# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_fax +86-431-85098620 _publ_contact_author_phone +86-431-85098620 _publ_author_name 'Jian-Fang Ma' #============================================================================= data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 873950' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H116 N20 O32 Zn4' _chemical_formula_sum 'C96 H116 N20 O32 Zn4' _chemical_formula_weight 2323.57 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 'C 2/c' _symmetry_space_group_name_hall '-c 2yc' 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 20.4862(5) _cell_length_b 16.2663(5) _cell_length_c 16.9774(5) _cell_angle_alpha 90 _cell_angle_beta 99.120(3) _cell_angle_gamma 90 _cell_volume 5585.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3581 _cell_measurement_theta_min 2.7781 _cell_measurement_theta_max 29.1291 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.835 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10512 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4918 _reflns_number_gt 3663 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In order to give a reasonable O1w and O8w distance, we used the DFIX restraint. For C1, O2, and O2W-O8W, some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR/DELU restraints. ; _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^)+(0.0837P)^2^+9.7930P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4918 _refine_ls_number_parameters 388 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1645 _refine_ls_wR_factor_gt 0.1505 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.076 _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 0.35418(2) 0.83067(3) 0.46295(3) 0.0439(2) Uani 1 1 d . . . C1 C 0.8175(2) 0.4125(3) 0.5901(3) 0.0555(11) Uani 1 1 d U . . C2 C 0.7741(2) 0.4453(3) 0.6449(2) 0.0445(10) Uani 1 1 d . . . C3 C 0.7994(2) 0.4906(3) 0.7139(3) 0.0579(12) Uani 1 1 d . . . H3 H 0.8446 0.5007 0.7255 0.069 Uiso 1 1 calc R . . C4 C 0.7593(2) 0.5195(3) 0.7632(3) 0.0604(13) Uani 1 1 d . . . H4 H 0.7775 0.5491 0.8082 0.072 Uiso 1 1 calc R . . C5 C 0.6903(2) 0.5058(3) 0.7481(3) 0.0545(11) Uani 1 1 d . . . C6 C 0.7081(2) 0.4317(3) 0.6309(2) 0.0442(10) Uani 1 1 d . . . H6 H 0.6902 0.4017 0.5859 0.053 Uiso 1 1 calc R . . C7 C 0.5958(2) 0.4447(3) 0.6624(3) 0.0497(11) Uani 1 1 d . . . H7A H 0.5795 0.4329 0.7118 0.060 Uiso 1 1 calc R . . H7B H 0.5881 0.3964 0.6286 0.060 Uiso 1 1 calc R . . C8 C 0.55715(19) 0.5162(3) 0.6212(2) 0.0416(9) Uani 1 1 d . . . C9 C 0.5799(2) 0.5612(3) 0.5632(3) 0.0619(13) Uani 1 1 d . . . H9 H 0.6216 0.5502 0.5506 0.074 Uiso 1 1 calc R . . C10 C 0.5421(2) 0.6223(3) 0.5234(3) 0.0595(13) Uani 1 1 d . . . H10 H 0.5583 0.6514 0.4834 0.071 Uiso 1 1 calc R . . C11 C 0.4809(2) 0.6417(3) 0.5413(2) 0.0427(9) Uani 1 1 d . . . C12 C 0.4576(2) 0.5973(3) 0.5997(3) 0.0566(12) Uani 1 1 d . . . H12 H 0.4165 0.6096 0.6132 0.068 Uiso 1 1 calc R . . C13 C 0.4950(2) 0.5343(3) 0.6387(3) 0.0567(12) Uani 1 1 d . . . H13 H 0.4781 0.5037 0.6772 0.068 Uiso 1 1 calc R . . C14 C 0.4406(2) 0.7094(3) 0.4981(3) 0.0471(10) Uani 1 1 d . . . C15 C 0.3111(3) 0.7656(3) 0.2955(3) 0.0667(14) Uani 1 1 d . . . H15 H 0.3542 0.7614 0.2848 0.080 Uiso 1 1 calc R . . C16 C 0.2561(3) 0.7514(4) 0.2429(3) 0.0780(17) Uani 1 1 d . . . H16 H 0.2540 0.7363 0.1897 0.094 Uiso 1 1 calc R . . C17 C 0.2288(2) 0.7845(3) 0.3573(3) 0.0492(11) Uani 1 1 d . . . H17 H 0.2037 0.7959 0.3971 0.059 Uiso 1 1 calc R . . C18 C 0.1328(3) 0.7568(4) 0.2523(3) 0.0784(16) Uani 1 1 d . . . H18A H 0.1159 0.8102 0.2338 0.094 Uiso 1 1 calc R . . H18B H 0.1097 0.7395 0.2950 0.094 Uiso 1 1 calc R . . C19 C 0.1196(3) 0.6935(4) 0.1821(4) 0.0824(17) Uani 1 1 d . . . H19A H 0.1388 0.7139 0.1371 0.099 Uiso 1 1 calc R . . H19B H 0.1409 0.6417 0.1989 0.099 Uiso 1 1 calc R . . C20 C 0.0501(3) 0.6802(4) 0.1577(4) 0.0784(16) Uani 1 1 d . . . H20A H 0.0280 0.7330 0.1502 0.094 Uiso 1 1 calc R . . H20B H 0.0326 0.6516 0.2000 0.094 Uiso 1 1 calc R . . C21 C 0.0344(3) 0.6312(3) 0.0822(3) 0.0741(16) Uani 1 1 d . . . H21A H -0.0124 0.6366 0.0617 0.089 Uiso 1 1 calc R . . H21B H 0.0588 0.6539 0.0427 0.089 Uiso 1 1 calc R . . C22 C 0.0933(2) 0.5001(3) 0.0584(3) 0.0529(11) Uani 1 1 d . . . H22 H 0.1200 0.5224 0.0243 0.064 Uiso 1 1 calc R . . N5 N 0.09334(17) 0.4221(2) 0.0778(2) 0.0477(9) Uani 1 1 d . . . C24 C 0.0208(3) 0.4901(3) 0.1375(4) 0.0705(15) Uani 1 1 d . . . H24 H -0.0116 0.5022 0.1684 0.085 Uiso 1 1 calc R . . N1 N 0.66711(16) 0.4602(2) 0.6802(2) 0.0445(8) Uani 1 1 d . . . N2 N 0.29387(17) 0.7871(2) 0.3672(2) 0.0466(9) Uani 1 1 d . . . N3 N 0.20363(19) 0.7632(3) 0.2825(2) 0.0590(10) Uani 1 1 d . . . N4 N 0.05067(19) 0.5435(2) 0.0931(2) 0.0543(10) Uani 1 1 d . . . C23 C 0.0477(3) 0.4161(3) 0.1277(3) 0.0647(14) Uani 1 1 d . . . H23 H 0.0366 0.3677 0.1517 0.078 Uiso 1 1 calc R . . O1 O 0.79043(15) 0.3805(2) 0.52506(19) 0.0549(8) Uani 1 1 d . . . O2 O 0.87850(18) 0.4170(2) 0.6110(2) 0.0730(9) Uani 1 1 d U . . O3 O 0.65020(18) 0.5298(3) 0.7905(2) 0.0789(11) Uani 1 1 d . . . O4 O 0.45410(17) 0.7363(2) 0.4343(2) 0.0622(9) Uani 1 1 d . . . O5 O 0.39324(15) 0.7381(2) 0.52973(19) 0.0583(8) Uani 1 1 d . . . O1W O 0.5418(9) 0.7214(17) 0.3237(9) 0.142(9) Uani 0.60 1 d PD . . O2W O 0.7046(3) 0.4963(5) 0.9476(4) 0.119(2) Uani 0.80 1 d PU . . O3W O 0.6304(6) 0.8624(8) 0.3981(8) 0.146(4) Uani 0.50 1 d PU . . O4W O 0.6612(8) 0.3540(13) 0.8895(11) 0.146(6) Uani 0.35 1 d PU . . O5W O 0.753(2) 0.337(3) 1.030(3) 0.136(14) Uani 0.15 1 d PU . . O6W O 0.775(3) 0.316(4) 0.982(4) 0.11(2) Uani 0.10 1 d PU . . O7W O 0.733(3) 0.848(3) 0.534(3) 0.128(18) Uani 0.15 1 d PU . . O8W O 0.4670(18) 0.731(3) 0.1708(14) 0.164(18) Uani 0.35 1 d PDU . . 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 0.0409(3) 0.0457(3) 0.0458(3) 0.0016(2) 0.0088(2) 0.0029(2) C1 0.0592(15) 0.055(3) 0.056(3) 0.007(2) 0.018(2) 0.007(2) C2 0.041(2) 0.045(2) 0.048(2) 0.000(2) 0.0058(19) 0.0044(19) C3 0.044(2) 0.061(3) 0.066(3) -0.006(2) 0.001(2) 0.001(2) C4 0.054(3) 0.064(3) 0.061(3) -0.024(2) 0.001(2) 0.001(2) C5 0.056(3) 0.056(3) 0.051(3) -0.013(2) 0.005(2) 0.008(2) C6 0.048(2) 0.042(2) 0.042(2) -0.0026(18) 0.0043(19) 0.0059(19) C7 0.043(2) 0.047(2) 0.058(3) -0.002(2) 0.004(2) 0.003(2) C8 0.037(2) 0.041(2) 0.046(2) -0.0046(19) 0.0054(18) 0.0012(18) C9 0.045(3) 0.081(4) 0.064(3) 0.013(3) 0.021(2) 0.021(3) C10 0.055(3) 0.072(3) 0.056(3) 0.016(3) 0.026(2) 0.012(3) C11 0.042(2) 0.041(2) 0.045(2) -0.0062(19) 0.0061(19) 0.0017(19) C12 0.038(2) 0.063(3) 0.071(3) 0.009(3) 0.017(2) 0.009(2) C13 0.045(2) 0.063(3) 0.065(3) 0.018(2) 0.020(2) 0.007(2) C14 0.044(2) 0.045(2) 0.050(3) -0.008(2) 0.000(2) -0.002(2) C15 0.066(3) 0.074(3) 0.063(3) -0.013(3) 0.019(3) -0.007(3) C16 0.084(4) 0.102(5) 0.050(3) -0.022(3) 0.017(3) -0.019(3) C17 0.054(3) 0.044(2) 0.049(3) -0.002(2) 0.007(2) -0.002(2) C18 0.070(4) 0.087(4) 0.071(4) -0.008(3) -0.009(3) -0.014(3) C19 0.085(4) 0.078(4) 0.077(4) -0.008(3) -0.010(3) 0.004(3) C20 0.076(4) 0.066(4) 0.089(4) -0.009(3) 0.000(3) 0.001(3) C21 0.086(4) 0.051(3) 0.078(4) -0.012(3) -0.013(3) 0.012(3) C22 0.058(3) 0.050(3) 0.051(3) -0.005(2) 0.009(2) -0.003(2) N5 0.046(2) 0.045(2) 0.053(2) -0.0042(17) 0.0086(17) -0.0006(17) C24 0.061(3) 0.064(3) 0.091(4) -0.011(3) 0.027(3) -0.005(3) N1 0.0389(18) 0.047(2) 0.047(2) -0.0058(16) 0.0045(16) 0.0067(16) N2 0.047(2) 0.048(2) 0.045(2) -0.0054(17) 0.0063(16) -0.0022(17) N3 0.059(2) 0.064(2) 0.051(2) -0.009(2) -0.0021(19) -0.013(2) N4 0.053(2) 0.049(2) 0.056(2) -0.0102(19) -0.0074(19) 0.0062(19) C23 0.070(3) 0.052(3) 0.079(4) -0.002(3) 0.033(3) -0.001(3) O1 0.0488(17) 0.065(2) 0.0518(18) -0.0074(16) 0.0106(15) 0.0125(16) O2 0.0651(11) 0.0801(13) 0.0743(13) -0.0027(9) 0.0124(9) 0.0003(9) O3 0.067(2) 0.102(3) 0.070(2) -0.032(2) 0.0164(19) 0.015(2) O4 0.071(2) 0.059(2) 0.059(2) 0.0107(16) 0.0157(17) 0.0097(17) O5 0.0525(18) 0.0588(19) 0.065(2) 0.0106(16) 0.0134(16) 0.0178(16) O1W 0.140(11) 0.198(17) 0.107(9) 0.037(8) 0.086(9) 0.058(10) O2W 0.124(4) 0.152(5) 0.082(4) -0.005(4) 0.019(3) -0.037(4) O3W 0.133(7) 0.147(8) 0.163(8) -0.006(7) 0.040(6) -0.022(7) O4W 0.130(9) 0.179(10) 0.146(9) -0.013(8) 0.074(8) -0.009(8) O5W 0.137(16) 0.136(17) 0.135(16) 0.005(10) 0.020(10) 0.009(10) O6W 0.11(2) 0.11(2) 0.11(2) -0.001(10) 0.019(11) 0.008(10) O7W 0.132(19) 0.13(2) 0.13(2) -0.001(10) 0.027(10) -0.001(10) O8W 0.17(2) 0.16(2) 0.17(2) 0.007(10) 0.027(10) -0.008(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 1.976(3) . ? Zn1 O1 1.978(3) 3_455 ? Zn1 N2 2.009(3) . ? Zn1 N5 2.020(3) 4 ? C1 O2 1.247(6) . ? C1 O1 1.266(6) . ? C1 C2 1.484(6) . ? C2 C6 1.354(6) . ? C2 C3 1.411(6) . ? C3 C4 1.347(7) . ? C3 H3 0.9300 . ? C4 C5 1.415(7) . ? C4 H4 0.9300 . ? C5 O3 1.238(5) . ? C5 N1 1.389(6) . ? C6 N1 1.358(5) . ? C6 H6 0.9300 . ? C7 N1 1.466(5) . ? C7 C8 1.514(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.366(6) . ? C8 C13 1.385(6) . ? C9 C10 1.372(7) . ? C9 H9 0.9300 . ? C10 C11 1.374(6) . ? C10 H10 0.9300 . ? C11 C12 1.372(6) . ? C11 C14 1.496(6) . ? C12 C13 1.384(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O4 1.241(5) . ? C14 O5 1.270(5) . ? C15 C16 1.344(7) . ? C15 N2 1.365(6) . ? C15 H15 0.9300 . ? C16 N3 1.368(6) . ? C16 H16 0.9300 . ? C17 N2 1.318(5) . ? C17 N3 1.339(6) . ? C17 H17 0.9300 . ? C18 N3 1.464(6) . ? C18 C19 1.565(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.436(8) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.501(8) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 N4 1.470(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N5 1.311(6) . ? C22 N4 1.332(6) . ? C22 H22 0.9300 . ? N5 C23 1.362(6) . ? N5 Zn1 2.020(3) 4_545 ? C24 C23 1.344(7) . ? C24 N4 1.358(7) . ? C24 H24 0.9300 . ? C23 H23 0.9300 . ? O1 Zn1 1.978(3) 3_545 ? O5W O6W 1.05(7) . ? O5W O7W 1.18(6) 4_646 ? O6W O7W 0.60(8) 4_646 ? O7W O6W 0.60(8) 4_656 ? O7W O5W 1.18(6) 4_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 O1 104.35(13) . 