3) 0.077(4) -0.004(3) 0.004(3) 0.012(3) C6 0.128(6) 0.027(3) 0.068(5) -0.006(3) 0.013(4) 0.018(3) C7 0.116(6) 0.025(3) 0.064(4) 0.002(3) 0.011(4) 0.005(3) C8 0.066(4) 0.038(3) 0.084(5) -0.010(3) 0.008(4) 0.009(3) C9 0.109(6) 0.055(4) 0.090(6) -0.017(4) 0.041(5) -0.009(4) C10 0.133(8) 0.064(5) 0.100(7) -0.023(4) 0.025(6) 0.015(5) C12 0.174(11) 0.059(5) 0.139(9) -0.012(5) 0.070(8) -0.010(6) C13 0.144(9) 0.065(5) 0.132(8) -0.036(5) 0.067(7) -0.017(5) C14 0.053(3) 0.019(2) 0.070(4) 0.006(2) 0.001(3) -0.007(2) C15 0.052(3) 0.022(2) 0.060(3) 0.005(2) 0.004(3) -0.004(2) C16 0.055(4) 0.038(3) 0.085(5) -0.015(3) 0.003(3) 0.005(3) C17 0.055(4) 0.040(3) 0.076(4) -0.015(3) -0.003(3) 0.003(3) C18 0.048(3) 0.034(3) 0.055(3) -0.003(2) 0.008(3) -0.004(2) C19 0.050(3) 0.036(3) 0.061(4) -0.004(2) 0.012(3) 0.000(2) C20 0.056(3) 0.034(3) 0.050(3) -0.005(2) 0.010(3) -0.005(2) C21 0.059(3) 0.035(3) 0.053(3) -0.005(2) 0.007(3) -0.004(2) C22 0.065(4) 0.072(4) 0.069(4) -0.007(3) 0.009(3) -0.004(3) C23 0.071(5) 0.086(5) 0.069(5) -0.003(4) -0.001(4) 0.000(4) C24 0.059(4) 0.069(5) 0.093(6) -0.011(4) -0.011(4) 0.004(3) C25 0.053(4) 0.048(4) 0.096(6) -0.019(3) 0.015(4) -0.005(3) C26 0.065(4) 0.035(3) 0.070(4) -0.005(3) 0.017(3) -0.003(3) C27 0.087(9) 0.019(5) 0.041(6) 0.003(4) 0.016(6) 0.000(5) C28 0.048(6) 0.022(5) 0.058(7) 0.009(4) 0.011(5) -0.005(4) C29 0.053(7) 0.011(4) 0.100(11) -0.001(5) 0.012(7) 0.007(4) C30 0.043(6) 0.022(5) 0.056(7) 0.013(5) 0.004(5) -0.002(4) C31 0.074(8) 0.011(4) 0.056(7) -0.008(4) -0.007(6) -0.005(4) C32 0.063(7) 0.008(4) 0.081(9) 0.002(5) -0.009(7) -0.006(4) C33 0.109(7) 0.061(5) 0.110(7) -0.018(5) 0.029(5) 0.003(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 Cu1 O3 1.977(3) 2 ? Cu1 O3 1.977(3) . ? Cu1 O1 1.978(4) . ? Cu1 O1 1.978(4) 2 ? Cu1 N1 2.187(5) . ? Cu1 Cu2 2.6182(11) . ? Cu2 O2 1.960(5) . ? Cu2 O2 1.960(5) 2 ? Cu2 O4 1.989(4) . ? Cu2 O4 1.989(4) 2 ? Cu2 N2 2.191(5) 1_545 ? O1 C1 1.274(6) . ? O2 C1 1.272(6) . ? O3 C14 1.264(6) . ? O4 C14 1.255(6) . ? N1 C29 1.416(11) 2 ? N1 C29 1.416(11) . ? N1 C31 1.474(10) 2 ? N1 C31 1.474(10) . ? N1 C27 1.542(11) . ? N1 C27 1.542(11) 2 ? N2 C30 1.427(10) . ? N2 C30 1.427(10) 2 ? N2 C32 1.429(11) 2 ? N2 C32 1.429(11) . ? N2 C28 1.613(11) . ? N2 C28 1.613(11) 2 ? N2 Cu2 2.191(5) 1_565 ? C1 C2 1.471(9) . ? C2 C3 1.399(8) . ? C2 C7 1.400(8) . ? C3 C4 1.347(9) . ? C3 H3 0.9500 . ? C4 C5 1.412(8) . ? C4 H4 0.9500 . ? C5 C6 1.397(9) . ? C5 C8 1.483(10) . ? C6 C7 1.345(10) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.368(9) . ? C8 C13 1.400(11) . ? C9 C10 1.401(11) . ? C9 H9 0.9500 . ? C10 C33 1.316(12) . ? C10 H10 0.9500 . ? C12 C33 1.348(12) . ? C12 C13 1.396(13) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.484(7) . ? C15 C20 1.378(7) . ? C15 C16 1.388(8) . ? C16 C17 1.363(8) . ? C16 H16 0.9500 . ? C17 C18 1.400(8) . ? C17 H17 0.9500 . ? C18 C19 1.378(7) . ? C18 C21 1.478(8) . ? C19 C20 1.380(7) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.388(9) . ? C21 C22 1.392(9) . ? C22 C23 1.370(9) . ? C22 H22 0.9500 . ? C23 C24 1.389(11) . ? C23 H23 0.9500 . ? C24 C25 1.358(10) . ? C24 H24 0.9500 . ? C25 C26 1.385(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.535(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.561(13) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.522(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H11 0.9500 . ? 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 Cu1 O3 169.37(19) 2 . ? O3 Cu1 O1 88.87(16) 2 . ? O3 Cu1 O1 89.76(16) . . ? O3 Cu1 O1 89.76(16) 2 2 ? O3 Cu1 O1 88.87(16) . 2 ? O1 Cu1 O1 165.18(19) . 2 ? O3 Cu1 N1 95.31(9) 2 . ? O3 Cu1 N1 95.31(9) . . ? O1 Cu1 N1 97.41(10) . . ? O1 Cu1 N1 97.41(10) 2 . ? O3 Cu1 Cu2 84.69(9) 2 . ? O3 Cu1 Cu2 84.69(9) . . ? O1 Cu1 Cu2 82.59(10) . . ? O1 Cu1 Cu2 82.59(10) 2 . ? N1 Cu1 Cu2 180.000(1) . . ? O2 Cu2 O2 169.70(19) . 2 ? O2 Cu2 O4 89.14(18) . . ? O2 Cu2 O4 89.49(18) 2 . ? O2 Cu2 O4 89.49(18) . 2 ? O2 Cu2 O4 89.14(18) 2 2 ? O4 Cu2 O4 164.63(19) . 2 ? O2 Cu2 N2 95.15(9) . 1_545 ? O2 Cu2 N2 95.15(9) 2 1_545 ? O4 Cu2 N2 97.69(10) . 1_545 ? O4 Cu2 N2 97.69(10) 2 1_545 ? O2 Cu2 Cu1 84.85(9) . . ? O2 Cu2 Cu1 84.85(9) 2 . ? O4 Cu2 Cu1 82.31(10) . . ? O4 Cu2 Cu1 82.31(10) 2 . ? N2 Cu2 Cu1 180.0 1_545 . ? C1 O1 Cu1 122.5(4) . . ? C1 O2 Cu2 120.8(4) . . ? C14 O3 Cu1 119.9(3) . . ? C14 O4 Cu2 122.2(4) . . ? C29 N1 C29 137.5(9) 2 . ? C29 N1 C31 111.6(7) 2 2 ? C29 N1 C31 50.2(7) . 2 ? C29 N1 C31 50.2(7) 2 . ? C29 N1 C31 111.6(7) . . ? C31 N1 C31 136.0(8) 2 . ? C29 N1 C27 58.6(7) 2 . ? C29 N1 C27 107.3(8) . . ? C31 N1 C27 59.1(7) 2 . ? C31 N1 C27 106.5(7) . . ? C29 N1 C27 107.3(8) 2 2 ? C29 N1 C27 58.6(7) . 2 ? C31 N1 C27 106.5(7) 2 2 ? C31 N1 C27 59.1(7) . 2 ? C27 N1 C27 144.2(8) . 2 ? C29 N1 Cu1 111.2(4) 2 . ? C29 N1 Cu1 111.2(4) . . ? C31 N1 Cu1 112.0(4) 2 . ? C31 N1 Cu1 112.0(4) . . ? C27 N1 Cu1 107.9(4) . . ? C27 N1 Cu1 107.9(4) 2 . ? C30 N2 C30 139.1(9) . 2 ? C30 N2 C32 49.1(7) . 2 ? C30 N2 C32 114.2(6) 2 2 ? C30 N2 C32 114.2(6) . . ? C30 N2 C32 49.1(7) 2 . ? C32 N2 C32 139.0(8) 2 . ? C30 N2 C28 106.1(6) . . ? C30 N2 C28 58.5(6) 2 . ? C32 N2 C28 59.9(7) 2 . ? C32 N2 C28 104.8(7) . . ? C30 N2 C28 58.5(6) . 2 ? C30 N2 C28 106.1(6) 2 2 ? C32 N2 C28 104.8(7) 2 2 ? C32 N2 C28 59.9(7) . 2 ? C28 N2 C28 138.9(7) . 2 ? C30 N2 Cu2 110.5(4) . 1_565 ? C30 N2 Cu2 110.5(4) 2 1_565 ? C32 N2 Cu2 110.5(4) 2 1_565 ? C32 N2 Cu2 110.5(4) . 1_565 ? C28 N2 Cu2 110.5(4) . 1_565 ? C28 N2 Cu2 110.5(4) 2 1_565 ? O2 C1 O1 124.4(6) . . ? O2 C1 C2 116.6(5) . . ? O1 C1 C2 119.1(5) . . ? C3 C2 C7 115.9(6) . . ? C3 C2 C1 121.6(5) . . ? C7 C2 C1 122.5(5) . . ? C4 C3 C2 121.6(5) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 122.3(6) . . ? C3 C4 H4 118.8 . . ? C5 C4 H4 118.8 . . ? C6 C5 C4 115.7(7) . . ? C6 C5 C8 121.3(5) . . ? C4 C5 C8 123.0(6) . . ? C7 C6 C5 121.8(6) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C2 122.6(6) . . ? C6 C7 H7 118.7 . . ? C2 C7 H7 118.7 . . ? C9 C8 C13 115.0(7) . . ? C9 C8 C5 121.6(6) . . ? C13 C8 C5 123.3(6) . . ? C8 C9 C10 120.9(8) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C33 C10 C9 122.6(8) . . ? C33 C10 H10 118.7 . . ? C9 C10 H10 118.7 . . ? C33 C12 C13 119.6(9) . . ? C33 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C8 122.5(8) . . ? C12 C13 H13 118.7 . . ? C8 C13 H13 118.7 . . ? O4 C14 O3 125.6(5) . . ? O4 C14 C15 117.3(4) . . ? O3 C14 C15 117.1(4) . . ? C20 C15 C16 118.8(5) . . ? C20 C15 C14 119.9(5) . . ? C16 C15 C14 121.3(5) . . ? C17 C16 C15 120.5(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 121.4(5) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 117.5(5) . . ? C19 C18 C21 120.6(5) . . ? C17 C18 C21 122.0(5) . . ? C18 C19 C20 121.4(5) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C15 C20 C19 120.5(5) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C26 C21 C22 117.7(6) . . ? C26 C21 C18 120.9(5) . . ? C22 C21 C18 121.4(6) . . ? C23 C22 C21 120.9(7) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.4(7) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 119.4(7) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 120.4(7) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 121.1(6) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C28 C27 N1 109.5(8) . . ? C28 C27 H27A 109.8 . . ? N1 C27 H27A 109.8 . . ? C28 C27 H27B 109.8 . . ? N1 C27 H27B 109.8 . . ? H27A C27 H27B 108.2 . . ? C27 C28 N2 108.9(8) . . ? C27 C28 H28A 109.9 . . ? N2 C28 H28A 109.9 . . ? C27 C28 H28B 109.9 . . ? N2 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? N1 C29 C30 111.9(8) . . ? N1 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? N1 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? N2 C30 C29 109.8(8) . . ? N2 C30 H30A 109.7 . . ? C29 C30 H30A 109.7 . . ? N2 C30 H30B 109.7 . . ? C29 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? N1 C31 C32 110.9(8) . . ? N1 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? N1 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.0 . . ? N2 C32 C31 111.6(8) . . ? N2 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? N2 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C10 C33 C12 119.3(10) . . ? C10 C33 H11 120.4 . . ? C12 C33 H11 120.4 . . ? 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 Cu1 Cu2 O2 73.81(17) 2 . . . ? O3 Cu1 Cu2 O2 -106.19(17) . . . . ? O1 Cu1 Cu2 O2 -15.74(16) . . . . ? O1 Cu1 Cu2 O2 164.26(16) 2 . . . ? N1 Cu1 Cu2 O2 117(100) . . . . ? O3 Cu1 Cu2 O2 -106.19(17) 2 . . 2 ? O3 Cu1 Cu2 O2 73.81(17) . . . 2 ? O1 Cu1 Cu2 O2 164.26(16) . . . 2 ? O1 Cu1 Cu2 O2 -15.74(16) 2 . . 2 ? N1 Cu1 Cu2 O2 -63(100) . . . 2 ? O3 Cu1 Cu2 O4 163.63(18) 2 . . . ? O3 Cu1 Cu2 O4 -16.37(18) . . . . ? O1 Cu1 Cu2 O4 74.09(17) . . . . ? O1 Cu1 Cu2 O4 -105.91(17) 2 . . . ? N1 Cu1 Cu2 O4 -153(100) . . . . ? O3 Cu1 Cu2 O4 -16.37(18) 2 . . 2 ? O3 Cu1 Cu2 O4 163.63(18) . . . 2 ? O1 Cu1 Cu2 O4 -105.91(17) . . . 2 ? O1 Cu1 Cu2 O4 74.09(17) 2 . . 2 ? N1 Cu1 Cu2 O4 27(100) . . . 2 ? O3 Cu1 Cu2 N2 -119(100) 2 . . 1_545 ? O3 Cu1 Cu2 N2 61(100) . . . 1_545 ? O1 Cu1 Cu2 N2 151(100) . . . 1_545 ? O1 Cu1 Cu2 N2 -29(100) 2 . . 1_545 ? N1 Cu1 Cu2 N2 0(60) . . . 1_545 ? O3 Cu1 O1 C1 -66.4(4) 2 . . . ? O3 Cu1 O1 C1 103.0(4) . . . . ? O1 Cu1 O1 C1 18.3(4) 2 . . . ? N1 Cu1 O1 C1 -161.7(4) . . . . ? Cu2 Cu1 O1 C1 18.3(4) . . . . ? O2 Cu2 O2 C1 19.0(4) 2 . . . ? O4 Cu2 O2 C1 -63.4(4) . . . . ? O4 Cu2 O2 C1 101.3(4) 2 . . . ? N2 Cu2 O2 C1 -161.0(4) 1_545 . . . ? Cu1 Cu2 O2 C1 19.0(4) . . . . ? O3 Cu1 O3 C14 19.1(4) 2 . . . ? O1 Cu1 O3 C14 -63.5(4) . . . . ? O1 Cu1 O3 C14 101.8(4) 2 . . . ? N1 Cu1 O3 C14 -160.9(4) . . . . ? Cu2 Cu1 O3 C14 19.1(4) . . . . ? O2 Cu2 O4 C14 104.7(5) . . . . ? O2 Cu2 O4 C14 -65.0(5) 2 . . . ? O4 Cu2 O4 C14 19.8(5) 2 . . . ? N2 Cu2 O4 C14 -160.2(5) 1_545 . . . ? Cu1 Cu2 O4 C14 19.8(5) . . . . ? O3 Cu1 N1 C29 -135.3(7) 2 . . 2 ? O3 Cu1 N1 C29 44.7(7) . . . 2 ? O1 Cu1 N1 C29 -45.7(7) . . . 2 ? O1 Cu1 N1 C29 134.3(7) 2 . . 2 ? Cu2 Cu1 N1 C29 -178(100) . . . 2 ? O3 Cu1 N1 C29 44.7(7) 2 . . . ? O3 Cu1 N1 C29 -135.3(7) . . . . ? O1 Cu1 N1 C29 134.3(7) . . . . ? O1 Cu1 N1 C29 -45.7(7) 2 . . . ? Cu2 Cu1 N1 C29 2(100) . . . . ? O3 Cu1 N1 C31 -9.6(6) 2 . . 2 ? O3 Cu1 N1 C31 170.4(6) . . . 2 ? O1 Cu1 N1 C31 79.9(6) . . . 2 ? O1 Cu1 N1 C31 -100.1(6) 2 . . 2 ? Cu2 Cu1 N1 C31 -53(100) . . . 2 ? O3 Cu1 N1 C31 170.4(6) 2 . . . ? O3 Cu1 N1 C31 -9.6(6) . . . . ? O1 Cu1 N1 C31 -100.1(6) . . . . ? O1 Cu1 N1 C31 79.9(6) 2 . . . ? Cu2 Cu1 N1 C31 127(100) . . . . ? O3 Cu1 N1 C27 -72.8(5) 2 . . . ? O3 Cu1 N1 C27 107.2(5) . . . . ? O1 Cu1 N1 C27 16.8(5) . . . . ? O1 Cu1 N1 C27 -163.2(5) 2 . . . ? Cu2 Cu1 N1 C27 -116(100) . . . . ? O3 Cu1 N1 C27 107.2(5) 2 . . 2 ? O3 Cu1 N1 C27 -72.8(5) . . . 2 ? O1 Cu1 N1 C27 -163.2(5) . . . 2 ? O1 Cu1 N1 C27 16.8(5) 2 . . 2 ? Cu2 Cu1 N1 C27 64(100) . . . 2 ? Cu2 O2 C1 O1 -11.3(7) . . . . ? Cu2 O2 C1 C2 167.9(3) . . . . ? Cu1 O1 C1 O2 -10.1(7) . . . . ? Cu1 O1 C1 C2 170.7(4) . . . . ? O2 C1 C2 C3 179.9(5) . . . . ? O1 C1 C2 C3 -0.8(8) . . . . ? O2 C1 C2 C7 -1.0(8) . . . . ? O1 C1 C2 C7 178.3(5) . . . . ? C7 C2 C3 C4 1.3(9) . . . . ? C1 C2 C3 C4 -179.6(5) . . . . ? C2 C3 C4 C5 -0.8(9) . . . . ? C3 C4 C5 C6 -1.8(9) . . . . ? C3 C4 C5 C8 178.2(6) . . . . ? C4 C5 C6 C7 3.9(10) . . . . ? C8 C5 C6 C7 -176.0(6) . . . . ? C5 C6 C7 C2 -3.6(11) . . . . ? C3 C2 C7 C6 0.9(10) . . . . ? C1 C2 C7 C6 -178.2(6) . . . . ? C6 C5 C8 C9 28.9(10) . . . . ? C4 C5 C8 C9 -151.0(7) . . . . ? C6 C5 C8 C13 -152.6(8) . . . . ? C4 C5 C8 C13 27.4(10) . . . . ? C13 C8 C9 C10 3.3(11) . . . . ? C5 C8 C9 C10 -178.1(7) . . . . ? C8 C9 C10 C33 -1.6(14) . . . . ? C33 C12 C13 C8 -1.2(16) . . . . ? C9 C8 C13 C12 -2.0(13) . . . . ? C5 C8 C13 C12 179.5(8) . . . . ? Cu2 O4 C14 O3 -11.8(9) . . . . ? Cu2 O4 C14 C15 167.3(4) . . . . ? Cu1 O3 C14 O4 -10.4(9) . . . . ? Cu1 O3 C14 C15 170.4(4) . . . . ? O4 C14 C15 C20 19.4(8) . . . . ? O3 C14 C15 C20 -161.4(5) . . . . ? O4 C14 C15 C16 -159.6(6) . . . . ? O3 C14 C15 C16 19.7(8) . . . . ? C20 C15 C16 C17 -0.4(9) . . . . ? C14 C15 C16 C17 178.6(6) . . . . ? C15 C16 C17 C18 2.0(10) . . . . ? C16 C17 C18 C19 -1.8(9) . . . . ? C16 C17 C18 C21 179.0(6) . . . . ? C17 C18 C19 C20 0.0(9) . . . . ? C21 C18 C19 C20 179.2(5) . . . . ? C16 C15 C20 C19 -1.4(9) . . . . ? C14 C15 C20 C19 179.7(5) . . . . ? C18 C19 C20 C15 1.6(9) . . . . ? C19 C18 C21 C26 49.3(8) . . . . ? C17 C18 C21 C26 -131.5(6) . . . . ? C19 C18 C21 C22 -129.8(6) . . . . ? C17 C18 C21 C22 49.4(8) . . . . ? C26 C21 C22 C23 -1.7(9) . . . . ? C18 C21 C22 C23 177.4(6) . . . . ? C21 C22 C23 C24 0.8(11) . . . . ? C22 C23 C24 C25 0.7(11) . . . . ? C23 C24 C25 C26 -1.2(10) . . . . ? C24 C25 C26 C21 0.3(9) . . . . ? C22 C21 C26 C25 1.1(8) . . . . ? C18 C21 C26 C25 -178.0(5) . . . . ? C29 N1 C27 C28 -75.5(9) 2 . . . ? C29 N1 C27 C28 60.1(10) . . . . ? C31 N1 C27 C28 74.7(9) 2 . . . ? C31 N1 C27 C28 -59.6(10) . . . . ? C27 N1 C27 C28 0.0(7) 2 . . . ? Cu1 N1 C27 C28 -180.0(7) . . . . ? N1 C27 C28 N2 -0.1(11) . . . . ? C30 N2 C28 C27 -60.2(9) . . . . ? C30 N2 C28 C27 78.0(9) 2 . . . ? C32 N2 C28 C27 -77.5(9) 2 . . . ? C32 N2 C28 C27 61.0(9) . . . . ? C28 N2 C28 C27 0.0(7) 2 . . . ? Cu2 N2 C28 C27 -180.0(7) 1_565 . . . ? C29 N1 C29 C30 0.4(8) 2 . . . ? C31 N1 C29 C30 -78.1(11) 2 . . . ? C31 N1 C29 C30 54.5(12) . . . . ? C27 N1 C29 C30 -61.8(12) . . . . ? C27 N1 C29 C30 81.8(11) 2 . . . ? Cu1 N1 C29 C30 -179.6(8) . . . . ? C30 N2 C30 C29 0.4(8) 2 . . . ? C32 N2 C30 C29 80.5(11) 2 . . . ? C32 N2 C30 C29 -54.3(11) . . . . ? C28 N2 C30 C29 60.6(11) . . . . ? C28 N2 C30 C29 -77.5(10) 2 . . . ? Cu2 N2 C30 C29 -179.6(8) 1_565 . . . ? N1 C29 C30 N2 -0.7(15) . . . . ? C29 N1 C31 C32 78.9(12) 2 . . . ? C29 N1 C31 C32 -55.7(12) . . . . ? C31 N1 C31 C32 -1.2(9) 2 . . . ? C27 N1 C31 C32 61.1(12) . . . . ? C27 N1 C31 C32 -82.9(11) 2 . . . ? Cu1 N1 C31 C32 178.8(9) . . . . ? C30 N2 C32 C31 53.5(13) . . . . ? C30 N2 C32 C31 -81.4(12) 2 . . . ? C32 N2 C32 C31 -1.2(9) 2 . . . ? C28 N2 C32 C31 -62.1(12) . . . . ? C28 N2 C32 C31 76.3(11) 2 . . . ? Cu2 N2 C32 C31 178.8(9) 1_565 . . . ? N1 C31 C32 N2 2.1(16) . . . . ? C9 C10 C33 C12 -1.8(15) . . . . ? C13 C12 C33 C10 3.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.916 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.092 #===end data_compound3_bath892 _database_code_depnum_ccdc_archive 'CCDC 859604' #TrackingRef '- warren-pw.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H62 N4 O10 Zn2' _chemical_formula_weight 1177.92 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 23.043(10) _cell_length_b 9.582(4) _cell_length_c 26.852(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.624(7) _cell_angle_gamma 90.00 _cell_volume 5737(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.74 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Station 11.3.1 ALS' _diffrn_radiation_monochromator 'Channel-cut Si(111)' _diffrn_measurement_device_type 'Bruker APEX2' _diffrn_measurement_method '3000 0.3 degree images with \f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10340 _diffrn_reflns_av_R_equivalents 0.1063 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.92 _diffrn_reflns_theta_max 20.65 _reflns_number_total 2253 _reflns_number_gt 1557 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1997)' _computing_molecular_graphics POVRAY _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In addition to the MOF fragment, the ASU also contains 1 molecule of DMF. Disorder (55:45) evident for carbons 22, 23, 25 and 26. CH2 groups in dabco ligan also disordered in 50:50 ratio, by virtue on the nitrogens therein being located on a crystallographic 2-fold rotation axis. Data truncated at 20o due to poor diffracting ability of this small sample at higher Bragg angles. ; _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^)+(0.0409P)^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 2253 _refine_ls_number_parameters 428 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.024 _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 -0.63772(12) 0.2500 0.0237(4) Uani 1 2 d S . . Zn2 Zn 0.0000 -0.93927(12) 0.2500 0.0261(4) Uani 1 2 d S . . O1 O 0.07643(19) -0.6726(5) 0.30704(16) 0.0242(13) Uani 1 1 d . . . O2 O 0.08841(18) -0.8952(5) 0.28428(17) 0.0283(12) Uani 1 1 d . . . O3 O -0.04841(17) -0.6800(5) 0.30392(17) 0.0269(13) Uani 1 1 d . . . O4 O -0.01824(19) -0.9046(5) 0.31870(17) 0.0283(13) Uani 1 1 d . . . O5 O 0.3198(3) -0.6973(7) 0.2645(2) 0.0789(19) Uani 1 1 d . . . N1 N 0.0000 -0.4205(8) 0.2500 0.021(2) Uani 1 2 d SU . . N2 N 0.0000 -0.1520(7) 0.2500 0.026(2) Uani 1 2 d SU . . N3 N 0.2621(3) -0.5276(7) 0.2894(2) 0.0493(18) Uani 1 1 d . . . C1 C 0.1070(3) -0.7847(10) 0.3087(3) 0.0254(17) Uani 1 1 d . . . C2 C 0.1696(3) -0.7835(8) 0.3424(3) 0.0228(16) Uani 1 1 d . . . C3 C 0.1874(3) -0.6919(8) 0.3830(3) 0.0332(19) Uani 1 1 d . . . H3 H 0.1595 -0.6257 0.3896 0.040 Uiso 1 1 calc R . . C4 C 0.2452(3) -0.6948(7) 0.4143(3) 0.0306(18) Uani 1 1 d . . . H4 H 0.2561 -0.6320 0.4425 0.037 Uiso 1 1 calc R . . C5 C 0.2876(3) -0.7883(8) 0.4051(3) 0.0275(17) Uani 1 1 d . . . C6 C 0.2691(3) -0.8817(7) 0.3638(3) 0.0307(19) Uani 1 1 d . . . H6 H 0.2970 -0.9472 0.3568 0.037 Uiso 1 1 calc R . . C7 C 0.2110(3) -0.8799(7) 0.3329(3) 0.0309(18) Uani 1 1 d . . . H7 H 0.1993 -0.9443 0.3053 0.037 Uiso 1 1 calc R . . C8 C 0.3495(3) -0.7958(7) 0.4387(3) 0.0285(18) Uani 1 1 d . . . C9 C 0.3606(3) -0.7917(8) 0.4919(3) 0.0359(19) Uani 1 1 d . . . H9 H 0.3279 -0.7802 0.5070 0.043 Uiso 1 1 calc R . . C10 C 0.4174(4) -0.8037(8) 0.5233(3) 0.050(2) Uani 1 1 d . . . H10 H 0.4238 -0.8008 0.5597 0.060 Uiso 1 1 calc R . . C11 C 0.4661(4) -0.8203(7) 0.5010(4) 0.049(2) Uani 1 1 d . . . H11 H 0.5057 -0.8298 0.5223 0.059 Uiso 1 1 calc R . . C12 C 0.4562(3) -0.8228(7) 0.4483(4) 0.041(2) Uani 1 1 d . . . H12 H 0.4891 -0.8335 0.4333 0.049 Uiso 1 1 calc R . . C13 C 0.3984(3) -0.8099(7) 0.4170(3) 0.034(2) Uani 1 1 d . . . H13 H 0.3921 -0.8107 0.3807 0.041 Uiso 1 1 calc R . . C14 C -0.0438(3) -0.7925(10) 0.3294(3) 0.0292(18) Uani 1 1 d . . . C15 C -0.0705(3) -0.7970(10) 0.3745(2) 0.0250(17) Uani 1 1 d . . . C16 C -0.1019(3) -0.6847(8) 0.3875(3) 0.029(2) Uani 1 1 d . . . H16 H -0.1076 -0.6035 0.3665 0.035 Uiso 1 1 calc R . . C17 C -0.1251(3) -0.6882(8) 0.4302(3) 0.0286(19) Uani 1 1 d . . . H17 H -0.1465 -0.6102 0.4382 0.034 Uiso 1 1 calc R . . C18 C -0.1169(3) -0.8071(9) 0.4619(3) 0.0335(19) Uani 1 1 d . A . C19 C -0.0854(3) -0.9214(8) 0.4483(3) 0.041(2) Uani 1 1 d . . . H19 H -0.0792 -1.0030 0.4691 0.049 Uiso 1 1 calc R . . C20 C -0.0634(3) -0.9156(8) 0.4051(3) 0.033(2) Uani 1 1 d . . . H20 H -0.0431 -0.9942 0.3962 0.039 Uiso 1 1 calc R . . C21 C -0.1379(3) -0.8096(9) 0.5099(3) 0.0332(18) Uani 1 1 d U . . C22 C -0.1888(7) -0.7289(14) 0.5158(5) 0.045(4) Uani 0.55 1 d P A 1 H22 H -0.2103 -0.6736 0.4878 0.054 Uiso 0.55 1 calc PR A 1 C23 C -0.2076(7) -0.7298(18) 0.5620(6) 0.057(4) Uani 0.55 1 d P A 1 H23 H -0.2401 -0.6736 0.5659 0.069 Uiso 0.55 1 calc PR A 1 C24 C -0.1768(4) -0.8161(10) 0.6016(3) 0.049(2) Uani 1 1 d . . . H24 H -0.1890 -0.8178 0.6328 0.058 Uiso 1 1 calc R A 1 C25 C -0.1318(9) -0.8949(18) 0.5978(7) 0.045(5) Uani 0.55 1 d P A 1 H25 H -0.1118 -0.9505 0.6262 0.054 Uiso 0.55 1 calc PR A 1 C26 C -0.1125(8) -0.8984(16) 0.5517(7) 0.039(4) Uani 0.55 1 d P A 1 H26 H -0.0819 -0.9620 0.5488 0.046 Uiso 0.55 1 calc PR A 1 C27 C 0.0492(6) -0.3629(16) 0.2935(6) 0.034(4) Uani 0.50 1 d PU B -1 H27A H 0.0883 -0.4011 0.2911 0.041 Uiso 0.50 1 calc PR B -1 H27B H 0.0424 -0.3932 0.3268 0.041 Uiso 0.50 1 calc PR B -1 C28 C 0.0514(5) -0.2036(15) 0.2920(5) 0.019(3) Uani 0.50 1 d PU B -1 H28A H 0.0487 -0.1647 0.3255 0.023 Uiso 0.50 1 calc PR B -1 H28B H 0.0898 -0.1727 0.2854 0.023 Uiso 0.50 1 calc PR B -1 C29 C 0.0144(7) -0.3689(17) 0.2021(6) 0.038(4) Uani 0.50 1 d PU B -1 H29A H -0.0157 -0.4053 0.1718 0.046 Uiso 0.50 1 calc PR B -1 H29B H 0.0542 -0.4049 0.2006 0.046 Uiso 0.50 1 calc PR B -1 C30 C 0.0149(6) -0.2104(16) 0.1998(5) 0.025(3) Uani 0.50 1 d PU B -1 H30A H -0.0153 -0.1773 0.1690 0.030 Uiso 0.50 1 calc PR B -1 H30B H 0.0549 -0.1769 0.1977 0.030 Uiso 0.50 1 calc PR B -1 C31 C -0.0549(6) -0.3658(16) 0.2542(7) 0.032(4) Uani 0.50 1 d PU B -1 H31A H -0.0631 -0.3982 0.2867 0.039 Uiso 0.50 1 calc PR B -1 H31B H -0.0874 -0.4009 0.2254 0.039 Uiso 0.50 1 calc PR B -1 C32 C -0.0546(6) -0.2084(15) 0.2532(6) 0.021(3) Uani 0.50 1 d PU B -1 H32A H -0.0864 -0.1759 0.2233 0.025 Uiso 0.50 1 calc PR B -1 H32B H -0.0643 -0.1731 0.2847 0.025 Uiso 0.50 1 calc PR B -1 C33 C 0.3122(4) -0.5993(11) 0.2943(4) 0.065(3) Uani 1 1 d . . . H33 H 0.3451 -0.5760 0.3222 0.078 Uiso 1 1 calc R . . C34 C 0.2067(3) -0.5536(9) 0.2507(3) 0.062(3) Uani 1 1 d . . . H34A H 0.2140 -0.6210 0.2255 0.093 Uiso 1 1 calc R . . H34B H 0.1919 -0.4660 0.2332 0.093 Uiso 1 1 calc R . . H34C H 0.1767 -0.5914 0.2672 0.093 Uiso 1 1 calc R . . C35 C 0.2598(4) -0.4153(9) 0.3277(3) 0.073(3) Uani 1 1 d . . . H35A H 0.2985 -0.4101 0.3532 0.110 Uiso 1 1 calc R . . H35B H 0.2282 -0.4368 0.3449 0.110 Uiso 1 1 calc R . . H35C H 0.2512 -0.3256 0.3098 0.110 Uiso 1 1 calc R . . C22A C -0.1370(7) -0.6874(17) 0.5381(6) 0.034(2) Uani 0.45 1 d PU A 2 H22A H -0.1224 -0.6030 0.5274 0.041 Uiso 0.45 1 calc PR A 2 C23A C -0.1574(8) -0.6907(18) 0.5813(7) 0.035(3) Uani 0.45 1 d PU A 2 H23A H -0.1590 -0.6055 0.5990 0.042 Uiso 0.45 1 calc PR A 2 C25A C -0.1723(9) -0.942(2) 0.5732(8) 0.029(5) Uani 0.45 1 d P A 2 H25A H -0.1826 -1.0299 0.5848 0.035 Uiso 0.45 1 calc PR A 2 C26A C -0.1520(9) -0.931(2) 0.5272(8) 0.028(6) Uani 0.45 1 d P A 2 H26A H -0.1485 -1.0137 0.5086 0.034 Uiso 0.45 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0232(8) 0.0113(8) 0.0372(9) 0.000 0.0085(6) 0.000 Zn2 0.0229(8) 0.0139(9) 0.0390(9) 0.000 0.0030(7) 0.000 O1 0.020(3) 0.021(4) 0.029(3) -0.003(2) 0.002(2) -0.003(2) O2 0.023(3) 0.020(3) 0.040(3) -0.005(3) 0.004(2) -0.003(2) O3 0.023(3) 0.025(4) 0.035(3) 0.011(3) 0.011(2) -0.003(2) O4 0.027(3) 0.015(3) 0.041(3) 0.009(2) 0.005(2) -0.002(2) O5 0.084(4) 0.072(5) 0.096(5) -0.012(4) 0.051(4) -0.002(4) N1 0.022(5) 0.007(5) 0.031(5) 0.000 0.004(4) 0.000 N2 0.020(5) 0.014(5) 0.041(6) 0.000 0.006(5) 0.000 N3 0.049(5) 0.053(5) 0.048(5) 0.007(4) 0.016(4) 0.008(4) C1 0.029(5) 0.016(5) 0.033(5) -0.002(5) 0.012(4) 0.001(5) C2 0.016(5) 0.020(4) 0.036(5) 0.001(5) 0.011(4) 0.003(4) C3 0.025(5) 0.030(6) 0.041(5) -0.013(4) 0.002(4) -0.003(4) C4 0.032(5) 0.021(5) 0.038(5) -0.007(4) 0.007(5) -0.011(4) C5 0.027(5) 0.018(4) 0.037(5) 0.002(5) 0.007(4) 0.005(4) C6 0.027(5) 0.023(5) 0.044(5) -0.005(4) 0.011(4) 0.003(4) C7 0.030(5) 0.022(5) 0.039(5) 0.000(4) 0.006(5) -0.006(4) C8 0.018(5) 0.025(4) 0.044(6) 0.008(4) 0.009(5) -0.002(4) C9 0.029(6) 0.042(5) 0.037(6) 0.006(5) 0.008(5) 0.006(4) C10 0.039(6) 0.058(6) 0.044(5) 0.001(5) -0.004(6) 0.005(5) C11 0.034(6) 0.035(6) 0.066(7) 0.002(5) -0.010(5) -0.004(4) C12 0.027(6) 0.033(6) 0.063(7) 0.006(5) 0.013(5) 0.003(4) C13 0.032(5) 0.016(5) 0.051(5) 0.001(4) 0.003(5) -0.003(4) C14 0.017(4) 0.024(6) 0.036(6) 0.017(5) -0.013(4) -0.006(5) C15 0.028(4) 0.025(5) 0.021(5) 0.005(5) 0.004(4) -0.005(4) C16 0.033(5) 0.018(6) 0.033(6) 0.010(4) 0.002(4) -0.004(4) C17 0.027(4) 0.014(6) 0.040(6) 0.003(4) 0.002(4) 0.004(4) C18 0.034(5) 0.030(6) 0.034(5) 0.005(5) 0.003(4) -0.006(5) C19 0.061(6) 0.011(6) 0.045(6) 0.007(4) 0.003(5) 0.005(5) C20 0.043(5) 0.028(6) 0.025(5) 0.002(5) 0.006(4) 0.001(4) C21 0.038(4) 0.024(5) 0.037(6) 0.006(4) 0.008(4) -0.007(4) C22 0.064(11) 0.033(10) 0.047(11) 0.024(8) 0.029(9) 0.012(9) C23 0.054(11) 0.070(14) 0.053(12) 0.002(11) 0.024(11) 0.013(10) C24 0.047(6) 0.055(8) 0.044(6) 0.013(6) 0.012(5) 0.005(5) C25 0.055(13) 0.040(13) 0.040(14) 0.028(9) 0.013(12) -0.004(11) C26 0.047(13) 0.035(12) 0.032(12) 0.019(9) 0.007(11) 0.010(9) C27 0.031(8) 0.021(8) 0.036(8) -0.006(7) -0.017(7) 0.009(7) C28 0.015(7) 0.010(7) 0.028(7) 0.008(7) -0.005(6) 0.002(6) C29 0.048(8) 0.032(8) 0.042(8) -0.004(7) 0.022(7) -0.003(7) C30 0.028(7) 0.023(7) 0.027(7) 0.004(7) 0.010(6) -0.008(7) C31 0.023(7) 0.024(8) 0.057(9) 0.001(7) 0.023(7) -0.004(7) C32 0.023(7) 0.008(7) 0.034(8) 0.000(7) 0.010(7) 0.006(7) C33 0.044(6) 0.083(9) 0.067(8) 0.023(6) 0.015(5) 0.002(6) C34 0.049(6) 0.079(7) 0.051(6) 0.009(5) -0.002(5) -0.008(5) C35 0.082(7) 0.072(8) 0.071(7) -0.008(6) 0.026(6) 0.004(5) C22A 0.039(5) 0.024(6) 0.038(6) 0.006(5) 0.008(5) -0.006(5) C23A 0.041(5) 0.024(6) 0.038(6) 0.004(5) 0.007(5) -0.005(5) C25A 0.030(13) 0.031(14) 0.032(14) 0.002(11) 0.020(12) -0.002(10) C26A 0.012(12) 0.037(16) 0.032(15) -0.016(12) -0.005(11) 0.010(10) _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 2.049(4) . ? Zn1 O1 2.049(4) 2 ? Zn1 O3 2.079(4) 2 ? Zn1 O3 2.079(4) . ? Zn1 N1 2.081(7) . ? Zn2 O4 2.020(5) 2 ? Zn2 O4 2.020(5) . ? Zn2 N2 2.039(7) 1_545 ? Zn2 O2 2.057(4) . ? Zn2 O2 2.057(4) 2 ? O1 C1 1.279(8) . ? O2 C1 1.262(8) . ? O3 C14 1.267(8) . ? O4 C14 1.292(9) . ? O5 C33 1.275(10) . ? N1 C31 1.399(13) 2 ? N1 C31 1.399(13) . ? N1 C29 1.492(15) 2 ? N1 C29 1.492(15) . ? N1 C27 1.513(13) . ? N1 C27 1.513(13) 2 ? N2 C32 1.391(13) 2 ? N2 C32 1.391(13) . ? N2 C28 1.497(12) . ? N2 C28 1.497(12) 2 ? N2 C30 1.575(13) . ? N2 C30 1.575(13) 2 ? N2 Zn2 2.039(7) 1_565 ? N3 C33 1.320(9) . ? N3 C34 1.451(9) . ? N3 C35 1.497(9) . ? C1 C2 1.497(9) . ? C2 C3 1.378(9) . ? C2 C7 1.398(9) . ? C3 C4 1.384(9) . ? C4 C5 1.392(9) . ? C5 C6 1.406(9) . ? C5 C8 1.485(9) . ? C6 C7 1.385(8) . ? C8 C9 1.385(9) . ? C8 C13 1.401(8) . ? C9 C10 1.372(9) . ? C10 C11 1.408(10) . ? C11 C12 1.374(10) . ? C12 C13 1.389(9) . ? C14 C15 1.489(9) . ? C15 C20 1.388(9) . ? C15 C16 1.390(9) . ? C16 C17 1.382(9) . ? C17 C18 1.406(9) . ? C18 C19 1.413(9) . ? C18 C21 1.485(10) . ? C19 C20 1.378(9) . ? C21 C26A 1.33(2) . ? C21 C22A 1.393(17) . ? C21 C26 1.412(17) . ? C21 C22 1.448(14) . ? C22 C23 1.412(17) . ? C23 C24 1.392(16) . ? C24 C25 1.307(17) . ? C24 C23A 1.436(18) . ? C24 C25A 1.44(2) . ? C25 C26 1.416(19) . ? C27 C28 1.529(15) . ? C29 C30 1.521(16) . ? C31 C32 1.508(16) . ? C22A C23A 1.36(2) . ? C25A C26A 1.43(2) . ? 