# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Shourong Zhu' _publ_contact_author_email SHOURONGZHU@SHU.EDU.CN _publ_section_title ; Coordination Polymers of Biphenyl-2,4,2',4'-Tetracarboxylic Acid-Synthesis, Structures and Adsorption Properties ; loop_ _publ_author_name 'Shourong Zhu' 'Juan Jia' 'Tiantian Jia' 'Ming-Xing Li' 'Min Shao' ; Feifei Xing ; 'Yongmei Zhao' # complex_2.cif===END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 692245' #TrackingRef 'complex1-8_2new1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H20 N3 O9 Zn2' _chemical_formula_weight 709.24 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2087(7) _cell_length_b 14.9912(13) _cell_length_c 21.9789(19) _cell_angle_alpha 90.00 _cell_angle_beta 94.7020(10) _cell_angle_gamma 90.00 _cell_volume 2695.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4895 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.59 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1436 _exptl_absorpt_coefficient_mu 1.846 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7692 _exptl_absorpt_correction_T_max 0.8369 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13806 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4748 _reflns_number_gt 3924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+3.0752P] 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 4748 _refine_ls_number_parameters 424 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.069 _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 0.67436(5) -0.08091(2) -0.135064(17) 0.02372(13) Uani 1 1 d . . . Zn2 Zn 0.96638(5) 0.73276(3) 0.257169(18) 0.02700(13) Uani 1 1 d . . . C1 C 1.0030(4) 0.5342(2) 0.24285(15) 0.0263(8) Uani 1 1 d . . . C2 C 0.9740(4) 0.4539(2) 0.20235(15) 0.0251(7) Uani 1 1 d . . . C3 C 1.0687(4) 0.3782(2) 0.21262(15) 0.0265(8) Uani 1 1 d . . . H3 H 1.1457 0.3766 0.2461 0.032 Uiso 1 1 calc R . . C4 C 1.0522(4) 0.3044(2) 0.17442(15) 0.0245(7) Uani 1 1 d . . . C5 C 0.9306(4) 0.3047(2) 0.12557(15) 0.0248(7) Uani 1 1 d . . . C6 C 0.8346(4) 0.3807(2) 0.11672(16) 0.0302(8) Uani 1 1 d . . . H6 H 0.7520 0.3813 0.0851 0.036 Uiso 1 1 calc R . . C7 C 0.8579(4) 0.4551(2) 0.15332(16) 0.0288(8) Uani 1 1 d . . . H7 H 0.7953 0.5060 0.1449 0.035 Uiso 1 1 calc R . . C8 C 1.1715(4) 0.2288(2) 0.18543(16) 0.0272(8) Uani 1 1 d . . . C9 C 0.8970(4) 0.2309(2) 0.08055(15) 0.0250(7) Uani 1 1 d . . . C10 C 0.7543(4) 0.1802(2) 0.07942(14) 0.0237(7) Uani 1 1 d . . . C11 C 0.6357(5) 0.1884(2) 0.12748(15) 0.0264(8) Uani 1 1 d . . . C12 C 0.7194(4) 0.1179(2) 0.03311(15) 0.0274(8) Uani 1 1 d . . . H12 H 0.6244 0.0840 0.0328 0.033 Uiso 1 1 calc R . . C13 C 0.8240(4) 0.1057(2) -0.01240(15) 0.0281(8) Uani 1 1 d . . . C14 C 0.9648(5) 0.1569(3) -0.01168(17) 0.0380(9) Uani 1 1 d . . . H14 H 1.0356 0.1497 -0.0423 0.046 Uiso 1 1 calc R . . C15 C 1.0005(5) 0.2184(2) 0.03405(17) 0.0350(9) Uani 1 1 d . . . H15 H 1.0954 0.2523 0.0339 0.042 Uiso 1 1 calc R . . C16 C 0.7841(5) 0.0396(2) -0.06292(17) 0.0332(9) Uani 1 1 d . . . C17 C 1.0484(6) 0.9163(3) 0.3185(3) 0.0613(14) Uani 1 1 d . . . H17 H 1.0950 0.8828 0.3510 0.074 Uiso 1 1 calc R . . C18 C 1.0608(7) 1.0085(4) 0.3207(3) 0.0805(19) Uani 1 1 d . . . H18 H 1.1127 1.0367 0.3546 0.097 Uiso 1 1 calc R . . C19 C 0.9950(10) 1.0577(4) 0.2718(4) 0.096(3) Uani 1 1 d . . . H19 H 1.0037 1.1196 0.2721 0.115 Uiso 1 1 calc R . . C20 C 0.9174(8) 1.0154(3) 0.2232(3) 0.0779(19) Uani 1 1 d . . . H20 H 0.8731 1.0479 0.1898 0.094 Uiso 1 1 calc R . . C21 C 0.9046(6) 0.9225(3) 0.2238(2) 0.0492(12) Uani 1 1 d . . . C22 C 0.8176(6) 0.8713(3) 0.1746(2) 0.0463(11) Uani 1 1 d . . . C23 C 0.7244(7) 0.9098(4) 0.1260(3) 0.0701(17) Uani 1 1 d . . . H23 H 0.7152 0.9716 0.1234 0.084 Uiso 1 1 calc R . . C24 C 0.6475(7) 0.8584(5) 0.0826(3) 0.0789(19) Uani 1 1 d . . . H24 H 0.5862 0.8842 0.0497 0.095 Uiso 1 1 calc R . . C25 C 0.6601(7) 0.7690(4) 0.0873(2) 0.0719(16) Uani 1 1 d . . . H25 H 0.6064 0.7325 0.0579 0.086 Uiso 1 1 calc R . . C26 C 0.7531(6) 0.7322(3) 0.1359(2) 0.0566(13) Uani 1 1 d . . . H26 H 0.7609 0.6704 0.1387 0.068 Uiso 1 1 calc R . . C27 C 0.2183(10) 0.1404(6) 0.4509(3) 0.102(2) Uani 1 1 d G . . H27 H 0.2181 0.2015 0.4437 0.122 Uiso 1 1 calc R . . C28 C 0.3591(15) 0.0927(7) 0.4367(5) 0.161(5) Uani 1 1 d GD . . H28 H 0.4492 0.1177 0.4201 0.193 Uiso 1 1 calc R . . C29 C 0.3427(12) 0.0023(7) 0.4513(5) 0.176(5) Uani 1 1 d GD . . H29 H 0.4288 -0.0345 0.4424 0.211 Uiso 1 1 calc R . . C30 C 0.2115(12) -0.0404(6) 0.4781(4) 0.127(3) Uani 1 1 d G . . H30 H 0.2142 -0.1004 0.4889 0.153 Uiso 1 1 calc R . . C31 C 0.0728(9) 0.0169(5) 0.4874(3) 0.0881(19) Uani 1 1 d G . . N1 N 0.9718(4) 0.8745(2) 0.27103(17) 0.0434(9) Uani 1 1 d . . . N2 N 0.8321(4) 0.7820(2) 0.17896(15) 0.0410(8) Uani 1 1 d . . . N3 N 0.0780(8) 0.1043(4) 0.4749(3) 0.1011(18) Uani 1 1 d G . . O1 O 0.9626(3) 0.60807(16) 0.22075(11) 0.0339(6) Uani 1 1 d . . . O2 O 1.0659(4) 0.51846(17) 0.29593(11) 0.0400(7) Uani 1 1 d . . . O3 O 1.1499(3) 0.16086(15) 0.15285(12) 0.0334(6) Uani 1 1 d . . . O4 O 1.2853(3) 0.23878(17) 0.22675(12) 0.0362(6) Uani 1 1 d . . . O5 O 0.6919(3) 0.20783(17) 0.18084(11) 0.0344(6) Uani 1 1 d . . . O6 O 0.4864(3) 0.17571(17) 0.11204(12) 0.0362(6) Uani 1 1 d . . . O7 O 0.6682(3) -0.01478(17) -0.05737(12) 0.0406(7) Uani 1 1 d . . . O8 O 0.8603(4) 0.0404(2) -0.10909(13) 0.0593(9) Uani 1 1 d . . . O9 O 0.2815(17) 0.2691(7) 0.3545(4) 0.126(4) Uani 0.50 1 d P . . 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 0.0313(2) 0.0180(2) 0.0215(2) -0.00317(15) -0.00013(16) 0.00125(16) Zn2 0.0355(3) 0.0189(2) 0.0263(2) -0.00049(16) 0.00065(18) 0.00156(17) C1 0.0254(19) 0.026(2) 0.0275(19) -0.0069(15) 0.0042(15) -0.0016(15) C2 0.0299(19) 0.0184(17) 0.0272(18) -0.0045(14) 0.0031(15) -0.0007(14) C3 0.0300(19) 0.0214(18) 0.0274(18) -0.0056(14) -0.0022(15) -0.0010(14) C4 0.0260(18) 0.0200(17) 0.0273(18) -0.0037(14) 0.0014(15) -0.0004(14) C5 0.0307(19) 0.0190(17) 0.0253(17) -0.0043(14) 0.0067(15) -0.0059(14) C6 0.033(2) 0.0269(19) 0.0288(18) -0.0043(15) -0.0109(16) 0.0010(15) C7 0.035(2) 0.0186(17) 0.0312(18) -0.0028(15) -0.0030(16) 0.0038(15) C8 0.0281(19) 0.0218(18) 0.0322(19) -0.0013(15) 0.0051(16) -0.0016(14) C9 0.0291(19) 0.0186(17) 0.0265(17) -0.0032(14) -0.0024(15) 0.0000(14) C10 0.0305(19) 0.0183(17) 0.0217(16) -0.0020(13) -0.0021(14) 0.0000(14) C11 0.040(2) 0.0128(16) 0.0270(18) -0.0005(14) 0.0035(16) -0.0023(14) C12 0.034(2) 0.0198(17) 0.0277(18) -0.0035(14) 0.0000(15) -0.0030(15) C13 0.036(2) 0.0225(18) 0.0254(18) -0.0066(15) -0.0008(15) -0.0003(15) C14 0.039(2) 0.041(2) 0.036(2) -0.0141(18) 0.0118(18) -0.0035(18) C15 0.035(2) 0.033(2) 0.038(2) -0.0104(17) 0.0060(17) -0.0102(16) C16 0.040(2) 0.028(2) 0.030(2) -0.0092(16) -0.0040(17) 0.0051(17) C17 0.058(3) 0.047(3) 0.080(4) -0.025(3) 0.018(3) -0.007(2) C18 0.083(4) 0.059(4) 0.106(5) -0.042(4) 0.044(4) -0.025(3) C19 0.143(6) 0.032(3) 0.124(6) -0.022(4) 0.088(5) -0.024(3) C20 0.120(5) 0.030(3) 0.093(4) 0.013(3) 0.061(4) 0.006(3) C21 0.064(3) 0.027(2) 0.061(3) 0.010(2) 0.036(2) 0.012(2) C22 0.055(3) 0.036(2) 0.051(3) 0.016(2) 0.025(2) 0.019(2) C23 0.079(4) 0.065(4) 0.069(4) 0.033(3) 0.024(3) 0.042(3) C24 0.067(4) 0.111(5) 0.058(3) 0.028(4) 0.000(3) 0.040(4) C25 0.062(3) 0.098(5) 0.054(3) 0.009(3) -0.009(3) 0.004(3) C26 0.071(3) 0.055(3) 0.041(3) 0.008(2) -0.010(2) 0.002(2) C27 0.114(6) 0.095(6) 0.098(5) -0.004(4) 0.015(5) -0.034(5) C28 0.172(11) 0.099(7) 0.203(11) -0.053(8) -0.038(9) 0.041(7) C29 0.101(7) 0.269(16) 0.167(10) -0.061(11) 0.069(7) 0.025(9) C30 0.151(8) 0.098(6) 0.140(7) 0.000(5) 0.055(6) 0.036(6) C31 0.111(6) 0.074(4) 0.081(4) -0.003(3) 0.019(4) 0.003(4) N1 0.043(2) 0.0274(18) 0.062(2) -0.0085(17) 0.0150(18) 0.0010(15) N2 0.052(2) 0.0341(19) 0.0365(18) 0.0092(15) 0.0033(16) 0.0080(16) N3 0.121(5) 0.084(4) 0.096(4) -0.006(3) -0.006(4) 0.003(4) O1 0.0460(16) 0.0169(13) 0.0373(14) -0.0048(11) -0.0055(12) 0.0034(11) O2 0.0625(19) 0.0241(14) 0.0312(14) -0.0065(11) -0.0091(13) -0.0017(12) O3 0.0348(14) 0.0205(13) 0.0445(15) -0.0125(12) 0.0001(12) 0.0032(11) O4 0.0353(15) 0.0307(14) 0.0410(15) -0.0064(12) -0.0066(12) 0.0060(11) O5 0.0438(16) 0.0348(14) 0.0250(13) -0.0058(11) 0.0052(12) -0.0045(12) O6 0.0339(15) 0.0356(15) 0.0392(15) 0.0011(12) 0.0037(12) -0.0090(12) O7 0.0550(18) 0.0320(15) 0.0342(14) -0.0143(12) -0.0001(13) -0.0121(13) O8 0.066(2) 0.071(2) 0.0436(17) -0.0345(16) 0.0185(16) -0.0169(17) O9 0.214(13) 0.091(7) 0.070(6) -0.010(5) -0.010(7) 0.029(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.936(2) 4_565 ? Zn1 O3 1.940(2) 3_755 ? Zn1 O7 1.979(2) . ? Zn1 O6 2.031(2) 3_655 ? Zn1 O8 2.412(3) . ? Zn2 O5 1.993(3) 2_655 ? Zn2 O1 2.033(2) . ? Zn2 O4 2.042(3) 2_755 ? Zn2 N2 2.098(3) . ? Zn2 N1 2.146(3) . ? C1 O1 1.244(4) . ? C1 O2 1.259(4) . ? C1 C2 1.504(5) . ? C2 C7 1.379(5) . ? C2 C3 1.384(5) . ? C3 C4 1.389(5) . ? C3 H3 0.9300 . ? C4 C5 1.405(5) . ? C4 C8 1.504(5) . ? C5 C6 1.389(5) . ? C5 C9 1.495(5) . ? C6 C7 1.380(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.249(4) . ? C8 O4 1.257(4) . ? C9 C15 1.394(5) . ? C9 C10 1.394(5) . ? C10 C12 1.394(5) . ? C10 C11 1.499(5) . ? C11 O5 1.259(4) . ? C11 O6 1.259(4) . ? C12 C13 1.383(5) . ? C12 H12 0.9300 . ? C13 C14 1.387(5) . ? C13 C16 1.503(5) . ? C14 C15 1.378(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O8 1.235(5) . ? C16 O7 1.267(5) . ? C17 N1 1.330(6) . ? C17 C18 1.386(7) . ? C17 H17 0.9300 . ? C18 C19 1.377(10) . ? C18 H18 0.9300 . ? C19 C20 1.355(9) . ? C19 H19 0.9300 . ? C20 C21 1.397(6) . ? C20 H20 0.9300 . ? C21 N1 1.344(6) . ? C21 C22 1.462(7) . ? C22 N2 1.347(5) . ? C22 C23 1.389(7) . ? C23 C24 1.342(8) . ? C23 H23 0.9300 . ? C24 C25 1.347(8) . ? C24 H24 0.9300 . ? C25 C26 1.376(7) . ? C25 H25 0.9300 . ? C26 N2 1.332(6) . ? C26 H26 0.9300 . ? C27 C28 1.415(12) . ? C27 N3 1.413(9) . ? C27 H27 0.9300 . ? C28 C29 1.403(2) . ? C28 H28 0.9300 . ? C29 C30 1.421(11) . ? C29 H29 0.9300 . ? C30 C31 1.454(10) . ? C30 H30 0.9300 . ? C31 N3 1.340(8) . ? C31 C31 1.449(13) 3_556 ? O2 Zn1 1.936(2) 4_666 ? O3 Zn1 1.940(2) 3_755 ? O4 Zn2 2.042(3) 2_745 ? O5 Zn2 1.993(3) 2_645 ? O6 Zn1 2.031(2) 3_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O3 116.28(11) 4_565 3_755 ? O2 Zn1 O7 113.02(12) 4_565 . ? O3 Zn1 O7 123.76(11) 3_755 . ? O2 Zn1 O6 105.49(11) 4_565 3_655 ? O3 Zn1 O6 97.29(11) 3_755 3_655 ? O7 Zn1 O6 94.15(11) . 3_655 ? O2 Zn1 O8 93.57(12) 4_565 . ? O3 Zn1 O8 92.68(11) 3_755 . ? O7 Zn1 O8 58.58(10) . . ? O6 Zn1 O8 151.61(10) 3_655 . ? O5 Zn2 O1 96.14(11) 2_655 . ? O5 Zn2 O4 125.96(10) 2_655 2_755 ? O1 Zn2 O4 95.25(11) . 2_755 ? O5 Zn2 N2 107.33(12) 2_655 . ? O1 Zn2 N2 90.61(12) . . ? O4 Zn2 N2 125.17(12) 2_755 . ? O5 Zn2 N1 95.49(12) 2_655 . ? O1 Zn2 N1 164.95(12) . . ? O4 Zn2 N1 85.58(12) 2_755 . ? N2 Zn2 N1 76.80(14) . . ? O1 C1 O2 127.2(3) . . ? O1 C1 C2 117.2(3) . . ? O2 C1 C2 115.6(3) . . ? C7 C2 C3 118.8(3) . . ? C7 C2 C1 121.2(3) . . ? C3 C2 C1 120.0(3) . . ? C2 C3 C4 122.0(3) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 C8 118.2(3) . . ? C5 C4 C8 122.6(3) . . ? C6 C5 C4 118.0(3) . . ? C6 C5 C9 116.2(3) . . ? C4 C5 C9 125.7(3) . . ? C7 C6 C5 122.1(3) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C2 C7 C6 119.9(3) . . ? C2 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? O3 C8 O4 125.0(3) . . ? O3 C8 C4 117.5(3) . . ? O4 C8 C4 117.5(3) . . ? C15 C9 C10 118.4(3) . . ? C15 C9 C5 119.6(3) . . ? C10 C9 C5 121.6(3) . . ? C12 C10 C9 120.0(3) . . ? C12 C10 C11 117.6(3) . . ? C9 C10 C11 122.4(3) . . ? O5 C11 O6 124.1(3) . . ? O5 C11 C10 117.8(3) . . ? O6 C11 C10 118.2(3) . . ? C13 C12 C10 120.9(3) . . ? C13 C12 H12 119.5 . . ? C10 C12 H12 119.5 . . ? C12 C13 C14 119.0(3) . . ? C12 C13 C16 120.7(3) . . ? C14 C13 C16 120.2(3) . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C9 121.2(3) . . ? C14 C15 H15 119.4 . . ? C9 C15 H15 119.4 . . ? O8 C16 O7 121.3(3) . . ? O8 C16 C13 120.5(4) . . ? O7 C16 C13 118.2(3) . . ? N1 C17 C18 121.7(6) . . ? N1 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C19 C18 C17 119.0(6) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C20 C19 C18 119.5(5) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 119.4(6) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? N1 C21 C20 120.9(5) . . ? N1 C21 C22 115.7(4) . . ? C20 C21 C22 123.3(5) . . ? N2 C22 C23 120.5(5) . . ? N2 C22 C21 115.8(4) . . ? C23 C22 C21 123.7(4) . . ? C24 C23 C22 120.3(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.2(5) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 119.6(6) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? N2 C26 C25 122.2(5) . . ? N2 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C28 C27 N3 126.5(8) . . ? C28 C27 H27 116.7 . . ? N3 C27 H27 116.7 . . ? C27 C28 C29 110.0(11) . . ? C27 C28 H28 125.0 . . ? C29 C28 H28 125.0 . . ? C28 C29 C30 128.4(10) . . ? C28 C29 H29 115.8 . . ? C30 C29 H29 115.8 . . ? C31 C30 C29 114.9(8) . . ? C31 C30 H30 122.6 . . ? C29 C30 H30 122.6 . . ? N3 C31 C30 120.7(7) . . ? N3 C31 C31 117.4(8) . 