# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Yao-Yu Wan' _publ_contact_author_email wyaoyu@nwu.edu.cn _publ_section_title ; Structural diversity of coordination polymers assembled from adamantane dicarboxylates and conformational bis-triazole ligand ; loop_ _publ_author_name 'Chen Ren' 'Ya-Nan Zhang' 'Wen-Juan Shi' 'Bo Liu' 'Yao-Yu Wang' ; Qizhen Shi ; # Attachment '- cifs 1-6.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 802233' #TrackingRef '- cifs 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H36 N6 O7 Zn' _chemical_formula_sum 'C30 H36 N6 O7 Zn' _chemical_formula_weight 658.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.793(3) _cell_length_b 21.363(4) _cell_length_c 10.187(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.379(3) _cell_angle_gamma 90.00 _cell_volume 3506.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3016 _cell_measurement_theta_min 2.286 _cell_measurement_theta_max 21.446 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7954 _exptl_absorpt_correction_T_max 0.9154 _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 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17281 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.10 _reflns_number_total 6242 _reflns_number_gt 3669 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1861P)^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 6242 _refine_ls_number_parameters 397 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2824 _refine_ls_wR_factor_gt 0.2420 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.056 _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 0.58544(4) -0.11208(3) 0.00394(6) 0.0664(3) Uani 1 1 d . . . C1 C 0.7196(4) -0.0198(3) -0.0112(7) 0.0836(17) Uani 1 1 d . . . H1 H 0.7466 -0.0489 -0.0513 0.100 Uiso 1 1 calc R . . C2 C 0.6317(3) 0.0233(3) 0.0799(5) 0.0657(14) Uani 1 1 d . . . H2 H 0.5866 0.0298 0.1144 0.079 Uiso 1 1 calc R . . C3 C 0.6888(4) 0.1311(3) 0.1122(7) 0.0815(17) Uani 1 1 d . . . H3A H 0.6369 0.1412 0.1315 0.098 Uiso 1 1 calc R . . H3B H 0.6919 0.1561 0.0343 0.098 Uiso 1 1 calc R . . C4 C 0.7600(3) 0.1496(3) 0.2349(6) 0.0685(15) Uani 1 1 d . . . C5 C 0.7884(4) 0.1110(3) 0.3446(8) 0.094(2) Uani 1 1 d . . . H5 H 0.7655 0.0713 0.3432 0.112 Uiso 1 1 calc R . . C6 C 0.8504(4) 0.1299(3) 0.4573(7) 0.0908(19) Uani 1 1 d . . . H6 H 0.8693 0.1019 0.5295 0.109 Uiso 1 1 calc R . . C7 C 0.8856(3) 0.1884(3) 0.4676(7) 0.0748(16) Uani 1 1 d . . . C8 C 0.8551(4) 0.2273(3) 0.3508(8) 0.105(2) Uani 1 1 d . . . H8 H 0.8769 0.2673 0.3508 0.126 Uiso 1 1 calc R . . C9 C 0.7945(4) 0.2072(3) 0.2388(7) 0.092(2) Uani 1 1 d . . . H9 H 0.7765 0.2336 0.1637 0.110 Uiso 1 1 calc R . . C10 C 0.9528(3) 0.2099(3) 0.5903(6) 0.0744(16) Uani 1 1 d . . . C11 C 0.9969(4) 0.1682(3) 0.6844(8) 0.111(3) Uani 1 1 d . . . H11 H 0.9854 0.1257 0.6727 0.133 Uiso 1 1 calc R . . C12 C 1.0586(5) 0.1887(4) 0.7967(9) 0.117(3) Uani 1 1 d . . . H12 H 1.0866 0.1592 0.8601 0.140 Uiso 1 1 calc R . . C13 C 1.0801(3) 0.2496(3) 0.8189(7) 0.0796(17) Uani 1 1 d . . . C14 C 1.0377(4) 0.2914(4) 0.7225(7) 0.102(2) Uani 1 1 d . . . H14 H 1.0518 0.3336 0.7318 0.122 Uiso 1 1 calc R . . C15 C 0.9740(4) 0.2719(3) 0.6113(7) 0.097(2) Uani 1 1 d . . . H15 H 0.9449 0.3015 0.5493 0.116 Uiso 1 1 calc R . . C16 C 1.1485(4) 0.2694(3) 0.9406(7) 0.093(2) Uani 1 1 d . . . H16A H 1.1509 0.3147 0.9459 0.112 Uiso 1 1 calc R . . H16B H 1.1381 0.2536 1.0235 0.112 Uiso 1 1 calc R . . C17 C 1.2732(3) 0.1994(3) 0.9985(5) 0.0713(15) Uani 1 1 d . . . H17 H 1.2633 0.1804 1.0745 0.086 Uiso 1 1 calc R . . C18 C 1.3223(4) 0.2250(4) 0.8421(8) 0.099(2) Uani 1 1 d . . . H18 H 1.3572 0.2271 0.7858 0.119 Uiso 1 1 calc R . . C19 C 0.5390(4) -0.1189(2) -0.2667(5) 0.0631(14) Uani 1 1 d . . . C20 C 0.4874(3) -0.1238(2) -0.4144(5) 0.0566(13) Uani 1 1 d . . . C21 C 0.5416(3) -0.1144(2) -0.5107(5) 0.0554(12) Uani 1 1 d . . . H21A H 0.5663 -0.0730 -0.4965 0.066 Uiso 1 1 calc R . . H21B H 0.5862 -0.1449 -0.4895 0.066 Uiso 1 1 calc R . . C22 C 0.4917(3) -0.1213(2) -0.6593(5) 0.0593(13) Uani 1 1 d . . . C23 C 0.4551(4) -0.1859(3) -0.6827(6) 0.0755(16) Uani 1 1 d . . . H23A H 0.4992 -0.2168 -0.6648 0.091 Uiso 1 1 calc R . . H23B H 0.4222 -0.1902 -0.7772 0.091 Uiso 1 1 calc R . . C24 C 0.4003(4) -0.1972(3) -0.5876(6) 0.0719(15) Uani 1 1 d . . . H24 H 0.3771 -0.2396 -0.6026 0.086 Uiso 1 1 calc R . . C25 C 0.4506(4) -0.1903(2) -0.4396(6) 0.0698(15) Uani 1 1 d . . . H25A H 0.4951 -0.2209 -0.4181 0.084 Uiso 1 1 calc R . . H25B H 0.4155 -0.1979 -0.3803 0.084 Uiso 1 1 calc R . . C26 C 0.4168(3) -0.0769(2) -0.4464(5) 0.0591(13) Uani 1 1 d . . . H26A H 0.4392 -0.0348 -0.4315 0.071 Uiso 1 1 calc R . . H26B H 0.3824 -0.0836 -0.3856 0.071 Uiso 1 1 calc R . . C27 C 0.3637(4) -0.0839(3) -0.5963(5) 0.0668(14) Uani 1 1 d . . . H27 H 0.3179 -0.0537 -0.6158 0.080 Uiso 1 1 calc R . . C28 C 0.4174(4) -0.0723(3) -0.6912(5) 0.0706(15) Uani 1 1 d . . . H28A H 0.4395 -0.0300 -0.6783 0.085 Uiso 1 1 calc R . . H28B H 0.3843 -0.0765 -0.7856 0.085 Uiso 1 1 calc R . . C29 C 0.3295(4) -0.1497(3) -0.6193(6) 0.0836(18) Uani 1 1 d . . . H29A H 0.2963 -0.1544 -0.7136 0.100 Uiso 1 1 calc R . . H29B H 0.2939 -0.1574 -0.5607 0.100 Uiso 1 1 calc R . . C30 C 0.5439(5) -0.1106(3) -0.7568(6) 0.084(2) Uani 1 1 d . . . N1 N 0.6493(3) -0.0303(2) 0.0283(4) 0.0734(13) Uani 1 1 d . . . N2 N 0.7431(4) 0.0407(3) 0.0183(6) 0.1036(18) Uani 1 1 d . . . N3 N 0.6874(3) 0.0658(2) 0.0750(5) 0.0701(12) Uani 1 1 d . . . N4 N 1.3345(3) 0.1846(2) 0.9471(4) 0.0695(12) Uani 1 1 d . . . N5 N 1.2281(3) 0.2446(2) 0.9284(5) 0.0773(13) Uani 1 1 d . . . N6 N 1.2577(4) 0.2610(3) 0.8256(7) 0.110(2) Uani 1 1 d . . . O1 O 0.5008(2) -0.11408(18) -0.1746(4) 0.0746(11) Uani 1 1 d . . . O2 O 0.6173(3) -0.1207(2) -0.2325(4) 0.0918(14) Uani 1 1 d . . . O3 O 0.6194(4) -0.1001(3) -0.7125(5) 0.143(3) Uani 1 1 d . . . O4 O 0.5087(3) -0.1142(2) -0.8834(4) 0.0887(14) Uani 1 1 d . . . O5 O 0.2328(5) 0.0855(4) 0.2778(13) 0.225(4) Uani 1 1 d U . . O6 O 0.2373(6) 0.0590(6) 0.5566(13) 0.267(5) Uani 1 1 d U . . O7 O 0.9069(8) 0.0817(7) 0.9636(18) 0.346(8) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0676(5) 0.0944(6) 0.0351(4) 0.0031(3) 0.0110(3) 0.0077(3) C1 0.073(4) 0.104(5) 0.083(5) -0.011(4) 0.038(3) 0.001(4) C2 0.065(3) 0.083(4) 0.047(3) -0.002(3) 0.013(2) 0.010(3) C3 0.068(4) 0.093(4) 0.076(4) -0.005(3) 0.007(3) 0.008(3) C4 0.052(3) 0.086(4) 0.063(4) -0.009(3) 0.007(2) 0.006(3) C5 0.094(5) 0.090(5) 0.081(5) -0.006(4) -0.001(4) -0.023(4) C6 0.094(4) 0.099(5) 0.066(4) 0.010(3) -0.001(3) -0.003(4) C7 0.054(3) 0.088(4) 0.078(4) -0.010(3) 0.011(3) 0.000(3) C8 0.084(4) 0.091(5) 0.111(6) 0.017(4) -0.017(4) -0.014(4) C9 0.078(4) 0.098(5) 0.080(5) 0.018(4) -0.010(3) -0.003(4) C10 0.055(3) 0.090(4) 0.072(4) -0.004(3) 0.008(3) 0.006(3) C11 0.096(5) 0.079(4) 0.118(6) -0.004(4) -0.033(4) 0.003(4) C12 0.104(5) 0.091(5) 0.117(6) 0.002(4) -0.030(4) 0.018(4) C13 0.057(3) 0.097(5) 0.080(4) -0.015(3) 0.011(3) 0.012(3) C14 0.088(4) 0.104(5) 0.097(6) -0.004(4) -0.002(4) 0.004(4) C15 0.098(5) 0.089(5) 0.081(5) -0.003(4) -0.011(4) 0.004(4) C16 0.074(4) 0.103(5) 0.087(5) -0.013(4) -0.003(3) 0.023(3) C17 0.072(3) 0.095(4) 0.039(3) 0.000(3) 0.003(3) 0.005(3) C18 0.073(4) 0.125(6) 0.099(5) 0.046(5) 0.022(4) 0.003(4) C19 0.086(4) 0.074(3) 0.032(3) 0.004(2) 0.021(3) 0.016(3) C20 0.079(3) 0.061(3) 0.030(2) 0.004(2) 0.015(2) 0.008(2) C21 0.075(3) 0.061(3) 0.031(2) 0.004(2) 0.017(2) 0.006(2) C22 0.080(3) 0.066(3) 0.031(3) -0.002(2) 0.016(2) 0.005(3) C23 0.108(4) 0.071(4) 0.045(3) -0.012(3) 0.018(3) 0.010(3) C24 0.099(4) 0.057(3) 0.062(4) -0.010(3) 0.027(3) -0.013(3) C25 0.097(4) 0.061(3) 0.058(3) 0.004(3) 0.032(3) 0.004(3) C26 0.084(3) 0.061(3) 0.034(3) -0.001(2) 0.019(2) 0.008(3) C27 0.080(4) 0.071(3) 0.043(3) 0.000(3) 0.008(3) 0.012(3) C28 0.096(4) 0.081(4) 0.027(3) 0.001(2) 0.005(2) 0.005(3) C29 0.090(4) 0.100(5) 0.057(4) -0.014(3) 0.015(3) -0.013(4) C30 0.102(5) 0.122(6) 0.031(3) -0.002(3) 0.020(3) 0.006(4) N1 0.072(3) 0.102(4) 0.047(3) 0.001(2) 0.017(2) -0.001(3) N2 0.085(4) 0.137(6) 0.095(4) -0.005(4) 0.036(3) 0.006(4) N3 0.065(3) 0.082(3) 0.060(3) -0.009(2) 0.013(2) 0.003(2) N4 0.065(3) 0.093(3) 0.044(3) 0.010(2) 0.005(2) 0.002(2) N5 0.065(3) 0.086(3) 0.071(3) 0.001(3) 0.003(2) 0.005(3) N6 0.079(4) 0.124(5) 0.123(6) 0.058(4) 0.023(4) 0.012(3) O1 0.080(2) 0.112(3) 0.0330(19) 0.0008(18) 0.0189(18) 0.008(2) O2 0.081(3) 0.156(4) 0.037(2) 0.005(2) 0.014(2) 0.032(3) O3 0.100(4) 0.287(8) 0.048(3) -0.007(3) 0.029(3) -0.040(4) O4 0.092(3) 0.143(4) 0.032(2) 0.001(2) 0.0205(19) 0.007(2) O5 0.164(7) 0.221(8) 0.327(12) -0.061(8) 0.132(7) -0.032(6) O6 0.201(8) 0.294(11) 0.266(11) -0.001(9) 0.000(7) -0.064(8) O7 0.294(12) 0.332(13) 0.474(17) -0.036(11) 0.210(13) -0.089(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.952(4) 1_556 ? Zn1 O1 1.968(4) . ? Zn1 N4 2.018(5) 3_756 ? Zn1 N1 2.029(5) . ? C1 N2 1.359(8) . ? C1 N1 1.369(7) . ? C1 H1 0.9300 . ? C2 N3 1.315(7) . ? C2 N1 1.328(7) . ? C2 H2 0.9300 . ? C3 N3 1.445(8) . ? C3 C4 1.519(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.356(8) . ? C4 C5 1.362(9) . ? C5 C6 1.375(9) . ? C5 H5 0.9300 . ? C6 C7 1.374(9) . ? C6 H6 0.9300 . ? C7 C8 1.423(9) . ? C7 C10 1.500(8) . ? C8 C9 1.366(9) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.364(8) . ? C10 C15 1.373(9) . ? C11 C12 1.379(9) . ? C11 H11 0.9300 . ? C12 C13 1.353(9) . ? C12 H12 0.9300 . ? C13 C14 1.370(9) . ? C13 C16 1.494(9) . ? C14 C15 1.384(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N5 1.475(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N5 1.307(7) . ? C17 N4 1.319(7) . ? C17 H17 0.9300 . ? C18 N6 1.300(8) . ? C18 N4 1.345(7) . ? C18 H18 0.9300 . ? C19 O2 1.263(6) . ? C19 O1 1.282(6) . ? C19 C20 1.513(7) . ? C20 C26 1.516(7) . ? C20 C21 1.529(7) . ? C20 C25 1.541(7) . ? C21 C22 1.517(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.501(7) . ? C22 C30 1.517(8) . ? C22 C28 1.590(7) . ? C23 C24 1.532(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.514(8) . ? C24 C29 1.527(9) . ? C24 H24 0.9800 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.543(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C29 1.513(9) . ? C27 C28 1.518(8) . ? C27 H27 0.9800 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O3 1.241(8) . ? C30 O4 1.260(7) . ? N2 N3 1.340(6) . ? N4 Zn1 2.018(5) 3_756 ? N5 N6 1.327(8) . ? O4 Zn1 1.952(4) 1_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O1 96.78(17) 1_556 . ? O4 Zn1 N4 109.91(18) 1_556 3_756 ? O1 Zn1 N4 117.95(17) . 3_756 ? O4 Zn1 N1 111.24(19) 1_556 . ? O1 Zn1 N1 110.56(17) . . ? N4 Zn1 N1 109.8(2) 3_756 . ? N2 C1 N1 108.1(5) . . ? N2 C1 H1 126.0 . . ? N1 C1 H1 126.0 . . ? N3 C2 N1 109.8(5) . . ? N3 C2 H2 125.1 . . ? N1 C2 H2 125.1 . . ? N3 C3 C4 114.7(5) . . ? N3 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? N3 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C9 C4 C5 118.5(5) . . ? C9 C4 C3 119.4(6) . . ? C5 C4 C3 122.0(6) . . ? C4 C5 C6 121.0(6) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 122.6(6) . . ? C7 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? C6 C7 C8 115.0(6) . . ? C6 C7 C10 123.3(6) . . ? C8 C7 C10 121.7(6) . . ? C9 C8 C7 121.5(6) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C4 C9 C8 121.4(6) . . ? C4 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C15 117.0(6) . . ? C11 C10 C7 121.2(6) . . ? C15 C10 C7 121.8(6) . . ? C10 C11 C12 120.6(7) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 123.1(7) . . ? C13 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? C12 C13 C14 116.6(6) . . ? C12 C13 C16 121.2(6) . . ? C14 C13 C16 122.3(6) . . ? C13 C14 C15 121.1(7) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C10 C15 C14 121.7(7) . . ? C10 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? N5 C16 C13 109.4(5) . . ? N5 C16 H16A 109.8 . . ? C13 C16 H16A 109.8 . . ? N5 C16 H16B 109.8 . . ? C13 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? N5 C17 N4 111.0(5) . . ? N5 C17 H17 124.5 . . ? N4 C17 H17 124.5 . . ? N6 C18 N4 114.7(6) . . ? N6 C18 H18 122.6 . . ? N4 C18 H18 122.6 . . ? O2 C19 O1 119.9(5) . . ? O2 C19 C20 122.2(5) . . ? O1 C19 C20 117.9(5) . . ? C19 C20 C26 111.2(4) . . ? C19 C20 C21 110.5(4) . . ? C26 C20 C21 110.2(4) . . ? C19 C20 C25 108.6(4) . . ? C26 C20 C25 108.8(5) . . ? C21 C20 C25 107.3(4) . . ? C22 C21 C20 111.5(4) . . ? C22 C21 H21A 109.3 . . ? C20 C21 H21A 109.3 . . ? C22 C21 H21B 109.3 . . ? C20 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C23 C22 C21 109.5(4) . . ? C23 C22 C30 108.8(4) . . ? C21 C22 C30 112.3(5) . . ? C23 C22 C28 108.1(5) . . ? C21 C22 C28 108.7(4) . . ? C30 C22 C28 109.3(4) . . ? C22 C23 C24 109.7(4) . . ? C22 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? C22 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? C25 C24 C29 109.2(4) . . ? C25 C24 C23 110.4(5) . . ? C29 C24 C23 109.4(5) . . ? C25 C24 H24 109.3 . . ? C29 C24 H24 109.3 . . ? C23 C24 H24 109.3 . . ? C24 C25 C20 109.9(4) . . ? C24 C25 H25A 109.7 . . ? C20 C25 H25A 109.7 . . ? C24 C25 H25B 109.7 . . ? C20 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C20 C26 C27 110.4(4) . . ? C20 C26 H26A 109.6 . . ? C27 C26 H26A 109.6 . . ? C20 C26 H26B 109.6 . . ? C27 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C29 C27 C28 108.8(4) . . ? C29 C27 C26 109.3(4) . . ? C28 C27 C26 109.4(4) . . ? C29 C27 H27 109.8 . . ? C28 C27 H27 109.8 . . ? C26 C27 H27 109.8 . . ? C27 C28 C22 109.6(4) . . ? C27 C28 H28A 109.8 . . ? C22 C28 H28A 109.8 . . ? C27 C28 H28B 109.8 . . ? C22 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? C27 C29 C24 110.3(5) . . ? C27 C29 H29A 109.6 . . ? C24 C29 H29A 109.6 . . ? C27 C29 H29B 109.6 . . ? C24 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? O3 C30 O4 121.3(6) . . ? O3 C30 C22 120.6(5) . . ? O4 C30 C22 118.1(6) . . ? C2 N1 C1 106.4(5) . . ? C2 N1 Zn1 128.4(4) . . ? C1 N1 Zn1 125.1(5) . . ? N3 N2 C1 106.4(5) . . ? C2 N3 N2 109.3(5) . . ? C2 N3 C3 128.0(5) . . ? N2 N3 C3 122.6(5) . . ? C17 N4 C18 101.5(5) . . ? C17 N4 Zn1 128.8(4) . 3_756 ? C18 N4 Zn1 129.1(5) . 3_756 ? C17 N5 N6 109.7(5) . . ? C17 N5 C16 128.2(6) . . ? N6 N5 C16 121.5(5) . . ? C18 N6 N5 103.1(5) . . ? C19 O1 Zn1 107.3(4) . . ? C30 O4 Zn1 113.8(5) . 