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 161.2(3) . 2 ? O1 Zn1 O3 88.72(17) . 2 ? O1 Zn1 O3 87.64(17) 2 2 ? O1 Zn1 O3 87.64(17) . . ? O1 Zn1 O3 88.72(17) 2 . ? O3 Zn1 O3 157.5(3) 2 . ? O1 Zn1 N1 99.38(13) . . ? O1 Zn1 N1 99.38(13) 2 . ? O3 Zn1 N1 101.24(13) 2 . ? O3 Zn1 N1 101.24(13) . . ? O4 Zn2 O4 161.1(3) 2 . ? O4 Zn2 N2 99.47(14) 2 1_545 ? O4 Zn2 N2 99.47(14) . 1_545 ? O4 Zn2 O2 87.93(17) 2 . ? O4 Zn2 O2 88.20(17) . . ? N2 Zn2 O2 101.85(14) 1_545 . ? O4 Zn2 O2 88.20(17) 2 2 ? O4 Zn2 O2 87.93(17) . 2 ? N2 Zn2 O2 101.85(14) 1_545 2 ? O2 Zn2 O2 156.3(3) . 2 ? C1 O1 Zn1 121.6(4) . . ? C1 O2 Zn2 124.9(4) . . ? C14 O3 Zn1 123.8(4) . . ? C14 O4 Zn2 123.5(4) . . ? C31 N1 C31 136.0(13) 2 . ? C31 N1 C29 110.3(8) 2 2 ? C31 N1 C29 53.4(8) . 2 ? C31 N1 C29 53.4(8) 2 . ? C31 N1 C29 110.3(8) . . ? C29 N1 C29 141.3(13) 2 . ? C31 N1 C27 53.7(8) 2 . ? C31 N1 C27 108.6(8) . . ? C29 N1 C27 60.0(8) 2 . ? C29 N1 C27 105.0(8) . . ? C31 N1 C27 108.6(8) 2 2 ? C31 N1 C27 53.7(8) . 2 ? C29 N1 C27 105.0(8) 2 2 ? C29 N1 C27 60.0(8) . 2 ? C27 N1 C27 137.2(12) . 2 ? C31 N1 Zn1 112.0(7) 2 . ? C31 N1 Zn1 112.0(7) . . ? C29 N1 Zn1 109.3(7) 2 . ? C29 N1 Zn1 109.3(7) . . ? C27 N1 Zn1 111.4(6) . . ? C27 N1 Zn1 111.4(6) 2 . ? C32 N2 C32 134.3(13) 2 . ? C32 N2 C28 50.4(7) 2 . ? C32 N2 C28 112.4(8) . . ? C32 N2 C28 112.4(8) 2 2 ? C32 N2 C28 50.4(7) . 2 ? C28 N2 C28 141.5(12) . 2 ? C32 N2 C30 54.1(7) 2 . ? C32 N2 C30 108.1(8) . . ? C28 N2 C30 103.0(8) . . ? C28 N2 C30 62.7(7) 2 . ? C32 N2 C30 108.1(8) 2 2 ? C32 N2 C30 54.1(7) . 2 ? C28 N2 C30 62.7(7) . 2 ? C28 N2 C30 103.0(8) 2 2 ? C30 N2 C30 138.4(12) . 2 ? C32 N2 Zn2 112.9(6) 2 1_565 ? C32 N2 Zn2 112.9(6) . 1_565 ? C28 N2 Zn2 109.3(6) . 1_565 ? C28 N2 Zn2 109.3(6) 2 1_565 ? C30 N2 Zn2 110.8(6) . 1_565 ? C30 N2 Zn2 110.8(6) 2 1_565 ? C33 N3 C34 124.8(7) . . ? C33 N3 C35 119.2(8) . . ? C34 N3 C35 115.9(7) . . ? O2 C1 O1 125.1(6) . . ? O2 C1 C2 118.0(7) . . ? O1 C1 C2 116.9(7) . . ? C3 C2 C7 119.0(6) . . ? C3 C2 C1 122.2(7) . . ? C7 C2 C1 118.8(7) . . ? C2 C3 C4 121.1(6) . . ? C3 C4 C5 121.0(6) . . ? C4 C5 C6 117.6(6) . . ? C4 C5 C8 122.2(7) . . ? C6 C5 C8 120.1(7) . . ? C7 C6 C5 121.3(6) . . ? C6 C7 C2 120.0(6) . . ? C9 C8 C13 118.2(6) . . ? C9 C8 C5 121.6(7) . . ? C13 C8 C5 120.2(7) . . ? C10 C9 C8 122.1(7) . . ? C9 C10 C11 119.1(7) . . ? C12 C11 C10 119.8(7) . . ? C11 C12 C13 120.4(7) . . ? C12 C13 C8 120.4(7) . . ? O3 C14 O4 124.6(7) . . ? O3 C14 C15 117.9(8) . . ? O4 C14 C15 117.5(7) . . ? C20 C15 C16 118.3(6) . . ? C20 C15 C14 119.7(8) . . ? C16 C15 C14 122.0(8) . . ? C17 C16 C15 121.6(6) . . ? C16 C17 C18 120.1(7) . . ? C17 C18 C19 118.0(7) . . ? C17 C18 C21 121.0(8) . . ? C19 C18 C21 120.9(8) . . ? C20 C19 C18 120.5(7) . . ? C19 C20 C15 121.3(7) . . ? C26A C21 C22A 121.2(12) . . ? C26A C21 C26 43.9(7) . . ? C22A C21 C26 97.3(11) . . ? C26A C21 C22 98.8(11) . . ? C22A C21 C22 52.5(8) . . ? C26 C21 C22 114.7(10) . . ? C26A C21 C18 118.8(11) . . ? C22A C21 C18 119.7(10) . . ? C26 C21 C18 122.6(9) . . ? C22 C21 C18 122.5(8) . . ? C23 C22 C21 122.0(12) . . ? C24 C23 C22 117.7(12) . . ? C25 C24 C23 123.0(11) . . ? C25 C24 C23A 97.2(11) . . ? C23 C24 C23A 50.2(8) . . ? C25 C24 C25A 46.5(8) . . ? C23 C24 C25A 100.6(12) . . ? C23A C24 C25A 115.4(11) . . ? C24 C25 C26 120.8(14) . . ? C21 C26 C25 121.5(13) . . ? N1 C27 C28 111.5(10) . . ? N2 C28 C27 109.0(10) . . ? N1 C29 C30 111.8(11) . . ? C29 C30 N2 108.3(10) . . ? N1 C31 C32 111.4(10) . . ? N2 C32 C31 113.4(10) . . ? O5 C33 N3 125.3(9) . . ? C23A C22A C21 119.1(15) . . ? C22A C23A C24 123.4(15) . . ? C26A C25A C24 118.6(15) . . ? C21 C26A C25A 122.0(16) . . ? 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 O1 Zn1 O1 C1 26.1(4) 2 . . . ? O3 Zn1 O1 C1 -52.7(5) 2 . . . ? O3 Zn1 O1 C1 105.1(5) . . . . ? N1 Zn1 O1 C1 -153.9(4) . . . . ? O4 Zn2 O2 C1 106.7(5) 2 . . . ? O4 Zn2 O2 C1 -54.8(5) . . . . ? N2 Zn2 O2 C1 -154.1(5) 1_545 . . . ? O2 Zn2 O2 C1 25.9(5) 2 . . . ? O1 Zn1 O3 C14 -56.5(5) . . . . ? O1 Zn1 O3 C14 105.1(5) 2 . . . ? O3 Zn1 O3 C14 24.4(5) 2 . . . ? N1 Zn1 O3 C14 -155.6(5) . . . . ? O4 Zn2 O4 C14 25.8(4) 2 . . . ? N2 Zn2 O4 C14 -154.2(4) 1_545 . . . ? O2 Zn2 O4 C14 104.1(5) . . . . ? O2 Zn2 O4 C14 -52.5(5) 2 . . . ? O1 Zn1 N1 C31 51.9(8) . . . 2 ? O1 Zn1 N1 C31 -128.1(8) 2 . . 2 ? O3 Zn1 N1 C31 -38.6(8) 2 . . 2 ? O3 Zn1 N1 C31 141.4(8) . . . 2 ? O1 Zn1 N1 C31 -128.1(8) . . . . ? O1 Zn1 N1 C31 51.9(8) 2 . . . ? O3 Zn1 N1 C31 141.4(8) 2 . . . ? O3 Zn1 N1 C31 -38.6(8) . . . . ? O1 Zn1 N1 C29 -70.7(7) . . . 2 ? O1 Zn1 N1 C29 109.3(7) 2 . . 2 ? O3 Zn1 N1 C29 -161.2(7) 2 . . 2 ? O3 Zn1 N1 C29 18.8(7) . . . 2 ? O1 Zn1 N1 C29 109.3(7) . . . . ? O1 Zn1 N1 C29 -70.7(7) 2 . . . ? O3 Zn1 N1 C29 18.8(7) 2 . . . ? O3 Zn1 N1 C29 -161.2(7) . . . . ? O1 Zn1 N1 C27 -6.3(7) . . . . ? O1 Zn1 N1 C27 173.7(7) 2 . . . ? O3 Zn1 N1 C27 -96.8(7) 2 . . . ? O3 Zn1 N1 C27 83.2(7) . . . . ? O1 Zn1 N1 C27 173.7(7) . . . 2 ? O1 Zn1 N1 C27 -6.3(7) 2 . . 2 ? O3 Zn1 N1 C27 83.2(7) 2 . . 2 ? O3 Zn1 N1 C27 -96.8(7) . . . 2 ? Zn2 O2 C1 O1 -15.3(9) . . . . ? Zn2 O2 C1 C2 164.6(4) . . . . ? Zn1 O1 C1 O2 -16.4(9) . . . . ? Zn1 O1 C1 C2 163.7(4) . . . . ? O2 C1 C2 C3 -157.3(6) . . . . ? O1 C1 C2 C3 22.7(9) . . . . ? O2 C1 C2 C7 21.8(9) . . . . ? O1 C1 C2 C7 -158.3(6) . . . . ? C7 C2 C3 C4 -0.4(10) . . . . ? C1 C2 C3 C4 178.6(6) . . . . ? C2 C3 C4 C5 1.5(10) . . . . ? C3 C4 C5 C6 -1.5(10) . . . . ? C3 C4 C5 C8 -178.7(6) . . . . ? C4 C5 C6 C7 0.6(10) . . . . ? C8 C5 C6 C7 177.8(6) . . . . ? C5 C6 C7 C2 0.4(10) . . . . ? C3 C2 C7 C6 -0.5(10) . . . . ? C1 C2 C7 C6 -179.6(6) . . . . ? C4 C5 C8 C9 43.4(10) . . . . ? C6 C5 C8 C9 -133.7(7) . . . . ? C4 C5 C8 C13 -137.9(7) . . . . ? C6 C5 C8 C13 45.1(9) . . . . ? C13 C8 C9 C10 -1.3(11) . . . . ? C5 C8 C9 C10 177.5(7) . . . . ? C8 C9 C10 C11 0.2(12) . . . . ? C9 C10 C11 C12 0.7(11) . . . . ? C10 C11 C12 C13 -0.4(11) . . . . ? C11 C12 C13 C8 -0.7(10) . . . . ? C9 C8 C13 C12 1.5(10) . . . . ? C5 C8 C13 C12 -177.3(6) . . . . ? Zn1 O3 C14 O4 -14.1(9) . . . . ? Zn1 O3 C14 C15 166.8(4) . . . . ? Zn2 O4 C14 O3 -16.5(8) . . . . ? Zn2 O4 C14 C15 162.6(4) . . . . ? O3 C14 C15 C20 -176.3(6) . . . . ? O4 C14 C15 C20 4.5(8) . . . . ? O3 C14 C15 C16 2.8(9) . . . . ? O4 C14 C15 C16 -176.3(6) . . . . ? C20 C15 C16 C17 1.0(10) . . . . ? C14 C15 C16 C17 -178.2(5) . . . . ? C15 C16 C17 C18 0.3(10) . . . . ? C16 C17 C18 C19 -0.8(10) . . . . ? C16 C17 C18 C21 176.0(6) . . . . ? C17 C18 C19 C20 0.0(10) . . . . ? C21 C18 C19 C20 -176.8(6) . . . . ? C18 C19 C20 C15 1.4(10) . . . . ? C16 C15 C20 C19 -1.8(10) . . . . ? C14 C15 C20 C19 177.4(6) . . . . ? C17 C18 C21 C26A 153.1(11) . . . . ? C19 C18 C21 C26A -30.3(14) . . . . ? C17 C18 C21 C22A -32.9(12) . . . . ? C19 C18 C21 C22A 143.7(10) . . . . ? C17 C18 C21 C26 -155.5(12) . . . . ? C19 C18 C21 C26 21.1(15) . . . . ? C17 C18 C21 C22 29.2(12) . . . . ? C19 C18 C21 C22 -154.1(9) . . . . ? C26A C21 C22 C23 48.8(18) . . . . ? C22A C21 C22 C23 -74.0(16) . . . . ? C26 C21 C22 C23 6(2) . . . . ? C18 C21 C22 C23 -178.6(11) . . . . ? C21 C22 C23 C24 -3(2) . . . . ? C22 C23 C24 C25 0(2) . . . . ? C22 C23 C24 C23A 69.9(15) . . . . ? C22 C23 C24 C25A -44.4(18) . . . . ? C23 C24 C25 C26 -1(3) . . . . ? C23A C24 C25 C26 -48(2) . . . . ? C25A C24 C25 C26 70(2) . . . . ? C26A C21 C26 C25 -83(2) . . . . ? C22A C21 C26 C25 45(2) . . . . ? C22 C21 C26 C25 -7(2) . . . . ? C18 C21 C26 C25 177.5(14) . . . . ? C24 C25 C26 C21 5(3) . . . . ? C31 N1 C27 C28 74.8(14) 2 . . . ? C31 N1 C27 C28 -59.2(13) . . . . ? C29 N1 C27 C28 -82.3(13) 2 . . . ? C29 N1 C27 C28 58.8(14) . . . . ? C27 N1 C27 C28 -2.9(9) 2 . . . ? Zn1 N1 C27 C28 177.1(9) . . . . ? C32 N2 C28 C27 -78.7(13) 2 . . . ? C32 N2 C28 C27 51.0(13) . . . . ? C28 N2 C28 C27 -2.9(9) 2 . . . ? C30 N2 C28 C27 -65.1(12) . . . . ? C30 N2 C28 C27 73.1(11) 2 . . . ? Zn2 N2 C28 C27 177.1(9) 1_565 . . . ? N1 C27 C28 N2 5.0(16) . . . . ? C31 N1 C29 C30 -76.6(13) 2 . . . ? C31 N1 C29 C30 56.2(13) . . . . ? C29 N1 C29 C30 -0.1(9) 2 . . . ? C27 N1 C29 C30 -60.5(13) . . . . ? C27 N1 C29 C30 75.8(12) 2 . . . ? Zn1 N1 C29 C30 179.9(9) . . . . ? N1 C29 C30 N2 0.2(15) . . . . ? C32 N2 C30 C29 76.1(13) 2 . . . ? C32 N2 C30 C29 -56.0(12) . . . . ? C28 N2 C30 C29 63.2(12) . . . . ? C28 N2 C30 C29 -78.5(12) 2 . . . ? C30 N2 C30 C29 -0.1(9) 2 . . . ? Zn2 N2 C30 C29 179.9(9) 1_565 . . . ? C31 N1 C31 C32 1.0(11) 2 . . . ? C29 N1 C31 C32 82.7(15) 2 . . . ? C29 N1 C31 C32 -56.9(15) . . . . ? C27 N1 C31 C32 57.6(15) . . . . ? C27 N1 C31 C32 -78.0(14) 2 . . . ? Zn1 N1 C31 C32 -179.0(11) . . . . ? C32 N2 C32 C31 1.0(11) 2 . . . ? C28 N2 C32 C31 -54.8(15) . . . . ? C28 N2 C32 C31 84.4(15) 2 . . . ? C30 N2 C32 C31 58.2(15) . . . . ? C30 N2 C32 C31 -79.2(14) 2 . . . ? Zn2 N2 C32 C31 -179.0(11) 1_565 . . . ? N1 C31 C32 N2 -2(2) . . . . ? C34 N3 C33 O5 3.2(13) . . . . ? C35 N3 C33 O5 179.8(8) . . . . ? C26A C21 C22A C23A -7(2) . . . . ? C26 C21 C22A C23A -46.9(17) . . . . ? C22 C21 C22A C23A 68.7(15) . . . . ? C18 C21 C22A C23A 178.7(12) . . . . ? C21 C22A C23A C24 4(2) . . . . ? C25 C24 C23A C22A 46(2) . . . . ? C23 C24 C23A C22A -81.6(18) . . . . ? C25A C24 C23A C22A 1(2) . . . . ? C25 C24 C25A C26A -78(2) . . . . ? C23 C24 C25A C26A 48(2) . . . . ? C23A C24 C25A C26A -3(3) . . . . ? C22A C21 C26A C25A 6(3) . . . . ? C26 C21 C26A C25A 71(2) . . . . ? C22 C21 C26A C25A -45(2) . . . . ? C18 C21 C26A C25A 179.7(15) . . . . ? C24 C25A C26A C21 -1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 20.65 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.296 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.055 #===end data_compound4_p09adb12 _database_code_depnum_ccdc_archive 'CCDC 859605' #TrackingRef '- warren-pw.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H10 Cu I2 N O4' _chemical_formula_sum 'C16 H10 Cu I2 N O4' _chemical_formula_weight 597.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 18.7750(10) _cell_length_b 18.7750(10) _cell_length_c 19.672(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6934.4(10) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3818 _cell_measurement_theta_min 2.9896 _cell_measurement_theta_max 32.8442 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4480 _exptl_absorpt_coefficient_mu 4.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.27158 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; 'Xcalibur, Atlas, Gemini ultra' ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3795 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12737 _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 32.94 _reflns_number_total 5843 _reflns_number_gt 3504 _reflns_threshold_expression >2sigma(I) _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -95.00 -17.00 1.0000 250.0000 omega____ theta____ kappa____ phi______ frames - -19.4617 -37.0000 150.0000 78 #__ type_ start__ end____ width___ exp.time_ 2 omega 63.00 107.00 1.0000 250.0000 omega____ theta____ kappa____ phi______ frames - 20.5554 179.0000 0.0000 44 ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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^)+(0.0970P)^2^+32.3195P] 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 5843 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1125 _refine_ls_R_factor_gt 0.0668 _refine_ls_wR_factor_ref 0.1890 _refine_ls_wR_factor_gt 0.1750 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 I1 I -0.31810(4) -0.18650(3) -0.62729(3) 0.0539(2) Uani 1 1 d . . . I2 I -0.09706(3) 0.49378(3) -0.13570(3) 0.03998(18) Uani 1 1 d . . . Cu1 Cu -0.5000 0.2500 -0.55741(4) 0.01131(19) Uani 1 2 d S . . Cu2 Cu -0.5000 0.2500 -0.19186(5) 0.0194(2) Uani 1 2 d S . . O1 O -0.4615(3) 0.1534(2) -0.5635(2) 0.0235(10) Uani 1 1 d . . . O2 O -0.4612(3) 0.1533(2) -0.6780(2) 0.0230(10) Uani 1 1 d . . . O3 O -0.4105(3) 0.3008(4) -0.1798(2) 0.0527(19) Uani 1 1 d . A . O4 O -0.4102(3) 0.3017(4) -0.0669(2) 0.0514(18) Uani 1 1 d . A . N1 N -0.5000 0.2500 -0.4454(3) 0.0214(15) Uani 1 2 d S . . N2 N -0.5000 0.2500 -0.3043(3) 0.0224(15) Uani 1 2 d S . . C1 C -0.4512(3) 0.1251(3) -0.6210(3) 0.0160(11) Uani 1 1 d . . . C2 C -0.4219(4) 0.0513(3) -0.6215(3) 0.0219(12) Uani 1 1 d . . . C3 C -0.4053(5) 0.0161(4) -0.5617(4) 0.039(2) Uani 1 1 d . . . H3 H -0.4128 0.0395 -0.5195 0.047 Uiso 1 1 calc R . . C4 C -0.3775(6) -0.0533(4) -0.5621(4) 0.050(3) Uani 1 1 d . . . H4 H -0.3678 -0.0778 -0.5208 0.059 Uiso 1 1 calc R . . C5 C -0.3650(5) -0.0848(4) -0.6240(4) 0.0380(18) Uani 1 1 d . . . C6 C -0.3832(5) -0.0534(4) -0.6840(4) 0.0358(18) Uani 1 1 d . . . H6 H -0.3768 -0.0779 -0.7258 0.043 Uiso 1 1 calc R . . C7 C -0.4112(4) 0.0151(4) -0.6829(4) 0.0308(15) Uani 1 1 d . . . H7 H -0.4233 0.0378 -0.7245 0.037 Uiso 1 1 calc R . . C8 C -0.4853(4) 0.1915(3) -0.4095(3) 0.0281(16) Uani 1 1 d . . . H8 H -0.4751 0.1485 -0.4329 0.034 Uiso 1 1 calc R . . C9 C -0.4846(4) 0.1917(3) -0.3386(3) 0.0253(14) Uani 1 1 d . . . H9 H -0.4728 0.1493 -0.3148 0.030 Uiso 1 1 calc R . . C10 C -0.3840(4) 0.3167(4) -0.1231(3) 0.0230(12) Uani 1 1 d . . . C11 C -0.3155(3) 0.3565(4) -0.1279(4) 0.0345(9) Uani 0.65 1 d PG A 1 C12 C -0.2656(4) 0.3418(4) -0.1782(3) 0.0345(9) Uani 0.65 1 d PG A 1 H12 H -0.2744 0.3049 -0.2102 0.041 Uiso 0.65 1 calc PR A 1 C13 C -0.2029(4) 0.3809(4) -0.1817(3) 0.0345(9) Uani 0.65 1 d PG A 1 H13 H -0.1688 0.3709 -0.2160 0.041 Uiso 0.65 1 calc PR A 1 C14 C -0.1900(3) 0.4349(4) -0.1348(4) 0.0345(9) Uani 0.65 1 d PG A 1 C15 C -0.2399(4) 0.4496(4) -0.0845(3) 0.0345(9) Uani 0.65 1 d PG A 1 H15 H -0.2311 0.4864 -0.0525 0.041 Uiso 0.65 1 calc PR A 1 C16 C -0.3026(4) 0.4104(4) -0.0811(3) 0.0345(9) Uani 0.65 1 d PG A 1 H16 H -0.3367 0.4205 -0.0467 0.041 Uiso 0.65 1 calc PR A 1 C11A C -0.3195(6) 0.3634(7) -0.1159(7) 0.0345(9) Uani 0.35 1 d PG A 2 C12A C -0.3122(6) 0.4226(8) -0.1578(7) 0.0345(9) Uani 0.35 1 d PG A 2 H12A H -0.3508 0.4373 -0.1858 0.041 Uiso 0.35 1 calc PR A 2 C13A C -0.2484(7) 0.4602(6) -0.1589(7) 0.0345(9) Uani 0.35 1 d PG A 2 H13A H -0.2434 0.5006 -0.1876 0.041 Uiso 0.35 1 calc PR A 2 C14A C -0.1920(6) 0.4387(7) -0.1181(7) 0.0345(9) Uani 0.35 1 d PG A 2 C15A C -0.1993(6) 0.3796(8) -0.0761(7) 0.0345(9) Uani 0.35 1 d PG A 2 H15A H -0.1607 0.3649 -0.0482 0.041 Uiso 0.35 1 calc PR A 2 C16A C -0.2630(7) 0.3419(6) -0.0750(7) 0.0345(9) Uani 0.35 1 d PG A 2 H16A H -0.2680 0.3015 -0.0464 0.041 Uiso 0.35 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0915(6) 0.0313(3) 0.0391(3) -0.0077(2) -0.0065(3) 0.0354(3) I2 0.0316(3) 0.0219(2) 0.0664(4) 0.0017(2) 0.0089(2) -0.0036(2) Cu1 0.0142(5) 0.0112(4) 0.0085(4) 0.000 0.000 0.0011(4) Cu2 0.0227(6) 0.0258(6) 0.0097(4) 0.000 0.000 0.0025(5) O1 0.034(3) 0.018(2) 0.018(2) 0.0009(16) 0.0004(18) 0.006(2) O2 0.030(3) 0.020(2) 0.019(2) -0.0053(17) -0.0057(18) 0.0053(19) O3 0.045(3) 0.093(5) 0.020(2) 0.023(3) -0.014(2) -0.038(4) O4 0.047(4) 0.087(5) 0.021(2) -0.019(3) 0.011(2) -0.038(3) N1 0.036(5) 0.017(4) 0.012(3) 0.000 0.000 0.009(3) N2 0.031(4) 0.026(4) 0.010(3) 0.000 0.000 0.011(4) C1 0.010(2) 0.012(2) 0.026(3) -0.003(2) 0.000(2) -0.005(2) C2 0.021(3) 0.016(3) 0.029(3) -0.002(2) -0.004(2) -0.004(2) C3 0.065(6) 0.023(4) 0.030(3) -0.008(3) -0.016(4) 0.023(4) C4 0.091(7) 0.027(4) 0.031(4) -0.005(3) -0.023(4) 0.033(5) C5 0.047(5) 0.022(3) 0.045(4) -0.006(3) -0.006(4) 0.011(3) C6 0.056(5) 0.017(3) 0.034(4) -0.005(3) 0.003(3) 0.009(3) C7 0.039(4) 0.021(3) 0.032(3) 0.005(3) 0.000(3) 0.007(3) C8 0.055(5) 0.017(3) 0.012(3) 0.000(2) 0.000(3) 0.016(3) C9 0.044(4) 0.024(3) 0.009(2) 0.005(2) 0.003(2) 0.014(3) C10 0.027(3) 0.025(3) 0.017(3) 0.006(2) 0.000(2) -0.004(3) C11 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) C12 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) C13 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) C14 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) C15 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) C16 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) C11A 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) C12A 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) C13A 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) C14A 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) C15A 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) C16A 0.0316(19) 0.039(2) 0.033(2) -0.0065(16) 0.0079(16) -0.0066(17) _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 I1 C5 2.104(8) . ? I2 C14 2.067(5) . ? I2 C14A 2.090(9) . ? Cu1 O1 1.956(4) . ? Cu1 O1 1.956(4) 3_455 ? Cu1 O2 1.978(4) 10_554 ? Cu1 O2 1.978(4) 12_564 ? Cu1 N1 2.204(7) . ? Cu1 Cu1 2.6595(17) 10_554 ? Cu2 O3 1.947(5) . ? Cu2 O3 1.947(5) 3_455 ? Cu2 O4 1.952(5) 12_565 ? Cu2 O4 1.952(5) 10 ? Cu2 N2 2.212(7) . ? Cu2 Cu2 2.6305(19) 10 ? O1 C1 1.265(7) . ? O2 C1 1.254(7) . ? O2 Cu1 1.978(4) 10_554 ? O3 C10 1.257(8) . ? O4 C10 1.243(8) . ? O4 Cu2 1.952(5) 10 ? N1 C8 1.335(7) 3_455 ? N1 C8 1.335(7) . ? N2 C9 1.318(7) 3_455 ? N2 C9 1.318(7) . ? C1 C2 1.491(8) . ? C2 C3 1.384(9) . ? C2 C7 1.401(9) . ? C3 C4 1.404(10) . ? C3 H3 0.9500 . ? C4 C5 1.374(10) . ? C4 H4 0.9500 . ? C5 C6 1.362(11) . ? C6 C7 1.391(9) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.394(8) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.491(8) . ? C10 C11A 1.502(12) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C12 H12 0.9500 . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C11A C12A 1.3900 . ? C11A C16A 1.3900 . ? C12A C13A 1.3900 . ? C12A H12A 0.9500 . ? C13A C14A 1.3900 . ? C13A H13A 0.9500 . ? C14A C15A 1.3900 . ? C15A C16A 1.3900 . ? C15A H15A 0.9500 . ? C16A H16A 0.9500 . ? 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 C14 I2 C14A 9.3(4) . . ? O1 Cu1 O1 173.0(2) . 3_455 ? O1 Cu1 O2 89.36(19) . 10_554 ? O1 Cu1 O2 89.6(2) 3_455 10_554 ? O1 Cu1 O2 89.6(2) . 12_564 ? O1 Cu1 O2 89.36(19) 3_455 12_564 ? O2 Cu1 O2 163.3(2) 10_554 12_564 ? O1 Cu1 N1 93.52(12) . . ? O1 Cu1 N1 93.52(12) 3_455 . ? O2 Cu1 N1 98.33(12) 10_554 . ? O2 Cu1 N1 98.33(12) 12_564 . ? O1 Cu1 Cu1 86.48(12) . 10_554 ? O1 Cu1 Cu1 86.48(12) 3_455 10_554 ? O2 Cu1 Cu1 81.67(12) 10_554 10_554 ? O2 Cu1 Cu1 81.67(12) 12_564 10_554 ? N1 Cu1 Cu1 180.0 . 10_554 ? O3 Cu2 O3 166.0(3) . 3_455 ? O3 Cu2 O4 89.8(3) . 12_565 ? O3 Cu2 O4 89.0(3) 3_455 12_565 ? O3 Cu2 O4 89.0(3) . 10 ? O3 Cu2 O4 89.8(3) 3_455 10 ? O4 Cu2 O4 169.9(3) 12_565 10 ? O3 Cu2 N2 97.00(15) . . ? O3 Cu2 N2 96.99(15) 3_455 . ? O4 Cu2 N2 95.07(14) 12_565 . ? O4 Cu2 N2 95.07(14) 10 . ? O3 Cu2 Cu2 83.00(15) . 10 ? O3 Cu2 Cu2 83.01(15) 3_455 10 ? O4 Cu2 Cu2 84.93(14) 12_565 10 ? O4 Cu2 Cu2 84.93(14) 10 10 ? N2 Cu2 Cu2 180.0 . 10 ? C1 O1 Cu1 120.1(4) . . ? C1 O2 Cu1 124.9(4) . 10_554 ? C10 O3 Cu2 124.5(5) . . ? C10 O4 Cu2 122.3(5) . 10 ? C8 N1 C8 116.0(7) 3_455 . ? C8 N1 Cu1 122.0(4) 3_455 . ? C8 N1 Cu1 122.0(4) . . ? C9 N2 C9 118.4(7) 3_455 . ? C9 N2 Cu2 120.8(4) 3_455 . ? C9 N2 Cu2 120.8(4) . . ? O2 C1 O1 126.9(6) . . ? O2 C1 C2 116.2(5) . . ? O1 C1 C2 116.9(5) . . ? C3 C2 C7 117.9(6) . . ? C3 C2 C1 121.5(6) . . ? C7 C2 C1 120.6(6) . . ? C2 C3 C4 121.5(7) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 117.8(7) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C6 C5 C4 122.7(7) . . ? C6 C5 I1 118.0(5) . . ? C4 C5 I1 119.3(6) . . ? C5 C6 C7 118.8(7) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C6 C7 C2 121.1(7) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? N1 C8 C9 122.0(6) . . ? N1 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? N2 C9 C8 120.8(6) . . ? N2 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? O4 C10 O3 125.3(7) . . ? O4 C10 C11 120.8(6) . . ? O3 C10 C11 113.9(6) . . ? O4 C10 C11A 111.6(7) . . ? O3 C10 C11A 122.8(7) . . ? C11 C10 C11A 10.8(6) . . ? C12 C11 C16 120.0 . . ? C12 C11 C10 121.8(5) . . ? C16 C11 C10 118.2(5) . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 I2 122.1(4) . . ? C15 C14 I2 117.9(4) . . ? C14 C15 C16 120.0 . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 120.0 . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C12A C11A C16A 120.0 . . ? C12A C11A C10 119.3(9) . . ? C16A C11A C10 120.0(9) . . ? C11A C12A C13A 120.0 . . ? C11A C12A H12A 120.0 . . ? C13A C12A H12A 120.0 . . ? C14A C13A C12A 120.0 . . ? C14A C13A H13A 120.0 . . ? C12A C13A H13A 120.0 . . ? C13A C14A C15A 120.0 . . ? C13A C14A I2 114.2(7) . . ? C15A C14A I2 125.3(7) . . ? C16A C15A C14A 120.0 . . ? C16A C15A H15A 120.0 . . ? C14A C15A H15A 120.0 . . ? C15A C16A C11A 120.0 . . ? C15A C16A H16A 120.0 . . ? C11A C16A H16A 120.0 . . ? 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 O1 Cu1 O1 C1 -0.8(4) 3_455 . . . ? O2 Cu1 O1 C1 80.9(5) 10_554 . . . ? O2 Cu1 O1 C1 -82.5(5) 12_564 . . . ? N1 Cu1 O1 C1 179.2(4) . . . . ? Cu1 Cu1 O1 C1 -0.8(4) 10_554 . . . ? O3 Cu2 O3 C10 -0.8(7) 3_455 . . . ? O4 Cu2 O3 C10 84.1(7) 12_565 . . . ? O4 Cu2 O3 C10 -85.8(7) 10 . . . ? N2 Cu2 O3 C10 179.2(7) . . . . ? Cu2 Cu2 O3 C10 -0.8(7) 10 . . . ? O1 Cu1 N1 C8 172.4(4) . . . 3_455 ? O1 Cu1 N1 C8 -7.6(4) 3_455 . . 3_455 ? O2 Cu1 N1 C8 -97.8(4) 10_554 . . 3_455 ? O2 Cu1 N1 C8 82.2(4) 12_564 . . 3_455 ? Cu1 Cu1 N1 C8 -121(100) 10_554 . . 3_455 ? O1 Cu1 N1 C8 -7.6(4) . . . . ? O1 Cu1 N1 C8 172.4(4) 3_455 . . . ? O2 Cu1 N1 C8 82.2(4) 10_554 . . . ? O2 Cu1 N1 C8 -97.8(4) 12_564 . . . ? Cu1 Cu1 N1 C8 59(100) 10_554 . . . ? O3 Cu2 N2 C9 -75.3(4) . . . 3_455 ? O3 Cu2 N2 C9 104.7(4) 3_455 . . 3_455 ? O4 Cu2 N2 C9 15.1(4) 12_565 . . 3_455 ? O4 Cu2 N2 C9 -164.9(4) 10 . . 3_455 ? Cu2 Cu2 N2 C9 -60(100) 10 . . 