3_556 ? C30 C31 C31 121.8(9) . 3_556 ? C17 N1 C21 119.4(4) . . ? C17 N1 Zn2 125.5(3) . . ? C21 N1 Zn2 114.7(3) . . ? C26 N2 C22 118.2(4) . . ? C26 N2 Zn2 125.3(3) . . ? C22 N2 Zn2 116.4(3) . . ? C31 N3 C27 119.4(7) . . ? C1 O1 Zn2 132.1(2) . . ? C1 O2 Zn1 139.7(2) . 4_666 ? C8 O3 Zn1 123.1(2) . 3_755 ? C8 O4 Zn2 142.3(2) . 2_745 ? C11 O5 Zn2 118.1(2) . 2_645 ? C11 O6 Zn1 132.5(2) . 3_655 ? C16 O7 Zn1 99.6(2) . . ? C16 O8 Zn1 80.5(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.480 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.077 # Attachment 'complex1-8_2new1.txt' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 744732' #TrackingRef 'complex1-8_2new1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H18 N2 O9 Zn' _chemical_formula_weight 567.79 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0122(9) _cell_length_b 17.3729(18) _cell_length_c 15.2421(15) _cell_angle_alpha 90.00 _cell_angle_beta 98.6840(10) _cell_angle_gamma 90.00 _cell_volume 2359.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2162 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 21.37 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8096 _exptl_absorpt_correction_T_max 0.8521 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12096 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4180 _reflns_number_gt 2884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.4920P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4180 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0789 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 -0.03854(5) 0.11783(3) 0.76650(3) 0.03646(16) Uani 1 1 d . . . C1 C 0.0702(4) 0.1570(2) 0.5993(2) 0.0339(9) Uani 1 1 d . . . C2 C 0.1987(4) 0.1574(2) 0.5469(2) 0.0298(8) Uani 1 1 d . . . C3 C 0.2095(4) 0.2170(2) 0.4879(2) 0.0328(8) Uani 1 1 d . . . H3 H 0.1357 0.2549 0.4808 0.039 Uiso 1 1 calc R . . C4 C 0.3272(4) 0.2218(2) 0.4394(2) 0.0320(8) Uani 1 1 d . . . C5 C 0.4346(4) 0.1646(2) 0.4493(2) 0.0431(10) Uani 1 1 d . . . H5 H 0.5131 0.1662 0.4162 0.052 Uiso 1 1 calc R . . C6 C 0.4262(4) 0.1048(2) 0.5081(3) 0.0437(10) Uani 1 1 d . . . H6 H 0.5002 0.0671 0.5148 0.052 Uiso 1 1 calc R . . C7 C 0.3093(4) 0.1002(2) 0.5573(2) 0.0333(9) Uani 1 1 d . . . C8 C 0.3379(4) 0.2885(2) 0.3782(2) 0.0388(9) Uani 1 1 d . . . C9 C 0.2994(4) 0.0309(2) 0.6153(2) 0.0343(9) Uani 1 1 d . . . C10 C 0.3779(4) 0.0238(2) 0.7010(2) 0.0360(9) Uani 1 1 d . . . C11 C 0.3641(4) -0.0438(2) 0.7484(3) 0.0428(10) Uani 1 1 d . . . H11 H 0.4161 -0.0484 0.8056 0.051 Uiso 1 1 calc R . . C12 C 0.2758(5) -0.1037(2) 0.7128(3) 0.0447(10) Uani 1 1 d . . . C13 C 0.1980(5) -0.0970(2) 0.6284(3) 0.0500(11) Uani 1 1 d . . . H13 H 0.1376 -0.1372 0.6036 0.060 Uiso 1 1 calc R . . C14 C 0.2097(4) -0.0304(2) 0.5803(3) 0.0437(10) Uani 1 1 d . . . H14 H 0.1565 -0.0264 0.5232 0.052 Uiso 1 1 calc R . . C15 C 0.4737(4) 0.0866(2) 0.7428(3) 0.0408(10) Uani 1 1 d . . . C16 C 0.2725(6) -0.1737(3) 0.7677(3) 0.0648(14) Uani 1 1 d . . . C17 C -0.1705(6) -0.0452(3) 0.7490(3) 0.0627(13) Uani 1 1 d . . . H17 H -0.2350 -0.0253 0.7009 0.075 Uiso 1 1 calc R . . C18 C -0.1856(8) -0.1218(3) 0.7725(4) 0.0885(18) Uani 1 1 d . . . H18 H -0.2597 -0.1525 0.7411 0.106 Uiso 1 1 calc R . . C19 C -0.0902(8) -0.1510(3) 0.8424(4) 0.0913(19) Uani 1 1 d . . . H19 H -0.0975 -0.2024 0.8585 0.110 Uiso 1 1 calc R . . C20 C 0.0171(6) -0.1043(3) 0.8890(3) 0.0681(14) Uani 1 1 d . . . H20 H 0.0817 -0.1235 0.9374 0.082 Uiso 1 1 calc R . . C21 C 0.0279(5) -0.0283(2) 0.8631(3) 0.0465(10) Uani 1 1 d . . . C22 C 0.1388(4) 0.0262(2) 0.9093(3) 0.0425(10) Uani 1 1 d . . . C23 C 0.2434(6) 0.0057(3) 0.9814(3) 0.0694(14) Uani 1 1 d . . . H23 H 0.2475 -0.0444 1.0031 0.083 Uiso 1 1 calc R . . C24 C 0.3408(6) 0.0607(4) 1.0206(3) 0.0843(18) Uani 1 1 d . . . H24 H 0.4135 0.0475 1.0682 0.101 Uiso 1 1 calc R . . C25 C 0.3316(6) 0.1345(3) 0.9899(3) 0.0723(15) Uani 1 1 d . . . H25 H 0.3948 0.1726 1.0172 0.087 Uiso 1 1 calc R . . C26 C 0.2267(5) 0.1506(3) 0.9178(3) 0.0564(12) Uani 1 1 d . . . H26 H 0.2215 0.2005 0.8955 0.068 Uiso 1 1 calc R . . N1 N -0.0666(4) 0.00040(19) 0.7932(2) 0.0442(8) Uani 1 1 d . . . N2 N 0.1307(4) 0.09776(19) 0.8775(2) 0.0420(8) Uani 1 1 d . . . O1 O 0.1002(3) 0.13367(15) 0.67914(15) 0.0404(7) Uani 1 1 d . . . O2 O -0.0541(3) 0.17845(18) 0.56205(17) 0.0555(8) Uani 1 1 d . . . O3 O 0.2707(3) 0.34927(16) 0.38978(17) 0.0512(7) Uani 1 1 d . . . O4 O 0.4201(3) 0.27914(16) 0.31849(17) 0.0515(8) Uani 1 1 d . . . O5 O 0.4861(3) 0.14990(16) 0.71188(18) 0.0493(7) Uani 1 1 d . . . O6 O 0.5511(4) 0.0658(2) 0.8201(2) 0.0829(12) Uani 1 1 d . . . H6A H 0.6109 0.0999 0.8382 0.124 Uiso 1 1 calc R . . O7 O 0.1857(7) -0.2274(2) 0.7294(3) 0.1266(18) Uani 1 1 d . . . H7 H 0.1858 -0.2642 0.7632 0.190 Uiso 1 1 calc R . . O8 O 0.3387(6) -0.1778(2) 0.8431(3) 0.1151(16) Uani 1 1 d . . . O1W O -0.2265(3) 0.11997(19) 0.66618(19) 0.0511(8) Uani 1 1 d . . . H1WA H -0.2060 0.1442 0.6234 0.077 Uiso 1 1 calc R . . H1WB H -0.314(6) 0.141(3) 0.674(3) 0.081(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0468(3) 0.0350(3) 0.0306(2) -0.0011(2) 0.01538(19) 0.0033(2) C1 0.038(2) 0.033(2) 0.032(2) -0.0004(17) 0.0084(17) 0.0008(17) C2 0.036(2) 0.028(2) 0.0264(18) 0.0005(16) 0.0086(16) -0.0005(16) C3 0.040(2) 0.031(2) 0.0292(19) 0.0001(16) 0.0088(16) 0.0060(17) C4 0.044(2) 0.027(2) 0.0274(18) 0.0044(16) 0.0134(17) -0.0008(17) C5 0.055(3) 0.038(2) 0.043(2) 0.0042(19) 0.030(2) 0.005(2) C6 0.049(3) 0.036(3) 0.051(2) 0.0084(19) 0.022(2) 0.0120(18) C7 0.040(2) 0.030(2) 0.032(2) 0.0022(16) 0.0108(17) 0.0035(16) C8 0.050(3) 0.032(2) 0.034(2) 0.0006(18) 0.0038(19) -0.0077(19) C9 0.043(2) 0.028(2) 0.035(2) 0.0052(17) 0.0175(17) 0.0065(17) C10 0.043(2) 0.032(2) 0.035(2) 0.0011(17) 0.0124(18) 0.0038(17) C11 0.054(3) 0.037(3) 0.038(2) 0.0072(19) 0.0096(19) 0.0031(19) C12 0.069(3) 0.029(2) 0.041(2) 0.0036(18) 0.024(2) 0.000(2) C13 0.070(3) 0.033(3) 0.049(3) 0.0000(19) 0.015(2) -0.010(2) C14 0.056(3) 0.041(3) 0.035(2) 0.0024(19) 0.0085(19) -0.004(2) C15 0.047(3) 0.037(2) 0.040(2) 0.0056(19) 0.011(2) 0.0005(19) C16 0.114(4) 0.036(3) 0.047(3) 0.002(2) 0.022(3) -0.015(3) C17 0.086(4) 0.052(3) 0.050(3) -0.010(2) 0.010(3) -0.009(3) C18 0.130(5) 0.057(4) 0.075(4) -0.024(3) 0.006(4) -0.027(3) C19 0.150(6) 0.043(3) 0.080(4) 0.002(3) 0.013(4) -0.023(4) C20 0.105(4) 0.039(3) 0.063(3) 0.006(2) 0.019(3) 0.003(3) C21 0.065(3) 0.039(3) 0.039(2) 0.004(2) 0.019(2) 0.004(2) C22 0.054(3) 0.040(3) 0.036(2) 0.0045(19) 0.0156(19) 0.004(2) C23 0.085(4) 0.063(4) 0.055(3) 0.020(3) -0.003(3) 0.007(3) C24 0.084(4) 0.096(5) 0.064(3) 0.020(3) -0.016(3) -0.011(4) C25 0.070(4) 0.086(4) 0.056(3) 0.004(3) -0.005(3) -0.021(3) C26 0.062(3) 0.056(3) 0.051(3) 0.007(2) 0.008(2) -0.010(2) N1 0.057(2) 0.040(2) 0.0364(19) -0.0075(16) 0.0104(17) -0.0018(17) N2 0.052(2) 0.041(2) 0.0355(18) 0.0029(15) 0.0129(16) -0.0008(16) O1 0.0402(16) 0.0516(19) 0.0323(14) 0.0047(12) 0.0148(12) 0.0079(12) O2 0.0424(18) 0.085(2) 0.0401(16) 0.0192(16) 0.0110(13) 0.0109(16) O3 0.070(2) 0.0349(17) 0.0483(17) 0.0086(14) 0.0074(15) 0.0080(15) O4 0.071(2) 0.0470(19) 0.0424(16) 0.0057(14) 0.0285(15) -0.0092(15) O5 0.0573(18) 0.0322(17) 0.0603(18) 0.0056(15) 0.0146(14) -0.0015(14) O6 0.104(3) 0.073(3) 0.060(2) 0.0222(19) -0.025(2) -0.041(2) O7 0.247(6) 0.059(3) 0.082(3) 0.000(2) 0.055(3) -0.051(3) O8 0.219(5) 0.062(3) 0.065(3) 0.018(2) 0.024(3) -0.004(3) O1W 0.0417(18) 0.065(2) 0.0487(17) 0.0058(16) 0.0147(14) 0.0019(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.978(2) . ? Zn1 O4 2.015(3) 4_566 ? Zn1 N1 2.103(3) . ? Zn1 O1W 2.104(3) . ? Zn1 N2 2.129(3) . ? C1 O2 1.235(4) . ? C1 O1 1.272(4) . ? C1 C2 1.503(5) . ? C2 C3 1.385(5) . ? C2 C7 1.399(5) . ? C3 C4 1.385(5) . ? C3 H3 0.9300 . ? C4 C5 1.379(5) . ? C4 C8 1.499(5) . ? C5 C6 1.381(5) . ? C5 H5 0.9300 . ? C6 C7 1.384(5) . ? C6 H6 0.9300 . ? C7 C9 1.505(5) . ? C8 O3 1.243(4) . ? C8 O4 1.268(4) . ? C9 C10 1.394(5) . ? C9 C14 1.393(5) . ? C10 C11 1.394(5) . ? C10 C15 1.475(5) . ? C11 C12 1.370(5) . ? C11 H11 0.9300 . ? C12 C13 1.374(5) . ? C12 C16 1.480(6) . ? C13 C14 1.382(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O5 1.209(4) . ? C15 O6 1.325(4) . ? C16 O8 1.214(5) . ? C16 O7 1.298(6) . ? C17 N1 1.330(5) . ? C17 C18 1.389(7) . ? C17 H17 0.9300 . ? C18 C19 1.362(7) . ? C18 H18 0.9300 . ? C19 C20 1.375(7) . ? C19 H19 0.9300 . ? C20 C21 1.385(6) . ? C20 H20 0.9300 . ? C21 N1 1.355(5) . ? C21 C22 1.476(6) . ? C22 N2 1.332(5) . ? C22 C23 1.383(6) . ? C23 C24 1.371(7) . ? C23 H23 0.9300 . ? C24 C25 1.363(7) . ? C24 H24 0.9300 . ? C25 C26 1.366(6) . ? C25 H25 0.9300 . ? C26 N2 1.344(5) . ? C26 H26 0.9300 . ? O4 Zn1 2.015(3) 4_665 ? O6 H6A 0.8200 . ? O7 H7 0.8200 . ? O1W H1WA 0.8200 . ? O1W H1WB 0.89(5) . ? 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 O4 108.32(11) . 4_566 ? O1 Zn1 N1 111.83(12) . . ? O4 Zn1 N1 138.66(12) 4_566 . ? O1 Zn1 O1W 91.69(11) . . ? O4 Zn1 O1W 95.37(12) 4_566 . ? N1 Zn1 O1W 92.90(13) . . ? O1 Zn1 N2 96.22(11) . . ? O4 Zn1 N2 89.18(12) 4_566 . ? N1 Zn1 N2 77.29(13) . . ? O1W Zn1 N2 169.16(12) . . ? O2 C1 O1 125.7(3) . . ? O2 C1 C2 118.2(3) . . ? O1 C1 C2 116.2(3) . . ? C3 C2 C7 119.1(3) . . ? C3 C2 C1 118.9(3) . . ? C7 C2 C1 122.0(3) . . ? C2 C3 C4 121.7(3) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 118.7(3) . . ? C5 C4 C8 121.0(3) . . ? C3 C4 C8 120.3(3) . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 121.0(3) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C6 C7 C2 119.0(3) . . ? C6 C7 C9 118.8(3) . . ? C2 C7 C9 122.0(3) . . ? O3 C8 O4 124.1(4) . . ? O3 C8 C4 119.4(3) . . ? O4 C8 C4 116.5(3) . . ? C10 C9 C14 118.3(3) . . ? C10 C9 C7 123.7(3) . . ? C14 C9 C7 117.9(3) . . ? C9 C10 C11 119.2(4) . . ? C9 C10 C15 121.4(3) . . ? C11 C10 C15 119.4(3) . . ? C12 C11 C10 121.7(4) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C13 119.3(4) . . ? C11 C12 C16 117.4(4) . . ? C13 C12 C16 123.3(4) . . ? C12 C13 C14 119.9(4) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C13 C14 C9 121.5(4) . . ? C13 C14 H14 119.2 . . ? C9 C14 H14 119.2 . . ? O5 C15 O6 121.8(4) . . ? O5 C15 C10 126.0(4) . . ? O6 C15 C10 112.2(4) . . ? O8 C16 O7 124.1(5) . . ? O8 C16 C12 122.3(5) . . ? O7 C16 C12 113.5(5) . . ? N1 C17 C18 121.9(5) . . ? N1 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C19 C18 C17 119.0(5) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 119.6(5) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C19 C20 C21 119.3(5) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? N1 C21 C20 120.8(4) . . ? N1 C21 C22 116.0(4) . . ? C20 C21 C22 123.2(4) . . ? N2 C22 C23 121.4(4) . . ? N2 C22 C21 115.5(4) . . ? C23 C22 C21 123.1(4) . . ? C24 C23 C22 118.8(5) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C25 C24 C23 120.2(5) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 117.9(5) . . ? C24 C25 H25 121.1 . . ? C26 C25 H25 121.1 . . ? N2 C26 C25 123.2(5) . . ? N2 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? C17 N1 C21 119.3(4) . . ? C17 N1 Zn1 125.2(3) . . ? C21 N1 Zn1 115.5(3) . . ? C22 N2 C26 118.4(4) . . ? C22 N2 Zn1 115.8(3) . . ? C26 N2 Zn1 125.9(3) . . ? C1 O1 Zn1 128.6(2) . . ? C8 O4 Zn1 109.4(2) . 4_665 ? C15 O6 H6A 109.5 . . ? C16 O7 H7 109.5 . . ? Zn1 O1W H1WA 109.5 . . ? Zn1 O1W H1WB 123(3) . . ? H1WA O1W H1WB 101.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6A O3 0.82 1.77 2.566(4) 163.6 4_666 O7 H7 O5 0.82 2.23 2.856(5) 134.0 2_546 O7 H7 O1 0.82 2.67 3.268(6) 131.1 2_546 O1W H1WA O2 0.82 1.87 2.590(4) 146.3 . O1W H1WB O5 0.89(5) 1.98(5) 2.830(4) 159(4) 1_455 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.382 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.065 # complex 1.cif===END data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 744733' #TrackingRef 'complex1-8_2new1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H34 N4 O18 Zn3' _chemical_formula_weight 1198.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7902(15) _cell_length_b 11.4610(19) _cell_length_c 12.866(2) _cell_angle_alpha 85.175(2) _cell_angle_beta 72.094(2) _cell_angle_gamma 69.382(2) _cell_volume 1154.