3_455 ? O5 Zn1 N2 109.67(14) . . ? O1 Zn1 N2 101.70(13) 3_455 . ? O5 Zn1 N5 124.62(14) . 4 ? O1 Zn1 N5 108.25(14) 3_455 4 ? N2 Zn1 N5 105.96(15) . 4 ? O2 C1 O1 123.6(4) . . ? O2 C1 C2 118.2(5) . . ? O1 C1 C2 118.2(4) . . ? C6 C2 C3 117.2(4) . . ? C6 C2 C1 120.8(4) . . ? C3 C2 C1 122.0(4) . . ? C4 C3 C2 121.2(4) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 121.5(4) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? O3 C5 N1 118.7(4) . . ? O3 C5 C4 125.5(4) . . ? N1 C5 C4 115.8(4) . . ? C2 C6 N1 122.2(4) . . ? C2 C6 H6 118.9 . . ? N1 C6 H6 118.9 . . ? N1 C7 C8 113.2(4) . . ? N1 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C13 118.2(4) . . ? C9 C8 C7 122.0(4) . . ? C13 C8 C7 119.7(4) . . ? C8 C9 C10 120.9(4) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 121.4(4) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C12 C11 C10 118.2(4) . . ? C12 C11 C14 120.9(4) . . ? C10 C11 C14 120.8(4) . . ? C11 C12 C13 120.5(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 120.8(4) . . ? C12 C13 H13 119.6 . . ? C8 C13 H13 119.6 . . ? O4 C14 O5 122.0(4) . . ? O4 C14 C11 120.4(4) . . ? O5 C14 C11 117.6(4) . . ? C16 C15 N2 109.1(5) . . ? C16 C15 H15 125.4 . . ? N2 C15 H15 125.4 . . ? C15 C16 N3 106.9(4) . . ? C15 C16 H16 126.5 . . ? N3 C16 H16 126.5 . . ? N2 C17 N3 111.0(4) . . ? N2 C17 H17 124.5 . . ? N3 C17 H17 124.5 . . ? N3 C18 C19 110.9(5) . . ? N3 C18 H18A 109.5 . . ? C19 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C20 C19 C18 111.3(5) . . ? C20 C19 H19A 109.4 . . ? C18 C19 H19A 109.4 . . ? C20 C19 H19B 109.4 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C19 C20 C21 113.2(5) . . ? C19 C20 H20A 108.9 . . ? C21 C20 H20A 108.9 . . ? C19 C20 H20B 108.9 . . ? C21 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? N4 C21 C20 113.2(5) . . ? N4 C21 H21A 108.9 . . ? C20 C21 H21A 108.9 . . ? N4 C21 H21B 108.9 . . ? C20 C21 H21B 108.9 . . ? H21A C21 H21B 107.8 . . ? N5 C22 N4 112.1(4) . . ? N5 C22 H22 124.0 . . ? N4 C22 H22 124.0 . . ? C22 N5 C23 104.7(4) . . ? C22 N5 Zn1 127.2(3) . 4_545 ? C23 N5 Zn1 128.0(3) . 4_545 ? C23 C24 N4 106.0(4) . . ? C23 C24 H24 127.0 . . ? N4 C24 H24 127.0 . . ? C6 N1 C5 122.1(4) . . ? C6 N1 C7 120.5(4) . . ? C5 N1 C7 117.5(3) . . ? C17 N2 C15 106.2(4) . . ? C17 N2 Zn1 126.4(3) . . ? C15 N2 Zn1 126.8(3) . . ? C17 N3 C16 106.8(4) . . ? C17 N3 C18 124.2(4) . . ? C16 N3 C18 129.0(4) . . ? C22 N4 C24 106.9(4) . . ? C22 N4 C21 127.7(5) . . ? C24 N4 C21 125.3(5) . . ? C24 C23 N5 110.3(5) . . ? C24 C23 H23 124.9 . . ? N5 C23 H23 124.9 . . ? C1 O1 Zn1 113.5(3) . 3_545 ? C14 O5 Zn1 107.8(3) . . ? O7W O6W O5W 87(10) 4_646 . ? O6W O7W O5W 63(9) 4_656 4_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C6 -170.5(4) . . . . ? O1 C1 C2 C6 8.7(7) . . . . ? O2 C1 C2 C3 8.5(7) . . . . ? O1 C1 C2 C3 -172.3(4) . . . . ? C6 C2 C3 C4 -0.6(7) . . . . ? C1 C2 C3 C4 -179.6(5) . . . . ? C2 C3 C4 C5 0.0(8) . . . . ? C3 C4 C5 O3 179.6(5) . . . . ? C3 C4 C5 N1 0.7(7) . . . . ? C3 C2 C6 N1 0.4(6) . . . . ? C1 C2 C6 N1 179.4(4) . . . . ? N1 C7 C8 C9 40.1(6) . . . . ? N1 C7 C8 C13 -143.8(4) . . . . ? C13 C8 C9 C10 -0.3(7) . . . . ? C7 C8 C9 C10 175.9(5) . . . . ? C8 C9 C10 C11 1.3(8) . . . . ? C9 C10 C11 C12 -0.9(8) . . . . ? C9 C10 C11 C14 179.1(5) . . . . ? C10 C11 C12 C13 -0.6(7) . . . . ? C14 C11 C12 C13 179.4(4) . . . . ? C11 C12 C13 C8 1.7(8) . . . . ? C9 C8 C13 C12 -1.3(7) . . . . ? C7 C8 C13 C12 -177.6(4) . . . . ? C12 C11 C14 O4 -163.3(4) . . . . ? C10 C11 C14 O4 16.7(7) . . . . ? C12 C11 C14 O5 17.4(6) . . . . ? C10 C11 C14 O5 -162.6(4) . . . . ? N2 C15 C16 N3 -0.7(7) . . . . ? N3 C18 C19 C20 173.8(5) . . . . ? C18 C19 C20 C21 170.4(5) . . . . ? C19 C20 C21 N4 73.5(7) . . . . ? N4 C22 N5 C23 0.2(5) . . . . ? N4 C22 N5 Zn1 176.9(3) . . . 4_545 ? C2 C6 N1 C5 0.4(6) . . . . ? C2 C6 N1 C7 179.4(4) . . . . ? O3 C5 N1 C6 -179.9(4) . . . . ? C4 C5 N1 C6 -0.9(7) . . . . ? O3 C5 N1 C7 1.0(7) . . . . ? C4 C5 N1 C7 -180.0(4) . . . . ? C8 C7 N1 C6 -97.8(5) . . . . ? C8 C7 N1 C5 81.3(5) . . . . ? N3 C17 N2 C15 -0.7(5) . . . . ? N3 C17 N2 Zn1 170.8(3) . . . . ? C16 C15 N2 C17 0.8(6) . . . . ? C16 C15 N2 Zn1 -170.6(4) . . . . ? O5 Zn1 N2 C17 102.1(4) . . . . ? O1 Zn1 N2 C17 -8.0(4) 3_455 . . . ? N5 Zn1 N2 C17 -121.1(4) 4 . . . ? O5 Zn1 N2 C15 -88.2(4) . . . . ? O1 Zn1 N2 C15 161.7(4) 3_455 . . . ? N5 Zn1 N2 C15 48.7(4) 4 . . . ? N2 C17 N3 C16 0.3(6) . . . . ? N2 C17 N3 C18 -178.6(5) . . . . ? C15 C16 N3 C17 0.3(6) . . . . ? C15 C16 N3 C18 179.0(5) . . . . ? C19 C18 N3 C17 -152.6(5) . . . . ? C19 C18 N3 C16 28.8(8) . . . . ? N5 C22 N4 C24 -0.4(6) . . . . ? N5 C22 N4 C21 -176.3(4) . . . . ? C23 C24 N4 C22 0.5(6) . . . . ? C23 C24 N4 C21 176.5(5) . . . . ? C20 C21 N4 C22 -119.0(6) . . . . ? C20 C21 N4 C24 65.8(7) . . . . ? N4 C24 C23 N5 -0.4(6) . . . . ? C22 N5 C23 C24 0.1(6) . . . . ? Zn1 N5 C23 C24 -176.6(4) 4_545 . . . ? O2 C1 O1 Zn1 4.3(6) . . . 3_545 ? C2 C1 O1 Zn1 -174.8(3) . . . 3_545 ? O4 C14 O5 Zn1 -3.1(5) . . . . ? C11 C14 O5 Zn1 176.2(3) . . . . ? O1 Zn1 O5 C14 -172.1(3) 3_455 . . . ? N2 Zn1 O5 C14 79.6(3) . . . . ? N5 Zn1 O5 C14 -47.4(3) 4 . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.731 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.069 #=========================END data_Compound-2 _database_code_depnum_ccdc_archive 'CCDC 873951' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H16 Co N3 O5' _chemical_formula_sum 'C19 H16 Co N3 O5' _chemical_formula_weight 425.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_hall '-c 2yc' 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 24.6475(19) _cell_length_b 7.5175(4) _cell_length_c 23.1062(17) _cell_angle_alpha 90 _cell_angle_beta 115.938(9) _cell_angle_gamma 90 _cell_volume 3850.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2035 _cell_measurement_theta_min 2.8554 _cell_measurement_theta_max 29.0920 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7621 _exptl_absorpt_correction_T_max 0.8363 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7635 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3392 _reflns_number_gt 2573 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In the refienment of the disordered imidazole rings, the PART instructions were used. For C12, C13, C15-C17, C15'-C17', N2, N3, N2' and N3', some anisotropic displacement ellipsoids were rather elongated which led us to use the SIMU/ISOR/DELU restraints. In order to restrict the C-C and C-N distances of the imidazole ring, we used the SAME restraints. In order to make all atoms of the imidazole ring be co-planar, we used the FLAT restraints. ; _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^)+(0.0305P)^2^+0.6493P] 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 3392 _refine_ls_number_parameters 299 _refine_ls_number_restraints 183 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.007 _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 0.039310(17) 0.34841(5) 0.519166(18) 0.02797(13) Uani 1 1 d . . . C1 C -0.04000(14) -0.3661(4) 0.07725(14) 0.0354(7) Uani 1 1 d . . . C2 C -0.06355(13) -0.3266(4) 0.12538(14) 0.0359(7) Uani 1 1 d . . . C3 C -0.09045(17) -0.4594(4) 0.14467(18) 0.0595(10) Uani 1 1 d . . . H3 H -0.0950 -0.5721 0.1265 0.071 Uiso 1 1 calc R . . C4 C -0.11069(17) -0.4272(4) 0.19057(17) 0.0587(11) Uani 1 1 d . . . H4 H -0.1282 -0.5190 0.2034 0.070 Uiso 1 1 calc R . . C5 C -0.10536(14) -0.2611(4) 0.21776(14) 0.0370(7) Uani 1 1 d . . . C6 C -0.07965(15) -0.1276(4) 0.19720(16) 0.0467(9) Uani 