3_455 ? O3 Cu2 N2 C9 104.7(4) . . . . ? O3 Cu2 N2 C9 -75.3(4) 3_455 . . . ? O4 Cu2 N2 C9 -164.9(4) 12_565 . . . ? O4 Cu2 N2 C9 15.1(4) 10 . . . ? Cu2 Cu2 N2 C9 120(100) 10 . . . ? Cu1 O2 C1 O1 -2.4(9) 10_554 . . . ? Cu1 O2 C1 C2 179.6(4) 10_554 . . . ? Cu1 O1 C1 O2 2.1(9) . . . . ? Cu1 O1 C1 C2 -179.9(4) . . . . ? O2 C1 C2 C3 176.7(7) . . . . ? O1 C1 C2 C3 -1.5(9) . . . . ? O2 C1 C2 C7 -4.0(9) . . . . ? O1 C1 C2 C7 177.7(6) . . . . ? C7 C2 C3 C4 0.9(13) . . . . ? C1 C2 C3 C4 -179.8(8) . . . . ? C2 C3 C4 C5 2.2(15) . . . . ? C3 C4 C5 C6 -5.0(16) . . . . ? C3 C4 C5 I1 176.6(7) . . . . ? C4 C5 C6 C7 4.4(15) . . . . ? I1 C5 C6 C7 -177.1(6) . . . . ? C5 C6 C7 C2 -1.1(13) . . . . ? C3 C2 C7 C6 -1.5(12) . . . . ? C1 C2 C7 C6 179.3(7) . . . . ? C8 N1 C8 C9 -0.7(5) 3_455 . . . ? Cu1 N1 C8 C9 179.3(5) . . . . ? C9 N2 C9 C8 -0.7(5) 3_455 . . . ? Cu2 N2 C9 C8 179.3(5) . . . . ? N1 C8 C9 N2 1.5(11) . . . . ? Cu2 O4 C10 O3 -0.5(12) 10 . . . ? Cu2 O4 C10 C11 179.8(6) 10 . . . ? Cu2 O4 C10 C11A 173.6(7) 10 . . . ? Cu2 O3 C10 O4 1.1(13) . . . . ? Cu2 O3 C10 C11 -179.2(6) . . . . ? Cu2 O3 C10 C11A -172.4(8) . . . . ? O4 C10 C11 C12 143.3(7) . . . . ? O3 C10 C11 C12 -36.4(9) . . . . ? C11A C10 C11 C12 176(4) . . . . ? O4 C10 C11 C16 -37.8(10) . . . . ? O3 C10 C11 C16 142.4(6) . . . . ? C11A C10 C11 C16 -5(4) . . . . ? C16 C11 C12 C13 0.0 . . . . ? C10 C11 C12 C13 178.8(8) . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C15 0.0 . . . . ? C12 C13 C14 I2 178.7(6) . . . . ? C14A I2 C14 C13 -156(3) . . . . ? C14A I2 C14 C15 23(3) . . . . ? C13 C14 C15 C16 0.0 . . . . ? I2 C14 C15 C16 -178.7(6) . . . . ? C14 C15 C16 C11 0.0 . . . . ? C12 C11 C16 C15 0.0 . . . . ? C10 C11 C16 C15 -178.9(8) . . . . ? O4 C10 C11A C12A -134.5(8) . . . . ? O3 C10 C11A C12A 39.8(13) . . . . ? C11 C10 C11A C12A 75(4) . . . . ? O4 C10 C11A C16A 55.0(11) . . . . ? O3 C10 C11A C16A -130.7(9) . . . . ? C11 C10 C11A C16A -95(4) . . . . ? C16A C11A C12A C13A 0.0 . . . . ? C10 C11A C12A C13A -170.5(12) . . . . ? C11A C12A C13A C14A 0.0 . . . . ? C12A C13A C14A C15A 0.0 . . . . ? C12A C13A C14A I2 172.7(9) . . . . ? C14 I2 C14A C13A -58(3) . . . . ? C14 I2 C14A C15A 114(3) . . . . ? C13A C14A C15A C16A 0.0 . . . . ? I2 C14A C15A C16A -171.8(10) . . . . ? C14A C15A C16A C11A 0.0 . . . . ? C12A C11A C16A C15A 0.0 . . . . ? C10 C11A C16A C15A 170.4(12) . . . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 4.985 _refine_diff_density_min -3.155 _refine_diff_density_rms 0.226 #===end data_compound5_k09adb06 _database_code_depnum_ccdc_archive 'CCDC 859606' #TrackingRef '- warren-pw.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H38 Cu2 I4 N3 O10' _chemical_formula_weight 1427.47 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' O O 0.0106 0.0060 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P41 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z+1/4' '-x, -y, z+1/2' 'y, -x, z+3/4' _cell_length_a 12.7970(5) _cell_length_b 12.7970(5) _cell_length_c 39.0980(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6402.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30076 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _exptl_crystal_description tabloid _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2740 _exptl_absorpt_coefficient_mu 2.637 # Absorption correction _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.579 _exptl_absorpt_correction_T_max 0.783 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6739 _diffrn_reflns_av_R_equivalents 0.1262 _diffrn_reflns_av_sigmaI/netI 0.0820 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 23.97 _reflns_number_total 3262 _reflns_number_gt 2490 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _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^ > 2\s(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. Obtaining a structural model in this instance is a testimony to detector technology in modern diffractometers. Crystal that were small in one dimension were not assisted in the diffraction process by disorder and diffuse solvent in the lattice. In particular, the amino group on the pyrazine appears to be disordered over 3 sites (50:25:25 ratios approximately). Additionally, the diffuse solvent in the lattice proved tricky. However, there was ample evidence for one coherent benzyl alcohol moiety before application of the SQUEEZE algorithm. Based on the PLATON output, 2 molecules of this solvent were include as being present in the asymmetric unit, which is a reasonable approximation based on the pre-SQUEEZE difference electron density map. The fundamental issue with this data collection is the rapid intensity drop-off above 14 degrees on Bragg. While data were collected up to a theta of 25 degrees, the completeness shows that they were both poor and virtually non-existent in terms of intensity. Thus, all aromatic rings were treated as rigid hexagons, and anisotropic refinements were restricted to very few atoms indeed. However, on balance, the gross structure is unambiguous. ; _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^)+(0.1909P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.45(9) _refine_ls_number_reflns 3262 _refine_ls_number_parameters 198 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.1056 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2617 _refine_ls_wR_factor_gt 0.2418 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.070 _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 I1 I 0.7461(2) 1.1689(2) 0.14847(10) 0.1336(17) Uani 1 1 d . . . I2 I 1.18287(18) 0.2919(2) 0.17072(8) 0.1048(12) Uani 1 1 d . . . I3 I 0.3037(2) -0.1451(2) 0.15612(9) 0.1254(14) Uani 1 1 d . . . I4 I -0.13355(18) 0.7314(2) 0.15852(8) 0.1035(11) Uani 1 1 d . . . Cu1 Cu 0.5279(3) 0.5086(3) 0.12554(7) 0.0396(12) Uani 1 1 d . . . Cu2 Cu 0.5237(3) 0.5146(3) 0.19300(7) 0.0383(11) Uani 1 1 d . . . O1 O 0.5645(14) 0.6631(14) 0.1290(5) 0.061(6) Uani 1 1 d U . . O2 O 0.5629(14) 0.6609(14) 0.1865(5) 0.059(6) Uani 1 1 d U . . O3 O 0.6749(10) 0.4714(10) 0.1319(3) 0.024(4) Uani 1 1 d U . . O4 O 0.6646(12) 0.4772(13) 0.1901(4) 0.047(5) Uani 1 1 d U . . O5 O 0.4977(11) 0.3589(11) 0.1323(4) 0.033(4) Uani 1 1 d U . . O6 O 0.4846(16) 0.3700(17) 0.1882(6) 0.086(7) Uani 1 1 d U . . O7 O 0.3794(12) 0.5536(12) 0.1857(4) 0.048(5) Uani 1 1 d U . . O8 O 0.3723(11) 0.5403(11) 0.1301(3) 0.029(4) Uani 1 1 d U . . N3A N 0.428(5) 0.654(4) 0.0638(17) 0.050 Uiso 0.25 1 d PD A 1 H31A H 0.4369 0.6672 0.0856 0.060 Uiso 0.25 1 calc PR A 1 H32A H 0.3895 0.6956 0.0511 0.060 Uiso 0.25 1 calc PR A 1 N1 N 0.5324(10) 0.5034(11) 0.0687(3) 0.028(5) Uiso 1 1 d G A . C29 C 0.4708(10) 0.5731(10) 0.0504(4) 0.068(9) Uiso 1 1 d GD . . C30 C 0.4636(10) 0.5645(10) 0.0150(4) 0.037(6) Uiso 1 1 d GD A . N2 N 0.5180(11) 0.4862(12) -0.0020(3) 0.068(8) Uiso 1 1 d G . . C31 C 0.5797(10) 0.4165(10) 0.0164(4) 0.026(6) Uiso 1 1 d GD A . C32 C 0.5869(9) 0.4251(10) 0.0517(4) 0.061(9) Uiso 1 1 d G . . H32 H 0.6290 0.3775 0.0643 0.074 Uiso 1 1 calc R A . C1 C 0.568(2) 0.707(2) 0.1556(7) 0.057(8) Uiso 1 1 d . . . C2 C 0.6152(8) 0.8159(10) 0.1557(3) 0.046(7) Uiso 1 1 d G . . C3 C 0.6252(13) 0.8628(11) 0.1238(3) 0.073(10) Uiso 1 1 d G . . H3 H 0.6106 0.8239 0.1037 0.087 Uiso 1 1 calc R . . C4 C 0.6565(14) 0.9665(11) 0.1214(4) 0.081(10) Uiso 1 1 d G . . H4 H 0.6633 0.9985 0.0996 0.097 Uiso 1 1 calc R . . C5 C 0.6779(11) 1.0234(9) 0.1508(4) 0.072(10) Uiso 1 1 d G . . C6 C 0.6679(14) 0.9766(10) 0.1828(4) 0.097(11) Uiso 1 1 d G . . H6 H 0.6826 1.0155 0.2029 0.116 Uiso 1 1 calc R . . C7 C 0.6366(13) 0.8728(10) 0.1852(3) 0.064(9) Uiso 1 1 d G . . H7 H 0.6298 0.8408 0.2070 0.077 Uiso 1 1 calc R . . C8 C 0.7121(17) 0.4557(9) 0.1602(6) 0.048(7) Uiso 1 1 d G . . C9 C 0.8286(9) 0.4183(8) 0.1653(3) 0.017(5) Uiso 1 1 d G . . C10 C 0.8842(10) 0.3982(12) 0.1355(3) 0.067(9) Uiso 1 1 d G . . H10 H 0.8505 0.4036 0.1139 0.081 Uiso 1 1 calc R . . C11 C 0.9889(9) 0.3700(14) 0.1373(4) 0.065(9) Uiso 1 1 d G . . H11 H 1.0269 0.3562 0.1169 0.078 Uiso 1 1 calc R . . C12 C 1.0382(9) 0.3620(11) 0.1689(5) 0.108(12) Uiso 1 1 d G . . C13 C 0.9826(10) 0.3822(14) 0.1987(4) 0.080(10) Uiso 1 1 d G . . H13 H 1.0162 0.3767 0.2203 0.096 Uiso 1 1 calc R . . C14 C 0.8778(10) 0.4103(12) 0.1969(3) 0.070(9) Uiso 1 1 d G . . H14 H 0.8399 0.4241 0.2173 0.084 Uiso 1 1 calc R . . C15 C 0.4754(9) 0.3161(18) 0.1571(6) 0.038(6) Uiso 1 1 d G . . C16 C 0.4558(7) 0.2082(7) 0.1617(3) 0.036(6) Uiso 1 1 d G . . C17 C 0.4467(8) 0.1586(7) 0.1302(3) 0.099(12) Uiso 1 1 d G . . H17 H 0.4727 0.1915 0.1101 0.119 Uiso 1 1 calc R . . C18 C 0.3996(9) 0.0609(7) 0.1281(3) 0.061(8) Uiso 1 1 d G . . H18 H 0.3934 0.0271 0.1065 0.073 Uiso 1 1 calc R . . C19 C 0.3616(10) 0.0129(6) 0.1574(4) 0.093(11) Uiso 1 1 d G . . C20 C 0.3707(10) 0.0624(7) 0.1889(3) 0.081(10) Uiso 1 1 d G . . H20 H 0.3447 0.0296 0.2090 0.097 Uiso 1 1 calc R . . C21 C 0.4178(9) 0.1601(7) 0.1911(3) 0.062(8) Uiso 1 1 d G . . H21 H 0.4240 0.1940 0.2126 0.074 Uiso 1 1 calc R . . C22 C 0.3280(7) 0.5726(6) 0.1564(3) 0.037(7) Uiso 1 1 d G . . C23 C 0.2234(7) 0.5957(6) 0.1573(2) 0.052(8) Uiso 1 1 d G . . C24 C 0.1810(8) 0.6341(6) 0.1271(3) 0.037(6) Uiso 1 1 d G . . H24 H 0.2215 0.6342 0.1067 0.044 Uiso 1 1 calc R . . C25 C 0.0792(8) 0.6721(7) 0.1267(3) 0.068(9) Uiso 1 1 d G . . H25 H 0.0502 0.6984 0.1060 0.082 Uiso 1 1 calc R . . C26 C 0.0199(8) 0.6718(7) 0.1565(3) 0.056(8) Uiso 1 1 d G . . C27 C 0.0624(9) 0.6335(7) 0.1867(3) 0.054(8) Uiso 1 1 d G . . H27 H 0.0219 0.6333 0.2070 0.065 Uiso 1 1 calc R . . C28 C 0.1641(8) 0.5954(7) 0.1871(2) 0.048(8) Uiso 1 1 d G . . H28 H 0.1931 0.5692 0.2077 0.057 Uiso 1 1 calc R . . N3B N 0.4064(16) 0.6308(12) -0.0007(3) 0.019(9) Uiso 0.50 1 d PGD A 1 H31B H 0.3734 0.6797 0.0108 0.022 Uiso 0.50 1 calc PR A 1 H32B H 0.4002 0.6276 -0.0231 0.022 Uiso 0.50 1 calc PR A 1 N3C N 0.622(6) 0.348(5) -0.0032(19) 0.07(3) Uiso 0.25 1 d PD A 1 H31C H 0.6100 0.3496 -0.0253 0.086 Uiso 0.25 1 calc PR A 1 H32C H 0.6627 0.2997 0.0056 0.086 Uiso 0.25 1 calc PR A 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 I1 0.079(2) 0.043(2) 0.278(5) 0.002(2) 0.006(2) -0.0142(15) I2 0.0404(18) 0.099(2) 0.175(3) 0.0085(19) 0.0052(16) 0.0260(14) I3 0.081(2) 0.050(2) 0.245(4) 0.012(2) -0.043(2) -0.0123(14) I4 0.0407(17) 0.079(2) 0.190(3) -0.0181(18) -0.0220(18) 0.0207(13) Cu1 0.057(3) 0.023(2) 0.039(2) -0.0024(14) -0.0033(18) -0.0017(18) Cu2 0.037(3) 0.035(3) 0.043(2) -0.0036(16) 0.0012(18) 0.0043(17) O1 0.060(6) 0.060(6) 0.062(6) 0.001(3) 0.000(3) 0.000(3) O2 0.060(6) 0.059(6) 0.058(6) -0.001(3) 0.000(3) -0.001(3) O3 0.022(5) 0.024(5) 0.026(5) -0.003(3) 0.002(3) 0.000(3) O4 0.047(6) 0.047(6) 0.048(5) 0.001(3) -0.001(3) 0.003(3) O5 0.033(5) 0.033(5) 0.034(5) 0.000(3) 0.002(3) -0.003(3) O6 0.086(7) 0.085(7) 0.087(7) 0.001(3) -0.001(3) -0.002(3) O7 0.047(6) 0.048(6) 0.049(6) 0.000(3) 0.002(3) 0.000(3) O8 0.028(5) 0.030(5) 0.030(5) 0.001(3) 0.000(3) 0.001(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 I1 C5 2.058(13) . ? I2 C12 2.059(12) . ? I3 C19 2.153(10) . ? I4 C26 2.109(9) . ? Cu1 O3 1.957(14) . ? Cu1 O5 1.973(15) . ? Cu1 O1 2.036(18) . ? Cu1 O8 2.039(15) . ? Cu1 N1 2.223(12) . ? Cu1 Cu2 2.639(3) . ? Cu2 O4 1.868(16) . ? Cu2 O6 1.93(2) . ? Cu2 O7 1.935(16) . ? Cu2 O2 1.955(18) . ? Cu2 N2 2.155(12) 2_655 ? O1 C1 1.18(3) . ? O2 C1 1.34(3) . ? O3 C8 1.22(3) . ? O4 C8 1.35(3) . ? O5 C15 1.15(2) . ? O6 C15 1.40(3) . ? O7 C22 1.344(18) . ? O8 C22 1.245(17) . ? N3A C29 1.28(2) . ? N3A H31A 0.8800 . ? N3A H32A 0.8800 . ? N1 C29 1.3900 . ? N1 C32 1.3900 . ? C29 C30 1.3900 . ? C30 N3B 1.278(17) . ? C30 N2 1.3900 . ? N2 C31 1.3900 . ? N2 Cu2 2.155(12) 4_564 ? C31 N3C 1.28(2) . ? C31 C32 1.3900 . ? C32 H32 0.9500 . ? C1 C2 1.52(3) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.58(2) . ? C9 C10 1.3900 . ? C9 C14 1.3900 . ? C10 C11 1.3900 . ? C10 H10 0.9500 . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.42(2) . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 C18 1.3900 . ? C17 H17 0.9500 . ? C18 C19 1.3900 . ? C18 H18 0.9500 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.3709 . ? C23 C28 1.3892 . ? C23 C24 1.3910 . ? C24 C25 1.3901 . ? C24 H24 0.9500 . ? C25 C26 1.3904 . ? C25 H25 0.9500 . ? C26 C27 1.3896 . ? C27 C28 1.3900 . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? N3B H31B 0.8800 . ? N3B H32B 0.8800 . ? N3C H31C 0.8800 . ? N3C H32C 0.8800 . ? 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 Cu1 O5 86.3(6) . . ? O3 Cu1 O1 90.3(6) . . ? O5 Cu1 O1 168.3(7) . . ? O3 Cu1 O8 167.5(6) . . ? O5 Cu1 O8 89.4(6) . . ? O1 Cu1 O8 91.5(6) . . ? O3 Cu1 N1 95.4(5) . . ? O5 Cu1 N1 96.4(6) . . ? O1 Cu1 N1 95.1(6) . . ? O8 Cu1 N1 96.8(5) . . ? O3 Cu1 Cu2 84.3(4) . . ? O5 Cu1 Cu2 83.7(4) . . ? O1 Cu1 Cu2 84.9(5) . . ? O8 Cu1 Cu2 83.6(4) . . ? N1 Cu1 Cu2 179.6(4) . . ? O4 Cu2 O6 89.9(7) . . ? O4 Cu2 O7 168.0(7) . . ? O6 Cu2 O7 89.2(8) . . ? O4 Cu2 O2 89.4(7) . . ? O6 Cu2 O2 166.9(9) . . ? O7 Cu2 O2 88.7(6) . . ? O4 Cu2 N2 97.0(17) . 2_655 ? O6 Cu2 N2 95.9(19) . 2_655 ? O7 Cu2 N2 95.0(17) . 2_655 ? O2 Cu2 N2 97.2(19) . 2_655 ? O4 Cu2 Cu1 85.0(5) . . ? O6 Cu2 Cu1 83.1(7) . . ? O7 Cu2 Cu1 83.0(5) . . ? O2 Cu2 Cu1 83.8(5) . . ? N2 Cu2 Cu1 177.7(16) 2_655 . ? C1 O1 Cu1 121.8(18) . . ? C1 O2 Cu2 123.4(17) . . ? C8 O3 Cu1 122.0(14) . . ? C8 O4 Cu2 122.7(14) . . ? C15 O5 Cu1 128.7(15) . . ? C15 O6 Cu2 125.3(16) . . ? C22 O7 Cu2 129.9(11) . . ? C22 O8 Cu1 125.7(10) . . ? C29 N3A H31A 120.0 . . ? C29 N3A H32A 120.0 . . ? H31A N3A H32A 120.0 . . ? C29 N1 C32 120.0 . . ? C29 N1 Cu1 118.8(8) . . ? C32 N1 Cu1 120.9(7) . . ? N3A C29 N1 123(3) . . ? N3A C29 C30 116(3) . . ? N1 C29 C30 120.0 . . ? N3B C30 C29 117.7(12) . . ? N3B C30 N2 122.3(12) . . ? C29 C30 N2 120.0 . . ? C31 N2 C30 120.0 . . ? C31 N2 Cu2 119.3(8) . 4_564 ? C30 N2 Cu2 120.6(8) . 4_564 ? N3C C31 N2 112(4) . . ? N3C C31 C32 128(4) . . ? N2 C31 C32 120.0 . . ? C31 C32 N1 120.0 . . ? C31 C32 H32 120.0 . . ? N1 C32 H32 120.0 . . ? O1 C1 O2 126(3) . . ? O1 C1 C2 117(2) . . ? O2 C1 C2 115(2) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 115.4(12) . . ? C7 C2 C1 124.2(12) . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 I1 118.0(8) . . ? C4 C5 I1 121.3(8) . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? O3 C8 O4 125.2(19) . . ? O3 C8 C9 122.2(19) . . ? O4 C8 C9 112.2(17) . . ? C10 C9 C14 120.0 . . ? C10 C9 C8 115.6(10) . . ? C14 C9 C8 124.3(10) . . ? C9 C10 C11 120.0 . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 I2 118.1(8) . . ? C13 C12 I2 120.7(8) . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C9 120.0 . . ? C13 C14 H14 120.0 . . ? C9 C14 H14 120.0 . . ? O5 C15 O6 118.4(19) . . ? O5 C15 C16 128(2) . . ? O6 C15 C16 112.6(18) . . ? C17 C16 C21 120.0 . . ? C17 C16 C15 110.4(9) . . ? C21 C16 C15 126.8(9) . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.0 . . ? C18 C19 I3 121.1(5) . . ? C20 C19 I3 118.6(5) . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C16 120.0 . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? O8 C22 O7 114.8(11) . . ? O8 C22 C23 122.6(8) . . ? O7 C22 C23 119.6(8) . . ? C22 C23 C28 123.7 . . ? C22 C23 C24 115.7 . . ? C28 C23 C24 120.0 . . ? C25 C24 C23 119.9 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 I4 117.3(5) . . ? C25 C26 I4 122.6(5) . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C23 C28 C27 120.0 . . ? C23 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C30 N3B H31B 120.0 . . ? C30 N3B H32B 120.0 . . ? H31B N3B H32B 120.0 . . ? C31 N3C H31C 120.0 . . ? C31 N3C H32C 120.0 . . ? H31C N3C H32C 120.0 . . ? 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 O3 Cu1 Cu2 O4 -0.5(7) . . . . ? O5 Cu1 Cu2 O4 86.4(7) . . . . ? O1 Cu1 Cu2 O4 -91.3(7) . . . . ? O8 Cu1 Cu2 O4 176.6(7) . . . . ? N1 Cu1 Cu2 O4 -5(63) . . . . ? O3 Cu1 Cu2 O6 -91.0(8) . . . . ? O5 Cu1 Cu2 O6 -4.1(8) . . . . ? O1 Cu1 Cu2 O6 178.1(8) . . . . ? O8 Cu1 Cu2 O6 86.1(7) . . . . ? N1 Cu1 Cu2 O6 -96(63) . . . . ? O3 Cu1 Cu2 O7 179.0(6) . . . . ? O5 Cu1 Cu2 O7 -94.1(7) . . . . ? O1 Cu1 Cu2 O7 88.1(8) . . . . ? O8 Cu1 Cu2 O7 -3.9(6) . . . . ? N1 Cu1 Cu2 O7 174(100) . . . . ? O3 Cu1 Cu2 O2 89.5(7) . . . . ? O5 Cu1 Cu2 O2 176.4(7) . . . . ? O1 Cu1 Cu2 O2 -1.3(7) . . . . ? O8 Cu1 Cu2 O2 -93.4(7) . . . . ? N1 Cu1 Cu2 O2 85(63) . . . . ? O3 Cu1 Cu2 N2 -154(45) . . . 2_655 ? O5 Cu1 Cu2 N2 -67(45) . . . 2_655 ? O1 Cu1 Cu2 N2 115(45) . . . 2_655 ? O8 Cu1 Cu2 N2 23(45) . . . 2_655 ? N1 Cu1 Cu2 N2 -159(100) . . . 2_655 ? O3 Cu1 O1 C1 -87(2) . . . . ? O5 Cu1 O1 C1 -14(5) . . . . ? O8 Cu1 O1 C1 80(2) . . . . ? N1 Cu1 O1 C1 177(2) . . . . ? Cu2 Cu1 O1 C1 -3(2) . . . . ? O4 Cu2 O2 C1 90.8(19) . . . . ? O6 Cu2 O2 C1 4(5) . . . . ? O7 Cu2 O2 C1 -77.3(19) . . . . ? N2 Cu2 O2 C1 -172(2) 2_655 . . . ? Cu1 Cu2 O2 C1 5.8(18) . . . . ? O5 Cu1 O3 C8 -78.3(13) . . . . ? O1 Cu1 O3 C8 90.5(14) . . . . ? O8 Cu1 O3 C8 -8(3) . . . . ? N1 Cu1 O3 C8 -174.3(13) . . . . ? Cu2 Cu1 O3 C8 5.7(12) . . . . ? O6 Cu2 O4 C8 78.8(15) . . . . ? O7 Cu2 O4 C8 -7(4) . . . . ? O2 Cu2 O4 C8 -88.0(15) . . . . ? N2 Cu2 O4 C8 175(2) 2_655 . . . ? Cu1 Cu2 O4 C8 -4.2(13) . . . . ? O3 Cu1 O5 C15 94.2(16) . . . . ? O1 Cu1 O5 C15 21(4) . . . . ? O8 Cu1 O5 C15 -74.0(16) . . . . ? N1 Cu1 O5 C15 -170.8(16) . . . . ? Cu2 Cu1 O5 C15 9.6(15) . . . . ? O4 Cu2 O6 C15 -83.2(17) . . . . ? O7 Cu2 O6 C15 84.8(16) . . . . ? O2 Cu2 O6 C15 4(5) . . . . ? N2 Cu2 O6 C15 180(2) 2_655 . . . ? Cu1 Cu2 O6 C15 1.7(15) . . . . ? O4 Cu2 O7 C22 -2(4) . . . . ? O6 Cu2 O7 C22 -88.0(15) . . . . ? O2 Cu2 O7 C22 79.0(15) . . . . ? N2 Cu2 O7 C22 176(2) 2_655 . . . ? Cu1 Cu2 O7 C22 -4.8(13) . . . . ? O3 Cu1 O8 C22 29(3) . . . . ? O5 Cu1 O8 C22 99.1(12) . . . . ? O1 Cu1 O8 C22 -69.3(13) . . . . ? N1 Cu1 O8 C22 -164.6(12) . . . . ? Cu2 Cu1 O8 C22 15.4(11) . . . . ? O3 Cu1 N1 C29 -145.8(7) . . . . ? O5 Cu1 N1 C29 127.3(7) . . . . ? O1 Cu1 N1 C29 -55.0(8) . . . . ? O8 Cu1 N1 C29 37.1(7) . . . . ? Cu2 Cu1 N1 C29 -141(63) . . . . ? O3 Cu1 N1 C32 41.0(8) . . . . ? O5 Cu1 N1 C32 -45.9(8) . . . . ? O1 Cu1 N1 C32 131.8(8) . . . . ? O8 Cu1 N1 C32 -136.1(8) . . . . ? Cu2 Cu1 N1 C32 46(63) . . . . ? C32 N1 C29 N3A -172(4) . . . . ? Cu1 N1 C29 N3A 15(4) . . . . ? C32 N1 C29 C30 0.0 . . . . ? Cu1 N1 C29 C30 -173.3(8) . . . . ? N3A C29 C30 N3B -7(4) . . . . ? N1 C29 C30 N3B -179.5(16) . . . . ? N3A C29 C30 N2 173(4) . . . . ? N1 C29 C30 N2 0.0 . . . . ? N3B C30 N2 C31 179.5(17) . . . . ? C29 C30 N2 C31 0.0 . . . . ? N3B C30 N2 Cu2 2.8(16) . . . 4_564 ? C29 C30 N2 Cu2 -176.8(9) . . . 4_564 ? C30 N2 C31 N3C 178(4) . . . . ? Cu2 N2 C31 N3C -5(4) 4_564 . . . ? C30 N2 C31 C32 0.0 . . . . ? Cu2 N2 C31 C32 176.8(9) 4_564 . . . ? N3C C31 C32 N1 -178(5) . . . . ? N2 C31 C32 N1 0.0 . . . . ? C29 N1 C32 C31 0.0 . . . . ? Cu1 N1 C32 C31 173.1(9) . . . . ? Cu1 O1 C1 O2 9(4) . . . . ? Cu1 O1 C1 C2 169.3(12) . . . . ? Cu2 O2 C1 O1 -11(4) . . . . ? Cu2 O2 C1 C2 -171.6(12) . . . . ? O1 C1 C2 C3 15(3) . . . . ? O2 C1 C2 C3 177.6(16) . . . . ? O1 C1 C2 C7 -172.3(18) . . . . ? O2 C1 C2 C7 -10(3) . . . . ? C7 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C4 173.1(12) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C3 C4 C5 I1 170.3(7) . . . . ? C4 C5 C6 C7 0.0 . . . . ? I1 C5 C6 C7 -170.7(6) . . . . ? C5 C6 C7 C2 0.0 . . . . ? C3 C2 C7 C6 0.0 . . . . ? C1 C2 C7 C6 -172.5(13) . . . . ? Cu1 O3 C8 O4 -11(2) . . . . ? Cu1 O3 C8 C9 175.8(8) . . . . ? Cu2 O4 C8 O3 11(2) . . . . ? Cu2 O4 C8 C9 -175.8(9) . . . . ? O3 C8 C9 C10 -3.9(17) . . . . ? O4 C8 C9 C10 -177.8(11) . . . . ? O3 C8 C9 C14 172.7(12) . . . . ? O4 C8 C9 C14 -1.2(16) . . . . ? C14 C9 C10 C11 0.0 . . . . ? C8 C9 C10 C11 176.7(7) . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C10 C11 C12 I2 167.8(7) . . . . ? C11 C12 C13 C14 0.0 . . . . ? I2 C12 C13 C14 -167.5(7) . . . . ? C12 C13 C14 C9 0.0 . . . . ? C10 C9 C14 C13 0.0 . . . . ? C8 C9 C14 C13 -176.5(8) . . . . ? Cu1 O5 C15 O6 -11(2) . . . . ? Cu1 O5 C15 C16 -178.7(9) . . . . ? Cu2 O6 C15 O5 4(3) . . . . ? Cu2 O6 C15 C16 174.0(11) . . . . ? O5 C15 C16 C17 -11.8(18) . . . . ? O6 C15 C16 C17 179.6(11) . . . . ? O5 C15 C16 C21 -172.4(13) . . . . ? O6 C15 C16 C21 19.0(15) . . . . ? C21 C16 C17 C18 0.0 . . . . ? C15 C16 C17 C18 -162.1(6) . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C20 0.0 . . . . ? C17 C18 C19 I3 -173.2(5) . . . . ? C18 C19 C20 C21 0.0 . . . . ? I3 C19 C20 C21 173.3(5) . . . . ? C19 C20 C21 C16 0.0 . . . . ? C17 C16 C21 C20 0.0 . . . . ? C15 C16 C21 C20 158.9(8) . . . . ? Cu1 O8 C22 O7 -21.7(16) . . . . ? Cu1 O8 C22 C23 177.8(6) . . . . ? Cu2 O7 C22 O8 16.4(18) . . . . ? Cu2 O7 C22 C23 177.6(8) . . . . ? O8 C22 C23 C28 156.1(9) . . . . ? O7 C22 C23 C28 -3.6(9) . . . . ? O8 C22 C23 C24 -32.4(9) . . . . ? O7 C22 C23 C24 167.9(9) . . . . ? C22 C23 C24 C25 -171.8 . . . . ? C28 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C24 C25 C26 I4 178.4(5) . . . . ? C25 C26 C27 C28 0.0 . . . . ? I4 C26 C27 C28 -178.5(4) . . . . ? C22 C23 C28 C27 171.1 . . . . ? C24 C23 C28 C27 0.0 . . . . ? C26 C27 C28 C23 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.433 _diffrn_reflns_theta_full 23.97 _diffrn_measured_fraction_theta_full 0.433 _refine_diff_density_max 0.745 _refine_diff_density_min -1.405 _refine_diff_density_rms 0.278 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.002 -0.011 -0.057 3260.0 418.7 _platon_squeeze_details ; ? ; #===end data_compound6_bath862 _database_code_depnum_ccdc_archive 'CCDC 859607' #TrackingRef '- warren-pw.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87.50 H101.50 I8 N10.50 O22.50 Zn4' _chemical_formula_weight 2936.97 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' I I -0.4742 1.8119 '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 12.4072(8) _cell_length_b 12.4082(7) _cell_length_c 33.608(2) _cell_angle_alpha 87.891(2) _cell_angle_beta 88.473(2) _cell_angle_gamma 83.785(2) _cell_volume 5138.