1_554 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C3 C4 C9 145.8(6) . . . . ? N3 C3 C4 C5 -37.0(9) . . . . ? C9 C4 C5 C6 0.2(11) . . . . ? C3 C4 C5 C6 -176.9(6) . . . . ? C4 C5 C6 C7 1.6(12) . . . . ? C5 C6 C7 C8 -2.0(10) . . . . ? C5 C6 C7 C10 179.4(6) . . . . ? C6 C7 C8 C9 0.8(11) . . . . ? C10 C7 C8 C9 179.4(7) . . . . ? C5 C4 C9 C8 -1.4(11) . . . . ? C3 C4 C9 C8 175.8(7) . . . . ? C7 C8 C9 C4 0.9(12) . . . . ? C6 C7 C10 C11 16.3(10) . . . . ? C8 C7 C10 C11 -162.2(7) . . . . ? C6 C7 C10 C15 -165.5(7) . . . . ? C8 C7 C10 C15 16.1(10) . . . . ? C15 C10 C11 C12 1.6(12) . . . . ? C7 C10 C11 C12 179.9(7) . . . . ? C10 C11 C12 C13 -1.6(14) . . . . ? C11 C12 C13 C14 -0.5(12) . . . . ? C11 C12 C13 C16 -178.7(8) . . . . ? C12 C13 C14 C15 2.4(11) . . . . ? C16 C13 C14 C15 -179.4(7) . . . . ? C11 C10 C15 C14 0.3(11) . . . . ? C7 C10 C15 C14 -178.0(6) . . . . ? C13 C14 C15 C10 -2.4(12) . . . . ? C12 C13 C16 N5 66.2(9) . . . . ? C14 C13 C16 N5 -111.9(7) . . . . ? O2 C19 C20 C26 -137.0(5) . . . . ? O1 C19 C20 C26 44.5(6) . . . . ? O2 C19 C20 C21 -14.2(7) . . . . ? O1 C19 C20 C21 167.3(4) . . . . ? O2 C19 C20 C25 103.3(6) . . . . ? O1 C19 C20 C25 -75.2(5) . . . . ? C19 C20 C21 C22 178.0(4) . . . . ? C26 C20 C21 C22 -58.6(5) . . . . ? C25 C20 C21 C22 59.7(5) . . . . ? C20 C21 C22 C23 -60.5(5) . . . . ? C20 C21 C22 C30 178.6(4) . . . . ? C20 C21 C22 C28 57.5(5) . . . . ? C21 C22 C23 C24 58.3(6) . . . . ? C30 C22 C23 C24 -178.6(5) . . . . ? C28 C22 C23 C24 -60.0(5) . . . . ? C22 C23 C24 C25 -59.1(6) . . . . ? C22 C23 C24 C29 61.1(6) . . . . ? C29 C24 C25 C20 -60.4(6) . . . . ? C23 C24 C25 C20 59.8(6) . . . . ? C19 C20 C25 C24 -178.6(5) . . . . ? C26 C20 C25 C24 60.2(5) . . . . ? C21 C20 C25 C24 -59.1(6) . . . . ? C19 C20 C26 C27 -178.5(4) . . . . ? C21 C20 C26 C27 58.5(6) . . . . ? C25 C20 C26 C27 -58.9(5) . . . . ? C20 C26 C27 C29 58.8(6) . . . . ? C20 C26 C27 C28 -60.2(6) . . . . ? C29 C27 C28 C22 -59.9(6) . . . . ? C26 C27 C28 C22 59.5(5) . . . . ? C23 C22 C28 C27 60.3(5) . . . . ? C21 C22 C28 C27 -58.5(6) . . . . ? C30 C22 C28 C27 178.6(5) . . . . ? C28 C27 C29 C24 60.6(6) . . . . ? C26 C27 C29 C24 -58.9(6) . . . . ? C25 C24 C29 C27 60.3(6) . . . . ? C23 C24 C29 C27 -60.6(6) . . . . ? C23 C22 C30 O3 -118.6(7) . . . . ? C21 C22 C30 O3 2.9(9) . . . . ? C28 C22 C30 O3 123.6(7) . . . . ? C23 C22 C30 O4 59.6(7) . . . . ? C21 C22 C30 O4 -179.0(5) . . . . ? C28 C22 C30 O4 -58.3(7) . . . . ? N3 C2 N1 C1 -0.4(6) . . . . ? N3 C2 N1 Zn1 -178.5(3) . . . . ? N2 C1 N1 C2 0.2(7) . . . . ? N2 C1 N1 Zn1 178.3(4) . . . . ? O4 Zn1 N1 C2 -17.7(5) 1_556 . . . ? O1 Zn1 N1 C2 88.6(5) . . . . ? N4 Zn1 N1 C2 -139.5(4) 3_756 . . . ? O4 Zn1 N1 C1 164.6(5) 1_556 . . . ? O1 Zn1 N1 C1 -89.1(5) . . . . ? N4 Zn1 N1 C1 42.7(5) 3_756 . . . ? N1 C1 N2 N3 0.1(7) . . . . ? N1 C2 N3 N2 0.5(6) . . . . ? N1 C2 N3 C3 175.7(5) . . . . ? C1 N2 N3 C2 -0.4(7) . . . . ? C1 N2 N3 C3 -175.9(5) . . . . ? C4 C3 N3 C2 114.3(6) . . . . ? C4 C3 N3 N2 -71.0(7) . . . . ? N5 C17 N4 C18 0.6(7) . . . . ? N5 C17 N4 Zn1 -171.4(4) . . . 3_756 ? N6 C18 N4 C17 -1.8(8) . . . . ? N6 C18 N4 Zn1 170.1(5) . . . 3_756 ? N4 C17 N5 N6 0.8(7) . . . . ? N4 C17 N5 C16 171.6(5) . . . . ? C13 C16 N5 C17 -108.2(7) . . . . ? C13 C16 N5 N6 61.7(8) . . . . ? N4 C18 N6 N5 2.3(9) . . . . ? C17 N5 N6 C18 -1.8(8) . . . . ? C16 N5 N6 C18 -173.3(6) . . . . ? O2 C19 O1 Zn1 -0.7(6) . . . . ? C20 C19 O1 Zn1 177.8(4) . . . . ? O4 Zn1 O1 C19 -174.1(3) 1_556 . . . ? N4 Zn1 O1 C19 -57.2(4) 3_756 . . . ? N1 Zn1 O1 C19 70.2(3) . . . . ? O3 C30 O4 Zn1 6.9(9) . . . 1_554 ? C22 C30 O4 Zn1 -171.2(4) . . . 1_554 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 -0.020 241.5 43.1 2 0.000 0.000 -0.039 241.5 43.2 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.937 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.123 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 802234' #TrackingRef '- cifs 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H62 Co2 N12 O9' _chemical_formula_sum 'C60 H62 Co2 N12 O9' _chemical_formula_weight 1213.08 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.042(2) _cell_length_b 19.550(2) _cell_length_c 17.324(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.211(2) _cell_angle_gamma 90.00 _cell_volume 5482.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1649 _cell_measurement_theta_min 2.4165 _cell_measurement_theta_max 21.1545 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 0.677 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7976 _exptl_absorpt_correction_T_max 0.9232 _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 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13687 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4870 _reflns_number_gt 3109 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.7764P] 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 4870 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1264 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Co1 Co 0.79967(3) 0.35186(3) 0.92662(3) 0.0396(2) Uani 1 1 d . . . C1 C 0.8574(3) 0.4480(4) 0.8233(4) 0.125(3) Uani 1 1 d . . . H1 H 0.8033 0.4576 0.7840 0.150 Uiso 1 1 calc R . . C2 C 0.9572(3) 0.4137(2) 0.9314(3) 0.0571(12) Uani 1 1 d . . . H2 H 0.9900 0.3920 0.9832 0.069 Uiso 1 1 calc R . . C3 C 1.0726(3) 0.4636(2) 0.9043(3) 0.0608(12) Uani 1 1 d . . . H3A H 1.0955 0.4985 0.9484 0.073 Uiso 1 1 calc R . . H3B H 1.0733 0.4813 0.8522 0.073 Uiso 1 1 calc R . . C4 C 1.1255(2) 0.4006(2) 0.9328(3) 0.0503(11) Uani 1 1 d . . . C5 C 1.1839(3) 0.3918(2) 1.0166(3) 0.0627(13) Uani 1 1 d . . . H5 H 1.1913 0.4260 1.0566 0.075 Uiso 1 1 calc R . . C6 C 1.2315(3) 0.3336(2) 1.0424(3) 0.0630(13) Uani 1 1 d . . . H6 H 1.2701 0.3295 1.0997 0.076 Uiso 1 1 calc R . . C7 C 1.2240(2) 0.2812(2) 0.9863(2) 0.0460(10) Uani 1 1 d . . . C8 C 1.1650(3) 0.2901(2) 0.9020(3) 0.0650(13) Uani 1 1 d . . . H8 H 1.1574 0.2559 0.8619 0.078 Uiso 1 1 calc R . . C9 C 1.1175(3) 0.3481(2) 0.8765(3) 0.0673(14) Uani 1 1 d . . . H9 H 1.0786 0.3522 0.8194 0.081 Uiso 1 1 calc R . . C10 C 0.7355(2) 0.4458(2) 1.0296(3) 0.0463(10) Uani 1 1 d . . . H10 H 0.7186 0.4807 0.9889 0.056 Uiso 1 1 calc R . . C11 C 0.7830(2) 0.35230(19) 1.0905(2) 0.0405(9) Uani 1 1 d . . . H11 H 0.8057 0.3087 1.1036 0.049 Uiso 1 1 calc R . . C12 C 0.7691(2) 0.3710(2) 1.2255(2) 0.0508(11) Uani 1 1 d . . . H12A H 0.8063 0.4033 1.2670 0.061 Uiso 1 1 calc R . . H12B H 0.7940 0.3260 1.2408 0.061 Uiso 1 1 calc R . . C13 C 0.6881(2) 0.3708(2) 1.2315(2) 0.0443(10) Uani 1 1 d . . . C14 C 0.6637(2) 0.4266(2) 1.2636(2) 0.0440(10) Uani 1 1 d . . . H14 H 0.6968 0.4655 1.2801 0.053 Uiso 1 1 calc R . . C15 C 0.5909(2) 0.42554(18) 1.2713(2) 0.0411(9) Uani 1 1 d . . . H15 H 0.5761 0.4636 1.2936 0.049 Uiso 1 1 calc R . . C16 C 0.5391(2) 0.36871(17) 1.2466(2) 0.0357(9) Uani 1 1 d . . . C17 C 0.5640(2) 0.31255(18) 1.2131(2) 0.0403(9) Uani 1 1 d . . . H17 H 0.5307 0.2739 1.1957 0.048 Uiso 1 1 calc R . . C18 C 0.6370(2) 0.3137(2) 1.2056(2) 0.0459(10) Uani 1 1 d . . . H18 H 0.6521 0.2760 1.1830 0.055 Uiso 1 1 calc R . . C19 C 0.6762(2) 0.35338(19) 0.7836(2) 0.0381(9) Uani 1 1 d . . . C20 C 0.6126(2) 0.34961(17) 0.6898(2) 0.0349(9) Uani 1 1 d . . . C21 C 0.5580(2) 0.28583(18) 0.6708(2) 0.0365(9) Uani 1 1 d . . . H21A H 0.5289 0.2863 0.7063 0.044 Uiso 1 1 calc R . . H21B H 0.5925 0.2452 0.6852 0.044 Uiso 1 1 calc R . . C22 C 0.4952(2) 0.28317(17) 0.5754(2) 0.0344(9) Uani 1 1 d . . . C23 C 0.4426(2) 0.34779(18) 0.5522(3) 0.0485(11) Uani 1 1 d . . . H23A H 0.4121 0.3504 0.5864 0.058 Uiso 1 1 calc R . . H23B H 0.4030 0.3464 0.4920 0.058 Uiso 1 1 calc R . . C24 C 0.4977(3) 0.4106(2) 0.5692(3) 0.0605(13) Uani 1 1 d . . . H24 H 0.4631 0.4517 0.5538 0.073 Uiso 1 1 calc R . . C25 C 0.5585(2) 0.41381(19) 0.6653(3) 0.0516(11) Uani 1 1 d . . . H25A H 0.5929 0.4542 0.6766 0.062 Uiso 1 1 calc R . . H25B H 0.5282 0.4166 0.6996 0.062 Uiso 1 1 calc R . . C26 C 0.6597(2) 0.3467(2) 0.6345(2) 0.0475(10) Uani 1 1 d . . . H26A H 0.6947 0.3868 0.6457 0.057 Uiso 1 1 calc R . . H26B H 0.6947 0.3065 0.6495 0.057 Uiso 1 1 calc R . . C27 C 0.5450(2) 0.28055(19) 0.5222(2) 0.0418(9) Uani 1 1 d . . . H27A H 0.5796 0.2401 0.5376 0.050 Uiso 1 1 calc R . . H27B H 0.5073 0.2778 0.4614 0.050 Uiso 1 1 calc R . . C28 C 0.5452(3) 0.4084(2) 0.5163(3) 0.0704(15) Uani 1 1 d . . . H28A H 0.5798 0.4487 0.5278 0.084 Uiso 1 1 calc R . . H28B H 0.5071 0.4079 0.4556 0.084 Uiso 1 1 calc R . . C29 C 0.5987(3) 0.3442(2) 0.5393(3) 0.0525(11) Uani 1 1 d . . . H29 H 0.6292 0.3424 0.5045 0.063 Uiso 1 1 calc R . . C30 C 0.4426(2) 0.2190(2) 0.5525(2) 0.0427(10) Uani 1 1 d . . . N1 N 0.8768(2) 0.41166(17) 0.8947(2) 0.0504(9) Uani 1 1 d . . . N2 N 0.9870(2) 0.44942(18) 0.8878(2) 0.0529(9) Uani 1 1 d . . . N3 N 0.9221(3) 0.4690(3) 0.8140(4) 0.127(2) Uani 1 1 d . . . N4 N 0.76862(17) 0.38628(16) 1.01913(19) 0.0386(8) Uani 1 1 d . . . N5 N 0.76063(17) 0.38889(16) 1.14020(19) 0.0398(8) Uani 1 1 d . . . N6 N 0.7293(2) 0.44978(17) 1.1020(2) 0.0537(9) Uani 1 1 d . . . O1 O 0.71775(15) 0.30046(13) 0.82061(16) 0.0509(7) Uani 1 1 d . . . O2 O 0.69224(16) 0.40855(13) 0.82390(16) 0.0490(7) Uani 1 1 d . . . O3 O 0.46718(18) 0.16513(14) 0.59251(18) 0.0603(8) Uani 1 1 d . . . O4 O 0.37299(16) 0.22425(14) 0.48517(17) 0.0569(8) Uani 1 1 d . . . O5 O 0.9678(4) 0.3923(3) 0.2396(6) 0.084(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 Co1 0.0337(3) 0.0483(3) 0.0307(3) -0.0009(2) 0.0087(2) 0.0028(2) C1 0.036(3) 0.206(7) 0.116(5) 0.104(5) 0.020(3) 0.001(4) C2 0.048(3) 0.067(3) 0.052(3) 0.011(2) 0.018(2) -0.003(2) C3 0.049(3) 0.067(3) 0.074(3) 0.002(2) 0.034(2) -0.013(2) C4 0.041(2) 0.061(3) 0.053(3) -0.009(2) 0.025(2) -0.013(2) C5 0.071(3) 0.064(3) 0.048(3) -0.014(2) 0.021(2) -0.010(3) C6 0.069(3) 0.072(3) 0.033(2) -0.010(2) 0.009(2) 0.003(3) C7 0.042(2) 0.061(3) 0.037(2) -0.011(2) 0.020(2) -0.0104(19) C8 0.055(3) 0.083(3) 0.044(3) -0.025(2) 0.011(2) 0.005(2) C9 0.053(3) 0.092(4) 0.041(3) -0.011(3) 0.006(2) 0.006(3) C10 0.055(3) 0.039(2) 0.048(3) 0.0137(19) 0.026(2) 0.0072(19) C11 0.039(2) 0.041(2) 0.042(2) 0.0038(19) 0.0176(18) 0.0051(17) C12 0.045(2) 0.071(3) 0.038(2) 0.009(2) 0.020(2) 0.009(2) C13 0.049(2) 0.054(3) 0.028(2) 0.0076(18) 0.0158(18) 0.010(2) C14 0.046(2) 0.045(2) 0.040(2) 0.0050(19) 0.0178(19) -0.0010(19) C15 0.049(2) 0.037(2) 0.041(2) 0.0000(18) 0.0234(19) 0.0053(18) C16 0.042(2) 0.041(2) 0.0271(19) 0.0025(16) 0.0173(17) 0.0029(16) C17 0.053(2) 0.037(2) 0.031(2) -0.0035(17) 0.0183(18) 0.0008(18) C18 0.058(3) 0.050(2) 0.033(2) -0.0010(19) 0.023(2) 0.011(2) C19 0.030(2) 0.046(2) 0.035(2) -0.0021(19) 0.0107(16) -0.0018(18) C20 0.0295(19) 0.041(2) 0.027(2) -0.0020(16) 0.0056(15) 0.0002(16) C21 0.035(2) 0.048(2) 0.0257(19) -0.0011(17) 0.0124(16) 0.0006(16) C22 0.0283(19) 0.042(2) 0.0252(19) -0.0008(16) 0.0047(15) -0.0032(16) C23 0.033(2) 0.053(2) 0.043(2) -0.0039(19) 0.0015(18) 0.0059(18) C24 0.057(3) 0.038(2) 0.053(3) 0.002(2) -0.005(2) 0.010(2) C25 0.043(2) 0.045(2) 0.046(3) -0.0106(19) 0.0015(19) 0.0052(18) C26 0.036(2) 0.058(3) 0.044(2) 0.007(2) 0.0136(18) -0.0058(19) C27 0.040(2) 0.055(2) 0.028(2) -0.0014(18) 0.0130(17) 0.0024(18) C28 0.076(3) 0.062(3) 0.043(3) 0.019(2) -0.002(2) -0.021(3) C29 0.049(3) 0.072(3) 0.038(2) 0.005(2) 0.020(2) -0.013(2) C30 0.044(2) 0.050(2) 0.032(2) -0.0062(19) 0.0150(19) -0.0068(19) N1 0.037(2) 0.069(2) 0.044(2) 0.0066(18) 0.0169(16) 0.0030(17) N2 0.043(2) 0.065(2) 0.051(2) 0.0087(18) 0.0208(18) 0.0002(18) N3 0.068(3) 0.181(6) 0.117(4) 0.069(4) 0.027(3) -0.005(3) N4 0.0320(17) 0.0447(19) 0.0379(19) 0.0016(15) 0.0143(14) -0.0022(14) N5 0.0387(18) 0.0443(19) 0.0398(19) 0.0044(16) 0.0205(15) 0.0067(15) N6 0.064(2) 0.049(2) 0.059(2) 0.0069(18) 0.0364(19) 0.0056(18) O1 0.0502(17) 0.0445(16) 0.0382(16) -0.0033(13) 0.0016(13) 0.0083(13) O2 0.0514(17) 0.0459(16) 0.0372(16) -0.0058(13) 0.0082(13) -0.0043(13) O3 0.065(2) 0.0500(17) 0.0457(18) 0.0043(14) 0.0059(15) -0.0133(15) O4 0.0489(17) 0.0609(18) 0.0415(17) -0.0012(14) 0.0023(14) -0.0138(14) O5 0.114(8) 0.072(4) 0.069(5) 0.013(4) 0.044(7) 0.036(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 Co1 O4 1.951(3) 8_556 ? Co1 N4 2.032(3) . ? Co1 O1 2.042(2) . ? Co1 N1 2.071(3) . ? Co1 O2 2.259(2) . ? C1 N3 1.312(6) . ? C1 N1 1.332(6) . ? C1 H1 0.9300 . ? C2 N1 1.303(5) . ? C2 N2 1.307(5) . ? C2 H2 0.9300 . ? C3 N2 1.469(5) . ? C3 C4 1.503(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.376(6) . ? C4 C9 1.377(6) . ? C5 C6 1.376(6) . ? C5 H5 0.9300 . ? C6 C7 1.377(5) . ? C6 H6 0.9300 . ? C7 C8 1.386(5) . ? C7 C7 1.485(8) 7_757 ? C8 C9 1.373(6) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 N6 1.309(5) . ? C10 N4 1.356(5) . ? C10 H10 0.9300 . ? C11 N5 1.312(4) . ? C11 N4 1.325(4) . ? C11 H11 0.9300 . ? C12 N5 1.459(5) . ? C12 C13 1.510(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.382(5) . ? C13 C18 1.390(5) . ? C14 C15 1.378(5) . ? C14 H14 0.9300 . ? C15 C16 1.393(5) . ? C15 H15 0.9300 . ? C16 C17 1.405(5) . ? C16 C16 1.466(7) 2_657 ? C17 C18 1.379(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 O2 1.247(4) . ? C19 O1 1.272(4) . ? C19 C20 1.522(5) . ? C20 C25 1.530(5) . ? C20 C21 1.531(5) . ? C20 C26 1.537(5) . ? C21 C22 1.537(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C30 1.517(5) . ? C22 C23 1.524(5) . ? C22 C27 1.547(5) . ? C23 C24 1.525(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C28 1.506(7) . ? C24 C25 1.538(5) . ? C24 H24 0.9800 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C29 1.527(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C29 1.524(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.524(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29 0.9800 . ? C30 O3 1.231(4) . ? C30 O4 1.286(4) . ? N2 N3 1.353(5) . ? N5 N6 1.358(4) . ? O4 Co1 1.951(3) 8_455 ? O5 O5 1.054(13) 2_755 ? 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 N4 101.67(12) 8_556 . ? O4 Co1 O1 98.48(11) 8_556 . ? N4 Co1 O1 122.02(12) . . ? O4 Co1 N1 100.85(13) 8_556 . ? N4 Co1 N1 118.40(13) . . ? O1 Co1 N1 110.02(12) . . ? O4 Co1 O2 158.79(11) 8_556 . ? N4 Co1 O2 91.11(11) . . ? O1 Co1 O2 60.31(9) . . ? N1 Co1 O2 87.50(12) . . ? N3 C1 N1 113.5(4) . . ? N3 C1 H1 123.3 . . ? N1 C1 H1 123.3 . . ? N1 C2 N2 112.8(4) . . ? N1 C2 H2 123.6 . . ? N2 C2 H2 123.6 . . ? N2 C3 C4 111.7(3) . . ? N2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C9 116.5(4) . . ? C5 C4 C3 121.9(4) . . ? C9 C4 C3 121.7(4) . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 122.1(4) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C6 C7 C8 116.2(4) . . ? C6 C7 C7 122.3(4) . 7_757 ? C8 C7 C7 121.5(4) . 7_757 ? C9 C8 C7 121.4(4) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C4 122.2(4) . . ? C8 C9 H9 118.9 . . ? C4 C9 H9 118.9 . . ? N6 C10 N4 114.1(3) . . ? N6 C10 H10 123.0 . . ? N4 C10 H10 123.0 . . ? N5 C11 N4 110.4(3) . . ? N5 C11 H11 124.8 . . ? N4 C11 H11 124.8 . . ? N5 C12 C13 113.5(3) . . ? N5 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N5 C12 H12B 108.9 . . ? C13 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C14 C13 C18 118.7(4) . . ? C14 C13 C12 121.1(4) . . ? C18 C13 C12 120.3(4) . . ? C15 C14 C13 120.9(4) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 121.4(4) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C17 117.2(3) . . ? C15 C16 C16 120.9(3) . 2_657 ? C17 C16 C16 121.9(3) . 2_657 ? C18 C17 C16 121.3(4) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C13 120.5(4) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? O2 C19 O1 118.8(3) . . ? O2 C19 C20 121.2(3) . . ? O1 C19 C20 119.8(3) . . ? C19 C20 C25 110.2(3) . . ? C19 C20 C21 112.3(3) . . ? C25 C20 C21 109.8(3) . . ? C19 C20 C26 107.6(3) . . ? C25 C20 C26 108.5(3) . . ? C21 C20 C26 108.4(3) . . ? C20 C21 C22 110.9(3) . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.0 . . ? C30 C22 C23 111.8(3) . . ? C30 C22 C21 112.9(3) . . ? C23 C22 C21 109.5(3) . . ? C30 C22 C27 106.1(3) . . ? C23 C22 C27 109.2(3) . . ? C21 C22 C27 107.2(3) . . ? C22 C23 C24 109.9(3) . . ? C22 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? C22 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? C28 C24 C23 110.9(4) . . ? C28 C24 C25 109.5(4) . . ? C23 C24 C25 109.5(4) . . ? C28 C24 H24 109.0 . . ? C23 C24 H24 109.0 . . ? C25 C24 H24 109.0 . . ? C20 C25 C24 109.2(3) . . ? C20 C25 H25A 109.8 . . ? C24 C25 H25A 109.8 . . ? C20 C25 H25B 109.8 . . ? C24 C25 H25B 109.8 . . ? H25A C25 H25B 108.3 . . ? C29 C26 C20 109.9(3) . . ? C29 C26 H26A 109.7 . . ? C20 C26 H26A 109.7 . . ? C29 C26 H26B 109.7 . . ? C20 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C29 C27 C22 110.1(3) . . ? C29 C27 H27A 109.6 . . ? C22 C27 H27A 109.6 . . ? C29 C27 H27B 109.6 . . ? C22 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? C24 C28 C29 109.3(3) . . ? C24 C28 H28A 109.8 . . ? C29 C28 H28A 109.8 . . ? C24 C28 H28B 109.8 . . ? C29 C28 H28B 109.8 . . ? H28A C28 H28B 108.3 . . ? C27 C29 C28 110.3(3) . . ? C27 C29 C26 109.2(3) . . ? C28 C29 C26 109.1(4) . . ? C27 C29 H29 109.4 . . ? C28 C29 H29 109.4 . . ? C26 C29 H29 109.4 . . ? O3 C30 O4 122.9(3) . . ? O3 C30 C22 122.1(3) . . ? O4 C30 C22 114.8(3) . . ? C2 N1 C1 102.5(4) . . ? C2 N1 Co1 128.4(3) . . ? C1 N1 Co1 128.2(3) . . ? C2 N2 N3 107.0(4) . . ? C2 N2 C3 130.9(4) . . ? N3 N2 C3 121.9(4) . . ? C1 N3 N2 103.9(4) . . ? C11 N4 C10 102.8(3) . . ? C11 N4 Co1 124.2(3) . . ? C10 N4 Co1 132.9(3) . . ? C11 N5 N6 109.9(3) . . ? C11 N5 C12 127.5(3) . . ? N6 N5 C12 122.6(3) . . ? C10 N6 N5 102.8(3) . . ? C19 O1 Co1 94.8(2) . . ? C19 O2 Co1 85.6(2) . . ? C30 O4 Co1 125.2(3) . 