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1195 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 22.76 _exptl_crystal_description block _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 1.635 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7358 _exptl_absorpt_correction_T_max 0.7916 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6051 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4034 _reflns_number_gt 2806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0552P)^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 4034 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1090 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 0.58156(7) 0.36016(5) 0.28071(5) 0.0302(2) Uani 1 1 d . . . Zn2 Zn 0.5000 0.5000 0.5000 0.0291(2) Uani 1 2 d S . . C1 C 0.8254(6) 0.2430(5) 0.4017(4) 0.0287(12) Uani 1 1 d . . . C2 C 0.9138(6) 0.2601(4) 0.4789(4) 0.0257(11) Uani 1 1 d . . . C3 C 1.0509(6) 0.3011(4) 0.4394(4) 0.0277(11) Uani 1 1 d . . . H3 H 1.0926 0.3111 0.3647 0.033 Uiso 1 1 calc R . . C4 C 1.1273(6) 0.3277(4) 0.5104(4) 0.0247(11) Uani 1 1 d . . . C5 C 1.0622(7) 0.3130(5) 0.6207(4) 0.0387(14) Uani 1 1 d . . . H5 H 1.1085 0.3341 0.6692 0.046 Uiso 1 1 calc R . . C6 C 0.9286(7) 0.2671(5) 0.6613(4) 0.0380(13) Uani 1 1 d . . . H6 H 0.8888 0.2556 0.7358 0.046 Uiso 1 1 calc R . . C7 C 0.8551(6) 0.2385(4) 0.5901(4) 0.0287(12) Uani 1 1 d . . . C8 C 0.7165(6) 0.1827(4) 0.6298(4) 0.0311(12) Uani 1 1 d . . . C9 C 0.5584(6) 0.2479(4) 0.7025(4) 0.0285(12) Uani 1 1 d . . . C10 C 0.4339(6) 0.1959(4) 0.7349(4) 0.0292(12) Uani 1 1 d . . . H10 H 0.3313 0.2384 0.7863 0.035 Uiso 1 1 calc R . . C11 C 0.4569(6) 0.0814(4) 0.6931(4) 0.0300(12) Uani 1 1 d . . . C12 C 0.6136(6) 0.0156(5) 0.6218(5) 0.0397(14) Uani 1 1 d . . . H12 H 0.6327 -0.0624 0.5942 0.048 Uiso 1 1 calc R . . C13 C 0.7409(7) 0.0661(5) 0.5920(5) 0.0414(14) Uani 1 1 d . . . H13 H 0.8465 0.0205 0.5451 0.050 Uiso 1 1 calc R . . C14 C 1.2786(6) 0.3687(4) 0.4643(4) 0.0270(11) Uani 1 1 d . . . C15 C 0.5166(7) 0.3782(5) 0.7406(4) 0.0334(12) Uani 1 1 d . . . C16 C 0.3122(7) 0.0334(5) 0.7237(4) 0.0327(12) Uani 1 1 d . . . C17 C 0.9118(7) 0.4270(5) 0.1983(5) 0.0474(15) Uani 1 1 d . . . H17 H 0.8673 0.4762 0.2618 0.057 Uiso 1 1 calc R . . C18 C 1.0697(8) 0.4204(6) 0.1298(5) 0.0501(16) Uani 1 1 d . . . H18 H 1.1305 0.4648 0.1460 0.060 Uiso 1 1 calc R . . C19 C 1.1344(8) 0.3465(6) 0.0370(5) 0.0570(17) Uani 1 1 d . . . H19 H 1.2407 0.3404 -0.0110 0.068 Uiso 1 1 calc R . . C20 C 1.0430(7) 0.2817(5) 0.0148(5) 0.0483(15) Uani 1 1 d . . . H20 H 1.0871 0.2308 -0.0477 0.058 Uiso 1 1 calc R . . C21 C 0.8844(7) 0.2927(5) 0.0863(4) 0.0364(13) Uani 1 1 d . . . C22 C 0.7698(7) 0.2319(5) 0.0699(4) 0.0365(13) Uani 1 1 d . . . C23 C 0.8106(8) 0.1583(5) -0.0221(5) 0.0510(16) Uani 1 1 d . . . H23 H 0.9156 0.1419 -0.0750 0.061 Uiso 1 1 calc R . . C24 C 0.6943(9) 0.1102(6) -0.0338(5) 0.0602(18) Uani 1 1 d . . . H24 H 0.7194 0.0616 -0.0952 0.072 Uiso 1 1 calc R . . C25 C 0.5401(9) 0.1344(6) 0.0459(5) 0.0581(18) Uani 1 1 d . . . H25 H 0.4589 0.1035 0.0390 0.070 Uiso 1 1 calc R . . C26 C 0.5089(7) 0.2060(5) 0.1366(5) 0.0438(14) Uani 1 1 d . . . H26 H 0.4061 0.2209 0.1916 0.053 Uiso 1 1 calc R . . N1 N 0.8196(5) 0.3656(4) 0.1776(3) 0.0346(10) Uani 1 1 d . . . N2 N 0.6207(5) 0.2544(4) 0.1482(3) 0.0341(10) Uani 1 1 d . . . O1 O 0.6756(4) 0.3246(3) 0.4123(3) 0.0288(8) Uani 1 1 d . . . O2 O 0.8947(4) 0.1579(3) 0.3329(3) 0.0378(9) Uani 1 1 d . . . O3 O 1.3597(4) 0.3396(3) 0.3652(3) 0.0352(9) Uani 1 1 d . . . O4 O 1.3136(4) 0.4267(3) 0.5280(3) 0.0305(8) Uani 1 1 d . . . O5 O 0.5093(4) 0.4614(3) 0.6665(3) 0.0317(8) Uani 1 1 d . . . O6 O 0.4838(6) 0.4032(4) 0.8361(3) 0.0651(13) Uani 1 1 d . . . O7 O 0.1863(5) 0.0752(3) 0.7988(3) 0.0489(11) Uani 1 1 d . . . O8 O 0.3371(5) -0.0576(3) 0.6580(3) 0.0481(10) Uani 1 1 d . . . H8 H 0.2573 -0.0837 0.6793 0.072 Uiso 1 1 calc R . . O9 O 0.6204(12) 0.4900(9) 0.9578(7) 0.079(3) Uani 0.50 1 d P . . 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(3) 0.0355(4) 0.0330(4) -0.0092(3) -0.0028(3) -0.0140(3) Zn2 0.0240(5) 0.0359(5) 0.0325(5) -0.0080(4) -0.0038(4) -0.0181(4) C1 0.020(3) 0.032(3) 0.037(3) -0.003(2) 0.001(2) -0.019(2) C2 0.014(3) 0.020(3) 0.040(3) -0.003(2) -0.004(2) -0.006(2) C3 0.020(3) 0.025(3) 0.038(3) -0.001(2) -0.005(2) -0.010(2) C4 0.017(3) 0.024(3) 0.035(3) 0.000(2) -0.007(2) -0.011(2) C5 0.034(3) 0.055(4) 0.043(3) 0.006(3) -0.019(3) -0.028(3) C6 0.034(3) 0.057(4) 0.031(3) 0.006(3) -0.008(2) -0.027(3) C7 0.021(3) 0.028(3) 0.039(3) 0.001(2) -0.007(2) -0.011(2) C8 0.027(3) 0.027(3) 0.038(3) 0.004(2) -0.005(2) -0.013(2) C9 0.030(3) 0.026(3) 0.034(3) -0.002(2) -0.010(2) -0.014(2) C10 0.021(3) 0.031(3) 0.032(3) -0.004(2) -0.001(2) -0.010(2) C11 0.023(3) 0.024(3) 0.044(3) 0.003(2) -0.010(2) -0.011(2) C12 0.029(3) 0.025(3) 0.062(4) -0.008(3) -0.003(3) -0.012(2) C13 0.023(3) 0.031(3) 0.061(4) -0.006(3) 0.003(3) -0.009(2) C14 0.016(3) 0.029(3) 0.037(3) -0.001(2) -0.007(2) -0.009(2) C15 0.031(3) 0.036(3) 0.037(3) -0.004(3) -0.008(2) -0.017(3) C16 0.031(3) 0.034(3) 0.033(3) -0.003(2) -0.005(3) -0.013(3) C17 0.040(4) 0.051(4) 0.052(4) -0.002(3) -0.010(3) -0.018(3) C18 0.043(4) 0.063(4) 0.053(4) 0.004(3) -0.013(3) -0.030(3) C19 0.036(4) 0.084(5) 0.048(4) 0.002(3) 0.004(3) -0.031(4) C20 0.034(3) 0.066(4) 0.039(4) -0.008(3) 0.004(3) -0.020(3) C21 0.030(3) 0.041(3) 0.036(3) 0.006(3) -0.005(3) -0.015(3) C22 0.037(3) 0.034(3) 0.035(3) 0.000(2) -0.009(3) -0.010(3) C23 0.046(4) 0.059(4) 0.043(4) -0.016(3) -0.001(3) -0.018(3) C24 0.063(5) 0.073(5) 0.047(4) -0.019(3) -0.009(4) -0.029(4) C25 0.059(4) 0.057(4) 0.066(5) -0.019(3) -0.014(4) -0.027(4) C26 0.040(4) 0.043(4) 0.045(4) -0.010(3) -0.006(3) -0.014(3) N1 0.026(2) 0.041(3) 0.038(3) -0.001(2) -0.007(2) -0.015(2) N2 0.030(3) 0.034(3) 0.039(3) -0.004(2) -0.010(2) -0.011(2) O1 0.0179(19) 0.036(2) 0.035(2) -0.0042(16) -0.0065(15) -0.0126(16) O2 0.028(2) 0.037(2) 0.048(2) -0.0138(18) -0.0055(17) -0.0131(17) O3 0.027(2) 0.047(2) 0.038(2) -0.0112(17) -0.0047(17) -0.0215(18) O4 0.0252(19) 0.037(2) 0.034(2) -0.0080(16) -0.0044(16) -0.0184(17) O5 0.035(2) 0.027(2) 0.033(2) -0.0022(16) -0.0059(16) -0.0131(17) O6 0.110(4) 0.049(3) 0.038(3) -0.008(2) -0.026(3) -0.024(3) O7 0.034(2) 0.058(3) 0.050(3) -0.019(2) 0.0124(19) -0.027(2) O8 0.038(2) 0.055(3) 0.058(3) -0.018(2) 0.000(2) -0.031(2) O9 0.084(7) 0.120(8) 0.060(6) -0.001(6) -0.022(6) -0.064(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 2.004(3) 1_455 ? Zn1 O5 2.008(3) 2_666 ? Zn1 N2 2.046(4) . ? Zn1 O1 2.055(3) . ? Zn1 N1 2.125(4) . ? Zn2 O4 2.019(3) 1_455 ? Zn2 O4 2.019(3) 2_766 ? Zn2 O5 2.171(3) . ? Zn2 O5 2.171(3) 2_666 ? Zn2 O1 2.196(3) . ? Zn2 O1 2.196(3) 2_666 ? Zn2 Zn1 3.1226(7) 2_666 ? C1 O2 1.225(6) . ? C1 O1 1.293(6) . ? C1 C2 1.499(6) . ? C2 C3 1.384(6) . ? C2 C7 1.396(7) . ? C3 C4 1.395(6) . ? C3 H3 0.9300 . ? C4 C5 1.378(7) . ? C4 C14 1.500(6) . ? C5 C6 1.392(6) . ? C5 H5 0.9300 . ? C6 C7 1.388(7) . ? C6 H6 0.9300 . ? C7 C8 1.505(6) . ? C8 C13 1.383(6) . ? C8 C9 1.397(7) . ? C9 C10 1.364(6) . ? C9 C15 1.494(6) . ? C10 C11 1.386(6) . ? C10 H10 0.9300 . ? C11 C12 1.384(7) . ? C11 C16 1.491(6) . ? C12 C13 1.374(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O3 1.261(6) . ? C14 O4 1.265(5) . ? C15 O6 1.207(6) . ? C15 O5 1.290(6) . ? C16 O7 1.197(6) . ? C16 O8 1.313(6) . ? C17 N1 1.338(6) . ? C17 C18 1.376(8) . ? C17 H17 0.9300 . ? C18 C19 1.371(8) . ? C18 H18 0.9300 . ? C19 C20 1.370(8) . ? C19 H19 0.9300 . ? C20 C21 1.383(7) . ? C20 H20 0.9300 . ? C21 N1 1.349(6) . ? C21 C22 1.481(7) . ? C22 N2 1.339(7) . ? C22 C23 1.392(7) . ? C23 C24 1.370(8) . ? C23 H23 0.9300 . ? C24 C25 1.377(8) . ? C24 H24 0.9300 . ? C25 C26 1.384(8) . ? C25 H25 0.9300 . ? C26 N2 1.335(6) . ? C26 H26 0.9300 . ? O3 Zn1 2.004(3) 1_655 ? O4 Zn2 2.019(3) 1_655 ? O5 Zn1 2.008(3) 2_666 ? O8 H8 0.8200 . ? 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 O5 90.35(13) 1_455 2_666 ? O3 Zn1 N2 95.23(15) 1_455 . ? O5 Zn1 N2 141.06(15) 2_666 . ? O3 Zn1 O1 93.81(13) 1_455 . ? O5 Zn1 O1 84.54(13) 2_666 . ? N2 Zn1 O1 133.20(15) . . ? O3 Zn1 N1 173.09(15) 1_455 . ? O5 Zn1 N1 95.61(15) 2_666 . ? N2 Zn1 N1 77.93(16) . . ? O1 Zn1 N1 90.23(14) . . ? O4 Zn2 O4 180 1_455 2_766 ? O4 Zn2 O5 89.92(12) 1_455 . ? O4 Zn2 O5 90.08(12) 2_766 . ? O4 Zn2 O5 90.08(12) 1_455 2_666 ? O4 Zn2 O5 89.92(12) 2_766 2_666 ? O5 Zn2 O5 180 . 2_666 ? O4 Zn2 O1 87.24(12) 1_455 . ? O4 Zn2 O1 92.76(12) 2_766 . ? O5 Zn2 O1 102.49(12) . . ? O5 Zn2 O1 77.51(12) 2_666 . ? O4 Zn2 O1 92.76(12) 1_455 2_666 ? O4 Zn2 O1 87.23(12) 2_766 2_666 ? O5 Zn2 O1 77.51(12) . 2_666 ? O5 Zn2 O1 102.49(12) 2_666 2_666 ? O1 Zn2 O1 180 . 2_666 ? O4 Zn2 Zn1 103.95(9) 1_455 2_666 ? O4 Zn2 Zn1 76.05(9) 2_766 2_666 ? O5 Zn2 Zn1 39.70(8) . 2_666 ? O5 Zn2 Zn1 140.30(8) 2_666 2_666 ? O1 Zn2 Zn1 138.99(8) . 2_666 ? O1 Zn2 Zn1 41.01(8) 2_666 2_666 ? O2 C1 O1 123.8(5) . . ? O2 C1 C2 120.9(5) . . ? O1 C1 C2 115.3(4) . . ? C3 C2 C7 120.4(4) . . ? C3 C2 C1 119.3(4) . . ? C7 C2 C1 120.3(4) . . ? C2 C3 C4 120.7(5) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 118.4(4) . . ? C5 C4 C14 122.4(4) . . ? C3 C4 C14 119.2(4) . . ? C4 C5 C6 121.5(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C7 C6 C5 119.8(5) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 119.0(4) . . ? C6 C7 C8 121.5(4) . . ? C2 C7 C8 119.5(4) . . ? C13 C8 C9 118.0(4) . . ? C13 C8 C7 120.5(4) . . ? C9 C8 C7 121.5(4) . . ? C10 C9 C8 120.1(4) . . ? C10 C9 C15 118.3(5) . . ? C8 C9 C15 121.5(4) . . ? C9 C10 C11 121.5(5) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 118.7(4) . . ? C12 C11 C16 121.8(4) . . ? C10 C11 C16 119.5(4) . . ? C13 C12 C11 119.7(5) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C8 121.8(5) . . ? C12 C13 H13 119.1 . . ? C8 C13 H13 119.1 . . ? O3 C14 O4 126.6(4) . . ? O3 C14 C4 115.8(4) . . ? O4 C14 C4 117.5(4) . . ? O6 C15 O5 123.0(5) . . ? O6 C15 C9 121.1(5) . . ? O5 C15 C9 115.8(4) . . ? O7 C16 O8 124.1(5) . . ? O7 C16 C11 123.5(5) . . ? O8 C16 C11 112.5(4) . . ? N1 C17 C18 122.9(6) . . ? N1 C17 H17 118.6 . . ? C18 C17 H17 118.6 . . ? C19 C18 C17 117.9(5) . . ? C19 C18 H18 121.0 . . ? C17 C18 H18 121.0 . . ? C20 C19 C18 120.2(6) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 119.3(6) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? N1 C21 C20 120.9(5) . . ? N1 C21 C22 114.3(4) . . ? C20 C21 C22 124.8(5) . . ? N2 C22 C23 121.2(5) . . ? N2 C22 C21 116.0(5) . . ? C23 C22 C21 122.8(5) . . ? C24 C23 C22 119.3(6) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 119.6(6) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C24 C25 C26 118.3(6) . . ? C24 C25 H25 120.9 . . ? C26 C25 H25 120.9 . . ? N2 C26 C25 122.6(6) . . ? N2 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C17 N1 C21 118.8(5) . . ? C17 N1 Zn1 126.4(4) . . ? C21 N1 Zn1 114.6(3) . . ? C26 N2 C22 119.0(5) . . ? C26 N2 Zn1 124.2(4) . . ? C22 N2 Zn1 116.8(3) . . ? C1 O1 Zn1 119.3(3) . . ? C1 O1 Zn2 141.4(3) . . ? Zn1 O1 Zn2 94.48(13) . . ? C14 O3 Zn1 127.3(3) . 1_655 ? C14 O4 Zn2 130.5(3) . 1_655 ? C15 O5 Zn1 116.3(3) . 2_666 ? C15 O5 Zn2 144.9(3) . . ? Zn1 O5 Zn2 96.62(13) 2_666 . ? C16 O8 H8 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8 O2 0.82 1.87 2.640(4) 156.6 2_656 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.682 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.098 # complex 3.cif===END data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 744734' #TrackingRef 'complex1-8_2new1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H24 N4 O9 Zn2' _chemical_formula_weight 787.33 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.4039(14) _cell_length_b 14.2659(13) _cell_length_c 16.5825(16) _cell_angle_alpha 90.00 _cell_angle_beta 111.7120(10) _cell_angle_gamma 90.00 _cell_volume 3165.