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7538 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 32.08 _exptl_crystal_description colorless _exptl_crystal_colour needle _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 3.397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Station 11.3.1 ALS' _diffrn_radiation_monochromator 'Channel-cut Si(111)' _diffrn_measurement_device_type 'Bruker APEX2' _diffrn_measurement_method '3000 0.3 degree images with \f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52084 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0999 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 32.00 _reflns_number_total 26906 _reflns_number_gt 17405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXTL (Sheldrick, 1997)' _computing_molecular_graphics POVRAY _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _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. The asymmetric unit in this structure is based on 4 zinc centres. The carbon atoms in the dabco ligand based on N3 were disordered in a 60:40 ratio. In addition to the MOF moiety, there are six full occupancy molecules of DMF present plus one molecule of DMF straddling an inversion centre and consequently present at 1/2 occupancy. Some distance restraints were applied in the solvent, while ADP restraints were applied to the partial carbons with 60% occupancy. Fragment atoms with occupancy of less than 50% were treated isotropically. ; _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^)+(0.1027P)^2^+20.7930P] 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 26906 _refine_ls_number_parameters 1229 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.2210 _refine_ls_wR_factor_gt 0.1937 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.022 _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 I1 I -0.62884(5) 0.40883(5) 0.535596(17) 0.03681(14) Uani 1 1 d . . . I2 I -0.21356(7) -0.56991(5) 0.634576(17) 0.04505(18) Uani 1 1 d . . . I3 I -0.33120(6) 0.64872(5) 0.795063(17) 0.04044(16) Uani 1 1 d . . . I4 I -0.04241(8) -0.20502(7) 0.90372(2) 0.0607(2) Uani 1 1 d . . . I5 I 0.53273(9) 0.81005(6) 0.61441(2) 0.0667(3) Uani 1 1 d . . . I6 I 0.91481(6) -0.15259(6) 0.715452(19) 0.04592(17) Uani 1 1 d . . . I7 I 0.72471(6) 1.09000(5) 0.876706(17) 0.03714(15) Uani 1 1 d . . . I8 I 1.17333(5) 0.18092(5) 0.962622(18) 0.03606(14) Uani 1 1 d . . . Zn1 Zn 0.04190(8) 0.04244(7) 0.53817(2) 0.02269(19) Uani 1 1 d . . . Zn2 Zn 0.24474(9) 0.21126(8) 0.70756(3) 0.0309(2) Uani 1 1 d . . . Zn3 Zn 0.33248(9) 0.29543(8) 0.78266(3) 0.0298(2) Uani 1 1 d . . . Zn4 Zn 0.47160(7) 0.45861(7) 0.96099(2) 0.02142(18) Uani 1 1 d . . . O1 O -0.0977(5) 0.1473(5) 0.53118(19) 0.0376(14) Uani 1 1 d . . . O2 O -0.1565(6) 0.0820(6) 0.47559(18) 0.0388(15) Uani 1 1 d . . . O3 O -0.0480(5) -0.0737(5) 0.56144(17) 0.0354(14) Uani 1 1 d . . . O4 O -0.1102(6) -0.1344(6) 0.50531(18) 0.0399(15) Uani 1 1 d . . . O5 O 0.2090(6) 0.4156(5) 0.76944(17) 0.0366(14) Uani 1 1 d . . . O6 O 0.1256(6) 0.3332(5) 0.72181(17) 0.0352(14) Uani 1 1 d . . . O7 O 0.2146(6) 0.2043(5) 0.80326(18) 0.0370(15) Uani 1 1 d . . . O8 O 0.1773(6) 0.1130(5) 0.74950(17) 0.0384(15) Uani 1 1 d . . . O9 O 0.4240(5) 0.3696(6) 0.74123(17) 0.0371(15) Uani 1 1 d . . . O10 O 0.3356(6) 0.3324(5) 0.68662(18) 0.0397(16) Uani 1 1 d . . . O11 O 0.4320(6) 0.1551(5) 0.77570(18) 0.0377(15) Uani 1 1 d . . . O12 O 0.3877(5) 0.1143(6) 0.71366(18) 0.0374(14) Uani 1 1 d . . . O13 O 0.5647(6) 0.6694(5) 1.00326(18) 0.0414(16) Uani 1 1 d . . . O14 O 0.5243(7) 0.6056(6) 0.94554(19) 0.0485(19) Uani 1 1 d . . . O15 O 0.6722(6) 0.4629(6) 1.02066(19) 0.0453(18) Uani 1 1 d . . . O16 O 0.6295(5) 0.3959(6) 0.9634(2) 0.0442(18) Uani 1 1 d . . . O17 O 0.4342(12) 0.0989(14) 0.5708(4) 0.119(5) Uani 1 1 d D . . O18 O 0.8041(10) 0.1944(8) 0.6763(3) 0.080(3) Uani 1 1 d . . . O19 O 0.7546(9) 0.3414(8) 0.8565(3) 0.077(3) Uani 1 1 d . . . O20 O 0.1308(9) -0.2101(8) 0.6710(3) 0.080(3) Uani 1 1 d . . . O21 O 0.4328(8) -0.2990(9) 0.8130(3) 0.074(3) Uani 1 1 d . . . O22 O 0.3767(6) 0.0567(6) 0.9294(3) 0.0501(19) Uani 1 1 d . . . O23 O 0.1255(18) -0.5523(18) 0.5538(7) 0.081(6) Uiso 0.50 1 d PD A -1 N1 N 0.3780(6) 0.3475(5) 0.83700(17) 0.0226(13) Uani 1 1 d . . . N2 N 0.4296(5) 0.4115(5) 0.90558(17) 0.0195(12) Uani 1 1 d . . . N3 N 0.1823(6) 0.1583(6) 0.65543(17) 0.0259(14) Uani 1 1 d . . . N4 N 0.1040(5) 0.0935(5) 0.59057(17) 0.0212(12) Uani 1 1 d . . . N5 N 0.5975(12) 0.1033(13) 0.6006(5) 0.130(7) Uani 1 1 d D . . N6 N 0.7718(8) 0.2359(7) 0.7419(3) 0.051(2) Uani 1 1 d D . . N7 N 0.9067(8) 0.4058(10) 0.8778(3) 0.067(3) Uani 1 1 d D . . N8 N 0.1563(8) -0.3660(7) 0.6361(3) 0.056(2) Uani 1 1 d D . . N9 N 0.3246(8) -0.2263(8) 0.7632(3) 0.054(2) Uani 1 1 d . . . N10 N 0.3319(8) -0.1134(8) 0.9199(4) 0.064(3) Uani 1 1 d . . . N11 N 0.0000(19) -0.5091(17) 0.4965(7) 0.048(4) Uiso 0.50 1 d PD A -1 C1 C -0.1677(7) 0.1432(7) 0.5053(2) 0.0274(16) Uani 1 1 d . . . C2 C -0.2723(7) 0.2134(7) 0.5097(2) 0.0263(16) Uani 1 1 d . . . C3 C -0.3589(8) 0.2043(8) 0.4852(3) 0.039(2) Uani 1 1 d . . . H3 H -0.3499 0.1560 0.4638 0.047 Uiso 1 1 calc R . . C4 C -0.4578(8) 0.2644(9) 0.4915(2) 0.039(2) Uani 1 1 d . . . H4 H -0.5149 0.2594 0.4736 0.047 Uiso 1 1 calc R . . C5 C -0.4748(7) 0.3315(7) 0.5234(3) 0.0312(18) Uani 1 1 d . . . C6 C -0.3894(8) 0.3445(8) 0.5474(3) 0.040(2) Uani 1 1 d . . . H6 H -0.3994 0.3935 0.5686 0.048 Uiso 1 1 calc R . . C7 C -0.2874(8) 0.2859(8) 0.5408(3) 0.038(2) Uani 1 1 d . . . H7 H -0.2288 0.2954 0.5574 0.046 Uiso 1 1 calc R . . C8 C -0.0948(7) -0.1394(7) 0.5421(2) 0.0278(16) Uani 1 1 d . . . C9 C -0.1345(7) -0.2331(7) 0.5653(2) 0.0270(16) Uani 1 1 d . . . C10 C -0.1923(8) -0.3075(7) 0.5465(2) 0.035(2) Uani 1 1 d . . . H10 H -0.2146 -0.2933 0.5198 0.042 Uiso 1 1 calc R . . C11 C -0.2174(9) -0.4031(8) 0.5669(3) 0.044(3) Uani 1 1 d . . . H11 H -0.2528 -0.4552 0.5537 0.053 Uiso 1 1 calc R . . C12 C -0.1901(9) -0.4200(8) 0.6062(2) 0.039(2) Uani 1 1 d . . . C13 C -0.1391(8) -0.3437(8) 0.6263(2) 0.037(2) Uani 1 1 d . . . H13 H -0.1236 -0.3551 0.6538 0.045 Uiso 1 1 calc R . . C14 C -0.1111(8) -0.2511(8) 0.6059(2) 0.039(2) Uani 1 1 d . . . H14 H -0.0758 -0.1995 0.6195 0.046 Uiso 1 1 calc R . . C15 C 0.1282(8) 0.4027(7) 0.7487(2) 0.035(2) Uani 1 1 d . . . C16 C 0.0243(8) 0.4721(7) 0.7563(2) 0.0319(19) Uani 1 1 d . . . C17 C -0.0657(8) 0.4664(8) 0.7326(2) 0.037(2) Uani 1 1 d . . . H17 H -0.0588 0.4245 0.7094 0.044 Uiso 1 1 calc R . . C18 C -0.1642(9) 0.5209(8) 0.7428(3) 0.041(2) Uani 1 1 d . . . H18 H -0.2250 0.5159 0.7266 0.049 Uiso 1 1 calc R . . C19 C -0.1766(8) 0.5837(7) 0.7766(2) 0.0334(19) Uani 1 1 d . . . C20 C -0.0866(9) 0.5940(8) 0.7994(3) 0.041(2) Uani 1 1 d . . . H20 H -0.0938 0.6383 0.8219 0.049 Uiso 1 1 calc R . . C21 C 0.0148(9) 0.5393(7) 0.7892(2) 0.035(2) Uani 1 1 d . . . H21 H 0.0765 0.5477 0.8045 0.042 Uiso 1 1 calc R . . C22 C 0.1760(8) 0.1286(7) 0.7867(2) 0.0316(18) Uani 1 1 d . . . C23 C 0.1215(7) 0.0502(7) 0.8141(3) 0.0317(18) Uani 1 1 d . . . C24 C 0.0673(9) -0.0295(7) 0.7984(3) 0.038(2) Uani 1 1 d . . . H24 H 0.0627 -0.0343 0.7703 0.046 Uiso 1 1 calc R . . C25 C 0.0194(9) -0.1030(8) 0.8239(3) 0.042(2) Uani 1 1 d . . . H25 H -0.0181 -0.1579 0.8134 0.051 Uiso 1 1 calc R . . C26 C 0.0270(8) -0.0954(8) 0.8645(3) 0.041(2) Uani 1 1 d . . . C27 C 0.0831(8) -0.0173(8) 0.8804(3) 0.037(2) Uani 1 1 d . . . H27 H 0.0906 -0.0149 0.9084 0.044 Uiso 1 1 calc R . . C28 C 0.1282(8) 0.0571(8) 0.8552(2) 0.0341(19) Uani 1 1 d . . . H28 H 0.1639 0.1131 0.8660 0.041 Uiso 1 1 calc R . . C29 C 0.3986(8) 0.3846(8) 0.7057(2) 0.036(2) Uani 1 1 d . . . C30 C 0.4435(8) 0.4792(7) 0.6836(2) 0.0299(18) Uani 1 1 d . . . C31 C 0.4883(9) 0.5568(7) 0.7044(3) 0.038(2) Uani 1 1 d . . . H31 H 0.4982 0.5467 0.7323 0.046 Uiso 1 1 calc R . . C32 C 0.5189(10) 0.6491(9) 0.6848(3) 0.048(3) Uani 1 1 d . . . H32 H 0.5511 0.7016 0.6991 0.058 Uiso 1 1 calc R . . C33 C 0.5021(9) 0.6646(8) 0.6439(3) 0.040(2) Uani 1 1 d . . . C34 C 0.4623(11) 0.5861(9) 0.6225(3) 0.052(3) Uani 1 1 d . . . H34 H 0.4560 0.5943 0.5944 0.063 Uiso 1 1 calc R . . C35 C 0.4316(9) 0.4950(8) 0.6427(3) 0.044(2) Uani 1 1 d . . . H35 H 0.4015 0.4415 0.6282 0.052 Uiso 1 1 calc R . . C36 C 0.4502(8) 0.1060(8) 0.7435(3) 0.037(2) Uani 1 1 d . . . C37 C 0.5536(8) 0.0328(8) 0.7391(2) 0.037(2) Uani 1 1 d . . . C38 C 0.5820(8) -0.0208(9) 0.7041(3) 0.045(3) Uani 1 1 d . . . H38 H 0.5307 -0.0185 0.6835 0.054 Uiso 1 1 calc R . . C39 C 0.6820(9) -0.0765(9) 0.6987(3) 0.046(2) Uani 1 1 d . . . H39 H 0.7000 -0.1111 0.6743 0.055 Uiso 1 1 calc R . . C40 C 0.7579(8) -0.0830(8) 0.7288(3) 0.036(2) Uani 1 1 d . . . C41 C 0.7294(9) -0.0371(8) 0.7655(3) 0.041(2) Uani 1 1 d . . . H41 H 0.7789 -0.0436 0.7868 0.049 Uiso 1 1 calc R . . C42 C 0.6264(10) 0.0184(8) 0.7699(3) 0.045(3) Uani 1 1 d . . . H42 H 0.6052 0.0476 0.7950 0.055 Uiso 1 1 calc R . . C43 C 0.5570(7) 0.6760(7) 0.9664(2) 0.0283(17) Uani 1 1 d . . . C44 C 0.5941(7) 0.7736(7) 0.9448(2) 0.0280(17) Uani 1 1 d . . . C45 C 0.6149(9) 0.7738(7) 0.9041(3) 0.040(2) Uani 1 1 d . . . H45 H 0.6039 0.7116 0.8898 0.048 Uiso 1 1 calc R . . C46 C 0.6515(9) 0.8627(8) 0.8840(2) 0.041(2) Uani 1 1 d . . . H46 H 0.6680 0.8610 0.8562 0.050 Uiso 1 1 calc R . . C47 C 0.6638(7) 0.9553(7) 0.9054(2) 0.0292(17) Uani 1 1 d . . . C48 C 0.6392(8) 0.9575(7) 0.9456(2) 0.0321(18) Uani 1 1 d . . . H48 H 0.6470 1.0210 0.9598 0.039 Uiso 1 1 calc R . . C49 C 0.6034(8) 0.8683(7) 0.9655(3) 0.0325(18) Uani 1 1 d . . . H49 H 0.5852 0.8709 0.9931 0.039 Uiso 1 1 calc R . . C50 C 0.6942(7) 0.4072(7) 0.9906(2) 0.0279(16) Uani 1 1 d . . . C51 C 0.8062(7) 0.3535(7) 0.9856(2) 0.0271(16) Uani 1 1 d . . . C52 C 0.8252(7) 0.2688(7) 0.9601(3) 0.0330(18) Uani 1 1 d . . . H52 H 0.7666 0.2466 0.9459 0.040 Uiso 1 1 calc R . . C53 C 0.9289(7) 0.2152(7) 0.9547(3) 0.0329(18) Uani 1 1 d . . . H53 H 0.9404 0.1542 0.9382 0.040 Uiso 1 1 calc R . . C54 C 1.0166(7) 0.2527(7) 0.9739(2) 0.0298(17) Uani 1 1 d . . . C55 C 0.9978(7) 0.3398(7) 0.9994(2) 0.0317(18) Uani 1 1 d . . . H55 H 1.0567 0.3646 1.0127 0.038 Uiso 1 1 calc R . . C56 C 0.8939(7) 0.3899(7) 1.0054(2) 0.0272(16) Uani 1 1 d . . . H56 H 0.8814 0.4487 1.0228 0.033 Uiso 1 1 calc R . . C57 C 0.0234(14) 0.1033(19) 0.6229(5) 0.047(4) Uani 0.60 1 d PU B 1 H57A H -0.0032 0.0318 0.6287 0.056 Uiso 0.60 1 calc PR B 1 H57B H -0.0390 0.1549 0.6146 0.056 Uiso 0.60 1 calc PR B 1 C58 C 0.0707(12) 0.1429(16) 0.6608(5) 0.041(4) Uani 0.60 1 d PU B 1 H58A H 0.0294 0.2122 0.6682 0.049 Uiso 0.60 1 calc PR B 1 H58B H 0.0626 0.0891 0.6828 0.049 Uiso 0.60 1 calc PR B 1 C59 C 0.1528(16) 0.1974(13) 0.5833(4) 0.032(3) Uani 0.60 1 d PU B 1 H59A H 0.0961 0.2549 0.5744 0.039 Uiso 0.60 1 calc PR B 1 H59B H 0.2094 0.1883 0.5620 0.039 Uiso 0.60 1 calc PR B 1 C60 C 0.2033(15) 0.2312(13) 0.6218(4) 0.031(3) Uani 0.60 1 d PU B 1 H60A H 0.2826 0.2311 0.6176 0.038 Uiso 0.60 1 calc PR B 1 H60B H 0.1728 0.3060 0.6280 0.038 Uiso 0.60 1 calc PR B 1 C61 C 0.1986(14) 0.0108(12) 0.6049(5) 0.033(3) Uani 0.60 1 d PU B 1 H61A H 0.1721 -0.0611 0.6097 0.040 Uiso 0.60 1 calc PR B 1 H61B H 0.2561 0.0036 0.5839 0.040 Uiso 0.60 1 calc PR B 1 C62 C 0.2462(14) 0.0468(11) 0.6435(5) 0.034(3) Uani 0.60 1 d PU B 1 H62A H 0.3242 0.0553 0.6393 0.041 Uiso 0.60 1 calc PR B 1 H62B H 0.2391 -0.0086 0.6651 0.041 Uiso 0.60 1 calc PR B 1 C63 C 0.2840(8) 0.4050(12) 0.8571(3) 0.060(4) Uani 1 1 d . . . H63A H 0.2246 0.3578 0.8593 0.072 Uiso 1 1 calc R . . H63B H 0.2581 0.4708 0.8410 0.072 Uiso 1 1 calc R . . C64 C 0.3132(7) 0.4380(8) 0.8991(2) 0.0337(19) Uani 1 1 d . . . H64A H 0.2934 0.5169 0.9019 0.040 Uiso 1 1 calc R . . H64B H 0.2715 0.3992 0.9195 0.040 Uiso 1 1 calc R . . C65 C 0.4635(9) 0.4223(10) 0.8319(3) 0.048(3) Uani 1 1 d . . . H65A H 0.4380 0.4838 0.8137 0.058 Uiso 1 1 calc R . . H65B H 0.5295 0.3835 0.8198 0.058 Uiso 1 1 calc R . . C66 C 0.4908(8) 0.4659(8) 0.8729(2) 0.038(2) Uani 1 1 d . . . H66A H 0.5697 0.4514 0.8773 0.045 Uiso 1 1 calc R . . H66B H 0.4708 0.5454 0.8731 0.045 Uiso 1 1 calc R . . C67 C 0.4205(13) 0.2549(8) 0.8620(3) 0.062(4) Uani 1 1 d . . . H67A H 0.4820 0.2139 0.8479 0.075 Uiso 1 1 calc R . . H67B H 0.3634 0.2060 0.8670 0.075 Uiso 1 1 calc R . . C68 C 0.4591(10) 0.2919(7) 0.9023(2) 0.042(3) Uani 1 1 d . . . H68A H 0.4245 0.2527 0.9245 0.050 Uiso 1 1 calc R . . H68B H 0.5387 0.2747 0.9040 0.050 Uiso 1 1 calc R . . C69 C 0.5272(17) 0.0713(13) 0.5731(5) 0.088(5) Uani 1 1 d D . . H69 H 0.5577 0.0216 0.5539 0.105 Uiso 1 1 calc R . . C70 C 0.5557(17) 0.1809(17) 0.6285(6) 0.114(7) Uani 1 1 d D . . H70A H 0.5607 0.2541 0.6170 0.171 Uiso 1 1 calc R . . H70B H 0.5978 0.1708 0.6528 0.171 Uiso 1 1 calc R . . H70C H 0.4796 0.1716 0.6348 0.171 Uiso 1 1 calc R . . C71 C 0.7054(13) 0.0548(14) 0.5988(5) 0.092(6) Uani 1 1 d D . . H71A H 0.7205 0.0090 0.6227 0.137 Uiso 1 1 calc R . . H71B H 0.7548 0.1115 0.5970 0.137 Uiso 1 1 calc R . . H71C H 0.7160 0.0104 0.5752 0.137 Uiso 1 1 calc R . . C72 C 0.7470(13) 0.2266(11) 0.7028(4) 0.070(4) Uani 1 1 d D . . H72 H 0.6738 0.2493 0.6962 0.084 Uiso 1 1 calc R . . C73 C 0.8740(12) 0.1895(13) 0.7552(5) 0.082(5) Uani 1 1 d . . . H73A H 0.8642 0.1437 0.7792 0.123 Uiso 1 1 calc R . . H73B H 0.9181 0.2473 0.7615 0.123 Uiso 1 1 calc R . . H73C H 0.9107 0.1453 0.7343 0.123 Uiso 1 1 calc R . . C74 C 0.6933(12) 0.2842(12) 0.7702(5) 0.073(4) Uani 1 1 d . . . H74A H 0.6207 0.2881 0.7592 0.109 Uiso 1 1 calc R . . H74B H 0.7103 0.3574 0.7757 0.109 Uiso 1 1 calc R . . H74C H 0.6957 0.2398 0.7950 0.109 Uiso 1 1 calc R . . C75 C 0.7986(10) 0.4091(12) 0.8748(4) 0.071(4) Uani 1 1 d D . . H75 H 0.7539 0.4657 0.8873 0.085 Uiso 1 1 calc R . . C76 C 0.9754(13) 0.3160(11) 0.8595(5) 0.076(4) Uani 1 1 d . . . H76A H 0.9311 0.2578 0.8539 0.114 Uiso 1 1 calc R . . H76B H 1.0328 0.2882 0.8779 0.114 Uiso 1 1 calc R . . H76C H 1.0081 0.3421 0.8346 0.114 Uiso 1 1 calc R . . C77 C 0.9704(14) 0.4707(11) 0.8981(4) 0.075(4) Uani 1 1 d . . . H77A H 1.0210 0.5022 0.8793 0.112 Uiso 1 1 calc R . . H77B H 1.0114 0.4264 0.9185 0.112 Uiso 1 1 calc R . . H77C H 0.9237 0.5290 0.9108 0.112 Uiso 1 1 calc R . . C78 C 0.1304(11) -0.3080(11) 0.6693(4) 0.065(3) Uani 1 1 d D . . H78 H 0.1105 -0.3466 0.6928 0.077 Uiso 1 1 calc R . . C79 C 0.1851(13) -0.3104(11) 0.6005(4) 0.079(4) Uani 1 1 d D . . H79A H 0.1244 -0.2575 0.5925 0.119 Uiso 1 1 calc R . . H79B H 0.2018 -0.3625 0.5794 0.119 Uiso 1 1 calc R . . H79C H 0.2488 -0.2725 0.6050 0.119 Uiso 1 1 calc R . . C80 C 0.1445(13) -0.4781(10) 0.6363(5) 0.082(5) Uani 1 1 d D . . H80A H 0.2089 -0.5192 0.6477 0.123 Uiso 1 1 calc R . . H80B H 0.1361 -0.5003 0.6090 0.123 Uiso 1 1 calc R . . H80C H 0.0802 -0.4924 0.6524 0.123 Uiso 1 1 calc R . . C81 C 0.4081(11) -0.2298(12) 0.7861(4) 0.062(3) Uani 1 1 d . . . H81 H 0.4546 -0.1742 0.7818 0.075 Uiso 1 1 calc R . . C82 C 0.2503(14) -0.3049(12) 0.7703(5) 0.088(5) Uani 1 1 d . . . H82A H 0.2803 -0.3739 0.7591 0.132 Uiso 1 1 calc R . . H82B H 0.1814 -0.2798 0.7577 0.132 Uiso 1 1 calc R . . H82C H 0.2381 -0.3153 0.7991 0.132 Uiso 1 1 calc R . . C83 C 0.3074(11) -0.1477(9) 0.7311(4) 0.057(3) Uani 1 1 d . . . H83A H 0.3748 -0.1153 0.7250 0.085 Uiso 1 1 calc R . . H83B H 0.2504 -0.0908 0.7388 0.085 Uiso 1 1 calc R . . H83C H 0.2853 -0.1832 0.7075 0.085 Uiso 1 1 calc R . . C84 C 0.3698(11) -0.0257(10) 0.9098(4) 0.062(3) Uani 1 1 d . . . H84 H 0.3973 -0.0218 0.8832 0.074 Uiso 1 1 calc R . . C85 C 0.2939(13) -0.1285(13) 0.9620(5) 0.080(4) Uani 1 1 d . . . H85A H 0.3484 -0.1764 0.9766 0.120 Uiso 1 1 calc R . . H85B H 0.2253 -0.1609 0.9625 0.120 Uiso 1 1 calc R . . H85C H 0.2831 -0.0579 0.9745 0.120 Uiso 1 1 calc R . . C86 C 0.3234(12) -0.2057(11) 0.8979(5) 0.078(5) Uani 1 1 d . . . H86A H 0.2474 -0.2087 0.8912 0.117 Uiso 1 1 calc R . . H86B H 0.3492 -0.2707 0.9138 0.117 Uiso 1 1 calc R . . H86C H 0.3675 -0.2021 0.8734 0.117 Uiso 1 1 calc R . . C87 C 0.025(2) -0.5831(19) 0.5272(6) 0.058(6) Uiso 0.50 1 d PD A -1 H87 H -0.0116 -0.6456 0.5324 0.070 Uiso 0.50 1 calc PR A -1 C88 C 0.055(2) -0.4160(19) 0.4882(8) 0.064(7) Uiso 0.50 1 d PD A -1 H88A H 0.0562 -0.3747 0.5125 0.096 Uiso 0.50 1 calc PR A -1 H88B H 0.0165 -0.3704 0.4675 0.096 Uiso 0.50 1 calc PR A -1 H88C H 0.1291 -0.4384 0.4790 0.096 Uiso 0.50 1 calc PR A -1 C89 C -0.090(2) -0.524(2) 0.4729(9) 0.071(7) Uiso 0.50 1 d PD A -1 H89A H -0.1212 -0.5896 0.4824 0.107 Uiso 0.50 1 calc PR A -1 H89B H -0.0653 -0.5320 0.4451 0.107 Uiso 0.50 1 calc PR A -1 H89C H -0.1441 -0.4612 0.4749 0.107 Uiso 0.50 1 calc PR A -1 C57A C 0.012(3) 0.166(3) 0.6109(10) 0.053(7) Uiso 0.40 1 d P B 2 H57C H -0.0487 0.1233 0.6189 0.064 Uiso 0.40 1 calc PR B 2 H57D H -0.0163 0.2261 0.5925 0.064 Uiso 0.40 1 calc PR B 2 C58A C 0.063(2) 0.214(2) 0.6504(8) 0.040(5) Uiso 0.40 1 d P B 2 H58C H 0.0636 0.2939 0.6470 0.048 Uiso 0.40 1 calc PR B 2 H58D H 0.0185 0.1992 0.6744 0.048 Uiso 0.40 1 calc PR B 2 C59A C 0.191(2) 0.164(2) 0.5804(7) 0.027(5) Uiso 0.40 1 d P B 2 H59C H 0.1604 0.2318 0.5664 0.032 Uiso 0.40 1 calc PR B 2 H59D H 0.2468 0.1262 0.5627 0.032 Uiso 0.40 1 calc PR B 2 C60A C 0.245(2) 0.192(2) 0.6210(8) 0.042(7) Uiso 0.40 1 d P B 2 H60C H 0.3194 0.1551 0.6222 0.051 Uiso 0.40 1 calc PR B 2 H60D H 0.2490 0.2713 0.6216 0.051 Uiso 0.40 1 calc PR B 2 C61A C 0.147(3) 0.007(3) 0.6151(11) 0.061(9) Uiso 0.40 1 d P B 2 H61C H 0.2087 -0.0338 0.6010 0.073 Uiso 0.40 1 calc PR B 2 H61D H 0.0911 -0.0429 0.6207 0.073 Uiso 0.40 1 calc PR B 2 C62A C 0.186(3) 0.046(3) 0.6546(10) 0.054(7) Uiso 0.40 1 d P B 2 H62C H 0.1403 0.0202 0.6768 0.065 Uiso 0.40 1 calc PR B 2 H62D H 0.2616 0.0138 0.6590 0.065 Uiso 0.40 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0358(3) 0.0504(4) 0.0257(3) -0.0120(2) -0.0069(2) -0.0061(3) I2 0.0820(5) 0.0370(3) 0.0219(3) 0.0040(2) -0.0171(3) -0.0304(3) I3 0.0565(4) 0.0443(3) 0.0234(3) -0.0078(2) -0.0025(2) -0.0163(3) I4 0.0878(6) 0.0514(4) 0.0458(4) 0.0125(3) 0.0081(4) -0.0273(4) I5 0.1325(8) 0.0433(4) 0.0333(3) 0.0054(3) -0.0269(4) -0.0465(5) I6 0.0534(4) 0.0562(4) 0.0319(3) -0.0187(3) -0.0012(3) -0.0170(3) I7 0.0570(4) 0.0308(3) 0.0268(3) -0.0033(2) -0.0039(2) -0.0175(3) I8 0.0293(3) 0.0423(3) 0.0357(3) 0.0008(2) -0.0045(2) 0.0002(2) Zn1 0.0319(5) 0.0261(4) 0.0124(4) -0.0037(3) -0.0079(3) -0.0108(4) Zn2 0.0500(6) 0.0358(5) 0.0113(4) -0.0043(3) -0.0079(4) -0.0218(5) Zn3 0.0481(6) 0.0342(5) 0.0112(4) -0.0047(3) -0.0073(4) -0.0195(4) Zn4 0.0285(5) 0.0248(4) 0.0118(4) -0.0066(3) -0.0073(3) -0.0032(3) O1 0.038(3) 0.039(3) 0.037(3) -0.010(3) -0.014(3) -0.002(3) O2 0.045(4) 0.044(4) 0.027(3) -0.010(3) -0.006(3) 0.000(3) O3 0.049(4) 0.038(3) 0.024(3) -0.008(2) -0.003(3) -0.024(3) O4 0.052(4) 0.048(4) 0.024(3) 0.003(3) -0.007(3) -0.024(3) O5 0.053(4) 0.037(3) 0.024(3) -0.003(2) -0.011(3) -0.017(3) O6 0.052(4) 0.039(3) 0.018(3) -0.006(2) -0.011(3) -0.014(3) O7 0.055(4) 0.035(3) 0.025(3) -0.005(2) -0.002(3) -0.021(3) O8 0.053(4) 0.046(4) 0.020(3) -0.001(3) -0.001(3) -0.025(3) O9 0.045(4) 0.052(4) 0.019(3) 0.003(3) -0.005(2) -0.023(3) O10 0.059(4) 0.042(4) 0.024(3) 0.000(3) -0.007(3) -0.032(3) O11 0.059(4) 0.034(3) 0.023(3) -0.010(2) 0.000(3) -0.018(3) O12 0.042(4) 0.048(4) 0.025(3) -0.013(3) -0.005(3) -0.012(3) O13 0.072(5) 0.034(3) 0.022(3) 0.000(2) -0.010(3) -0.023(3) O14 0.087(6) 0.040(4) 0.025(3) 0.000(3) -0.015(3) -0.035(4) O15 0.044(4) 0.062(5) 0.029(3) -0.027(3) -0.006(3) 0.012(3) O16 0.026(3) 0.071(5) 0.036(3) -0.030(3) -0.011(3) 0.006(3) O17 0.085(9) 0.171(15) 0.110(10) 0.009(9) -0.002(8) -0.053(9) O18 0.118(9) 0.071(6) 0.051(5) -0.001(5) 0.028(6) -0.015(6) O19 0.088(7) 0.067(6) 0.081(7) 0.005(5) -0.006(6) -0.027(5) O20 0.082(7) 0.059(6) 0.103(8) -0.015(5) -0.015(6) -0.016(5) O21 0.084(7) 0.090(7) 0.045(5) 0.020(5) -0.012(4) 0.007(5) O22 0.038(4) 0.034(4) 0.078(6) 0.003(4) -0.001(4) 0.000(3) N1 0.037(4) 0.024(3) 0.010(3) -0.006(2) -0.004(2) -0.014(3) N2 0.027(3) 0.021(3) 0.012(3) -0.003(2) -0.007(2) -0.007(2) N3 0.038(4) 0.034(4) 0.009(3) -0.004(2) -0.005(2) -0.015(3) N4 0.030(3) 0.026(3) 0.011(3) -0.002(2) -0.005(2) -0.014(3) N5 0.127(15) 0.124(15) 0.123(15) 0.061(12) 0.052(13) 0.014(12) N6 0.051(5) 0.046(5) 0.055(6) 0.009(4) 0.003(4) -0.007(4) N7 0.043(6) 0.089(8) 0.068(7) 0.038(6) -0.005(5) -0.018(5) N8 0.058(6) 0.040(5) 0.070(7) 0.007(5) 0.000(5) -0.006(4) N9 0.052(6) 0.048(5) 0.061(6) 0.021(4) -0.011(5) -0.004(4) N10 0.053(6) 0.038(5) 0.101(9) -0.020(5) -0.028(6) 0.006(4) C1 0.037(4) 0.025(4) 0.022(4) -0.006(3) -0.004(3) -0.010(3) C2 0.033(4) 0.029(4) 0.019(3) -0.005(3) -0.006(3) -0.011(3) C3 0.050(6) 0.044(5) 0.024(4) -0.007(4) -0.014(4) 0.001(4) C4 0.038(5) 0.061(6) 0.018(4) -0.014(4) -0.009(3) 0.002(4) C5 0.035(5) 0.031(4) 0.031(4) -0.006(3) -0.005(3) -0.013(3) C6 0.038(5) 0.049(6) 0.035(5) -0.023(4) -0.009(4) -0.003(4) C7 0.042(5) 0.036(5) 0.037(5) -0.017(4) -0.009(4) -0.003(4) C8 0.037(4) 0.027(4) 0.021(4) -0.001(3) -0.005(3) -0.008(3) C9 0.038(4) 0.030(4) 0.016(3) -0.001(3) -0.003(3) -0.013(3) C10 0.056(6) 0.039(5) 0.015(4) 0.001(3) -0.014(4) -0.025(4) C11 0.074(7) 0.039(5) 0.027(4) 0.005(4) -0.016(4) -0.033(5) C12 0.062(6) 0.040(5) 0.018(4) 0.000(3) -0.012(4) -0.021(4) C13 0.059(6) 0.042(5) 0.015(4) -0.004(3) -0.012(4) -0.018(4) C14 0.056(6) 0.046(5) 0.018(4) 0.000(3) -0.009(4) -0.026(5) C15 0.057(6) 0.036(5) 0.018(4) -0.001(3) -0.014(4) -0.026(4) C16 0.050(5) 0.035(4) 0.015(3) -0.002(3) -0.005(3) -0.019(4) C17 0.043(5) 0.055(6) 0.015(4) -0.007(4) -0.003(3) -0.016(4) C18 0.057(6) 0.048(6) 0.022(4) -0.007(4) -0.016(4) -0.021(5) C19 0.047(5) 0.037(5) 0.019(4) -0.004(3) -0.004(3) -0.017(4) C20 0.069(7) 0.038(5) 0.021(4) 0.000(3) -0.008(4) -0.024(5) C21 0.059(6) 0.029(4) 0.023(4) -0.002(3) -0.010(4) -0.022(4) C22 0.043(5) 0.036(4) 0.019(4) 0.001(3) -0.007(3) -0.018(4) C23 0.038(5) 0.033(4) 0.025(4) 0.004(3) -0.005(3) -0.012(4) C24 0.057(6) 0.034(5) 0.027(4) -0.004(4) -0.007(4) -0.013(4) C25 0.053(6) 0.042(5) 0.036(5) 0.004(4) -0.014(4) -0.020(4) C26 0.043(5) 0.041(5) 0.038(5) 0.012(4) 0.001(4) -0.015(4) C27 0.042(5) 0.045(5) 0.025(4) -0.001(4) -0.006(4) -0.012(4) C28 0.043(5) 0.037(5) 0.023(4) -0.002(3) -0.006(3) -0.005(4) C29 0.053(6) 0.040(5) 0.019(4) -0.001(3) -0.002(4) -0.023(4) C30 0.045(5) 0.029(4) 0.019(4) -0.011(3) -0.003(3) -0.015(4) C31 0.062(6) 0.034(5) 0.021(4) -0.006(3) -0.009(4) -0.019(4) C32 0.076(8) 0.052(6) 0.023(4) -0.007(4) -0.012(4) -0.032(5) C33 0.065(7) 0.033(5) 0.024(4) -0.004(3) -0.013(4) -0.018(4) C34 0.092(9) 0.047(6) 0.026(5) -0.005(4) -0.009(5) -0.037(6) C35 0.072(7) 0.043(5) 0.021(4) -0.003(4) -0.003(4) -0.030(5) C36 0.056(6) 0.037(5) 0.022(4) -0.006(3) -0.002(4) -0.025(4) C37 0.056(6) 0.043(5) 0.018(4) -0.013(3) 0.004(4) -0.025(4) C38 0.043(6) 0.067(7) 0.030(5) -0.025(5) -0.001(4) -0.022(5) C39 0.044(6) 0.066(7) 0.030(5) -0.017(5) 0.000(4) -0.021(5) C40 0.046(5) 0.037(5) 0.029(4) -0.010(4) 0.002(4) -0.021(4) C41 0.064(7) 0.039(5) 0.024(4) -0.007(4) -0.006(4) -0.017(5) C42 0.080(8) 0.037(5) 0.021(4) -0.009(4) -0.005(4) -0.008(5) C43 0.038(5) 0.032(4) 0.017(3) -0.001(3) -0.005(3) -0.010(3) C44 0.032(4) 0.029(4) 0.025(4) -0.002(3) -0.013(3) -0.009(3) C45 0.068(7) 0.031(5) 0.022(4) -0.012(3) -0.002(4) -0.016(4) C46 0.072(7) 0.042(5) 0.015(4) -0.006(3) 0.001(4) -0.028(5) C47 0.037(5) 0.030(4) 0.023(4) -0.002(3) -0.008(3) -0.010(3) C48 0.044(5) 0.028(4) 0.025(4) -0.008(3) -0.010(3) -0.004(4) C49 0.046(5) 0.029(4) 0.023(4) -0.007(3) -0.005(3) -0.006(4) C50 0.034(4) 0.031(4) 0.019(3) -0.002(3) -0.004(3) -0.001(3) C51 0.036(4) 0.030(4) 0.017(3) -0.004(3) -0.008(3) -0.008(3) C52 0.031(4) 0.039(5) 0.031(4) -0.010(4) -0.006(3) -0.004(4) C53 0.034(5) 0.031(4) 0.034(4) -0.010(3) -0.003(4) 0.000(3) C54 0.026(4) 0.040(5) 0.023(4) 0.002(3) -0.007(3) 0.000(3) C55 0.039(5) 0.035(4) 0.023(4) 0.000(3) -0.010(3) -0.008(4) C56 0.028(4) 0.034(4) 0.021(4) -0.004(3) -0.004(3) -0.009(3) C57 0.036(7) 0.075(9) 0.033(7) -0.018(7) 0.003(6) -0.014(7) C58 0.028(6) 0.064(8) 0.032(6) -0.016(6) -0.011(5) -0.009(6) C59 0.050(8) 0.025(6) 0.026(6) 0.000(5) -0.015(6) -0.015(6) C60 0.047(7) 0.029(6) 0.021(5) 0.002(5) -0.013(5) -0.015(6) C61 0.038(7) 0.035(6) 0.029(6) -0.017(5) -0.019(5) 0.000(5) C62 0.045(7) 0.022(6) 0.034(6) -0.009(5) -0.007(6) 0.003(5) C63 0.034(5) 0.113(11) 0.034(5) -0.044(6) -0.008(4) 0.009(6) C64 0.035(5) 0.049(5) 0.019(4) -0.006(3) -0.003(3) -0.009(4) C65 0.060(7) 0.071(7) 0.023(4) -0.014(4) 0.004(4) -0.047(6) C66 0.050(5) 0.053(6) 0.018(4) -0.016(4) 0.002(3) -0.036(5) C67 0.129(12) 0.031(5) 0.029(5) -0.009(4) -0.038(6) -0.003(6) C68 0.083(8) 0.021(4) 0.020(4) -0.004(3) -0.027(4) 0.007(4) C69 0.107(14) 0.068(10) 0.093(13) 0.028(9) -0.033(11) -0.035(10) C70 0.101(15) 0.125(17) 0.118(17) -0.017(14) 0.013(13) -0.024(13) C71 0.093(12) 0.086(11) 0.086(11) 0.040(9) 0.042(9) 0.009(9) C72 0.088(10) 0.063(8) 0.064(8) 0.016(7) 0.005(8) -0.034(7) C73 0.071(9) 0.072(9) 0.107(12) 0.020(9) -0.029(9) -0.028(8) C74 0.074(9) 0.065(9) 0.078(10) -0.024(7) 0.016(8) 0.002(7) C75 0.079(10) 0.072(9) 0.065(8) 0.030(7) -0.024(7) -0.030(7) C76 0.083(10) 0.056(8) 0.090(11) 0.002(7) -0.011(8) -0.015(7) C77 0.129(13) 0.055(8) 0.047(7) 0.011(6) -0.010(8) -0.042(8) C78 0.071(9) 0.068(9) 0.058(8) 0.000(6) -0.018(6) -0.021(7) C79 0.090(11) 0.063(9) 0.081(10) 0.017(7) 0.023(8) -0.003(8) C80 0.082(10) 0.057(8) 0.112(13) 0.032(8) -0.038(9) -0.033(7) C81 0.060(8) 0.077(9) 0.051(7) -0.006(6) 0.001(6) -0.010(7) C82 0.103(12) 0.058(8) 0.106(13) 0.026(8) -0.040(10) -0.018(8) C83 0.066(8) 0.044(6) 0.062(7) 0.015(5) 0.000(6) -0.013(5) C84 0.057(7) 0.051(7) 0.073(9) 0.003(6) -0.006(6) 0.010(6) C85 0.075(10) 0.085(11) 0.076(10) 0.032(8) -0.015(8) -0.002(8) C86 0.082(10) 0.057(8) 0.097(11) -0.047(8) -0.035(8) 0.013(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 C5 2.081(9) . ? I2 C12 2.103(9) . ? I3 C19 2.087(10) . ? I4 C26 2.096(9) . ? I5 C33 2.093(9) . ? I6 C40 2.086(10) . ? I7 C47 2.100(8) . ? I8 C54 2.081(8) . ? Zn1 O3 2.038(6) . ? Zn1 O2 2.040(7) 2_556 ? Zn1 O4 2.044(6) 2_556 ? Zn1 O1 2.064(6) . ? Zn1 N4 2.087(6) . ? Zn1 Zn1 3.0582(16) 2_556 ? Zn2 O12 2.043(7) . ? Zn2 O8 2.051(6) . ? Zn2 O6 2.058(7) . ? Zn2 O10 2.067(6) . ? Zn2 N3 2.090(6) . ? Zn2 Zn3 3.0387(12) . ? Zn3 O9 2.031(6) . ? Zn3 O7 2.035(6) . ? Zn3 O11 2.040(7) . ? Zn3 O5 2.064(7) . ? Zn3 N1 2.072(6) . ? Zn4 O15 2.030(7) 2_667 ? Zn4 O16 2.031(6) . ? Zn4 O13 2.039(6) 2_667 ? Zn4 O14 2.048(6) . ? Zn4 N2 2.069(6) . ? Zn4 Zn4 2.9802(15) 2_667 ? O1 C1 1.252(10) . ? O2 C1 1.272(10) . ? O2 Zn1 2.040(7) 2_556 ? O3 C8 1.259(9) . ? O4 C8 1.254(10) . ? O4 Zn1 2.044(6) 2_556 ? O5 C15 1.263(10) . ? O6 C15 1.277(10) . ? O7 C22 1.253(10) . ? O8 C22 1.273(10) . ? O9 C29 1.247(10) . ? O10 C29 1.267(10) . ? O11 C36 