1 1 d . . . H6 H -0.0764 -0.0139 0.2142 0.056 Uiso 1 1 calc R . . C7 C -0.05872(15) -0.1602(4) 0.15174(16) 0.0458(8) Uani 1 1 d . . . H7 H -0.0412 -0.0685 0.1388 0.055 Uiso 1 1 calc R . . C8 C -0.12660(15) -0.2362(4) 0.26919(15) 0.0408(8) Uani 1 1 d . . . H8A H -0.1632 -0.3047 0.2577 0.049 Uiso 1 1 calc R . . H8B H -0.0963 -0.2837 0.3094 0.049 Uiso 1 1 calc R . . C9 C -0.19100(14) 0.0262(4) 0.23217(15) 0.0383(7) Uani 1 1 d . . . C10 C -0.20326(14) 0.2015(4) 0.24713(15) 0.0440(8) Uani 1 1 d . . . H10 H -0.2385 0.2582 0.2190 0.053 Uiso 1 1 calc R . . C11 C -0.16513(14) 0.2874(4) 0.30098(15) 0.0383(7) Uani 1 1 d . . . H11 H -0.1748 0.4013 0.3091 0.046 Uiso 1 1 calc R . . C12 C -0.11121(13) 0.2082(4) 0.34498(13) 0.0313(6) Uani 1 1 d U A . C13 C -0.10023(13) 0.0381(3) 0.33295(13) 0.0314(6) Uani 1 1 d U . . H13 H -0.0656 -0.0190 0.3622 0.038 Uiso 1 1 calc R . . C14 C -0.06828(14) 0.3024(4) 0.40389(14) 0.0347(7) Uani 1 1 d . . . C15 C 0.2087(4) 0.0970(18) 0.5940(6) 0.041(2) Uani 0.47(3) 1 d PDU A 1 H15 H 0.2501 0.0920 0.6193 0.050 Uiso 0.47(3) 1 calc PR A 1 C16 C 0.1712(5) 0.2331(16) 0.5895(6) 0.0353(19) Uani 0.47(3) 1 d PDU A 1 H16 H 0.1830 0.3400 0.6118 0.042 Uiso 0.47(3) 1 calc PR A 1 N2 N 0.1133(6) 0.190(3) 0.5471(11) 0.029(2) Uani 0.47(3) 1 d PDU A 1 C17 C 0.1163(7) 0.029(3) 0.5266(14) 0.031(2) Uani 0.47(3) 1 d PDU A 1 H17 H 0.0832 -0.0345 0.4974 0.037 Uiso 0.47(3) 1 calc PR A 1 N3 N 0.1725(7) -0.0333(18) 0.5530(9) 0.036(2) Uani 0.47(3) 1 d PDU A 1 C15' C 0.2129(4) 0.1481(16) 0.5795(5) 0.040(2) Uani 0.53(3) 1 d PDU A 2 H15' H 0.2546 0.1609 0.5984 0.048 Uiso 0.53(3) 1 calc PR A 2 C16' C 0.1729(4) 0.2738(15) 0.5747(6) 0.0385(19) Uani 0.53(3) 1 d PDU A 2 H16' H 0.1822 0.3900 0.5895 0.046 Uiso 0.53(3) 1 calc PR A 2 N2' N 0.1160(5) 0.204(2) 0.5443(10) 0.031(2) Uani 0.53(3) 1 d PDU A 2 C17' C 0.1230(7) 0.038(3) 0.5302(13) 0.035(2) Uani 0.53(3) 1 d PDU A 2 H17' H 0.0914 -0.0401 0.5081 0.042 Uiso 0.53(3) 1 calc PR A 2 N3' N 0.1812(6) -0.0034(17) 0.5516(8) 0.036(2) Uani 0.53(3) 1 d PDU A 2 C18 C 0.20092(16) -0.1886(4) 0.54284(18) 0.0569(10) Uani 1 1 d . . . H18A H 0.1700 -0.2778 0.5220 0.068 Uiso 1 1 calc R A 1 H18B H 0.2284 -0.2354 0.5846 0.068 Uiso 1 1 calc R A 1 C19 C 0.23567(17) -0.1641(4) 0.50326(18) 0.0594(10) Uani 1 1 d . . . H19A H 0.2086 -0.1210 0.4608 0.071 Uiso 1 1 calc R . . H19B H 0.2668 -0.0753 0.5235 0.071 Uiso 1 1 calc R . . N1 N -0.13854(11) -0.0505(3) 0.27938(11) 0.0339(6) Uani 1 1 d . . . O1 O -0.00105(9) -0.2632(3) 0.07423(10) 0.0413(5) Uani 1 1 d . . . O2 O -0.06046(9) -0.5007(3) 0.04255(10) 0.0476(6) Uani 1 1 d . . . O3 O -0.22268(10) -0.0590(3) 0.18353(10) 0.0530(6) Uani 1 1 d . . . O4 O -0.08242(9) 0.4591(3) 0.41134(10) 0.0452(6) Uani 1 1 d . . . O5 O -0.02172(10) 0.2213(3) 0.44155(10) 0.0444(5) Uani 1 1 d . A . 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 0.0280(2) 0.0285(2) 0.0276(2) 0.00281(17) 0.01224(18) 0.00421(17) C1 0.0356(19) 0.0424(17) 0.0285(16) 0.0001(15) 0.0143(15) 0.0056(15) C2 0.0377(19) 0.0402(17) 0.0362(17) -0.0052(14) 0.0220(15) -0.0016(14) C3 0.091(3) 0.0381(18) 0.075(3) -0.0208(18) 0.060(3) -0.0115(18) C4 0.094(3) 0.0399(18) 0.075(3) -0.0119(18) 0.068(3) -0.0156(18) C5 0.042(2) 0.0383(17) 0.0345(17) -0.0068(14) 0.0200(16) -0.0035(14) C6 0.063(2) 0.0379(18) 0.054(2) -0.0144(16) 0.039(2) -0.0088(16) C7 0.058(2) 0.0381(17) 0.055(2) -0.0102(16) 0.0381(19) -0.0108(16) C8 0.056(2) 0.0334(17) 0.0408(19) -0.0045(14) 0.0288(18) -0.0021(15) C9 0.0299(19) 0.0503(19) 0.0347(18) -0.0023(16) 0.0141(16) -0.0060(15) C10 0.035(2) 0.0485(19) 0.0404(19) 0.0011(15) 0.0094(16) 0.0092(15) C11 0.039(2) 0.0374(16) 0.0391(18) -0.0049(15) 0.0176(16) -0.0011(14) C12 0.0302(17) 0.0373(13) 0.0268(16) -0.0003(13) 0.0129(14) -0.0007(13) C13 0.0336(18) 0.0388(13) 0.0249(15) 0.0026(13) 0.0155(14) 0.0009(13) C14 0.040(2) 0.0409(18) 0.0263(17) -0.0024(14) 0.0174(16) -0.0078(15) C15 0.032(3) 0.041(3) 0.047(3) 0.006(3) 0.013(2) 0.005(3) C16 0.036(2) 0.035(2) 0.035(2) -0.0009(10) 0.0154(11) 0.0006(10) N2 0.028(3) 0.029(4) 0.030(3) 0.004(3) 0.014(3) 0.003(3) C17 0.026(4) 0.033(4) 0.037(4) -0.001(3) 0.018(3) 0.006(3) N3 0.033(4) 0.034(4) 0.042(3) -0.002(3) 0.016(3) 0.001(3) C15' 0.032(3) 0.040(3) 0.047(3) -0.002(3) 0.017(2) 0.000(3) C16' 0.036(3) 0.032(3) 0.042(4) 0.001(3) 0.012(3) 0.006(3) N2' 0.027(3) 0.031(3) 0.033(3) 0.000(3) 0.012(3) 0.008(3) C17' 0.030(4) 0.033(3) 0.037(3) -0.002(3) 0.011(3) -0.001(3) N3' 0.031(4) 0.033(4) 0.047(3) -0.005(3) 0.021(3) 0.010(3) C18 0.062(3) 0.050(2) 0.060(2) -0.0012(18) 0.028(2) 0.0265(18) C19 0.063(3) 0.053(2) 0.069(2) -0.0018(19) 0.036(2) 0.0244(18) N1 0.0389(16) 0.0354(13) 0.0304(14) -0.0063(11) 0.0178(13) -0.0016(12) O1 0.0473(14) 0.0436(12) 0.0450(13) -0.0054(10) 0.0314(12) -0.0044(10) O2 0.0488(15) 0.0578(14) 0.0434(13) -0.0228(12) 0.0270(12) -0.0074(11) O3 0.0410(14) 0.0667(15) 0.0416(14) -0.0158(12) 0.0091(12) -0.0113(11) O4 0.0456(14) 0.0396(12) 0.0488(14) -0.0170(10) 0.0191(12) -0.0062(10) O5 0.0417(14) 0.0466(12) 0.0316(12) -0.0030(10) 0.0038(11) -0.0002(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.008(2) . ? Co1 N2 2.030(16) . ? Co1 N2' 2.031(14) . ? Co1 O1 2.0314(19) 6_556 ? Co1 O2 2.0595(19) 2_565 ? Co1 O4 2.076(2) 5_566 ? Co1 Co1 2.8692(7) 5_566 ? C1 O2 1.252(3) . ? C1 O1 1.259(3) . ? C1 C2 1.492(4) . ? C2 C7 1.374(4) . ? C2 C3 1.376(4) . ? C3 C4 1.377(4) . ? C3 H3 0.9300 . ? C4 C5 1.378(4) . ? C4 H4 0.9300 . ? C5 C6 1.377(4) . ? C5 C8 1.505(4) . ? C6 C7 1.380(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.467(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O3 1.231(3) . ? C9 N1 1.400(4) . ? C9 C10 1.428(4) . ? C10 C11 1.351(4) . ? C10 H10 0.9300 . ? C11 C12 1.404(4) . ? C11 H11 0.9300 . ? C12 C13 1.360(4) . ? C12 C14 1.488(4) . ? C13 N1 1.358(3) . ? C13 H13 0.9300 . ? C14 O5 1.254(3) . ? C14 O4 1.261(3) . ? C15 C16 1.351(9) . ? C15 N3 1.383(11) . ? C15 H15 0.9300 . ? C16 N2 1.370(11) . ? C16 H16 0.9300 . ? N2 C17 1.320(11) . ? C17 N3 1.331(11) . ? C17 H17 0.9300 . ? N3 C18 1.432(16) . ? C15' C16' 1.334(8) . ? C15' N3' 1.373(9) . ? C15' H15' 0.9300 . ? C16' N2' 1.369(10) . ? C16' H16' 0.9300 . ? N2' C17' 1.320(10) . ? C17' N3' 1.333(10) . ? C17' H17' 0.9300 . ? N3' C18 1.517(12) . ? C18 C19 1.513(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C19 1.510(6) 7_546 ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? O1 Co1 2.0314(19) 6 ? O2 Co1 2.0595(19) 2_545 ? O4 Co1 2.0759(19) 5_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 N2 102.9(5) . . ? O5 Co1 N2' 103.9(5) . . ? N2 Co1 N2' 4.3(13) . . ? O5 Co1 O1 91.64(9) . 6_556 ? N2 Co1 O1 103.5(7) . 6_556 ? N2' Co1 O1 107.6(7) . 6_556 ? O5 Co1 O2 87.78(9) . 2_565 ? N2 Co1 O2 94.5(7) . 2_565 ? N2' Co1 O2 90.4(7) . 2_565 ? O1 Co1 O2 161.63(8) 6_556 2_565 ? O5 Co1 O4 162.29(8) . 5_566 ? N2 Co1 O4 94.4(5) . 5_566 ? N2' Co1 O4 93.1(5) . 5_566 ? O1 Co1 O4 87.74(8) 6_556 5_566 ? O2 Co1 O4 87.29(9) 2_565 5_566 ? O5 Co1 Co1 87.79(6) . 5_566 ? N2 Co1 Co1 162.6(6) . 5_566 ? N2' Co1 Co1 158.6(6) . 5_566 ? O1 Co1 Co1 89.67(6) 6_556 5_566 ? O2 Co1 Co1 71.96(6) 2_565 5_566 ? O4 Co1 Co1 74.52(6) 5_566 5_566 ? O2 C1 O1 124.4(3) . . ? O2 C1 C2 117.3(3) . . ? O1 C1 C2 118.3(3) . . ? C7 C2 C3 118.6(3) . . ? C7 C2 C1 121.7(3) . . ? C3 C2 C1 119.8(3) . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 121.1(3) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 118.0(3) . . ? C6 C5 C8 123.6(2) . . ? C4 C5 C8 118.4(3) . . ? C5 C6 C7 121.0(3) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 120.7(3) . . ? C2 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? N1 C8 C5 114.1(2) . . ? N1 C8 H8A 108.7 . . ? C5 C8 H8A 108.7 . . ? N1 C8 H8B 108.7 . . ? C5 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? O3 C9 N1 119.9(3) . . ? O3 C9 C10 125.7(3) . . ? N1 C9 C10 114.4(3) . . ? C11 C10 C9 121.9(3) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C12 121.4(3) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 117.4(3) . . ? C13 C12 C14 120.6(3) . . ? C11 C12 C14 122.0(3) . . ? N1 C13 C12 121.7(3) . . ? N1 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? O5 C14 O4 125.7(3) . . ? O5 C14 C12 118.2(3) . . ? O4 C14 C12 116.2(3) . . ? C16 C15 N3 105.7(8) . . ? C16 C15 H15 127.2 . . ? N3 C15 H15 127.2 . . ? C15 C16 N2 109.9(9) . . ? C15 C16 H16 125.0 . . ? N2 C16 H16 125.0 . . ? C17 N2 C16 105.6(10) . . ? C17 N2 Co1 127.5(11) . . ? C16 N2 Co1 126.9(12) . . ? N2 C17 N3 111.6(11) . . ? N2 C17 H17 124.2 . . ? N3 C17 H17 124.2 . . ? C17 N3 C15 107.2(10) . . ? C17 N3 C18 134.1(12) . . ? C15 N3 C18 118.4(11) . . ? C16' C15' N3' 107.5(7) . . ? C16' C15' H15' 126.3 . . ? N3' C15' H15' 126.3 . . ? C15' C16' N2' 109.0(8) . . ? C15' C16' H16' 125.5 . . ? N2' C16' H16' 125.5 . . ? C17' N2' C16' 105.8(9) . . ? C17' N2' Co1 129.9(10) . . ? C16' N2' Co1 123.9(10) . . ? N2' C17' N3' 111.5(9) . . ? N2' C17' H17' 124.3 . . ? N3' C17' H17' 124.3 . . ? C17' N3' C15' 106.2(8) . . ? C17' N3' C18 121.4(10) . . ? C15' N3' C18 132.4(10) . . ? N3 C18 C19 116.5(9) . . ? C19 C18 N3' 105.6(8) . . ? N3 C18 H18A 108.2 . . ? C19 C18 H18A 108.2 . . ? N3' C18 H18A 118.2 . . ? N3 C18 H18B 108.2 . . ? C19 C18 H18B 108.2 . . ? N3' C18 H18B 109.0 . . ? H18A C18 H18B 107.3 . . ? C19 C19 C18 111.7(4) 7_546 . ? C19 C19 H19A 109.3 7_546 . ? C18 C19 H19A 109.3 . . ? C19 C19 H19B 109.3 7_546 . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C13 N1 C9 123.0(2) . . ? C13 N1 C8 120.3(2) . . ? C9 N1 C8 116.7(2) . . ? C1 O1 Co1 115.80(18) . 6 ? C1 O2 Co1 137.3(2) . 2_545 ? C14 O4 Co1 132.7(2) . 5_566 ? C14 O5 Co1 119.28(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -160.2(3) . . . . ? O1 C1 C2 C7 19.9(4) . . . . ? O2 C1 C2 C3 20.3(4) . . . . ? O1 C1 C2 C3 -159.5(3) . . . . ? C7 C2 C3 C4 -1.6(5) . . . . ? C1 C2 C3 C4 177.9(3) . . . . ? C2 C3 C4 C5 0.9(6) . . . . ? C3 C4 C5 C6 0.6(5) . . . . ? C3 C4 C5 C8 -178.1(3) . . . . ? C4 C5 C6 C7 -1.3(5) . . . . ? C8 C5 C6 C7 177.3(3) . . . . ? C3 C2 C7 C6 0.9(5) . . . . ? C1 C2 C7 C6 -178.6(3) . . . . ? C5 C6 C7 C2 0.6(5) . . . . ? C6 C5 C8 N1 21.2(4) . . . . ? C4 C5 C8 N1 -160.2(3) . . . . ? O3 C9 C10 C11 -178.2(3) . . . . ? N1 C9 C10 C11 3.4(4) . . . . ? C9 C10 C11 C12 0.2(5) . . . . ? C10 C11 C12 C13 -3.2(4) . . . . ? C10 C11 C12 C14 178.9(3) . . . . ? C11 C12 C13 N1 2.4(4) . . . . ? C14 C12 C13 N1 -179.7(2) . . . . ? C13 C12 C14 O5 0.6(4) . . . . ? C11 C12 C14 O5 178.5(3) . . . . ? C13 C12 C14 O4 -179.4(3) . . . . ? C11 C12 C14 O4 -1.5(4) . . . . ? N3 C15 C16 N2 0.1(13) . . . . ? C15 C16 N2 C17 0.3(17) . . . . ? C15 C16 N2 Co1 -177.4(16) . . . . ? O5 Co1 N2 C17 -12(2) . . . . ? N2' Co1 N2 C17 -115(16) . . . . ? O1 Co1 N2 C17 83.3(19) 6_556 . . . ? O2 Co1 N2 C17 -100.3(19) 2_565 . . . ? O4 Co1 N2 C17 172.1(19) 5_566 . . . ? Co1 Co1 N2 C17 -138(2) 5_566 . . . ? O5 Co1 N2 C16 165.6(18) . . . . ? N2' Co1 N2 C16 62(14) . . . . ? O1 Co1 N2 C16 -99.5(19) 6_556 . . . ? O2 Co1 N2 C16 77(2) 2_565 . . . ? O4 Co1 N2 C16 -11(2) 5_566 . . . ? Co1 Co1 N2 C16 39(4) 5_566 . . . ? C16 N2 C17 N3 -1(2) . . . . ? Co1 N2 C17 N3 177(2) . . . . ? N2 C17 N3 C15 1(3) . . . . ? N2 C17 N3 C18 -173(2) . . . . ? C16 C15 N3 C17 -0.4(19) . . . . ? C16 C15 N3 C18 174.0(14) . . . . ? N3' C15' C16' N2' 0.4(12) . . . . ? C15' C16' N2' C17' -1.4(15) . . . . ? C15' C16' N2' Co1 -175.0(13) . . . . ? O5 Co1 N2' C17' -21(2) . . . . ? N2 Co1 N2' C17' 56(14) . . . . ? O1 Co1 N2' C17' 75.5(19) 6_556 . . . ? O2 Co1 N2' C17' -108.6(19) 2_565 . . . ? O4 Co1 N2' C17' 164.1(19) 5_566 . . . ? Co1 Co1 N2' C17' -142.3(17) 5_566 . . . ? O5 Co1 N2' C16' 151.2(15) . . . . ? N2 Co1 N2' C16' -132(16) . . . . ? O1 Co1 N2' C16' -112.6(16) 6_556 . . . ? O2 Co1 N2' C16' 63.4(16) 2_565 . . . ? O4 Co1 N2' C16' -24.0(17) 5_566 . . . ? Co1 Co1 N2' C16' 30(3) 5_566 . . . ? C16' N2' C17' N3' 2(2) . . . . ? Co1 N2' C17' N3' 175.0(19) . . . . ? N2' C17' N3' C15' -2(2) . . . . ? N2' C17' N3' C18 178.3(16) . . . . ? C16' C15' N3' C17' 0.8(17) . . . . ? C16' C15' N3' C18 -179.2(15) . . . . ? C17 N3 C18 C19 101(3) . . . . ? C15 N3 C18 C19 -71.5(17) . . . . ? C17 N3 C18 N3' 127(8) . . . . ? C15 N3 C18 N3' -46(5) . . . . ? C17' N3' C18 N3 -36(6) . . . . ? C15' N3' C18 N3 144(8) . . . . ? C17' N3' C18 C19 119.8(18) . . . . ? C15' N3' C18 C19 -60.2(19) . . . . ? N3 C18 C19 C19 179.1(8) . . . 7_546 ? N3' C18 C19 C19 173.7(7) . . . 7_546 ? C12 C13 N1 C9 1.4(4) . . . . ? C12 C13 N1 C8 -177.5(3) . . . . ? O3 C9 N1 C13 177.3(3) . . . . ? C10 C9 N1 C13 -4.2(4) . . . . ? O3 C9 N1 C8 -3.8(4) . . . . ? C10 C9 N1 C8 174.8(2) . . . . ? C5 C8 N1 C13 -107.0(3) . . . . ? C5 C8 N1 C9 74.0(3) . . . . ? O2 C1 O1 Co1 -10.1(4) . . . 6 ? C2 C1 O1 Co1 169.71(19) . . . 6 ? O1 C1 O2 Co1 12.7(5) . . . 2_545 ? C2 C1 O2 Co1 -167.1(2) . . . 2_545 ? O5 C14 O4 Co1 2.5(5) . . . 5_566 ? C12 C14 O4 Co1 -177.47(18) . . . 5_566 ? O4 C14 O5 Co1 -3.1(4) . . . . ? C12 C14 O5 Co1 176.90(18) . . . . ? N2 Co1 O5 C14 -164.1(8) . . . . ? N2' Co1 O5 C14 -159.9(7) . . . . ? O1 Co1 O5 C14 91.6(2) 6_556 . . . ? O2 Co1 O5 C14 -70.1(2) 2_565 . . . ? O4 Co1 O5 C14 3.9(4) 5_566 . . . ? Co1 Co1 O5 C14 2.0(2) 5_566 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.342 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.058 #=========================END data_Compound-3 _database_code_depnum_ccdc_archive 'CCDC 873952' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C79 H74 N8 O14 Zn2' _chemical_formula_sum 'C79 H74 N8 O14 Zn2' _chemical_formula_weight 1490.20 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/n _symmetry_space_group_name_hall -p2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1730(6) _cell_length_b 24.0550(10) _cell_length_c 14.2350(6) _cell_angle_alpha 90 _cell_angle_beta 91.543(4) _cell_angle_gamma 90 _cell_volume 4166.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2262 _cell_measurement_theta_min 3.2711 _cell_measurement_theta_max 29.2146 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8268 _exptl_absorpt_correction_T_max 0.8831 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15054 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.1038 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7238 _reflns_number_gt 3494 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In the refienment of the disordered t-butyl group, the PART instructions were used. For the high temperature factor of C atoms, SIMU restraints were used for all the C atoms. For C1, O1, O2, O2W, O3W, O4W and O6, some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR/DELU restraints. In order to give the reasonable O...H distance and H-O-H angle of the water molecule, we used the DFIX restraints. In order to restrict the C-C distance of the t-butyl group, we used the SADI restraints. ; _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^)+(0.0132P)^2^+10.0000P] 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 7238 _refine_ls_number_parameters 533 _refine_ls_number_restraints 1106 _refine_ls_R_factor_all 0.1754 _refine_ls_R_factor_gt 0.0870 _refine_ls_wR_factor_ref 0.1887 _refine_ls_wR_factor_gt 0.1588 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.060 _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 0.18642(7) 0.09642(3) 0.16320(6) 0.0751(3) Uani 1 1 d . . . C1 C 0.5316(7) 0.3287(3) 0.6173(6) 0.0771(17) Uani 1 1 d U . . C2 C 0.4524(6) 0.2814(3) 0.6233(5) 0.0816(16) Uani 1 1 d U . . C3 C 0.4625(7) 0.2420(3) 0.6919(6) 0.0919(17) Uani 1 1 d U . . H3 H 0.5187 0.2448 0.7373 0.110 Uiso 1 1 calc R . . C4 C 0.3877(7) 0.1970(3) 0.6942(6) 0.0936(16) Uani 1 1 d U . . H4 H 0.3958 0.1699 0.7404 0.112 Uiso 1 1 calc R . . C5 C 0.3035(7) 0.1931(3) 0.6285(6) 0.0874(16) Uani 1 1 d U . . C6 C 0.2934(7) 0.2340(3) 0.5614(6) 0.0902(16) Uani 1 1 d U . . H6 H 0.2359 0.2326 0.5171 0.108 Uiso 1 1 calc R . . C7 C 0.3682(6) 0.2772(3) 0.5594(6) 0.0877(16) Uani 1 1 d U . . H7 H 0.3605 0.3042 0.5129 0.105 Uiso 1 1 calc R . . C8 C 0.2271(7) 0.1447(3) 0.6301(6) 0.0942(16) Uani 1 1 d U . . H8A H 0.1572 0.1550 0.6007 0.113 Uiso 1 1 calc R . . H8B H 0.2141 0.1343 0.6947 0.113 Uiso 1 1 calc R . . C9 C 0.3315(7) 0.0555(4) 0.6282(7) 0.0971(17) Uani 1 1 d U . . C10 C 0.3678(7) 0.0102(4) 0.5760(6) 0.1058(19) Uani 1 1 d U . . H10 H 0.4035 -0.0190 0.6068 0.127 Uiso 1 1 calc R . . C11 C 0.3520(7) 0.0078(4) 0.4801(6) 0.1041(19) Uani 1 1 d U . . H11 H 0.3759 -0.0231 0.4471 0.125 Uiso 1 1 calc R . . C12 C 0.3006(6) 0.0513(3) 0.4322(6) 0.0893(17) Uani 1 1 d U . . C13 C 0.2618(6) 0.0944(3) 0.4827(6) 0.0897(16) Uani 1 1 d U . . H13 H 0.2261 0.1235 0.4516 0.108 Uiso 1 1 calc R . . C14 C 0.2839(7) 0.0512(4) 0.3272(6) 0.0906(19) Uani 1 1 d U . . C15 C -0.0159(6) 0.0265(3) 0.2341(5) 0.0873(17) Uani 1 1 d U . . H15 H -0.0244 0.0554 0.2766 0.105 Uiso 1 1 calc R . . C16 C -0.0889(6) -0.0155(3) 0.2349(5) 0.0906(18) Uani 1 1 d U . . H16 H -0.1457 -0.0157 0.2773 0.109 Uiso 1 1 calc R . . C17 C -0.0776(6) -0.0567(3) 0.1737(5) 0.0857(17) Uani 1 1 d U . . H17 H -0.1278 -0.0858 0.1726 0.103 Uiso 1 1 calc R . . C18 C 0.0073(6) -0.0566(3) 0.1117(5) 0.0789(16) Uani 1 1 d U . . H18 H 0.0157 -0.0854 0.0688 0.095 Uiso 1 1 calc R . . C19 C 0.0791(6) -0.0127(3) 0.1155(5) 0.0708(15) Uani 1 1 d U . . C20 C 0.1742(5) -0.0071(3) 0.0505(5) 0.0679(13) Uani 1 1 d U . . C21 C 0.2022(5) -0.0461(3) -0.0145(4) 0.0697(14) Uani 1 1 d U . . H21 H 0.1634 -0.0793 -0.0195 0.084 Uiso 1 1 calc R . . C22 C 0.2902(5) -0.0355(3) -0.0738(5) 0.0684(13) Uani 1 1 d U . . C23 C 0.3470(5) 0.0143(3) -0.0618(5) 0.0703(14) Uani 