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4756 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 26.58 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6483 _exptl_absorpt_correction_T_max 0.6932 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16156 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5592 _reflns_number_gt 4229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+1.2189P] 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 5592 _refine_ls_number_parameters 460 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.10216(2) 0.66499(2) 0.19607(2) 0.02713(11) Uani 1 1 d . . . Zn2 Zn 0.37848(2) 0.67412(2) 0.32467(2) 0.02993(11) Uani 1 1 d . . . C1 C 0.0199(3) 0.7226(3) 0.3357(2) 0.0551(10) Uani 1 1 d . . . H1 H 0.0090 0.6587 0.3384 0.066 Uiso 1 1 calc R . . C2 C -0.0073(3) 0.7823(3) 0.3885(3) 0.0687(12) Uani 1 1 d . . . H2 H -0.0353 0.7590 0.4268 0.082 Uiso 1 1 calc R . . C3 C 0.0078(3) 0.8764(3) 0.3835(3) 0.0655(12) Uani 1 1 d . . . H3 H -0.0102 0.9183 0.4181 0.079 Uiso 1 1 calc R . . C4 C 0.0494(3) 0.9080(3) 0.3269(2) 0.0522(10) Uani 1 1 d . . . H4 H 0.0597 0.9718 0.3224 0.063 Uiso 1 1 calc R . . C5 C 0.0762(2) 0.8450(2) 0.2764(2) 0.0348(7) Uani 1 1 d . . . C6 C 0.1198(2) 0.8722(2) 0.2120(2) 0.0353(7) Uani 1 1 d . . . C7 C 0.1407(3) 0.9650(2) 0.1983(3) 0.0551(10) Uani 1 1 d . . . H7 H 0.1315 1.0131 0.2325 0.066 Uiso 1 1 calc R . . C8 C 0.1749(3) 0.9835(3) 0.1333(3) 0.0737(13) Uani 1 1 d . . . H8 H 0.1888 1.0449 0.1226 0.088 Uiso 1 1 calc R . . C9 C 0.1889(3) 0.9116(3) 0.0836(3) 0.0686(13) Uani 1 1 d . . . H9 H 0.2111 0.9238 0.0386 0.082 Uiso 1 1 calc R . . C10 C 0.1695(3) 0.8217(3) 0.1018(2) 0.0499(9) Uani 1 1 d . . . H10 H 0.1799 0.7728 0.0691 0.060 Uiso 1 1 calc R . . C11 C 0.3141(3) 0.8136(3) 0.4337(2) 0.0465(9) Uani 1 1 d . . . H11 H 0.2899 0.7612 0.4530 0.056 Uiso 1 1 calc R . . C12 C 0.3179(3) 0.8972(3) 0.4753(3) 0.0654(12) Uani 1 1 d . . . H12 H 0.2959 0.9016 0.5213 0.078 Uiso 1 1 calc R . . C13 C 0.3548(3) 0.9743(3) 0.4475(3) 0.0719(13) Uani 1 1 d . . . H13 H 0.3596 1.0316 0.4756 0.086 Uiso 1 1 calc R . . C14 C 0.3844(3) 0.9662(3) 0.3782(3) 0.0598(11) Uani 1 1 d . . . H14 H 0.4081 1.0181 0.3579 0.072 Uiso 1 1 calc R . . C15 C 0.3784(2) 0.8794(2) 0.3387(2) 0.0382(8) Uani 1 1 d . . . C16 C 0.4088(2) 0.8631(2) 0.2637(2) 0.0399(8) Uani 1 1 d . . . C17 C 0.4296(3) 0.9344(3) 0.2163(3) 0.0573(10) Uani 1 1 d . . . H17 H 0.4276 0.9966 0.2324 0.069 Uiso 1 1 calc R . . C18 C 0.4531(3) 0.9131(3) 0.1461(3) 0.0646(12) Uani 1 1 d . . . H18 H 0.4660 0.9604 0.1132 0.078 Uiso 1 1 calc R . . C19 C 0.4573(3) 0.8212(4) 0.1248(2) 0.0630(12) Uani 1 1 d . . . H19 H 0.4735 0.8053 0.0772 0.076 Uiso 1 1 calc R . . C20 C 0.4372(3) 0.7521(3) 0.1743(2) 0.0544(10) Uani 1 1 d . . . H20 H 0.4408 0.6897 0.1597 0.065 Uiso 1 1 calc R . . C21 C 0.2114(2) 0.5535(2) 0.34991(19) 0.0319(7) Uani 1 1 d . . . C22 C 0.2195(2) 0.46777(19) 0.40340(17) 0.0269(6) Uani 1 1 d . . . C23 C 0.3128(2) 0.4322(2) 0.45456(18) 0.0293(7) Uani 1 1 d . . . H23 H 0.3702 0.4652 0.4590 0.035 Uiso 1 1 calc R . . C24 C 0.3214(2) 0.3483(2) 0.49903(18) 0.0280(7) Uani 1 1 d . . . C25 C 0.2349(2) 0.30012(19) 0.49666(17) 0.0269(6) Uani 1 1 d . . . C26 C 0.1423(2) 0.3407(2) 0.44917(18) 0.0307(7) Uani 1 1 d . . . H26 H 0.0843 0.3122 0.4494 0.037 Uiso 1 1 calc R . . C27 C 0.1347(2) 0.4215(2) 0.40212(18) 0.0305(7) Uani 1 1 d . . . H27 H 0.0720 0.4453 0.3691 0.037 Uiso 1 1 calc R . . C28 C 0.4249(2) 0.3082(2) 0.54253(19) 0.0310(7) Uani 1 1 d . . . C29 C 0.2733(2) -0.0515(2) 0.68008(18) 0.0309(7) Uani 1 1 d . . . C30 C 0.2577(2) 0.0415(2) 0.63523(18) 0.0282(7) Uani 1 1 d . . . C31 C 0.1879(2) 0.0509(2) 0.55107(18) 0.0280(7) Uani 1 1 d . . . H31 H 0.1461 0.0007 0.5254 0.034 Uiso 1 1 calc R . . C32 C 0.17938(19) 0.1336(2) 0.50482(17) 0.0254(6) Uani 1 1 d . . . C33 C 0.2402(2) 0.2110(2) 0.54403(18) 0.0272(6) Uani 1 1 d . . . C34 C 0.3038(2) 0.2023(2) 0.63059(19) 0.0365(8) Uani 1 1 d . . . H34 H 0.3408 0.2541 0.6589 0.044 Uiso 1 1 calc R . . C35 C 0.3135(2) 0.1195(2) 0.67521(19) 0.0373(8) Uani 1 1 d . . . H35 H 0.3578 0.1157 0.7326 0.045 Uiso 1 1 calc R . . C36 C 0.1036(2) 0.13595(19) 0.41273(19) 0.0279(7) Uani 1 1 d . . . N1 N 0.06130(19) 0.75310(18) 0.28099(16) 0.0355(6) Uani 1 1 d . . . N2 N 0.13596(18) 0.80196(18) 0.16545(16) 0.0332(6) Uani 1 1 d . . . N3 N 0.34373(18) 0.80373(18) 0.36641(16) 0.0350(6) Uani 1 1 d . . . N4 N 0.41267(19) 0.77231(19) 0.24282(16) 0.0392(7) Uani 1 1 d . . . O1 O 0.20974(15) -0.11509(14) 0.65034(13) 0.0372(5) Uani 1 1 d . . . O2 O 0.35284(15) -0.06179(15) 0.74583(13) 0.0425(6) Uani 1 1 d . . . O3 O 0.01292(14) 0.13256(15) 0.40837(12) 0.0369(5) Uani 1 1 d . . . O4 O 0.13036(16) 0.13756(17) 0.35086(13) 0.0448(6) Uani 1 1 d . . . O5 O 0.13362(16) 0.56029(14) 0.28205(13) 0.0407(5) Uani 1 1 d . . . O6 O 0.27953(17) 0.61323(15) 0.37497(14) 0.0430(6) Uani 1 1 d . . . O7 O 0.44314(16) 0.22957(16) 0.52363(16) 0.0531(7) Uani 1 1 d . . . O8 O 0.48807(15) 0.36395(15) 0.59494(14) 0.0453(6) Uani 1 1 d . . . O1W O 0.3229(3) 0.1856(2) 0.3361(3) 0.1166(13) Uani 1 1 d D . . H1WA H 0.3735 0.1619 0.3756 0.140 Uiso 1 1 d RD . . H1WB H 0.2703 0.1851 0.2899 0.140 Uiso 1 1 d RD . . 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 0.02410(19) 0.0273(2) 0.02405(19) 0.00046(14) 0.00194(14) 0.00158(14) Zn2 0.02280(19) 0.0290(2) 0.0300(2) -0.00213(15) 0.00050(15) 0.00026(14) C1 0.069(3) 0.057(3) 0.049(2) -0.0018(19) 0.033(2) -0.008(2) C2 0.071(3) 0.096(4) 0.051(2) -0.013(2) 0.036(2) -0.002(3) C3 0.052(3) 0.080(3) 0.069(3) -0.035(2) 0.028(2) 0.004(2) C4 0.040(2) 0.044(2) 0.067(3) -0.0223(19) 0.0128(19) 0.0036(16) C5 0.0272(16) 0.0326(19) 0.0363(18) -0.0058(14) 0.0021(13) 0.0044(13) C6 0.0238(16) 0.0302(18) 0.0415(19) 0.0067(15) -0.0001(14) 0.0034(13) C7 0.044(2) 0.033(2) 0.080(3) 0.0093(19) 0.013(2) -0.0017(16) C8 0.056(3) 0.050(3) 0.103(4) 0.037(3) 0.016(3) -0.003(2) C9 0.054(3) 0.080(3) 0.072(3) 0.042(3) 0.023(2) -0.001(2) C10 0.041(2) 0.066(3) 0.044(2) 0.0158(18) 0.0165(17) 0.0068(17) C11 0.045(2) 0.053(2) 0.043(2) -0.0011(17) 0.0167(17) 0.0098(16) C12 0.073(3) 0.066(3) 0.060(3) -0.011(2) 0.028(2) 0.020(2) C13 0.080(3) 0.052(3) 0.076(3) -0.023(2) 0.020(3) 0.014(2) C14 0.061(3) 0.035(2) 0.078(3) -0.006(2) 0.020(2) 0.0007(18) C15 0.0292(17) 0.035(2) 0.0421(19) 0.0022(15) 0.0032(14) 0.0039(14) C16 0.0320(18) 0.038(2) 0.041(2) 0.0064(16) 0.0031(15) -0.0021(14) C17 0.046(2) 0.056(3) 0.063(3) 0.015(2) 0.012(2) -0.0078(18) C18 0.045(2) 0.084(3) 0.058(3) 0.024(2) 0.011(2) -0.014(2) C19 0.046(2) 0.106(4) 0.038(2) 0.009(2) 0.0169(18) -0.014(2) C20 0.054(2) 0.064(3) 0.043(2) -0.0086(19) 0.0150(19) -0.0081(19) C21 0.0330(17) 0.0303(18) 0.0318(17) 0.0010(13) 0.0112(14) 0.0039(14) C22 0.0267(16) 0.0263(16) 0.0230(15) 0.0009(12) 0.0036(12) 0.0012(12) C23 0.0253(15) 0.0284(17) 0.0310(16) -0.0011(13) 0.0066(13) -0.0041(12) C24 0.0232(15) 0.0284(17) 0.0268(15) -0.0001(13) 0.0025(12) -0.0006(12) C25 0.0268(16) 0.0238(16) 0.0259(15) 0.0000(12) 0.0050(12) -0.0008(12) C26 0.0216(15) 0.0328(18) 0.0327(16) 0.0020(13) 0.0042(13) -0.0043(12) C27 0.0215(15) 0.0304(17) 0.0322(16) 0.0034(13) 0.0012(12) 0.0002(12) C28 0.0221(15) 0.0321(18) 0.0319(17) 0.0075(14) 0.0019(13) -0.0019(13) C29 0.0278(16) 0.0323(18) 0.0327(17) 0.0056(13) 0.0113(14) -0.0012(13) C30 0.0221(15) 0.0288(17) 0.0311(16) 0.0060(13) 0.0068(13) 0.0015(12) C31 0.0213(15) 0.0284(17) 0.0310(16) -0.0018(13) 0.0061(12) -0.0030(12) C32 0.0199(14) 0.0274(16) 0.0257(15) 0.0005(12) 0.0046(12) 0.0014(12) C33 0.0212(15) 0.0295(17) 0.0272(15) 0.0019(13) 0.0046(12) -0.0011(12) C34 0.0350(18) 0.0323(18) 0.0320(17) 0.0005(14) 0.0006(14) -0.0088(14) C35 0.0343(18) 0.039(2) 0.0265(16) 0.0053(14) -0.0032(13) -0.0062(14) C36 0.0265(16) 0.0205(16) 0.0296(17) 0.0004(13) 0.0020(13) -0.0007(12) N1 0.0405(16) 0.0351(16) 0.0318(14) -0.0025(12) 0.0142(12) -0.0020(12) N2 0.0294(14) 0.0331(15) 0.0355(15) 0.0050(12) 0.0103(12) 0.0022(11) N3 0.0285(14) 0.0368(16) 0.0352(15) 0.0001(12) 0.0064(12) 0.0042(11) N4 0.0375(16) 0.0436(18) 0.0338(15) -0.0011(13) 0.0098(12) -0.0028(12) O1 0.0377(13) 0.0359(13) 0.0360(12) 0.0037(10) 0.0114(10) -0.0100(10) O2 0.0330(12) 0.0393(14) 0.0420(13) 0.0183(10) -0.0018(10) 0.0005(10) O3 0.0236(11) 0.0477(14) 0.0298(11) 0.0054(10) -0.0014(9) -0.0021(9) O4 0.0434(14) 0.0602(16) 0.0267(12) -0.0022(11) 0.0082(10) -0.0010(11) O5 0.0385(13) 0.0377(13) 0.0345(12) 0.0110(10) 0.0004(10) 0.0029(10) O6 0.0487(14) 0.0353(14) 0.0420(13) 0.0027(10) 0.0133(11) -0.0151(11) O7 0.0315(13) 0.0432(16) 0.0695(17) -0.0079(13) 0.0011(12) 0.0084(11) O8 0.0264(12) 0.0384(14) 0.0510(14) -0.0026(11) -0.0090(10) -0.0006(10) O1W 0.138(4) 0.095(3) 0.135(3) -0.003(2) 0.071(3) 0.002(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 O3 1.9590(19) 2 ? Zn1 O5 1.998(2) . ? Zn1 O1 2.086(2) 4_565 ? Zn1 N2 2.120(3) . ? Zn1 N1 2.126(2) . ? Zn2 O8 1.967(2) 3_666 ? Zn2 O2 2.014(2) 4_565 ? Zn2 O6 2.088(2) . ? Zn2 N3 2.099(3) . ? Zn2 N4 2.131(3) . ? C1 N1 1.329(4) . ? C1 C2 1.379(5) . ? C1 H1 0.9300 . ? C2 C3 1.368(6) . ? C2 H2 0.9300 . ? C3 C4 1.363(5) . ? C3 H3 0.9300 . ? C4 C5 1.378(4) . ? C4 H4 0.9300 . ? C5 N1 1.335(4) . ? C5 C6 1.477(4) . ? C6 N2 1.337(4) . ? C6 C7 1.394(4) . ? C7 C8 1.367(6) . ? C7 H7 0.9300 . ? C8 C9 1.376(6) . ? C8 H8 0.9300 . ? C9 C10 1.370(5) . ? C9 H9 0.9300 . ? C10 N2 1.342(4) . ? C10 H10 0.9300 . ? C11 N3 1.341(4) . ? C11 C12 1.369(5) . ? C11 H11 0.9300 . ? C12 C13 1.374(6) . ? C12 H12 0.9300 . ? C13 C14 1.371(5) . ? C13 H13 0.9300 . ? C14 C15 1.389(5) . ? C14 H14 0.9300 . ? C15 N3 1.340(4) . ? C15 C16 1.480(5) . ? C16 N4 1.347(4) . ? C16 C17 1.385(5) . ? C17 C18 1.361(5) . ? C17 H17 0.9300 . ? C18 C19 1.365(6) . ? C18 H18 0.9300 . ? C19 C20 1.381(5) . ? C19 H19 0.9300 . ? C20 N4 1.340(4) . ? C20 H20 0.9300 . ? C21 O6 1.249(3) . ? C21 O5 1.264(3) . ? C21 C22 1.490(4) . ? C22 C27 1.381(4) . ? C22 C23 1.393(4) . ? C23 C24 1.387(4) . ? C23 H23 0.9300 . ? C24 C25 1.411(4) . ? C24 C28 1.508(4) . ? C25 C26 1.399(4) . ? C25 C33 1.482(4) . ? C26 C27 1.374(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 O7 1.219(4) . ? C28 O8 1.277(3) . ? C29 O1 1.253(3) . ? C29 O2 1.264(3) . ? C29 C30 1.497(4) . ? C30 C35 1.389(4) . ? C30 C31 1.393(4) . ? C31 C32 1.388(4) . ? C31 H31 0.9300 . ? C32 C33 1.410(4) . ? C32 C36 1.514(4) . ? C33 C34 1.394(4) . ? C34 C35 1.373(4) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 O4 1.222(3) . ? C36 O3 1.282(3) . ? O1 Zn1 2.086(2) 4_566 ? O2 Zn2 2.014(2) 4_566 ? O3 Zn1 1.9589(19) 2_545 ? O8 Zn2 1.967(2) 3_666 ? O1W H1WA 0.8501 . ? O1W H1WB 0.8550 . ? 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 O5 110.41(9) 2 . ? O3 Zn1 O1 95.59(8) 2 4_565 ? O5 Zn1 O1 90.08(9) . 4_565 ? O3 Zn1 N2 101.54(9) 2 . ? O5 Zn1 N2 148.03(9) . . ? O1 Zn1 N2 87.72(9) 4_565 . ? O3 Zn1 N1 111.97(9) 2 . ? O5 Zn1 N1 90.84(10) . . ? O1 Zn1 N1 150.12(9) 4_565 . ? N2 Zn1 N1 76.01(10) . . ? O8 Zn2 O2 96.82(9) 3_666 4_565 ? O8 Zn2 O6 104.76(9) 3_666 . ? O2 Zn2 O6 86.55(9) 4_565 . ? O8 Zn2 N3 108.19(9) 3_666 . ? O2 Zn2 N3 154.99(9) 4_565 . ? O6 Zn2 N3 87.33(10) . . ? O8 Zn2 N4 102.41(10) 3_666 . ? O2 Zn2 N4 98.03(10) 4_565 . ? O6 Zn2 N4 151.70(9) . . ? N3 Zn2 N4 76.73(10) . . ? N1 C1 C2 122.5(4) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 118.6(4) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 119.1(4) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 121.2(3) . . ? N1 C5 C6 114.9(3) . . ? C4 C5 C6 123.9(3) . . ? N2 C6 C7 121.6(3) . . ? N2 C6 C5 115.5(3) . . ? C7 C6 C5 122.9(3) . . ? C8 C7 C6 118.3(4) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C7 C8 C9 120.2(4) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 118.6(4) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N2 C10 C9 122.1(4) . . ? N2 C10 H10 118.9 . . ? C9 C10 H10 118.9 . . ? N3 C11 C12 123.0(4) . . ? N3 C11 H11 118.5 . . ? C12 C11 H11 118.5 . . ? C11 C12 C13 118.5(4) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? C14 C13 C12 119.5(4) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 119.2(4) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? N3 C15 C14 121.4(3) . . ? N3 C15 C16 115.1(3) . . ? C14 C15 C16 123.4(3) . . ? N4 C16 C17 121.5(3) . . ? N4 C16 C15 114.9(3) . . ? C17 C16 C15 123.6(3) . . ? C18 C17 C16 119.7(4) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 119.1(4) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C18 C19 C20 119.5(4) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? N4 C20 C19 122.0(4) . . ? N4 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? O6 C21 O5 124.9(3) . . ? O6 C21 C22 118.9(3) . . ? O5 C21 C22 116.2(3) . . ? C27 C22 C23 118.9(3) . . ? C27 C22 C21 120.6(3) . . ? C23 C22 C21 120.5(3) . . ? C24 C23 C22 121.0(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 120.1(3) . . ? C23 C24 C28 117.4(2) . . ? C25 C24 C28 122.3(3) . . ? C26 C25 C24 117.5(3) . . ? C26 C25 C33 120.4(3) . . ? C24 C25 C33 122.1(3) . . ? C27 C26 C25 121.7(3) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C26 C27 C22 120.5(3) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? O7 C28 O8 125.5(3) . . ? O7 C28 C24 119.7(3) . . ? O8 C28 C24 114.7(3) . . ? O1 C29 O2 123.5(3) . . ? O1 C29 C30 119.5(3) . . ? O2 C29 C30 116.9(3) . . ? C35 C30 C31 118.5(3) . . ? C35 C30 C29 121.3(3) . . ? C31 C30 C29 120.2(3) . . ? C32 C31 C30 121.2(3) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C33 119.9(2) . . ? C31 C32 C36 117.4(2) . . ? C33 C32 C36 122.8(3) . . ? C34 C33 C32 117.7(3) . . ? C34 C33 C25 120.5(3) . . ? C32 C33 C25 121.7(2) . . ? C35 C34 C33 121.9(3) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C34 C35 C30 120.4(3) . . ? C34 C35 H35 119.8 . . ? C30 C35 H35 119.8 . . ? O4 C36 O3 125.8(3) . . ? O4 C36 C32 120.9(3) . . ? O3 C36 C32 113.3(3) . . ? C1 N1 C5 118.9(3) . . ? C1 N1 Zn1 124.2(2) . . ? C5 N1 Zn1 116.9(2) . . ? C6 N2 C10 119.1(3) . . ? C6 N2 Zn1 116.6(2) . . ? C10 N2 Zn1 124.3(2) . . ? C15 N3 C11 118.4(3) . . ? C15 N3 Zn2 115.6(2) . . ? C11 N3 Zn2 123.7(2) . . ? C20 N4 C16 118.3(3) . . ? C20 N4 Zn2 126.5(2) . . ? C16 N4 Zn2 115.2(2) . . ? C29 O1 Zn1 129.55(19) . 4_566 ? C29 O2 Zn2 122.84(19) . 4_566 ? C36 O3 Zn1 123.51(19) . 2_545 ? C21 O5 Zn1 125.8(2) . . ? C21 O6 Zn2 136.0(2) . . ? C28 O8 Zn2 124.1(2) . 3_666 ? H1WA O1W H1WB 155.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O7 0.85 2.48 3.013(5) 121.7 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.438 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.062 # complex 4.cif===END data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 744735' #TrackingRef 'complex1-8_2new1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 Cd2 N4 O10' _chemical_formula_weight 899.41 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2298(7) _cell_length_b 15.2279(11) _cell_length_c 23.9952(17) _cell_angle_alpha 90.00 _cell_angle_beta 94.9400(10) _cell_angle_gamma 90.00 _cell_volume 3360.