1.264(10) . ? O12 C36 1.279(11) . ? O13 C43 1.245(9) . ? O13 Zn4 2.039(6) 2_667 ? O14 C43 1.247(10) . ? O15 C50 1.252(10) . ? O15 Zn4 2.030(7) 2_667 ? O16 C50 1.255(10) . ? O17 C69 1.17(2) . ? O18 C72 1.178(16) . ? O19 C75 1.239(16) . ? O20 C78 1.219(15) . ? O21 C81 1.245(15) . ? O22 C84 1.249(15) . ? O23 C87 1.64(3) . ? N1 C67 1.458(12) . ? N1 C63 1.462(12) . ? N1 C65 1.485(11) . ? N2 C64 1.466(11) . ? N2 C68 1.497(10) . ? N2 C66 1.501(10) . ? N3 C62A 1.39(3) . ? N3 C58 1.424(17) . ? N3 C60A 1.45(3) . ? N3 C60 1.456(15) . ? N3 C58A 1.58(3) . ? N3 C62 1.578(16) . ? N4 C61A 1.40(4) . ? N4 C57 1.457(17) . ? N4 C59A 1.49(2) . ? N4 C59 1.491(15) . ? N4 C57A 1.54(3) . ? N4 C61 1.548(16) . ? N5 C69 1.387(13) . ? N5 C71 1.408(13) . ? N5 C70 1.415(13) . ? N6 C72 1.371(12) . ? N6 C73 1.411(17) . ? N6 C74 1.441(15) . ? N7 C75 1.344(12) . ? N7 C77 1.396(17) . ? N7 C76 1.470(19) . ? N8 C78 1.363(12) . ? N8 C80 1.414(12) . ? N8 C79 1.415(12) . ? N9 C81 1.302(16) . ? N9 C82 1.422(17) . ? N9 C83 1.434(13) . ? N10 C84 1.264(17) . ? N10 C86 1.400(14) . ? N10 C85 1.490(19) . ? N11 C87 1.376(16) . ? N11 C89 1.415(16) . ? N11 C88 1.416(16) . ? C1 C2 1.490(12) . ? C2 C3 1.386(11) . ? C2 C7 1.400(11) . ? C3 C4 1.381(14) . ? C3 H3 0.9500 . ? C4 C5 1.380(12) . ? C4 H4 0.9500 . ? C5 C6 1.376(12) . ? C6 C7 1.406(14) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.496(11) . ? C9 C10 1.406(11) . ? C9 C14 1.409(11) . ? C10 C11 1.408(12) . ? C10 H10 0.9500 . ? C11 C12 1.375(12) . ? C11 H11 0.9500 . ? C12 C13 1.398(12) . ? C13 C14 1.387(13) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.491(14) . ? C16 C17 1.398(12) . ? C16 C21 1.405(11) . ? C17 C18 1.373(15) . ? C17 H17 0.9500 . ? C18 C19 1.396(12) . ? C18 H18 0.9500 . ? C19 C20 1.389(13) . ? C20 C21 1.404(15) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.515(11) . ? C23 C24 1.382(12) . ? C23 C28 1.393(12) . ? C24 C25 1.398(13) . ? C24 H24 0.9500 . ? C25 C26 1.376(14) . ? C25 H25 0.9500 . ? C26 C27 1.383(13) . ? C27 C28 1.383(13) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.514(12) . ? C30 C31 1.382(11) . ? C30 C35 1.392(12) . ? C31 C32 1.382(13) . ? C31 H31 0.9500 . ? C32 C33 1.400(12) . ? C32 H32 0.9500 . ? C33 C34 1.373(12) . ? C34 C35 1.381(13) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.496(15) . ? C37 C42 1.386(14) . ? C37 C38 1.393(12) . ? C38 C39 1.364(15) . ? C38 H38 0.9500 . ? C39 C40 1.394(13) . ? C39 H39 0.9500 . ? C40 C41 1.400(12) . ? C41 C42 1.391(16) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.498(11) . ? C44 C45 1.383(12) . ? C44 C49 1.405(11) . ? C45 C46 1.386(13) . ? C45 H45 0.9500 . ? C46 C47 1.402(12) . ? C46 H46 0.9500 . ? C47 C48 1.378(11) . ? C48 C49 1.381(12) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 C51 1.482(12) . ? C51 C52 1.379(12) . ? C51 C56 1.413(11) . ? C52 C53 1.394(12) . ? C52 H52 0.9500 . ? C53 C54 1.409(12) . ? C53 H53 0.9500 . ? C54 C55 1.401(12) . ? C55 C56 1.382(12) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C58 1.53(2) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.543(18) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.540(19) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.549(12) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.558(11) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.549(12) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69 0.9500 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72 0.9500 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75 0.9500 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78 0.9500 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81 0.9500 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84 0.9500 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87 0.9500 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C57A C58A 1.65(4) . ? C57A H57C 0.9900 . ? C57A H57D 0.9900 . ? C58A H58C 0.9900 . ? C58A H58D 0.9900 . ? C59A C60A 1.60(4) . ? C59A H59C 0.9900 . ? C59A H59D 0.9900 . ? C60A H60C 0.9900 . ? C60A H60D 0.9900 . ? C61A C62A 1.54(5) . ? C61A H61C 0.9900 . ? C61A H61D 0.9900 . ? C62A H62C 0.9900 . ? C62A H62D 0.9900 . ? 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 O2 86.3(3) . 2_556 ? O3 Zn1 O4 156.9(2) . 2_556 ? O2 Zn1 O4 88.0(3) 2_556 2_556 ? O3 Zn1 O1 89.9(3) . . ? O2 Zn1 O1 156.8(2) 2_556 . ? O4 Zn1 O1 86.6(3) 2_556 . ? O3 Zn1 N4 99.5(2) . . ? O2 Zn1 N4 100.6(3) 2_556 . ? O4 Zn1 N4 103.5(2) 2_556 . ? O1 Zn1 N4 102.6(3) . . ? O3 Zn1 Zn1 79.63(16) . 2_556 ? O2 Zn1 Zn1 76.78(18) 2_556 2_556 ? O4 Zn1 Zn1 77.31(18) 2_556 2_556 ? O1 Zn1 Zn1 80.00(17) . 2_556 ? N4 Zn1 Zn1 177.25(19) . 2_556 ? O12 Zn2 O8 88.1(3) . . ? O12 Zn2 O6 156.5(2) . . ? O8 Zn2 O6 88.4(3) . . ? O12 Zn2 O10 87.2(3) . . ? O8 Zn2 O10 156.4(2) . . ? O6 Zn2 O10 86.7(3) . . ? O12 Zn2 N3 103.3(3) . . ? O8 Zn2 N3 100.8(3) . . ? O6 Zn2 N3 100.2(3) . . ? O10 Zn2 N3 102.7(2) . . ? O12 Zn2 Zn3 78.17(17) . . ? O8 Zn2 Zn3 80.20(17) . . ? O6 Zn2 Zn3 78.33(16) . . ? O10 Zn2 Zn3 76.25(17) . . ? N3 Zn2 Zn3 178.2(2) . . ? O9 Zn3 O7 156.6(2) . . ? O9 Zn3 O11 89.1(3) . . ? O7 Zn3 O11 88.3(3) . . ? O9 Zn3 O5 86.8(3) . . ? O7 Zn3 O5 86.7(3) . . ? O11 Zn3 O5 157.3(2) . . ? O9 Zn3 N1 105.3(2) . . ? O7 Zn3 N1 98.0(2) . . ? O11 Zn3 N1 102.9(3) . . ? O5 Zn3 N1 99.7(3) . . ? O9 Zn3 Zn2 80.55(17) . . ? O7 Zn3 Zn2 76.15(17) . . ? O11 Zn3 Zn2 78.60(17) . . ? O5 Zn3 Zn2 78.74(16) . . ? N1 Zn3 Zn2 173.95(19) . . ? O15 Zn4 O16 158.4(2) 2_667 . ? O15 Zn4 O13 87.3(3) 2_667 2_667 ? O16 Zn4 O13 87.6(3) . 2_667 ? O15 Zn4 O14 89.1(3) 2_667 . ? O16 Zn4 O14 88.0(3) . . ? O13 Zn4 O14 158.3(2) 2_667 . ? O15 Zn4 N2 100.0(3) 2_667 . ? O16 Zn4 N2 101.6(2) . . ? O13 Zn4 N2 101.9(2) 2_667 . ? O14 Zn4 N2 99.8(2) . . ? O15 Zn4 Zn4 78.16(18) 2_667 2_667 ? O16 Zn4 Zn4 80.30(17) . 2_667 ? O13 Zn4 Zn4 81.35(17) 2_667 2_667 ? O14 Zn4 Zn4 76.96(18) . 2_667 ? N2 Zn4 Zn4 176.27(18) . 2_667 ? C1 O1 Zn1 126.4(6) . . ? C1 O2 Zn1 131.6(6) . 2_556 ? C8 O3 Zn1 126.4(5) . . ? C8 O4 Zn1 129.3(6) . 2_556 ? C15 O5 Zn3 124.5(6) . . ? C15 O6 Zn2 127.2(6) . . ? C22 O7 Zn3 128.8(6) . . ? C22 O8 Zn2 123.8(5) . . ? C29 O9 Zn3 123.4(6) . . ? C29 O10 Zn2 128.6(6) . . ? C36 O11 Zn3 125.7(6) . . ? C36 O12 Zn2 127.5(6) . . ? C43 O13 Zn4 125.6(6) . 2_667 ? C43 O14 Zn4 131.0(6) . . ? C50 O15 Zn4 129.7(6) . 2_667 ? C50 O16 Zn4 126.8(6) . . ? C67 N1 C63 109.3(9) . . ? C67 N1 C65 108.1(9) . . ? C63 N1 C65 108.3(8) . . ? C67 N1 Zn3 110.1(5) . . ? C63 N1 Zn3 109.5(5) . . ? C65 N1 Zn3 111.4(5) . . ? C64 N2 C68 109.6(7) . . ? C64 N2 C66 108.4(7) . . ? C68 N2 C66 106.9(7) . . ? C64 N2 Zn4 111.1(5) . . ? C68 N2 Zn4 109.4(4) . . ? C66 N2 Zn4 111.2(4) . . ? C62A N3 C58 78.4(17) . . ? C62A N3 C60A 106.6(19) . . ? C58 N3 C60A 132.0(14) . . ? C62A N3 C60 126.3(16) . . ? C58 N3 C60 113.3(11) . . ? C60A N3 C60 26.6(11) . . ? C62A N3 C58A 111.4(18) . . ? C58 N3 C58A 35.9(11) . . ? C60A N3 C58A 106.7(16) . . ? C60 N3 C58A 82.0(13) . . ? C62A N3 C62 31.5(14) . . ? C58 N3 C62 108.2(11) . . ? C60A N3 C62 79.0(14) . . ? C60 N3 C62 103.5(11) . . ? C58A N3 C62 135.6(12) . . ? C62A N3 Zn2 112.8(14) . . ? C58 N3 Zn2 111.0(7) . . ? C60A N3 Zn2 110.3(12) . . ? C60 N3 Zn2 110.6(6) . . ? C58A N3 Zn2 108.9(10) . . ? C62 N3 Zn2 110.0(7) . . ? C61A N4 C57 81.3(18) . . ? C61A N4 C59A 108.5(19) . . ? C57 N4 C59A 128.6(13) . . ? C61A N4 C59 125.1(18) . . ? C57 N4 C59 110.7(12) . . ? C59A N4 C59 23.4(9) . . ? C61A N4 C57A 113(2) . . ? C57 N4 C57A 33.4(13) . . ? C59A N4 C57A 106.3(16) . . ? C59 N4 C57A 83.9(15) . . ? C61A N4 C61 27.8(15) . . ? C57 N4 C61 107.1(12) . . ? C59A N4 C61 84.4(12) . . ? C59 N4 C61 105.1(11) . . ? C57A N4 C61 135.5(14) . . ? C61A N4 Zn1 112.6(15) . . ? C57 N4 Zn1 112.6(7) . . ? C59A N4 Zn1 109.3(10) . . ? C59 N4 Zn1 110.8(6) . . ? C57A N4 Zn1 106.7(12) . . ? C61 N4 Zn1 110.1(6) . . ? C69 N5 C71 116.9(17) . . ? C69 N5 C70 118.0(14) . . ? C71 N5 C70 125.2(18) . . ? C72 N6 C73 118.8(13) . . ? C72 N6 C74 121.5(12) . . ? C73 N6 C74 119.5(12) . . ? C75 N7 C77 131.3(15) . . ? C75 N7 C76 118.4(14) . . ? C77 N7 C76 110.1(11) . . ? C78 N8 C80 120.2(12) . . ? C78 N8 C79 118.9(11) . . ? C80 N8 C79 120.6(12) . . ? C81 N9 C82 118.2(11) . . ? C81 N9 C83 121.9(11) . . ? C82 N9 C83 119.9(10) . . ? C84 N10 C86 130.1(15) . . ? C84 N10 C85 118.2(12) . . ? C86 N10 C85 111.7(13) . . ? C87 N11 C89 118(2) . . ? C87 N11 C88 124(2) . . ? C89 N11 C88 118.0(18) . . ? O1 C1 O2 124.6(8) . . ? O1 C1 C2 118.1(7) . . ? O2 C1 C2 117.4(7) . . ? C3 C2 C7 118.3(8) . . ? C3 C2 C1 121.7(7) . . ? C7 C2 C1 119.8(7) . . ? C4 C3 C2 121.0(8) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C5 C4 C3 120.9(8) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 119.2(9) . . ? C6 C5 I1 120.7(7) . . ? C4 C5 I1 120.2(6) . . ? C5 C6 C7 120.4(8) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C2 C7 C6 120.0(8) . . ? C2 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? O4 C8 O3 126.3(8) . . ? O4 C8 C9 117.1(7) . . ? O3 C8 C9 116.6(7) . . ? C10 C9 C14 118.6(7) . . ? C10 C9 C8 120.5(7) . . ? C14 C9 C8 120.8(7) . . ? C9 C10 C11 120.4(7) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 119.3(8) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 121.2(8) . . ? C11 C12 I2 118.7(6) . . ? C13 C12 I2 119.8(6) . . ? C14 C13 C12 119.6(8) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C9 120.5(8) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? O5 C15 O6 125.9(10) . . ? O5 C15 C16 118.6(8) . . ? O6 C15 C16 115.5(8) . . ? C17 C16 C21 119.4(9) . . ? C17 C16 C15 121.1(8) . . ? C21 C16 C15 119.3(8) . . ? C18 C17 C16 120.3(8) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 121.1(9) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 119.2(10) . . ? C20 C19 I3 120.9(7) . . ? C18 C19 I3 119.7(7) . . ? C19 C20 C21 120.4(9) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C16 119.5(8) . . ? C20 C21 H21 120.3 . . ? C16 C21 H21 120.3 . . ? O7 C22 O8 126.1(8) . . ? O7 C22 C23 116.0(7) . . ? O8 C22 C23 117.9(7) . . ? C24 C23 C28 120.2(8) . . ? C24 C23 C22 120.1(8) . . ? C28 C23 C22 119.7(8) . . ? C23 C24 C25 119.6(8) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 119.6(9) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 121.1(9) . . ? C25 C26 I4 120.7(7) . . ? C27 C26 I4 118.2(7) . . ? C28 C27 C26 119.4(8) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C23 120.1(9) . . ? C27 C28 H28 119.9 . . ? C23 C28 H28 119.9 . . ? O9 C29 O10 127.1(8) . . ? O9 C29 C30 116.1(7) . . ? O10 C29 C30 116.8(7) . . ? C31 C30 C35 118.6(8) . . ? C31 C30 C29 120.3(7) . . ? C35 C30 C29 120.8(7) . . ? C30 C31 C32 120.4(8) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 119.6(8) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C34 C33 C32 120.8(9) . . ? C34 C33 I5 118.6(7) . . ? C32 C33 I5 120.6(7) . . ? C33 C34 C35 118.5(9) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? C34 C35 C30 122.0(9) . . ? C34 C35 H35 119.0 . . ? C30 C35 H35 119.0 . . ? O11 C36 O12 125.4(10) . . ? O11 C36 C37 118.3(8) . . ? O12 C36 C37 116.3(8) . . ? C42 C37 C38 117.5(10) . . ? C42 C37 C36 120.5(8) . . ? C38 C37 C36 122.0(9) . . ? C39 C38 C37 121.3(9) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C38 C39 C40 120.5(9) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C41 119.8(10) . . ? C39 C40 I6 117.8(7) . . ? C41 C40 I6 122.3(7) . . ? C42 C41 C40 117.9(9) . . ? C42 C41 H41 121.0 . . ? C40 C41 H41 121.0 . . ? C37 C42 C41 122.6(9) . . ? C37 C42 H42 118.7 . . ? C41 C42 H42 118.7 . . ? O13 C43 O14 125.1(8) . . ? O13 C43 C44 118.0(7) . . ? O14 C43 C44 116.8(7) . . ? C45 C44 C49 119.1(8) . . ? C45 C44 C43 120.9(7) . . ? C49 C44 C43 119.9(8) . . ? C44 C45 C46 121.4(8) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C45 C46 C47 118.6(8) . . ? C45 C46 H46 120.7 . . ? C47 C46 H46 120.7 . . ? C48 C47 C46 120.4(8) . . ? C48 C47 I7 119.5(6) . . ? C46 C47 I7 120.1(6) . . ? C47 C48 C49 120.6(8) . . ? C47 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? C48 C49 C44 119.7(8) . . ? C48 C49 H49 120.2 . . ? C44 C49 H49 120.2 . . ? O15 C50 O16 124.9(8) . . ? O15 C50 C51 118.2(7) . . ? O16 C50 C51 116.9(7) . . ? C52 C51 C56 119.6(8) . . ? C52 C51 C50 119.0(7) . . ? C56 C51 C50 121.4(7) . . ? C51 C52 C53 121.1(8) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? C52 C53 C54 119.2(8) . . ? C52 C53 H53 120.4 . . ? C54 C53 H53 120.4 . . ? C55 C54 C53 119.8(8) . . ? C55 C54 I8 120.7(6) . . ? C53 C54 I8 119.5(6) . . ? C56 C55 C54 120.2(8) . . ? C56 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C55 C56 C51 120.0(8) . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? N4 C57 C58 111.5(13) . . ? N4 C57 H57A 109.3 . . ? C58 C57 H57A 109.3 . . ? N4 C57 H57B 109.3 . . ? C58 C57 H57B 109.3 . . ? H57A C57 H57B 108.0 . . ? N3 C58 C57 111.9(12) . . ? N3 C58 H58A 109.2 . . ? C57 C58 H58A 109.2 . . ? N3 C58 H58B 109.2 . . ? C57 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? N4 C59 C60 110.2(11) . . ? N4 C59 H59A 109.6 . . ? C60 C59 H59A 109.6 . . ? N4 C59 H59B 109.6 . . ? C60 C59 H59B 109.6 . . ? H59A C59 H59B 108.1 . . ? N3 C60 C59 111.6(11) . . ? N3 C60 H60A 109.3 . . ? C59 C60 H60A 109.3 . . ? N3 C60 H60B 109.3 . . ? C59 C60 H60B 109.3 . . ? H60A C60 H60B 108.0 . . ? C62 C61 N4 111.1(11) . . ? C62 C61 H61A 109.4 . . ? N4 C61 H61A 109.4 . . ? C62 C61 H61B 109.4 . . ? N4 C61 H61B 109.4 . . ? H61A C61 H61B 108.0 . . ? C61 C62 N3 108.5(11) . . ? C61 C62 H62A 110.0 . . ? N3 C62 H62A 110.0 . . ? C61 C62 H62B 110.0 . . ? N3 C62 H62B 110.0 . . ? H62A C62 H62B 108.4 . . ? N1 C63 C64 110.9(8) . . ? N1 C63 H63A 109.5 . . ? C64 C63 H63A 109.5 . . ? N1 C63 H63B 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 108.0 . . ? N2 C64 C63 110.3(7) . . ? N2 C64 H64A 109.6 . . ? C63 C64 H64A 109.6 . . ? N2 C64 H64B 109.6 . . ? C63 C64 H64B 109.6 . . ? H64A C64 H64B 108.1 . . ? N1 C65 C66 110.3(7) . . ? N1 C65 H65A 109.6 . . ? C66 C65 H65A 109.6 . . ? N1 C65 H65B 109.6 . . ? C66 C65 H65B 109.6 . . ? H65A C65 H65B 108.1 . . ? N2 C66 C65 109.8(6) . . ? N2 C66 H66A 109.7 . . ? C65 C66 H66A 109.7 . . ? N2 C66 H66B 109.7 . . ? C65 C66 H66B 109.7 . . ? H66A C66 H66B 108.2 . . ? N1 C67 C68 111.2(7) . . ? N1 C67 H67A 109.4 . . ? C68 C67 H67A 109.4 . . ? N1 C67 H67B 109.4 . . ? C68 C67 H67B 109.4 . . ? H67A C67 H67B 108.0 . . ? N2 C68 C67 109.6(7) . . ? N2 C68 H68A 109.8 . . ? C67 C68 H68A 109.8 . . ? N2 C68 H68B 109.8 . . ? C67 C68 H68B 109.8 . . ? H68A C68 H68B 108.2 . . ? O17 C69 N5 127.1(19) . . ? O17 C69 H69 116.5 . . ? N5 C69 H69 116.5 . . ? N5 C70 H70A 109.5 . . ? N5 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N5 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N5 C71 H71A 109.5 . . ? N5 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N5 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O18 C72 N6 128.7(15) . . ? O18 C72 H72 115.6 . . ? N6 C72 H72 115.6 . . ? N6 C73 H73A 109.5 . . ? N6 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? N6 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? N6 C74 H74A 109.5 . . ? N6 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? N6 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O19 C75 N7 122.9(16) . . ? O19 C75 H75 118.6 . . ? N7 C75 H75 118.6 . . ? N7 C76 H76A 109.5 . . ? N7 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? N7 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N7 C77 H77A 109.5 . . ? N7 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? N7 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? O20 C78 N8 124.6(13) . . ? O20 C78 H78 117.7 . . ? N8 C78 H78 117.7 . . ? N8 C79 H79A 109.5 . . ? N8 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? N8 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? N8 C80 H80A 109.5 . . ? N8 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? N8 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O21 C81 N9 126.1(14) . . ? O21 C81 H81 116.9 . . ? N9 C81 H81 116.9 . . ? N9 C82 H82A 109.5 . . ? N9 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N9 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N9 C83 H83A 109.5 . . ? N9 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N9 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? O22 C84 N10 129.9(14) . . ? O22 C84 H84 115.1 . . ? N10 C84 H84 115.1 . . ? N10 C85 H85A 109.5 . . ? N10 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? N10 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? N10 C86 H86A 109.5 . . ? N10 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? N10 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N11 C87 O23 113(2) . . ? N11 C87 H87 123.6 . . ? O23 C87 H87 123.6 . . ? N4 C57A C58A 107(2) . . ? N4 C57A H57C 110.4 . . ? C58A C57A H57C 110.4 . . ? N4 C57A H57D 110.4 . . ? C58A C57A H57D 110.4 . . ? H57C C57A H57D 108.6 . . ? N3 C58A C57A 108.5(19) . . ? N3 C58A H58C 110.0 . . ? C57A C58A H58C 110.0 . . ? N3 C58A H58D 110.0 . . ? C57A C58A H58D 110.0 . . ? H58C C58A H58D 108.4 . . ? N4 C59A C60A 107.8(17) . . ? N4 C59A H59C 110.1 . . ? C60A C59A H59C 110.1 . . ? N4 C59A H59D 110.1 . . ? C60A C59A H59D 110.1 . . ? H59C C59A H59D 108.5 . . ? N3 C60A C59A 111(2) . . ? N3 C60A H60C 109.3 . . ? C59A C60A H60C 109.3 . . ? N3 C60A H60D 109.3 . . ? C59A C60A H60D 109.3 . . ? H60C C60A H60D 108.0 . . ? N4 C61A C62A 112(3) . . ? N4 C61A H61C 109.3 . . ? C62A C61A H61C 109.3 . . ? N4 C61A H61D 109.3 . . ? C62A C61A H61D 109.3 . . ? H61C C61A H61D 107.9 . . ? N3 C62A C61A 113(2) . . ? N3 C62A H62C 109.0 . . ? C61A C62A H62C 109.0 . . ? N3 C62A H62D 109.0 . . ? C61A C62A H62D 109.0 . . ? H62C C62A H62D 107.8 . . ? 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 O12 Zn2 Zn3 O9 78.5(3) . . . . ? O8 Zn2 Zn3 O9 168.6(3) . . . . ? O6 Zn2 Zn3 O9 -101.0(3) . . . . ? O10 Zn2 Zn3 O9 -11.5(3) . . . . ? N3 Zn2 Zn3 O9 -67(6) . . . . ? O12 Zn2 Zn3 O7 -103.6(3) . . . . ? O8 Zn2 Zn3 O7 -13.5(3) . . . . ? O6 Zn2 Zn3 O7 76.9(3) . . . . ? O10 Zn2 Zn3 O7 166.4(3) . . . . ? N3 Zn2 Zn3 O7 111(6) . . . . ? O12 Zn2 Zn3 O11 -12.5(3) . . . . ? O8 Zn2 Zn3 O11 77.6(3) . . . . ? O6 Zn2 Zn3 O11 168.0(3) . . . . ? O10 Zn2 Zn3 O11 -102.6(3) . . . . ? N3 Zn2 Zn3 O11 -158(6) . . . . ? O12 Zn2 Zn3 O5 167.1(3) . . . . ? O8 Zn2 Zn3 O5 -102.8(3) . . . . ? O6 Zn2 Zn3 O5 -12.4(3) . . . . ? O10 Zn2 Zn3 O5 77.1(3) . . . . ? N3 Zn2 Zn3 O5 22(6) . . . . ? O12 Zn2 Zn3 N1 -117.1(19) . . . . ? O8 Zn2 Zn3 N1 -27.0(19) . . . . ? O6 Zn2 Zn3 N1 63.5(19) . . . . ? O10 Zn2 Zn3 N1 152.9(19) . . . . ? N3 Zn2 Zn3 N1 98(6) . . . . ? O3 Zn1 O1 C1 -74.3(7) . . . . ? O2 Zn1 O1 C1 6.1(12) 2_556 . . . ? O4 Zn1 O1 C1 82.9(8) 2_556 . . . ? N4 Zn1 O1 C1 -174.1(7) . . . . ? Zn1 Zn1 O1 C1 5.2(7) 2_556 . . . ? O2 Zn1 O3 C8 -71.9(8) 2_556 . . . ? O4 Zn1 O3 C8 4.1(13) 2_556 . . . ? O1 Zn1 O3 C8 85.2(8) . . . . ? N4 Zn1 O3 C8 -172.0(7) . . . . ? Zn1 Zn1 O3 C8 5.4(7) 2_556 . . . ? O9 Zn3 O5 C15 104.2(7) . . . . ? O7 Zn3 O5 C15 -53.3(7) . . . . ? O11 Zn3 O5 C15 24.2(11) . . . . ? N1 Zn3 O5 C15 -150.9(7) . . . . ? Zn2 Zn3 O5 C15 23.2(7) . . . . ? O12 Zn2 O6 C15 6.8(11) . . . . ? O8 Zn2 O6 C15 88.5(7) . . . . ? O10 Zn2 O6 C15 -68.5(7) . . . . ? N3 Zn2 O6 C15 -170.8(7) . . . . ? Zn3 Zn2 O6 C15 8.1(7) . . . . ? O9 Zn3 O7 C22 28.0(13) . . . . ? O11 Zn3 O7 C22 -55.8(8) . . . . ? O5 Zn3 O7 C22 102.1(8) . . . . ? N1 Zn3 O7 C22 -158.6(8) . . . . ? Zn2 Zn3 O7 C22 22.9(8) . . . . ? O12 Zn2 O8 C22 90.2(8) . . . . ? O6 Zn2 O8 C22 -66.5(8) . . . . ? O10 Zn2 O8 C22 11.6(13) . . . . ? N3 Zn2 O8 C22 -166.6(8) . . . . ? Zn3 Zn2 O8 C22 11.9(7) . . . . ? O7 Zn3 O9 C29 15.4(13) . . . . ? O11 Zn3 O9 C29 99.0(8) . . . . ? O5 Zn3 O9 C29 -58.6(8) . . . . ? N1 Zn3 O9 C29 -157.9(8) . . . . ? Zn2 Zn3 O9 C29 20.5(8) . . . . ? O12 Zn2 O10 C29 -69.9(9) . . . . ? O8 Zn2 O10 C29 8.9(14) . . . . ? O6 Zn2 O10 C29 87.3(9) . . . . ? N3 Zn2 O10 C29 -173.0(9) . . . . ? Zn3 Zn2 O10 C29 8.6(8) . . . . ? O9 Zn3 O11 C36 -58.8(7) . . . . ? O7 Zn3 O11 C36 98.0(7) . . . . ? O5 Zn3 O11 C36 20.8(12) . . . . ? N1 Zn3 O11 C36 -164.2(7) . . . . ? Zn2 Zn3 O11 C36 21.8(7) . . . . ? O8 Zn2 O12 C36 -70.2(8) . . . . ? O6 Zn2 O12 C36 11.5(12) . . . . ? O10 Zn2 O12 C36 86.7(8) . . . . ? N3 Zn2 O12 C36 -170.9(7) . . . . ? Zn3 Zn2 O12 C36 10.2(7) . . . . ? O15 Zn4 O14 C43 77.1(10) 2_667 . . . ? O16 Zn4 O14 C43 -81.4(10) . . . . ? O13 Zn4 O14 C43 -3.2(16) 2_667 . . . ? N2 Zn4 O14 C43 177.1(9) . . . . ? Zn4 Zn4 O14 C43 -0.9(9) 2_667 . . . ? O15 Zn4 O16 C50 -5.9(15) 2_667 . . . ? O13 Zn4 O16 C50 -82.3(8) 2_667 . . . ? O14 Zn4 O16 C50 76.5(8) . . . . ? N2 Zn4 O16 C50 176.1(8) . . . . ? Zn4 Zn4 O16 C50 -0.7(8) 2_667 . . . ? O9 Zn3 N1 C67 -120.4(8) . . . . ? O7 Zn3 N1 C67 62.3(8) . . . . ? O11 Zn3 N1 C67 -27.7(8) . . . . ? O5 Zn3 N1 C67 150.3(8) . . . . ? Zn2 Zn3 N1 C67 76(2) . . . . ? O9 Zn3 N1 C63 119.4(8) . . . . ? O7 Zn3 N1 C63 -57.9(8) . . . . ? O11 Zn3 N1 C63 -148.0(8) . . . . ? O5 Zn3 N1 C63 30.0(8) . . . . ? Zn2 Zn3 N1 C63 -45(2) . . . . ? O9 Zn3 N1 C65 -0.4(7) . . . . ? O7 Zn3 N1 C65 -177.7(7) . . . . ? O11 Zn3 N1 C65 92.2(7) . . . . ? O5 Zn3 N1 C65 -89.7(7) . . . . ? Zn2 Zn3 N1 C65 -164.5(16) . . . . ? O15 Zn4 N2 C64 -5.7(6) 2_667 . . . ? O16 Zn4 N2 C64 173.5(6) . . . . ? O13 Zn4 N2 C64 83.6(6) 2_667 . . . ? O14 Zn4 N2 C64 -96.5(6) . . . . ? Zn4 Zn4 N2 C64 -66(3) 2_667 . . . ? O15 Zn4 N2 C68 -126.9(6) 2_667 . . . ? O16 Zn4 N2 C68 52.4(7) . . . . ? O13 Zn4 N2 C68 -37.6(7) 2_667 . . . ? O14 Zn4 N2 C68 142.3(6) . . . . ? Zn4 Zn4 N2 C68 173(3) 2_667 . . . ? O15 Zn4 N2 C66 115.2(6) 2_667 . . . ? O16 Zn4 N2 C66 -65.5(6) . . . . ? O13 Zn4 N2 C66 -155.5(6) 2_667 . . . ? O14 Zn4 N2 C66 24.4(6) . . . . ? Zn4 Zn4 N2 C66 55(3) 2_667 . . . ? O12 Zn2 N3 C62A 47.4(17) . . . . ? O8 Zn2 N3 C62A -43.2(17) . . . . ? O6 Zn2 N3 C62A -133.5(17) . . . . ? O10 Zn2 N3 C62A 137.6(17) . . . . ? Zn3 Zn2 N3 C62A -168(6) . . . . ? O12 Zn2 N3 C58 133.3(10) . . . . ? O8 Zn2 N3 C58 42.7(10) . . . . ? O6 Zn2 N3 C58 -47.6(10) . . . . ? O10 Zn2 N3 C58 -136.5(10) . . . . ? Zn3 Zn2 N3 C58 -82(6) . . . . ? O12 Zn2 N3 C60A -71.6(14) . . . . ? O8 Zn2 N3 C60A -162.3(14) . . . . ? O6 Zn2 N3 C60A 107.4(14) . . . . ? O10 Zn2 N3 C60A 18.5(14) . . . . ? Zn3 Zn2 N3 C60A 73(7) . . . . ? O12 Zn2 N3 C60 -100.0(10) . . . . ? O8 Zn2 N3 C60 169.3(9) . . . . ? O6 Zn2 N3 C60 79.0(10) . . . . ? O10 Zn2 N3 C60 -9.9(10) . . . . ? Zn3 Zn2 N3 C60 45(7) . . . . ? O12 Zn2 N3 C58A 171.6(11) . . . . ? O8 Zn2 N3 C58A 81.0(11) . . . . ? O6 Zn2 N3 C58A -9.4(11) . . . . ? O10 Zn2 N3 C58A -98.3(11) . . . . ? Zn3 Zn2 N3 C58A -43(7) . . . . ? O12 Zn2 N3 C62 13.7(8) . . . . ? O8 Zn2 N3 C62 -77.0(8) . . . . ? O6 Zn2 N3 C62 -167.3(8) . . . . ? O10 Zn2 N3 C62 103.8(8) . . . . ? Zn3 Zn2 N3 C62 159(6) . . . . ? O3 Zn1 N4 C61A 47.9(18) . . . . ? O2 Zn1 N4 C61A -40.1(18) 2_556 . . . ? O4 Zn1 N4 C61A -130.5(18) 2_556 . . . ? O1 Zn1 N4 C61A 140.0(18) . . . . ? Zn1 Zn1 N4 C61A -24(4) 2_556 . . . ? O3 Zn1 N4 C57 -41.8(11) . . . . ? O2 Zn1 N4 C57 -129.8(11) 2_556 . . . ? O4 Zn1 N4 C57 139.8(11) 2_556 . . . ? O1 Zn1 N4 C57 50.3(11) . . . . ? Zn1 Zn1 N4 C57 -114(4) 2_556 . . . ? O3 Zn1 N4 C59A 168.7(11) . . . . ? O2 Zn1 N4 C59A 80.7(11) 2_556 . . . ? O4 Zn1 N4 C59A -9.8(11) 2_556 . . . ? O1 Zn1 N4 C59A -99.3(11) . . . . ? Zn1 Zn1 N4 C59A 97(4) 2_556 . . . ? O3 Zn1 N4 C59 -166.5(10) . . . . ? O2 Zn1 N4 C59 105.5(10) 2_556 . . . ? O4 Zn1 N4 C59 15.1(10) 2_556 . . . ? O1 Zn1 N4 C59 -74.4(10) . . . . ? Zn1 Zn1 N4 C59 122(4) 2_556 . . . ? O3 Zn1 N4 C57A -76.7(14) . . . . ? O2 Zn1 N4 C57A -164.8(14) 2_556 . . . ? O4 Zn1 N4 C57A 104.8(14) 2_556 . . . ? O1 Zn1 N4 C57A 15.3(14) . . . . ? Zn1 Zn1 N4 C57A -149(4) 2_556 . . . ? O3 Zn1 N4 C61 77.7(9) . . . . ? O2 Zn1 N4 C61 -10.3(9) 2_556 . . . ? O4 Zn1 N4 C61 -100.7(9) 2_556 . . . ? O1 Zn1 N4 C61 169.7(9) . . . . ? Zn1 Zn1 N4 C61 6(4) 2_556 . . . ? Zn1 O1 C1 O2 -10.3(13) . . . . ? Zn1 O1 C1 C2 168.9(6) . . . . ? Zn1 O2 C1 O1 10.2(14) 2_556 . . . ? Zn1 O2 C1 C2 -169.0(6) 2_556 . . . ? O1 C1 C2 C3 -172.1(9) . . . . ? O2 C1 C2 C3 7.2(12) . . . . ? O1 C1 C2 C7 3.6(12) . . . . ? O2 C1 C2 C7 -177.2(8) . . . . ? C7 C2 C3 C4 -0.5(14) . . . . ? C1 C2 C3 C4 175.2(9) . . . . ? C2 C3 C4 C5 -3.0(16) . . . . ? C3 C4 C5 C6 4.9(16) . . . . ? C3 C4 C5 I1 -173.7(8) . . . . ? C4 C5 C6 C7 -3.3(15) . . . . ? I1 C5 C6 C7 175.3(8) . . . . ? C3 C2 C7 C6 2.1(14) . . . . ? C1 C2 C7 C6 -173.7(9) . . . . ? C5 C6 C7 C2 -0.2(16) . . . . ? Zn1 O4 C8 O3 14.0(15) 2_556 . . . ? Zn1 O4 C8 C9 -165.2(6) 2_556 . . . ? Zn1 O3 C8 O4 -12.8(14) . . . . ? Zn1 O3 C8 C9 166.5(6) . . . . ? O4 C8 C9 C10 -3.8(13) . . . . ? O3 C8 C9 C10 176.9(9) . . . . ? O4 C8 C9 C14 173.6(9) . . . . ? O3 C8 C9 C14 -5.8(13) . . . . ? C14 C9 C10 C11 -5.8(15) . . . . ? C8 C9 C10 C11 171.7(10) . . . . ? C9 C10 C11 C12 3.6(17) . . . . ? C10 C11 C12 C13 0.7(18) . . . . ? C10 C11 C12 I2 -173.8(8) . . . . ? C11 C12 C13 C14 -2.8(17) . . . . ? I2 C12 C13 C14 171.7(8) . . . . ? C12 C13 C14 C9 0.6(16) . . . . ? C10 C9 C14 C13 3.7(15) . . . . ? C8 C9 C14 C13 -173.8(9) . . . . ? Zn3 O5 C15 O6 -26.7(12) . . . . ? Zn3 O5 C15 C16 151.9(6) . . . . ? Zn2 O6 C15 O5 6.8(13) . . . . ? Zn2 O6 C15 C16 -171.9(5) . . . . ? O5 C15 C16 C17 175.9(8) . . . . ? O6 C15 C16 C17 -5.4(12) . . . . ? O5 C15 C16 C21 -8.2(12) . . . . ? O6 C15 C16 C21 170.5(8) . . . . ? C21 C16 C17 C18 -3.8(14) . . . . ? C15 C16 C17 C18 172.2(9) . . . . ? C16 C17 C18 C19 0.5(15) . . . . ? C17 C18 C19 C20 2.3(14) . . . . ? C17 C18 C19 I3 -172.1(7) . . . . ? C18 C19 C20 C21 -1.9(14) . . . . ? I3 C19 C20 C21 172.5(7) . . . . ? C19 C20 C21 C16 -1.3(13) . . . . ? C17 C16 C21 C20 4.1(13) . . . . ? C15 C16 C21 C20 -171.8(8) . . . . ? Zn3 O7 C22 O8 -22.8(15) . . . . ? Zn3 O7 C22 C23 158.1(6) . . . . ? Zn2 O8 C22 O7 -0.1(14) . . . . ? Zn2 O8 C22 C23 179.0(6) . . . . ? O7 C22 C23 C24 173.7(9) . . . . ? O8 C22 C23 C24 -5.5(14) . . . . ? O7 C22 C23 C28 -7.7(14) . . . . ? O8 C22 C23 C28 173.1(9) . . . . ? C28 C23 C24 C25 0.0(15) . . . . ? C22 C23 C24 C25 178.6(9) . . . . ? C23 C24 C25 C26 -0.2(16) . . . . ? C24 C25 C26 C27 -1.3(17) . . . . ? C24 C25 C26 I4 -179.4(8) . . . . ? C25 C26 C27 C28 2.9(16) . . . . ? I4 C26 C27 C28 -178.9(7) . . . . ? C26 C27 C28 C23 -3.0(15) . . . . ? C24 C23 C28 C27 1.6(15) . . . . ? C22 C23 C28 C27 -176.9(9) . . . . ? Zn3 O9 C29 O10 -22.7(15) . . . . ? Zn3 O9 C29 C30 154.0(7) . . . . ? Zn2 O10 C29 O9 4.3(17) . . . . ? Zn2 O10 C29 C30 -172.3(6) . . . . ? O9 C29 C30 C31 -14.1(14) . . . . ? O10 C29 C30 C31 162.9(10) . . . . ? O9 C29 C30 C35 171.8(10) . . . . ? O10 C29 C30 C35 -11.1(15) . . . . ? C35 C30 C31 C32 1.1(16) . . . . ? C29 C30 C31 C32 -173.1(10) . . . . ? C30 C31 C32 C33 1.3(18) . . . . ? C31 C32 C33 C34 -4.3(19) . . . . ? C31 C32 C33 I5 173.8(9) . . . . ? C32 C33 C34 C35 4.8(19) . . . . ? I5 C33 C34 C35 -173.4(9) . . . . ? C33 C34 C35 C30 -2.3(19) . . . . ? C31 C30 C35 C34 -0.6(17) . . . . ? C29 C30 C35 C34 173.5(11) . . . . ? Zn3 O11 C36 O12 -23.0(13) . . . . ? Zn3 O11 C36 C37 156.2(6) . . . . ? Zn2 O12 C36 O11 2.4(13) . . . . ? Zn2 O12 C36 C37 -176.7(6) . . . . ? O11 C36 C37 C42 0.9(13) . . . . ? O12 C36 C37 C42 -179.9(9) . . . . ? O11 C36 C37 C38 -177.3(9) . . . . ? O12 C36 C37 C38 1.9(13) . . . . ? C42 C37 C38 C39 -6.4(16) . . . . ? C36 C37 C38 C39 171.9(10) . . . . ? C37 C38 C39 C40 1.3(17) . . . . ? C38 C39 C40 C41 3.5(16) . . . . ? C38 C39 C40 I6 -172.4(8) . . . . ? C39 C40 C41 C42 -3.0(14) . . . . ? I6 C40 C41 C42 172.7(7) . . . . ? C38 C37 C42 C41 6.9(15) . . . . ? C36 C37 C42 C41 -171.4(9) . . . . ? C40 C41 C42 C37 -2.3(15) . . . . ? Zn4 O13 C43 O14 1.1(15) 2_667 . . . ? Zn4 O13 C43 C44 -176.2(6) 2_667 . . . ? Zn4 O14 C43 O13 0.3(16) . . . . ? Zn4 O14 C43 C44 177.6(7) . . . . ? O13 C43 C44 C45 162.8(9) . . . . ? O14 C43 C44 C45 -14.7(13) . . . . ? O13 C43 C44 C49 -20.0(13) . . . . ? O14 C43 C44 C49 162.5(9) . . . . ? C49 C44 C45 C46 4.3(15) . . . . ? C43 C44 C45 C46 -178.6(10) . . . . ? C44 C45 C46 C47 -2.2(17) . . . . ? C45 C46 C47 C48 -0.4(15) . . . . ? C45 C46 C47 I7 177.6(8) . . . . ? C46 C47 C48 C49 0.8(14) . . . . ? I7 C47 C48 C49 -177.2(7) . . . . ? C47 C48 C49 C44 1.3(14) . . . . ? C45 C44 C49 C48 -3.8(14) . . . . ? C43 C44 C49 C48 179.0(8) . . . . ? Zn4 O15 C50 O16 5.9(15) 2_667 . . . ? Zn4 O15 C50 C51 -176.7(6) 2_667 . . . ? Zn4 O16 C50 O15 -2.4(14) . . . . ? Zn4 O16 C50 C51 -179.9(6) . . . . ? O15 C50 C51 C52 161.6(9) . . . . ? O16 C50 C51 C52 -20.8(12) . . . . ? O15 C50 C51 C56 -20.6(12) . . . . ? O16 C50 C51 C56 157.0(8) . . . . ? C56 C51 C52 C53 2.7(13) . . . . ? C50 C51 C52 C53 -179.4(8) . . . . ? C51 C52 C53 C54 -3.7(14) . . . . ? C52 C53 C54 C55 2.7(13) . . . . ? C52 C53 C54 I8 -175.3(7) . . . . ? C53 C54 C55 C56 -0.7(13) . . . . ? I8 C54 C55 C56 177.3(6) . . . . ? C54 C55 C56 C51 -0.3(13) . . . . ? C52 C51 C56 C55 -0.7(12) . . . . ? C50 C51 C56 C55 -178.5(8) . . . . ? C61A N4 C57 C58 70(2) . . . . ? C59A N4 C57 C58 -37(2) . . . . ? C59 N4 C57 C58 -54.2(19) . . . . ? C57A N4 C57 C58 -93(3) . . . . ? C61 N4 C57 C58 59.9(18) . . . . ? Zn1 N4 C57 C58 -178.9(13) . . . . ? C62A N3 C58 C57 -69(2) . . . . ? C60A N3 C58 C57 33(3) . . . . ? C60 N3 C58 C57 55.3(19) . . . . ? C58A N3 C58 C57 87(2) . . . . ? C62 N3 C58 C57 -58.8(18) . . . . ? Zn2 N3 C58 C57 -179.6(13) . . . . ? N4 C57 C58 N3 -1(2) . . . . ? C61A N4 C59 C60 -37(3) . . . . ? C57 N4 C59 C60 57.0(18) . . . . ? C59A N4 C59 C60 -87(3) . . . . ? C57A N4 C59 C60 77.2(19) . . . . ? C61 N4 C59 C60 -58.4(17) . . . . ? Zn1 N4 C59 C60 -177.3(12) . . . . ? C62A N3 C60 C59 41(3) . . . . ? C58 N3 C60 C59 -51.6(18) . . . . ? C60A N3 C60 C59 89(3) . . . . ? C58A N3 C60 C59 -69.8(17) . . . . ? C62 N3 C60 C59 65.2(17) . . . . ? Zn2 N3 C60 C59 -177.0(12) . . . . ? N4 C59 C60 N3 -5(2) . . . . ? C61A N4 C61 C62 -80(4) . . . . ? C57 N4 C61 C62 -57.4(16) . . . . ? C59A N4 C61 C62 71.3(16) . . . . ? C59 N4 C61 C62 60.4(16) . . . . ? C57A N4 C61 C62 -36(3) . . . . ? Zn1 N4 C61 C62 179.8(11) . . . . ? N4 C61 C62 N3 -0.5(18) . . . . ? C62A N3 C62 C61 79(3) . . . . ? C58 N3 C62 C61 58.9(15) . . . . ? C60A N3 C62 C61 -71.9(17) . . . . ? C60 N3 C62 C61 -61.5(15) . . . . ? C58A N3 C62 C61 31(2) . . . . ? Zn2 N3 C62 C61 -179.7(11) . . . . ? C67 N1 C63 C64 55.2(12) . . . . ? C65 N1 C63 C64 -62.4(12) . . . . ? Zn3 N1 C63 C64 176.0(8) . . . . ? C68 N2 C64 C63 -60.5(10) . . . . ? C66 N2 C64 C63 55.9(10) . . . . ? Zn4 N2 C64 C63 178.4(8) . . . . ? N1 C63 C64 N2 5.4(14) . . . . ? C67 N1 C65 C66 -62.5(11) . . . . ? C63 N1 C65 C66 55.9(11) . . . . ? Zn3 N1 C65 C66 176.4(7) . . . . ? C64 N2 C66 C65 -61.6(10) . . . . ? C68 N2 C66 C65 56.5(10) . . . . ? Zn4 N2 C66 C65 175.9(7) . . . . ? N1 C65 C66 N2 5.0(13) . . . . ? C63 N1 C67 C68 -61.7(13) . . . . ? C65 N1 C67 C68 56.0(13) . . . . ? Zn3 N1 C67 C68 177.9(9) . . . . ? C64 N2 C68 C67 54.0(11) . . . . ? C66 N2 C68 C67 -63.4(11) . . . . ? Zn4 N2 C68 C67 176.1(8) . . . . ? N1 C67 C68 N2 6.5(15) . . . . ? C71 N5 C69 O17 176.8(17) . . . . ? C70 N5 C69 O17 -3(3) . . . . ? C73 N6 C72 O18 -9(2) . . . . ? C74 N6 C72 O18 175.8(14) . . . . ? C77 N7 C75 O19 -177.0(12) . . . . ? C76 N7 C75 O19 -2.0(18) . . . . ? C80 N8 C78 O20 -174.6(13) . . . . ? C79 N8 C78 O20 -1(2) . . . . ? C82 N9 C81 O21 3(2) . . . . ? C83 N9 C81 O21 -175.3(13) . . . . ? C86 N10 C84 O22 179.5(12) . . . . ? C85 N10 C84 O22 -4(2) . . . . ? C89 N11 C87 O23 -176(2) . . . . ? C88 N11 C87 O23 0(2) . . . . ? C61A N4 C57A C58A 60(3) . . . . ? C57 N4 C57A C58A 78(3) . . . . ? C59A N4 C57A C58A -59(2) . . . . ? C59 N4 C57A C58A -66(2) . . . . ? C61 N4 C57A C58A 40(3) . . . . ? Zn1 N4 C57A C58A -175.6(16) . . . . ? C62A N3 C58A C57A -51(3) . . . . ? C58 N3 C58A C57A -76(2) . . . . ? C60A N3 C58A C57A 65(2) . . . . ? C60 N3 C58A C57A 74.6(19) . . . . ? C62 N3 C58A C57A -27(3) . . . . ? Zn2 N3 C58A C57A -176.3(16) . . . . ? N4 C57A C58A N3 -6(3) . . . . ? C61A N4 C59A C60A -51(2) . . . . ? C57 N4 C59A C60A 42(3) . . . . ? C59 N4 C59A C60A 88(3) . . . . ? C57A N4 C59A C60A 71(2) . . . . ? C61 N4 C59A C60A -65.2(18) . . . . ? Zn1 N4 C59A C60A -174.5(15) . . . . ? C62A N3 C60A C59A 63(3) . . . . ? C58 N3 C60A C59A -26(3) . . . . ? C60 N3 C60A C59A -78(3) . . . . ? C58A N3 C60A C59A -56(2) . . . . ? C62 N3 C60A C59A 79(2) . . . . ? Zn2 N3 C60A C59A -173.8(16) . . . . ? N4 C59A C60A N3 -10(3) . . . . ? C57 N4 C61A C62A -66(3) . . . . ? C59A N4 C61A C62A 62(3) . . . . ? C59 N4 C61A C62A 44(4) . . . . ? C57A N4 C61A C62A -56(3) . . . . ? C61 N4 C61A C62A 93(4) . . . . ? Zn1 N4 C61A C62A -177(2) . . . . ? C58 N3 C62A C61A 76(3) . . . . ? C60A N3 C62A C61A -55(3) . . . . ? C60 N3 C62A C61A -35(4) . . . . ? C58A N3 C62A C61A 61(3) . . . . ? C62 N3 C62A C61A -85(4) . . . . ? Zn2 N3 C62A C61A -176(2) . . . . ? N4 C61A C62A N3 -7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 6.503 _refine_diff_density_min -4.242 _refine_diff_density_rms 0.235 #===end data_compound7_k08adb29 _database_code_depnum_ccdc_archive 'CCDC 859608' #TrackingRef '- warren-pw.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H58 Cu N2 O8' _chemical_formula_weight 1046.66 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' O O 0.0106 0.0060 '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' Cu Cu 0.3201 1.2651 '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 15.6030(2) _cell_length_b 11.1260(1) _cell_length_c 29.8590(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.711(1) _cell_angle_gamma 90.00 _cell_volume 5183.09(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 41600 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.341 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2196 _exptl_absorpt_coefficient_mu 0.482 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32492 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5831 _reflns_number_gt 4877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. Asymmetric unit contains 1/2 of a copper, 1 carboxylate ligands, 1 bipy ligand and 2 solvent molecules ; _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^)+(0.0287P)^2^+7.8501P] 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 5831 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Cu1 Cu 0.5000 0.19924(2) -0.2500 0.01720(9) Uani 1 2 d S . . O1 O 0.50783(7) 0.19179(10) -0.31543(4) 0.0199(2) Uani 1 1 d . . . N1 N 0.5000 0.01960(17) -0.2500 0.0172(4) Uani 1 2 d S . . C1 C 0.56348(11) 0.24219(15) -0.33995(6) 0.0199(3) Uani 1 1 d . . . O2 O 0.62929(8) 0.29471(12) -0.32562(4) 0.0277(3) Uani 1 1 d . . . N2 N 0.5000 -0.61901(16) -0.2500 0.0156(4) Uani 1 2 d S . . C2 C 0.54540(10) 0.23917(15) -0.38960(5) 0.0194(3) Uani 1 1 d . . . O3 O 0.66240(8) 0.18859(12) -0.24608(4) 0.0303(3) Uani 1 1 d . . . H3A H 0.6625 0.2298 -0.2696 0.036 Uiso 1 1 calc R . . C3 C 0.58609(11) 0.32086(16) -0.41737(6) 0.0228(4) Uani 1 1 d . . . H3 H 0.6273 0.3746 -0.4050 0.027 Uiso 1 1 calc R . . O4 O 0.78541(10) 0.40035(18) -0.34447(5) 0.0529(5) Uani 1 1 d . . . H4A H 0.7349 0.3768 -0.3407 0.063 Uiso 1 1 calc R . . C4 C 0.56734(11) 0.32500(16) -0.46283(6) 0.0239(4) Uani 1 1 d . . . H4 H 0.5958 0.3817 -0.4812 0.029 Uiso 1 1 calc R . . C5 C 0.50711(10) 0.24696(15) -0.48212(6) 0.0204(3) Uani 1 1 d . . . C6 C 0.46732(11) 0.16329(16) -0.45398(6) 0.0228(4) Uani 1 1 d . . . H6 H 0.4267 0.1085 -0.4663 0.027 Uiso 1 1 calc R . . C7 C 0.48643(11) 0.15938(15) -0.40843(6) 0.0217(3) Uani 1 1 d . . . H7 H 0.4590 0.1018 -0.3900 0.026 Uiso 1 1 calc R . . C8 C 0.48516(11) 0.25331(16) -0.53080(6) 0.0218(3) Uani 1 1 d . . . C9 C 0.49465(12) 0.35976(18) -0.55477(6) 0.0284(4) Uani 1 1 d . . . H9 H 0.5170 0.4289 -0.5401 0.034 Uiso 1 1 calc R . . C10 C 0.47185(13) 0.36656(19) -0.59995(6) 0.0323(4) Uani 1 1 d . . . H10 H 0.4791 0.4398 -0.6158 0.039 Uiso 1 1 calc R . . C11 C 0.43883(12) 0.2672(2) -0.62176(6) 0.0334(5) Uani 1 1 d . . . H11 H 0.4223 0.2723 -0.6524 0.040 Uiso 1 1 calc R . . C12 C 0.42993(12) 0.15989(19) -0.59874(6) 0.0319(4) Uani 1 1 d . . . H12 H 0.4078 0.0910 -0.6137 0.038 Uiso 1 1 calc R . . C13 C 0.45327(12) 0.15279(18) -0.55371(6) 0.0269(4) Uani 1 1 d . . . H13 H 0.4475 0.0786 -0.5383 0.032 Uiso 1 1 calc R . . C14 C 0.44912(11) -0.04260(15) -0.27810(5) 0.0192(3) Uani 1 1 d . . . H14 H 0.4130 0.0005 -0.2983 0.023 Uiso 1 1 calc R . . C15 C 0.44693(11) -0.16662(14) -0.27899(5) 0.0191(3) Uani 1 1 d . . . H15 H 0.4095 -0.2072 -0.2992 0.023 Uiso 1 1 calc R . . C16 C 0.5000 -0.2320(2) -0.2500 0.0162(4) Uani 1 2 d S . . C17 C 0.5000 -0.3661(2) -0.2500 0.0165(4) Uani 1 2 d S . . C18 C 0.46069(11) -0.43199(15) -0.28415(5) 0.0205(3) Uani 1 1 d . . . H18 H 0.4328 -0.3915 -0.3082 0.025 Uiso 1 1 calc R . . C19 C 0.46213(11) -0.55610(15) -0.28312(5) 0.0203(3) Uani 1 1 d . . . H19 H 0.4351 -0.5989 -0.3069 0.024 Uiso 1 1 calc R . . C20 C 0.74032(13) 0.2086(2) -0.22156(7) 0.0381(5) Uani 1 1 d . . . H20A H 0.7865 0.2288 -0.2427 0.046 Uiso 1 1 calc R . . H20B H 0.7569 0.1337 -0.2058 0.046 Uiso 1 1 calc R . . C21 C 0.73185(12) 0.30839(18) -0.18798(7) 0.0303(4) Uani 1 1 d . . . C22 C 0.76355(13) 0.4238(2) -0.19565(7) 0.0364(5) Uani 1 1 d . . . H22 H 0.7947 0.4400 -0.2221 0.044 Uiso 1 1 calc R . . C23 C 0.74991(14) 0.51480(19) -0.16490(8) 0.0407(5) Uani 1 1 d . . . H23 H 0.7723 0.5928 -0.1702 0.049 Uiso 1 1 calc R . . C24 C 0.70385(14) 0.4927(2) -0.12655(7) 0.0402(5) Uani 1 1 d . . . H24 H 0.6941 0.5556 -0.1057 0.048 Uiso 1 1 calc R . . C25 C 0.67207(14) 0.3790(2) -0.11858(7) 0.0363(5) Uani 1 1 d . . . H25 H 0.6402 0.3636 -0.0923 0.044 Uiso 1 1 calc R . . C26 C 0.68666(12) 0.28779(18) -0.14881(7) 0.0318(4) Uani 1 1 d . . . H26 H 0.6655 0.2095 -0.1428 0.038 Uiso 1 1 calc R . . C27 C 0.81619(14) 0.3549(2) -0.38537(8) 0.0484(6) Uani 1 1 d . . . H27A H 0.7940 0.2723 -0.3895 0.058 Uiso 1 1 calc R . . H27B H 0.8795 0.3499 -0.3834 0.058 Uiso 1 1 calc R . . C28 C 0.79195(11) 0.42838(17) -0.42616(6) 0.0261(4) Uani 1 1 d . . . C29 C 0.75255(11) 0.53905(17) -0.42267(7) 0.0299(4) Uani 1 1 d . . . H29 H 0.7398 0.5709 -0.3940 0.036 Uiso 1 1 calc R . . C30 C 0.73162(13) 0.60381(19) -0.46098(8) 0.0403(5) Uani 1 1 d . . . H30 H 0.7044 0.6798 -0.4585 0.048 Uiso 1 1 calc R . . C31 C 0.75023(14) 0.5582(2) -0.50273(8) 0.0461(6) Uani 1 1 d . . . H31 H 0.7364 0.6031 -0.5289 0.055 Uiso 1 1 calc R . . C32 C 0.78888(14) 0.4476(2) -0.50638(7) 0.0433(6) Uani 1 1 d . . . H32 H 0.8016 0.4160 -0.5351 0.052 Uiso 1 1 calc R . . C33 C 0.80908(12) 0.38284(19) -0.46849(7) 0.0344(5) Uani 1 1 d . . . H33 H 0.8351 0.3060 -0.4712 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02579(16) 0.00943(14) 0.01645(14) 0.000 0.00257(11) 0.000 O1 0.0272(6) 0.0158(6) 0.0168(5) -0.0003(5) 0.0025(5) -0.0022(5) N1 0.0213(10) 0.0116(9) 0.0186(9) 0.000 0.0015(7) 0.000 C1 0.0240(8) 0.0141(8) 0.0217(8) -0.0003(7) 0.0038(7) 0.0025(6) O2 0.0266(6) 0.0342(7) 0.0224(6) 0.0005(6) 0.0000(5) -0.0081(5) N2 0.0204(9) 0.0110(9) 0.0153(9) 0.000 0.0020(7) 0.000 C2 0.0203(8) 0.0187(8) 0.0192(8) -0.0006(7) 0.0024(6) 0.0023(6) O3 0.0292(7) 0.0350(8) 0.0266(7) 0.0028(6) -0.0014(5) -0.0058(6) C3 0.0226(8) 0.0221(9) 0.0238(8) 0.0002(7) 0.0023(7) -0.0037(7) O4 0.0331(8) 0.0932(14) 0.0322(8) 0.0152(9) -0.0061(6) -0.0225(8) C4 0.0253(9) 0.0229(9) 0.0236(8) 0.0029(7) 0.0046(7) -0.0039(7) C5 0.0206(8) 0.0211(8) 0.0197(8) 0.0000(7) 0.0032(6) 0.0029(6) C6 0.0243(9) 0.0205(9) 0.0236(8) -0.0019(7) 0.0018(7) -0.0030(7) C7 0.0261(9) 0.0171(8) 0.0219(8) 0.0009(7) 0.0048(7) -0.0019(7) C8 0.0192(8) 0.0263(9) 0.0199(8) -0.0003(7) 0.0037(6) 0.0032(7) C9 0.0328(10) 0.0273(10) 0.0253(9) 0.0003(8) 0.0035(7) 0.0032(8) C10 0.0383(11) 0.0342(11) 0.0243(9) 0.0074(8) 0.0048(8) 0.0076(8) C11 0.0307(10) 0.0495(13) 0.0199(9) 0.0008(8) 0.0005(7) 0.0065(9) C12 0.0300(10) 0.0397(11) 0.0259(9) -0.0053(8) -0.0002(8) -0.0028(8) C13 0.0276(9) 0.0289(10) 0.0244(9) -0.0006(8) 0.0022(7) -0.0007(7) C14 0.0242(8) 0.0142(8) 0.0192(8) 0.0012(6) -0.0014(6) 0.0017(6) C15 0.0237(8) 0.0136(8) 0.0199(8) -0.0016(6) -0.0036(6) -0.0004(6) C16 0.0190(11) 0.0131(11) 0.0166(10) 0.000 0.0012(8) 0.000 C17 0.0188(11) 0.0127(11) 0.0180(11) 0.000 0.0016(9) 0.000 C18 0.0266(9) 0.0152(8) 0.0196(8) 0.0014(6) -0.0061(7) 0.0012(6) C19 0.0285(9) 0.0140(8) 0.0184(8) -0.0016(6) -0.0044(7) -0.0016(6) C20 0.0282(10) 0.0422(12) 0.0436(12) -0.0036(10) -0.0071(9) 0.0042(9) C21 0.0228(9) 0.0341(11) 0.0338(10) 0.0050(9) -0.0084(7) -0.0012(8) C22 0.0306(10) 0.0417(12) 0.0369(11) 0.0113(10) -0.0011(8) -0.0067(9) C23 0.0416(12) 0.0294(11) 0.0509(13) 0.0094(10) -0.0110(10) -0.0115(9) C24 0.0466(13) 0.0382(12) 0.0353(11) -0.0018(9) -0.0134(9) -0.0044(10) C25 0.0394(11) 0.0428(12) 0.0266(10) 0.0070(9) -0.0064(8) -0.0056(9) C26 0.0308(10) 0.0309(10) 0.0333(10) 0.0101(8) -0.0107(8) -0.0058(8) C27 0.0328(11) 0.0610(16) 0.0514(14) 0.0249(12) 0.0023(10) 0.0066(10) C28 0.0173(8) 0.0284(10) 0.0329(10) 0.0047(8) 0.0018(7) -0.0030(7) C29 0.0230(9) 0.0279(10) 0.0388(11) -0.0043(8) 0.0046(8) -0.0055(7) C30 0.0255(10) 0.0272(11) 0.0682(16) 0.0127(10) -0.0024(10) -0.0001(8) C31 0.0355(12) 0.0606(16) 0.0418(12) 0.0236(12) -0.0128(10) -0.0148(11) C32 0.0394(12) 0.0609(16) 0.0298(11) -0.0046(10) 0.0033(9) -0.0166(11) C33 0.0267(10) 0.0329(11) 0.0437(12) -0.0051(9) 0.0085(8) -0.0026(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 Cu1 O1 1.9609(11) . ? Cu1 O1 1.9609(11) 2_654 ? Cu1 N1 1.9986(19) . ? Cu1 N2 2.0222(18) 1_565 ? O1 C1 1.273(2) . ? N1 C14 1.3404(19) . ? N1 C14 1.3404(19) 2_654 ? C1 O2 1.252(2) . ? C1 C2 1.506(2) . ? N2 C19 1.3426(18) . ? N2 C19 1.3426(18) 2_654 ? N2 Cu1 2.0222(18) 1_545 ? C2 C3 1.389(2) . ? C2 C7 1.392(2) . ? O3 C20 1.429(2) . ? O3 H3A 0.8400 . ? C3 C4 1.386(2) . ? C3 H3 0.9500 . ? O4 C27 1.411(3) . ? O4 H4A 0.8400 . ? C4 C5 1.398(2) . ? C4 H4 0.9500 . ? C5 C6 1.404(2) . ? C5 C8 1.491(2) . ? C6 C7 1.389(2) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.393(3) . ? C8 C13 1.399(3) . ? C9 C10 1.393(3) . ? C9 H9 0.9500 . ? C10 C11 1.380(3) . ? C10 H10 0.9500 . ? C11 C12 1.385(3) . ? C11 H11 0.9500 . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.381(2) . ? C14 H14 0.9500 . ? C15 C16 1.395(2) . ? C15 H15 0.9500 . ? C16 C15 1.395(2) 2_654 ? C16 C17 1.492(3) . ? C17 C18 1.392(2) . ? C17 C18 1.392(2) 2_654 ? C18 C19 1.381(2) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.503(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C26 1.392(3) . ? C21 C22 1.396(3) . ? C22 C23 1.385(3) . ? C22 H22 0.9500 . ? C23 C24 1.381(3) . ? C23 H23 0.9500 . ? C24 C25 1.380(3) . ? C24 H24 0.9500 . ? C25 C26 1.379(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.511(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.381(3) . ? C28 C33 1.390(3) . ? C29 C30 1.387(3) . ? C29 H29 0.9500 . ? C30 C31 1.380(3) . ? C30 H30 0.9500 . ? C31 C32 1.375(4) . ? C31 H31 0.9500 . ? C32 C33 1.375(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? 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 Cu1 O1 175.15(7) . 2_654 ? O1 Cu1 N1 87.58(3) . . ? O1 Cu1 N1 87.58(3) 2_654 . ? O1 Cu1 N2 92.42(3) . 1_565 ? O1 Cu1 N2 92.42(3) 2_654 1_565 ? N1 Cu1 N2 180.0 . 1_565 ? C1 O1 Cu1 127.29(11) . . ? C14 N1 C14 117.83(19) . 2_654 ? C14 N1 Cu1 121.09(10) . . ? C14 N1 Cu1 121.09(10) 2_654 . ? O2 C1 O1 124.84(16) . . ? O2 C1 C2 119.31(15) . . ? O1 C1 C2 115.82(15) . . ? C19 N2 C19 117.16(19) . 2_654 ? C19 N2 Cu1 121.42(10) . 1_545 ? C19 N2 Cu1 121.42(9) 2_654 1_545 ? C3 C2 C7 118.74(15) . . ? C3 C2 C1 119.44(15) . . ? C7 C2 C1 121.78(15) . . ? C20 O3 H3A 109.5 . . ? C4 C3 C2 120.93(16) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C27 O4 H4A 109.5 . . ? C3 C4 C5 121.03(16) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 117.72(15) . . ? C4 C5 C8 121.15(15) . . ? C6 C5 C8 121.12(16) . . ? C7 C6 C5 121.02(16) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C2 120.54(16) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C9 C8 C13 117.90(16) . . ? C9 C8 C5 121.12(16) . . ? C13 C8 C5 120.98(16) . . ? C8 C9 C10 121.09(19) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C11 C10 C9 120.19(19) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 119.71(18) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 120.13(19) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C8 120.95(18) . . ? C12 C13 H13 119.5 . . ? C8 C13 H13 119.5 . . ? N1 C14 C15 122.85(16) . . ? N1 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? C14 C15 C16 119.67(16) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C15 117.1(2) . 2_654 ? C15 C16 C17 121.44(10) . . ? C15 C16 C17 121.44(10) 2_654 . ? C18 C17 C18 116.5(2) . 2_654 ? C18 C17 C16 121.77(10) . . ? C18 C17 C16 121.77(10) 2_654 . ? C19 C18 C17 120.21(16) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? N2 C19 C18 122.98(15) . . ? N2 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? O3 C20 C21 112.05(16) . . ? O3 C20 H20A 109.2 . . ? C21 C20 H20A 109.2 . . ? O3 C20 H20B 109.2 . . ? C21 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C26 C21 C22 118.25(19) . . ? C26 C21 C20 119.24(18) . . ? C22 C21 C20 122.41(19) . . ? C23 C22 C21 120.41(19) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.3(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 119.9(2) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 119.9(2) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 121.21(19) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? O4 C27 C28 114.8(2) . . ? O4 C27 H27A 108.6 . . ? C28 C27 H27A 108.6 . . ? O4 C27 H27B 108.6 . . ? C28 C27 H27B 108.6 . . ? H27A C27 H27B 107.5 . . ? C29 C28 C33 118.97(18) . . ? C29 C28 C27 121.92(19) . . ? C33 C28 C27 119.11(19) . . ? C28 C29 C30 120.09(19) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 120.2(2) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 119.9(2) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C33 C32 C31 120.0(2) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C28 120.8(2) . . ? C32 C33 H33 119.6 . . ? C28 C33 H33 119.6 . . ? 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 O1 Cu1 O1 C1 -125.91(13) 2_654 . . . ? N1 Cu1 O1 C1 -125.91(13) . . . . ? N2 Cu1 O1 C1 54.09(13) 1_565 . . . ? O1 Cu1 N1 C14 -47.33(9) . . . . ? O1 Cu1 N1 C14 132.67(9) 2_654 . . . ? N2 Cu1 N1 C14 -133(100) 1_565 . . . ? O1 Cu1 N1 C14 132.67(9) . . . 2_654 ? O1 Cu1 N1 C14 -47.33(9) 2_654 . . 2_654 ? N2 Cu1 N1 C14 47(100) 1_565 . . 2_654 ? Cu1 O1 C1 O2 8.7(2) . . . . ? Cu1 O1 C1 C2 -169.72(10) . . . . ? O2 C1 C2 C3 -18.3(2) . . . . ? O1 C1 C2 C3 160.20(15) . . . . ? O2 C1 C2 C7 164.08(16) . . . . ? O1 C1 C2 C7 -17.4(2) . . . . ? C7 C2 C3 C4 1.3(3) . . . . ? C1 C2 C3 C4 -176.36(16) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C3 C4 C5 C6 -0.9(3) . . . . ? C3 C4 C5 C8 178.41(16) . . . . ? C4 C5 C6 C7 0.8(3) . . . . ? C8 C5 C6 C7 -178.50(16) . . . . ? C5 C6 C7 C2 0.3(3) . . . . ? C3 C2 C7 C6 -1.4(3) . . . . ? C1 C2 C7 C6 176.22(15) . . . . ? C4 C5 C8 C9 -25.9(2) . . . . ? C6 C5 C8 C9 153.34(17) . . . . ? C4 C5 C8 C13 154.91(17) . . . . ? C6 C5 C8 C13 -25.8(2) . . . . ? C13 C8 C9 C10 1.0(3) . . . . ? C5 C8 C9 C10 -178.17(16) . . . . ? C8 C9 C10 C11 0.3(3) . . . . ? C9 C10 C11 C12 -1.2(3) . . . . ? C10 C11 C12 C13 0.7(3) . . . . ? C11 C12 C13 C8 0.6(3) . . . . ? C9 C8 C13 C12 -1.5(3) . . . . ? C5 C8 C13 C12 177.69(16) . . . . ? C14 N1 C14 C15 0.32(12) 2_654 . . . ? Cu1 N1 C14 C15 -179.68(12) . . . . ? N1 C14 C15 C16 -0.6(2) . . . . ? C14 C15 C16 C15 0.30(11) . . . 2_654 ? C14 C15 C16 C17 -179.70(11) . . . . ? C15 C16 C17 C18 12.86(12) . . . . ? C15 C16 C17 C18 -167.15(12) 2_654 . . . ? C15 C16 C17 C18 -167.14(12) . . . 2_654 ? C15 C16 C17 C18 12.86(12) 2_654 . . 2_654 ? C18 C17 C18 C19 -0.17(12) 2_654 . . . ? C16 C17 C18 C19 179.83(12) . . . . ? C19 N2 C19 C18 -0.18(12) 2_654 . . . ? Cu1 N2 C19 C18 179.82(12) 1_545 . . . ? C17 C18 C19 N2 0.4(2) . . . . ? O3 C20 C21 C26 74.6(2) . . . . ? O3 C20 C21 C22 -101.7(2) . . . . ? C26 C21 C22 C23 -0.1(3) . . . . ? C20 C21 C22 C23 176.23(18) . . . . ? C21 C22 C23 C24 -0.8(3) . . . . ? C22 C23 C24 C25 0.7(3) . . . . ? C23 C24 C25 C26 0.3(3) . . . . ? C24 C25 C26 C21 -1.2(3) . . . . ? C22 C21 C26 C25 1.1(3) . . . . ? C20 C21 C26 C25 -175.35(18) . . . . ? O4 C27 C28 C29 8.1(3) . . . . ? O4 C27 C28 C33 -171.36(18) . . . . ? C33 C28 C29 C30 -0.8(3) . . . . ? C27 C28 C29 C30 179.77(18) . . . . ? C28 C29 C30 C31 -0.2(3) . . . . ? C29 C30 C31 C32 0.7(3) . . . . ? C30 C31 C32 C33 -0.2(3) . . . . ? C31 C32 C33 C28 -0.8(3) . . . . ? C29 C28 C33 C32 1.3(3) . . . . ? C27 C28 C33 C32 -179.24(19) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.334 _refine_diff_density_min -0.701 _refine_diff_density_rms 0.103 #===end data_compound8_h08adb16 _database_code_depnum_ccdc_archive 'CCDC 859609' #TrackingRef '- warren-pw.