1 1 d U . . H23 H 0.4067 0.0225 -0.0988 0.084 Uiso 1 1 calc R . . C24 C 0.3136(6) 0.0513(3) 0.0056(5) 0.0705(13) Uani 1 1 d U . . C25 C 0.3633(6) 0.1066(3) 0.0226(5) 0.0770(15) Uani 1 1 d U . . C26 C 0.4518(6) 0.1262(3) -0.0270(5) 0.0897(17) Uani 1 1 d U . . H26 H 0.4843 0.1046 -0.0727 0.108 Uiso 1 1 calc R . . C27 C 0.4909(7) 0.1803(3) -0.0057(6) 0.1003(19) Uani 1 1 d U . . H27 H 0.5495 0.1951 -0.0381 0.120 Uiso 1 1 calc R . . C28 C 0.4422(7) 0.2105(4) 0.0624(6) 0.105(2) Uani 1 1 d U . . H28 H 0.4667 0.2461 0.0770 0.125 Uiso 1 1 calc R . . C29 C 0.3560(7) 0.1873(3) 0.1094(6) 0.0957(18) Uani 1 1 d U . . H29 H 0.3227 0.2081 0.1558 0.115 Uiso 1 1 calc R . . C30 C 0.3192(6) -0.0760(3) -0.1494(5) 0.0695(13) Uani 1 1 d U A . C31 C 0.2461(6) -0.1148(3) -0.1827(5) 0.0807(15) Uani 1 1 d U . . H31 H 0.1764 -0.1159 -0.1575 0.097 Uiso 1 1 calc R . . C32 C 0.2710(6) -0.1523(3) -0.2516(5) 0.0888(15) Uani 1 1 d U A . H32 H 0.2181 -0.1780 -0.2712 0.107 Uiso 1 1 calc R . . C33 C 0.3722(6) -0.1529(3) -0.2926(5) 0.0832(15) Uani 1 1 d U . . C34 C 0.4467(6) -0.1141(3) -0.2596(5) 0.0866(15) Uani 1 1 d U A . H34 H 0.5162 -0.1133 -0.2851 0.104 Uiso 1 1 calc R . . C35 C 0.4223(6) -0.0755(3) -0.1888(5) 0.0792(14) Uani 1 1 d U . . H35 H 0.4749 -0.0498 -0.1685 0.095 Uiso 1 1 calc R A . C36 C 0.4019(7) -0.1916(3) -0.3699(6) 0.0938(15) Uani 0.677(9) 1 d PU A 1 C37 C 0.4260(12) -0.1599(5) -0.4594(8) 0.104(3) Uani 0.677(9) 1 d PDU A 1 H37A H 0.4447 -0.1857 -0.5079 0.156 Uiso 0.677(9) 1 calc PR A 1 H37B H 0.4864 -0.1349 -0.4477 0.156 Uiso 0.677(9) 1 calc PR A 1 H37C H 0.3622 -0.1391 -0.4791 0.156 Uiso 0.677(9) 1 calc PR A 1 C38 C 0.5045(11) -0.2224(6) -0.3404(9) 0.112(3) Uani 0.677(9) 1 d PDU A 1 H38A H 0.5245 -0.2476 -0.3894 0.167 Uiso 0.677(9) 1 calc PR A 1 H38B H 0.4914 -0.2430 -0.2840 0.167 Uiso 0.677(9) 1 calc PR A 1 H38C H 0.5630 -0.1964 -0.3288 0.167 Uiso 0.677(9) 1 calc PR A 1 C39 C 0.3163(11) -0.2350(6) -0.3917(11) 0.115(3) Uani 0.677(9) 1 d PDU A 1 H39A H 0.3404 -0.2582 -0.4420 0.172 Uiso 0.677(9) 1 calc PR A 1 H39B H 0.2485 -0.2172 -0.4101 0.172 Uiso 0.677(9) 1 calc PR A 1 H39C H 0.3052 -0.2574 -0.3369 0.172 Uiso 0.677(9) 1 calc PR A 1 C36' C 0.4019(7) -0.1916(3) -0.3699(6) 0.0938(15) Uani 0.323(9) 1 d PDU A 2 C37' C 0.491(2) -0.1664(11) -0.428(2) 0.106(4) Uani 0.323(9) 1 d PDU A 2 H37D H 0.5096 -0.1917 -0.4771 0.159 Uiso 0.323(9) 1 calc PR A 2 H37E H 0.5545 -0.1592 -0.3887 0.159 Uiso 0.323(9) 1 calc PR A 2 H37F H 0.4647 -0.1321 -0.4552 0.159 Uiso 0.323(9) 1 calc PR A 2 C38' C 0.415(3) -0.2490(7) -0.3316(18) 0.107(4) Uani 0.323(9) 1 d PDU A 2 H38D H 0.4341 -0.2739 -0.3813 0.160 Uiso 0.323(9) 1 calc PR A 2 H38E H 0.3470 -0.2608 -0.3052 0.160 Uiso 0.323(9) 1 calc PR A 2 H38F H 0.4719 -0.2493 -0.2837 0.160 Uiso 0.323(9) 1 calc PR A 2 C39' C 0.3057(17) -0.1974(13) -0.4403(17) 0.107(4) Uani 0.323(9) 1 d PDU A 2 H39D H 0.3255 -0.2224 -0.4896 0.161 Uiso 0.323(9) 1 calc PR A 2 H39E H 0.2882 -0.1616 -0.4666 0.161 Uiso 0.323(9) 1 calc PR A 2 H39F H 0.2429 -0.2118 -0.4089 0.161 Uiso 0.323(9) 1 calc PR A 2 C40 C 0.781(3) 0.1554(14) -0.276(3) 0.103(9) Uani 0.25 1 d PU . . C41 C 0.753(3) 0.1614(12) -0.193(2) 0.079(7) Uani 0.25 1 d PU . . N1 N 0.2741(5) 0.0962(3) 0.5792(4) 0.0854(17) Uani 1 1 d . . . N2 N 0.0685(5) 0.0289(2) 0.1754(4) 0.0749(16) Uani 1 1 d . . . N3 N 0.2290(4) 0.0405(2) 0.0595(3) 0.0627(14) Uani 1 1 d . . . N4 N 0.3186(5) 0.1362(2) 0.0908(4) 0.0772(16) Uani 1 1 d . . . O1 O 0.5952(5) 0.3358(2) 0.6858(4) 0.0999(16) Uani 1 1 d U . . O2 O 0.5278(5) 0.3591(2) 0.5529(4) 0.120(2) Uani 1 1 d U . . O3 O 0.3477(6) 0.0617(3) 0.7132(4) 0.133(2) Uani 1 1 d . . . O4 O 0.2419(5) 0.0940(2) 0.2941(3) 0.0973(16) Uani 1 1 d . . . O5 O 0.3101(6) 0.0104(3) 0.2822(5) 0.139(2) Uani 1 1 d . . . O6 O 0.6684(13) 0.1669(6) -0.1767(10) 0.053(4) Uani 0.25 1 d PU . . O1W O 0.4393(6) -0.0653(3) 0.2090(5) 0.149(3) Uani 0.90 1 d PD . . H1A H 0.5126 -0.0575 0.2334 0.224 Uiso 0.90 1 d PRD . . H1B H 0.3978 -0.0412 0.2434 0.224 Uiso 0.90 1 d PRD . . O2W O 0.1535(15) 0.2166(7) 0.3632(11) 0.101(5) Uani 0.35 1 d PU . . O3W O 0.0764(18) 0.1881(9) 0.3894(14) 0.118(6) Uani 0.30 1 d PU . . O4W O -0.004(2) 0.1561(11) 0.4983(19) 0.104(8) Uani 0.20 1 d PU . . 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 0.0867(6) 0.0670(5) 0.0723(5) -0.0111(4) 0.0150(4) 0.0016(5) C1 0.087(4) 0.064(3) 0.080(4) 0.004(3) 0.009(3) 0.007(3) C2 0.092(4) 0.071(3) 0.083(4) 0.004(3) 0.012(3) 0.002(3) C3 0.100(4) 0.083(3) 0.093(3) 0.005(3) 0.003(3) -0.008(3) C4 0.107(4) 0.083(3) 0.091(3) 0.008(3) 0.008(3) -0.009(3) C5 0.096(3) 0.082(3) 0.084(3) -0.002(3) 0.016(3) -0.008(3) C6 0.099(3) 0.082(3) 0.090(3) -0.002(3) 0.010(3) 0.000(3) C7 0.101(4) 0.077(3) 0.086(3) 0.002(3) 0.013(3) 0.001(3) C8 0.104(3) 0.090(3) 0.090(3) -0.002(3) 0.016(3) -0.012(3) C9 0.110(4) 0.093(4) 0.089(4) 0.006(3) 0.010(3) -0.012(3) C10 0.119(4) 0.096(4) 0.102(4) 0.009(4) 0.004(4) -0.003(3) C11 0.117(4) 0.093(4) 0.102(4) 0.000(4) 0.007(4) 0.000(4) C12 0.098(4) 0.085(4) 0.085(4) 0.006(3) 0.010(3) -0.008(3) C13 0.098(3) 0.085(3) 0.087(3) 0.003(3) 0.011(3) -0.013(3) C14 0.095(4) 0.086(4) 0.091(4) 0.001(4) 0.005(4) -0.005(4) C15 0.091(4) 0.092(4) 0.081(4) -0.009(3) 0.030(3) -0.003(3) C16 0.089(4) 0.099(4) 0.085(4) -0.006(4) 0.038(3) -0.013(4) C17 0.086(4) 0.090(4) 0.082(4) -0.002(3) 0.026(3) -0.015(3) C18 0.082(3) 0.082(3) 0.074(3) -0.006(3) 0.028(3) -0.009(3) C19 0.076(3) 0.072(3) 0.066(3) -0.001(3) 0.019(3) -0.005(3) C20 0.073(3) 0.068(3) 0.064(3) -0.005(2) 0.018(2) -0.007(3) C21 0.075(3) 0.066(3) 0.069(3) -0.005(3) 0.019(2) -0.010(3) C22 0.074(3) 0.066(3) 0.066(3) -0.005(2) 0.017(2) -0.003(2) C23 0.076(3) 0.066(3) 0.070(3) -0.004(3) 0.018(2) -0.009(3) C24 0.075(3) 0.066(3) 0.071(3) -0.004(3) 0.015(3) -0.008(2) C25 0.084(3) 0.071(3) 0.078(3) -0.004(3) 0.017(3) -0.015(3) C26 0.100(4) 0.081(3) 0.090(4) -0.010(3) 0.020(3) -0.020(3) C27 0.111(4) 0.087(4) 0.105(4) -0.006(3) 0.026(3) -0.030(3) C28 0.121(4) 0.084(4) 0.109(4) -0.015(4) 0.023(4) -0.027(4) C29 0.109(4) 0.083(4) 0.096(4) -0.015(3) 0.020(3) -0.017(3) C30 0.074(3) 0.067(3) 0.069(3) -0.006(2) 0.019(2) -0.007(2) C31 0.083(3) 0.080(3) 0.081(3) -0.013(3) 0.028(3) -0.008(3) C32 0.095(3) 0.085(3) 0.088(3) -0.020(3) 0.023(3) -0.009(3) C33 0.090(3) 0.081(3) 0.080(3) -0.017(3) 0.023(3) -0.004(3) C34 0.089(3) 0.088(3) 0.084(3) -0.011(3) 0.024(3) 0.004(3) C35 0.083(3) 0.077(3) 0.079(3) -0.008(3) 0.018(3) -0.005(3) C36 0.098(3) 0.093(3) 0.091(3) -0.015(3) 0.022(3) 0.000(3) C37 0.109(6) 0.110(6) 0.093(6) -0.017(5) 0.011(5) 0.010(5) C38 0.124(6) 0.109(6) 0.104(6) -0.024(5) 0.021(5) 0.019(5) C39 0.128(6) 0.108(6) 0.109(6) -0.025(5) 0.034(5) -0.002(6) C36' 0.098(3) 0.093(3) 0.091(3) -0.015(3) 0.022(3) 0.000(3) C37' 0.111(7) 0.108(6) 0.101(7) -0.021(6) 0.028(6) 0.004(7) C38' 0.115(7) 0.105(7) 0.102(7) -0.018(6) 0.021(6) 0.004(6) C39' 0.115(7) 0.105(7) 0.102(7) -0.018(6) 0.020(6) 0.009(6) C40 0.107(11) 0.095(11) 0.106(11) 0.004(9) 0.007(9) -0.016(8) C41 0.084(10) 0.074(10) 0.076(10) -0.015(8) -0.014(8) -0.007(8) N1 0.089(4) 0.081(4) 0.086(4) 0.005(4) 0.014(3) -0.022(4) N2 0.083(4) 0.076(4) 0.068(4) -0.011(3) 0.025(3) 0.001(3) N3 0.066(3) 0.063(3) 0.060(3) 0.000(3) 0.011(3) -0.005(3) N4 0.090(4) 0.063(4) 0.080(4) -0.009(3) 0.012(3) -0.011(3) O1 0.106(4) 0.080(4) 0.115(4) 0.010(3) 0.011(3) -0.017(3) O2 0.145(5) 0.097(4) 0.119(4) 0.020(3) 0.013(4) -0.015(4) O3 0.169(6) 0.145(6) 0.084(4) 0.016(4) 0.009(4) -0.037(5) O4 0.129(5) 0.092(4) 0.071(3) -0.006(3) 0.003(3) -0.014(4) O5 0.156(6) 0.139(6) 0.122(5) -0.047(5) -0.009(4) 0.045(5) O6 0.060(8) 0.041(7) 0.059(7) -0.014(6) 0.023(6) -0.015(6) O1W 0.139(6) 0.155(7) 0.155(7) -0.065(5) 0.038(5) -0.017(5) O2W 0.122(9) 0.094(8) 0.088(8) -0.014(7) -0.013(7) 0.012(7) O3W 0.122(10) 0.118(10) 0.112(10) -0.028(8) -0.009(8) 0.039(8) O4W 0.099(11) 0.099(11) 0.114(11) -0.006(9) 0.006(9) 0.037(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O4 1.965(5) . ? Zn1 O1 2.004(5) 4_565 ? Zn1 N3 2.073(5) . ? Zn1 N4 2.158(6) . ? Zn1 N2 2.178(6) . ? C1 O2 1.173(8) . ? C1 O1 1.240(8) . ? C1 C2 1.495(10) . ? C2 C7 1.356(10) . ? C2 C3 1.363(10) . ? C3 C4 1.416(10) . ? C3 H3 0.9300 . ? C4 C5 1.372(10) . ? C4 H4 0.9300 . ? C5 C6 1.374(10) . ? C5 C8 1.491(10) . ? C6 C7 1.383(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.494(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O3 1.230(9) . ? C9 N1 1.382(10) . ? C9 C10 1.398(11) . ? C10 C11 1.375(10) . ? C10 H10 0.9300 . ? C11 C12 1.388(10) . ? C11 H11 0.9300 . ? C12 C13 1.355(10) . ? C12 C14 1.503(11) . ? C13 N1 1.378(9) . ? C13 H13 0.9300 . ? C14 O5 1.219(9) . ? C14 O4 1.237(9) . ? C15 C16 1.345(9) . ? C15 N2 1.343(8) . ? C15 H15 0.9300 . ? C16 C17 1.329(9) . ? C16 H16 0.9300 . ? C17 C18 1.377(9) . ? C17 H17 0.9300 . ? C18 C19 1.371(9) . ? C18 H18 0.9300 . ? C19 N2 1.323(8) . ? C19 C20 1.508(8) . ? C20 N3 1.330(7) . ? C20 C21 1.366(8) . ? C21 C22 1.405(8) . ? C21 H21 0.9300 . ? C22 C23 1.391(8) . ? C22 C30 1.501(9) . ? C23 C24 1.378(8) . ? C23 H23 0.9300 . ? C24 N3 1.327(7) . ? C24 C25 1.479(9) . ? C25 N4 1.333(8) . ? C25 C26 1.386(9) . ? C26 C27 1.415(10) . ? C26 H26 0.9300 . ? C27 C28 1.360(10) . ? C27 H27 0.9300 . ? C28 C29 1.377(10) . ? C28 H28 0.9300 . ? C29 N4 1.335(8) . ? C29 H29 0.9300 . ? C30 C31 1.367(9) . ? C30 C35 1.388(9) . ? C31 C32 1.372(9) . ? C31 H31 0.9300 . ? C32 C33 1.377(9) . ? C32 H32 0.9300 . ? C33 C34 1.376(9) . ? C33 C36 1.494(10) . ? C34 C35 1.408(9) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C38 1.503(11) . ? C36 C39 1.502(11) . ? C36 C37 1.520(11) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C37' H37D 0.9600 . ? C37' H37E 0.9600 . ? C37' H37F 0.9600 . ? C38' H38D 0.9600 . ? C38' H38E 0.9600 . ? C38' H38F 0.9600 . ? C39' H39D 0.9600 . ? C39' H39E 0.9600 . ? C39' H39F 0.9600 . ? C40 C41 1.25(4) . ? C41 O6 1.06(3) . ? O1 Zn1 2.004(5) 4_666 ? O1W H1A 0.9661 . ? O1W H1B 0.9195 . ? O2W O3W 1.23(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Zn1 O1 92.9(3) . 