8_455 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C3 C4 C5 -107.5(5) . . . . ? N2 C3 C4 C9 72.0(5) . . . . ? C9 C4 C5 C6 -0.1(7) . . . . ? C3 C4 C5 C6 179.4(4) . . . . ? C4 C5 C6 C7 0.5(8) . . . . ? C5 C6 C7 C8 -0.6(7) . . . . ? C5 C6 C7 C7 179.2(5) . . . 7_757 ? C6 C7 C8 C9 0.4(7) . . . . ? C7 C7 C8 C9 -179.4(5) 7_757 . . . ? C7 C8 C9 C4 -0.1(8) . . . . ? C5 C4 C9 C8 -0.1(7) . . . . ? C3 C4 C9 C8 -179.5(4) . . . . ? N5 C12 C13 C14 -97.5(4) . . . . ? N5 C12 C13 C18 83.3(5) . . . . ? C18 C13 C14 C15 1.2(5) . . . . ? C12 C13 C14 C15 -178.1(3) . . . . ? C13 C14 C15 C16 -0.6(6) . . . . ? C14 C15 C16 C17 -0.1(5) . . . . ? C14 C15 C16 C16 -178.7(4) . . . 2_657 ? C15 C16 C17 C18 0.3(5) . . . . ? C16 C16 C17 C18 178.8(4) 2_657 . . . ? C16 C17 C18 C13 0.3(6) . . . . ? C14 C13 C18 C17 -1.0(5) . . . . ? C12 C13 C18 C17 178.2(3) . . . . ? O2 C19 C20 C25 -16.2(5) . . . . ? O1 C19 C20 C25 168.1(4) . . . . ? O2 C19 C20 C21 -138.8(4) . . . . ? O1 C19 C20 C21 45.4(5) . . . . ? O2 C19 C20 C26 101.9(4) . . . . ? O1 C19 C20 C26 -73.8(4) . . . . ? C19 C20 C21 C22 -179.3(3) . . . . ? C25 C20 C21 C22 57.8(4) . . . . ? C26 C20 C21 C22 -60.6(4) . . . . ? C20 C21 C22 C30 177.1(3) . . . . ? C20 C21 C22 C23 -57.7(4) . . . . ? C20 C21 C22 C27 60.6(4) . . . . ? C30 C22 C23 C24 -175.1(3) . . . . ? C21 C22 C23 C24 59.1(4) . . . . ? C27 C22 C23 C24 -58.0(4) . . . . ? C22 C23 C24 C28 59.9(4) . . . . ? C22 C23 C24 C25 -61.1(5) . . . . ? C19 C20 C25 C24 177.1(3) . . . . ? C21 C20 C25 C24 -58.8(5) . . . . ? C26 C20 C25 C24 59.5(4) . . . . ? C28 C24 C25 C20 -61.2(4) . . . . ? C23 C24 C25 C20 60.7(5) . . . . ? C19 C20 C26 C29 -178.9(3) . . . . ? C25 C20 C26 C29 -59.8(4) . . . . ? C21 C20 C26 C29 59.4(4) . . . . ? C30 C22 C27 C29 178.6(3) . . . . ? C23 C22 C27 C29 58.0(4) . . . . ? C21 C22 C27 C29 -60.5(4) . . . . ? C23 C24 C28 C29 -59.6(4) . . . . ? C25 C24 C28 C29 61.4(4) . . . . ? C22 C27 C29 C28 -58.6(4) . . . . ? C22 C27 C29 C26 61.2(4) . . . . ? C24 C28 C29 C27 59.0(4) . . . . ? C24 C28 C29 C26 -60.9(4) . . . . ? C20 C26 C29 C27 -60.3(4) . . . . ? C20 C26 C29 C28 60.3(4) . . . . ? C23 C22 C30 O3 -151.1(4) . . . . ? C21 C22 C30 O3 -27.2(5) . . . . ? C27 C22 C30 O3 89.9(4) . . . . ? C23 C22 C30 O4 33.1(5) . . . . ? C21 C22 C30 O4 157.1(3) . . . . ? C27 C22 C30 O4 -85.8(4) . . . . ? N2 C2 N1 C1 0.9(6) . . . . ? N2 C2 N1 Co1 170.4(3) . . . . ? N3 C1 N1 C2 2.8(8) . . . . ? N3 C1 N1 Co1 -166.7(5) . . . . ? O4 Co1 N1 C2 -24.4(4) 8_556 . . . ? N4 Co1 N1 C2 85.4(4) . . . . ? O1 Co1 N1 C2 -127.6(4) . . . . ? O2 Co1 N1 C2 175.3(4) . . . . ? O4 Co1 N1 C1 142.5(5) 8_556 . . . ? N4 Co1 N1 C1 -107.8(5) . . . . ? O1 Co1 N1 C1 39.2(5) . . . . ? O2 Co1 N1 C1 -17.8(5) . . . . ? N1 C2 N2 N3 -4.1(6) . . . . ? N1 C2 N2 C3 -178.5(4) . . . . ? C4 C3 N2 C2 43.8(6) . . . . ? C4 C3 N2 N3 -130.0(5) . . . . ? N1 C1 N3 N2 -5.2(9) . . . . ? C2 N2 N3 C1 5.4(7) . . . . ? C3 N2 N3 C1 -179.6(5) . . . . ? N5 C11 N4 C10 -0.4(4) . . . . ? N5 C11 N4 Co1 176.3(2) . . . . ? N6 C10 N4 C11 0.2(4) . . . . ? N6 C10 N4 Co1 -176.0(3) . . . . ? O4 Co1 N4 C11 -13.0(3) 8_556 . . . ? O1 Co1 N4 C11 94.9(3) . . . . ? N1 Co1 N4 C11 -122.2(3) . . . . ? O2 Co1 N4 C11 150.0(3) . . . . ? O4 Co1 N4 C10 162.6(3) 8_556 . . . ? O1 Co1 N4 C10 -89.5(3) . . . . ? N1 Co1 N4 C10 53.4(4) . . . . ? O2 Co1 N4 C10 -34.4(3) . . . . ? N4 C11 N5 N6 0.5(4) . . . . ? N4 C11 N5 C12 -177.5(3) . . . . ? C13 C12 N5 C11 -122.3(4) . . . . ? C13 C12 N5 N6 60.0(5) . . . . ? N4 C10 N6 N5 0.0(4) . . . . ? C11 N5 N6 C10 -0.3(4) . . . . ? C12 N5 N6 C10 177.8(3) . . . . ? O2 C19 O1 Co1 -7.2(4) . . . . ? C20 C19 O1 Co1 168.6(3) . . . . ? O4 Co1 O1 C19 -175.7(2) 8_556 . . . ? N4 Co1 O1 C19 74.7(3) . . . . ? N1 Co1 O1 C19 -70.8(3) . . . . ? O2 Co1 O1 C19 4.0(2) . . . . ? O1 C19 O2 Co1 6.5(4) . . . . ? C20 C19 O2 Co1 -169.2(3) . . . . ? O4 Co1 O2 C19 -3.4(5) 8_556 . . . ? N4 Co1 O2 C19 -130.9(2) . . . . ? O1 Co1 O2 C19 -4.1(2) . . . . ? N1 Co1 O2 C19 110.7(2) . . . . ? O3 C30 O4 Co1 -6.9(6) . . . 8_455 ? C22 C30 O4 Co1 168.8(2) . . . 8_455 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.404 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.068 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 802235' #TrackingRef '- cifs 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H34 Cd N6 O6' _chemical_formula_sum 'C30 H34 Cd N6 O6' _chemical_formula_weight 687.03 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2524(13) _cell_length_b 10.5382(13) _cell_length_c 16.458(2) _cell_angle_alpha 72.288(2) _cell_angle_beta 84.972(2) _cell_angle_gamma 61.580(2) _cell_volume 1486.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1777 _cell_measurement_theta_min 2.344 _cell_measurement_theta_max 20.8275 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7699 _exptl_absorpt_correction_T_max 0.8519 _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 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7506 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5203 _reflns_number_gt 3884 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+0.4643P] 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 5203 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1459 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 0.60176(4) 0.73327(4) 0.92149(2) 0.04153(17) Uani 1 1 d . . . C1 C 0.6005(7) 0.5889(7) 1.1282(4) 0.0548(16) Uani 1 1 d . . . H1 H 0.5947 0.5093 1.1185 0.066 Uiso 1 1 calc R . . C2 C 0.6185(6) 0.7873(6) 1.1050(3) 0.0426(13) Uani 1 1 d . . . H2 H 0.6268 0.8746 1.0789 0.051 Uiso 1 1 calc R . . C3 C 0.6035(7) 0.8030(7) 1.2541(4) 0.0533(15) Uani 1 1 d . . . H3A H 0.5086 0.8279 1.2794 0.064 Uiso 1 1 calc R . . H3B H 0.6065 0.8971 1.2267 0.064 Uiso 1 1 calc R . . C4 C 0.7256(6) 0.7074(6) 1.3244(3) 0.0454(14) Uani 1 1 d . . . C5 C 0.8589(7) 0.5849(7) 1.3200(4) 0.0600(17) Uani 1 1 d . . . H5 H 0.8769 0.5553 1.2706 0.072 Uiso 1 1 calc R . . C6 C 0.9666(7) 0.5046(7) 1.3873(4) 0.0568(16) Uani 1 1 d . . . H6 H 1.0561 0.4235 1.3820 0.068 Uiso 1 1 calc R . . C7 C 0.9423(6) 0.5444(7) 1.4633(3) 0.0469(14) Uani 1 1 d . . . C8 C 0.8127(7) 0.6722(8) 1.4641(4) 0.080(2) Uani 1 1 d . . . H8 H 0.7958 0.7067 1.5117 0.096 Uiso 1 1 calc R . . C9 C 0.7070(7) 0.7508(8) 1.3966(4) 0.078(2) Uani 1 1 d . . . H9 H 0.6202 0.8360 1.4002 0.094 Uiso 1 1 calc R . . C10 C 0.5818(8) 0.6410(8) 0.7505(4) 0.0669(19) Uani 1 1 d . . . H10 H 0.5555 0.5693 0.7842 0.080 Uiso 1 1 calc R . . C11 C 0.6495(8) 0.8026(9) 0.7092(4) 0.072(2) Uani 1 1 d . . . H11 H 0.6825 0.8708 0.7096 0.086 Uiso 1 1 calc R . . C12 C 0.5323(8) 0.6216(9) 0.6091(5) 0.074(2) Uani 1 1 d . . . H12A H 0.5358 0.5255 0.6401 0.088 Uiso 1 1 calc R . . H12B H 0.5977 0.6066 0.5627 0.088 Uiso 1 1 calc R . . C13 C 0.3739(10) 0.7374(9) 0.5729(6) 0.0981(12) Uani 1 1 d . . . C14 C 0.3331(10) 0.8809(9) 0.5238(6) 0.0981(12) Uani 1 1 d . . . H14 H 0.4051 0.9121 0.5083 0.118 Uiso 1 1 calc R . . C15 C 0.1874(10) 0.9810(10) 0.4967(6) 0.0981(12) Uani 1 1 d . . . H15 H 0.1638 1.0794 0.4643 0.118 Uiso 1 1 calc R . . C16 C 0.0783(9) 0.9454(9) 0.5139(6) 0.0981(12) Uani 1 1 d . . . C17 C 0.1190(10) 0.8015(9) 0.5617(6) 0.0981(12) Uani 1 1 d . . . H17 H 0.0463 0.7714 0.5775 0.118 Uiso 1 1 calc R . . C18 C 0.2688(9) 0.6958(10) 0.5883(6) 0.0981(12) Uani 1 1 d . . . H18 H 0.2942 0.5954 0.6170 0.118 Uiso 1 1 calc R . . C19 C 0.2958(6) 0.8496(6) 0.8894(3) 0.0398(13) Uani 1 1 d . . . C20 C 0.1343(5) 0.9365(6) 0.8524(3) 0.0369(12) Uani 1 1 d . . . C21 C 0.1390(6) 0.9585(7) 0.7553(3) 0.0513(15) Uani 1 1 d . . . H21A H 0.1944 1.0126 0.7303 0.062 Uiso 1 1 calc R . . H21B H 0.1890 0.8607 0.7451 0.062 Uiso 1 1 calc R . . C22 C -0.0188(7) 1.0476(9) 0.7137(4) 0.065(2) Uani 1 1 d . . . H22 H -0.0152 1.0605 0.6522 0.078 Uiso 1 1 calc R . . C23 C -0.1045(6) 0.9615(7) 0.7529(3) 0.0508(15) Uani 1 1 d . . . H23A H -0.0556 0.8633 0.7433 0.061 Uiso 1 1 calc R . . H23B H -0.2042 1.0167 0.7257 0.061 Uiso 1 1 calc R . . C24 C -0.1125(6) 0.9409(6) 0.8495(3) 0.0407(13) Uani 1 1 d . . . C25 C 0.0470(5) 0.8520(6) 0.8905(3) 0.0350(12) Uani 1 1 d . . . H25A H 0.0446 0.8367 0.9516 0.042 Uiso 1 1 calc R . . H25B H 0.0960 0.7535 0.8811 0.042 Uiso 1 1 calc R . . C26 C 0.0554(6) 1.0959(6) 0.8653(4) 0.0484(14) Uani 1 1 d . . . H26A H 0.0544 1.0856 0.9260 0.058 Uiso 1 1 calc R . . H26B H 0.1099 1.1503 0.8391 0.058 Uiso 1 1 calc R . . C27 C -0.1038(6) 1.1849(7) 0.8254(5) 0.0612(18) Uani 1 1 d . . . H27 H -0.1535 1.2839 0.8355 0.073 Uiso 1 1 calc R . . C28 C -0.0972(7) 1.2054(7) 0.7288(4) 0.067(2) Uani 1 1 d . . . H28A H -0.0427 1.2604 0.7038 0.081 Uiso 1 1 calc R . . H28B H -0.1970 1.2633 0.7015 0.081 Uiso 1 1 calc R . . C29 C -0.1892(6) 1.0966(6) 0.8648(4) 0.0529(16) Uani 1 1 d . . . H29A H -0.2903 1.1533 0.8393 0.064 Uiso 1 1 calc R . . H29B H -0.1934 1.0837 0.9257 0.064 Uiso 1 1 calc R . . C30 C -0.2035(6) 0.8586(7) 0.8829(4) 0.0447(14) Uani 1 1 d . . . N1 N 0.6118(5) 0.6987(5) 1.0652(3) 0.0441(11) Uani 1 1 d . . . N2 N 0.5985(6) 0.6035(6) 1.2038(3) 0.0623(15) Uani 1 1 d . . . N3 N 0.6117(5) 0.7316(5) 1.1886(3) 0.0438(11) Uani 1 1 d . . . N4 N 0.6203(6) 0.7191(6) 0.7806(3) 0.0557(13) Uani 1 1 d . . . N5 N 0.6275(8) 0.7794(8) 0.6388(4) 0.0830(19) Uani 1 1 d . . . N6 N 0.5840(6) 0.6742(6) 0.6674(3) 0.0604(14) Uani 1 1 d . . . O1 O 0.3584(4) 0.7104(4) 0.9209(3) 0.0518(10) Uani 1 1 d . . . O2 O 0.3638(4) 0.9248(5) 0.8845(3) 0.0584(11) Uani 1 1 d . . . O3 O -0.1396(4) 0.7179(5) 0.9195(3) 0.0627(12) Uani 1 1 d . . . O4 O -0.3396(4) 0.9305(5) 0.8717(3) 0.0706(13) Uani 1 1 d . . . O5 O 0.7107(5) 0.4762(5) 0.9462(3) 0.0628(12) Uani 1 1 d . . . O6 O 0.9993(5) 0.5789(5) 0.0899(3) 0.0838(15) Uani 1 1 d . . . H5A H 0.7015 0.4108 0.9874 0.101 Uiso 1 1 d R . . H5B H 0.8014 0.4522 0.9440 0.101 Uiso 1 1 d R . . H6A H 0.9573 0.5994 0.0421 0.101 Uiso 1 1 d R . . H6B H 1.0183 0.4868 0.1156 0.101 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 Cd1 0.0359(2) 0.0443(3) 0.0432(3) -0.00810(18) -0.00380(17) -0.0199(2) C1 0.079(4) 0.049(4) 0.049(4) -0.006(3) -0.006(3) -0.044(4) C2 0.035(3) 0.041(3) 0.048(3) -0.003(3) -0.005(2) -0.021(3) C3 0.061(4) 0.048(4) 0.048(3) -0.013(3) -0.011(3) -0.022(3) C4 0.050(3) 0.049(4) 0.037(3) -0.008(3) -0.007(3) -0.024(3) C5 0.070(4) 0.055(4) 0.042(3) -0.016(3) -0.015(3) -0.015(4) C6 0.054(4) 0.052(4) 0.053(4) -0.008(3) -0.014(3) -0.018(3) C7 0.045(3) 0.057(4) 0.037(3) -0.004(3) -0.007(2) -0.028(3) C8 0.058(4) 0.089(5) 0.046(4) -0.029(4) -0.015(3) 0.010(4) C9 0.053(4) 0.083(5) 0.056(4) -0.029(4) -0.013(3) 0.009(4) C10 0.083(5) 0.074(5) 0.051(4) -0.003(3) -0.006(3) -0.050(4) C11 0.094(5) 0.099(6) 0.057(4) -0.030(4) 0.018(4) -0.071(5) C12 0.083(5) 0.080(5) 0.072(5) -0.037(4) 0.002(4) -0.041(4) C13 0.093(3) 0.077(2) 0.121(3) 0.007(2) -0.025(2) -0.054(2) C14 0.093(3) 0.077(2) 0.121(3) 0.007(2) -0.025(2) -0.054(2) C15 0.093(3) 0.077(2) 0.121(3) 0.007(2) -0.025(2) -0.054(2) C16 0.093(3) 0.077(2) 0.121(3) 0.007(2) -0.025(2) -0.054(2) C17 0.093(3) 0.077(2) 0.121(3) 0.007(2) -0.025(2) -0.054(2) C18 0.093(3) 0.077(2) 0.121(3) 0.007(2) -0.025(2) -0.054(2) C19 0.037(3) 0.047(4) 0.041(3) -0.016(3) 0.005(2) -0.022(3) C20 0.030(3) 0.042(3) 0.042(3) -0.013(2) -0.001(2) -0.020(2) C21 0.047(3) 0.073(4) 0.047(3) -0.019(3) 0.008(3) -0.038(3) C22 0.062(4) 0.111(6) 0.032(3) -0.004(3) -0.003(3) -0.059(4) C23 0.045(3) 0.069(4) 0.047(3) -0.012(3) -0.006(3) -0.036(3) C24 0.035(3) 0.038(3) 0.046(3) -0.004(2) -0.006(2) -0.018(3) C25 0.027(3) 0.036(3) 0.040(3) -0.008(2) -0.006(2) -0.013(2) C26 0.040(3) 0.048(4) 0.062(4) -0.016(3) -0.005(3) -0.023(3) C27 0.041(3) 0.040(4) 0.101(5) -0.017(3) -0.006(3) -0.018(3) C28 0.056(4) 0.059(4) 0.075(5) 0.014(4) -0.026(3) -0.033(4) C29 0.028(3) 0.046(4) 0.075(4) -0.017(3) -0.005(3) -0.010(3) C30 0.037(3) 0.048(4) 0.051(3) -0.013(3) -0.001(3) -0.022(3) N1 0.047(3) 0.049(3) 0.041(3) -0.008(2) -0.007(2) -0.028(2) N2 0.095(4) 0.055(3) 0.045(3) -0.005(2) -0.011(3) -0.045(3) N3 0.046(3) 0.046(3) 0.035(3) -0.005(2) -0.012(2) -0.020(2) N4 0.063(3) 0.067(4) 0.050(3) -0.017(3) -0.001(3) -0.040(3) N5 0.118(5) 0.110(5) 0.059(4) -0.032(4) 0.020(4) -0.082(5) N6 0.071(4) 0.069(4) 0.054(3) -0.025(3) 0.010(3) -0.041(3) O1 0.037(2) 0.038(2) 0.074(3) -0.007(2) -0.0103(19) -0.0158(19) O2 0.040(2) 0.054(3) 0.084(3) -0.009(2) -0.013(2) -0.029(2) O3 0.045(2) 0.057(3) 0.085(3) -0.007(2) -0.004(2) -0.030(2) O4 0.037(2) 0.057(3) 0.109(4) -0.005(3) -0.005(2) -0.026(2) O5 0.055(3) 0.051(3) 0.071(3) -0.010(2) 0.001(2) -0.020(2) O6 0.069(3) 0.073(3) 0.099(4) -0.032(3) -0.002(3) -0.020(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 Cd1 N1 2.284(4) . ? Cd1 O2 2.285(4) . ? Cd1 O5 2.298(4) . ? Cd1 O4 2.328(4) 1_655 ? Cd1 N4 2.353(5) . ? Cd1 O3 2.576(4) 1_655 ? Cd1 O1 2.620(4) . ? C1 N2 1.296(8) . ? C1 N1 1.343(7) . ? C1 H1 0.9300 . ? C2 N1 1.323(7) . ? C2 N3 1.331(7) . ? C2 H2 0.9300 . ? C3 N3 1.468(7) . ? C3 C4 1.504(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.365(8) . ? C4 C5 1.378(8) . ? C5 C6 1.384(8) . ? C5 H5 0.9300 . ? C6 C7 1.403(8) . ? C6 H6 0.9300 . ? C7 C8 1.372(8) . ? C7 C7 1.498(10) 2_768 ? C8 C9 1.376(8) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 N4 1.292(8) . ? C10 N6 1.305(8) . ? C10 H10 0.9300 . ? C11 N5 1.313(8) . ? C11 N4 1.344(8) . ? C11 H11 0.9300 . ? C12 N6 1.484(8) . ? C12 C13 1.524(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C18 1.324(10) . ? C13 C14 1.352(10) . ? C14 C15 1.369(11) . ? C14 H14 0.9300 . ? C15 C16 1.324(11) . ? C15 H15 0.9300 . ? C16 C17 1.350(10) . ? C16 C16 1.470(16) 2_576 ? C17 C18 1.409(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 O1 1.238(6) . ? C19 O2 1.264(6) . ? C19 C20 1.531(7) . ? C20 C25 1.518(7) . ? C20 C21 1.543(7) . ? C20 C26 1.554(7) . ? C21 C22 1.525(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.521(8) . ? C22 C28 1.555(9) . ? C22 H22 0.9800 . ? C23 C24 1.538(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C30 1.521(7) . ? C24 C25 1.535(7) . ? C24 C29 1.537(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.527(8) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C29 1.536(8) . ? C27 C28 1.539(9) . ? C27 H27 0.9800 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 O4 1.229(6) . ? C30 O3 1.262(7) . ? N2 N3 1.366(6) . ? N5 N6 1.329(7) . ? O3 Cd1 2.576(4) 1_455 ? O4 Cd1 2.328(4) 1_455 ? O5 H5A 0.8428 . ? O5 H5B 0.8400 . ? O6 H6A 0.8482 . ? O6 H6B 0.8614 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cd1 O2 99.88(16) . . ? N1 Cd1 O5 90.22(16) . . ? O2 Cd1 O5 133.54(15) . . ? N1 Cd1 O4 100.09(17) . 1_655 ? O2 Cd1 O4 83.02(14) . 1_655 ? O5 Cd1 O4 139.85(15) . 1_655 ? N1 Cd1 N4 169.16(17) . . ? O2 Cd1 N4 89.02(17) . . ? O5 Cd1 N4 79.12(17) . . ? O4 Cd1 N4 87.04(18) 1_655 . ? N1 Cd1 O3 87.82(15) . 1_655 ? O2 Cd1 O3 135.04(14) . 1_655 ? O5 Cd1 O3 90.17(15) . 1_655 ? O4 Cd1 O3 52.06(14) 1_655 1_655 ? N4 Cd1 O3 90.22(16) . 1_655 ? N1 Cd1 O1 94.43(14) . . ? O2 Cd1 O1 52.27(13) . . ? O5 Cd1 O1 81.98(14) . . ? O4 Cd1 O1 134.81(13) 1_655 . ? N4 Cd1 O1 86.11(15) . . ? O3 Cd1 O1 171.84(13) 1_655 . ? N2 C1 N1 114.2(5) . . ? N2 C1 H1 122.9 . . ? N1 C1 H1 122.9 . . ? N1 C2 N3 109.1(5) . . ? N1 C2 H2 125.4 . . ? N3 C2 H2 125.4 . . ? N3 C3 C4 114.5(5) . . ? N3 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? N3 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C9 C4 C5 117.0(5) . . ? C9 C4 C3 117.4(5) . . ? C5 C4 C3 125.4(5) . . ? C4 C5 C6 121.7(6) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C7 120.7(6) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C8 C7 C6 116.4(5) . . ? C8 C7 C7 122.9(7) . 