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4020 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 23.98 _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 1.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6906 _exptl_absorpt_correction_T_max 0.7764 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17223 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5921 _reflns_number_gt 4618 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+2.9081P] 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 5921 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 Cd1 Cd 0.16477(4) 0.89897(2) 0.631428(14) 0.02673(11) Uani 1 1 d . . . Cd2 Cd 0.15802(4) 0.63395(2) 0.458414(14) 0.02858(11) Uani 1 1 d . . . C1 C 0.3529(5) 0.7662(3) 0.54346(19) 0.0277(11) Uani 1 1 d . . . C2 C 0.4882(5) 0.7252(3) 0.57330(19) 0.0245(10) Uani 1 1 d . . . C3 C 0.5427(5) 0.6466(3) 0.55590(18) 0.0254(10) Uani 1 1 d . . . H3 H 0.4954 0.6175 0.5255 0.031 Uiso 1 1 calc R . . C4 C 0.6673(5) 0.6101(3) 0.58320(18) 0.0239(10) Uani 1 1 d . . . C5 C 0.7404(5) 0.6537(3) 0.62908(18) 0.0227(10) Uani 1 1 d . . . C6 C 0.6835(5) 0.7330(3) 0.64548(19) 0.0295(11) Uani 1 1 d . . . H6 H 0.7311 0.7631 0.6754 0.035 Uiso 1 1 calc R . . C7 C 0.5590(5) 0.7685(3) 0.61887(19) 0.0295(11) Uani 1 1 d . . . H7 H 0.5223 0.8212 0.6313 0.035 Uiso 1 1 calc R . . C8 C 0.7197(5) 0.5226(3) 0.56356(18) 0.0274(11) Uani 1 1 d . . . C9 C 0.8615(5) 0.6116(3) 0.66441(18) 0.0241(10) Uani 1 1 d . . . C10 C 0.9926(5) 0.6540(3) 0.68215(17) 0.0234(10) Uani 1 1 d . . . C11 C 1.0915(5) 0.6129(3) 0.72077(18) 0.0256(10) Uani 1 1 d . . . H11 H 1.1771 0.6419 0.7330 0.031 Uiso 1 1 calc R . . C12 C 1.0655(5) 0.5295(3) 0.74161(18) 0.0263(10) Uani 1 1 d . . . C13 C 0.9354(5) 0.4875(3) 0.72407(19) 0.0303(11) Uani 1 1 d . . . H13 H 0.9149 0.4324 0.7382 0.036 Uiso 1 1 calc R . . C14 C 0.8376(5) 0.5277(3) 0.68586(19) 0.0274(11) Uani 1 1 d . . . H14 H 0.7524 0.4982 0.6738 0.033 Uiso 1 1 calc R . . C15 C 1.0353(5) 0.7433(3) 0.6621(2) 0.0282(11) Uani 1 1 d . . . C16 C 1.1725(6) 0.4878(3) 0.7845(2) 0.0321(12) Uani 1 1 d . . . C17 C 0.3083(6) 1.0359(4) 0.5462(2) 0.0430(14) Uani 1 1 d . . . H17 H 0.3898 1.0014 0.5554 0.052 Uiso 1 1 calc R . . C18 C 0.3198(7) 1.1061(4) 0.5106(2) 0.0498(15) Uani 1 1 d . . . H18 H 0.4083 1.1191 0.4967 0.060 Uiso 1 1 calc R . . C19 C 0.2008(7) 1.1562(4) 0.4961(2) 0.0518(16) Uani 1 1 d . . . H19 H 0.2069 1.2035 0.4719 0.062 Uiso 1 1 calc R . . C20 C 0.0702(6) 1.1362(3) 0.5176(2) 0.0413(13) Uani 1 1 d . . . H20 H -0.0129 1.1692 0.5078 0.050 Uiso 1 1 calc R . . C21 C 0.0663(5) 1.0656(3) 0.55405(19) 0.0286(11) Uani 1 1 d . . . C22 C -0.0672(5) 1.0407(3) 0.58080(19) 0.0266(10) Uani 1 1 d . . . C23 C -0.1969(6) 1.0851(3) 0.5694(2) 0.0394(13) Uani 1 1 d . . . H23 H -0.2036 1.1311 0.5438 0.047 Uiso 1 1 calc R . . C24 C -0.3158(6) 1.0603(4) 0.5964(2) 0.0463(14) Uani 1 1 d . . . H24 H -0.4039 1.0894 0.5890 0.056 Uiso 1 1 calc R . . C25 C -0.3044(6) 0.9924(4) 0.6343(2) 0.0472(15) Uani 1 1 d . . . H25 H -0.3835 0.9749 0.6531 0.057 Uiso 1 1 calc R . . C26 C -0.1710(6) 0.9512(3) 0.6433(2) 0.0423(13) Uani 1 1 d . . . H26 H -0.1615 0.9056 0.6692 0.051 Uiso 1 1 calc R . . C27 C 0.3139(8) 0.7264(4) 0.3583(3) 0.0634(19) Uani 1 1 d . . . H27 H 0.3980 0.7066 0.3786 0.076 Uiso 1 1 calc R . . C28 C 0.3259(10) 0.7831(5) 0.3138(3) 0.086(3) Uani 1 1 d . . . H28 H 0.4170 0.7987 0.3032 0.103 Uiso 1 1 calc R . . C29 C 0.2042(12) 0.8156(5) 0.2860(3) 0.087(3) Uani 1 1 d . . . H29 H 0.2106 0.8567 0.2577 0.104 Uiso 1 1 calc R . . C30 C 0.0699(9) 0.7873(4) 0.3002(3) 0.072(2) Uani 1 1 d . . . H30 H -0.0151 0.8080 0.2810 0.086 Uiso 1 1 calc R . . C31 C 0.0644(7) 0.7273(3) 0.3435(2) 0.0443(14) Uani 1 1 d . . . C32 C -0.0750(6) 0.6880(4) 0.3582(2) 0.0427(14) Uani 1 1 d . . . C33 C -0.1989(7) 0.6829(4) 0.3205(3) 0.0627(18) Uani 1 1 d . . . H33 H -0.1983 0.7076 0.2851 0.075 Uiso 1 1 calc R . . C34 C -0.3207(8) 0.6416(5) 0.3356(3) 0.083(2) Uani 1 1 d . . . H34 H -0.4043 0.6387 0.3111 0.100 Uiso 1 1 calc R . . C35 C -0.3169(7) 0.6048(5) 0.3875(3) 0.081(2) Uani 1 1 d . . . H35 H -0.3976 0.5752 0.3988 0.097 Uiso 1 1 calc R . . C36 C -0.1923(7) 0.6118(5) 0.4231(3) 0.067(2) Uani 1 1 d . . . H36 H -0.1921 0.5874 0.4586 0.080 Uiso 1 1 calc R . . N1 N 0.1839(4) 1.0159(2) 0.56772(16) 0.0316(10) Uani 1 1 d . . . N2 N -0.0560(4) 0.9734(2) 0.61692(16) 0.0298(9) Uani 1 1 d . . . N3 N 0.1844(5) 0.6994(3) 0.37283(18) 0.0417(11) Uani 1 1 d . . . N4 N -0.0719(5) 0.6516(3) 0.40937(18) 0.0425(11) Uani 1 1 d . . . O1 O 0.2964(4) 0.8310(2) 0.56501(14) 0.0438(9) Uani 1 1 d . . . O2 O 0.3094(4) 0.7346(2) 0.49639(14) 0.0362(8) Uani 1 1 d . . . O3 O 0.8519(4) 0.5148(2) 0.55381(14) 0.0363(8) Uani 1 1 d . . . O4 O 0.6337(4) 0.4600(2) 0.55788(15) 0.0411(9) Uani 1 1 d . . . O5 O 1.0196(4) 0.7611(2) 0.61094(14) 0.0427(9) Uani 1 1 d . . . O6 O 1.0915(5) 0.7963(2) 0.69717(15) 0.0542(11) Uani 1 1 d . . . O7 O 1.3002(4) 0.5130(3) 0.78919(15) 0.0506(10) Uani 1 1 d . . . O8 O 1.1258(4) 0.4281(2) 0.81473(14) 0.0409(9) Uani 1 1 d . . . O1W O 0.0667(5) 0.6283(2) 0.54135(15) 0.0589(12) Uani 1 1 d . . . H1WB H 0.0076 0.5900 0.5516 0.071 Uiso 1 1 d R . . H1WA H 0.0324 0.6786 0.5483 0.071 Uiso 1 1 d R . . O2W O 0.4789(8) 0.5570(6) 0.7041(3) 0.059(2) Uani 0.50 1 d P . . 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 Cd1 0.0272(2) 0.02219(19) 0.0298(2) 0.00007(14) -0.00350(15) -0.00013(15) Cd2 0.0303(2) 0.0249(2) 0.0302(2) -0.00258(14) 0.00106(15) 0.00292(15) C1 0.024(3) 0.028(3) 0.031(3) 0.005(2) 0.003(2) -0.002(2) C2 0.020(2) 0.024(2) 0.029(3) 0.0010(19) 0.000(2) 0.000(2) C3 0.026(3) 0.026(3) 0.024(2) -0.0016(19) -0.004(2) 0.000(2) C4 0.026(3) 0.022(2) 0.024(2) 0.0009(18) 0.002(2) 0.001(2) C5 0.018(2) 0.025(2) 0.025(2) 0.0033(19) 0.0014(19) 0.0003(19) C6 0.033(3) 0.030(3) 0.024(3) -0.009(2) -0.006(2) 0.001(2) C7 0.028(3) 0.023(2) 0.036(3) -0.002(2) -0.003(2) 0.006(2) C8 0.030(3) 0.032(3) 0.019(2) -0.0015(19) -0.006(2) 0.002(2) C9 0.023(3) 0.026(2) 0.024(2) -0.0015(19) 0.0019(19) 0.004(2) C10 0.025(3) 0.025(2) 0.020(2) 0.0000(18) -0.0004(19) 0.002(2) C11 0.023(3) 0.029(3) 0.024(2) -0.0002(19) -0.001(2) -0.001(2) C12 0.027(3) 0.028(3) 0.024(2) 0.0011(19) 0.001(2) 0.007(2) C13 0.033(3) 0.026(3) 0.032(3) 0.004(2) 0.002(2) 0.000(2) C14 0.026(3) 0.027(3) 0.029(3) -0.004(2) 0.000(2) -0.007(2) C15 0.028(3) 0.022(2) 0.034(3) 0.000(2) -0.002(2) 0.003(2) C16 0.037(3) 0.029(3) 0.030(3) 0.001(2) 0.002(2) 0.006(2) C17 0.034(3) 0.046(3) 0.049(3) 0.008(3) 0.003(3) 0.003(3) C18 0.046(4) 0.048(3) 0.057(4) 0.009(3) 0.013(3) -0.011(3) C19 0.065(4) 0.039(3) 0.053(4) 0.016(3) 0.007(3) -0.004(3) C20 0.040(3) 0.032(3) 0.051(3) 0.006(3) -0.003(3) 0.005(3) C21 0.037(3) 0.021(2) 0.027(3) -0.0018(19) -0.003(2) 0.000(2) C22 0.029(3) 0.020(2) 0.030(3) -0.0055(19) -0.003(2) 0.000(2) C23 0.033(3) 0.035(3) 0.049(3) 0.004(2) -0.006(3) 0.004(2) C24 0.030(3) 0.044(3) 0.063(4) -0.006(3) -0.007(3) 0.010(3) C25 0.030(3) 0.052(4) 0.061(4) -0.007(3) 0.011(3) -0.002(3) C26 0.041(3) 0.036(3) 0.050(4) 0.003(3) 0.007(3) 0.002(3) C27 0.064(5) 0.067(4) 0.063(4) -0.007(3) 0.025(4) -0.012(4) C28 0.113(7) 0.087(6) 0.066(5) -0.010(4) 0.052(5) -0.035(5) C29 0.158(9) 0.066(5) 0.040(4) 0.008(4) 0.030(5) -0.042(6) C30 0.116(7) 0.057(4) 0.042(4) 0.019(3) 0.002(4) -0.005(4) C31 0.065(4) 0.040(3) 0.028(3) 0.001(2) 0.006(3) 0.002(3) C32 0.046(4) 0.044(3) 0.037(3) 0.006(2) -0.003(3) 0.011(3) C33 0.059(5) 0.082(5) 0.044(4) 0.005(3) -0.014(3) 0.020(4) C34 0.041(4) 0.128(7) 0.077(5) 0.019(5) -0.012(4) 0.010(4) C35 0.036(4) 0.121(7) 0.083(6) 0.017(5) -0.004(4) -0.005(4) C36 0.042(4) 0.103(6) 0.057(4) 0.022(4) 0.007(3) -0.003(4) N1 0.033(2) 0.028(2) 0.034(2) 0.0062(18) 0.0035(19) 0.0039(19) N2 0.029(2) 0.027(2) 0.033(2) 0.0024(18) 0.0029(18) 0.0018(18) N3 0.047(3) 0.041(3) 0.039(3) 0.000(2) 0.012(2) -0.004(2) N4 0.034(3) 0.055(3) 0.038(3) 0.013(2) 0.001(2) 0.009(2) O1 0.042(2) 0.048(2) 0.042(2) -0.0047(18) 0.0038(17) 0.0227(19) O2 0.035(2) 0.0311(19) 0.040(2) -0.0010(16) -0.0143(16) -0.0010(16) O3 0.032(2) 0.0312(19) 0.048(2) -0.0017(16) 0.0141(17) 0.0027(16) O4 0.029(2) 0.0267(19) 0.066(3) -0.0137(17) -0.0035(18) 0.0004(16) O5 0.066(3) 0.0299(19) 0.033(2) 0.0068(15) 0.0067(18) -0.0016(18) O6 0.079(3) 0.034(2) 0.045(2) 0.0068(18) -0.022(2) -0.024(2) O7 0.032(2) 0.063(3) 0.054(2) 0.025(2) -0.0100(19) -0.0036(19) O8 0.037(2) 0.045(2) 0.039(2) 0.0150(17) -0.0052(17) -0.0004(17) O1W 0.081(3) 0.052(2) 0.049(2) -0.0194(19) 0.035(2) -0.029(2) O2W 0.033(5) 0.090(6) 0.056(5) -0.014(4) 0.027(4) -0.030(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O8 2.274(3) 2_656 ? Cd1 O1 2.328(3) . ? Cd1 N2 2.332(4) . ? Cd1 O6 2.361(4) 1_455 ? Cd1 N1 2.363(4) . ? Cd1 O5 2.516(3) 1_455 ? Cd1 O7 2.577(3) 2_656 ? Cd2 O2 2.216(3) . ? Cd2 O1W 2.229(3) . ? Cd2 O3 2.285(3) 3_666 ? Cd2 N3 2.314(4) . ? Cd2 N4 2.352(4) . ? Cd2 O4 2.455(3) 3_666 ? Cd2 C8 2.708(5) 3_666 ? C1 O1 1.249(5) . ? C1 O2 1.262(5) . ? C1 C2 1.519(6) . ? C2 C3 1.378(6) . ? C2 C7 1.390(6) . ? C3 C4 1.389(6) . ? C3 H3 0.9300 . ? C4 C5 1.407(6) . ? C4 C8 1.508(6) . ? C5 C6 1.387(6) . ? C5 C9 1.489(6) . ? C6 C7 1.377(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O4 1.240(5) . ? C8 O3 1.268(5) . ? C8 Cd2 2.708(5) 3_666 ? C9 C14 1.401(6) . ? C9 C10 1.404(6) . ? C10 C11 1.392(6) . ? C10 C15 1.507(6) . ? C11 C12 1.394(6) . ? C11 H11 0.9300 . ? C12 C13 1.393(6) . ? C12 C16 1.505(6) . ? C13 C14 1.374(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 O6 1.247(5) . ? C15 O5 1.252(5) . ? C16 O7 1.236(6) . ? C16 O8 1.261(6) . ? C17 N1 1.335(6) . ? C17 C18 1.377(7) . ? C17 H17 0.9300 . ? C18 C19 1.358(8) . ? C18 H18 0.9300 . ? C19 C20 1.385(8) . ? C19 H19 0.9300 . ? C20 C21 1.388(7) . ? C20 H20 0.9300 . ? C21 N1 1.341(6) . ? C21 C22 1.487(6) . ? C22 N2 1.340(6) . ? C22 C23 1.382(6) . ? C23 C24 1.374(7) . ? C23 H23 0.9300 . ? C24 C25 1.375(8) . ? C24 H24 0.9300 . ? C25 C26 1.382(7) . ? C25 H25 0.9300 . ? C26 N2 1.327(6) . ? C26 H26 0.9300 . ? C27 N3 1.339(7) . ? C27 C28 1.384(9) . ? C27 H27 0.9300 . ? C28 C29 1.350(11) . ? C28 H28 0.9300 . ? C29 C30 1.382(10) . ? C29 H29 0.9300 . ? C30 C31 1.388(7) . ? C30 H30 0.9300 . ? C31 N3 1.330(7) . ? C31 C32 1.489(8) . ? C32 N4 1.344(6) . ? C32 C33 1.399(8) . ? C33 C34 1.363(9) . ? C33 H33 0.9300 . ? C34 C35 1.365(10) . ? C34 H34 0.9300 . ? C35 C36 1.376(9) . ? C35 H35 0.9300 . ? C36 N4 1.332(7) . ? C36 H36 0.9300 . ? O3 Cd2 2.285(3) 3_666 ? O4 Cd2 2.455(3) 3_666 ? O5 Cd1 2.516(3) 1_655 ? O6 Cd1 2.361(4) 1_655 ? O7 Cd1 2.578(3) 2_646 ? O8 Cd1 2.274(3) 2_646 ? O1W H1WB 0.8499 . ? O1W H1WA 0.8501 . ? 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 O8 Cd1 O1 90.43(13) 2_656 . ? O8 Cd1 N2 132.76(13) 2_656 . ? O1 Cd1 N2 127.93(13) . . ? O8 Cd1 O6 91.60(13) 2_656 1_455 ? O1 Cd1 O6 111.07(14) . 1_455 ? N2 Cd1 O6 97.18(14) . 1_455 ? O8 Cd1 N1 96.51(14) 2_656 . ? O1 Cd1 N1 79.60(13) . . ? N2 Cd1 N1 69.51(13) . . ? O6 Cd1 N1 166.61(14) 1_455 . ? O8 Cd1 O5 133.33(12) 2_656 1_455 ? O1 Cd1 O5 78.24(13) . 1_455 ? N2 Cd1 O5 86.14(13) . 1_455 ? O6 Cd1 O5 53.11(11) 1_455 1_455 ? N1 Cd1 O5 124.78(13) . 1_455 ? O8 Cd1 O7 53.30(12) 2_656 2_656 ? O1 Cd1 O7 139.98(13) . 2_656 ? N2 Cd1 O7 80.50(12) . 2_656 ? O6 Cd1 O7 88.70(13) 1_455 2_656 ? N1 Cd1 O7 87.64(13) . 2_656 ? O5 Cd1 O7 137.50(12) 1_455 2_656 ? O2 Cd2 O1W 86.15(13) . . ? O2 Cd2 O3 139.02(12) . 3_666 ? O1W Cd2 O3 93.59(13) . 3_666 ? O2 Cd2 N3 87.50(14) . . ? O1W Cd2 N3 152.32(16) . . ? O3 Cd2 N3 108.62(13) 3_666 . ? O2 Cd2 N4 129.53(14) . . ? O1W Cd2 N4 93.26(16) . . ? O3 Cd2 N4 91.42(14) 3_666 . ? N3 Cd2 N4 70.49(16) . . ? O2 Cd2 O4 89.65(12) . 3_666 ? O1W Cd2 O4 118.78(14) . 3_666 ? O3 Cd2 O4 54.89(11) 3_666 3_666 ? N3 Cd2 O4 88.07(14) . 3_666 ? N4 Cd2 O4 132.25(14) . 3_666 ? O2 Cd2 C8 115.46(13) . 3_666 ? O1W Cd2 C8 109.64(14) . 3_666 ? O3 Cd2 C8 27.79(12) 3_666 3_666 ? N3 Cd2 C8 97.41(14) . 3_666 ? N4 Cd2 C8 112.12(15) . 3_666 ? O4 Cd2 C8 27.22(12) 3_666 3_666 ? O1 C1 O2 124.1(4) . . ? O1 C1 C2 119.0(4) . . ? O2 C1 C2 116.7(4) . . ? C3 C2 C7 119.4(4) . . ? C3 C2 C1 121.4(4) . . ? C7 C2 C1 119.1(4) . . ? C2 C3 C4 120.9(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 C8 118.7(4) . . ? C5 C4 C8 121.1(4) . . ? C6 C5 C4 117.7(4) . . ? C6 C5 C9 119.8(4) . . ? C4 C5 C9 121.9(4) . . ? C7 C6 C5 122.1(4) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C6 C7 C2 119.7(4) . . ? C6 C7 H7 120.2 . . ? C2 C7 H7 120.2 . . ? O4 C8 O3 121.7(4) . . ? O4 C8 C4 119.7(4) . . ? O3 C8 C4 118.6(4) . . ? O4 C8 Cd2 64.9(2) . 3_666 ? O3 C8 Cd2 57.2(2) . 3_666 ? C4 C8 Cd2 171.6(3) . 