4_565 ? O4 Zn1 N3 124.7(2) . . ? O1 Zn1 N3 142.4(2) 4_565 . ? O4 Zn1 N4 103.0(2) . . ? O1 Zn1 N4 98.0(2) 4_565 . ? N3 Zn1 N4 75.2(2) . . ? O4 Zn1 N2 96.4(2) . . ? O1 Zn1 N2 103.0(2) 4_565 . ? N3 Zn1 N2 75.6(2) . . ? N4 Zn1 N2 150.5(2) . . ? O2 C1 O1 122.6(8) . . ? O2 C1 C2 120.5(8) . . ? O1 C1 C2 116.7(8) . . ? C7 C2 C3 118.8(8) . . ? C7 C2 C1 119.7(7) . . ? C3 C2 C1 121.6(8) . . ? C2 C3 C4 120.1(8) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.4(8) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 118.5(8) . . ? C6 C5 C8 121.7(8) . . ? C4 C5 C8 119.8(8) . . ? C5 C6 C7 120.4(8) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C2 C7 C6 121.9(8) . . ? C2 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C5 C8 N1 110.8(6) . . ? C5 C8 H8A 109.5 . . ? N1 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? O3 C9 N1 118.4(9) . . ? O3 C9 C10 125.0(10) . . ? N1 C9 C10 116.6(9) . . ? C11 C10 C9 121.5(9) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 120.4(9) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 118.4(8) . . ? C13 C12 C14 119.3(8) . . ? C11 C12 C14 122.3(8) . . ? C12 C13 N1 121.5(8) . . ? C12 C13 H13 119.2 . . ? N1 C13 H13 119.2 . . ? O5 C14 O4 125.4(9) . . ? O5 C14 C12 119.6(9) . . ? O4 C14 C12 115.0(8) . . ? C16 C15 N2 123.7(7) . . ? C16 C15 H15 118.2 . . ? N2 C15 H15 118.2 . . ? C17 C16 C15 118.3(7) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C16 C17 C18 120.8(7) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 117.7(7) . . ? C19 C18 H18 121.2 . . ? C17 C18 H18 121.2 . . ? N2 C19 C18 122.3(6) . . ? N2 C19 C20 114.7(6) . . ? C18 C19 C20 122.9(6) . . ? N3 C20 C21 121.5(6) . . ? N3 C20 C19 114.1(6) . . ? C21 C20 C19 124.4(6) . . ? C20 C21 C22 119.4(6) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 117.8(6) . . ? C23 C22 C30 121.4(6) . . ? C21 C22 C30 120.7(6) . . ? C24 C23 C22 119.1(6) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? N3 C24 C23 121.7(6) . . ? N3 C24 C25 113.7(6) . . ? C23 C24 C25 124.6(6) . . ? N4 C25 C26 121.8(7) . . ? N4 C25 C24 115.2(6) . . ? C26 C25 C24 122.9(7) . . ? C25 C26 C27 117.8(7) . . ? C25 C26 H26 121.1 . . ? C27 C26 H26 121.1 . . ? C28 C27 C26 119.5(8) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 118.9(8) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? N4 C29 C28 122.4(8) . . ? N4 C29 H29 118.8 . . ? C28 C29 H29 118.8 . . ? C31 C30 C35 117.0(6) . . ? C31 C30 C22 121.9(6) . . ? C35 C30 C22 121.1(6) . . ? C32 C31 C30 122.9(7) . . ? C32 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? C31 C32 C33 121.8(7) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C34 C33 C32 116.0(7) . . ? C34 C33 C36 120.3(7) . . ? C32 C33 C36 123.7(7) . . ? C35 C34 C33 122.8(7) . . ? C35 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? C34 C35 C30 119.6(7) . . ? C34 C35 H35 120.2 . . ? C30 C35 H35 120.2 . . ? C38 C36 C33 108.5(8) . . ? C38 C36 C39 106.4(9) . . ? C33 C36 C39 113.9(8) . . ? C38 C36 C37 107.7(9) . . ? C33 C36 C37 111.1(8) . . ? C39 C36 C37 109.0(9) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? H37D C37' H37E 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? H38D C38' H38E 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? H39D C39' H39E 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? O6 C41 C40 121(3) . . ? C13 N1 C9 121.4(8) . . ? C13 N1 C8 118.4(7) . . ? C9 N1 C8 120.2(7) . . ? C19 N2 C15 117.3(6) . . ? C19 N2 Zn1 115.9(4) . . ? C15 N2 Zn1 126.8(5) . . ? C20 N3 C24 120.5(6) . . ? C20 N3 Zn1 119.6(4) . . ? C24 N3 Zn1 119.8(4) . . ? C29 N4 C25 119.5(6) . . ? C29 N4 Zn1 124.7(5) . . ? C25 N4 Zn1 115.8(5) . . ? C1 O1 Zn1 108.9(5) . 4_666 ? C14 O4 Zn1 121.0(6) . . ? H1A O1W H1B 101.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -7.4(12) . . . . ? O1 C1 C2 C7 168.1(7) . . . . ? O2 C1 C2 C3 172.8(8) . . . . ? O1 C1 C2 C3 -11.7(11) . . . . ? C7 C2 C3 C4 1.7(12) . . . . ? C1 C2 C3 C4 -178.4(7) . . . . ? C2 C3 C4 C5 -1.2(12) . . . . ? C3 C4 C5 C6 -0.4(12) . . . . ? C3 C4 C5 C8 178.3(7) . . . . ? C4 C5 C6 C7 1.4(11) . . . . ? C8 C5 C6 C7 -177.3(7) . . . . ? C3 C2 C7 C6 -0.7(12) . . . . ? C1 C2 C7 C6 179.4(7) . . . . ? C5 C6 C7 C2 -0.9(12) . . . . ? C6 C5 C8 N1 94.5(9) . . . . ? C4 C5 C8 N1 -84.2(9) . . . . ? O3 C9 C10 C11 -176.1(8) . . . . ? N1 C9 C10 C11 3.2(12) . . . . ? C9 C10 C11 C12 1.0(13) . . . . ? C10 C11 C12 C13 -3.2(12) . . . . ? C10 C11 C12 C14 178.5(7) . . . . ? C11 C12 C13 N1 1.1(12) . . . . ? C14 C12 C13 N1 179.4(7) . . . . ? C13 C12 C14 O5 -173.8(8) . . . . ? C11 C12 C14 O5 4.5(13) . . . . ? C13 C12 C14 O4 5.2(11) . . . . ? C11 C12 C14 O4 -176.5(8) . . . . ? N2 C15 C16 C17 -0.7(13) . . . . ? C15 C16 C17 C18 0.8(12) . . . . ? C16 C17 C18 C19 -0.2(11) . . . . ? C17 C18 C19 N2 -0.5(11) . . . . ? C17 C18 C19 C20 -178.8(7) . . . . ? N2 C19 C20 N3 -3.8(9) . . . . ? C18 C19 C20 N3 174.6(6) . . . . ? N2 C19 C20 C21 177.7(7) . . . . ? C18 C19 C20 C21 -3.8(11) . . . . ? N3 C20 C21 C22 -0.6(10) . . . . ? C19 C20 C21 C22 177.7(6) . . . . ? C20 C21 C22 C23 1.5(10) . . . . ? C20 C21 C22 C30 -176.6(6) . . . . ? C21 C22 C23 C24 -1.3(10) . . . . ? C30 C22 C23 C24 176.8(6) . . . . ? C22 C23 C24 N3 0.3(10) . . . . ? C22 C23 C24 C25 -177.1(7) . . . . ? N3 C24 C25 N4 2.1(9) . . . . ? C23 C24 C25 N4 179.6(7) . . . . ? N3 C24 C25 C26 -179.3(7) . . . . ? C23 C24 C25 C26 -1.7(12) . . . . ? N4 C25 C26 C27 -2.6(12) . . . . ? C24 C25 C26 C27 178.8(7) . . . . ? C25 C26 C27 C28 0.8(12) . . . . ? C26 C27 C28 C29 0.4(13) . . . . ? C27 C28 C29 N4 0.2(14) . . . . ? C23 C22 C30 C31 -158.2(7) . . . . ? C21 C22 C30 C31 19.8(10) . . . . ? C23 C22 C30 C35 21.8(10) . . . . ? C21 C22 C30 C35 -160.2(7) . . . . ? C35 C30 C31 C32 0.2(11) . . . . ? C22 C30 C31 C32 -179.9(7) . . . . ? C30 C31 C32 C33 -0.5(12) . . . . ? C31 C32 C33 C34 0.6(12) . . . . ? C31 C32 C33 C36 -178.0(7) . . . . ? C32 C33 C34 C35 -0.5(11) . . . . ? C36 C33 C34 C35 178.2(7) . . . . ? C33 C34 C35 C30 0.2(11) . . . . ? C31 C30 C35 C34 0.0(10) . . . . ? C22 C30 C35 C34 -180.0(6) . . . . ? C34 C33 C36 C38 56.1(11) . . . . ? C32 C33 C36 C38 -125.3(10) . . . . ? C34 C33 C36 C39 174.4(10) . . . . ? C32 C33 C36 C39 -7.1(13) . . . . ? C34 C33 C36 C37 -62.1(11) . . . . ? C32 C33 C36 C37 116.4(10) . . . . ? C12 C13 N1 C9 3.4(11) . . . . ? C12 C13 N1 C8 -178.8(7) . . . . ? O3 C9 N1 C13 174.0(7) . . . . ? C10 C9 N1 C13 -5.4(11) . . . . ? O3 C9 N1 C8 -3.8(11) . . . . ? C10 C9 N1 C8 176.8(7) . . . . ? C5 C8 N1 C13 -82.4(8) . . . . ? C5 C8 N1 C9 95.4(8) . . . . ? C18 C19 N2 C15 0.5(11) . . . . ? C20 C19 N2 C15 179.0(6) . . . . ? C18 C19 N2 Zn1 -176.5(5) . . . . ? C20 C19 N2 Zn1 1.9(8) . . . . ? C16 C15 N2 C19 0.1(11) . . . . ? C16 C15 N2 Zn1 176.8(6) . . . . ? O4 Zn1 N2 C19 -124.2(5) . . . . ? O1 Zn1 N2 C19 141.3(5) 4_565 . . . ? N3 Zn1 N2 C19 0.0(5) . . . . ? N4 Zn1 N2 C19 7.0(8) . . . . ? O4 Zn1 N2 C15 59.1(6) . . . . ? O1 Zn1 N2 C15 -35.4(7) 4_565 . . . ? N3 Zn1 N2 C15 -176.7(7) . . . . ? N4 Zn1 N2 C15 -169.7(6) . . . . ? C21 C20 N3 C24 -0.5(10) . . . . ? C19 C20 N3 C24 -178.9(6) . . . . ? C21 C20 N3 Zn1 -177.5(5) . . . . ? C19 C20 N3 Zn1 4.1(8) . . . . ? C23 C24 N3 C20 0.6(10) . . . . ? C25 C24 N3 C20 178.3(6) . . . . ? C23 C24 N3 Zn1 177.6(5) . . . . ? C25 C24 N3 Zn1 -4.7(8) . . . . ? O4 Zn1 N3 C20 85.5(5) . . . . ? O1 Zn1 N3 C20 -95.0(6) 4_565 . . . ? N4 Zn1 N3 C20 -178.8(5) . . . . ? N2 Zn1 N3 C20 -2.4(5) . . . . ? O4 Zn1 N3 C24 -91.5(5) . . . . ? O1 Zn1 N3 C24 88.0(6) 4_565 . . . ? N4 Zn1 N3 C24 4.2(5) . . . . ? N2 Zn1 N3 C24 -179.4(5) . . . . ? C28 C29 N4 C25 -2.0(12) . . . . ? C28 C29 N4 Zn1 178.6(6) . . . . ? C26 C25 N4 C29 3.2(11) . . . . ? C24 C25 N4 C29 -178.1(7) . . . . ? C26 C25 N4 Zn1 -177.3(6) . . . . ? C24 C25 N4 Zn1 1.3(8) . . . . ? O4 Zn1 N4 C29 -60.5(7) . . . . ? O1 Zn1 N4 C29 34.4(6) 4_565 . . . ? N3 Zn1 N4 C29 176.6(7) . . . . ? N2 Zn1 N4 C29 169.6(6) . . . . ? O4 Zn1 N4 C25 120.1(5) . . . . ? O1 Zn1 N4 C25 -145.0(5) 4_565 . . . ? N3 Zn1 N4 C25 -2.8(5) . . . . ? N2 Zn1 N4 C25 -9.8(8) . . . . ? O2 C1 O1 Zn1 -1.7(10) . . . 