2_768 ? C6 C7 C7 120.7(7) . 2_768 ? C7 C8 C9 121.9(6) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C4 C9 C8 122.0(6) . . ? C4 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? N4 C10 N6 112.5(6) . . ? N4 C10 H10 123.8 . . ? N6 C10 H10 123.8 . . ? N5 C11 N4 114.1(6) . . ? N5 C11 H11 123.0 . . ? N4 C11 H11 123.0 . . ? N6 C12 C13 110.3(6) . . ? N6 C12 H12A 109.6 . . ? C13 C12 H12A 109.6 . . ? N6 C12 H12B 109.6 . . ? C13 C12 H12B 109.6 . . ? H12A C12 H12B 108.1 . . ? C18 C13 C14 117.0(8) . . ? C18 C13 C12 118.7(7) . . ? C14 C13 C12 124.2(8) . . ? C13 C14 C15 121.0(8) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 123.6(8) . . ? C16 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? C15 C16 C17 115.6(8) . . ? C15 C16 C16 123.1(9) . 2_576 ? C17 C16 C16 121.3(10) . 2_576 ? C16 C17 C18 121.7(8) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C13 C18 C17 120.9(8) . . ? C13 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? O1 C19 O2 121.3(5) . . ? O1 C19 C20 121.1(5) . . ? O2 C19 C20 117.6(5) . . ? C25 C20 C19 112.6(4) . . ? C25 C20 C21 109.0(4) . . ? C19 C20 C21 106.8(4) . . ? C25 C20 C26 110.1(4) . . ? C19 C20 C26 110.4(4) . . ? C21 C20 C26 107.7(4) . . ? C22 C21 C20 109.8(5) . . ? C22 C21 H21A 109.7 . . ? C20 C21 H21A 109.7 . . ? C22 C21 H21B 109.7 . . ? C20 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C23 C22 C21 109.3(5) . . ? C23 C22 C28 109.7(5) . . ? C21 C22 C28 109.4(5) . . ? C23 C22 H22 109.4 . . ? C21 C22 H22 109.4 . . ? C28 C22 H22 109.4 . . ? C22 C23 C24 110.4(5) . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C30 C24 C25 113.0(4) . . ? C30 C24 C29 110.2(5) . . ? C25 C24 C29 109.1(4) . . ? C30 C24 C23 106.9(4) . . ? C25 C24 C23 108.1(4) . . ? C29 C24 C23 109.5(5) . . ? C20 C25 C24 110.7(4) . . ? C20 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C20 110.5(5) . . ? C27 C26 H26A 109.5 . . ? C20 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C26 C27 C29 109.7(5) . . ? C26 C27 C28 108.0(5) . . ? C29 C27 C28 109.6(5) . . ? C26 C27 H27 109.8 . . ? C29 C27 H27 109.8 . . ? C28 C27 H27 109.8 . . ? C27 C28 C22 109.4(5) . . ? C27 C28 H28A 109.8 . . ? C22 C28 H28A 109.8 . . ? C27 C28 H28B 109.8 . . ? C22 C28 H28B 109.8 . . ? H28A C28 H28B 108.3 . . ? C27 C29 C24 110.4(5) . . ? C27 C29 H29A 109.6 . . ? C24 C29 H29A 109.6 . . ? C27 C29 H29B 109.6 . . ? C24 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? O4 C30 O3 120.6(5) . . ? O4 C30 C24 119.0(5) . . ? O3 C30 C24 120.4(5) . . ? C2 N1 C1 104.1(5) . . ? C2 N1 Cd1 128.3(4) . . ? C1 N1 Cd1 127.4(4) . . ? C1 N2 N3 103.2(5) . . ? C2 N3 N2 109.3(5) . . ? C2 N3 C3 126.1(5) . . ? N2 N3 C3 124.3(5) . . ? C10 N4 C11 101.7(6) . . ? C10 N4 Cd1 126.9(4) . . ? C11 N4 Cd1 130.7(5) . . ? C11 N5 N6 102.9(5) . . ? C10 N6 N5 108.8(5) . . ? C10 N6 C12 128.4(6) . . ? N5 N6 C12 122.4(6) . . ? C19 O1 Cd1 85.2(3) . . ? C19 O2 Cd1 100.4(3) . . ? C30 O3 Cd1 87.2(3) . 1_455 ? C30 O4 Cd1 99.9(4) . 1_455 ? Cd1 O5 H5A 128.7 . . ? Cd1 O5 H5B 102.1 . . ? H5A O5 H5B 108.2 . . ? H6A O6 H6B 104.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C3 C4 C9 -165.5(6) . . . . ? N3 C3 C4 C5 18.7(9) . . . . ? C9 C4 C5 C6 2.9(10) . . . . ? C3 C4 C5 C6 178.7(6) . . . . ? C4 C5 C6 C7 1.1(10) . . . . ? C5 C6 C7 C8 -4.9(10) . . . . ? C5 C6 C7 C7 178.8(7) . . . 2_768 ? C6 C7 C8 C9 4.8(11) . . . . ? C7 C7 C8 C9 -179.0(7) 2_768 . . . ? C5 C4 C9 C8 -3.1(11) . . . . ? C3 C4 C9 C8 -179.2(7) . . . . ? C7 C8 C9 C4 -0.9(13) . . . . ? N6 C12 C13 C18 -119.8(9) . . . . ? N6 C12 C13 C14 61.8(12) . . . . ? C18 C13 C14 C15 4.5(15) . . . . ? C12 C13 C14 C15 -177.0(9) . . . . ? C13 C14 C15 C16 -1.7(17) . . . . ? C14 C15 C16 C17 0.6(16) . . . . ? C14 C15 C16 C16 178.5(11) . . . 2_576 ? C15 C16 C17 C18 -2.4(16) . . . . ? C16 C16 C17 C18 179.7(11) 2_576 . . . ? C14 C13 C18 C17 -6.2(15) . . . . ? C12 C13 C18 C17 175.2(8) . . . . ? C16 C17 C18 C13 5.4(16) . . . . ? O1 C19 C20 C25 24.1(7) . . . . ? O2 C19 C20 C25 -157.8(5) . . . . ? O1 C19 C20 C21 -95.5(6) . . . . ? O2 C19 C20 C21 82.5(6) . . . . ? O1 C19 C20 C26 147.6(5) . . . . ? O2 C19 C20 C26 -34.3(6) . . . . ? C25 C20 C21 C22 59.2(6) . . . . ? C19 C20 C21 C22 -178.8(5) . . . . ? C26 C20 C21 C22 -60.2(6) . . . . ? C20 C21 C22 C23 -59.6(7) . . . . ? C20 C21 C22 C28 60.5(6) . . . . ? C21 C22 C23 C24 60.5(7) . . . . ? C28 C22 C23 C24 -59.5(6) . . . . ? C22 C23 C24 C30 178.3(5) . . . . ? C22 C23 C24 C25 -59.8(6) . . . . ? C22 C23 C24 C29 59.0(6) . . . . ? C19 C20 C25 C24 -178.2(4) . . . . ? C21 C20 C25 C24 -59.8(6) . . . . ? C26 C20 C25 C24 58.0(6) . . . . ? C30 C24 C25 C20 177.9(4) . . . . ? C29 C24 C25 C20 -59.2(6) . . . . ? C23 C24 C25 C20 59.8(6) . . . . ? C25 C20 C26 C27 -57.2(6) . . . . ? C19 C20 C26 C27 177.8(5) . . . . ? C21 C20 C26 C27 61.5(6) . . . . ? C20 C26 C27 C29 57.4(7) . . . . ? C20 C26 C27 C28 -61.9(6) . . . . ? C26 C27 C28 C22 60.5(6) . . . . ? C29 C27 C28 C22 -59.0(6) . . . . ? C23 C22 C28 C27 59.5(6) . . . . ? C21 C22 C28 C27 -60.5(6) . . . . ? C26 C27 C29 C24 -59.1(7) . . . . ? C28 C27 C29 C24 59.3(6) . . . . ? C30 C24 C29 C27 -175.9(5) . . . . ? C25 C24 C29 C27 59.4(6) . . . . ? C23 C24 C29 C27 -58.7(6) . . . . ? C25 C24 C30 O4 162.5(5) . . . . ? C29 C24 C30 O4 40.2(7) . . . . ? C23 C24 C30 O4 -78.7(7) . . . . ? C25 C24 C30 O3 -19.4(7) . . . . ? C29 C24 C30 O3 -141.7(5) . . . . ? C23 C24 C30 O3 99.4(6) . . . . ? N3 C2 N1 C1 0.1(6) . . . . ? N3 C2 N1 Cd1 175.5(3) . . . . ? N2 C1 N1 C2 0.6(7) . . . . ? N2 C1 N1 Cd1 -174.9(4) . . . . ? O2 Cd1 N1 C2 -72.4(5) . . . . ? O5 Cd1 N1 C2 153.2(5) . . . . ? O4 Cd1 N1 C2 12.2(5) 1_655 . . . ? N4 Cd1 N1 C2 142.7(8) . . . . ? O3 Cd1 N1 C2 63.0(5) 1_655 . . . ? O1 Cd1 N1 C2 -124.9(5) . . . . ? O2 Cd1 N1 C1 101.9(5) . . . . ? O5 Cd1 N1 C1 -32.5(5) . . . . ? O4 Cd1 N1 C1 -173.5(5) 1_655 . . . ? N4 Cd1 N1 C1 -42.9(11) . . . . ? O3 Cd1 N1 C1 -122.7(5) 1_655 . . . ? O1 Cd1 N1 C1 49.5(5) . . . . ? N1 C1 N2 N3 -0.9(7) . . . . ? N1 C2 N3 N2 -0.7(6) . . . . ? N1 C2 N3 C3 -174.7(5) . . . . ? C1 N2 N3 C2 1.0(7) . . . . ? C1 N2 N3 C3 175.1(5) . . . . ? C4 C3 N3 C2 -123.1(6) . . . . ? C4 C3 N3 N2 63.8(7) . . . . ? N6 C10 N4 C11 -1.0(8) . . . . ? N6 C10 N4 Cd1 170.1(4) . . . . ? N5 C11 N4 C10 1.2(9) . . . . ? N5 C11 N4 Cd1 -169.4(5) . . . . ? N1 Cd1 N4 C10 58.5(11) . . . . ? O2 Cd1 N4 C10 -87.0(6) . . . . ? O5 Cd1 N4 C10 47.9(6) . . . . ? O4 Cd1 N4 C10 -170.0(6) 1_655 . . . ? O3 Cd1 N4 C10 138.0(6) 1_655 . . . ? O1 Cd1 N4 C10 -34.7(6) . . . . ? N1 Cd1 N4 C11 -133.0(9) . . . . ? O2 Cd1 N4 C11 81.5(6) . . . . ? O5 Cd1 N4 C11 -143.7(6) . . . . ? O4 Cd1 N4 C11 -1.5(6) 1_655 . . . ? O3 Cd1 N4 C11 -53.5(6) 1_655 . . . ? O1 Cd1 N4 C11 133.8(6) . . . . ? N4 C11 N5 N6 -0.9(9) . . . . ? N4 C10 N6 N5 0.6(9) . . . . ? N4 C10 N6 C12 -172.9(6) . . . . ? C11 N5 N6 C10 0.2(8) . . . . ? C11 N5 N6 C12 174.1(6) . . . . ? C13 C12 N6 C10 95.6(9) . . . . ? C13 C12 N6 N5 -77.1(9) . . . . ? O2 C19 O1 Cd1 -8.4(5) . . . . ? C20 C19 O1 Cd1 169.6(4) . . . . ? N1 Cd1 O1 C19 104.1(3) . . . . ? O2 Cd1 O1 C19 5.0(3) . . . . ? O5 Cd1 O1 C19 -166.3(3) . . . . ? O4 Cd1 O1 C19 -4.8(4) 1_655 . . . ? N4 Cd1 O1 C19 -86.8(3) . . . . ? O3 Cd1 O1 C19 -150.2(8) 1_655 . . . ? O1 C19 O2 Cd1 9.8(6) . . . . ? C20 C19 O2 Cd1 -168.3(4) . . . . ? N1 Cd1 O2 C19 -92.9(3) . . . . ? O5 Cd1 O2 C19 6.9(4) . . . . ? O4 Cd1 O2 C19 168.0(4) 1_655 . . . ? N4 Cd1 O2 C19 80.9(3) . . . . ? O3 Cd1 O2 C19 170.2(3) 1_655 . . . ? O1 Cd1 O2 C19 -5.0(3) . . . . ? O4 C30 O3 Cd1 4.4(6) . . . 1_455 ? C24 C30 O3 Cd1 -173.7(5) . . . 1_455 ? O3 C30 O4 Cd1 -5.0(7) . . . 1_455 ? C24 C30 O4 Cd1 173.1(4) . . . 1_455 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.266 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.098 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 802236' #TrackingRef '- cifs 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H28 N3 O5 Zn' _chemical_formula_sum 'C23 H28 N3 O5 Zn' _chemical_formula_weight 491.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.981(5) _cell_length_b 8.4913(13) _cell_length_c 18.479(3) _cell_angle_alpha 90.00 _cell_angle_beta 121.777(2) _cell_angle_gamma 90.00 _cell_volume 4666.2(12) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2360 _cell_measurement_theta_min 2.5935 _cell_measurement_theta_max 21.456 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 1.091 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7014 _exptl_absorpt_correction_T_max 0.8196 _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 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11216 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4144 _reflns_number_gt 3047 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1254P)^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 4144 _refine_ls_number_parameters 289 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1909 _refine_ls_wR_factor_gt 0.1672 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.090 _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 0.226257(15) -0.30499(6) 0.20523(3) 0.0415(2) Uani 1 1 d . . . C1 C 0.27235(15) -0.1270(6) 0.1262(3) 0.0514(12) Uani 1 1 d . . . H1 H 0.2614 -0.0312 0.1322 0.062 Uiso 1 1 calc R . . C2 C 0.28569(15) -0.3706(6) 0.1324(3) 0.0484(11) Uani 1 1 d . . . H2 H 0.2869 -0.4784 0.1422 0.058 Uiso 1 1 calc R . . C3 C 0.33093(17) -0.3670(9) 0.0622(3) 0.0739(18) Uani 1 1 d . . . H3A H 0.3230 -0.3116 0.0102 0.089 Uiso 1 1 calc R . . H3B H 0.3221 -0.4762 0.0474 0.089 Uiso 1 1 calc R . . C4 C 0.38097(17) -0.3597(8) 0.1217(3) 0.0615(15) Uani 1 1 d . . . C5 C 0.40425(17) -0.2232(8) 0.1282(3) 0.0668(16) Uani 1 1 d . . . H5 H 0.3887 -0.1330 0.0991 0.080 Uiso 1 1 calc R . . C6 C 0.45122(17) -0.2212(7) 0.1788(4) 0.0654(15) Uani 1 1 d . . . H6 H 0.4666 -0.1298 0.1819 0.078 Uiso 1 1 calc R . . C7 C 0.47508(15) -0.3522(7) 0.2240(3) 0.0518(12) Uani 1 1 d . . . C8 C 0.45157(16) -0.4845(7) 0.2188(3) 0.0571(13) Uani 1 1 d . . . H8 H 0.4670 -0.5733 0.2500 0.068 Uiso 1 1 calc R . . C9 C 0.40479(18) -0.4886(8) 0.1675(3) 0.0631(14) Uani 1 1 d . . . H9 H 0.3896 -0.5806 0.1644 0.076 Uiso 1 1 calc R . . C10 C 0.14194(16) -0.1948(5) 0.1421(4) 0.0495(12) Uani 1 1 d . . . C11 C 0.09633(14) -0.1348(6) 0.0738(3) 0.0490(11) Uani 1 1 d . . . H11A H 0.0738 -0.1773 0.0839 0.059 Uiso 1 1 calc R . . H11B H 0.0898 -0.1738 0.0191 0.059 Uiso 1 1 calc R . . C12 C 0.09252(13) 0.0455(5) 0.0697(3) 0.0402(10) Uani 1 1 d . . . C13 C 0.08937(15) 0.1102(6) 0.1442(3) 0.0483(11) Uani 1 1 d . . . H13A H 0.0633 0.0653 0.1423 0.058 Uiso 1 1 calc R . . H13B H 0.1160 0.0797 0.1977 0.058 Uiso 1 1 calc R . . C14 C 0.08538(17) 0.2903(6) 0.1396(3) 0.0547(13) Uani 1 1 d . . . H14 H 0.0837 0.3290 0.1878 0.066 Uiso 1 1 calc R . . C15 C 0.12663(17) 0.3602(6) 0.1438(3) 0.0511(12) Uani 1 1 d . . . H15A H 0.1535 0.3301 0.1969 0.061 Uiso 1 1 calc R . . H15B H 0.1246 0.4742 0.1420 0.061 Uiso 1 1 calc R . . C16 C 0.12980(14) 0.3008(5) 0.0687(3) 0.0398(10) Uani 1 1 d . . . C17 C 0.13336(14) 0.1204(5) 0.0738(3) 0.0384(9) Uani 1 1 d . . . H17A H 0.1358 0.0811 0.0270 0.046 Uiso 1 1 calc R . . H17B H 0.1604 0.0900 0.1266 0.046 Uiso 1 1 calc R . . C18 C 0.04996(14) 0.0981(6) -0.0146(3) 0.0480(11) Uani 1 1 d . . . H18A H 0.0518 0.0610 -0.0623 0.058 Uiso 1 1 calc R . . H18B H 0.0236 0.0513 -0.0188 0.058 Uiso 1 1 calc R . . C19 C 0.04267(19) 0.3387(7) 0.0562(4) 0.0699(16) Uani 1 1 d . . . H19A H 0.0400 0.4525 0.0529 0.084 Uiso 1 1 calc R . . H19B H 0.0164 0.2957 0.0542 0.084 Uiso 1 1 calc R . . C20 C 0.04538(16) 0.2755(7) -0.0187(3) 0.0567(13) Uani 1 1 d . . . H20 H 0.0182 0.3059 -0.0724 0.068 Uiso 1 1 calc R . . C21 C 0.08701(15) 0.3479(7) -0.0143(3) 0.0563(13) Uani 1 1 d . . . H21A H 0.0887 0.3115 -0.0623 0.068 Uiso 1 1 calc R . . H21B H 0.0843 0.4617 -0.0175 0.068 Uiso 1 1 calc R . . C22 C 0.17135(15) 0.3760(6) 0.0699(3) 0.0461(11) Uani 1 1 d . . . H22A H 0.1741 0.3295 0.0249 0.055 Uiso 1 1 calc R . . H22B H 0.1663 0.4881 0.0588 0.055 Uiso 1 1 calc R . . C23 C 0.21430(15) 0.3509(5) 0.1537(3) 0.0412(10) Uani 1 1 d . . . N1 N 0.26453(12) -0.2676(5) 0.1521(2) 0.0458(9) Uani 1 1 d . . . N2 N 0.30488(13) -0.2985(5) 0.0970(2) 0.0521(11) Uani 1 1 d . . . N3 N 0.29663(15) -0.1408(6) 0.0922(3) 0.0653(12) Uani 1 1 d . . . O1 O 0.16840(11) -0.2296(4) 0.1162(2) 0.0549(9) Uani 1 1 d . . . O2 O 0.15299(15) -0.2070(5) 0.2165(3) 0.0830(13) Uani 1 1 d . . . O3 O 0.23088(10) 0.4602(4) 0.20922(18) 0.0469(8) Uani 1 1 d . . . O4 O 0.23292(10) 0.2181(3) 0.17104(19) 0.0447(7) Uani 1 1 d . . . O5 O 0.1758(4) 0.7162(11) 0.3794(6) 0.226(4) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0359(4) 0.0365(4) 0.0506(4) 0.0012(2) 0.0217(3) 0.0011(2) C1 0.042(3) 0.056(3) 0.052(3) 0.005(2) 0.022(2) -0.001(2) C2 0.038(2) 0.058(3) 0.054(3) -0.003(2) 0.028(2) -0.005(2) C3 0.043(3) 0.133(6) 0.054(3) -0.022(3) 0.031(2) -0.012(3) C4 0.039(3) 0.111(5) 0.042(3) -0.012(3) 0.027(2) -0.013(3) C5 0.046(3) 0.091(5) 0.057(3) 0.011(3) 0.023(3) -0.001(3) C6 0.036(3) 0.082(4) 0.068(3) 0.014(3) 0.020(2) -0.007(3) C7 0.039(2) 0.080(4) 0.040(2) -0.006(2) 0.023(2) -0.005(3) C8 0.048(3) 0.073(4) 0.052(3) 0.000(3) 0.027(2) -0.003(3) C9 0.063(3) 0.079(4) 0.062(3) -0.012(3) 0.044(3) -0.017(3) C10 0.040(3) 0.031(2) 0.069(3) 0.007(2) 0.023(3) 0.0000(19) C11 0.031(2) 0.050(3) 0.064(3) 0.001(2) 0.023(2) -0.002(2) C12 0.026(2) 0.044(3) 0.045(2) 0.001(2) 0.0152(18) 0.0004(18) C13 0.041(3) 0.066(3) 0.043(2) 0.001(2) 0.025(2) 0.000(2) C14 0.053(3) 0.062(3) 0.058(3) -0.004(2) 0.036(3) 0.010(2) C15 0.058(3) 0.040(3) 0.059(3) -0.005(2) 0.033(3) 0.005(2) C16 0.034(2) 0.037(2) 0.042(2) 0.0047(19) 0.0155(19) 0.0002(18) C17 0.033(2) 0.038(2) 0.042(2) -0.0014(19) 0.0187(19) 0.0006(18) C18 0.031(2) 0.058(3) 0.046(2) 0.001(2) 0.015(2) -0.004(2) C19 0.056(3) 0.063(4) 0.094(4) 0.007(3) 0.041(3) 0.016(3) C20 0.036(3) 0.071(4) 0.050(3) 0.017(3) 0.014(2) 0.010(2) C21 0.045(3) 0.055(3) 0.054(3) 0.017(2) 0.015(2) 0.006(2) C22 0.047(3) 0.048(3) 0.040(2) 0.003(2) 0.020(2) -0.006(2) C23 0.042(2) 0.037(2) 0.048(3) 0.004(2) 0.026(2) -0.004(2) N1 0.039(2) 0.045(2) 0.051(2) 0.0016(18) 0.0223(18) -0.0035(18) N2 0.034(2) 0.075(3) 0.046(2) -0.011(2) 0.0201(18) -0.0133(19) N3 0.053(3) 0.083(4) 0.061(3) 0.013(3) 0.030(2) -0.004(2) O1 0.0349(18) 0.050(2) 0.069(2) 0.0045(17) 0.0200(17) 0.0065(15) O2 0.081(3) 0.094(4) 0.067(3) 0.029(2) 0.034(2) 0.020(2) O3 0.0484(19) 0.0307(17) 0.0524(18) -0.0028(13) 0.0201(16) -0.0024(13) O4 0.0449(18) 0.0349(18) 0.0527(18) -0.0010(14) 0.0246(15) 0.0028(14) O5 0.337(9) 0.219(7) 0.198(6) 0.062(5) 0.193(6) 0.138(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 O1 1.925(3) . ? Zn1 O4 1.966(3) 4_545 ? Zn1 O3 1.999(3) 1_545 ? Zn1 N1 2.059(4) . ? C1 N3 1.301(6) . ? C1 N1 1.367(6) . ? C1 H1 0.9300 . ? C2 N2 1.310(6) . ? C2 N1 1.315(6) . ? C2 H2 0.9300 . ? C3 N2 1.483(6) . ? C3 C4 1.500(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.367(8) . ? C4 C5 1.385(8) . ? C5 C6 1.398(7) . ? C5 H5 0.9300 . ? C6 C7 1.377(8) . ? C6 H6 0.9300 . ? C7 C8 1.365(7) . ? C7 C7 1.483(9) 2_655 ? C8 C9 1.394(7) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 O2 1.221(6) . ? C10 O1 1.281(6) . ? C10 C11 1.509(6) . ? C11 C12 1.536(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.529(5) . ? C12 C13 1.539(6) . ? C12 C18 1.549(6) . ? C13 C14 1.534(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.524(7) . ? C14 C19 1.533(8) . ? C14 H14 0.9800 . ? C15 C16 1.534(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.528(6) . ? C16 C17 1.536(6) . ? C16 C22 1.577(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C20 1.513(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.534(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.542(7) . ? C20 H20 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.501(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 O4 1.257(5) . ? C23 O3 1.274(5) . ? N2 N3 1.362(6) . ? O3 Zn1 1.999(3) 1_565 ? O4 Zn1 1.966(3) 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 O4 138.92(14) . 