3_666 ? C14 C9 C10 117.8(4) . . ? C14 C9 C5 117.9(4) . . ? C10 C9 C5 124.0(4) . . ? C11 C10 C9 119.6(4) . . ? C11 C10 C15 116.3(4) . . ? C9 C10 C15 124.1(4) . . ? C10 C11 C12 121.7(4) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C13 C12 C11 118.7(4) . . ? C13 C12 C16 120.7(4) . . ? C11 C12 C16 120.5(4) . . ? C14 C13 C12 119.8(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C9 122.4(4) . . ? C13 C14 H14 118.8 . . ? C9 C14 H14 118.8 . . ? O6 C15 O5 121.9(4) . . ? O6 C15 C10 118.2(4) . . ? O5 C15 C10 119.8(4) . . ? O7 C16 O8 122.8(5) . . ? O7 C16 C12 119.7(4) . . ? O8 C16 C12 117.4(5) . . ? N1 C17 C18 122.2(5) . . ? N1 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C19 C18 C17 119.4(5) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 119.4(5) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C19 C20 C21 118.4(5) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? N1 C21 C20 121.8(5) . . ? N1 C21 C22 115.7(4) . . ? C20 C21 C22 122.5(5) . . ? N2 C22 C23 121.3(5) . . ? N2 C22 C21 117.0(4) . . ? C23 C22 C21 121.7(4) . . ? C24 C23 C22 119.1(5) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C23 C24 C25 120.0(5) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 117.5(5) . . ? C24 C25 H25 121.3 . . ? C26 C25 H25 121.3 . . ? N2 C26 C25 123.2(5) . . ? N2 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? N3 C27 C28 121.7(7) . . ? N3 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C29 C28 C27 119.4(7) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C28 C29 C30 119.4(7) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C29 C30 C31 118.7(7) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? N3 C31 C30 121.6(6) . . ? N3 C31 C32 116.3(5) . . ? C30 C31 C32 122.0(6) . . ? N4 C32 C33 121.3(6) . . ? N4 C32 C31 115.6(5) . . ? C33 C32 C31 123.0(5) . . ? C34 C33 C32 120.1(6) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 118.4(7) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? C34 C35 C36 119.2(7) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? N4 C36 C35 123.6(6) . . ? N4 C36 H36 118.2 . . ? C35 C36 H36 118.2 . . ? C17 N1 C21 118.8(4) . . ? C17 N1 Cd1 122.5(3) . . ? C21 N1 Cd1 118.7(3) . . ? C26 N2 C22 118.9(4) . . ? C26 N2 Cd1 122.0(3) . . ? C22 N2 Cd1 119.1(3) . . ? C31 N3 C27 119.0(5) . . ? C31 N3 Cd2 117.5(4) . . ? C27 N3 Cd2 121.9(4) . . ? C36 N4 C32 117.4(5) . . ? C36 N4 Cd2 124.1(4) . . ? C32 N4 Cd2 116.8(4) . . ? C1 O1 Cd1 153.6(3) . . ? C1 O2 Cd2 140.7(3) . . ? C8 O3 Cd2 95.0(3) . 3_666 ? C8 O4 Cd2 87.9(3) . 3_666 ? C15 O5 Cd1 88.5(3) . 1_655 ? C15 O6 Cd1 95.9(3) . 1_655 ? C16 O7 Cd1 85.2(3) . 2_646 ? C16 O8 Cd1 98.7(3) . 2_646 ? Cd2 O1W H1WB 126.0 . . ? Cd2 O1W H1WA 108.5 . . ? H1WB O1W H1WA 107.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WB O3 0.85 1.84 2.667(5) 163.1 1_455 O1W H1WA O5 0.85 1.97 2.682(5) 140.5 1_455 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.734 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.101 # complex_5.cif===END data_complex_6 _database_code_depnum_ccdc_archive 'CCDC 744736' #TrackingRef 'complex1-8_2new1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H16 N2 O9 Zn2' _chemical_formula_weight 655.17 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.8527(9) _cell_length_b 13.6187(14) _cell_length_c 19.956(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.4330(10) _cell_angle_gamma 90.00 _cell_volume 2358.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4368 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.43 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 2.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5714 _exptl_absorpt_correction_T_max 0.6787 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12070 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4174 _reflns_number_gt 3368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.6855P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4174 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0777 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 0.03287(3) 0.01217(2) 0.187012(17) 0.02701(11) Uani 1 1 d . . . Zn2 Zn 0.02560(3) 0.00460(2) 0.424280(15) 0.02536(11) Uani 1 1 d . . . C1 C 0.2779(4) -0.1039(2) 0.28599(15) 0.0365(7) Uani 1 1 d . . . H1 H 0.1993 -0.1399 0.2990 0.044 Uiso 1 1 calc R . . C2 C 0.4282(4) -0.1173(2) 0.32181(16) 0.0424(8) Uani 1 1 d . . . H2 H 0.4501 -0.1642 0.3562 0.051 Uiso 1 1 calc R . . C3 C 0.5431(4) -0.0604(2) 0.30560(16) 0.0425(8) Uani 1 1 d . . . H3 H 0.6431 -0.0660 0.3307 0.051 Uiso 1 1 calc R . . C4 C 0.5103(3) 0.0065(2) 0.25134(17) 0.0336(7) Uani 1 1 d . . . C5 C 0.6229(3) 0.0671(2) 0.22948(18) 0.0432(8) Uani 1 1 d . . . H5 H 0.7232 0.0677 0.2547 0.052 Uiso 1 1 calc R . . C6 C 0.5873(3) 0.1232(2) 0.17333(19) 0.0429(8) Uani 1 1 d . . . H6 H 0.6639 0.1607 0.1599 0.051 Uiso 1 1 calc R . . C7 C 0.4336(3) 0.1265(2) 0.13371(17) 0.0365(7) Uani 1 1 d . . . C8 C 0.3894(4) 0.1783(2) 0.07237(18) 0.0478(9) Uani 1 1 d . . . H8 H 0.4618 0.2150 0.0552 0.057 Uiso 1 1 calc R . . C9 C 0.2411(5) 0.1751(2) 0.03796(19) 0.0548(10) Uani 1 1 d . . . H9 H 0.2126 0.2070 -0.0039 0.066 Uiso 1 1 calc R . . C10 C 0.1311(4) 0.1237(2) 0.06570(17) 0.0472(8) Uani 1 1 d . . . H10 H 0.0289 0.1244 0.0427 0.057 Uiso 1 1 calc R . . C11 C 0.3176(3) 0.07271(19) 0.15643(14) 0.0279(6) Uani 1 1 d . . . C12 C 0.3578(3) 0.01116(18) 0.21572(14) 0.0260(6) Uani 1 1 d . . . C13 C 0.0344(3) 0.13426(19) 0.30059(13) 0.0228(6) Uani 1 1 d . . . C14 C 0.0195(3) 0.22925(18) 0.33680(13) 0.0216(6) Uani 1 1 d . . . C15 C -0.1196(3) 0.27956(18) 0.32005(14) 0.0234(6) Uani 1 1 d . . . H15 H -0.1936 0.2592 0.2828 0.028 Uiso 1 1 calc R . . C16 C -0.1491(3) 0.35966(18) 0.35831(14) 0.0240(6) Uani 1 1 d . . . C17 C -0.0357(3) 0.39182(19) 0.41208(14) 0.0263(6) Uani 1 1 d . . . H17 H -0.0552 0.4446 0.4387 0.032 Uiso 1 1 calc R . . C18 C 0.1063(3) 0.34564(19) 0.42632(14) 0.0263(6) Uani 1 1 d . . . H18 H 0.1834 0.3699 0.4609 0.032 Uiso 1 1 calc R . . C19 C 0.1352(3) 0.26322(18) 0.38944(13) 0.0215(6) Uani 1 1 d . . . C20 C -0.3002(3) 0.4110(2) 0.34067(15) 0.0282(6) Uani 1 1 d . . . C21 C 0.2891(3) 0.21325(18) 0.40725(13) 0.0218(6) Uani 1 1 d . . . C22 C 0.3330(3) 0.16697(18) 0.47034(13) 0.0201(5) Uani 1 1 d . . . C23 C 0.2212(3) 0.16006(18) 0.51808(13) 0.0231(6) Uani 1 1 d . . . C24 C 0.4791(3) 0.12531(19) 0.48841(13) 0.0217(6) Uani 1 1 d . . . H24 H 0.5089 0.0961 0.5311 0.026 Uiso 1 1 calc R . . C25 C 0.5814(3) 0.12667(18) 0.44360(13) 0.0213(6) Uani 1 1 d . . . C26 C 0.5360(3) 0.17210(18) 0.38043(13) 0.0235(6) Uani 1 1 d . . . H26 H 0.6025 0.1731 0.3498 0.028 Uiso 1 1 calc R . . C27 C 0.3922(3) 0.2159(2) 0.36289(14) 0.0265(6) Uani 1 1 d . . . H27 H 0.3643 0.2474 0.3209 0.032 Uiso 1 1 calc R . . C28 C 0.7388(3) 0.08113(18) 0.46438(14) 0.0220(6) Uani 1 1 d . . . N1 N 0.2425(2) -0.04193(16) 0.23427(11) 0.0259(5) Uani 1 1 d . . . N2 N 0.1683(3) 0.07384(17) 0.12366(12) 0.0306(5) Uani 1 1 d . . . O1 O 0.0002(2) 0.13423(13) 0.23622(9) 0.0302(4) Uani 1 1 d . . . O2 O 0.0765(2) 0.05907(13) 0.33550(9) 0.0278(4) Uani 1 1 d . . . O3 O -0.3882(2) 0.39580(14) 0.28405(10) 0.0340(5) Uani 1 1 d . . . O4 O -0.3378(2) 0.47167(15) 0.38241(10) 0.0365(5) Uani 1 1 d . . . O5 O 0.09331(19) 0.11739(13) 0.49655(9) 0.0282(4) Uani 1 1 d . . . O6 O 0.2599(2) 0.19614(14) 0.57603(9) 0.0313(4) Uani 1 1 d . . . O7 O 0.78509(19) 0.06702(13) 0.52773(9) 0.0273(4) Uani 1 1 d . . . O8 O 0.81004(19) 0.06064(13) 0.41760(9) 0.0260(4) Uani 1 1 d . . . O1W O -0.0498(2) -0.11656(14) 0.36144(11) 0.0311(5) Uani 1 1 d . . . H1WB H -0.1144 -0.1472 0.3773 0.047 Uiso 1 1 calc R . . H1WA H -0.082(4) -0.109(3) 0.3182(19) 0.061(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01704(18) 0.0317(2) 0.0315(2) -0.00559(14) 0.00301(14) -0.00549(12) Zn2 0.01739(17) 0.0378(2) 0.02043(19) 0.00026(13) 0.00257(13) 0.00892(12) C1 0.0405(18) 0.0385(18) 0.0323(17) 0.0001(14) 0.0119(15) 0.0027(14) C2 0.050(2) 0.0470(19) 0.0283(17) 0.0017(14) 0.0036(16) 0.0134(16) C3 0.0329(17) 0.052(2) 0.0371(19) -0.0136(16) -0.0054(15) 0.0116(15) C4 0.0215(14) 0.0392(18) 0.0394(18) -0.0157(14) 0.0041(13) 0.0007(12) C5 0.0202(15) 0.046(2) 0.063(2) -0.0206(18) 0.0069(15) -0.0063(13) C6 0.0288(17) 0.0386(18) 0.067(2) -0.0134(17) 0.0232(17) -0.0130(14) C7 0.0393(18) 0.0254(15) 0.050(2) -0.0058(14) 0.0224(16) -0.0064(13) C8 0.062(2) 0.0340(18) 0.055(2) -0.0028(16) 0.032(2) -0.0070(16) C9 0.080(3) 0.040(2) 0.048(2) 0.0139(16) 0.023(2) 0.0074(18) C10 0.049(2) 0.050(2) 0.040(2) 0.0057(16) 0.0042(17) 0.0118(16) C11 0.0244(14) 0.0273(15) 0.0336(16) -0.0089(12) 0.0095(13) -0.0050(11) C12 0.0226(14) 0.0279(15) 0.0284(15) -0.0100(12) 0.0071(12) -0.0017(11) C13 0.0157(13) 0.0265(15) 0.0268(16) -0.0012(12) 0.0058(12) 0.0010(10) C14 0.0194(13) 0.0252(14) 0.0210(14) 0.0026(11) 0.0060(11) 0.0016(10) C15 0.0188(13) 0.0268(14) 0.0238(15) 0.0034(11) 0.0022(11) 0.0020(11) C16 0.0203(13) 0.0255(14) 0.0261(15) 0.0082(11) 0.0047(11) 0.0063(11) C17 0.0284(15) 0.0238(14) 0.0263(15) 0.0000(11) 0.0049(12) 0.0083(11) C18 0.0203(14) 0.0303(15) 0.0256(15) -0.0005(12) -0.0018(12) 0.0020(11) C19 0.0189(13) 0.0238(14) 0.0216(14) 0.0039(11) 0.0036(11) 0.0033(10) C20 0.0230(14) 0.0299(16) 0.0333(17) 0.0097(13) 0.0091(13) 0.0052(11) C21 0.0174(13) 0.0208(13) 0.0261(15) -0.0015(11) 0.0015(11) 0.0005(10) C22 0.0153(12) 0.0240(13) 0.0199(14) -0.0026(11) 0.0011(11) 0.0009(10) C23 0.0173(13) 0.0265(14) 0.0251(15) 0.0041(12) 0.0034(12) 0.0076(11) C24 0.0180(13) 0.0261(15) 0.0206(14) -0.0001(11) 0.0025(11) 0.0018(10) C25 0.0168(13) 0.0215(13) 0.0258(15) -0.0017(11) 0.0044(11) 0.0016(10) C26 0.0193(13) 0.0274(14) 0.0255(15) -0.0010(11) 0.0085(11) 0.0029(11) C27 0.0236(14) 0.0331(16) 0.0229(15) 0.0057(12) 0.0047(12) 0.0036(11) C28 0.0173(13) 0.0221(14) 0.0264(15) -0.0007(11) 0.0039(12) -0.0004(10) N1 0.0210(11) 0.0313(13) 0.0252(13) -0.0025(10) 0.0044(10) -0.0013(9) N2 0.0283(13) 0.0343(14) 0.0289(14) 0.0010(11) 0.0050(11) 0.0002(10) O1 0.0352(11) 0.0311(11) 0.0220(11) -0.0029(8) 0.0000(9) 0.0034(8) O2 0.0334(11) 0.0260(10) 0.0258(10) 0.0035(8) 0.0098(9) 0.0061(8) O3 0.0238(10) 0.0441(12) 0.0311(12) 0.0026(9) -0.0019(9) 0.0118(9) O4 0.0282(11) 0.0457(12) 0.0350(12) -0.0004(10) 0.0049(9) 0.0175(9) O5 0.0151(9) 0.0394(11) 0.0300(11) -0.0059(9) 0.0043(8) -0.0014(8) O6 0.0267(10) 0.0437(12) 0.0239(11) -0.0037(9) 0.0060(9) -0.0055(8) O7 0.0173(9) 0.0398(11) 0.0244(11) 0.0021(8) 0.0035(8) 0.0071(8) O8 0.0156(9) 0.0357(11) 0.0274(11) -0.0001(8) 0.0059(8) 0.0057(8) O1W 0.0313(11) 0.0365(12) 0.0267(12) 0.0027(9) 0.0089(10) -0.0031(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.9808(18) . ? Zn1 N1 2.045(2) . ? Zn1 O4 2.063(2) 2_445 ? Zn1 N2 2.084(2) . ? Zn1 O3 2.1861(18) 2_445 ? Zn1 C20 2.448(3) 2_445 ? Zn2 O7 2.0102(17) 3_656 ? Zn2 O8 2.0349(16) 1_455 ? Zn2 O2 2.0514(18) . ? Zn2 O1W 2.100(2) . ? Zn2 O5 2.1110(18) . ? Zn2 Zn2 3.1462(7) 3_556 ? C1 N1 1.322(4) . ? C1 C2 1.392(4) . ? C1 H1 0.9300 . ? C2 C3 1.368(4) . ? C2 H2 0.9300 . ? C3 C4 1.400(4) . ? C3 H3 0.9300 . ? C4 C12 1.397(4) . ? C4 C5 1.428(4) . ? C5 C6 1.342(5) . ? C5 H5 0.9300 . ? C6 C7 1.433(4) . ? C6 H6 0.9300 . ? C7 C8 1.400(5) . ? C7 C11 1.407(4) . ? C8 C9 1.356(5) . ? C8 H8 0.9300 . ? C9 C10 1.399(5) . ? C9 H9 0.9300 . ? C10 N2 1.325(4) . ? C10 H10 0.9300 . ? C11 N2 1.354(3) . ? C11 C12 1.436(4) . ? C12 N1 1.360(3) . ? C13 O2 1.253(3) . ? C13 O1 1.260(3) . ? C13 C14 1.500(4) . ? C14 C15 1.391(3) . ? C14 C19 1.393(4) . ? C15 C16 1.386(4) . ? C15 H15 0.9300 . ? C16 C17 1.387(4) . ? C16 C20 1.488(3) . ? C17 C18 1.384(4) . ? C17 H17 0.9300 . ? C18 C19 1.393(4) . ? C18 H18 0.9300 . ? C19 C21 1.501(3) . ? C20 O3 1.256(3) . ? C20 O4 1.264(3) . ? C20 Zn1 2.448(3) 2_455 ? C21 C27 1.392(3) . ? C21 C22 1.393(4) . ? C22 C24 1.393(3) . ? C22 C23 1.507(3) . ? C23 O6 1.241(3) . ? C23 O5 1.269(3) . ? C24 C25 1.393(3) . ? C24 H24 0.9300 . ? C25 C26 1.390(4) . ? C25 C28 1.506(3) . ? C26 C27 1.386(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 O8 1.258(3) . ? C28 O7 1.264(3) . ? O3 Zn1 2.1861(18) 2_455 ? O4 Zn1 2.063(2) 2_455 ? O7 Zn2 2.0102(17) 3_656 ? O8 Zn2 2.0349(16) 1_655 ? O1W H1WB 0.8200 . ? O1W H1WA 0.86(4) . ? 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 N1 106.37(8) . . ? O1 Zn1 O4 111.86(8) . 2_445 ? N1 Zn1 O4 140.85(9) . 2_445 ? O1 Zn1 N2 96.92(8) . . ? N1 Zn1 N2 81.16(9) . . ? O4 Zn1 N2 101.88(8) 2_445 . ? O1 Zn1 O3 109.07(7) . 2_445 ? N1 Zn1 O3 98.21(8) . 2_445 ? O4 Zn1 O3 61.79(7) 2_445 2_445 ? N2 Zn1 O3 152.90(8) . 2_445 ? O1 Zn1 C20 112.65(8) . 2_445 ? N1 Zn1 C20 123.19(9) . 2_445 ? O4 Zn1 C20 31.06(8) 2_445 2_445 ? N2 Zn1 C20 130.49(9) . 2_445 ? O3 Zn1 C20 30.79(8) 2_445 2_445 ? O7 Zn2 O8 153.59(7) 3_656 1_455 ? O7 Zn2 O2 106.37(7) 3_656 . ? O8 Zn2 O2 99.87(7) 1_455 . ? O7 Zn2 O1W 92.27(8) 3_656 . ? O8 Zn2 O1W 94.16(7) 1_455 . ? O2 Zn2 O1W 82.33(8) . . ? O7 Zn2 O5 86.02(7) 3_656 . ? O8 Zn2 O5 84.69(7) 1_455 . ? O2 Zn2 O5 104.22(7) . . ? O1W Zn2 O5 173.44(7) . . ? O7 Zn2 Zn2 77.78(5) 3_656 3_556 ? O8 Zn2 Zn2 76.47(5) 1_455 3_556 ? O2 Zn2 Zn2 160.41(5) . 