4_666 ? C2 C1 O1 Zn1 -177.1(5) . . . 4_666 ? O5 C14 O4 Zn1 11.3(12) . . . . ? C12 C14 O4 Zn1 -167.6(5) . . . . ? O1 Zn1 O4 C14 162.2(6) 4_565 . . . ? N3 Zn1 O4 C14 -18.1(7) . . . . ? N4 Zn1 O4 C14 -98.9(6) . . . . ? N2 Zn1 O4 C14 58.7(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1B O5 0.92 1.74 2.640(9) 166.3 . O1W H1A O3 0.97 1.85 2.793(10) 165.4 3_656 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.494 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.065 #=========================END data_Compound-4 _database_code_depnum_ccdc_archive 'CCDC 873953' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H32 Co N4 O5' _chemical_formula_sum 'C39 H32 Co N4 O5' _chemical_formula_weight 695.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc _symmetry_space_group_name_hall 'c -2yc' 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' _cell_length_a 12.6170(8) _cell_length_b 25.8660(10) _cell_length_c 11.4610(7) _cell_angle_alpha 90 _cell_angle_beta 120.449(8) _cell_angle_gamma 90 _cell_volume 3224.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1830 _cell_measurement_theta_min 3.0088 _cell_measurement_theta_max 29.1443 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1444 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8393 _exptl_absorpt_correction_T_max 0.8919 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6208 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3966 _reflns_number_gt 3410 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In the refienment of the disordered t-butyl group, the PART instructions were used. For C36-C39 and C36'-C39', some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. In order to restrict the C-C distance of t-butyl group, we used the SADI restraints. ; _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(15) _refine_ls_number_reflns 3966 _refine_ls_number_parameters 470 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.997 _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 1.26643(5) 0.884026(18) 0.42711(5) 0.03220(15) Uani 1 1 d . . . C1 C 1.5587(4) 0.63795(17) -0.0385(4) 0.0340(11) Uani 1 1 d . . . C2 C 1.4215(4) 0.63286(15) -0.1235(4) 0.0316(10) Uani 1 1 d . . . C3 C 1.3476(4) 0.67276(15) -0.1377(4) 0.0321(10) Uani 1 1 d . . . H3 H 1.3828 0.7021 -0.0853 0.039 Uiso 1 1 calc R . . C4 C 1.1637(4) 0.62888(16) -0.3033(5) 0.0401(11) Uani 1 1 d . . . C5 C 1.2403(5) 0.58575(19) -0.2801(5) 0.0477(14) Uani 1 1 d . . . H5 H 1.2046 0.5547 -0.3231 0.057 Uiso 1 1 calc R . . C6 C 1.3636(5) 0.58769(17) -0.1978(5) 0.0447(14) Uani 1 1 d . . . H6 H 1.4109 0.5589 -0.1900 0.054 Uiso 1 1 calc R . . C7 C 1.1517(4) 0.72071(16) -0.2486(4) 0.0419(12) Uani 1 1 d . . . H7A H 1.0648 0.7122 -0.2975 0.050 Uiso 1 1 calc R . . H7B H 1.1673 0.7436 -0.3053 0.050 Uiso 1 1 calc R . . C8 C 1.1815(4) 0.74880(15) -0.1204(4) 0.0354(11) Uani 1 1 d . . . C9 C 1.1193(4) 0.73626(15) -0.0544(4) 0.0383(11) Uani 1 1 d . . . H9 H 1.0614 0.7098 -0.0876 0.046 Uiso 1 1 calc R . . C10 C 1.1424(4) 0.76271(16) 0.0608(4) 0.0394(11) Uani 1 1 d . . . H10 H 1.0993 0.7542 0.1042 0.047 Uiso 1 1 calc R . . C11 C 1.2299(4) 0.80221(15) 0.1126(4) 0.0338(10) Uani 1 1 d . . . C12 C 1.2927(4) 0.81374(16) 0.0476(4) 0.0387(11) Uani 1 1 d . . . H12 H 1.3526 0.8394 0.0823 0.046 Uiso 1 1 calc R . . C13 C 1.2682(5) 0.78775(14) -0.0695(6) 0.0402(10) Uani 1 1 d . . . H13 H 1.3103 0.7966 -0.1137 0.048 Uiso 1 1 calc R . . C14 C 1.2510(4) 0.83180(16) 0.2346(4) 0.0383(11) Uani 1 1 d . . . C15 C 1.1759(5) 0.97266(19) 0.2159(5) 0.0522(14) Uani 1 1 d . . . H15 H 1.1305 0.9465 0.1551 0.063 Uiso 1 1 calc R . . C16 C 1.1638(4) 1.02216(18) 0.1683(4) 0.0516(14) Uani 1 1 d . . . H16 H 1.1112 1.0294 0.0771 0.062 Uiso 1 1 calc R . . C17 C 1.2297(4) 1.06068(17) 0.2564(5) 0.0483(13) Uani 1 1 d . . . H17 H 1.2231 1.0946 0.2264 0.058 Uiso 1 1 calc R . . C18 C 1.3067(4) 1.04839(16) 0.3915(4) 0.0403(12) Uani 1 1 d . . . H18 H 1.3527 1.0740 0.4538 0.048 Uiso 1 1 calc R . . C19 C 1.3144(4) 0.99824(14) 0.4324(4) 0.0294(10) Uani 1 1 d . . . C20 C 1.3955(4) 0.98015(15) 0.5719(4) 0.0305(10) Uani 1 1 d . . . C21 C 1.4721(4) 1.01126(16) 0.6810(4) 0.0370(11) Uani 1 1 d . . . H21 H 1.4711 1.0469 0.6699 0.044 Uiso 1 1 calc R . . C22 C 1.5500(4) 0.98957(15) 0.8060(4) 0.0321(10) Uani 1 1 d . . . C23 C 1.5466(4) 0.93587(15) 0.8184(4) 0.0342(10) Uani 1 1 d . . . H23 H 1.5976 0.9198 0.9010 0.041 Uiso 1 1 calc R . . C24 C 1.4676(4) 0.90711(15) 0.7075(4) 0.0308(10) Uani 1 1 d . . . C25 C 1.4552(4) 0.84963(15) 0.7055(4) 0.0308(10) Uani 1 1 d . . . C26 C 1.5200(4) 0.81907(16) 0.8181(5) 0.0432(12) Uani 1 1 d . . . H26 H 1.5722 0.8339 0.9021 0.052 Uiso 1 1 calc R . . C27 C 1.5064(5) 0.76576(17) 0.8047(5) 0.0498(13) Uani 1 1 d . . . H27 H 1.5498 0.7442 0.8790 0.060 Uiso 1 1 calc R . . C28 C 1.4269(5) 0.74573(17) 0.6785(5) 0.0488(13) Uani 1 1 d . . . H28 H 1.4167 0.7102 0.6661 0.059 Uiso 1 1 calc R . . C29 C 1.3632(4) 0.77847(16) 0.5719(5) 0.0416(12) Uani 1 1 d . . . H29 H 1.3075 0.7645 0.4879 0.050 Uiso 1 1 calc R . . C30 C 1.6332(4) 1.02233(16) 0.9238(4) 0.0365(11) Uani 1 1 d . A . C31 C 1.5935(4) 1.06817(17) 0.9494(4) 0.0448(13) Uani 1 1 d . . . H31 H 1.5133 1.0793 0.8915 0.054 Uiso 1 1 calc R . . C32 C 1.6719(5) 1.09794(19) 1.0605(5) 0.0464(14) Uani 1 1 d . A . H32 H 1.6429 1.1288 1.0758 0.056 Uiso 1 1 calc R . . C33 C 1.7921(4) 1.08327(18) 1.1497(5) 0.0361(12) Uani 1 1 d . . . C34 C 1.8319(4) 1.03742(16) 1.1206(4) 0.0465(13) Uani 1 1 d . A . H34 H 1.9129 1.0269 1.1763 0.056 Uiso 1 1 calc R . . C35 C 1.7535(4) 1.00702(16) 1.0102(4) 0.0446(12) Uani 1 1 d . . . H35 H 1.7819 0.9762 0.9943 0.054 Uiso 1 1 calc R A . C36 C 1.8806(4) 1.11744(17) 1.2691(4) 0.0454(12) Uani 0.100(8) 1 d PU A 1 C37 C 1.849(5) 1.1732(19) 1.239(5) 0.061(10) Uani 0.100(8) 1 d PDU A 1 H37A H 1.7875 1.1823 1.2609 0.092 Uiso 0.100(8) 1 calc PR A 1 H37B H 1.8186 1.1796 1.1448 0.092 Uiso 0.100(8) 1 calc PR A 1 H37C H 1.9215 1.1937 1.2924 0.092 Uiso 0.100(8) 1 calc PR A 1 C38 C 2.020(5) 1.104(2) 1.332(7) 0.063(18) Uani 0.100(8) 1 d PDU A 1 H38A H 2.0679 1.1260 1.4090 0.094 Uiso 0.100(8) 1 calc PR A 1 H38B H 2.0438 1.1102 1.2655 0.094 Uiso 0.100(8) 1 calc PR A 1 H38C H 2.0338 1.0688 1.3591 0.094 Uiso 0.100(8) 1 calc PR A 1 C39 C 1.873(6) 1.099(2) 1.397(5) 0.069(19) Uani 0.100(8) 1 d PU A 1 H39A H 1.7917 1.0856 1.3673 0.104 Uiso 0.100(8) 1 calc PR A 1 H39B H 1.8887 1.1275 1.4569 0.104 Uiso 0.100(8) 1 calc PR A 1 H39C H 1.9322 1.0722 1.4439 0.104 Uiso 0.100(8) 1 calc PR A 1 C36' C 1.8806(4) 1.11744(17) 1.2691(4) 0.0454(12) Uani 0.900(8) 1 d PD A 2 C37' C 1.8119(6) 1.1451(3) 1.3284(6) 0.081(3) Uani 0.900(8) 1 d PDU A 2 H37D H 1.8682 1.1666 1.4026 0.122 Uiso 0.900(8) 1 calc PR A 2 H37E H 1.7762 1.1201 1.3602 0.122 Uiso 0.900(8) 1 calc PR A 2 H37F H 1.7481 1.1662 1.2600 0.122 Uiso 0.900(8) 1 calc PR A 2 C38' C 1.9367(7) 1.1563(3) 1.2183(6) 0.079(3) Uani 0.900(8) 1 d PU A 2 H38D H 1.9739 1.1386 1.1745 0.118 Uiso 0.900(8) 1 calc PR A 2 H38E H 1.9980 1.1760 1.2931 0.118 Uiso 0.900(8) 1 calc PR A 2 H38F H 1.8738 1.1791 1.1548 0.118 Uiso 0.900(8) 1 calc PR A 2 C39' C 1.9817(7) 1.0859(2) 1.3830(6) 0.084(3) Uani 0.900(8) 1 d PU A 2 H39D H 2.0324 1.0704 1.3523 0.125 Uiso 0.900(8) 1 calc PR A 2 H39E H 1.9456 1.0593 1.4101 0.125 Uiso 0.900(8) 1 calc PR A 2 H39F H 2.0311 1.1081 1.4587 0.125 Uiso 0.900(8) 1 calc PR A 2 N1 N 1.2239(3) 0.67246(12) -0.2247(3) 0.0329(8) Uani 1 1 d . . . N2 N 1.3776(3) 0.82941(14) 0.5830(4) 0.0351(10) Uani 1 1 d . . . N3 N 1.3933(3) 0.92891(12) 0.5873(3) 0.0305(8) Uani 1 1 d . . . N4 N 1.2495(3) 0.96043(13) 0.3448(3) 0.0382(9) Uani 1 1 d . . . O1 O 1.6194(3) 0.60262(10) -0.0543(3) 0.0416(7) Uani 1 1 d . . . O2 O 1.6029(3) 0.67592(12) 0.0362(3) 0.0510(9) Uani 1 1 d . . . O3 O 1.0509(3) 0.62996(12) -0.3860(3) 0.0513(9) Uani 1 1 d . . . O4 O 1.3447(3) 0.85912(12) 0.2978(3) 0.0562(9) Uani 1 1 d . . . O5 O 1.1721(3) 0.83015(13) 0.2710(3) 0.0475(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0309(3) 0.0302(3) 0.0317(3) -0.0046(3) 0.0131(2) -0.0054(3) C1 0.036(3) 0.033(2) 0.036(3) 0.013(2) 0.021(2) 0.007(2) C2 0.029(3) 0.035(3) 0.033(2) 0.003(2) 0.017(2) 0.004(2) C3 0.033(3) 0.032(2) 0.031(2) -0.006(2) 0.015(2) -0.001(2) C4 