4_545 ? O1 Zn1 O3 113.04(13) . 1_545 ? O4 Zn1 O3 93.52(12) 4_545 1_545 ? O1 Zn1 N1 101.30(15) . . ? O4 Zn1 N1 106.41(14) 4_545 . ? O3 Zn1 N1 96.37(14) 1_545 . ? N3 C1 N1 113.1(5) . . ? N3 C1 H1 123.4 . . ? N1 C1 H1 123.4 . . ? N2 C2 N1 109.8(5) . . ? N2 C2 H2 125.1 . . ? N1 C2 H2 125.1 . . ? N2 C3 C4 114.3(4) . . ? N2 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? N2 C3 H3B 108.7 . . ? C4 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C9 C4 C5 118.5(5) . . ? C9 C4 C3 121.1(6) . . ? C5 C4 C3 120.3(6) . . ? C4 C5 C6 119.9(6) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 121.3(5) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C8 C7 C6 118.1(4) . . ? C8 C7 C7 120.3(3) . 2_655 ? C6 C7 C7 121.5(3) . 2_655 ? C7 C8 C9 121.1(5) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C4 C9 C8 121.0(5) . . ? C4 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? O2 C10 O1 122.6(5) . . ? O2 C10 C11 122.6(5) . . ? O1 C10 C11 114.8(5) . . ? C10 C11 C12 113.8(4) . . ? C10 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? C10 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C17 C12 C11 110.9(3) . . ? C17 C12 C13 108.2(3) . . ? C11 C12 C13 110.9(4) . . ? C17 C12 C18 107.9(3) . . ? C11 C12 C18 110.4(4) . . ? C13 C12 C18 108.3(4) . . ? C14 C13 C12 110.7(4) . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C19 110.0(4) . . ? C15 C14 C13 109.2(4) . . ? C19 C14 C13 109.6(4) . . ? C15 C14 H14 109.3 . . ? C19 C14 H14 109.3 . . ? C13 C14 H14 109.3 . . ? C14 C15 C16 110.1(4) . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.2 . . ? C21 C16 C15 108.8(4) . . ? C21 C16 C17 109.1(4) . . ? C15 C16 C17 108.4(3) . . ? C21 C16 C22 108.4(3) . . ? C15 C16 C22 111.1(4) . . ? C17 C16 C22 111.0(3) . . ? C12 C17 C16 111.6(3) . . ? C12 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? C12 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C20 C18 C12 111.0(4) . . ? C20 C18 H18A 109.4 . . ? C12 C18 H18A 109.4 . . ? C20 C18 H18B 109.4 . . ? C12 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C14 C19 C20 108.8(4) . . ? C14 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? C14 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C18 C20 C19 111.0(4) . . ? C18 C20 C21 108.8(4) . . ? C19 C20 C21 108.6(5) . . ? C18 C20 H20 109.5 . . ? C19 C20 H20 109.5 . . ? C21 C20 H20 109.5 . . ? C16 C21 C20 110.3(4) . . ? C16 C21 H21A 109.6 . . ? C20 C21 H21A 109.6 . . ? C16 C21 H21B 109.6 . . ? C20 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C16 111.8(3) . . ? C23 C22 H22A 109.3 . . ? C16 C22 H22A 109.3 . . ? C23 C22 H22B 109.3 . . ? C16 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? O4 C23 O3 119.6(4) . . ? O4 C23 C22 119.5(4) . . ? O3 C23 C22 120.8(4) . . ? C2 N1 C1 103.8(4) . . ? C2 N1 Zn1 129.2(3) . . ? C1 N1 Zn1 127.0(3) . . ? C2 N2 N3 110.2(4) . . ? C2 N2 C3 128.8(5) . . ? N3 N2 C3 120.9(4) . . ? C1 N3 N2 103.1(4) . . ? C10 O1 Zn1 113.5(3) . . ? C23 O3 Zn1 134.7(3) . 1_565 ? C23 O4 Zn1 110.3(3) . 4 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C3 C4 C9 100.8(6) . . . . ? N2 C3 C4 C5 -82.2(7) . . . . ? C9 C4 C5 C6 2.1(8) . . . . ? C3 C4 C5 C6 -175.0(5) . . . . ? C4 C5 C6 C7 -1.3(9) . . . . ? C5 C6 C7 C8 -0.6(8) . . . . ? C5 C6 C7 C7 178.5(6) . . . 2_655 ? C6 C7 C8 C9 1.7(7) . . . . ? C7 C7 C8 C9 -177.4(5) 2_655 . . . ? C5 C4 C9 C8 -1.0(7) . . . . ? C3 C4 C9 C8 176.0(4) . . . . ? C7 C8 C9 C4 -0.9(7) . . . . ? O2 C10 C11 C12 81.8(6) . . . . ? O1 C10 C11 C12 -97.1(5) . . . . ? C10 C11 C12 C17 45.9(5) . . . . ? C10 C11 C12 C13 -74.4(5) . . . . ? C10 C11 C12 C18 165.5(4) . . . . ? C17 C12 C13 C14 58.3(4) . . . . ? C11 C12 C13 C14 -179.8(4) . . . . ? C18 C12 C13 C14 -58.4(5) . . . . ? C12 C13 C14 C15 -59.9(5) . . . . ? C12 C13 C14 C19 60.8(5) . . . . ? C19 C14 C15 C16 -59.9(5) . . . . ? C13 C14 C15 C16 60.4(5) . . . . ? C14 C15 C16 C21 58.8(5) . . . . ? C14 C15 C16 C17 -59.7(5) . . . . ? C14 C15 C16 C22 178.1(4) . . . . ? C11 C12 C17 C16 179.4(3) . . . . ? C13 C12 C17 C16 -58.7(4) . . . . ? C18 C12 C17 C16 58.2(4) . . . . ? C21 C16 C17 C12 -58.7(5) . . . . ? C15 C16 C17 C12 59.7(4) . . . . ? C22 C16 C17 C12 -178.1(3) . . . . ? C17 C12 C18 C20 -59.6(5) . . . . ? C11 C12 C18 C20 179.0(4) . . . . ? C13 C12 C18 C20 57.4(5) . . . . ? C15 C14 C19 C20 60.7(6) . . . . ? C13 C14 C19 C20 -59.5(5) . . . . ? C12 C18 C20 C19 -58.8(5) . . . . ? C12 C18 C20 C21 60.6(5) . . . . ? C14 C19 C20 C18 59.1(6) . . . . ? C14 C19 C20 C21 -60.4(6) . . . . ? C15 C16 C21 C20 -59.6(5) . . . . ? C17 C16 C21 C20 58.4(5) . . . . ? C22 C16 C21 C20 179.5(4) . . . . ? C18 C20 C21 C16 -59.9(5) . . . . ? C19 C20 C21 C16 60.9(6) . . . . ? C21 C16 C22 C23 173.4(4) . . . . ? C15 C16 C22 C23 53.9(5) . . . . ? C17 C16 C22 C23 -66.7(5) . . . . ? C16 C22 C23 O4 76.2(5) . . . . ? C16 C22 C23 O3 -100.3(5) . . . . ? N2 C2 N1 C1 -0.1(5) . . . . ? N2 C2 N1 Zn1 177.7(3) . . . . ? N3 C1 N1 C2 0.2(5) . . . . ? N3 C1 N1 Zn1 -177.7(3) . . . . ? O1 Zn1 N1 C2 -117.6(4) . . . . ? O4 Zn1 N1 C2 93.1(4) 4_545 . . . ? O3 Zn1 N1 C2 -2.5(4) 1_545 . . . ? O1 Zn1 N1 C1 59.8(4) . . . . ? O4 Zn1 N1 C1 -89.5(4) 4_545 . . . ? O3 Zn1 N1 C1 174.9(4) 1_545 . . . ? N1 C2 N2 N3 0.0(5) . . . . ? N1 C2 N2 C3 -177.8(4) . . . . ? C4 C3 N2 C2 -98.2(7) . . . . ? C4 C3 N2 N3 84.2(7) . . . . ? N1 C1 N3 N2 -0.2(5) . . . . ? C2 N2 N3 C1 0.2(5) . . . . ? C3 N2 N3 C1 178.1(4) . . . . ? O2 C10 O1 Zn1 0.9(6) . . . . ? C11 C10 O1 Zn1 179.8(3) . . . . ? O4 Zn1 O1 C10 -27.9(4) 4_545 . . . ? O3 Zn1 O1 C10 98.2(3) 1_545 . . . ? N1 Zn1 O1 C10 -159.8(3) . . . . ? O4 C23 O3 Zn1 159.4(3) . . . 1_565 ? C22 C23 O3 Zn1 -24.2(6) . . . 1_565 ? O3 C23 O4 Zn1 17.3(5) . . . 4 ? C22 C23 O4 Zn1 -159.2(3) . . . 4 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.278 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.093 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 802237' #TrackingRef '- cifs 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H70 Co2 N12 O9' _chemical_formula_sum 'C64 H70 Co2 N12 O9' _chemical_formula_weight 1269.18 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1247(19) _cell_length_b 12.1808(19) _cell_length_c 13.519(4) _cell_angle_alpha 82.922(3) _cell_angle_beta 88.411(2) _cell_angle_gamma 84.781(2) _cell_volume 1484.7(6) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3351 _cell_measurement_theta_min 2.406 _cell_measurement_theta_max 27.0215 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.628 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8291 _exptl_absorpt_correction_T_max 0.9228 _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 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7471 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.09 _reflns_number_total 5194 _reflns_number_gt 4404 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.8199P] 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 5194 _refine_ls_number_parameters 397 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1052 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.032 _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 Co1 Co 0.66690(4) -0.05788(2) 0.90982(2) 0.03603(12) Uani 1 1 d . . . C1 C 0.4481(3) -0.0129(2) 0.72561(19) 0.0446(6) Uani 1 1 d . . . H1 H 0.3850 -0.0634 0.7558 0.054 Uiso 1 1 calc R . . C2 C 0.6226(3) 0.0857(2) 0.70338(19) 0.0477(6) Uani 1 1 d . . . H2 H 0.7073 0.1205 0.7118 0.057 Uiso 1 1 calc R . . C3 C 0.5721(3) 0.1690(2) 0.5270(2) 0.0519(7) Uani 1 1 d . . . H3A H 0.5791 0.1204 0.4751 0.062 Uiso 1 1 calc R . . H3B H 0.6668 0.1986 0.5302 0.062 Uiso 1 1 calc R . . C4 C 0.4576(3) 0.2641(2) 0.49809(18) 0.0445(6) Uani 1 1 d . . . C5 C 0.4258(4) 0.3468(2) 0.5586(2) 0.0557(7) Uani 1 1 d . . . H5 H 0.4655 0.3394 0.6219 0.067 Uiso 1 1 calc R . . C6 C 0.3351(4) 0.4409(2) 0.52563(19) 0.0537(7) Uani 1 1 d . . . H6 H 0.3147 0.4960 0.5672 0.064 Uiso 1 1 calc R . . C7 C 0.2738(3) 0.4544(2) 0.43093(17) 0.0393(6) Uani 1 1 d . . . C8 C 0.3021(3) 0.3688(2) 0.37264(18) 0.0430(6) Uani 1 1 d . . . H8 H 0.2600 0.3749 0.3101 0.052 Uiso 1 1 calc R . . C9 C 0.3916(3) 0.2746(2) 0.40581(19) 0.0452(6) Uani 1 1 d . . . H9 H 0.4078 0.2176 0.3658 0.054 Uiso 1 1 calc R . . C10 C 0.1851(3) 0.5597(2) 0.39393(17) 0.0393(6) Uani 1 1 d . . . C11 C 0.0902(3) 0.6157(2) 0.45683(18) 0.0468(6) Uani 1 1 d . . . H11 H 0.0809 0.5864 0.5233 0.056 Uiso 1 1 calc R . . C12 C 0.0089(3) 0.7143(2) 0.42268(18) 0.0462(6) Uani 1 1 d . . . H12 H -0.0542 0.7498 0.4663 0.055 Uiso 1 1 calc R . . C13 C 0.0211(3) 0.7600(2) 0.32431(18) 0.0392(6) Uani 1 1 d . . . C14 C 0.1149(3) 0.7052(2) 0.26163(19) 0.0519(7) Uani 1 1 d . . . H14 H 0.1239 0.7350 0.1953 0.062 Uiso 1 1 calc R . . C15 C 0.1962(3) 0.6067(2) 0.29497(19) 0.0506(7) Uani 1 1 d . . . H15 H 0.2588 0.5716 0.2509 0.061 Uiso 1 1 calc R . . C16 C -0.0659(3) 0.8677(2) 0.28672(19) 0.0458(6) Uani 1 1 d . . . H16A H -0.1326 0.8905 0.3390 0.055 Uiso 1 1 calc R . . H16B H 0.0009 0.9250 0.2700 0.055 Uiso 1 1 calc R . . C17 C -0.1521(3) 0.9142(2) 0.10855(18) 0.0413(6) Uani 1 1 d . . . H17 H -0.0950 0.9728 0.0888 0.050 Uiso 1 1 calc R . . C18 C -0.3028(4) 0.7927(2) 0.1126(2) 0.0647(9) Uani 1 1 d . . . H18 H -0.3744 0.7505 0.0929 0.078 Uiso 1 1 calc R . . C19 C 0.3854(3) -0.16108(19) 1.00815(17) 0.0352(5) Uani 1 1 d . . . C20 C 0.3571(3) -0.28330(19) 1.01938(18) 0.0418(6) Uani 1 1 d . . . H20A H 0.2904 -0.2972 1.0757 0.050 Uiso 1 1 calc R . . H20B H 0.4494 -0.3271 1.0354 0.050 Uiso 1 1 calc R . . C21 C 0.2923(3) -0.32545(18) 0.92857(17) 0.0347(5) Uani 1 1 d . . . C22 C 0.1703(3) -0.24161(18) 0.88095(17) 0.0342(5) Uani 1 1 d . . . H22A H 0.0945 -0.2274 0.9307 0.041 Uiso 1 1 calc R . . H22B H 0.2112 -0.1720 0.8581 0.041 Uiso 1 1 calc R . . C23 C 0.1015(3) -0.28514(18) 0.79278(17) 0.0351(5) Uani 1 1 d . . . C24 C 0.2247(3) -0.3102(2) 0.71663(18) 0.0415(6) Uani 1 1 d . . . H24A H 0.1831 -0.3376 0.6602 0.050 Uiso 1 1 calc R . . H24B H 0.2689 -0.2422 0.6925 0.050 Uiso 1 1 calc R . . C25 C 0.3430(3) -0.3962(2) 0.76288(19) 0.0437(6) Uani 1 1 d . . . H25 H 0.4195 -0.4113 0.7128 0.052 Uiso 1 1 calc R . . C26 C 0.4105(3) -0.3508(2) 0.84996(18) 0.0390(5) Uani 1 1 d . . . H26A H 0.4563 -0.2836 0.8257 0.047 Uiso 1 1 calc R . . H26B H 0.4861 -0.4050 0.8799 0.047 Uiso 1 1 calc R . . C27 C 0.2214(3) -0.43413(19) 0.96528(19) 0.0428(6) Uani 1 1 d . . . H27A H 0.2954 -0.4887 0.9965 0.051 Uiso 1 1 calc R . . H27B H 0.1453 -0.4197 1.0148 0.051 Uiso 1 1 calc R . . C28 C 0.0342(3) -0.3944(2) 0.8307(2) 0.0455(6) Uani 1 1 d . . . H28A H -0.0428 -0.3806 0.8797 0.055 Uiso 1 1 calc R . . H28B H -0.0093 -0.4232 0.7757 0.055 Uiso 1 1 calc R . . C29 C 0.2731(3) -0.5031(2) 0.8007(2) 0.0498(7) Uani 1 1 d . . . H29A H 0.2307 -0.5321 0.7453 0.060 Uiso 1 1 calc R . . H29B H 0.3478 -0.5583 0.8299 0.060 Uiso 1 1 calc R . . C30 C 0.1541(3) -0.4803(2) 0.8780(2) 0.0449(6) Uani 1 1 d . . . H30 H 0.1105 -0.5494 0.9024 0.054 Uiso 1 1 calc R . . C31 C -0.0125(3) -0.1978(2) 0.74011(18) 0.0411(6) Uani 1 1 d . . . H31A H 0.0390 -0.1368 0.7072 0.049 Uiso 1 1 calc R . . H31B H -0.0589 -0.2311 0.6888 0.049 Uiso 1 1 calc R . . C32 C -0.1318(3) -0.1510(2) 0.80708(18) 0.0395(6) Uani 1 1 d . . . N1 N 0.5673(2) 0.01268(16) 0.77081(15) 0.0409(5) Uani 1 1 d . . . N2 N 0.4277(3) 0.03909(19) 0.63504(16) 0.0494(5) Uani 1 1 d . . . N3 N 0.5426(2) 0.10302(16) 0.62262(15) 0.0407(5) Uani 1 1 d . . . N4 N -0.2460(3) 0.87691(16) 0.05180(15) 0.0455(5) Uani 1 1 d . . . N5 N -0.2460(3) 0.7776(2) 0.2014(2) 0.0710(8) Uani 1 1 d . . . N6 N -0.1504(2) 0.85577(16) 0.19865(15) 0.0403(5) Uani 1 1 d . . . O1 O 0.4757(2) -0.12662(16) 0.94323(13) 0.0531(5) Uani 1 1 d . . . O2 O 0.3139(2) -0.10287(14) 1.06591(13) 0.0508(5) Uani 1 1 d . . . O3 O -0.2428(2) -0.20163(15) 0.83128(15) 0.0542(5) Uani 1 1 d . . . O4 O -0.1187(2) -0.05883(14) 0.83790(14) 0.0501(5) Uani 1 1 d . . . O5 O 0.1702(16) 0.0266(12) 0.4765(10) 0.264(6) Uani 0.50 1 d PU . . H5A H 0.1099 -0.0231 0.4830 0.396 Uiso 0.50 1 d PR . . H5B H 0.1231 0.0903 0.4740 0.396 Uiso 0.50 1 d PR . . 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 0.0377(2) 0.03340(19) 0.03549(19) -0.00015(13) -0.00733(14) 0.00137(13) C1 0.0451(15) 0.0411(13) 0.0466(14) 0.0025(11) -0.0059(12) -0.0078(11) C2 0.0426(15) 0.0499(15) 0.0488(15) 0.0080(12) -0.0153(12) -0.0085(12) C3 0.0525(17) 0.0542(16) 0.0427(14) 0.0113(12) 0.0019(13) 0.0058(13) C4 0.0465(16) 0.0456(14) 0.0371(13) 0.0090(11) -0.0014(11) 0.0001(12) C5 0.074(2) 0.0550(16) 0.0354(14) 0.0018(12) -0.0170(13) 0.0054(15) C6 0.073(2) 0.0479(15) 0.0380(14) -0.0048(12) -0.0129(13) 0.0071(14) C7 0.0394(14) 0.0427(13) 0.0343(12) 0.0039(10) -0.0035(10) -0.0058(11) C8 0.0423(15) 0.0533(15) 0.0323(12) -0.0003(11) -0.0084(11) -0.0021(12) C9 0.0493(16) 0.0464(14) 0.0388(13) -0.0032(11) 0.0003(12) -0.0011(12) C10 0.0409(14) 0.0410(13) 0.0342(12) 0.0038(10) -0.0072(11) -0.0037(11) C11 0.0617(18) 0.0471(14) 0.0291(12) 0.0033(10) -0.0042(12) -0.0013(13) C12 0.0575(17) 0.0454(14) 0.0348(13) -0.0054(11) -0.0029(12) 0.0009(12) C13 0.0393(14) 0.0402(13) 0.0375(13) 0.0002(10) -0.0103(11) -0.0046(11) C14 0.0555(18) 0.0598(17) 0.0331(13) 0.0136(12) 0.0022(12) 0.0062(14) C15 0.0484(16) 0.0606(17) 0.0370(13) 0.0063(12) 0.0027(12) 0.0089(13) C16 0.0541(17) 0.0414(14) 0.0418(14) -0.0026(11) -0.0149(12) -0.0018(12) C17 0.0449(15) 0.0366(13) 0.0408(13) 0.0033(10) -0.0059(11) -0.0038(11) C18 0.092(2) 0.0404(15) 0.0623(18) 0.0147(13) -0.0441(18) -0.0244(15) C19 0.0368(13) 0.0381(12) 0.0304(12) -0.0010(10) -0.0119(10) -0.0026(10) C20 0.0509(16) 0.0357(12) 0.0373(13) -0.0005(10) -0.0040(11) 0.0003(11) C21 0.0370(13) 0.0295(11) 0.0368(12) -0.0021(9) 0.0000(10) -0.0021(10) C22 0.0349(13) 0.0301(11) 0.0373(12) -0.0041(9) 0.0001(10) -0.0011(10) C23 0.0351(13) 0.0315(11) 0.0390(12) -0.0059(10) -0.0018(10) -0.0022(10) C24 0.0467(15) 0.0432(13) 0.0369(13) -0.0121(10) 0.0022(11) -0.0067(11) C25 0.0418(15) 0.0430(14) 0.0478(14) -0.0150(11) 0.0079(12) -0.0013(11) C26 0.0335(13) 0.0379(13) 0.0452(14) -0.0063(10) 0.0018(11) -0.0006(10) C27 0.0466(15) 0.0332(12) 0.0462(14) 0.0030(10) 0.0025(12) -0.0023(11) C28 0.0412(15) 0.0416(14) 0.0551(16) -0.0059(12) -0.0021(12) -0.0114(11) C29 0.0532(17) 0.0362(13) 0.0616(17) -0.0153(12) -0.0029(14) -0.0001(12) C30 0.0469(16) 0.0310(12) 0.0572(16) -0.0019(11) -0.0014(13) -0.0093(11) C31 0.0399(14) 0.0445(14) 0.0390(13) -0.0073(10) -0.0063(11) 0.0009(11) C32 0.0348(14) 0.0374(13) 0.0447(14) -0.0005(10) -0.0100(11) 0.0022(11) N1 0.0398(12) 0.0403(11) 0.0404(11) 0.0036(9) -0.0086(9) -0.0011(9) N2 0.0498(14) 0.0540(13) 0.0439(12) 0.0004(10) -0.0125(10) -0.0067(11) N3 0.0410(12) 0.0383(11) 0.0397(11) 0.0067(9) -0.0071(9) -0.0001(9) N4 0.0567(14) 0.0349(11) 0.0439(12) 0.0001(9) -0.0170(11) 0.0003(10) N5 0.081(2) 0.0579(15) 0.0735(18) 0.0197(13) -0.0321(15) -0.0289(14) N6 0.0465(13) 0.0333(10) 0.0403(11) 0.0026(8) -0.0141(9) -0.0040(9) O1 0.0538(12) 0.0627(12) 0.0441(10) 0.0000(9) -0.0008(9) -0.0204(10) O2 0.0651(13) 0.0381(9) 0.0485(10) -0.0084(8) 0.0012(9) 0.0030(9) O3 0.0422(11) 0.0502(11) 0.0719(13) -0.0132(9) 0.0041(10) -0.0070(9) O4 0.0440(11) 0.0421(10) 0.0649(12) -0.0119(9) -0.0039(9) 0.0009(8) O5 0.271(9) 0.263(9) 0.247(9) -0.036(8) -0.013(8) 0.044(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.0197(19) . ? Co1 O2 2.0485(18) 2_657 ? Co1 N4 2.131(2) 1_646 ? Co1 N1 2.156(2) . ? Co1 O4 2.1605(19) 1_655 ? Co1 O3 2.2405(19) 1_655 ? C1 N2 1.317(3) . ? C1 N1 1.341(3) . ? C1 H1 0.9300 . ? C2 N3 1.315(3) . ? C2 N1 1.316(3) . ? C2 H2 0.9300 . ? C3 N3 1.468(3) . ? C3 C4 1.509(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.380(4) . ? C4 C9 1.387(4) . ? C5 C6 1.385(4) . ? C5 H5 0.9300 . ? C6 C7 1.396(3) . ? C6 H6 0.9300 . ? C7 C8 1.384(4) . ? C7 C10 1.492(3) . ? C8 C9 1.382(4) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.391(4) . ? C10 C15 1.394(3) . ? C11 C12 1.387(4) . ? C11 H11 0.9300 . ? C12 C13 1.383(3) . ? C12 H12 0.9300 . ? C13 C14 1.376(4) . ? C13 C16 1.508(3) . ? C14 C15 1.384(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N6 1.465(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N4 1.313(3) . ? C17 N6 1.333(3) . ? C17 H17 0.9300 . ? C18 N5 1.307(4) . ? C18 N4 1.364(3) . ? C18 H18 0.9300 . ? C19 O1 1.248(3) . ? C19 O2 1.250(3) . ? C19 C20 1.523(3) . ? C20 C21 1.540(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C26 1.531(3) . ? C21 C22 1.539(3) . ? C21 C27 1.547(3) . ? C22 C23 1.534(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.539(3) . ? C23 C28 1.541(3) . ? C23 C31 1.541(3) . ? C24 C25 1.524(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.527(3) . ? C25 C29 1.527(4) . ? C25 H25 0.9800 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C30 1.534(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C30 1.538(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.517(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30 0.9800 . ? C31 C32 1.513(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 O3 1.248(3) . ? C32 O4 1.262(3) . ? N2 N3 1.357(3) . ? N4 Co1 2.131(2) 1_464 ? N5 N6 1.345(3) . ? O2 Co1 2.0485(18) 2_657 ? O3 Co1 2.2405(19) 1_455 ? O4 Co1 2.1605(19) 1_455 ? O5 H5A 0.8500 . ? O5 H5B 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 O1 Co1 O2 119.86(8) . 