3_556 ? O1W Zn2 Zn2 116.95(6) . 3_556 ? O5 Zn2 Zn2 56.51(5) . 3_556 ? N1 C1 C2 122.6(3) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 118.9(3) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 120.1(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C12 C4 C3 117.0(3) . . ? C12 C4 C5 118.8(3) . . ? C3 C4 C5 124.2(3) . . ? C6 C5 C4 121.5(3) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 121.3(3) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C11 116.7(3) . . ? C8 C7 C6 124.6(3) . . ? C11 C7 C6 118.7(3) . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 119.7(3) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? N2 C10 C9 122.0(3) . . ? N2 C10 H10 119.0 . . ? C9 C10 H10 119.0 . . ? N2 C11 C7 122.9(3) . . ? N2 C11 C12 117.6(2) . . ? C7 C11 C12 119.4(3) . . ? N1 C12 C4 122.6(3) . . ? N1 C12 C11 117.2(2) . . ? C4 C12 C11 120.2(2) . . ? O2 C13 O1 123.5(2) . . ? O2 C13 C14 118.8(2) . . ? O1 C13 C14 117.7(2) . . ? C15 C14 C19 120.1(2) . . ? C15 C14 C13 117.8(2) . . ? C19 C14 C13 121.9(2) . . ? C16 C15 C14 120.6(2) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 119.2(2) . . ? C15 C16 C20 119.9(2) . . ? C17 C16 C20 120.9(2) . . ? C18 C17 C16 120.3(2) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.8(2) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C14 C19 C18 118.8(2) . . ? C14 C19 C21 121.7(2) . . ? C18 C19 C21 119.6(2) . . ? O3 C20 O4 120.2(2) . . ? O3 C20 C16 120.2(2) . . ? O4 C20 C16 119.5(3) . . ? O3 C20 Zn1 62.99(13) . 2_455 ? O4 C20 Zn1 57.39(13) . 2_455 ? C16 C20 Zn1 173.79(19) . 2_455 ? C27 C21 C22 119.1(2) . . ? C27 C21 C19 121.1(2) . . ? C22 C21 C19 119.7(2) . . ? C21 C22 C24 119.8(2) . . ? C21 C22 C23 120.0(2) . . ? C24 C22 C23 120.2(2) . . ? O6 C23 O5 124.1(2) . . ? O6 C23 C22 118.0(2) . . ? O5 C23 C22 117.9(2) . . ? C25 C24 C22 121.1(2) . . ? C25 C24 H24 119.4 . . ? C22 C24 H24 119.4 . . ? C26 C25 C24 118.7(2) . . ? C26 C25 C28 121.2(2) . . ? C24 C25 C28 120.1(2) . . ? C27 C26 C25 120.4(2) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C21 120.9(2) . . ? C26 C27 H27 119.5 . . ? C21 C27 H27 119.5 . . ? O8 C28 O7 126.7(2) . . ? O8 C28 C25 117.4(2) . . ? O7 C28 C25 115.9(2) . . ? C1 N1 C12 118.5(2) . . ? C1 N1 Zn1 130.01(19) . . ? C12 N1 Zn1 110.14(18) . . ? C10 N2 C11 118.5(3) . . ? C10 N2 Zn1 131.5(2) . . ? C11 N2 Zn1 109.05(18) . . ? C13 O1 Zn1 118.46(17) . . ? C13 O2 Zn2 133.15(16) . . ? C20 O3 Zn1 86.22(16) . 2_455 ? C20 O4 Zn1 91.55(17) . 2_455 ? C23 O5 Zn2 132.68(16) . . ? C28 O7 Zn2 128.67(16) . 3_656 ? C28 O8 Zn2 129.54(17) . 1_655 ? Zn2 O1W H1WB 109.5 . . ? Zn2 O1W H1WA 120(2) . . ? H1WB O1W H1WA 109.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O3 0.86(4) 2.01(4) 2.851(3) 167(3) 2_445 O1W H1WB O5 0.82 2.52 2.935(3) 112.6 3_556 O1W H1WB O6 0.82 1.86 2.667(3) 169.1 3_556 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.357 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.065 # complex_6.cif===END data_complex_7 _database_code_depnum_ccdc_archive 'CCDC 744737' #TrackingRef 'complex1-8_2new1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 Co5 O24' _chemical_formula_weight 1089.18 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0444(17) _cell_length_b 16.460(3) _cell_length_c 12.074(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.437(3) _cell_angle_gamma 90.00 _cell_volume 1794.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 826 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 21.35 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1086 _exptl_absorpt_coefficient_mu 2.365 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6492 _exptl_absorpt_correction_T_max 0.7979 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9270 _diffrn_reflns_av_R_equivalents 0.0879 _diffrn_reflns_av_sigmaI/netI 0.1010 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3175 _reflns_number_gt 2038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.7756P] 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 3175 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Co1 Co 1.0000 0.0000 1.0000 0.0101(3) Uani 1 2 d S . . Co2 Co 1.08409(9) -0.02513(5) 0.74278(7) 0.0162(2) Uani 1 1 d . . . Co3 Co 1.15564(10) -0.00610(5) 0.45240(7) 0.0213(3) Uani 1 1 d . . . C1 C 0.7912(7) 0.0581(4) 0.7858(5) 0.0196(15) Uani 1 1 d . . . C2 C 0.6844(7) 0.0946(4) 0.8602(5) 0.0189(15) Uani 1 1 d . . . C3 C 0.5400(7) 0.0661(4) 0.8574(5) 0.0188(15) Uani 1 1 d . . . H3 H 0.5106 0.0266 0.8056 0.023 Uiso 1 1 calc R . . C4 C 0.4376(7) 0.0946(4) 0.9293(5) 0.0195(15) Uani 1 1 d . . . C5 C 0.4810(7) 0.1535(4) 1.0067(5) 0.0257(17) Uani 1 1 d . . . H5 H 0.4155 0.1712 1.0582 0.031 Uiso 1 1 calc R . . C6 C 0.6239(7) 0.1864(4) 1.0070(5) 0.0246(17) Uani 1 1 d . . . H6 H 0.6518 0.2272 1.0573 0.029 Uiso 1 1 calc R . . C7 C 0.7252(7) 0.1585(4) 0.9325(5) 0.0186(15) Uani 1 1 d . . . C8 C 0.8659(7) 0.2037(4) 0.9219(5) 0.0180(15) Uani 1 1 d . . . C9 C 0.9764(7) 0.2124(3) 1.0071(5) 0.0171(15) Uani 1 1 d . . . C10 C 1.0941(7) 0.2666(4) 0.9945(5) 0.0198(15) Uani 1 1 d . . . H10 H 1.1656 0.2738 1.0523 0.024 Uiso 1 1 calc R . . C11 C 1.1041(7) 0.3090(4) 0.8972(5) 0.0201(16) Uani 1 1 d . . . C12 C 0.9979(8) 0.2990(4) 0.8113(5) 0.0303(18) Uani 1 1 d . . . H12 H 1.0058 0.3270 0.7451 0.036 Uiso 1 1 calc R . . C13 C 0.8804(7) 0.2475(4) 0.8240(6) 0.0271(17) Uani 1 1 d . . . H13 H 0.8088 0.2417 0.7660 0.033 Uiso 1 1 calc R . . C14 C 1.2309(8) 0.3676(4) 0.8876(6) 0.0229(16) Uani 1 1 d . . . C15 C 0.9763(7) 0.1671(4) 1.1149(5) 0.0213(16) Uani 1 1 d . . . C16 C 0.2803(7) 0.0653(4) 0.9161(5) 0.0187(15) Uani 1 1 d . . . O1 O 0.9216(4) 0.0410(2) 0.8248(3) 0.0197(10) Uani 1 1 d . . . O2 O 0.7463(5) 0.0446(3) 0.6870(4) 0.0331(12) Uani 1 1 d . . . O3 O 0.2364(5) 0.0506(3) 0.8172(3) 0.0248(11) Uani 1 1 d . . . O4 O 0.2047(5) 0.0566(3) 0.9986(4) 0.0254(11) Uani 1 1 d . . . O5 O 0.9355(5) 0.0931(2) 1.1113(3) 0.0207(11) Uani 1 1 d . . . O6 O 1.0220(6) 0.2041(3) 1.2001(4) 0.0396(14) Uani 1 1 d . . . O7 O 1.2450(5) 0.4011(3) 0.7960(4) 0.0318(12) Uani 1 1 d . . . O8 O 1.3171(5) 0.3786(3) 0.9741(4) 0.0299(12) Uani 1 1 d . . . O1W O 1.0619(4) 0.0377(2) 0.5966(3) 0.0190(10) Uani 1 1 d . . . H1W H 1.0810 0.0875 0.6094 0.023 Uiso 1 1 d R . . O2W O 1.0745(5) 0.1053(2) 0.3690(4) 0.0299(12) Uani 1 1 d . . . H2WA H 1.0023 0.1275 0.3994 0.036 Uiso 1 1 d R . . H2WB H 1.0848 0.1341 0.3116 0.036 Uiso 1 1 d R . . O3W O 1.3605(5) 0.0453(3) 0.4999(4) 0.0434(14) Uani 1 1 d . . . H3WA H 1.4267 0.0253 0.4610 0.052 Uiso 1 1 d R . . H3WB H 1.3729 0.0745 0.5579 0.052 Uiso 1 1 d R . . O4W O 0.3238(6) 0.1538(3) 0.6579(4) 0.0452(15) Uani 1 1 d . . . H4WA H 0.3926 0.1881 0.6716 0.054 Uiso 1 1 d R . . H4WB H 0.3039 0.1247 0.7132 0.054 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0045(6) 0.0156(6) 0.0106(6) -0.0041(5) 0.0030(5) -0.0021(5) Co2 0.0135(5) 0.0195(5) 0.0157(5) -0.0008(4) 0.0021(4) 0.0010(4) Co3 0.0161(5) 0.0302(5) 0.0175(5) -0.0010(4) 0.0015(4) 0.0030(4) C1 0.016(4) 0.023(4) 0.021(4) 0.001(3) 0.005(3) -0.005(3) C2 0.017(4) 0.026(4) 0.013(4) -0.001(3) -0.001(3) 0.003(3) C3 0.015(4) 0.022(4) 0.018(4) -0.006(3) -0.003(3) -0.004(3) C4 0.005(3) 0.033(4) 0.020(4) 0.004(3) -0.002(3) -0.001(3) C5 0.013(4) 0.046(4) 0.019(4) -0.009(3) 0.002(3) -0.002(3) C6 0.023(4) 0.028(4) 0.023(4) -0.009(3) 0.002(3) -0.003(3) C7 0.015(4) 0.024(4) 0.017(4) -0.001(3) 0.004(3) -0.002(3) C8 0.014(4) 0.022(3) 0.019(4) -0.001(3) 0.004(3) 0.000(3) C9 0.017(4) 0.015(3) 0.019(4) -0.001(3) -0.003(3) -0.003(3) C10 0.018(4) 0.021(3) 0.019(4) 0.003(3) -0.007(3) -0.002(3) C11 0.016(4) 0.019(3) 0.025(4) 0.002(3) 0.005(3) -0.006(3) C12 0.030(5) 0.045(5) 0.016(4) 0.006(3) -0.002(3) -0.009(4) C13 0.014(4) 0.037(4) 0.029(4) -0.004(3) -0.003(3) -0.005(3) C14 0.023(4) 0.018(3) 0.028(4) -0.004(3) 0.004(3) -0.005(3) C15 0.018(4) 0.022(4) 0.025(4) 0.003(3) 0.002(3) -0.011(3) C16 0.018(4) 0.017(3) 0.022(4) 0.002(3) 0.004(3) 0.005(3) O1 0.007(2) 0.030(2) 0.022(2) -0.001(2) 0.0021(19) 0.003(2) O2 0.018(3) 0.055(3) 0.026(3) -0.012(2) 0.003(2) 0.005(3) O3 0.022(3) 0.035(3) 0.018(3) -0.003(2) 0.004(2) -0.007(2) O4 0.024(3) 0.032(3) 0.021(3) 0.001(2) 0.006(2) -0.004(2) O5 0.016(3) 0.018(2) 0.028(3) -0.002(2) -0.001(2) -0.005(2) O6 0.062(4) 0.032(3) 0.023(3) 0.004(2) -0.012(3) -0.016(3) O7 0.027(3) 0.046(3) 0.022(3) 0.007(2) 0.000(2) -0.019(3) O8 0.029(3) 0.035(3) 0.026(3) 0.002(2) -0.004(2) -0.014(2) O1W 0.018(3) 0.019(2) 0.019(2) 0.0002(19) -0.001(2) 0.001(2) O2W 0.032(3) 0.031(3) 0.027(3) 0.007(2) 0.009(2) 0.004(2) O3W 0.022(3) 0.066(4) 0.043(3) -0.027(3) 0.009(2) -0.007(3) O4W 0.064(4) 0.042(3) 0.029(3) 0.008(3) -0.004(3) -0.024(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 Co1 O4 2.073(4) 3_657 ? Co1 O4 2.073(4) 1_655 ? Co1 O5 2.142(4) . ? Co1 O5 2.142(4) 3_757 ? Co1 O1 2.292(4) 3_757 ? Co1 O1 2.292(4) . ? Co2 O3 2.028(4) 1_655 ? Co2 O7 2.042(5) 2_746 ? Co2 O1W 2.045(4) . ? Co2 O5 2.104(4) 3_757 ? Co2 O1 2.121(4) . ? Co2 O2W 2.322(4) 3_756 ? Co3 O2 2.049(5) 3_756 ? Co3 O3W 2.086(5) . ? Co3 O1W 2.086(4) 3_756 ? Co3 O8 2.104(4) 2_746 ? Co3 O1W 2.108(4) . ? Co3 O2W 2.197(4) . ? C1 O2 1.256(7) . ? C1 O1 1.275(7) . ? C1 C2 1.485(9) . ? C2 C3 1.386(8) . ? C2 C7 1.402(8) . ? C3 C4 1.389(8) . ? C3 H3 0.9300 . ? C4 C5 1.387(8) . ? C4 C16 1.502(8) . ? C5 C6 1.401(9) . ? C5 H5 0.9300 . ? C6 C7 1.399(9) . ? C6 H6 0.9300 . ? C7 C8 1.487(8) . ? C8 C13 1.397(8) . ? C8 C9 1.398(8) . ? C9 C10 1.404(8) . ? C9 C15 1.501(8) . ? C10 C11 1.374(8) . ? C10 H10 0.9300 . ? C11 C12 1.381(8) . ? C11 C14 1.508(8) . ? C12 C13 1.374(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O7 1.250(7) . ? C14 O8 1.278(7) . ? C15 O6 1.244(7) . ? C15 O5 1.272(7) . ? C16 O4 1.250(7) . ? C16 O3 1.259(7) . ? O2 Co3 2.049(5) 3_756 ? O3 Co2 2.028(4) 1_455 ? O4 Co1 2.073(4) 1_455 ? O5 Co2 2.104(4) 3_757 ? O7 Co2 2.042(5) 2_756 ? O8 Co3 2.104(4) 2_756 ? O1W Co3 2.086(4) 3_756 ? O1W H1W 0.8501 . ? O2W Co2 2.321(4) 3_756 ? O2W H2WA 0.8500 . ? O2W H2WB 0.8500 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8501 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Co1 O4 180.0 3_657 1_655 ? O4 Co1 O5 92.27(16) 3_657 . ? O4 Co1 O5 87.73(16) 1_655 . ? O4 Co1 O5 87.73(16) 3_657 3_757 ? O4 Co1 O5 92.27(16) 1_655 3_757 ? O5 Co1 O5 180 . 3_757 ? O4 Co1 O1 94.98(15) 3_657 3_757 ? O4 Co1 O1 85.02(15) 1_655 3_757 ? O5 Co1 O1 73.31(15) . 3_757 ? O5 Co1 O1 106.69(15) 3_757 3_757 ? O4 Co1 O1 85.02(15) 3_657 . ? O4 Co1 O1 94.98(15) 1_655 . ? O5 Co1 O1 106.69(15) . . ? O5 Co1 O1 73.31(15) 3_757 . ? O1 Co1 O1 180 3_757 . ? O3 Co2 O7 87.89(19) 1_655 2_746 ? O3 Co2 O1W 95.78(17) 1_655 . ? O7 Co2 O1W 97.98(17) 2_746 . ? O3 Co2 O5 92.57(16) 1_655 3_757 ? O7 Co2 O5 88.79(17) 2_746 3_757 ? O1W Co2 O5 169.41(16) . 3_757 ? O3 Co2 O1 87.07(17) 1_655 . ? O7 Co2 O1 165.32(17) 2_746 . ? O1W Co2 O1 96.23(16) . . ? O5 Co2 O1 77.68(16) 3_757 . ? O3 Co2 O2W 170.74(17) 1_655 3_756 ? O7 Co2 O2W 88.78(17) 2_746 3_756 ? O1W Co2 O2W 76.13(15) . 3_756 ? O5 Co2 O2W 96.00(15) 3_757 3_756 ? O1 Co2 O2W 98.18(16) . 3_756 ? O2 Co3 O3W 86.00(19) 3_756 . ? O2 Co3 O1W 97.91(17) 3_756 3_756 ? O3W Co3 O1W 170.48(18) . 3_756 ? O2 Co3 O8 91.27(19) 3_756 2_746 ? O3W Co3 O8 99.79(19) . 2_746 ? O1W Co3 O8 88.83(17) 3_756 2_746 ? O2 Co3 O1W 177.42(18) 3_756 . ? O3W Co3 O1W 91.63(17) . . ? O1W Co3 O1W 84.26(16) 3_756 . ? O8 Co3 O1W 90.16(17) 2_746 . ? O2 Co3 O2W 91.76(18) 3_756 . ? O3W Co3 O2W 93.11(18) . . ? O1W Co3 O2W 78.16(16) 3_756 . ? O8 Co3 O2W 166.92(18) 2_746 . ? O1W Co3 O2W 87.32(16) . . ? O2 C1 O1 123.5(6) . . ? O2 C1 C2 117.5(6) . . ? O1 C1 C2 119.1(6) . . ? C3 C2 C7 118.8(6) . . ? C3 C2 C1 119.6(5) . . ? C7 C2 C1 121.6(6) . . ? C2 C3 C4 122.2(6) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? C5 C4 C3 119.0(6) . . ? C5 C4 C16 121.6(6) . . ? C3 C4 C16 119.2(6) . . ? C4 C5 C6 119.7(6) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 120.8(6) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C2 C7 C6 119.2(6) . . ? C2 C7 C8 121.1(6) . . ? C6 C7 C8 119.2(5) . . ? C13 C8 C9 118.1(6) . . ? C13 C8 C7 117.1(5) . . ? C9 C8 C7 124.4(6) . . ? C8 C9 C10 119.9(6) . . ? C8 C9 C15 123.4(6) . . ? C10 C9 C15 116.7(5) . . ? C11 C10 C9 120.3(6) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.2(6) . . ? C10 C11 C14 118.7(6) . . ? C12 C11 C14 121.1(6) . . ? C13 C12 C11 119.9(6) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C8 121.6(6) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? O7 C14 O8 124.8(6) . . ? O7 C14 C11 117.9(6) . . ? O8 C14 C11 117.2(6) . . ? O6 C15 O5 125.4(6) . . ? O6 C15 C9 117.1(5) . . ? O5 C15 C9 117.5(6) . . ? O4 C16 O3 125.3(6) . . ? O4 C16 C4 120.8(6) . . ? O3 C16 C4 113.9(6) . . ? C1 O1 Co2 126.3(4) . . ? C1 O1 Co1 129.4(4) . . ? Co2 O1 Co1 95.45(15) . . ? C1 O2 Co3 134.7(4) . 3_756 ? C16 O3 Co2 134.9(4) . 1_455 ? C16 O4 Co1 126.1(4) . 1_455 ? C15 O5 Co2 121.3(4) . 