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H52 N4 O8 Zn2' _chemical_formula_weight 1231.92 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' O O 0.0106 0.0060 '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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 25.7330(6) _cell_length_b 13.5820(3) _cell_length_c 17.2990(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.939(1) _cell_angle_gamma 90.00 _cell_volume 5783.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 34276 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Tabloid _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.893 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51278 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.0895 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.80 _diffrn_reflns_theta_max 27.49 _reflns_number_total 13211 _reflns_number_gt 8592 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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. The only ambiguity regarding this structure concerns the chelating carboxylate groups attached to Zn1. The ADPs of the atoms concerned are larger than those for the remaining atoms in the asymmetric unit. Moreover, the residual maxima in the difference Fourier electron density map are in this region. This indicates some disorder within these groups. However, efforts to refine a model wherein the carboxylates might be disordered between monodentate and bidentate coordination to the metal proved unsuccessful. ; _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^)+(0.0769P)^2^+1.4716P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.011(12) _refine_ls_number_reflns 13211 _refine_ls_number_parameters 776 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.74527(2) 0.86813(4) 0.49855(3) 0.03568(16) Uani 1 1 d . . . Zn2 Zn 0.758030(19) 1.38706(3) 0.00218(3) 0.03284(15) Uani 1 1 d . . . N1 N 0.74091(15) 0.9630(3) 0.5894(2) 0.0351(9) Uani 1 1 d . . . N3 N 0.75305(15) 0.9669(3) 0.4112(2) 0.0361(9) Uani 1 1 d . . . N4 N 0.75948(15) 1.2950(3) 0.0975(2) 0.0329(9) Uani 1 1 d . . . O5 O 0.69144(14) 1.4578(2) -0.04392(18) 0.0465(9) Uani 1 1 d . . . O7 O 0.82501(13) 1.4570(2) 0.05181(19) 0.0424(8) Uani 1 1 d . . . C47 C 0.67394(18) 1.5061(3) 0.0072(3) 0.0358(10) Uani 1 1 d . . . O6 O 0.69198(14) 1.4964(2) 0.0811(2) 0.0496(9) Uani 1 1 d . . . C62 C 0.89833(19) 1.6529(3) -0.0120(3) 0.0351(11) Uani 1 1 d . . . H62 H 0.8816 1.6497 -0.0686 0.042 Uiso 1 1 calc R . . O8 O 0.81909(14) 1.5098(3) -0.0717(2) 0.0505(9) Uani 1 1 d . . . C48 C 0.62999(17) 1.5795(3) -0.0281(3) 0.0335(10) Uani 1 1 d . . . C52 C 0.57770(18) 1.7203(3) -0.0090(3) 0.0381(11) Uani 1 1 d . . . H52 H 0.5700 1.7688 0.0256 0.046 Uiso 1 1 calc R . . C63 C 0.93704(17) 1.7252(3) 0.0196(3) 0.0351(10) Uani 1 1 d . . . H63 H 0.9458 1.7720 -0.0155 0.042 Uiso 1 1 calc R . . C60 C 0.84008(19) 1.5125(3) 0.0015(3) 0.0378(11) Uani 1 1 d . . . C59 C 0.50928(17) 1.8895(4) -0.0936(3) 0.0402(10) Uani 1 1 d . . . H59 H 0.5413 1.9085 -0.0529 0.048 Uiso 1 1 calc R . . C53 C 0.6167(2) 1.6510(3) 0.0214(3) 0.0374(11) Uani 1 1 d . . . H53 H 0.6353 1.6512 0.0776 0.045 Uiso 1 1 calc R . . C66 C 0.90918(19) 1.5900(4) 0.1213(3) 0.0386(11) Uani 1 1 d . . . H66 H 0.8996 1.5443 0.1564 0.046 Uiso 1 1 calc R . . C38 C 0.7972(2) 1.1048(3) 0.3707(3) 0.0440(12) Uani 1 1 d . . . H38 H 0.8247 1.1538 0.3846 0.053 Uiso 1 1 calc R . . C61 C 0.88398(17) 1.5860(3) 0.0382(3) 0.0316(10) Uani 1 1 d . . . C15 C 0.7246(2) 1.1213(3) 0.6353(3) 0.0424(12) Uani 1 1 d . . . H15 H 0.7141 1.1878 0.6224 0.051 Uiso 1 1 calc R . . C68 C 1.00236(18) 1.8990(3) 0.1007(2) 0.0385(10) Uani 1 1 d . . . H68 H 0.9700 1.9175 0.0605 0.046 Uiso 1 1 calc R . . C54 C 0.50535(18) 1.7937(3) -0.1248(3) 0.0368(10) Uani 1 1 d . . . C39 C 0.76163(18) 1.0999(3) 0.2924(3) 0.0338(10) Uani 1 1 d . . . C67 C 1.00591(18) 1.8050(3) 0.1348(3) 0.0352(10) Uani 1 1 d . . . C56 C 0.4167(2) 1.8370(5) -0.2122(3) 0.0586(17) Uani 1 1 d . . . H56 H 0.3848 1.8196 -0.2539 0.070 Uiso 1 1 calc R . . C28 C 0.5194(2) 0.5765(4) 0.3719(3) 0.0424(12) Uani 1 1 d . . . C58 C 0.4682(2) 1.9565(4) -0.1201(3) 0.0478(12) Uani 1 1 d . . . H58 H 0.4716 2.0209 -0.0979 0.057 Uiso 1 1 calc R . . C49 C 0.60197(18) 1.5799(4) -0.1098(3) 0.0370(11) Uani 1 1 d . . . H49 H 0.6105 1.5324 -0.1446 0.044 Uiso 1 1 calc R . . C37 C 0.7917(2) 1.0372(4) 0.4272(3) 0.0449(12) Uani 1 1 d . . . H37 H 0.8164 1.0403 0.4800 0.054 Uiso 1 1 calc R . . C16 C 0.7373(2) 1.0899(4) 0.7144(3) 0.0378(11) Uani 1 1 d . . . C46 C 0.7161(2) 1.2168(3) 0.1844(3) 0.0399(11) Uani 1 1 d . . . H46 H 0.6836 1.2057 0.1986 0.048 Uiso 1 1 calc R . . C50 C 0.56182(19) 1.6487(4) -0.1409(3) 0.0367(12) Uani 1 1 d . . . H50 H 0.5427 1.6475 -0.1969 0.044 Uiso 1 1 calc R . . C27 C 0.5676(2) 0.5490(4) 0.3567(3) 0.0494(13) Uani 1 1 d . . . H27 H 0.5708 0.4860 0.3347 0.059 Uiso 1 1 calc R . . C14 C 0.7272(2) 1.0574(4) 0.5749(3) 0.0465(12) Uani 1 1 d . . . H14 H 0.7189 1.0812 0.5210 0.056 Uiso 1 1 calc R . . C69 C 1.0443(2) 1.9651(4) 0.1237(3) 0.0475(13) Uani 1 1 d . . . H69 H 1.0410 2.0282 0.0991 0.057 Uiso 1 1 calc R . . C42 C 0.76308(18) 1.1705(3) 0.2269(3) 0.0314(10) Uani 1 1 d . . . C18 C 0.75167(19) 0.9297(3) 0.6657(2) 0.0388(11) Uani 1 1 d . . . H18 H 0.7607 0.8623 0.6764 0.047 Uiso 1 1 calc R . . C65 C 0.94861(19) 1.6617(4) 0.1524(3) 0.0363(11) Uani 1 1 d . . . H65 H 0.9657 1.6638 0.2090 0.044 Uiso 1 1 calc R . . C70 C 1.0912(2) 1.9399(4) 0.1829(3) 0.0524(14) Uani 1 1 d . . . H70 H 1.1206 1.9851 0.1986 0.063 Uiso 1 1 calc R . . C72 C 1.05354(18) 1.7820(4) 0.1963(3) 0.0404(11) Uani 1 1 d . . . H72 H 1.0569 1.7197 0.2223 0.049 Uiso 1 1 calc R . . C55 C 0.45777(19) 1.7689(4) -0.1852(3) 0.0471(13) Uani 1 1 d . . . H55 H 0.4537 1.7046 -0.2077 0.057 Uiso 1 1 calc R . . C17 C 0.74998(19) 0.9901(3) 0.7285(3) 0.0384(11) Uani 1 1 d . . . H17 H 0.7575 0.9641 0.7816 0.046 Uiso 1 1 calc R . . C11 C 1.1060(2) 0.3817(5) 0.6597(4) 0.0643(15) Uani 1 1 d . . . H11 H 1.1340 0.3340 0.6666 0.077 Uiso 1 1 calc R . . C71 C 1.0953(2) 1.8486(4) 0.2190(3) 0.0518(16) Uani 1 1 d . . . H71 H 1.1274 1.8316 0.2602 0.062 Uiso 1 1 calc R . . C5 C 0.9763(2) 0.5905(4) 0.6240(3) 0.0435(12) Uani 1 1 d . . . C44 C 0.8063(2) 1.2515(4) 0.1406(3) 0.0453(12) Uani 1 1 d . . . H44 H 0.8385 1.2651 0.1262 0.054 Uiso 1 1 calc R . . C6 C 0.9260(2) 0.5589(4) 0.6299(3) 0.0490(13) Uani 1 1 d . . . H6 H 0.9216 0.4935 0.6464 0.059 Uiso 1 1 calc R . . C43 C 0.80953(19) 1.1892(4) 0.2037(3) 0.0425(11) Uani 1 1 d . . . H43 H 0.8431 1.1590 0.2315 0.051 Uiso 1 1 calc R . . C8 C 1.0230(2) 0.5196(4) 0.6390(3) 0.0432(11) Uani 1 1 d . . . C57 C 0.4216(2) 1.9294(5) -0.1795(3) 0.0579(16) Uani 1 1 d . . . H57 H 0.3927 1.9753 -0.1977 0.069 Uiso 1 1 calc R . . C51 C 0.54892(17) 1.7196(3) -0.0917(3) 0.0333(10) Uani 1 1 d . . . C40 C 0.72281(19) 1.0274(4) 0.2761(3) 0.0398(11) Uani 1 1 d . . . H40 H 0.6984 1.0215 0.2232 0.048 Uiso 1 1 calc R . . C31 C 0.4731(2) 0.5041(4) 0.3542(3) 0.0437(12) Uani 1 1 d . . . C64 C 0.96337(17) 1.7293(3) 0.1037(3) 0.0342(10) Uani 1 1 d . . . C26 C 0.6106(2) 0.6135(4) 0.3738(3) 0.0526(14) Uani 1 1 d . . . H26 H 0.6429 0.5954 0.3613 0.063 Uiso 1 1 calc R . . C45 C 0.71542(19) 1.2791(3) 0.1212(3) 0.0375(11) Uani 1 1 d . . . H45 H 0.6826 1.3118 0.0939 0.045 Uiso 1 1 calc R . . C7 C 0.8821(2) 0.6239(5) 0.6112(3) 0.0531(15) Uani 1 1 d . . . H7 H 0.8479 0.6021 0.6152 0.064 Uiso 1 1 calc R . . C33 C 0.4196(2) 0.3773(5) 0.2699(3) 0.0570(13) Uani 1 1 d . . . H33 H 0.4112 0.3396 0.2215 0.068 Uiso 1 1 calc R . . C2 C 0.8872(2) 0.7188(4) 0.5871(3) 0.0473(13) Uani 1 1 d . . . C34 C 0.3894(2) 0.3647(5) 0.3227(3) 0.0590(14) Uani 1 1 d . . . H34 H 0.3611 0.3172 0.3121 0.071 Uiso 1 1 calc R . . C3 C 0.9377(2) 0.7513(4) 0.5837(3) 0.0485(13) Uani 1 1 d . . . H3 H 0.9421 0.8175 0.5689 0.058 Uiso 1 1 calc R . . C4 C 0.9814(2) 0.6875(4) 0.6017(3) 0.0469(13) Uani 1 1 d . . . H4 H 1.0157 0.7104 0.5987 0.056 Uiso 1 1 calc R . . C41 C 0.71912(19) 0.9633(3) 0.3359(3) 0.0393(11) Uani 1 1 d . . . H41 H 0.6915 0.9145 0.3233 0.047 Uiso 1 1 calc R . . C35 C 0.4009(2) 0.4225(5) 0.3920(3) 0.0627(16) Uani 1 1 d . . . H35 H 0.3805 0.4134 0.4293 0.075 Uiso 1 1 calc R . . C13 C 1.0299(2) 0.4465(4) 0.6966(3) 0.0522(14) Uani 1 1 d . . . H13 H 1.0055 0.4423 0.7286 0.063 Uiso 1 1 calc R . . C32 C 0.4621(2) 0.4439(4) 0.2860(3) 0.0511(13) Uani 1 1 d . . . H32 H 0.4839 0.4487 0.2503 0.061 Uiso 1 1 calc R . . C36 C 0.4412(2) 0.4926(5) 0.4078(3) 0.0580(15) Uani 1 1 d . . . H36 H 0.4476 0.5331 0.4544 0.070 Uiso 1 1 calc R . . C29 C 0.5161(2) 0.6694(4) 0.4049(3) 0.0512(13) Uani 1 1 d . . . H29 H 0.4832 0.6893 0.4146 0.061 Uiso 1 1 calc R . . C9 C 1.0589(2) 0.5231(4) 0.5922(3) 0.0501(13) Uani 1 1 d . . . H9 H 1.0554 0.5742 0.5535 0.060 Uiso 1 1 calc R . . C30 C 0.5598(2) 0.7323(5) 0.4235(3) 0.0604(16) Uani 1 1 d . . . H30 H 0.5569 0.7949 0.4464 0.072 Uiso 1 1 calc R . . C12 C 1.0719(2) 0.3794(5) 0.7084(3) 0.0617(15) Uani 1 1 d . . . H12 H 1.0773 0.3315 0.7500 0.074 Uiso 1 1 calc R . . C10 C 1.0995(2) 0.4534(5) 0.6012(4) 0.0635(16) Uani 1 1 d . . . H10 H 1.1226 0.4550 0.5673 0.076 Uiso 1 1 calc R . . O1 O 0.8438(2) 0.8730(5) 0.5436(3) 0.120(2) Uani 1 1 d . . . N2 N 0.75402(16) 1.2885(3) 0.9113(2) 0.0362(9) Uani 1 1 d . . . C23 C 0.7197(2) 1.1376(3) 0.8449(3) 0.0454(13) Uani 1 1 d . . . H23 H 0.7004 1.0779 0.8451 0.054 Uiso 1 1 calc R . . O2 O 0.79320(17) 0.7541(3) 0.5596(4) 0.121(2) Uani 1 1 d . . . C22 C 0.7270(2) 1.2040(4) 0.9075(3) 0.0454(12) Uani 1 1 d . . . H22 H 0.7120 1.1887 0.9501 0.055 Uiso 1 1 calc R . . C25 C 0.6081(2) 0.7049(5) 0.4091(3) 0.0513(14) Uani 1 1 d . . . C1 C 0.8378(2) 0.7864(5) 0.5608(3) 0.0619(17) Uani 1 1 d . . . C19 C 0.7407(2) 1.1592(3) 0.7821(3) 0.0373(12) Uani 1 1 d . . . C24 C 0.6573(2) 0.7731(6) 0.4315(4) 0.0642(18) Uani 1 1 d . . . C20 C 0.7680(2) 1.2485(4) 0.7843(3) 0.0547(15) Uani 1 1 d . . . H20 H 0.7822 1.2668 0.7415 0.066 Uiso 1 1 calc R . . C21 C 0.7739(2) 1.3093(4) 0.8501(3) 0.0507(14) Uani 1 1 d . . . H21 H 0.7931 1.3694 0.8519 0.061 Uiso 1 1 calc R . . O3 O 0.6605(3) 0.8362(6) 0.4767(4) 0.176(4) Uani 1 1 d . . . O4 O 0.6941(2) 0.7577(3) 0.4002(5) 0.126(2) 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 0.0517(3) 0.0326(3) 0.0233(2) 0.0004(2) 0.0119(2) 0.0005(3) Zn2 0.0419(3) 0.0308(3) 0.0260(2) 0.0017(3) 0.0102(2) 0.0019(4) N1 0.040(2) 0.036(2) 0.028(2) 0.0003(18) 0.0081(17) 0.0022(19) N3 0.045(2) 0.042(2) 0.0210(19) -0.0010(17) 0.0088(16) 0.0006(19) N4 0.038(2) 0.028(2) 0.032(2) 0.0033(17) 0.0097(17) -0.0011(17) O5 0.055(2) 0.045(2) 0.0325(18) -0.0023(15) 0.0019(15) 0.0220(18) O7 0.0451(19) 0.0363(18) 0.0443(19) 0.0022(15) 0.0108(15) -0.0097(16) C47 0.040(3) 0.026(2) 0.039(3) -0.002(2) 0.008(2) -0.0035(19) O6 0.060(2) 0.048(2) 0.0363(19) 0.0067(15) 0.0058(16) 0.0153(17) C62 0.040(3) 0.040(3) 0.025(2) -0.0027(19) 0.008(2) 0.000(2) O8 0.062(2) 0.051(2) 0.0325(19) -0.0003(16) 0.0054(16) -0.0113(17) C48 0.032(2) 0.035(2) 0.035(2) 0.002(2) 0.0123(19) -0.0001(19) C52 0.039(3) 0.044(3) 0.034(2) -0.004(2) 0.016(2) 0.000(2) C63 0.036(2) 0.041(3) 0.032(2) 0.003(2) 0.0153(19) 0.000(2) C60 0.042(3) 0.024(2) 0.049(3) 0.000(2) 0.016(2) 0.000(2) C59 0.039(2) 0.045(3) 0.038(2) 0.004(2) 0.0147(18) 0.002(2) C53 0.046(3) 0.040(3) 0.025(2) 0.0003(19) 0.009(2) -0.003(2) C66 0.045(3) 0.040(3) 0.032(3) 0.007(2) 0.012(2) 0.001(2) C38 0.051(3) 0.037(3) 0.039(3) 0.005(2) 0.005(2) -0.007(2) C61 0.033(2) 0.034(2) 0.028(2) -0.0013(19) 0.0102(18) 0.0025(19) C15 0.060(3) 0.036(2) 0.033(3) 0.004(2) 0.015(2) 0.012(2) C68 0.040(2) 0.046(3) 0.033(2) -0.005(2) 0.0154(18) 0.001(2) C54 0.033(2) 0.046(3) 0.035(2) 0.006(2) 0.014(2) 0.004(2) C39 0.037(2) 0.038(3) 0.027(2) 0.002(2) 0.0107(19) 0.005(2) C67 0.040(3) 0.042(3) 0.029(2) -0.003(2) 0.019(2) -0.001(2) C56 0.041(3) 0.089(5) 0.041(3) 0.001(3) 0.004(2) 0.015(3) C28 0.046(3) 0.057(3) 0.024(2) 0.005(2) 0.010(2) -0.002(2) C58 0.053(3) 0.048(3) 0.048(3) 0.008(2) 0.022(3) 0.011(3) C49 0.034(3) 0.043(3) 0.033(3) -0.005(2) 0.009(2) 0.001(2) C37 0.051(3) 0.048(3) 0.029(3) -0.005(2) 0.001(2) -0.012(2) C16 0.044(3) 0.041(3) 0.030(3) 0.002(2) 0.014(2) 0.000(2) C46 0.042(3) 0.043(3) 0.035(3) 0.005(2) 0.012(2) -0.005(2) C50 0.033(3) 0.048(3) 0.027(2) -0.005(2) 0.004(2) -0.005(2) C27 0.049(3) 0.054(3) 0.049(3) 0.012(3) 0.022(3) 0.009(3) C14 0.056(3) 0.052(3) 0.032(3) 0.013(2) 0.013(2) 0.013(2) C69 0.068(4) 0.039(3) 0.042(3) -0.005(2) 0.025(3) -0.010(3) C42 0.037(3) 0.029(2) 0.027(2) -0.002(2) 0.009(2) 0.000(2) C18 0.056(3) 0.036(2) 0.024(2) 0.004(2) 0.012(2) 0.007(2) C65 0.040(3) 0.046(3) 0.024(2) 0.001(2) 0.011(2) -0.001(2) C70 0.051(3) 0.062(4) 0.046(3) -0.018(3) 0.018(3) -0.022(3) C72 0.036(3) 0.052(3) 0.034(3) -0.003(2) 0.012(2) -0.001(2) C55 0.040(3) 0.059(3) 0.041(3) -0.007(3) 0.009(2) 0.001(3) C17 0.051(3) 0.038(3) 0.026(2) 0.003(2) 0.012(2) 0.003(2) C11 0.063(3) 0.057(4) 0.074(4) 0.006(4) 0.022(3) 0.020(3) C71 0.039(3) 0.074(4) 0.041(3) -0.010(3) 0.010(2) -0.007(3) C5 0.046(3) 0.054(3) 0.030(3) -0.001(2) 0.010(2) 0.002(2) C44 0.044(3) 0.047(3) 0.047(3) 0.014(2) 0.017(2) 0.007(2) C6 0.051(3) 0.060(3) 0.037(3) -0.009(3) 0.014(2) -0.010(3) C43 0.036(3) 0.052(3) 0.040(3) 0.012(2) 0.012(2) 0.005(2) C8 0.045(3) 0.050(3) 0.035(3) -0.004(2) 0.013(2) 0.007(2) C57 0.051(4) 0.083(4) 0.042(3) 0.013(3) 0.017(3) 0.031(3) C51 0.030(2) 0.044(3) 0.029(2) 0.003(2) 0.0112(18) -0.003(2) C40 0.046(3) 0.045(3) 0.025(2) 0.001(2) 0.004(2) -0.006(2) C31 0.047(3) 0.052(3) 0.032(3) 0.004(2) 0.012(2) -0.003(2) C64 0.028(2) 0.039(3) 0.035(2) -0.002(2) 0.0087(19) 0.001(2) C26 0.046(3) 0.058(3) 0.057(3) 0.027(3) 0.020(3) 0.017(3) C45 0.041(3) 0.032(2) 0.039(3) 0.008(2) 0.010(2) 0.002(2) C7 0.039(3) 0.073(4) 0.053(3) -0.018(3) 0.022(3) -0.012(3) C33 0.072(3) 0.048(3) 0.050(3) -0.005(3) 0.017(3) -0.007(3) C2 0.037(3) 0.070(4) 0.036(3) -0.008(3) 0.013(2) -0.002(3) C34 0.059(3) 0.053(3) 0.067(4) 0.006(3) 0.022(3) -0.005(3) C3 0.051(3) 0.067(3) 0.030(3) 0.004(2) 0.015(2) 0.006(3) C4 0.042(3) 0.061(3) 0.040(3) 0.004(2) 0.017(2) -0.002(3) C41 0.044(3) 0.044(3) 0.028(2) 0.006(2) 0.008(2) -0.009(2) C35 0.053(3) 0.087(5) 0.056(3) 0.008(3) 0.029(3) -0.004(3) C13 0.056(3) 0.062(4) 0.042(3) -0.002(3) 0.019(2) 0.012(3) C32 0.062(3) 0.052(3) 0.043(3) 0.000(3) 0.021(3) 0.005(3) C36 0.054(3) 0.082(4) 0.043(3) -0.016(3) 0.022(3) -0.011(3) C29 0.047(3) 0.065(3) 0.044(3) -0.014(3) 0.017(2) -0.007(3) C9 0.050(3) 0.059(3) 0.044(3) 0.013(3) 0.019(2) 0.005(3) C30 0.062(4) 0.078(4) 0.043(3) -0.014(3) 0.018(3) -0.024(3) C12 0.078(4) 0.055(3) 0.053(3) 0.004(3) 0.020(3) 0.013(4) C10 0.054(3) 0.078(4) 0.067(4) -0.001(3) 0.030(3) 0.010(3) O1 0.105(4) 0.158(5) 0.125(4) 0.098(4) 0.078(3) 0.083(4) N2 0.048(2) 0.029(2) 0.035(2) -0.0024(18) 0.0174(18) 0.0021(19) C23 0.061(3) 0.041(3) 0.037(3) -0.008(2) 0.021(2) -0.009(2) O2 0.038(2) 0.054(3) 0.266(7) -0.067(4) 0.037(3) -0.006(2) C22 0.055(3) 0.043(3) 0.045(3) -0.003(2) 0.024(2) -0.006(2) C25 0.042(3) 0.079(4) 0.030(3) 0.010(3) 0.006(2) -0.007(3) C1 0.059(4) 0.080(5) 0.048(3) -0.028(3) 0.017(3) 0.018(3) C19 0.050(3) 0.035(3) 0.027(2) -0.001(2) 0.013(2) 0.007(2) C24 0.042(3) 0.088(5) 0.065(4) 0.037(4) 0.019(3) -0.008(3) C20 0.086(4) 0.043(3) 0.050(3) -0.008(3) 0.041(3) -0.012(3) C21 0.080(4) 0.035(3) 0.051(3) -0.008(2) 0.040(3) -0.017(3) O3 0.139(5) 0.258(9) 0.177(6) -0.179(7) 0.118(5) -0.132(6) O4 0.066(3) 0.048(3) 0.280(8) 0.032(4) 0.074(4) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 2.061(4) . ? Zn1 O2 2.069(6) . ? Zn1 N3 2.073(4) . ? Zn1 O3 2.146(5) . ? Zn1 O4 2.361(7) . ? Zn1 O1 2.426(5) . ? Zn1 C1 2.562(6) . ? Zn1 C24 2.570(6) . ? Zn2 O5 1.923(3) . ? Zn2 O7 1.936(3) . ? Zn2 N2 2.045(4) 1_554 ? Zn2 N4 2.061(4) . ? N1 C14 1.333(6) . ? N1 C18 1.345(5) . ? N3 C41 1.342(5) . ? N3 C37 1.349(6) . ? N4 C45 1.331(6) . ? N4 C44 1.354(6) . ? O5 C47 1.283(5) . ? O7 C60 1.293(5) . ? C47 O6 1.234(5) . ? C47 C48 1.498(6) . ? C62 C61 1.380(6) . ? C62 C63 1.392(6) . ? C62 H62 0.9500 . ? O8 C60 1.224(5) . ? C48 C49 1.387(6) . ? C48 C53 1.402(6) . ? C52 C53 1.364(6) . ? C52 C51 1.407(6) . ? C52 H52 0.9500 . ? C63 C64 1.417(6) . ? C63 H63 0.9500 . ? C60 C61 1.502(6) . ? C59 C58 1.369(6) . ? C59 C54 1.401(7) . ? C59 H59 0.9500 . ? C53 H53 0.9500 . ? C66 C61 1.395(6) . ? C66 C65 1.397(7) . ? C66 H66 0.9500 . ? C38 C37 1.378(7) . ? C38 C39 1.397(6) . ? C38 H38 0.9500 . ? C15 C14 1.375(7) . ? C15 C16 1.379(6) . ? C15 H15 0.9500 . ? C68 C69 1.370(7) . ? C68 C67 1.398(6) . ? C68 H68 0.9500 . ? C54 C55 1.399(6) . ? C54 C51 1.491(6) . ? C39 C40 1.372(6) . ? C39 C42 1.494(6) . ? C67 C72 1.404(6) . ? C67 C64 1.483(6) . ? C56 C57 1.367(8) . ? C56 C55 1.380(8) . ? C56 H56 0.9500 . ? C28 C27 1.392(7) . ? C28 C29 1.398(7) . ? C28 C31 1.504(7) . ? C58 C57 1.382(8) . ? C58 H58 0.9500 . ? C49 C50 1.381(7) . ? C49 H49 0.9500 . ? C37 H37 0.9500 . ? C16 C17 1.399(7) . ? C16 C19 1.484(6) . ? C46 C42 1.371(6) . ? C46 C45 1.379(6) . ? C46 H46 0.9500 . ? C50 C51 1.388(6) . ? C50 H50 0.9500 . ? C27 C26 1.375(8) . ? C27 H27 0.9500 . ? C14 H14 0.9500 . ? C69 C70 1.380(8) . ? C69 H69 0.9500 . ? C42 C43 1.390(6) . ? C18 C17 1.372(6) . ? C18 H18 0.9500 . ? C65 C64 1.372(6) . ? C65 H65 0.9500 . ? C70 C71 1.380(8) . ? C70 H70 0.9500 . ? C72 C71 1.371(7) . ? C72 H72 0.9500 . ? C55 H55 0.9500 . ? C17 H17 0.9500 . ? C11 C10 1.378(8) . ? C11 C12 1.384(7) . ? C11 H11 0.9500 . ? C71 H71 0.9500 . ? C5 C4 1.389(7) . ? C5 C6 1.396(7) . ? C5 C8 1.501(7) . ? C44 C43 1.365(6) . ? C44 H44 0.9500 . ? C6 C7 1.395(8) . ? C6 H6 0.9500 . ? C43 H43 0.9500 . ? C8 C13 1.381(7) . ? C8 C9 1.396(7) . ? C57 H57 0.9500 . ? C40 C41 1.376(6) . ? C40 H40 0.9500 . ? C31 C32 1.396(7) . ? C31 C36 1.415(7) . ? C26 C25 1.393(8) . ? C26 H26 0.9500 . ? C45 H45 0.9500 . ? C7 C2 1.372(8) . ? C7 H7 0.9500 . ? C33 C34 1.372(7) . ? C33 C32 1.384(7) . ? C33 H33 0.9500 . ? C2 C3 1.388(7) . ? C2 C1 1.527(8) . ? C34 C35 1.392(8) . ? C34 H34 0.9500 . ? C3 C4 1.383(7) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C41 H41 0.9500 . ? C35 C36 1.375(8) . ? C35 H35 0.9500 . ? C13 C12 1.382(8) . ? C13 H13 0.9500 . ? C32 H32 0.9500 . ? C36 H36 0.9500 . ? C29 C30 1.373(7) . ? C29 H29 0.9500 . ? C9 C10 1.384(8) . ? C9 H9 0.9500 . ? C30 C25 1.388(8) . ? C30 H30 0.9500 . ? C12 H12 0.9500 . ? C10 H10 0.9500 . ? O1 C1 1.235(9) . ? N2 C22 1.334(6) . ? N2 C21 1.334(6) . ? N2 Zn2 2.045(4) 1_556 ? C23 C22 1.379(6) . ? C23 C19 1.380(7) . ? C23 H23 0.9500 . ? O2 C1 1.223(8) . ? C22 H22 0.9500 . ? C25 C24 1.525(8) . ? C19 C20 1.397(7) . ? C24 O3 1.147(9) . ? C24 O4 1.237(8) . ? C20 C21 1.378(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? 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 N1 Zn1 O2 103.6(2) . . ? N1 Zn1 N3 100.91(17) . . ? O2 Zn1 N3 133.4(2) . . ? N1 Zn1 O3 88.98(18) . . ? O2 Zn1 O3 111.3(3) . . ? N3 Zn1 O3 108.2(3) . . ? N1 Zn1 O4 143.52(17) . . ? O2 Zn1 O4 90.97(19) . . ? N3 Zn1 O4 92.19(18) . . ? O3 Zn1 O4 54.54(18) . . ? N1 Zn1 O1 91.3(2) . . ? O2 Zn1 O1 56.28(18) . . ? N3 Zn1 O1 84.40(15) . . ? O3 Zn1 O1 167.2(3) . . ? O4 Zn1 O1 124.1(2) . . ? N1 Zn1 C1 101.58(16) . . ? O2 Zn1 C1 28.1(2) . . ? N3 Zn1 C1 108.2(2) . . ? O3 Zn1 C1 139.3(3) . . ? O4 Zn1 C1 106.42(18) . . ? O1 Zn1 C1 28.5(2) . . ? N1 Zn1 C24 115.0(2) . . ? O2 Zn1 C24 99.79(19) . . ? N3 Zn1 C24 104.81(16) . . ? O3 Zn1 C24 26.2(2) . . ? O4 Zn1 C24 28.7(2) . . ? O1 Zn1 C24 149.2(3) . . ? C1 Zn1 C24 124.1(3) . . ? O5 Zn2 O7 120.62(16) . . ? O5 Zn2 N2 99.74(15) . 1_554 ? O7 Zn2 N2 120.09(15) . 1_554 ? O5 Zn2 N4 116.17(15) . . ? O7 Zn2 N4 97.87(14) . . ? N2 Zn2 N4 101.68(17) 1_554 . ? C14 N1 C18 118.4(4) . . ? C14 N1 Zn1 121.8(3) . . ? C18 N1 Zn1 119.8(3) . . ? C41 N3 C37 117.2(4) . . ? C41 N3 Zn1 120.7(3) . . ? C37 N3 Zn1 122.1(3) . . ? C45 N4 C44 117.5(4) . . ? C45 N4 Zn2 121.8(3) . . ? C44 N4 Zn2 120.7(3) . . ? C47 O5 Zn2 114.8(3) . . ? C60 O7 Zn2 113.0(3) . . ? O6 C47 O5 123.9(4) . . ? O6 C47 C48 120.3(4) . . ? O5 C47 C48 115.8(4) . . ? C61 C62 C63 120.7(4) . . ? C61 C62 H62 119.6 . . ? C63 C62 H62 119.6 . . ? C49 C48 C53 118.3(4) . . ? C49 C48 C47 121.6(4) . . ? C53 C48 C47 120.2(4) . . ? C53 C52 C51 119.9(4) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C62 C63 C64 120.2(4) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? O8 C60 O7 123.4(4) . . ? O8 C60 C61 120.5(4) . . ? O7 C60 C61 116.0(4) . . ? C58 C59 C54 121.7(4) . . ? C58 C59 H59 119.2 . . ? C54 C59 H59 119.2 . . ? C52 C53 C48 121.7(4) . . ? C52 C53 H53 119.2 . . ? C48 C53 H53 119.2 . . ? C61 C66 C65 119.5(4) . . ? C61 C66 H66 120.2 . . ? C65 C66 H66 120.2 . . ? C37 C38 C39 118.8(4) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.6 . . ? C62 C61 C66 119.5(4) . . ? C62 C61 C60 118.6(4) . . ? C66 C61 C60 121.9(4) . . ? C14 C15 C16 120.6(4) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C69 C68 C67 121.8(4) . . ? C69 C68 H68 119.1 . . ? C67 C68 H68 119.1 . . ? C55 C54 C59 117.4(4) . . ? C55 C54 C51 121.4(4) . . ? C59 C54 C51 121.1(4) . . ? C40 C39 C38 117.8(4) . . ? C40 C39 C42 118.8(4) . . ? C38 C39 C42 123.4(4) . . ? C68 C67 C72 117.3(4) . . ? C68 C67 C64 122.0(4) . . ? C72 C67 C64 120.6(4) . . ? C57 C56 C55 120.4(5) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C27 C28 C29 118.8(5) . . ? C27 C28 C31 118.9(5) . . ? C29 C28 C31 122.4(5) . . ? C59 C58 C57 119.4(5) . . ? C59 C58 H58 120.3 . . ? C57 C58 H58 120.3 . . ? C50 C49 C48 120.5(4) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? N3 C37 C38 123.2(4) . . ? N3 C37 H37 118.4 . . ? C38 C37 H37 118.4 . . ? C15 C16 C17 116.6(4) . . ? C15 C16 C19 122.0(4) . . ? C17 C16 C19 121.3(4) . . ? C42 C46 C45 120.8(5) . . ? C42 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C49 C50 C51 121.1(4) . . ? C49 C50 H50 119.4 . . ? C51 C50 H50 119.4 . . ? C26 C27 C28 119.7(5) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? N1 C14 C15 122.1(4) . . ? N1 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C68 C69 C70 119.8(5) . . ? C68 C69 H69 120.1 . . ? C70 C69 H69 120.1 . . ? C46 C42 C43 117.4(4) . . ? C46 C42 C39 119.2(4) . . ? C43 C42 C39 123.3(4) . . ? N1 C18 C17 122.0(4) . . ? N1 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C64 C65 C66 122.0(4) . . ? C64 C65 H65 119.0 . . ? C66 C65 H65 119.0 . . ? C71 C70 C69 119.6(5) . . ? C71 C70 H70 120.2 . . ? C69 C70 H70 120.2 . . ? C71 C72 C67 120.5(5) . . ? C71 C72 H72 119.7 . . ? C67 C72 H72 119.7 . . ? C56 C55 C54 120.6(5) . . ? C56 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C10 C11 C12 119.9(5) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C72 C71 C70 120.9(5) . . ? C72 C71 H71 119.5 . . ? C70 C71 H71 119.5 . . ? C4 C5 C6 118.5(5) . . ? C4 C5 C8 121.3(5) . . ? C6 C5 C8 120.2(5) . . ? N4 C44 C43 123.2(5) . . ? N4 C44 H44 118.4 . . ? C43 C44 H44 118.4 . . ? C7 C6 C5 119.6(5) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C44 C43 C42 119.2(4) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C13 C8 C9 118.4(5) . . ? C13 C8 C5 121.0(4) . . ? C9 C8 C5 120.6(5) . . ? C56 C57 C58 120.5(5) . . ? C56 C57 H57 119.7 . . ? C58 C57 H57 119.7 . . ? C50 C51 C52 118.6(4) . . ? C50 C51 C54 121.4(4) . . ? C52 C51 C54 120.1(4) . . ? C39 C40 C41 120.3(4) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C32 C31 C36 118.4(5) . . ? C32 C31 C28 120.6(4) . . ? C36 C31 C28 121.0(5) . . ? C65 C64 C63 118.0(4) . . ? C65 C64 C67 123.3(4) . . ? C63 C64 C67 118.7(4) . . ? C27 C26 C25 121.7(5) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? N4 C45 C46 121.9(4) . . ? N4 C45 H45 119.0 . . ? C46 C45 H45 119.0 . . ? C2 C7 C6 121.4(5) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C34 C33 C32 121.0(5) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C7 C2 C3 119.1(5) . . ? C7 C2 C1 120.6(5) . . ? C3 C2 C1 120.3(6) . . ? C33 C34 C35 118.9(5) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? C4 C3 C2 120.0(5) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 121.3(5) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? N3 C41 C40 122.6(4) . . ? N3 C41 H41 118.7 . . ? C40 C41 H41 118.7 . . ? C36 C35 C34 121.3(5) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C8 C13 C12 120.8(5) . . ? C8 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C33 C32 C31 120.5(5) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C35 C36 C31 119.7(5) . . ? C35 C36 H36 120.2 . . ? C31 C36 H36 120.2 . . ? C30 C29 C28 121.1(5) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C10 C9 C8 121.1(5) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C29 C30 C25 120.4(6) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C13 C12 C11 120.2(6) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C11 C10 C9 119.5(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C1 O1 Zn1 81.9(5) . . ? C22 N2 C21 117.3(4) . . ? C22 N2 Zn2 120.7(3) . 