2_657 ? O1 Co1 N4 91.53(8) . 1_646 ? O2 Co1 N4 92.75(8) 2_657 1_646 ? O1 Co1 N1 86.44(8) . . ? O2 Co1 N1 85.81(8) 2_657 . ? N4 Co1 N1 176.50(8) 1_646 . ? O1 Co1 O4 151.10(8) . 1_655 ? O2 Co1 O4 88.35(7) 2_657 1_655 ? N4 Co1 O4 93.34(8) 1_646 1_655 ? N1 Co1 O4 89.81(8) . 1_655 ? O1 Co1 O3 92.07(8) . 1_655 ? O2 Co1 O3 146.75(8) 2_657 1_655 ? N4 Co1 O3 95.62(8) 1_646 1_655 ? N1 Co1 O3 87.30(8) . 1_655 ? O4 Co1 O3 59.12(7) 1_655 1_655 ? N2 C1 N1 114.6(2) . . ? N2 C1 H1 122.7 . . ? N1 C1 H1 122.7 . . ? N3 C2 N1 111.2(2) . . ? N3 C2 H2 124.4 . . ? N1 C2 H2 124.4 . . ? N3 C3 C4 114.5(2) . . ? N3 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? N3 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C9 118.8(2) . . ? C5 C4 C3 121.0(2) . . ? C9 C4 C3 120.0(2) . . ? C4 C5 C6 120.5(2) . . ? 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 . . ? C8 C7 C6 117.8(2) . . ? C8 C7 C10 121.9(2) . . ? C6 C7 C10 120.3(2) . . ? C9 C8 C7 121.1(2) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C4 120.7(2) . . ? C8 C9 H9 119.7 . . ? C4 C9 H9 119.7 . . ? C11 C10 C15 117.4(2) . . ? C11 C10 C7 121.5(2) . . ? C15 C10 C7 121.1(2) . . ? C12 C11 C10 121.5(2) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C13 C12 C11 120.5(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 118.3(2) . . ? C14 C13 C16 120.8(2) . . ? C12 C13 C16 120.9(2) . . ? C13 C14 C15 121.6(2) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C10 120.7(2) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? N6 C16 C13 111.2(2) . . ? N6 C16 H16A 109.4 . . ? C13 C16 H16A 109.4 . . ? N6 C16 H16B 109.4 . . ? C13 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N4 C17 N6 110.0(2) . . ? N4 C17 H17 125.0 . . ? N6 C17 H17 125.0 . . ? N5 C18 N4 112.8(2) . . ? N5 C18 H18 123.6 . . ? N4 C18 H18 123.6 . . ? O1 C19 O2 125.2(2) . . ? O1 C19 C20 118.7(2) . . ? O2 C19 C20 116.0(2) . . ? C19 C20 C21 116.46(19) . . ? C19 C20 H20A 108.2 . . ? C21 C20 H20A 108.2 . . ? C19 C20 H20B 108.2 . . ? C21 C20 H20B 108.2 . . ? H20A C20 H20B 107.3 . . ? C26 C21 C22 109.76(19) . . ? C26 C21 C20 112.1(2) . . ? C22 C21 C20 111.17(19) . . ? C26 C21 C27 108.19(19) . . ? C22 C21 C27 107.41(19) . . ? C20 C21 C27 108.02(19) . . ? C23 C22 C21 111.37(18) . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22B 109.4 . . ? C21 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 108.24(19) . . ? C22 C23 C28 108.72(19) . . ? C24 C23 C28 108.38(19) . . ? C22 C23 C31 111.43(19) . . ? C24 C23 C31 107.79(19) . . ? C28 C23 C31 112.2(2) . . ? C25 C24 C23 111.3(2) . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24B 109.4 . . ? C23 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 108.9(2) . . ? C24 C25 C29 109.2(2) . . ? C26 C25 C29 109.6(2) . . ? C24 C25 H25 109.7 . . ? C26 C25 H25 109.7 . . ? C29 C25 H25 109.7 . . ? C25 C26 C21 110.6(2) . . ? C25 C26 H26A 109.5 . . ? C21 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C30 C27 C21 110.6(2) . . ? C30 C27 H27A 109.5 . . ? C21 C27 H27A 109.5 . . ? C30 C27 H27B 109.5 . . ? C21 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C30 C28 C23 110.0(2) . . ? C30 C28 H28A 109.7 . . ? C23 C28 H28A 109.7 . . ? C30 C28 H28B 109.7 . . ? C23 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C30 C29 C25 110.1(2) . . ? C30 C29 H29A 109.6 . . ? C25 C29 H29A 109.6 . . ? C30 C29 H29B 109.6 . . ? C25 C29 H29B 109.6 . . ? H29A C29 H29B 108.2 . . ? C29 C30 C27 109.5(2) . . ? C29 C30 C28 109.5(2) . . ? C27 C30 C28 109.1(2) . . ? C29 C30 H30 109.6 . . ? C27 C30 H30 109.6 . . ? C28 C30 H30 109.6 . . ? C32 C31 C23 115.4(2) . . ? C32 C31 H31A 108.4 . . ? C23 C31 H31A 108.4 . . ? C32 C31 H31B 108.4 . . ? C23 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? O3 C32 O4 119.9(2) . . ? O3 C32 C31 121.1(2) . . ? O4 C32 C31 119.0(2) . . ? C2 N1 C1 102.6(2) . . ? C2 N1 Co1 126.27(18) . . ? C1 N1 Co1 130.76(17) . . ? C1 N2 N3 102.4(2) . . ? C2 N3 N2 109.2(2) . . ? C2 N3 C3 128.9(2) . . ? N2 N3 C3 121.5(2) . . ? C17 N4 C18 103.7(2) . . ? C17 N4 Co1 131.65(17) . 1_464 ? C18 N4 Co1 123.62(18) . 1_464 ? C18 N5 N6 104.3(2) . . ? C17 N6 N5 109.2(2) . . ? C17 N6 C16 129.9(2) . . ? N5 N6 C16 120.9(2) . . ? C19 O1 Co1 148.46(17) . . ? C19 O2 Co1 129.86(17) . 2_657 ? C32 O3 Co1 88.77(15) . 1_455 ? C32 O4 Co1 92.08(15) . 1_455 ? H5A O5 H5B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C3 C4 C5 58.9(4) . . . . ? N3 C3 C4 C9 -126.7(3) . . . . ? C9 C4 C5 C6 -3.0(4) . . . . ? C3 C4 C5 C6 171.5(3) . . . . ? C4 C5 C6 C7 0.0(5) . . . . ? C5 C6 C7 C8 2.4(4) . . . . ? C5 C6 C7 C10 -175.7(3) . . . . ? C6 C7 C8 C9 -1.9(4) . . . . ? C10 C7 C8 C9 176.1(2) . . . . ? C7 C8 C9 C4 -1.0(4) . . . . ? C5 C4 C9 C8 3.5(4) . . . . ? C3 C4 C9 C8 -171.0(2) . . . . ? C8 C7 C10 C11 143.9(3) . . . . ? C6 C7 C10 C11 -38.1(4) . . . . ? C8 C7 C10 C15 -37.2(4) . . . . ? C6 C7 C10 C15 140.8(3) . . . . ? C15 C10 C11 C12 0.3(4) . . . . ? C7 C10 C11 C12 179.3(2) . . . . ? C10 C11 C12 C13 -0.4(4) . . . . ? C11 C12 C13 C14 0.3(4) . . . . ? C11 C12 C13 C16 -179.5(2) . . . . ? C12 C13 C14 C15 -0.1(4) . . . . ? C16 C13 C14 C15 179.6(3) . . . . ? C13 C14 C15 C10 0.1(5) . . . . ? C11 C10 C15 C14 -0.2(4) . . . . ? C7 C10 C15 C14 -179.2(3) . . . . ? C14 C13 C16 N6 53.6(3) . . . . ? C12 C13 C16 N6 -126.6(3) . . . . ? O1 C19 C20 C21 -62.2(3) . . . . ? O2 C19 C20 C21 117.6(2) . . . . ? C19 C20 C21 C26 80.8(3) . . . . ? C19 C20 C21 C22 -42.4(3) . . . . ? C19 C20 C21 C27 -160.0(2) . . . . ? C26 C21 C22 C23 57.5(2) . . . . ? C20 C21 C22 C23 -177.89(19) . . . . ? C27 C21 C22 C23 -59.9(2) . . . . ? C21 C22 C23 C24 -57.4(2) . . . . ? C21 C22 C23 C28 60.2(3) . . . . ? C21 C22 C23 C31 -175.72(19) . . . . ? C22 C23 C24 C25 59.2(2) . . . . ? C28 C23 C24 C25 -58.5(3) . . . . ? C31 C23 C24 C25 179.9(2) . . . . ? C23 C24 C25 C26 -60.5(3) . . . . ? C23 C24 C25 C29 59.1(3) . . . . ? C24 C25 C26 C21 59.3(3) . . . . ? C29 C25 C26 C21 -60.1(3) . . . . ? C22 C21 C26 C25 -57.9(2) . . . . ? C20 C21 C26 C25 178.03(19) . . . . ? C27 C21 C26 C25 59.0(3) . . . . ? C26 C21 C27 C30 -58.6(3) . . . . ? C22 C21 C27 C30 59.8(3) . . . . ? C20 C21 C27 C30 179.8(2) . . . . ? C22 C23 C28 C30 -59.0(3) . . . . ? C24 C23 C28 C30 58.4(3) . . . . ? C31 C23 C28 C30 177.3(2) . . . . ? C24 C25 C29 C30 -59.6(3) . . . . ? C26 C25 C29 C30 59.7(3) . . . . ? C25 C29 C30 C27 -59.2(3) . . . . ? C25 C29 C30 C28 60.4(3) . . . . ? C21 C27 C30 C29 59.3(3) . . . . ? C21 C27 C30 C28 -60.6(3) . . . . ? C23 C28 C30 C29 -60.2(3) . . . . ? C23 C28 C30 C27 59.6(3) . . . . ? C22 C23 C31 C32 -53.4(3) . . . . ? C24 C23 C31 C32 -172.0(2) . . . . ? C28 C23 C31 C32 68.7(3) . . . . ? C23 C31 C32 O3 -82.5(3) . . . . ? C23 C31 C32 O4 98.1(3) . . . . ? N3 C2 N1 C1 -0.2(3) . . . . ? N3 C2 N1 Co1 173.28(17) . . . . ? N2 C1 N1 C2 0.4(3) . . . . ? N2 C1 N1 Co1 -172.64(18) . . . . ? O1 Co1 N1 C2 172.3(2) . . . . ? O2 Co1 N1 C2 52.0(2) 2_657 . . . ? N4 Co1 N1 C2 117.8(13) 1_646 . . . ? O4 Co1 N1 C2 -36.3(2) 1_655 . . . ? O3 Co1 N1 C2 -95.4(2) 1_655 . . . ? O1 Co1 N1 C1 -16.1(2) . . . . ? O2 Co1 N1 C1 -136.5(2) 2_657 . . . ? N4 Co1 N1 C1 -70.7(13) 1_646 . . . ? O4 Co1 N1 C1 135.2(2) 1_655 . . . ? O3 Co1 N1 C1 76.1(2) 1_655 . . . ? N1 C1 N2 N3 -0.4(3) . . . . ? N1 C2 N3 N2 -0.1(3) . . . . ? N1 C2 N3 C3 -173.6(2) . . . . ? C1 N2 N3 C2 0.3(3) . . . . ? C1 N2 N3 C3 174.4(2) . . . . ? C4 C3 N3 C2 -119.6(3) . . . . ? C4 C3 N3 N2 67.6(3) . . . . ? N6 C17 N4 C18 0.5(3) . . . . ? N6 C17 N4 Co1 168.90(18) . . . 1_464 ? N5 C18 N4 C17 -0.9(4) . . . . ? N5 C18 N4 Co1 -170.5(2) . . . 1_464 ? N4 C18 N5 N6 0.9(4) . . . . ? N4 C17 N6 N5 0.0(3) . . . . ? N4 C17 N6 C16 -178.9(2) . . . . ? C18 N5 N6 C17 -0.5(3) . . . . ? C18 N5 N6 C16 178.5(3) . . . . ? C13 C16 N6 C17 -125.3(3) . . . . ? C13 C16 N6 N5 55.9(3) . . . . ? O2 C19 O1 Co1 62.7(4) . . . . ? C20 C19 O1 Co1 -117.6(3) . . . . ? O2 Co1 O1 C19 -67.4(4) 2_657 . . . ? N4 Co1 O1 C19 26.6(3) 1_646 . . . ? N1 Co1 O1 C19 -150.5(3) . . . . ? O4 Co1 O1 C19 126.3(3) 1_655 . . . ? O3 Co1 O1 C19 122.3(3) 1_655 . . . ? O1 C19 O2 Co1 -8.8(4) . . . 2_657 ? C20 C19 O2 Co1 171.54(16) . . . 2_657 ? O4 C32 O3 Co1 3.6(2) . . . 1_455 ? C31 C32 O3 Co1 -175.8(2) . . . 1_455 ? O3 C32 O4 Co1 -3.7(2) . . . 1_455 ? C31 C32 O4 Co1 175.65(18) . . . 1_455 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.329 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.049 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 802238' #TrackingRef '- cifs 1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H68 Cd2 N12 O8' _chemical_formula_sum 'C64 H68 Cd2 N12 O8' _chemical_formula_weight 1358.10 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0628(10) _cell_length_b 12.4562(14) _cell_length_c 27.207(3) _cell_angle_alpha 83.7860(10) _cell_angle_beta 85.363(2) _cell_angle_gamma 82.622(2) _cell_volume 3021.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3070 _cell_measurement_theta_min 2.349 _cell_measurement_theta_max 22.1625 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7533 _exptl_absorpt_correction_T_max 0.8550 _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 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15113 _diffrn_reflns_av_R_equivalents 0.0822 _diffrn_reflns_av_sigmaI/netI 0.1144 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.10 _reflns_number_total 10478 _reflns_number_gt 5941 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^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 10478 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 0.78580(5) 0.53785(3) 0.297528(16) 0.04027(15) Uani 1 1 d . . . Cd2 Cd 0.14616(5) 0.44703(3) 0.214617(15) 0.03741(15) Uani 1 1 d . . . C1 C 0.3606(7) 0.3497(5) 0.1522(2) 0.0368(15) Uani 1 1 d . . . C2 C 0.4889(6) 0.3033(5) 0.1175(2) 0.0427(16) Uani 1 1 d . . . H2A H 0.4467 0.2743 0.0908 0.051 Uiso 1 1 calc R . . H2B H 0.5428 0.3626 0.1028 0.051 Uiso 1 1 calc R . . C3 C 0.5999(7) 0.2145(4) 0.1414(2) 0.0372(15) Uani 1 1 d . . . C4 C 0.7333(7) 0.1941(5) 0.1044(2) 0.0433(16) Uani 1 1 d . . . H4A H 0.7766 0.2613 0.0952 0.052 Uiso 1 1 calc R . . H4B H 0.7005 0.1705 0.0747 0.052 Uiso 1 1 calc R . . C5 C 0.8522(7) 0.1065(5) 0.1268(2) 0.0467(17) Uani 1 1 d . . . H5 H 0.9364 0.0940 0.1023 0.056 Uiso 1 1 calc R . . C6 C 0.9064(7) 0.1448(5) 0.1726(2) 0.0439(16) Uani 1 1 d . . . H6A H 0.9514 0.2114 0.1636 0.053 Uiso 1 1 calc R . . H6B H 0.9816 0.0901 0.1867 0.053 Uiso 1 1 calc R . . C7 C 0.7734(7) 0.1654(4) 0.2117(2) 0.0356(15) Uani 1 1 d . . . C8 C 0.6539(6) 0.2501(4) 0.1885(2) 0.0345(14) Uani 1 1 d . . . H8A H 0.6945 0.3187 0.1805 0.041 Uiso 1 1 calc R . . H8B H 0.5696 0.2615 0.2125 0.041 Uiso 1 1 calc R . . C9 C 0.5313(6) 0.1077(4) 0.1550(2) 0.0410(16) Uani 1 1 d . . . H9A H 0.4982 0.0833 0.1255 0.049 Uiso 1 1 calc R . . H9B H 0.4454 0.1195 0.1783 0.049 Uiso 1 1 calc R . . C10 C 0.6483(7) 0.0204(5) 0.1782(2) 0.0439(16) Uani 1 1 d . . . H10 H 0.6041 -0.0474 0.1874 0.053 Uiso 1 1 calc R . . C11 C 0.7825(7) 0.0002(5) 0.1411(2) 0.0497(18) Uani 1 1 d . . . H11A H 0.7510 -0.0257 0.1117 0.060 Uiso 1 1 calc R . . H11B H 0.8559 -0.0551 0.1557 0.060 Uiso 1 1 calc R . . C12 C 0.7026(7) 0.0592(4) 0.2245(2) 0.0414(16) Uani 1 1 d . . . H12A H 0.7754 0.0034 0.2391 0.050 Uiso 1 1 calc R . . H12B H 0.6191 0.0709 0.2488 0.050 Uiso 1 1 calc R . . C13 C 0.8246(7) 0.1997(4) 0.2595(2) 0.0462(17) Uani 1 1 d . . . H13A H 0.7561 0.1774 0.2868 0.055 Uiso 1 1 calc R . . H13B H 0.9219 0.1603 0.2655 0.055 Uiso 1 1 calc R . . C14 C 0.8346(8) 0.3201(5) 0.2598(2) 0.0400(16) Uani 1 1 d . . . C15 C 0.5895(8) 0.6586(5) 0.3568(2) 0.0460(17) Uani 1 1 d . . . C16 C 0.4716(7) 0.7370(5) 0.3836(2) 0.0516(18) Uani 1 1 d . . . H16A H 0.4105 0.6946 0.4071 0.062 Uiso 1 1 calc R . . H16B H 0.5221 0.7820 0.4020 0.062 Uiso 1 1 calc R . . C17 C 0.3712(7) 0.8102(5) 0.3485(2) 0.0410(16) Uani 1 1 d . . . C18 C 0.2837(7) 0.9010(5) 0.3771(2) 0.0511(18) Uani 1 1 d . . . H18A H 0.2242 0.8689 0.4048 0.061 Uiso 1 1 calc R . . H18B H 0.3530 0.9419 0.3903 0.061 Uiso 1 1 calc R . . C19 C 0.1820(7) 0.9774(5) 0.3431(2) 0.0501(18) Uani 1 1 d . . . H19 H 0.1268 1.0346 0.3618 0.060 Uiso 1 1 calc R . . C20 C 0.2729(8) 1.0283(5) 0.2996(3) 0.061(2) Uani 1 1 d . . . H20A H 0.3430 1.0706 0.3114 0.073 Uiso 1 1 calc R . . H20B H 0.2074 1.0768 0.2783 0.073 Uiso 1 1 calc R . . C21 C 0.3568(7) 0.9390(5) 0.2705(2) 0.0466(17) Uani 1 1 d . . . H21 H 0.4159 0.9720 0.2424 0.056 Uiso 1 1 calc R . . C22 C 0.4605(7) 0.8637(5) 0.3040(2) 0.0479(17) Uani 1 1 d . . . H22A H 0.5318 0.9050 0.3159 0.057 Uiso 1 1 calc R . . H22B H 0.5156 0.8078 0.2853 0.057 Uiso 1 1 calc R . . C23 C 0.2583(6) 0.7470(4) 0.3288(2) 0.0377(15) Uani 1 1 d . . . H23A H 0.3111 0.6886 0.3111 0.045 Uiso 1 1 calc R . . H23B H 0.1991 0.7147 0.3565 0.045 Uiso 1 1 calc R . . C24 C 0.1554(6) 0.8204(4) 0.2943(2) 0.0329(14) Uani 1 1 d . . . C25 C 0.0730(7) 0.9106(5) 0.3239(2) 0.0475(17) Uani 1 1 d . . . H25A H 0.0055 0.9580 0.3029 0.057 Uiso 1 1 calc R . . H25B H 0.0140 0.8783 0.3516 0.057 Uiso 1 1 calc R . . C26 C 0.2494(7) 0.8727(5) 0.2515(2) 0.0465(17) Uani 1 1 d . . . H26A H 0.3046 0.8165 0.2330 0.056 Uiso 1 1 calc R . . H26B H 0.1845 0.9192 0.2293 0.056 Uiso 1 1 calc R . . C27 C 0.0399(7) 0.7575(5) 0.2766(2) 0.0519(18) Uani 1 1 d . . . H27A H -0.0284 0.7396 0.3048 0.062 Uiso 1 1 calc R . . H27B H -0.0172 0.8059 0.2528 0.062 Uiso 1 1 calc R . . C28 C 0.0952(8) 0.6533(5) 0.2531(2) 0.0408(16) Uani 1 1 d . . . C29 C 0.6010(7) 0.5920(5) 0.1945(2) 0.0438(16) Uani 1 1 d . . . H29 H 0.5411 0.5366 0.2029 0.053 Uiso 1 1 calc R . . C30 C 0.7538(8) 0.7053(5) 0.1961(2) 0.055(2) Uani 1 1 d . . . H30 H 0.8237 0.7437 0.2073 0.066 Uiso 1 1 calc R . . C31 C 0.5289(7) 0.6427(5) 0.1067(2) 0.0483(18) Uani 1 1 d . . . H31A H 0.4580 0.5902 0.1144 0.058 Uiso 1 1 calc R . . H31B H 0.6007 0.6166 0.0809 0.058 Uiso 1 1 calc R . . C32 C 0.4481(7) 0.7508(5) 0.0880(2) 0.0395(15) Uani 1 1 d . . . C33 C 0.3500(8) 0.8102(5) 0.1182(2) 0.0531(19) Uani 1 1 d . . . H33 H 0.3318 0.7827 0.1510 0.064 Uiso 1 1 calc R . . C34 C 0.2773(7) 0.9097(5) 0.1016(2) 0.0480(17) Uani 1 1 d . . . H34 H 0.2116 0.9485 0.1232 0.058 Uiso 1 1 calc R . . C35 C 0.3010(7) 0.9529(5) 0.0526(2) 0.0383(15) Uani 1 1 d . . . C36 C 0.4004(7) 0.8924(5) 0.0218(2) 0.0469(17) Uani 1 1 d . . . H36 H 0.4177 0.9190 -0.0112 0.056 Uiso 1 1 calc R . . C37 C 0.4740(7) 0.7936(5) 0.0392(2) 0.0450(17) Uani 1 1 d . . . H37 H 0.5417 0.7551 0.0181 0.054 Uiso 1 1 calc R . . C38 C 0.2208(7) 1.0582(5) 0.0336(2) 0.0411(16) Uani 1 1 d . . . C39 C 0.2007(7) 1.1480(5) 0.0600(2) 0.0428(16) Uani 1 1 d . . . H39 H 0.2449 1.1451 0.0898 0.051 Uiso 1 1 calc R . . C40 C 0.1151(7) 1.2426(5) 0.0424(2) 0.0462(17) Uani 1 1 d . . . H40 H 0.1040 1.3028 0.0604 0.055 Uiso 1 1 calc R . . C41 C 0.0451(7) 1.2487(5) -0.0021(2) 0.0469(17) Uani 1 1 d . . . C42 C 0.0704(8) 1.1604(5) -0.0290(2) 0.061(2) Uani 1 1 d . . . H42 H 0.0293 1.1636 -0.0595 0.074 Uiso 1 1 calc R . . C43 C 0.1567(8) 1.0667(5) -0.0113(2) 0.059(2) Uani 1 1 d . . . H43 H 0.1721 1.0077 -0.0301 0.070 Uiso 1 1 calc R . . C44 C -0.0660(8) 1.3471(5) -0.0177(2) 0.0561(19) Uani 1 1 d . . . H44A H -0.1635 1.3232 -0.0186 0.067 Uiso 1 1 calc R . . H44B H -0.0736 1.3982 0.0071 0.067 Uiso 1 1 calc R . . C45 C -0.0945(7) 1.4084(5) -0.1082(2) 0.0492(18) Uani 1 1 d . . . H45 H -0.1748 1.3714 -0.1122 0.059 Uiso 1 1 calc R . . C46 C 0.0758(7) 1.5071(5) -0.1196(2) 0.0456(17) Uani 1 1 d . . . H46 H 0.1384 1.5557 -0.1353 0.055 Uiso 1 1 calc R . . C47 C 1.0225(8) 0.4952(5) 0.3892(2) 0.0493(18) Uani 1 1 d . . . H47 H 1.0824 0.5439 0.3719 0.059 Uiso 1 1 calc R . . C48 C 0.8579(7) 0.3943(5) 0.4054(2) 0.0509(18) Uani 1 1 d . . . H48 H 0.7784 0.3549 0.4034 0.061 Uiso 1 1 calc R . . C49 C 0.9084(8) 0.3327(5) 0.4940(2) 0.0560(19) Uani 1 1 d . . . H49A H 0.8115 0.3066 0.4962 0.067 Uiso 1 1 calc R . . H49B H 0.9064 0.3833 0.5188 0.067 Uiso 1 1 calc R . . C50 C 1.0245(7) 0.2379(5) 0.5058(2) 0.0466(17) Uani 1 1 d . . . C51 C 1.0584(8) 0.1550(5) 0.4755(2) 0.058(2) Uani 1 1 d . . . H51 H 1.0155 0.1615 0.4452 0.069 Uiso 1 1 calc R . . C52 C 1.1525(8) 0.0640(5) 0.4885(2) 0.059(2) Uani 1 1 d . . . H52 H 1.1734 0.0097 0.4671 0.071 Uiso 1 1 calc R . . C53 C 1.2176(7) 0.0520(5) 0.5336(2) 0.0448(17) Uani 1 1 d . . . C54 C 1.1889(7) 0.1368(5) 0.5631(2) 0.0501(18) Uani 1 1 d . . . H54 H 1.2343 0.1320 0.5928 0.060 Uiso 1 1 calc R . . C55 C 1.0939(8) 0.2284(5) 0.5491(2) 0.0544(19) Uani 1 1 d . . . H55 H 1.0767 0.2847 0.5694 0.065 Uiso 1 1 calc R . . C56 C 1.3133(7) -0.0501(5) 0.5494(2) 0.0467(17) Uani 1 1 d . . . C57 C 1.4017(8) -0.1109(5) 0.5158(2) 0.056(2) Uani 1 1 d . . . H57 H 1.4014 -0.0867 0.4822 0.068 Uiso 1 1 calc R . . C58 C 1.4904(8) -0.2066(5) 0.5304(2) 0.0557(19) Uani 1 1 d . . . H58 H 1.5488 -0.2448 0.5068 0.067 Uiso 1 1 calc R . . C59 C 1.4918(7) -0.2452(5) 0.5805(2) 0.0451(17) Uani 1 1 d . . . C60 C 1.4064(8) -0.1852(6) 0.6137(2) 0.068(2) Uani 1 1 d . . . H60 H 1.4084 -0.2088 0.6473 0.082 Uiso 1 1 calc R . . C61 C 1.3158(8) -0.0891(6) 0.5989(2) 0.065(2) Uani 1 1 d . . . H61 H 1.2570 -0.0514 0.6225 0.078 Uiso 1 1 calc R . . C62 C 1.5886(7) -0.3500(5) 0.5968(2) 0.0524(19) Uani 1 1 d . . . H62A H 1.5262 -0.4083 0.6041 0.063 Uiso 1 1 calc R . . H62B H 1.6605 -0.3691 0.5698 0.063 Uiso 1 1 calc R . . C63 C 1.6626(7) -0.3961(5) 0.6844(2) 0.0462(17) Uani 1 1 d . . . H63 H 1.6005 -0.4495 0.6944 0.055 Uiso 1 1 calc R . . C64 C 1.8231(7) -0.2892(4) 0.6817(2) 0.0421(16) Uani 1 1 d . . . H64 H 1.8974 -0.2526 0.6915 0.050 Uiso 1 1 calc R . . N1 N 0.6925(6) 0.6224(4) 0.22401(18) 0.0460(14) Uani 1 1 d . . . N2 N 0.6063(6) 0.6516(4) 0.15104(18) 0.0418(13) Uani 1 1 d . . . N3 N 0.7032(7) 0.7252(4) 0.1513(2) 0.0628(17) Uani 1 1 d . . . N4 N -0.0330(6) 1.4730(4) -0.14286(18) 0.0433(13) Uani 1 1 d . . . N5 N -0.0255(6) 1.4030(4) -0.06608(18) 0.0436(14) Uani 1 1 d . . . N6 N 0.0872(6) 1.4667(4) -0.07322(19) 0.0520(15) Uani 1 1 d . . . N7 N 0.9091(6) 0.4601(4) 0.36882(18) 0.0469(14) Uani 1 1 d . . . N8 N 0.9326(6) 0.3907(4) 0.44517(18) 0.0448(14) Uani 1 1 d . . . N9 N 1.0422(6) 0.4555(4) 0.43507(19) 0.0501(15) Uani 1 1 d . . . N10 N 1.7575(6) -0.3654(4) 0.71221(18) 0.0443(14) Uani 1 1 d . . . N11 N 1.6675(6) -0.3405(4) 0.64037(18) 0.0412(13) Uani 1 1 d . . . N12 N 1.7733(6) -0.2713(4) 0.6375(2) 0.0506(15) Uani 1 1 d . . . O1 O 0.2528(5) 0.2991(3) 0.16403(17) 0.0567(13) Uani 1 1 d . . . O2 O 0.3718(5) 0.4390(3) 0.16826(16) 0.0495(11) Uani 1 1 d . . . O3 O 0.7383(6) 0.3697(3) 0.28755(17) 0.0605(13) Uani 1 1 d . . . O4 O 0.9325(6) 0.3626(4) 0.23391(18) 0.0701(15) Uani 1 1 d . . . O5 O 0.5526(5) 0.5705(3) 0.34599(17) 0.0591(13) Uani 1 1 d . . . O6 O 0.7152(5) 0.6872(3) 0.34407(18) 0.0612(14) Uani 1 1 d . . . O7 O 0.2053(6) 0.6409(4) 0.22416(19) 0.0681(15) Uani 1 1 d . . . O8 O 0.0164(5) 0.5744(3) 0.26467(15) 0.0502(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0429(3) 0.0369(3) 0.0389(3) 0.0009(2) -0.0099(2) 0.0038(2) Cd2 0.0401(3) 0.0380(3) 0.0329(3) 0.0015(2) -0.0094(2) 0.0000(2) C1 0.030(4) 0.043(4) 0.036(4) 0.003(3) -0.011(3) 0.001(3) C2 0.036(4) 0.055(4) 0.034(4) 0.005(3) -0.004(3) 0.000(3) C3 0.045(4) 0.033(3) 0.034(3) -0.004(3) -0.005(3) -0.005(3) C4 0.049(4) 0.050(4) 0.032(4) -0.007(3) 0.004(3) -0.010(3) C5 0.043(4) 0.048(4) 0.048(4) -0.012(3) 0.017(3) -0.008(3) C6 0.035(4) 0.039(4) 0.056(4) -0.004(3) 0.001(3) -0.002(3) C7 0.042(4) 0.027(3) 0.037(3) -0.006(3) 0.003(3) -0.004(3) C8 0.036(4) 0.026(3) 0.041(4) -0.003(3) 0.001(3) -0.003(3) C9 0.037(4) 0.048(4) 0.040(4) -0.007(3) 0.003(3) -0.011(3) C10 0.051(4) 0.031(3) 0.051(4) -0.012(3) 0.008(3) -0.011(3) C11 0.054(5) 0.039(4) 0.058(4) -0.017(3) -0.002(4) -0.001(3) C12 0.046(4) 0.032(3) 0.045(4) -0.001(3) 0.002(3) -0.005(3) C13 0.060(5) 0.032(3) 0.044(4) 0.004(3) -0.010(3) -0.001(3) C14 0.044(5) 0.039(4) 0.039(4) -0.006(3) -0.019(4) 0.000(3) C15 0.049(5) 0.051(4) 0.037(4) -0.006(3) -0.014(4) 0.006(4) C16 0.056(5) 0.059(4) 0.040(4) -0.013(3) -0.009(4) 0.005(4) C17 0.044(4) 0.036(4) 0.042(4) -0.008(3) -0.003(3) 0.003(3) C18 0.048(5) 0.054(4) 0.054(4) -0.024(3) -0.004(4) -0.001(3) C19 0.056(5) 0.035(4) 0.060(5) -0.021(3) -0.007(4) 0.008(3) C20 0.061(5) 0.036(4) 0.085(6) -0.005(4) -0.009(4) -0.008(4) C21 0.044(4) 0.041(4) 0.052(4) 0.006(3) 0.008(3) -0.011(3) C22 0.045(4) 0.040(4) 0.061(4) -0.015(3) 0.001(4) -0.013(3) C23 0.036(4) 0.032(3) 0.044(4) -0.006(3) 0.001(3) 0.000(3) C24 0.033(4) 0.027(3) 0.038(3) -0.005(3) -0.001(3) -0.002(3) C25 0.043(4) 0.039(4) 0.057(4) -0.009(3) -0.004(4) 0.009(3) C26 0.051(5) 0.047(4) 0.040(4) 0.003(3) -0.002(3) -0.005(3) C27 0.041(4) 0.044(4) 0.072(5) -0.010(3) -0.005(4) -0.006(3) C28 0.046(5) 0.034(4) 0.045(4) -0.006(3) -0.015(4) -0.005(3) C29 0.049(5) 0.042(4) 0.042(4) -0.001(3) -0.016(3) -0.007(3) C30 0.060(5) 0.041(4) 0.066(5) 0.012(4) -0.034(4) -0.013(4) C31 0.056(5) 0.051(4) 0.039(4) 0.003(3) -0.021(4) -0.005(3) C32 0.041(4) 0.041(4) 0.038(4) -0.002(3) -0.011(3) -0.005(3) C33 0.069(5) 0.055(4) 0.032(4) 0.008(3) -0.010(4) -0.003(4) C34 0.055(5) 0.050(4) 0.035(4) 0.003(3) -0.002(3) 0.006(3) C35 0.044(4) 0.041(4) 0.029(3) 0.002(3) -0.009(3) -0.001(3) C36 0.053(5) 0.052(4) 0.033(4) 0.005(3) -0.003(3) -0.003(3) C37 0.047(4) 0.044(4) 0.042(4) -0.004(3) -0.005(3) 0.003(3) C38 0.041(4) 0.049(4) 0.032(4) 0.007(3) -0.009(3) -0.004(3) C39 0.047(4) 0.047(4) 0.032(4) 0.008(3) -0.010(3) -0.003(3) C40 0.055(5) 0.047(4) 0.037(4) -0.006(3) -0.002(3) -0.005(3) C41 0.053(5) 0.047(4) 0.036(4) 0.012(3) -0.002(3) -0.001(3) C42 0.089(6) 0.057(5) 0.036(4) -0.004(3) -0.025(4) 0.009(4) C43 0.094(6) 0.044(4) 0.036(4) -0.006(3) -0.018(4) 0.009(4) C44 0.061(5) 0.058(4) 0.040(4) 0.014(3) 0.003(4) 0.010(4) C45 0.046(5) 0.046(4) 0.055(4) 0.014(3) -0.020(4) -0.004(3) C46 0.054(5) 0.038(4) 0.045(4) 0.002(3) -0.008(4) -0.006(3) C47 0.054(5) 0.038(4) 0.056(5) 0.000(3) -0.004(4) -0.008(3) C48 0.043(5) 0.052(4) 0.056(4) 0.003(4) -0.006(4) -0.006(3) C49 0.062(5) 0.063(5) 0.038(4) 0.009(3) -0.003(4) -0.001(4) C50 0.053(5) 0.049(4) 0.034(4) 0.011(3) -0.006(3) -0.002(3) C51 0.078(6) 0.058(5) 0.034(4) 0.002(3) -0.020(4) 0.008(4) C52 0.090(6) 0.050(4) 0.034(4) -0.001(3) -0.023(4) 0.012(4) C53 0.044(4) 0.050(4) 0.036(4) 0.013(3) -0.005(3) -0.001(3) C54 0.049(5) 0.071(5) 0.029(4) 0.002(3) -0.005(3) -0.004(4) C55 0.073(5) 0.050(4) 0.040(4) -0.006(3) -0.006(4) -0.002(4) C56 0.049(5) 0.061(4) 0.027(4) 0.009(3) -0.007(3) -0.002(4) C57 0.078(6) 0.056(4) 0.030(4) 0.011(3) -0.009(4) 0.004(4) C58 0.074(6) 0.056(4) 0.034(4) -0.001(3) -0.004(4) 0.003(4) C59 0.039(4) 0.056(4) 0.039(4) 0.005(3) -0.015(3) -0.002(3) C60 0.066(6) 0.094(6) 0.033(4) 0.021(4) -0.006(4) 0.013(5) C61 0.063(5) 0.080(5) 0.041(4) 0.008(4) 0.005(4) 0.019(4) C62 0.060(5) 0.048(4) 0.049(4) 0.004(3) -0.019(4) -0.006(4) C63 0.046(5) 0.055(4) 0.034(4) 0.015(3) -0.010(3) -0.004(3) C64 0.048(4) 0.032(4) 0.048(4) -0.004(3) -0.019(4) 0.001(3) N1 0.053(4) 0.038(3) 0.046(3) 0.002(3) -0.016(3) 0.001(3) N2 0.049(4) 0.033(3) 0.044(3) 0.004(2) -0.014(3) -0.007(3) N3 0.071(5) 0.052(4) 0.068(4) 0.011(3) -0.028(4) -0.018(3) N4 0.049(4) 0.040(3) 0.040(3) 0.006(2) -0.012(3) -0.003(3) N5 0.049(4) 0.045(3) 0.033(3) 0.009(2) -0.008(3) 0.000(3) N6 0.059(4) 0.061(4) 0.040(3) -0.001(3) -0.015(3) -0.017(3) N7 0.048(4) 0.046(3) 0.044(3) 0.005(3) -0.015(3) 0.005(3) N8 0.049(4) 0.045(3) 0.039(3) 0.001(2) -0.017(3) 0.004(3) N9 0.060(4) 0.051(3) 0.041(3) -0.004(3) -0.016(3) -0.007(3) N10 0.044(4) 0.045(3) 0.041(3) 0.007(3) -0.015(3) 0.004(3) N11 0.039(3) 0.043(3) 0.040(3) 0.006(2) -0.016(3) 0.001(3) N12 0.055(4) 0.041(3) 0.056(4) 0.007(3) -0.020(3) -0.006(3) O1 0.043(3) 0.053(3) 0.076(3) -0.016(2) 0.006(3) -0.011(2) O2 0.042(3) 0.043(3) 0.063(3) -0.011(2) -0.003(2) -0.002(2) O3 0.076(4) 0.045(3) 0.061(3) -0.011(2) -0.007(3) -0.003(3) O4 0.058(4) 0.083(4) 0.074(4) 0.008(3) -0.007(3) -0.037(3) O5 0.060(3) 0.034(3) 0.082(4) -0.010(2) -0.005(3) -0.001(2) O6 0.046(3) 0.051(3) 0.088(4) -0.021(3) -0.007(3) 0.004(3) O7 0.059(4) 0.063(3) 0.086(4) -0.031(3) 0.026(3) -0.021(3) O8 0.053(3) 0.040(3) 0.058(3) -0.006(2) -0.007(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O3 2.240(4) . ? Cd1 O8 2.286(5) 1_655 ? Cd1 N1 2.327(5) . ? Cd1 O6 2.355(4) . ? Cd1 N7 2.369(5) . ? Cd1 O5 2.411(5) . ? Cd2 O2 2.311(4) . ? Cd2 O4 2.317(5) 1_455 ? Cd2 N10 2.318(4) 2_756 ? Cd2 O8 2.342(4) . ? Cd2 N4 2.344(4) 2_575 ? Cd2 O1 2.470(4) . ? Cd2 O7 2.584(4) . ? C1 O1 1.233(7) . ? C1 O2 1.257(7) . ? C1 C2 1.531(8) . ? C2 C3 1.524(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.522(8) . ? C3 C8 1.536(7) . ? C3 C9 1.537(7) . ? C4 C5 1.544(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.520(8) . ? C5 C11 1.539(8) . ? C5 H5 0.9800 . ? C6 C7 1.556(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C13 1.534(7) . ? C7 C8 1.535(7) . ? C7 C12 1.538(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.540(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.530(8) . ? C10 C12 1.536(8) . ? C10 H10 0.9800 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.516(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 O4 1.226(7) . ? C14 O3 1.253(7) . ? C15 O6 1.248(7) . ? C15 O5 1.259(7) . ? C15 C16 1.544(8) . ? C16 C17 1.520(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C23 1.529(7) . ? C17 C22 1.539(8) . ? C17 C18 1.541(8) . ? C18 C19 1.527(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.516(9) . ? C19 C25 1.528(8) . ? C19 H19 0.9800 . ? C20 C21 1.523(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C26 1.510(8) . ? C21 C22 1.524(8) . ? C21 H21 0.9800 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.524(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C27 1.521(7) . ? C24 C26 1.525(8) . ? C24 C25 1.533(7) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.519(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 O7 1.224(7) . ? C28 O8 1.286(7) . ? C29 N1 1.315(7) . ? C29 N2 1.327(7) . ? C29 H29 0.9300 . ? C30 N3 1.324(7) . ? C30 N1 1.364(7) . ? C30 H30 0.9300 . ? C31 N2 1.465(7) . ? C31 C32 1.505(7) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.364(8) . ? C32 C37 1.390(8) . ? C33 C34 1.376(7) . ? C33 H33 0.9300 . ? C34 C35 1.392(7) . ? C34 H34 0.9300 . ? C35 C36 1.387(8) . ? C35 C38 1.479(7) . ? C36 C37 1.378(7) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.379(8) . ? C38 C43 1.382(8) . ? C39 C40 1.386(7) . ? C39 H39 0.9300 . ? C40 C41 1.403(8) . ? C40 H40 0.9300 . ? C41 C42 1.372(8) . ? C41 C44 1.528(8) . ? C42 C43 1.383(8) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 N5 1.464(7) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 N4 1.310(7) . ? C45 N5 1.339(7) . ? C45 H45 0.9300 . ? C46 N6 1.315(7) . ? C46 N4 1.348(7) . ? C46 H46 0.9300 . ? C47 N9 1.310(7) . ? C47 N7 1.346(7) . ? C47 H47 0.9300 . ? C48 N7 1.312(7) . ? C48 N8 1.317(7) . ? C48 H48 0.9300 . ? C49 N8 1.456(7) . ? C49 C50 1.502(8) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C55 1.367(8) . ? C50 C51 1.379(8) . ? C51 C52 1.361(8) . ? C51 H51 0.9300 . ? C52 C53 1.389(8) . ? C52 H52 0.9300 . ? C53 C54 1.382(8) . ? C53 C56 1.487(8) . ? C54 C55 1.376(8) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 C61 1.382(8) . ? C56 C57 1.388(9) . ? C57 C58 1.388(8) . ? C57 H57 0.9300 . ? C58 C59 1.396(8) . ? C58 H58 0.9300 . ? C59 C60 1.363(9) . ? C59 C62 1.522(8) . ? C60 C61 1.402(8) . ? C60 H60 0.9300 . ? C61 H61 0.9300 . ? C62 N11 1.456(7) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 N10 1.308(7) . ? C63 N11 1.318(7) . ? C63 H63 0.9300 . ? C64 N12 1.305(7) . ? C64 N10 1.355(7) . ? C64 H64 0.9300 . ? N2 N3 1.349(7) . ? N4 Cd2 2.344(4) 2_575 ? N5 N6 1.362(7) . ? N8 N9 1.352(7) . ? N10 Cd2 2.318(4) 2_756 ? N11 N12 1.362(6) . ? O4 Cd2 2.317(5) 1_655 ? O8 Cd1 2.286(5) 1_455 ? 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 Cd1 O8 113.27(16) . 1_655 ? O3 Cd1 N1 96.81(17) . . ? O8 Cd1 N1 87.24(17) 1_655 . ? O3 Cd1 O6 143.97(19) . . ? O8 Cd1 O6 100.88(16) 1_655 . ? N1 Cd1 O6 95.90(17) . . ? O3 Cd1 N7 87.07(17) . . ? O8 Cd1 N7 85.75(17) 1_655 . ? N1 Cd1 N7 172.9(2) . . ? O6 Cd1 N7 84.26(17) . . ? O3 Cd1 O5 90.68(17) . . ? O8 Cd1 O5 155.65(15) 1_655 . ? N1 Cd1 O5 94.48(17) . . ? O6 Cd1 O5 54.77(15) . . ? N7 Cd1 O5 91.42(17) . . ? O2 Cd2 O4 144.26(17) . 1_455 ? O2 Cd2 N10 95.85(17) . 2_756 ? O4 Cd2 N10 89.99(17) 1_455 2_756 ? O2 Cd2 O8 133.65(15) . . ? O4 Cd2 O8 81.94(17) 1_455 . ? N10 Cd2 O8 84.71(16) 2_756 . ? O2 Cd2 N4 87.81(17) . 2_575 ? O4 Cd2 N4 86.35(17) 1_455 2_575 ? N10 Cd2 N4 176.16(19) 2_756 2_575 ? O8 Cd2 N4 93.62(16) . 2_575 ? O2 Cd2 O1 54.19(14) . . ? O4 Cd2 O1 90.20(17) 1_455 . ? N10 Cd2 O1 95.44(16) 2_756 . ? O8 Cd2 O1 172.14(15) . . ? N4 Cd2 O1 85.75(16) 2_575 . ? O2 Cd2 O7 82.20(15) . . ? O4 Cd2 O7 132.22(17) 1_455 . ? N10 Cd2 O7 96.46(17) 2_756 . ? O8 Cd2 O7 51.90(15) . . ? N4 Cd2 O7 85.17(17) 2_575 . ? O1 Cd2 O7 135.70(15) . . ? O1 C1 O2 122.4(6) . . ? O1 C1 C2 120.1(6) . . ? O2 C1 C2 117.4(6) . . ? C3 C2 C1 115.7(5) . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2B 108.4 . . ? C1 C2 H2B 108.4 . . ? H2A C2 H2B 107.4 . . ? C4 C3 C2 108.2(5) . . ? C4 C3 C8 108.9(5) . . ? C2 C3 C8 110.8(4) . . ? C4 C3 C9 108.7(5) . . ? C2 C3 C9 111.6(5) . . ? C8 C3 C9 108.6(4) . . ? C3 C4 C5 110.9(5) . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? C5 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C6 C5 C11 109.6(5) . . ? C6 C5 C4 109.5(5) . . ? C11 C5 C4 109.1(5) . . ? C6 C5 H5 109.6 . . ? C11 C5 H5 109.6 . . ? C4 C5 H5 109.6 . . ? C5 C6 C7 110.0(5) . . ? C5 C6 H6A 109.7 . . ? C7 C6 H6A 109.7 . . ? C5 C6 H6B 109.7 . . ? C7 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C13 C7 C8 112.1(4) . . ? C13 C7 C12 108.4(5) . . ? C8 C7 C12 107.0(5) . . ? C13 C7 C6 111.6(5) . . ? C8 C7 C6 109.0(4) . . ? C12 C7 C6 108.5(5) . . ? C7 C8 C3 112.1(4) . . ? C7 C8 H8A 109.2 . . ? C3 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C3 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C3 C9 C10 109.6(5) . . ? C3 C9 H9A 109.8 . . ? C10 C9 H9A 109.8 . . ? C3 C9 H9B 109.8 . . ? C10 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C12 108.3(5) . . ? C11 C10 C9 109.8(5) . . ? C12 C10 C9 110.0(5) . . ? C11 C10 H10 109.6 . . ? C12 C10 H10 109.6 . . ? C9 C10 H10 109.6 . . ? C10 C11 C5 109.6(5) . . ? C10 C11 H11A 109.7 . . ? C5 C11 H11A 109.7 . . ? C10 C11 H11B 109.7 . . ? C5 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C10 C12 C7 111.1(5) . . ? C10 C12 H12A 109.4 . . ? C7 C12 H12A 109.4 . . ? C10 C12 H12B 109.4 . . ? C7 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C7 115.7(5) . . ? C14 C13 H13A 108.4 . . ? C7 C13 H13A 108.4 . . ? C14 C13 H13B 108.4 . . ? C7 C13 H13B 108.4 . . ? H13A C13 H13B 107.4 . . ? O4 C14 O3 124.4(6) . . ? O4 C14 C13 120.0(6) . . ? O3 C14 C13 115.6(6) . . ? O6 C15 O5 122.0(6) . . ? O6 C15 C16 119.2(6) . . ? O5 C15 C16 118.6(7) . . ? C17 C16 C15 113.3(5) . . ? C17 C16 H16A 108.9 . . ? C15 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? C15 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C16 C17 C23 111.3(5) . . ? C16 C17 C22 112.1(5) . . ? C23 C17 C22 108.5(5) . . ? C16 C17 C18 108.6(5) . . ? C23 C17 C18 107.9(5) . . ? C22 C17 C18 108.2(5) . . ? C19 C18 C17 110.5(5) . . ? C19 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C18 110.4(6) . . ? C20 C19 C25 109.2(5) . . ? C18 C19 C25 108.0(5) . . ? C20 C19 H19 109.7 . . ? C18 C19 H19 109.7 . . ? C25 C19 H19 109.7 . . ? C19 C20 C21 109.4(5) . . ? C19 C20 H20A 109.8 . . ? C21 C20 H20A 109.8 . . ? C19 C20 H20B 109.8 . . ? C21 C20 H20B 109.8 . . ? H20A C20 H20B 108.2 . . ? C26 C21 C20 110.6(5) . . ? C26 C21 C22 108.6(5) . . ? C20 C21 C22 109.6(5) . . ? C26 C21 H21 109.3 . . ? C20 C21 H21 109.3 . . ? C22 C21 H21 109.3 . . ? C21 C22 C17 110.7(5) . . ? C21 C22 H22A 109.5 . . ? C17 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C17 111.5(4) . . ? C24 C23 H23A 109.3 . . ? C17 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? C17 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C27 C24 C23 111.0(4) . . ? C27 C24 C26 112.4(5) . . ? C23 C24 C26 109.1(5) . . ? C27 C24 C25 108.1(5) . . ? C23 C24 C25 107.7(5) . . ? C26 C24 C25 108.5(5) . . ? C19 C25 C24 111.3(5) . . ? C19 C25 H25A 109.4 . . ? C24 C25 H25A 109.4 . . ? C19 C25 H25B 109.4 . . ? C24 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C21 C26 C24 110.7(5) . . ? C21 C26 H26A 109.5 . . ? C24 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C28 C27 C24 117.8(5) . . ? C28 C27 H27A 107.8 . . ? C24 C27 H27A 107.8 . . ? C28 C27 H27B 107.8 . . ? C24 C27 H27B 107.8 . . ? H27A C27 H27B 107.2 . . ? O7 C28 O8 119.3(6) . . ? O7 C28 C27 125.0(6) . . ? O8 C28 C27 115.6(6) . . ? N1 C29 N2 110.4(5) . . ? N1 C29 H29 124.8 . . ? N2 C29 H29 124.8 . . ? N3 C30 N1 112.8(6) . . ? N3 C30 H30 123.6 . . ? N1 C30 H30 123.6 . . ? N2 C31 C32 111.2(5) . . ? N2 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? N2 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C33 C32 C37 118.1(6) . . ? C33 C32 C31 121.5(5) . . ? C37 C32 C31 120.4(6) . . ? C32 C33 C34 121.8(6) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C33 C34 C35 120.6(6) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C36 C35 C34 117.7(6) . . ? C36 C35 C38 120.8(5) . . ? C34 C35 C38 121.5(6) . . ? C37 C36 C35 121.0(6) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C36 C37 C32 120.8(6) . . ? C36 C37 H37 119.6 . . ? C32 C37 H37 119.6 . . ? C39 C38 C43 118.0(6) . . ? C39 C38 C35 122.6(5) . . ? C43 C38 C35 119.4(6) . . ? C38 C39 C40 120.6(5) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C41 121.0(6) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C42 C41 C40 118.0(6) . . ? C42 C41 C44 121.2(6) . . ? C40 C41 C44 120.7(6) . . ? C41 C42 C43 120.5(6) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C38 C43 C42 121.9(6) . . ? C38 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? N5 C44 C41 113.7(5) . . ? N5 C44 H44A 108.8 . . ? C41 C44 H44A 108.8 . . ? N5 C44 H44B 108.8 . . ? C41 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? N4 C45 N5 110.6(6) . . ? N4 C45 H45 124.7 . . ? N5 C45 H45 124.7 . . ? N6 C46 N4 115.3(6) . . ? N6 C46 H46 122.3 . . ? N4 C46 H46 122.3 . . ? N9 C47 N7 115.0(6) . . ? N9 C47 H47 122.5 . . ? N7 C47 H47 122.5 . . ? N7 C48 N8 111.9(6) . . ? N7 C48 H48 124.1 . . ? N8 C48 H48 124.1 . . ? N8 C49 C50 114.2(5) . . ? N8 C49 H49A 108.7 . . ? C50 C49 H49A 108.7 . . ? N8 C49 H49B 108.7 . . ? C50 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? C55 C50 C51 117.7(6) . . ? C55 C50 C49 120.1(6) . . ? C51 C50 C49 122.1(6) . . ? C52 C51 C50 122.1(6) . . ? C52 C51 H51 118.9 . . ? C50 C51 H51 118.9 . . ? C51 C52 C53 120.1(6) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C54 C53 C52 117.9(6) . . ? C54 C53 C56 121.6(6) . . ? C52 C53 C56 120.5(6) . . ? C55 C54 C53 120.9(6) . . ? C55 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C50 C55 C54 121.1(6) . . ? C50 C55 H55 119.4 . . ? C54 C55 H55 119.4 . . ? C61 C56 C57 117.1(6) . . ? C61 C56 C53 120.6(6) . . ? C57 C56 C53 122.3(5) . . ? C58 C57 C56 122.5(6) . . ? C58 C57 H57 118.8 . . ? C56 C57 H57 118.8 . . ? C57 C58 C59 119.9(6) . . ? C57 C58 H58 120.1 . . ? C59 C58 H58 120.1 . . ? C60 C59 C58 117.9(6) . . ? C60 C59 C62 121.8(6) . . ? C58 C59 C62 120.2(6) . . ? C59 C60 C61 122.1(6) . . ? C59 C60 H60 118.9 . . ? C61 C60 H60 118.9 . . ? C56 C61 C60 120.5(7) . . ? C56 C61 H61 119.7 . . ? C60 C61 H61 119.7 . . ? N11 C62 C59 112.3(5) . . ? N11 C62 H62A 109.1 . . ? C59 C62 H62A 109.1 . . ? N11 C62 H62B 109.1 . . ? C59 C62 H62B 109.1 . . ? H62A C62 H62B 107.9 . . ? N10 C63 N11 110.3(6) . . ? N10 C63 H63 124.9 . . ? N11 C63 H63 124.9 . . ? N12 C64 N10 114.4(6) . . ? N12 C64 H64 122.8 . . ? N10 C64 H64 122.8 . . ? C29 N1 C30 103.6(5) . . ? C29 N1 Cd1 131.3(4) . . ? C30 N1 Cd1 123.5(4) . . ? C29 N2 N3 109.7(5) . . ? C29 N2 C31 129.0(5) . . ? N3 N2 C31 121.3(5) . . ? C30 N3 N2 103.6(5) . . ? C45 N4 C46 102.8(5) . . ? C45 N4 Cd2 124.9(4) . 2_575 ? C46 N4 Cd2 128.8(4) . 2_575 ? C45 N5 N6 109.3(5) . . ? C45 N5 C44 128.1(6) . . ? N6 N5 C44 122.5(5) . . ? C46 N6 N5 102.0(5) . . ? C48 N7 C47 101.7(5) . . ? C48 N7 Cd1 127.3(5) . . ? C47 N7 Cd1 128.3(4) . . ? C48 N8 N9 108.7(5) . . ? C48 N8 C49 129.7(6) . . ? N9 N8 C49 121.6(5) . . ? C47 N9 N8 102.7(5) . . ? C63 N10 C64 103.2(5) . . ? C63 N10 Cd2 131.0(4) . 2_756 ? C64 N10 Cd2 123.5(4) . 2_756 ? C63 N11 N12 109.9(5) . . ? C63 N11 C62 130.0(6) . . ? N12 N11 C62 119.9(5) . . ? C64 N12 N11 102.2(5) . . ? C1 O1 Cd2 88.3(4) . . ? C1 O2 Cd2 95.1(4) . . ? C14 O3 Cd1 113.5(4) . . ? C14 O4 Cd2 158.3(4) . 1_655 ? C15 O5 Cd1 90.0(4) . . ? C15 O6 Cd1 92.9(4) . . ? C28 O7 Cd2 89.4(4) . . ? C28 O8 Cd1 141.9(4) . 1_455 ? C28 O8 Cd2 99.3(4) . . ? Cd1 O8 Cd2 116.23(17) 1_455 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -78.9(7) . . . . ? O2 C1 C2 C3 100.0(6) . . . . ? C1 C2 C3 C4 -169.3(5) . . . . ? C1 C2 C3 C8 -50.0(7) . . . . ? C1 C2 C3 C9 71.2(7) . . . . ? C2 C3 C4 C5 178.7(5) . . . . ? C8 C3 C4 C5 58.2(6) . . . . ? C9 C3 C4 C5 -60.0(6) . . . . ? C3 C4 C5 C6 -60.6(6) . . . . ? C3 C4 C5 C11 59.4(6) . . . . ? C11 C5 C6 C7 -60.0(6) . . . . ? C4 C5 C6 C7 59.6(6) . . . . ? C5 C6 C7 C13 177.6(4) . . . . ? C5 C6 C7 C8 -58.0(6) . . . . ? C5 C6 C7 C12 58.2(6) . . . . ? C13 C7 C8 C3 -178.6(5) . . . . ? C12 C7 C8 C3 -59.8(6) . . . . ? C6 C7 C8 C3 57.3(6) . . . . ? C4 C3 C8 C7 -57.6(6) . . . . ? C2 C3 C8 C7 -176.4(5) . . . . ? C9 C3 C8 C7 60.7(6) . . . . ? C4 C3 C9 C10 60.0(6) . . . . ? C2 C3 C9 C10 179.2(5) . . . . ? C8 C3 C9 C10 -58.4(6) . . . . ? C3 C9 C10 C11 -60.5(6) . . . . ? C3 C9 C10 C12 58.7(6) . . . . ? C12 C10 C11 C5 -60.4(6) . . . . ? C9 C10 C11 C5 59.7(6) . . . . ? C6 C5 C11 C10 61.4(7) . . . . ? C4 C5 C11 C10 -58.5(6) . . . . ? C11 C10 C12 C7 60.3(6) . . . . ? C9 C10 C12 C7 -59.7(6) . . . . ? C13 C7 C12 C10 179.8(5) . . . . ? C8 C7 C12 C10 58.7(6) . . . . ? C6 C7 C12 C10 -58.8(6) . . . . ? C8 C7 C13 C14 -36.8(8) . . . . ? C12 C7 C13 C14 -154.7(5) . . . . ? C6 C7 C13 C14 85.9(6) . . . . ? C7 C13 C14 O4 -70.3(8) . . . . ? C7 C13 C14 O3 109.7(6) . . . . ? O6 C15 C16 C17 92.1(7) . . . . ? O5 C15 C16 C17 -83.7(7) . . . . ? C15 C16 C17 C23 74.0(7) . . . . ? C15 C16 C17 C22 -47.7(7) . . . . ? C15 C16 C17 C18 -167.3(6) . . . . ? C16 C17 C18 C19 179.5(5) . . . . ? C23 C17 C18 C19 -59.8(7) . . . . ? C22 C17 C18 C19 57.5(7) . . . . ? C17 C18 C19 C20 -59.1(7) . . . . ? C17 C18 C19 C25 60.2(7) . . . . ? C18 C19 C20 C21 59.6(7) . . . . ? C25 C19 C20 C21 -59.0(7) . . . . ? C19 C20 C21 C26 59.7(7) . . . . ? C19 C20 C21 C22 -60.0(7) . . . . ? C26 C21 C22 C17 -60.5(6) . . . . ? C20 C21 C22 C17 60.4(6) . . . . ? C16 C17 C22 C21 -178.3(5) . . . . ? C23 C17 C22 C21 58.4(6) . . . . ? C18 C17 C22 C21 -58.5(6) . . . . ? C16 C17 C23 C24 179.0(5) . . . . ? C22 C17 C23 C24 -57.2(6) . . . . ? C18 C17 C23 C24 59.9(6) . . . . ? C17 C23 C24 C27 -177.8(5) . . . . ? C17 C23 C24 C26 57.8(6) . . . . ? C17 C23 C24 C25 -59.6(6) . . . . ? C20 C19 C25 C24 59.5(7) . . . . ? C18 C19 C25 C24 -60.6(7) . . . . ? C27 C24 C25 C19 179.9(5) . . . . ? C23 C24 C25 C19 59.8(6) . . . . ? C26 C24 C25 C19 -58.0(6) . . . . ? C20 C21 C26 C24 -59.4(7) . . . . ? C22 C21 C26 C24 60.8(7) . . . . ? C27 C24 C26 C21 177.0(5) . . . . ? C23 C24 C26 C21 -59.5(6) . . . . ? C25 C24 C26 C21 57.5(6) . . . . ? C23 C24 C27 C28 -53.1(7) . . . . ? C26 C24 C27 C28 69.4(7) . . . . ? C25 C24 C27 C28 -170.9(5) . . . . ? C24 C27 C28 O7 -40.9(9) . . . . ? C24 C27 C28 O8 140.4(6) . . . . ? N2 C31 C32 C33 -53.3(8) . . . . ? N2 C31 C32 C37 125.7(6) . . . . ? C37 C32 C33 C34 0.2(10) . . . . ? C31 C32 C33 C34 179.1(6) . . . . ? C32 C33 C34 C35 0.5(10) . . . . ? C33 C34 C35 C36 -0.3(9) . . . . ? C33 C34 C35 C38 178.2(6) . . . . ? C34 C35 C36 C37 -0.6(10) . . . . ? C38 C35 C36 C37 -179.2(5) . . . . ? C35 C36 C37 C32 1.3(10) . . . . ? C33 C32 C37 C36 -1.1(9) . . . . ? C31 C32 C37 C36 179.9(5) . . . . ? C36 C35 C38 C39 -138.1(7) . . . . ? C34 C35 C38 C39 43.4(9) . . . . ? C36 C35 C38 C43 45.1(9) . . . . ? C34 C35 C38 C43 -133.5(7) . . . . ? C43 C38 C39 C40 1.8(9) . . . . ? C35 C38 C39 C40 -175.1(5) . . . . ? C38 C39 C40 C41 1.0(9) . . . . ? C39 C40 C41 C42 -3.5(10) . . . . ? C39 C40 C41 C44 171.5(6) . . . . ? C40 C41 C42 C43 3.1(11) . . . . ? C44 C41 C42 C43 -171.9(6) . . . . ? C39 C38 C43 C42 -2.2(10) . . . . ? C35 C38 C43 C42 174.8(6) . . . . ? C41 C42 C43 C38 -0.3(11) . . . . ? C42 C41 C44 N5 -62.6(9) . . . . ? C40 C41 C44 N5 122.6(7) . . . . ? N8 C49 C50 C55 128.9(7) . . . . ? N8 C49 C50 C51 -55.1(9) . . . . ? C55 C50 C51 C52 2.7(11) . . . . ? C49 C50 C51 C52 -173.4(6) . . . . ? C50 C51 C52 C53 0.3(11) . . . . ? C51 C52 C53 C54 -2.9(10) . . . . ? C51 C52 C53 C56 176.3(6) . . . . ? C52 C53 C54 C55 2.6(10) . . . . ? C56 C53 C54 C55 -176.6(6) . . . . ? C51 C50 C55 C54 -3.1(10) . . . . ? C49 C50 C55 C54 173.1(6) . . . . ? C53 C54 C55 C50 0.4(10) . . . . ? C54 C53 C56 C61 32.9(10) . . . . ? C52 C53 C56 C61 -146.3(7) . . . . ? C54 C53 C56 C57 -148.1(7) . . . . ? C52 C53 C56 C57 32.8(10) . . . . ? C61 C56 C57 C58 -0.5(11) . . . . ? C53 C56 C57 C58 -179.6(6) . . . . ? C56 C57 C58 C59 0.6(11) . . . . ? C57 C58 C59 C60 -1.2(10) . . . . ? C57 C58 C59 C62 179.9(6) . . . . ? C58 C59 C60 C61 1.8(11) . . . . ? C62 C59 C60 C61 -179.3(6) . . . . ? C57 C56 C61 C60 1.0(11) . . . . ? C53 C56 C61 C60 -179.9(6) . . . . ? C59 C60 C61 C56 -1.8(12) . . . . ? C60 C59 C62 N11 -42.7(9) . . . . ? C58 C59 C62 N11 136.1(6) . . . . ? N2 C29 N1 C30 0.5(7) . . . . ? N2 C29 N1 Cd1 -164.9(4) . . . . ? N3 C30 N1 C29 -0.2(8) . . . . ? N3 C30 N1 Cd1 166.6(5) . . . . ? O3 Cd1 N1 C29 18.9(6) . . . . ? O8 Cd1 N1 C29 132.0(6) 1_655 . . . ? O6 Cd1 N1 C29 -127.3(6) . . . . ? N7 Cd1 N1 C29 141.7(13) . . . . ? O5 Cd1 N1 C29 -72.3(6) . . . . ? O3 Cd1 N1 C30 -143.9(5) . . . . ? O8 Cd1 N1 C30 -30.8(5) 1_655 . . . ? O6 Cd1 N1 C30 69.8(5) . . . . ? N7 Cd1 N1 C30 -21.1(17) . . . . ? O5 Cd1 N1 C30 124.8(5) . . . . ? N1 C29 N2 N3 -0.6(8) . . . . ? N1 C29 N2 C31 176.9(6) . . . . ? C32 C31 N2 C29 128.7(7) . . . . ? C32 C31 N2 N3 -54.1(8) . . . . ? N1 C30 N3 N2 -0.1(8) . . . . ? C29 N2 N3 C30 0.4(8) . . . . ? C31 N2 N3 C30 -177.3(6) . . . . ? N5 C45 N4 C46 -0.5(7) . . . . ? N5 C45 N4 Cd2 -160.9(4) . . . 2_575 ? N6 C46 N4 C45 1.0(8) . . . . ? N6 C46 N4 Cd2 160.4(4) . . . 2_575 ? N4 C45 N5 N6 -0.2(8) . . . . ? N4 C45 N5 C44 174.9(6) . . . . ? C41 C44 N5 C45 111.6(7) . . . . ? C41 C44 N5 N6 -73.9(8) . . . . ? N4 C46 N6 N5 -1.1(8) . . . . ? C45 N5 N6 C46 0.7(7) . . . . ? C44 N5 N6 C46 -174.7(5) . . . . ? N8 C48 N7 C47 0.9(7) . . . . ? N8 C48 N7 Cd1 -161.7(4) . . . . ? N9 C47 N7 C48 -0.2(8) . . . . ? N9 C47 N7 Cd1 162.1(4) . . . . ? O3 Cd1 N7 C48 -50.0(6) . . . . ? O8 Cd1 N7 C48 -163.7(6) 1_655 . . . ? N1 Cd1 N7 C48 -173.4(12) . . . . ? O6 Cd1 N7 C48 94.9(6) . . . . ? O5 Cd1 N7 C48 40.6(6) . . . . ? O3 Cd1 N7 C47 151.8(6) . . . . ? O8 Cd1 N7 C47 38.2(5) 1_655 . . . ? N1 Cd1 N7 C47 28.5(17) . . . . ? O6 Cd1 N7 C47 -63.2(6) . . . . ? O5 Cd1 N7 C47 -117.6(6) . . . . ? N7 C48 N8 N9 -1.3(8) . . . . ? N7 C48 N8 C49 176.9(6) . . . . ? C50 C49 N8 C48 109.1(8) . . . . ? C50 C49 N8 N9 -72.9(8) . . . . ? N7 C47 N9 N8 -0.5(8) . . . . ? C48 N8 N9 C47 1.0(7) . . . . ? C49 N8 N9 C47 -177.3(6) . . . . ? N11 C63 N10 C64 -1.3(7) . . . . ? N11 C63 N10 Cd2 -164.1(4) . . . 2_756 ? N12 C64 N10 C63 0.5(8) . . . . ? N12 C64 N10 Cd2 164.9(4) . . . 2_756 ? N10 C63 N11 N12 1.8(8) . . . . ? N10 C63 N11 C62 176.6(6) . . . . ? C59 C62 N11 C63 120.3(7) . . . . ? C59 C62 N11 N12 -65.3(7) . . . . ? N10 C64 N12 N11 0.5(7) . . . . ? C63 N11 N12 C64 -1.4(7) . . . . ? C62 N11 N12 C64 -176.8(5) . . . . ? O2 C1 O1 Cd2 0.9(6) . . . . ? C2 C1 O1 Cd2 179.7(4) . . . . ? O2 Cd2 O1 C1 -0.5(3) . . . . ? O4 Cd2 O1 C1 176.2(3) 1_455 . . . ? N10 Cd2 O1 C1 -93.8(4) 2_756 . . . ? O8 Cd2 O1 C1 175.5(9) . . . . ? N4 Cd2 O1 C1 89.9(4) 2_575 . . . ? O7 Cd2 O1 C1 11.2(4) . . . . ? O1 C1 O2 Cd2 -0.9(6) . . . . ? C2 C1 O2 Cd2 -179.8(4) . . . . ? O4 Cd2 O2 C1 -5.2(5) 1_455 . . . ? N10 Cd2 O2 C1 93.0(4) 2_756 . . . ? O8 Cd2 O2 C1 -178.8(3) . . . . ? N4 Cd2 O2 C1 -85.9(3) 2_575 . . . ? O1 Cd2 O2 C1 0.5(3) . . . . ? O7 Cd2 O2 C1 -171.3(4) . . . . ? O4 C14 O3 Cd1 -11.2(8) . . . . ? C13 C14 O3 Cd1 168.8(4) . . . . ? O8 Cd1 O3 C14 -8.7(5) 1_655 . . . ? N1 Cd1 O3 C14 81.2(4) . . . . ? O6 Cd1 O3 C14 -168.9(4) . . . . ? N7 Cd1 O3 C14 -92.8(4) . . . . ? O5 Cd1 O3 C14 175.8(4) . . . . ? O3 C14 O4 Cd2 68.2(15) . . . 1_655 ? C13 C14 O4 Cd2 -111.8(12) . . . 1_655 ? O6 C15 O5 Cd1 -4.9(6) . . . . ? C16 C15 O5 Cd1 170.8(5) . . . . ? O3 Cd1 O5 C15 171.7(4) . . . . ? O8 Cd1 O5 C15 1.8(6) 1_655 . . . ? N1 Cd1 O5 C15 -91.4(4) . . . . ? O6 Cd1 O5 C15 2.7(3) . . . . ? N7 Cd1 O5 C15 84.7(4) . . . . ? O5 C15 O6 Cd1 5.0(6) . . . . ? C16 C15 O6 Cd1 -170.6(5) . . . . ? O3 Cd1 O6 C15 -21.6(5) . . . . ? O8 Cd1 O6 C15 176.9(4) 1_655 . . . ? N1 Cd1 O6 C15 88.6(4) . . . . ? N7 Cd1 O6 C15 -98.6(4) . . . . ? O5 Cd1 O6 C15 -2.7(3) . . . . ? O8 C28 O7 Cd2 1.9(6) . . . . ? C27 C28 O7 Cd2 -176.8(6) . . . . ? O2 Cd2 O7 C28 -174.3(4) . . . . ? O4 Cd2 O7 C28 16.6(5) 1_455 . . . ? N10 Cd2 O7 C28 -79.2(4) 2_756 . . . ? O8 Cd2 O7 C28 -1.2(4) . . . . ? N4 Cd2 O7 C28 97.3(4) 2_575 . . . ? O1 Cd2 O7 C28 176.1(3) . . . . ? O7 C28 O8 Cd1 -161.3(5) . . . 1_455 ? C27 C28 O8 Cd1 17.5(9) . . . 1_455 ? O7 C28 O8 Cd2 -2.2(6) . . . . ? C27 C28 O8 Cd2 176.7(4) . . . . ? O2 Cd2 O8 C28 10.6(4) . . . . ? O4 Cd2 O8 C28 -165.6(4) 1_455 . . . ? N10 Cd2 O8 C28 103.6(4) 2_756 . . . ? N4 Cd2 O8 C28 -79.8(4) 2_575 . . . ? O1 Cd2 O8 C28 -164.9(9) . . . . ? O7 Cd2 O8 C28 1.1(3) . . . . ? O2 Cd2 O8 Cd1 176.42(15) . . . 1_455 ? O4 Cd2 O8 Cd1 0.21(18) 1_455 . . 1_455 ? N10 Cd2 O8 Cd1 -90.5(2) 2_756 . . 1_455 ? N4 Cd2 O8 Cd1 86.0(2) 2_575 . . 1_455 ? O1 Cd2 O8 Cd1 0.9(11) . . . 1_455 ? O7 Cd2 O8 Cd1 167.0(3) . . . 1_455 ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.888 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.161 #===END