3_757 ? C15 O5 Co1 128.1(4) . . ? Co2 O5 Co1 100.64(17) 3_757 . ? C14 O7 Co2 125.7(4) . 2_756 ? C14 O8 Co3 121.5(4) . 2_756 ? Co2 O1W Co3 99.25(17) . 3_756 ? Co2 O1W Co3 121.09(19) . . ? Co3 O1W Co3 95.73(16) 3_756 . ? Co2 O1W H1W 108.7 . . ? Co3 O1W H1W 118.0 3_756 . ? Co3 O1W H1W 113.2 . . ? Co3 O2W Co2 88.26(15) . 3_756 ? Co3 O2W H2WA 113.9 . . ? Co2 O2W H2WA 91.8 3_756 . ? Co3 O2W H2WB 142.2 . . ? Co2 O2W H2WB 86.4 3_756 . ? H2WA O2W H2WB 103.7 . . ? Co3 O3W H3WA 109.6 . . ? Co3 O3W H3WB 121.8 . . ? H3WA O3W H3WB 127.6 . . ? H4WA O4W H4WB 114.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2W H2WA O8 0.85 1.95 2.730(7) 151.6 4_565 O2W H2WA O7 0.85 2.62 3.059(6) 113.7 4_565 O2W H2WB O6 0.85 1.84 2.630(6) 154.7 1_554 O3W H3WA O3W 0.85 2.27 2.932(10) 134.4 3_856 O3W H3WB O4W 0.85 1.85 2.648(7) 155.5 1_655 O4W H4WA O6 0.85 2.14 2.972(7) 165.7 4_565 O4W H4WB O3 0.85 1.88 2.719(6) 169.7 . O1W H1W O4W 0.85 2.49 3.098(6) 129.2 1_655 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.875 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.143 # complex 7.cif===END data_complex_8 _database_code_depnum_ccdc_archive 'CCDC 744738' #TrackingRef 'complex1-8_2new1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 Co5 O28' _chemical_formula_weight 1163.26 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6129(10) _cell_length_b 19.542(2) _cell_length_c 11.4698(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.5640(10) _cell_angle_gamma 90.00 _cell_volume 1930.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3006 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.16 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.001 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1174 _exptl_absorpt_coefficient_mu 2.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6660 _exptl_absorpt_correction_T_max 0.6660 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6569 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0817 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2339 _reflns_number_gt 1770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0068P)^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 2339 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_restrained_S_all 0.905 _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 Co1 Co 0.60742(7) 0.54020(3) 0.73898(5) 0.01356(16) Uani 1 1 d . . . Co2 Co 1.0000 1.0000 0.5000 0.0142(2) Uani 1 2 d S . . Co3 Co 0.51693(8) 0.57860(3) 0.47748(5) 0.01905(17) Uani 1 1 d . . . C1 C 0.7483(6) 0.6603(2) 0.6133(4) 0.0203(11) Uani 1 1 d . . . C2 C 0.8733(5) 0.7148(2) 0.6072(4) 0.0163(10) Uani 1 1 d . . . C3 C 0.9879(6) 0.7197(2) 0.6933(4) 0.0248(12) Uani 1 1 d . . . H3 H 0.9837 0.6916 0.7586 0.030 Uiso 1 1 calc R . . C4 C 1.1078(6) 0.7661(2) 0.6822(4) 0.0236(11) Uani 1 1 d . . . H4 H 1.1841 0.7684 0.7400 0.028 Uiso 1 1 calc R . . C5 C 1.1166(5) 0.8093(2) 0.5860(4) 0.0170(11) Uani 1 1 d . . . C6 C 0.9997(5) 0.8059(2) 0.5012(4) 0.0154(10) Uani 1 1 d . . . C7 C 0.8806(5) 0.7590(2) 0.5134(4) 0.0190(11) Uani 1 1 d . . . H7 H 0.8029 0.7572 0.4567 0.023 Uiso 1 1 calc R . . C8 C 0.9990(5) 0.8485(2) 0.3918(4) 0.0191(11) Uani 1 1 d . . . C9 C 1.1509(5) 0.9356(2) 0.7256(4) 0.0178(11) Uani 1 1 d . . . C10 C 1.2775(5) 0.9105(2) 0.6479(4) 0.0143(10) Uani 1 1 d . . . C11 C 1.4162(5) 0.9455(2) 0.6487(4) 0.0172(11) Uani 1 1 d . . . H11 H 1.4286 0.9830 0.6979 0.021 Uiso 1 1 calc R . . C12 C 1.5376(5) 0.9262(2) 0.5776(4) 0.0169(10) Uani 1 1 d . . . C13 C 1.5163(5) 0.8719(2) 0.5005(4) 0.0210(11) Uani 1 1 d . . . H13 H 1.5937 0.8600 0.4482 0.025 Uiso 1 1 calc R . . C14 C 1.3783(5) 0.8359(2) 0.5030(4) 0.0277(12) Uani 1 1 d . . . H14 H 1.3663 0.7984 0.4539 0.033 Uiso 1 1 calc R . . C15 C 1.2566(5) 0.8535(2) 0.5758(4) 0.0157(10) Uani 1 1 d . . . C16 C 1.6894(5) 0.9623(2) 0.5917(4) 0.0152(10) Uani 1 1 d . . . O1 O 0.7542(4) 0.61994(15) 0.6977(3) 0.0244(8) Uani 1 1 d . . . O2 O 0.6524(4) 0.65852(16) 0.5301(3) 0.0278(9) Uani 1 1 d . . . O3 O 0.9487(5) 0.82000(17) 0.3020(3) 0.0394(10) Uani 1 1 d . . . O4 O 1.0533(3) 0.90910(14) 0.3955(3) 0.0182(7) Uani 1 1 d . . . O5 O 1.0376(3) 0.96743(15) 0.6787(2) 0.0155(7) Uani 1 1 d . . . O6 O 1.1653(4) 0.92615(17) 0.8331(3) 0.0276(8) Uani 1 1 d . . . O7 O 1.7077(4) 0.99489(16) 0.6852(3) 0.0238(8) Uani 1 1 d . . . O8 O 1.7878(3) 0.95749(16) 0.5108(3) 0.0192(7) Uani 1 1 d . . . O1W O 0.3981(4) 0.58802(16) 0.6432(3) 0.0268(8) Uani 1 1 d . . . H1WA H 0.3107 0.5684 0.6512 0.032 Uiso 1 1 d R . . H1WB H 0.4099 0.6210 0.6908 0.032 Uiso 1 1 d R . . O2W O 0.3726(3) 0.50018(14) 0.4261(2) 0.0187(7) Uani 1 1 d . . . H2W H 0.2793 0.5077 0.4459 0.022 Uiso 1 1 d R . . O3W O 0.3804(5) 0.6550(2) 0.3906(4) 0.0577(12) Uani 1 1 d . . . H3WA H 0.3190 0.6210 0.3945 0.069 Uiso 1 1 d R . . H3WB H 0.3116 0.6697 0.3433 0.069 Uiso 1 1 d R . . O4W O 0.4183(6) 0.0572(3) 0.8654(5) 0.100(2) Uani 1 1 d . . . H4WA H 0.3630 0.0332 0.9109 0.120 Uiso 1 1 d R . . H4WB H 0.4715 0.0906 0.8402 0.120 Uiso 1 1 d R . . O5W O 0.9037(6) 0.3067(2) 0.7234(4) 0.0818(16) Uani 1 1 d . . . H5WA H 0.9318 0.3335 0.6691 0.098 Uiso 1 1 d R . . H5WB H 0.9229 0.3289 0.7857 0.098 Uiso 1 1 d R . . O6W O 0.5107(9) 0.9125(3) 0.9199(5) 0.152(3) Uani 1 1 d . . . H6WA H 0.4146 0.9069 0.9056 0.183 Uiso 1 1 d R . . H6WB H 0.5069 0.9406 0.8634 0.183 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0132(3) 0.0145(3) 0.0130(3) 0.0012(2) 0.0015(3) -0.0011(3) Co2 0.0104(5) 0.0187(5) 0.0134(5) -0.0009(4) 0.0019(4) -0.0033(4) Co3 0.0230(4) 0.0183(3) 0.0158(3) -0.0007(3) 0.0003(3) -0.0076(3) C1 0.022(3) 0.020(3) 0.019(3) -0.003(2) 0.002(2) -0.008(2) C2 0.015(3) 0.017(2) 0.017(2) 0.0008(19) -0.002(2) -0.005(2) C3 0.028(3) 0.030(3) 0.016(2) 0.010(2) 0.000(2) -0.010(2) C4 0.020(3) 0.031(3) 0.020(3) 0.006(2) -0.012(2) -0.011(2) C5 0.018(3) 0.014(2) 0.019(3) -0.0046(19) 0.003(2) -0.002(2) C6 0.016(3) 0.016(2) 0.015(2) 0.0019(18) -0.001(2) -0.003(2) C7 0.016(3) 0.022(3) 0.019(3) 0.003(2) -0.005(2) -0.003(2) C8 0.019(3) 0.017(3) 0.021(3) 0.007(2) -0.001(2) -0.003(2) C9 0.015(3) 0.017(3) 0.021(3) 0.000(2) 0.002(2) -0.005(2) C10 0.013(3) 0.019(3) 0.011(2) 0.0028(18) 0.000(2) -0.0009(19) C11 0.015(3) 0.016(2) 0.021(3) -0.002(2) -0.001(2) -0.004(2) C12 0.014(3) 0.019(3) 0.018(2) -0.002(2) 0.000(2) -0.001(2) C13 0.013(3) 0.029(3) 0.021(3) -0.005(2) 0.005(2) -0.001(2) C14 0.026(3) 0.027(3) 0.030(3) -0.018(2) 0.009(3) -0.008(2) C15 0.010(2) 0.020(2) 0.017(2) 0.0014(19) -0.001(2) -0.0027(19) C16 0.012(3) 0.014(2) 0.020(3) 0.0012(19) 0.001(2) 0.000(2) O1 0.026(2) 0.0247(19) 0.0228(18) 0.0098(15) -0.0019(16) -0.0106(15) O2 0.032(2) 0.0245(19) 0.027(2) 0.0053(15) -0.0083(18) -0.0165(16) O3 0.064(3) 0.034(2) 0.0194(19) 0.0054(16) -0.015(2) -0.023(2) O4 0.0174(18) 0.0150(17) 0.0222(17) 0.0037(13) 0.0055(15) -0.0041(13) O5 0.0133(18) 0.0204(17) 0.0129(17) -0.0003(13) 0.0002(14) 0.0037(14) O6 0.022(2) 0.045(2) 0.0160(18) 0.0028(16) 0.0035(16) 0.0089(17) O7 0.0130(18) 0.032(2) 0.027(2) -0.0078(16) 0.0036(15) -0.0081(15) O8 0.0117(17) 0.0289(19) 0.0169(17) -0.0016(14) 0.0023(15) -0.0069(14) O1W 0.030(2) 0.0260(19) 0.0243(19) -0.0093(15) 0.0026(17) -0.0037(16) O2W 0.0174(18) 0.0190(17) 0.0197(18) -0.0048(13) 0.0027(15) -0.0030(14) O3W 0.051(3) 0.045(3) 0.076(3) 0.018(2) -0.017(3) 0.007(2) O4W 0.076(4) 0.078(4) 0.145(5) -0.042(4) -0.022(4) 0.002(3) O5W 0.100(4) 0.068(3) 0.077(4) -0.021(3) -0.007(3) -0.011(3) O6W 0.237(9) 0.154(7) 0.067(4) 0.030(4) 0.003(5) 0.091(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 Co1 O7 2.012(3) 2_746 ? Co1 O2W 2.060(3) 3_666 ? Co1 O1 2.065(3) . ? Co1 O4 2.107(3) 4_576 ? Co1 O5 2.121(3) 2_646 ? Co1 O1W 2.300(3) . ? Co2 O8 2.013(3) 1_455 ? Co2 O8 2.013(3) 3_876 ? Co2 O5 2.168(3) . ? Co2 O5 2.168(3) 3_776 ? Co2 O4 2.194(3) . ? Co2 O4 2.194(3) 3_776 ? Co3 O2 2.038(3) . ? Co3 O2W 2.056(3) . ? Co3 O6 2.104(3) 4_575 ? Co3 O2W 2.116(3) 3_666 ? Co3 O3W 2.140(4) . ? Co3 O1W 2.176(3) . ? C1 O1 1.249(5) . ? C1 O2 1.256(5) . ? C1 C2 1.517(6) . ? C2 C7 1.381(6) . ? C2 C3 1.393(6) . ? C3 C4 1.380(6) . ? C3 H3 0.9300 . ? C4 C5 1.393(6) . ? C4 H4 0.9300 . ? C5 C6 1.394(6) . ? C5 C15 1.488(6) . ? C6 C7 1.384(6) . ? C6 C8 1.506(6) . ? C7 H7 0.9300 . ? C8 O3 1.244(5) . ? C8 O4 1.274(5) . ? C9 O6 1.252(5) . ? C9 O5 1.272(5) . ? C9 C10 1.497(6) . ? C10 C11 1.377(6) . ? C10 C15 1.397(6) . ? C11 C12 1.385(6) . ? C11 H11 0.9300 . ? C12 C13 1.392(6) . ? C12 C16 1.492(6) . ? C13 C14 1.382(6) . ? C13 H13 0.9300 . ? C14 C15 1.390(6) . ? C14 H14 0.9300 . ? C16 O7 1.257(5) . ? C16 O8 1.266(5) . ? O4 Co1 2.107(3) 4_675 ? O5 Co1 2.121(3) 2_656 ? O6 Co3 2.104(3) 4_676 ? O7 Co1 2.012(3) 2_756 ? O8 Co2 2.013(3) 1_655 ? O1W H1WA 0.8500 . ? O1W H1WB 0.8499 . ? O2W Co1 2.060(3) 3_666 ? O2W Co3 2.116(3) 3_666 ? O2W H2W 0.8500 . ? O3W H3WA 0.8501 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8501 . ? O5W H5WA 0.8499 . ? O5W H5WB 0.8500 . ? O6W H6WA 0.8500 . ? O6W H6WB 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Co1 O2W 98.95(12) 2_746 3_666 ? O7 Co1 O1 86.99(13) 2_746 . ? O2W Co1 O1 91.22(12) 3_666 . ? O7 Co1 O4 91.13(12) 2_746 4_576 ? O2W Co1 O4 169.91(12) 3_666 4_576 ? O1 Co1 O4 88.95(12) . 4_576 ? O7 Co1 O5 88.85(12) 2_746 2_646 ? O2W Co1 O5 101.96(11) 3_666 2_646 ? O1 Co1 O5 166.65(12) . 2_646 ? O4 Co1 O5 78.45(11) 4_576 2_646 ? O7 Co1 O1W 176.73(13) 2_746 . ? O2W Co1 O1W 77.83(11) 3_666 . ? O1 Co1 O1W 93.59(12) . . ? O4 Co1 O1W 92.09(11) 4_576 . ? O5 Co1 O1W 91.29(11) 2_646 . ? O8 Co2 O8 180.0 1_455 3_876 ? O8 Co2 O5 87.02(12) 1_455 . ? O8 Co2 O5 92.98(12) 3_876 . ? O8 Co2 O5 92.98(12) 1_455 3_776 ? O8 Co2 O5 87.01(12) 3_876 3_776 ? O5 Co2 O5 180 . 3_776 ? O8 Co2 O4 83.93(11) 1_455 . ? O8 Co2 O4 96.07(11) 3_876 . ? O5 Co2 O4 104.40(11) . . ? O5 Co2 O4 75.60(11) 3_776 . ? O8 Co2 O4 96.07(11) 1_455 3_776 ? O8 Co2 O4 83.93(11) 3_876 3_776 ? O5 Co2 O4 75.60(11) . 3_776 ? O5 Co2 O4 104.40(11) 3_776 3_776 ? O4 Co2 O4 180 . 3_776 ? O2 Co3 O2W 177.74(14) . . ? O2 Co3 O6 85.21(13) . 4_575 ? O2W Co3 O6 96.41(12) . 4_575 ? O2 Co3 O2W 98.59(12) . 3_666 ? O2W Co3 O2W 82.83(12) . 3_666 ? O6 Co3 O2W 96.08(12) 4_575 3_666 ? O2 Co3 O3W 85.07(15) . . ? O2W Co3 O3W 93.34(14) . . ? O6 Co3 O3W 89.97(15) 4_575 . ? O2W Co3 O3W 173.15(14) 3_666 . ? O2 Co3 O1W 87.10(12) . . ? O2W Co3 O1W 91.45(12) . . ? O6 Co3 O1W 170.46(13) 4_575 . ? O2W Co3 O1W 79.50(11) 3_666 . ? O3W Co3 O1W 94.98(14) . . ? O1 C1 O2 126.4(4) . . ? O1 C1 C2 117.1(4) . . ? O2 C1 C2 116.5(4) . . ? C7 C2 C3 118.1(4) . . ? C7 C2 C1 120.9(4) . . ? C3 C2 C1 120.9(4) . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 121.2(5) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 118.6(4) . . ? C4 C5 C15 117.7(4) . . ? C6 C5 C15 123.6(4) . . ? C7 C6 C5 119.5(4) . . ? C7 C6 C8 116.9(4) . . ? C5 C6 C8 123.5(4) . . ? C2 C7 C6 122.2(4) . . ? C2 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? O3 C8 O4 124.6(4) . . ? O3 C8 C6 116.2(4) . . ? O4 C8 C6 119.1(4) . . ? O6 C9 O5 123.8(4) . . ? O6 C9 C10 118.2(4) . . ? O5 C9 C10 118.0(4) . . ? C11 C10 C15 120.5(4) . . ? C11 C10 C9 118.0(4) . . ? C15 C10 C9 121.5(4) . . ? C10 C11 C12 121.4(4) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 119.1(4) . . ? C11 C12 C16 118.2(4) . . ? C13 C12 C16 122.6(4) . . ? C14 C13 C12 118.9(4) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C13 C14 C15 122.7(4) . . ? C13 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? C14 C15 C10 117.3(4) . . ? C14 C15 C5 121.3(4) . . ? C10 C15 C5 121.0(4) . . ? O7 C16 O8 125.7(4) . . ? O7 C16 C12 115.8(4) . . ? O8 C16 C12 118.5(4) . . ? C1 O1 Co1 129.4(3) . . ? C1 O2 Co3 128.0(3) . . ? C8 O4 Co1 119.5(3) . 4_675 ? C8 O4 Co2 133.8(3) . . ? Co1 O4 Co2 97.70(11) 4_675 . ? C9 O5 Co1 126.4(3) . 2_656 ? C9 O5 Co2 130.6(3) . . ? Co1 O5 Co2 98.09(12) 2_656 . ? C9 O6 Co3 136.6(3) . 4_676 ? C16 O7 Co1 133.2(3) . 2_756 ? C16 O8 Co2 129.0(3) . 1_655 ? Co3 O1W Co1 90.54(11) . . ? Co3 O1W H1WA 118.7 . . ? Co1 O1W H1WA 117.1 . . ? Co3 O1W H1WB 124.8 . . ? Co1 O1W H1WB 85.0 . . ? H1WA O1W H1WB 112.0 . . ? Co3 O2W Co1 119.56(14) . 3_666 ? Co3 O2W Co3 97.17(12) . 3_666 ? Co1 O2W Co3 99.24(12) 3_666 3_666 ? Co3 O2W H2W 111.4 . . ? Co1 O2W H2W 113.6 3_666 . ? Co3 O2W H2W 114.0 3_666 . ? Co3 O3W H3WA 76.7 . . ? Co3 O3W H3WB 155.5 . . ? H3WA O3W H3WB 82.4 . . ? H4WA O4W H4WB 159.9 . . ? H5WA O5W H5WB 104.3 . . ? H6WA O6W H6WB 84.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6W H6WB O4W 0.85 2.40 3.002(8) 128.0 1_565 O6W H6WA O6 0.85 2.33 3.139(8) 160.6 1_455 O5W H5WA O6W 0.85 1.92 2.746(8) 164.1 2_646 O4W H4WB O1 0.85 2.47 3.167(6) 139.2 2_646 O3W H3WB O5W 0.85 2.05 2.863(6) 159.4 3_666 O3W H3WA O2W 0.85 2.43 3.053(5) 130.4 . O1W H1WB O3 0.85 1.75 2.593(4) 171.4 4_576 O1W H1WA O4W 0.85 1.99 2.791(6) 156.3 2_556 _diffrn_measured_fraction_theta_max 0.689 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.689 _refine_diff_density_max 0.431 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.074 # complex 8.cif===END