1_556 ? C21 N2 Zn2 121.7(3) . 1_556 ? C22 C23 C19 118.9(4) . . ? C22 C23 H23 120.5 . . ? C19 C23 H23 120.5 . . ? C1 O2 Zn1 99.0(5) . . ? N2 C22 C23 123.5(5) . . ? N2 C22 H22 118.2 . . ? C23 C22 H22 118.2 . . ? C30 C25 C26 118.4(5) . . ? C30 C25 C24 120.9(6) . . ? C26 C25 C24 120.7(5) . . ? O2 C1 O1 121.4(6) . . ? O2 C1 C2 119.1(7) . . ? O1 C1 C2 119.5(6) . . ? O2 C1 Zn1 52.9(4) . . ? O1 C1 Zn1 69.6(4) . . ? C2 C1 Zn1 167.8(4) . . ? C23 C19 C20 118.2(4) . . ? C23 C19 C16 122.7(4) . . ? C20 C19 C16 119.1(4) . . ? O3 C24 O4 120.8(7) . . ? O3 C24 C25 121.1(6) . . ? O4 C24 C25 118.1(7) . . ? O3 C24 Zn1 55.8(4) . . ? O4 C24 Zn1 66.3(4) . . ? C25 C24 Zn1 167.6(4) . . ? C21 C20 C19 118.5(5) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? N2 C21 C20 123.6(5) . . ? N2 C21 H21 118.2 . . ? C20 C21 H21 118.2 . . ? C24 O3 Zn1 98.0(5) . . ? C24 O4 Zn1 85.1(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 O2 Zn1 N1 C14 160.3(4) . . . . ? N3 Zn1 N1 C14 20.3(4) . . . . ? O3 Zn1 N1 C14 -88.0(5) . . . . ? O4 Zn1 N1 C14 -88.7(5) . . . . ? O1 Zn1 N1 C14 104.8(4) . . . . ? C1 Zn1 N1 C14 131.6(4) . . . . ? C24 Zn1 N1 C14 -91.9(4) . . . . ? O2 Zn1 N1 C18 -20.2(4) . . . . ? N3 Zn1 N1 C18 -160.3(4) . . . . ? O3 Zn1 N1 C18 91.4(4) . . . . ? O4 Zn1 N1 C18 90.7(4) . . . . ? O1 Zn1 N1 C18 -75.8(4) . . . . ? C1 Zn1 N1 C18 -49.0(4) . . . . ? C24 Zn1 N1 C18 87.6(4) . . . . ? N1 Zn1 N3 C41 -126.5(4) . . . . ? O2 Zn1 N3 C41 112.6(4) . . . . ? O3 Zn1 N3 C41 -34.0(4) . . . . ? O4 Zn1 N3 C41 19.2(4) . . . . ? O1 Zn1 N3 C41 143.3(4) . . . . ? C1 Zn1 N3 C41 127.3(4) . . . . ? C24 Zn1 N3 C41 -6.8(4) . . . . ? N1 Zn1 N3 C37 53.2(4) . . . . ? O2 Zn1 N3 C37 -67.6(5) . . . . ? O3 Zn1 N3 C37 145.7(4) . . . . ? O4 Zn1 N3 C37 -161.0(4) . . . . ? O1 Zn1 N3 C37 -37.0(4) . . . . ? C1 Zn1 N3 C37 -53.0(4) . . . . ? C24 Zn1 N3 C37 172.9(4) . . . . ? O5 Zn2 N4 C45 5.4(4) . . . . ? O7 Zn2 N4 C45 135.3(4) . . . . ? N2 Zn2 N4 C45 -101.7(4) 1_554 . . . ? O5 Zn2 N4 C44 -171.7(3) . . . . ? O7 Zn2 N4 C44 -41.8(4) . . . . ? N2 Zn2 N4 C44 81.3(4) 1_554 . . . ? O7 Zn2 O5 C47 -65.5(4) . . . . ? N2 Zn2 O5 C47 160.6(3) 1_554 . . . ? N4 Zn2 O5 C47 52.4(4) . . . . ? O5 Zn2 O7 C60 -62.7(3) . . . . ? N2 Zn2 O7 C60 62.1(3) 1_554 . . . ? N4 Zn2 O7 C60 170.5(3) . . . . ? Zn2 O5 C47 O6 -11.9(6) . . . . ? Zn2 O5 C47 C48 166.5(3) . . . . ? O6 C47 C48 C49 -167.9(5) . . . . ? O5 C47 C48 C49 13.7(6) . . . . ? O6 C47 C48 C53 12.9(6) . . . . ? O5 C47 C48 C53 -165.5(4) . . . . ? C61 C62 C63 C64 1.7(7) . . . . ? Zn2 O7 C60 O8 -10.5(6) . . . . ? Zn2 O7 C60 C61 166.6(3) . . . . ? C51 C52 C53 C48 1.4(7) . . . . ? C49 C48 C53 C52 -0.6(7) . . . . ? C47 C48 C53 C52 178.6(4) . . . . ? C63 C62 C61 C66 -0.9(7) . . . . ? C63 C62 C61 C60 177.1(4) . . . . ? C65 C66 C61 C62 -0.1(7) . . . . ? C65 C66 C61 C60 -178.0(4) . . . . ? O8 C60 C61 C62 2.9(6) . . . . ? O7 C60 C61 C62 -174.4(4) . . . . ? O8 C60 C61 C66 -179.1(4) . . . . ? O7 C60 C61 C66 3.6(6) . . . . ? C58 C59 C54 C55 0.6(7) . . . . ? C58 C59 C54 C51 -176.1(4) . . . . ? C37 C38 C39 C40 0.0(7) . . . . ? C37 C38 C39 C42 178.7(5) . . . . ? C69 C68 C67 C72 2.5(6) . . . . ? C69 C68 C67 C64 -173.0(4) . . . . ? C54 C59 C58 C57 -0.3(7) . . . . ? C53 C48 C49 C50 -0.5(7) . . . . ? C47 C48 C49 C50 -179.7(4) . . . . ? C41 N3 C37 C38 0.9(7) . . . . ? Zn1 N3 C37 C38 -178.9(4) . . . . ? C39 C38 C37 N3 -1.0(8) . . . . ? C14 C15 C16 C17 -2.9(8) . . . . ? C14 C15 C16 C19 173.3(5) . . . . ? C48 C49 C50 C51 0.8(7) . . . . ? C29 C28 C27 C26 -0.5(7) . . . . ? C31 C28 C27 C26 -178.8(5) . . . . ? C18 N1 C14 C15 1.1(7) . . . . ? Zn1 N1 C14 C15 -179.4(4) . . . . ? C16 C15 C14 N1 1.1(8) . . . . ? C67 C68 C69 C70 -0.9(7) . . . . ? C45 C46 C42 C43 0.0(7) . . . . ? C45 C46 C42 C39 -177.2(4) . . . . ? C40 C39 C42 C46 49.9(6) . . . . ? C38 C39 C42 C46 -128.8(5) . . . . ? C40 C39 C42 C43 -127.1(5) . . . . ? C38 C39 C42 C43 54.2(7) . . . . ? C14 N1 C18 C17 -1.3(7) . . . . ? Zn1 N1 C18 C17 179.2(4) . . . . ? C61 C66 C65 C64 0.3(7) . . . . ? C68 C69 C70 C71 -0.8(8) . . . . ? C68 C67 C72 C71 -2.4(7) . . . . ? C64 C67 C72 C71 173.1(4) . . . . ? C57 C56 C55 C54 -1.0(9) . . . . ? C59 C54 C55 C56 0.1(7) . . . . ? C51 C54 C55 C56 176.7(5) . . . . ? N1 C18 C17 C16 -0.6(7) . . . . ? C15 C16 C17 C18 2.7(7) . . . . ? C19 C16 C17 C18 -173.6(5) . . . . ? C67 C72 C71 C70 0.8(8) . . . . ? C69 C70 C71 C72 0.8(8) . . . . ? C45 N4 C44 C43 3.4(7) . . . . ? Zn2 N4 C44 C43 -179.4(4) . . . . ? C4 C5 C6 C7 1.7(7) . . . . ? C8 C5 C6 C7 -176.3(5) . . . . ? N4 C44 C43 C42 -1.6(8) . . . . ? C46 C42 C43 C44 -0.1(7) . . . . ? C39 C42 C43 C44 176.9(5) . . . . ? C4 C5 C8 C13 146.6(5) . . . . ? C6 C5 C8 C13 -35.4(7) . . . . ? C4 C5 C8 C9 -36.5(7) . . . . ? C6 C5 C8 C9 141.4(5) . . . . ? C55 C56 C57 C58 1.4(9) . . . . ? C59 C58 C57 C56 -0.7(8) . . . . ? C49 C50 C51 C52 0.0(7) . . . . ? C49 C50 C51 C54 -179.6(4) . . . . ? C53 C52 C51 C50 -1.1(7) . . . . ? C53 C52 C51 C54 178.5(4) . . . . ? C55 C54 C51 C50 37.1(7) . . . . ? C59 C54 C51 C50 -146.4(5) . . . . ? C55 C54 C51 C52 -142.5(5) . . . . ? C59 C54 C51 C52 34.0(6) . . . . ? C38 C39 C40 C41 1.0(7) . . . . ? C42 C39 C40 C41 -177.7(4) . . . . ? C27 C28 C31 C32 -38.7(7) . . . . ? C29 C28 C31 C32 143.0(5) . . . . ? C27 C28 C31 C36 138.8(5) . . . . ? C29 C28 C31 C36 -39.5(7) . . . . ? C66 C65 C64 C63 0.4(7) . . . . ? C66 C65 C64 C67 -178.6(4) . . . . ? C62 C63 C64 C65 -1.4(6) . . . . ? C62 C63 C64 C67 177.7(4) . . . . ? C68 C67 C64 C65 -145.3(5) . . . . ? C72 C67 C64 C65 39.3(7) . . . . ? C68 C67 C64 C63 35.6(6) . . . . ? C72 C67 C64 C63 -139.7(4) . . . . ? C28 C27 C26 C25 2.6(8) . . . . ? C44 N4 C45 C46 -3.5(7) . . . . ? Zn2 N4 C45 C46 179.3(3) . . . . ? C42 C46 C45 N4 1.9(7) . . . . ? C5 C6 C7 C2 0.0(8) . . . . ? C6 C7 C2 C3 -1.9(8) . . . . ? C6 C7 C2 C1 175.3(5) . . . . ? C32 C33 C34 C35 2.1(9) . . . . ? C7 C2 C3 C4 2.2(7) . . . . ? C1 C2 C3 C4 -175.1(4) . . . . ? C2 C3 C4 C5 -0.5(7) . . . . ? C6 C5 C4 C3 -1.5(7) . . . . ? C8 C5 C4 C3 176.5(4) . . . . ? C37 N3 C41 C40 0.2(7) . . . . ? Zn1 N3 C41 C40 180.0(4) . . . . ? C39 C40 C41 N3 -1.2(8) . . . . ? C33 C34 C35 C36 1.0(9) . . . . ? C9 C8 C13 C12 0.9(8) . . . . ? C5 C8 C13 C12 177.8(5) . . . . ? C34 C33 C32 C31 -3.8(9) . . . . ? C36 C31 C32 C33 2.3(8) . . . . ? C28 C31 C32 C33 179.9(5) . . . . ? C34 C35 C36 C31 -2.4(9) . . . . ? C32 C31 C36 C35 0.7(8) . . . . ? C28 C31 C36 C35 -176.8(5) . . . . ? C27 C28 C29 C30 -1.1(8) . . . . ? C31 C28 C29 C30 177.2(5) . . . . ? C13 C8 C9 C10 2.0(8) . . . . ? C5 C8 C9 C10 -174.9(5) . . . . ? C28 C29 C30 C25 0.6(8) . . . . ? C8 C13 C12 C11 -3.1(9) . . . . ? C10 C11 C12 C13 2.4(9) . . . . ? C12 C11 C10 C9 0.6(9) . . . . ? C8 C9 C10 C11 -2.8(9) . . . . ? N1 Zn1 O1 C1 112.4(4) . . . . ? O2 Zn1 O1 C1 6.8(4) . . . . ? N3 Zn1 O1 C1 -146.8(4) . . . . ? O3 Zn1 O1 C1 21.4(12) . . . . ? O4 Zn1 O1 C1 -57.9(4) . . . . ? C24 Zn1 O1 C1 -37.1(6) . . . . ? N1 Zn1 O2 C1 -89.1(4) . . . . ? N3 Zn1 O2 C1 30.7(5) . . . . ? O3 Zn1 O2 C1 176.6(4) . . . . ? O4 Zn1 O2 C1 124.6(5) . . . . ? O1 Zn1 O2 C1 -6.9(4) . . . . ? C24 Zn1 O2 C1 152.0(4) . . . . ? C21 N2 C22 C23 1.2(8) . . . . ? Zn2 N2 C22 C23 175.4(4) 1_556 . . . ? C19 C23 C22 N2 -0.7(8) . . . . ? C29 C30 C25 C26 1.4(8) . . . . ? C29 C30 C25 C24 -178.5(5) . . . . ? C27 C26 C25 C30 -3.0(8) . . . . ? C27 C26 C25 C24 176.9(5) . . . . ? Zn1 O2 C1 O1 13.2(8) . . . . ? Zn1 O2 C1 C2 -169.0(4) . . . . ? Zn1 O1 C1 O2 -11.2(7) . . . . ? Zn1 O1 C1 C2 171.0(5) . . . . ? C7 C2 C1 O2 -1.7(8) . . . . ? C3 C2 C1 O2 175.5(6) . . . . ? C7 C2 C1 O1 176.1(6) . . . . ? C3 C2 C1 O1 -6.7(8) . . . . ? C7 C2 C1 Zn1 -48(2) . . . . ? C3 C2 C1 Zn1 130(2) . . . . ? N1 Zn1 C1 O2 97.3(4) . . . . ? N3 Zn1 C1 O2 -157.0(4) . . . . ? O3 Zn1 C1 O2 -4.9(5) . . . . ? O4 Zn1 C1 O2 -59.1(5) . . . . ? O1 Zn1 C1 O2 168.0(7) . . . . ? C24 Zn1 C1 O2 -33.9(5) . . . . ? N1 Zn1 C1 O1 -70.7(4) . . . . ? O2 Zn1 C1 O1 -168.0(7) . . . . ? N3 Zn1 C1 O1 35.0(4) . . . . ? O3 Zn1 C1 O1 -172.8(4) . . . . ? O4 Zn1 C1 O1 133.0(4) . . . . ? C24 Zn1 C1 O1 158.1(4) . . . . ? N1 Zn1 C1 C2 149(2) . . . . ? O2 Zn1 C1 C2 52(2) . . . . ? N3 Zn1 C1 C2 -105(2) . . . . ? O3 Zn1 C1 C2 47(2) . . . . ? O4 Zn1 C1 C2 -7(2) . . . . ? O1 Zn1 C1 C2 -140(2) . . . . ? C24 Zn1 C1 C2 18(2) . . . . ? C22 C23 C19 C20 -0.8(8) . . . . ? C22 C23 C19 C16 176.7(5) . . . . ? C15 C16 C19 C23 137.8(5) . . . . ? C17 C16 C19 C23 -46.1(8) . . . . ? C15 C16 C19 C20 -44.7(7) . . . . ? C17 C16 C19 C20 131.4(6) . . . . ? C30 C25 C24 O3 18.5(10) . . . . ? C26 C25 C24 O3 -161.3(8) . . . . ? C30 C25 C24 O4 -162.3(6) . . . . ? C26 C25 C24 O4 17.8(8) . . . . ? C30 C25 C24 Zn1 90(3) . . . . ? C26 C25 C24 Zn1 -90(2) . . . . ? N1 Zn1 C24 O3 8.7(7) . . . . ? O2 Zn1 C24 O3 118.8(7) . . . . ? N3 Zn1 C24 O3 -101.1(6) . . . . ? O4 Zn1 C24 O3 -167.5(8) . . . . ? O1 Zn1 C24 O3 154.6(6) . . . . ? C1 Zn1 C24 O3 134.3(6) . . . . ? N1 Zn1 C24 O4 176.1(4) . . . . ? O2 Zn1 C24 O4 -73.7(4) . . . . ? N3 Zn1 C24 O4 66.3(4) . . . . ? O3 Zn1 C24 O4 167.5(8) . . . . ? O1 Zn1 C24 O4 -37.9(5) . . . . ? C1 Zn1 C24 O4 -58.3(4) . . . . ? N1 Zn1 C24 C25 -71(3) . . . . ? O2 Zn1 C24 C25 39(3) . . . . ? O3 Zn1 C24 C25 -79(2) . . . . ? O4 Zn1 C24 C25 113(3) . . . . ? O1 Zn1 C24 C25 75(3) . . . . ? C1 Zn1 C24 C25 55(3) . . . . ? C23 C19 C20 C21 1.7(8) . . . . ? C16 C19 C20 C21 -176.0(5) . . . . ? C22 N2 C21 C20 -0.3(8) . . . . ? Zn2 N2 C21 C20 -174.4(4) 1_556 . . . ? C19 C20 C21 N2 -1.2(9) . . . . ? O4 C24 O3 Zn1 -13.4(9) . . . . ? C25 C24 O3 Zn1 165.7(5) . . . . ? N1 Zn1 O3 C24 -172.1(6) . . . . ? O2 Zn1 O3 C24 -67.9(6) . . . . ? N3 Zn1 O3 C24 86.7(6) . . . . ? O4 Zn1 O3 C24 7.3(5) . . . . ? O1 Zn1 O3 C24 -80.9(11) . . . . ? C1 Zn1 O3 C24 -65.4(7) . . . . ? O3 C24 O4 Zn1 12.1(8) . . . . ? C25 C24 O4 Zn1 -167.1(5) . . . . ? N1 Zn1 O4 C24 -5.9(6) . . . . ? O2 Zn1 O4 C24 108.9(4) . . . . ? N3 Zn1 O4 C24 -117.6(4) . . . . ? O3 Zn1 O4 C24 -6.8(5) . . . . ? O1 Zn1 O4 C24 157.7(4) . . . . ? C1 Zn1 O4 C24 132.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.912 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.079 #===end data_compound9_h08adb17 _database_code_depnum_ccdc_archive 'CCDC 859610' #TrackingRef '- warren-pw.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H16 I2 N2 O4 Zn1' _chemical_formula_weight 715.56 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' N N 0.0061 0.0033 '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 26.7860(7) _cell_length_b 24.7060(7) _cell_length_c 7.4370(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.858(2) _cell_angle_gamma 90.00 _cell_volume 4757.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 77044 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Tabloid _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 3.662 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.63 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35694 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5451 _reflns_number_gt 3640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0830P)^2^+31.7815P] 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 5451 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1728 _refine_ls_wR_factor_gt 0.1590 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 I1 I 0.07442(2) 0.44540(2) 0.65318(7) 0.0572(2) Uani 1 1 d . . . I2 I -0.32712(2) 0.05524(2) 0.86656(8) 0.0601(2) Uani 1 1 d . . . Zn1 Zn -0.12374(3) 0.16631(3) 0.16341(10) 0.0378(2) Uani 1 1 d . . . O1 O -0.0610(2) 0.2093(2) 0.2900(9) 0.0694(17) Uani 1 1 d . . . O2 O -0.1257(2) 0.2619(3) 0.2763(8) 0.0697(17) Uani 1 1 d . . . O3 O -0.17956(19) 0.1368(2) 0.2562(6) 0.0471(12) Uani 1 1 d . . . O4 O -0.1175(2) 0.1062(2) 0.4850(7) 0.0585(15) Uani 1 1 d . . . N1 N -0.0811(2) 0.1052(2) 0.0844(7) 0.0354(12) Uani 1 1 d . . . N2 N -0.1680(2) 0.1958(2) -0.0862(7) 0.0388(13) Uani 1 1 d . . . C1 C -0.0800(3) 0.2536(4) 0.3206(11) 0.0535(19) Uani 1 1 d . . . C2 C -0.0420(3) 0.2966(4) 0.4128(11) 0.055(2) Uani 1 1 d . . . C3 C -0.0592(3) 0.3487(3) 0.3872(10) 0.0527(19) Uani 1 1 d . . . H3 H -0.0941 0.3560 0.3232 0.063 Uiso 1 1 calc R . . C4 C -0.0251(3) 0.3916(3) 0.4558(10) 0.0526(19) Uani 1 1 d . . . H4 H -0.0367 0.4280 0.4355 0.063 Uiso 1 1 calc R . . C5 C 0.0250(3) 0.3809(3) 0.5522(9) 0.0432(16) Uani 1 1 d . . . C6 C 0.0419(3) 0.3284(3) 0.5808(12) 0.056(2) Uani 1 1 d . . . H6 H 0.0762 0.3209 0.6513 0.067 Uiso 1 1 calc R . . C7 C 0.0093(3) 0.2870(4) 0.5075(15) 0.067(2) Uani 1 1 d . . . H7 H 0.0219 0.2508 0.5212 0.080 Uiso 1 1 calc R . . C8 C -0.1638(3) 0.1125(3) 0.4115(9) 0.0426(16) Uani 1 1 d . . . C9 C -0.2037(3) 0.0945(3) 0.5042(9) 0.0396(15) Uani 1 1 d . . . C10 C -0.2555(3) 0.1059(3) 0.4338(10) 0.0482(18) Uani 1 1 d . . . H10 H -0.2668 0.1225 0.3152 0.058 Uiso 1 1 calc R . . C11 C -0.2910(3) 0.0935(3) 0.5317(11) 0.054(2) Uani 1 1 d . . . H11 H -0.3264 0.1022 0.4819 0.064 Uiso 1 1 calc R . . C12 C -0.2749(3) 0.0680(3) 0.7051(10) 0.0450(16) Uani 1 1 d . . . C13 C -0.2234(3) 0.0535(3) 0.7745(10) 0.0488(18) Uani 1 1 d . . . H13 H -0.2127 0.0347 0.8894 0.059 Uiso 1 1 calc R . . C14 C -0.1877(3) 0.0666(3) 0.6749(9) 0.0462(17) Uani 1 1 d . . . H14 H -0.1524 0.0568 0.7218 0.055 Uiso 1 1 calc R . . C15 C -0.0363(3) 0.1159(3) 0.0407(9) 0.0374(15) Uani 1 1 d . . . H15 H -0.0264 0.1526 0.0345 0.045 Uiso 1 1 calc R . . C16 C -0.0046(2) 0.0765(3) 0.0052(8) 0.0355(14) Uani 1 1 d . . . H16 H 0.0265 0.0861 -0.0261 0.043 Uiso 1 1 calc R . . C17 C -0.0175(2) 0.0222(2) 0.0144(7) 0.0310(13) Uani 1 1 d . . . C18 C -0.0639(2) 0.0117(3) 0.0561(8) 0.0336(14) Uani 1 1 d . . . H18 H -0.0749 -0.0247 0.0608 0.040 Uiso 1 1 calc R . . C19 C -0.0941(2) 0.0528(3) 0.0906(8) 0.0332(14) Uani 1 1 d . . . H19 H -0.1255 0.0441 0.1203 0.040 Uiso 1 1 calc R . . C20 C -0.2186(3) 0.1998(3) -0.1091(9) 0.0488(18) Uani 1 1 d . . . H20 H -0.2326 0.1878 -0.0110 0.059 Uiso 1 1 calc R . . C21 C -0.2523(3) 0.2205(3) -0.2688(10) 0.0503(18) Uani 1 1 d . . . H21 H -0.2884 0.2218 -0.2787 0.060 Uiso 1 1 calc R . . C22 C -0.2329(3) 0.2394(2) -0.4138(8) 0.0340(14) Uani 1 1 d . . . C23 C -0.1792(3) 0.2359(3) -0.3863(9) 0.0484(18) Uani 1 1 d . . . H23 H -0.1634 0.2487 -0.4789 0.058 Uiso 1 1 calc R . . C24 C -0.1496(3) 0.2138(3) -0.2237(10) 0.0496(18) Uani 1 1 d . . . H24 H -0.1134 0.2114 -0.2095 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0646(4) 0.0469(3) 0.0562(3) -0.0020(2) 0.0081(3) -0.0144(2) I2 0.0585(4) 0.0586(4) 0.0584(3) 0.0098(2) 0.0063(3) -0.0127(2) Zn1 0.0411(4) 0.0327(4) 0.0314(4) 0.0031(3) -0.0058(3) 0.0031(3) O1 0.060(4) 0.049(3) 0.087(4) -0.004(3) -0.002(3) -0.005(3) O2 0.048(4) 0.089(5) 0.067(4) -0.001(3) 0.007(3) -0.017(3) O3 0.048(3) 0.047(3) 0.038(2) 0.014(2) -0.004(2) -0.006(2) O4 0.055(4) 0.073(4) 0.046(3) 0.016(3) 0.011(3) 0.027(3) N1 0.036(3) 0.036(3) 0.026(2) 0.004(2) -0.007(2) 0.001(2) N2 0.049(3) 0.030(3) 0.030(3) 0.000(2) -0.005(2) 0.005(2) C1 0.056(5) 0.055(5) 0.055(5) -0.002(4) 0.025(4) -0.001(4) C2 0.048(5) 0.068(6) 0.053(4) -0.020(4) 0.020(4) -0.011(4) C3 0.050(4) 0.057(5) 0.049(4) 0.003(3) 0.008(3) 0.006(4) C4 0.057(5) 0.047(4) 0.047(4) 0.003(3) 0.000(4) -0.001(4) C5 0.050(4) 0.048(4) 0.032(3) -0.004(3) 0.012(3) -0.001(3) C6 0.042(4) 0.048(5) 0.074(5) -0.013(4) 0.008(4) 0.003(3) C7 0.048(5) 0.045(5) 0.107(7) -0.020(5) 0.018(5) -0.001(4) C8 0.055(5) 0.036(4) 0.034(3) -0.002(3) 0.006(3) 0.004(3) C9 0.048(4) 0.031(3) 0.031(3) 0.001(2) -0.007(3) 0.005(3) C10 0.062(5) 0.038(4) 0.036(4) 0.006(3) -0.005(3) -0.006(3) C11 0.043(4) 0.050(4) 0.054(4) 0.015(3) -0.013(3) -0.011(3) C12 0.052(4) 0.040(4) 0.041(4) -0.002(3) 0.007(3) -0.013(3) C13 0.061(5) 0.046(4) 0.031(3) 0.004(3) -0.005(3) 0.006(4) C14 0.062(5) 0.045(4) 0.025(3) 0.004(3) 0.001(3) 0.001(3) C15 0.034(3) 0.033(3) 0.039(3) 0.007(3) -0.001(3) -0.007(3) C16 0.030(3) 0.039(4) 0.031(3) 0.004(3) -0.003(3) -0.007(3) C17 0.031(3) 0.039(3) 0.015(2) 0.002(2) -0.008(2) -0.005(2) C18 0.039(4) 0.033(3) 0.022(3) -0.002(2) -0.004(2) -0.004(3) C19 0.028(3) 0.041(4) 0.024(3) 0.004(2) -0.005(2) -0.003(3) C20 0.056(5) 0.062(5) 0.027(3) 0.010(3) 0.007(3) 0.021(4) C21 0.044(4) 0.070(5) 0.035(4) 0.013(3) 0.008(3) 0.018(4) C22 0.045(4) 0.027(3) 0.024(3) -0.001(2) -0.002(3) 0.007(3) C23 0.052(4) 0.055(5) 0.032(3) 0.008(3) 0.000(3) -0.011(3) C24 0.046(4) 0.050(4) 0.042(4) 0.013(3) -0.007(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 C5 2.085(7) . ? I2 C12 2.087(8) . ? Zn1 O3 1.942(5) . ? Zn1 O1 2.007(6) . ? Zn1 N2 2.062(5) . ? Zn1 N1 2.067(6) . ? Zn1 C1 2.586(9) . ? O1 C1 1.253(10) . ? O2 C1 1.202(9) . ? O3 C8 1.274(8) . ? O4 C8 1.230(8) . ? N1 C19 1.343(8) . ? N1 C15 1.348(9) . ? N2 C24 1.320(9) . ? N2 C20 1.325(9) . ? C1 C2 1.508(12) . ? C2 C3 1.363(12) . ? C2 C7 1.397(12) . ? C3 C4 1.407(11) . ? C3 H3 0.9500 . ? C4 C5 1.377(11) . ? C4 H4 0.9500 . ? C5 C6 1.372(11) . ? C6 C7 1.365(11) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.482(11) . ? C9 C10 1.380(10) . ? C9 C14 1.411(9) . ? C10 C11 1.372(11) . ? C10 H10 0.9500 . ? C11 C12 1.401(10) . ? C11 H11 0.9500 . ? C12 C13 1.391(11) . ? C13 C14 1.391(12) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.362(10) . ? C15 H15 0.9500 . ? C16 C17 1.391(9) . ? C16 H16 0.9500 . ? C17 C18 1.380(9) . ? C17 C17 1.494(13) 5 ? C18 C19 1.363(9) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.393(9) . ? C20 H20 0.9500 . ? C21 C22 1.392(10) . ? C21 H21 0.9500 . ? C22 C23 1.402(10) . ? C22 C22 1.469(11) 7_454 ? C23 C24 1.377(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? 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 O1 131.4(2) . . ? O3 Zn1 N2 97.8(2) . . ? O1 Zn1 N2 117.0(2) . . ? O3 Zn1 N1 111.0(2) . . ? O1 Zn1 N1 93.6(2) . . ? N2 Zn1 N1 103.5(2) . . ? O3 Zn1 C1 117.0(2) . . ? O1 Zn1 C1 28.2(3) . . ? N2 Zn1 C1 101.6(2) . . ? N1 Zn1 C1 121.2(2) . . ? C1 O1 Zn1 102.5(5) . . ? C8 O3 Zn1 113.1(5) . . ? C19 N1 C15 116.8(6) . . ? C19 N1 Zn1 121.9(5) . . ? C15 N1 Zn1 121.1(4) . . ? C24 N2 C20 116.5(6) . . ? C24 N2 Zn1 125.1(5) . . ? C20 N2 Zn1 118.3(5) . . ? O2 C1 O1 122.2(8) . . ? O2 C1 C2 121.7(8) . . ? O1 C1 C2 116.1(8) . . ? O2 C1 Zn1 72.9(5) . . ? O1 C1 Zn1 49.3(4) . . ? C2 C1 Zn1 165.3(6) . . ? C3 C2 C7 119.0(8) . . ? C3 C2 C1 115.9(8) . . ? C7 C2 C1 124.9(8) . . ? C2 C3 C4 119.8(8) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 119.9(8) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.2(7) . . ? C6 C5 I1 120.9(6) . . ? C4 C5 I1 119.0(6) . . ? C5 C6 C7 119.6(8) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 121.4(8) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? O4 C8 O3 121.7(7) . . ? O4 C8 C9 121.4(6) . . ? O3 C8 C9 116.8(6) . . ? C10 C9 C14 119.0(7) . . ? C10 C9 C8 122.6(6) . . ? C14 C9 C8 118.4(6) . . ? C11 C10 C9 121.3(6) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 119.9(7) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 120.0(7) . . ? C13 C12 I2 119.7(5) . . ? C11 C12 I2 120.3(6) . . ? C12 C13 C14 119.7(6) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C9 120.1(7) . . ? C13 C14 H14 120.0 . . ? C9 C14 H14 120.0 . . ? N1 C15 C16 123.0(6) . . ? N1 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C15 C16 C17 120.3(6) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 116.2(6) . . ? C18 C17 C17 121.9(7) . 5 ? C16 C17 C17 121.9(7) . 5 ? C19 C18 C17 120.9(6) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? N1 C19 C18 122.8(6) . . ? N1 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? N2 C20 C21 123.7(7) . . ? N2 C20 H20 118.1 . . ? C21 C20 H20 118.1 . . ? C22 C21 C20 119.6(7) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 116.1(6) . . ? C21 C22 C22 121.5(8) . 7_454 ? C23 C22 C22 122.4(8) . 7_454 ? C24 C23 C22 119.3(7) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? N2 C24 C23 124.7(7) . . ? N2 C24 H24 117.7 . . ? C23 C24 H24 117.7 . . ? 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 O3 Zn1 O1 C1 -68.8(6) . . . . ? N2 Zn1 O1 C1 61.9(6) . . . . ? N1 Zn1 O1 C1 169.0(5) . . . . ? O1 Zn1 O3 C8 -46.1(6) . . . . ? N2 Zn1 O3 C8 177.0(5) . . . . ? N1 Zn1 O3 C8 69.2(5) . . . . ? C1 Zn1 O3 C8 -75.7(5) . . . . ? O3 Zn1 N1 C19 3.2(5) . . . . ? O1 Zn1 N1 C19 140.3(5) . . . . ? N2 Zn1 N1 C19 -100.8(4) . . . . ? C1 Zn1 N1 C19 146.4(4) . . . . ? O3 Zn1 N1 C15 -170.5(4) . . . . ? O1 Zn1 N1 C15 -33.4(5) . . . . ? N2 Zn1 N1 C15 85.5(5) . . . . ? C1 Zn1 N1 C15 -27.3(5) . . . . ? O3 Zn1 N2 C24 -169.4(6) . . . . ? O1 Zn1 N2 C24 45.7(6) . . . . ? N1 Zn1 N2 C24 -55.5(6) . . . . ? C1 Zn1 N2 C24 70.9(6) . . . . ? O3 Zn1 N2 C20 14.2(6) . . . . ? O1 Zn1 N2 C20 -130.7(5) . . . . ? N1 Zn1 N2 C20 128.1(5) . . . . ? C1 Zn1 N2 C20 -105.5(5) . . . . ? Zn1 O1 C1 O2 0.2(10) . . . . ? Zn1 O1 C1 C2 -178.6(6) . . . . ? O3 Zn1 C1 O2 -51.6(5) . . . . ? O1 Zn1 C1 O2 -179.9(8) . . . . ? N2 Zn1 C1 O2 53.5(5) . . . . ? N1 Zn1 C1 O2 167.3(4) . . . . ? O3 Zn1 C1 O1 128.3(5) . . . . ? N2 Zn1 C1 O1 -126.7(6) . . . . ? N1 Zn1 C1 O1 -12.9(6) . . . . ? O3 Zn1 C1 C2 133(2) . . . . ? O1 Zn1 C1 C2 5(2) . . . . ? N2 Zn1 C1 C2 -122(2) . . . . ? N1 Zn1 C1 C2 -8(2) . . . . ? O2 C1 C2 C3 -21.4(11) . . . . ? O1 C1 C2 C3 157.4(7) . . . . ? Zn1 C1 C2 C3 153(2) . . . . ? O2 C1 C2 C7 163.8(8) . . . . ? O1 C1 C2 C7 -17.4(12) . . . . ? Zn1 C1 C2 C7 -22(3) . . . . ? C7 C2 C3 C4 0.1(12) . . . . ? C1 C2 C3 C4 -175.0(7) . . . . ? C2 C3 C4 C5 -1.5(12) . . . . ? C3 C4 C5 C6 0.4(11) . . . . ? C3 C4 C5 I1 -179.7(6) . . . . ? C4 C5 C6 C7 2.3(12) . . . . ? I1 C5 C6 C7 -177.7(7) . . . . ? C5 C6 C7 C2 -3.8(14) . . . . ? C3 C2 C7 C6 2.6(14) . . . . ? C1 C2 C7 C6 177.2(8) . . . . ? Zn1 O3 C8 O4 -4.4(9) . . . . ? Zn1 O3 C8 C9 172.8(4) . . . . ? O4 C8 C9 C10 173.5(7) . . . . ? O3 C8 C9 C10 -3.8(10) . . . . ? O4 C8 C9 C14 -3.9(10) . . . . ? O3 C8 C9 C14 178.8(6) . . . . ? C14 C9 C10 C11 4.0(10) . . . . ? C8 C9 C10 C11 -173.4(7) . . . . ? C9 C10 C11 C12 -1.2(11) . . . . ? C10 C11 C12 C13 -2.4(11) . . . . ? C10 C11 C12 I2 174.4(6) . . . . ? C11 C12 C13 C14 2.9(10) . . . . ? I2 C12 C13 C14 -173.9(5) . . . . ? C12 C13 C14 C9 0.0(10) . . . . ? C10 C9 C14 C13 -3.4(10) . . . . ? C8 C9 C14 C13 174.1(6) . . . . ? C19 N1 C15 C16 -0.4(9) . . . . ? Zn1 N1 C15 C16 173.6(5) . . . . ? N1 C15 C16 C17 -0.5(9) . . . . ? C15 C16 C17 C18 1.6(8) . . . . ? C15 C16 C17 C17 -176.9(6) . . . 5 ? C16 C17 C18 C19 -1.7(8) . . . . ? C17 C17 C18 C19 176.8(6) 5 . . . ? C15 N1 C19 C18 0.3(8) . . . . ? Zn1 N1 C19 C18 -173.6(4) . . . . ? C17 C18 C19 N1 0.7(9) . . . . ? C24 N2 C20 C21 1.3(11) . . . . ? Zn1 N2 C20 C21 178.0(6) . . . . ? N2 C20 C21 C22 -1.2(12) . . . . ? C20 C21 C22 C23 -0.1(11) . . . . ? C20 C21 C22 C22 178.8(8) . . . 7_454 ? C21 C22 C23 C24 1.1(11) . . . . ? C22 C22 C23 C24 -177.7(8) 7_454 . . . ? C20 N2 C24 C23 -0.2(11) . . . . ? Zn1 N2 C24 C23 -176.6(6) . . . . ? C22 C23 C24 N2 -1.1(12) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.660 _refine_diff_density_min -1.781 _refine_diff_density_rms 0.169 #===end