0.040(3) 0.039(3) 0.044(3) 0.001(2) 0.023(2) 0.002(2) C5 0.052(4) 0.038(3) 0.051(3) -0.011(2) 0.025(3) -0.004(3) C6 0.052(4) 0.029(3) 0.053(3) 0.002(3) 0.026(3) 0.008(2) C7 0.039(3) 0.046(3) 0.033(2) 0.000(2) 0.012(2) 0.015(2) C8 0.035(3) 0.031(2) 0.039(3) 0.000(2) 0.018(2) 0.012(2) C9 0.035(3) 0.036(2) 0.042(3) -0.011(2) 0.018(2) -0.011(2) C10 0.041(3) 0.038(3) 0.047(3) -0.005(2) 0.028(2) -0.004(2) C11 0.028(2) 0.034(2) 0.038(3) -0.006(2) 0.015(2) -0.001(2) C12 0.028(3) 0.041(3) 0.048(3) -0.006(2) 0.020(2) 0.000(2) C13 0.042(2) 0.043(2) 0.046(2) 0.003(3) 0.030(2) 0.004(3) C14 0.041(3) 0.029(2) 0.040(3) -0.004(2) 0.017(2) -0.001(2) C15 0.056(3) 0.049(3) 0.031(3) -0.004(2) 0.006(3) -0.014(2) C16 0.052(3) 0.054(3) 0.027(3) 0.007(2) 0.003(2) -0.005(3) C17 0.051(3) 0.043(3) 0.043(3) 0.010(2) 0.018(3) 0.002(2) C18 0.040(3) 0.034(3) 0.036(3) 0.000(2) 0.011(2) -0.003(2) C19 0.031(3) 0.028(2) 0.029(2) -0.001(2) 0.015(2) -0.0051(18) C20 0.029(3) 0.029(2) 0.030(2) -0.003(2) 0.013(2) -0.0055(19) C21 0.033(3) 0.034(2) 0.036(3) 0.000(2) 0.012(2) -0.006(2) C22 0.028(3) 0.032(2) 0.030(2) -0.003(2) 0.010(2) -0.0053(19) C23 0.030(2) 0.038(3) 0.026(2) 0.002(2) 0.009(2) -0.001(2) C24 0.030(3) 0.028(2) 0.033(2) 0.003(2) 0.015(2) 0.0026(19) C25 0.025(2) 0.034(2) 0.033(2) 0.002(2) 0.014(2) 0.001(2) C26 0.043(3) 0.038(3) 0.044(3) 0.006(2) 0.019(2) -0.001(2) C27 0.056(4) 0.038(3) 0.055(3) 0.011(2) 0.028(3) 0.006(2) C28 0.060(3) 0.028(2) 0.066(3) 0.000(3) 0.037(3) 0.002(2) C29 0.045(3) 0.027(2) 0.049(3) -0.007(2) 0.022(2) -0.005(2) C30 0.033(3) 0.035(3) 0.030(2) -0.001(2) 0.007(2) -0.005(2) C31 0.029(3) 0.046(3) 0.042(3) -0.006(2) 0.005(2) 0.002(2) C32 0.037(3) 0.046(3) 0.046(3) -0.007(3) 0.014(3) 0.002(2) C33 0.027(3) 0.035(3) 0.037(3) 0.001(2) 0.009(2) -0.007(2) C34 0.028(3) 0.044(3) 0.049(3) -0.001(2) 0.006(2) 0.001(2) C35 0.034(3) 0.033(2) 0.047(3) -0.002(2) 0.006(2) 0.001(2) C36 0.049(3) 0.045(3) 0.032(3) -0.005(2) 0.013(2) -0.012(2) C37 0.060(13) 0.059(12) 0.054(12) -0.005(9) 0.022(8) -0.007(9) C38 0.06(2) 0.07(2) 0.07(2) -0.004(10) 0.034(12) -0.004(10) C39 0.07(2) 0.07(2) 0.07(2) -0.007(10) 0.037(13) -0.001(10) C36' 0.049(3) 0.045(3) 0.032(3) -0.005(2) 0.013(2) -0.012(2) C37' 0.074(5) 0.098(5) 0.067(4) -0.051(4) 0.032(4) -0.025(4) C38' 0.087(5) 0.086(5) 0.060(4) -0.019(4) 0.035(4) -0.049(4) C39' 0.082(5) 0.077(4) 0.043(4) -0.009(3) -0.004(3) -0.009(4) N1 0.029(2) 0.035(2) 0.0305(19) -0.0057(17) 0.0125(17) 0.0031(16) N2 0.039(2) 0.025(2) 0.041(2) 0.0018(18) 0.020(2) 0.0003(17) N3 0.027(2) 0.0280(19) 0.030(2) -0.0024(16) 0.0096(17) -0.0018(16) N4 0.037(2) 0.038(2) 0.030(2) 0.0003(17) 0.0097(18) -0.0052(18) O1 0.0357(19) 0.0365(17) 0.059(2) 0.0126(16) 0.0288(16) 0.0086(15) O2 0.038(2) 0.046(2) 0.057(2) -0.0076(18) 0.0151(16) 0.0025(16) O3 0.031(2) 0.050(2) 0.051(2) -0.0088(17) 0.0053(17) 0.0024(15) O4 0.051(2) 0.062(2) 0.055(2) -0.0258(18) 0.0269(19) -0.0254(19) O5 0.045(2) 0.055(2) 0.049(2) -0.0204(18) 0.029(2) -0.0119(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.002(3) 4_465 ? Co1 N3 2.074(3) . ? Co1 O5 2.098(3) . ? Co1 N2 2.148(4) . ? Co1 N4 2.153(3) . ? Co1 O4 2.252(3) . ? Co1 C14 2.509(4) . ? C1 O2 1.235(5) . ? C1 O1 1.262(5) . ? C1 C2 1.501(6) . ? C2 C3 1.345(5) . ? C2 C6 1.412(6) . ? C3 N1 1.361(5) . ? C3 H3 0.9300 . ? C4 O3 1.248(5) . ? C4 N1 1.402(5) . ? C4 C5 1.411(6) . ? C5 C6 1.350(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N1 1.486(5) . ? C7 C8 1.506(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.377(6) . ? C8 C13 1.380(6) . ? C9 C10 1.380(5) . ? C9 H9 0.9300 . ? C10 C11 1.397(5) . ? C10 H10 0.9300 . ? C11 C12 1.367(6) . ? C11 C14 1.495(6) . ? C12 C13 1.389(6) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O4 1.246(5) . ? C14 O5 1.259(5) . ? C15 N4 1.325(5) . ? C15 C16 1.369(6) . ? C15 H15 0.9300 . ? C16 C17 1.361(6) . ? C16 H16 0.9300 . ? C17 C18 1.385(6) . ? C17 H17 0.9300 . ? C18 C19 1.366(5) . ? C18 H18 0.9300 . ? C19 N4 1.342(5) . ? C19 C20 1.471(5) . ? C20 N3 1.339(5) . ? C20 C21 1.385(5) . ? C21 C22 1.381(5) . ? C21 H21 0.9300 . ? C22 C23 1.399(5) . ? C22 C30 1.485(5) . ? C23 C24 1.370(5) . ? C23 H23 0.9300 . ? C24 N3 1.336(5) . ? C24 C25 1.494(5) . ? C25 N2 1.346(5) . ? C25 C26 1.374(5) . ? C26 C27 1.388(6) . ? C26 H26 0.9300 . ? C27 C28 1.377(7) . ? C27 H27 0.9300 . ? C28 C29 1.364(6) . ? C28 H28 0.9300 . ? C29 N2 1.327(5) . ? C29 H29 0.9300 . ? C30 C31 1.376(6) . ? C30 C35 1.384(6) . ? C31 C32 1.385(6) . ? C31 H31 0.9300 . ? C32 C33 1.385(6) . ? C32 H32 0.9300 . ? C33 C34 1.393(6) . ? C33 C36 1.533(6) . ? C34 C35 1.389(5) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.49(5) . ? C36 C38 1.56(6) . ? C36 C39 1.60(6) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C37' H37D 0.9600 . ? C37' H37E 0.9600 . ? C37' H37F 0.9600 . ? C38' H38D 0.9600 . ? C38' H38E 0.9600 . ? C38' H38F 0.9600 . ? C39' H39D 0.9600 . ? C39' H39E 0.9600 . ? C39' H39F 0.9600 . ? O1 Co1 2.002(3) 4_564 ? 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 N3 98.62(13) 4_465 . ? O1 Co1 O5 92.87(13) 4_465 . ? N3 Co1 O5 167.54(14) . . ? O1 Co1 N2 105.93(14) 4_465 . ? N3 Co1 N2 75.29(14) . . ? O5 Co1 N2 96.98(11) . . ? O1 Co1 N4 89.82(13) 4_465 . ? N3 Co1 N4 74.62(13) . . ? O5 Co1 N4 110.40(13) . . ? N2 Co1 N4 147.76(14) . . ? O1 Co1 O4 149.17(11) 4_465 . ? N3 Co1 O4 110.12(13) . . ? O5 Co1 O4 59.78(12) . . ? N2 Co1 O4 92.30(14) . . ? N4 Co1 O4 87.33(13) . . ? O1 Co1 C14 121.56(14) 4_465 . ? N3 Co1 C14 139.57(15) . . ? O5 Co1 C14 30.06(13) . . ? N2 Co1 C14 96.00(14) . . ? N4 Co1 C14 99.36(14) . . ? O4 Co1 C14 29.73(12) . . ? O2 C1 O1 125.5(4) . . ? O2 C1 C2 119.1(4) . . ? O1 C1 C2 115.3(4) . . ? C3 C2 C6 116.5(4) . . ? C3 C2 C1 120.8(4) . . ? C6 C2 C1 122.6(4) . . ? C2 C3 N1 123.5(4) . . ? C2 C3 H3 118.2 . . ? N1 C3 H3 118.2 . . ? O3 C4 N1 120.5(4) . . ? O3 C4 C5 124.7(4) . . ? N1 C4 C5 114.7(4) . . ? C6 C5 C4 122.6(5) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C2 120.9(4) . . ? C5 C6 H6 119.6 . . ? C2 C6 H6 119.6 . . ? N1 C7 C8 113.5(3) . . ? N1 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C13 119.4(4) . . ? C9 C8 C7 119.5(4) . . ? C13 C8 C7 121.1(4) . . ? C8 C9 C10 120.4(4) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C11 120.5(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 118.7(4) . . ? C12 C11 C14 121.3(4) . . ? C10 C11 C14 120.0(4) . . ? C11 C12 C13 121.0(4) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C8 C13 C12 120.1(5) . . ? C8 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? O4 C14 O5 120.2(4) . . ? O4 C14 C11 120.0(4) . . ? O5 C14 C11 119.8(4) . . ? O4 C14 Co1 63.6(2) . . ? O5 C14 Co1 56.6(2) . . ? C11 C14 Co1 174.8(3) . . ? N4 C15 C16 122.7(4) . . ? N4 C15 H15 118.6 . . ? C16 C15 H15 118.6 . . ? C17 C16 C15 119.1(4) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 118.7(4) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? C19 C18 C17 119.3(4) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? N4 C19 C18 121.7(4) . . ? N4 C19 C20 114.0(3) . . ? C18 C19 C20 124.3(4) . . ? N3 C20 C21 120.5(4) . . ? N3 C20 C19 114.1(3) . . ? C21 C20 C19 125.4(3) . . ? C22 C21 C20 120.3(4) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 117.8(3) . . ? C21 C22 C30 121.0(4) . . ? C23 C22 C30 121.2(3) . . ? C24 C23 C22 119.4(3) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? N3 C24 C23 121.8(4) . . ? N3 C24 C25 113.0(3) . . ? C23 C24 C25 125.1(4) . . ? N2 C25 C26 121.9(4) . . ? N2 C25 C24 114.7(3) . . ? C26 C25 C24 123.4(4) . . ? C25 C26 C27 119.1(4) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C28 C27 C26 118.2(4) . . ? C28 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? C29 C28 C27 119.5(4) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? N2 C29 C28 122.7(4) . . ? N2 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? C31 C30 C35 118.7(4) . . ? C31 C30 C22 121.3(4) . . ? C35 C30 C22 120.0(4) . . ? C30 C31 C32 120.5(4) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 122.1(5) . . ? C31 C32 H32 118.9 . . ? C33 C32 H32 118.9 . . ? C32 C33 C34 116.7(4) . . ? C32 C33 C36 122.0(4) . . ? C34 C33 C36 121.1(4) . . ? C35 C34 C33 121.6(4) . . ? C35 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? C30 C35 C34 120.4(4) . . ? C30 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 C33 111(2) . . ? C37 C36 C38 115(3) . . ? C33 C36 C38 115(2) . . ? C37 C36 C39 112(3) . . ? C33 C36 C39 107(2) . . ? C38 C36 C39 95(3) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? H37D C37' H37E 109.5 . . ? H37D C37' H37F 109.5 . . ? H37E C37' H37F 109.5 . . ? H38D C38' H38E 109.5 . . ? H38D C38' H38F 109.5 . . ? H38E C38' H38F 109.5 . . ? H39D C39' H39E 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? C3 N1 C4 121.5(3) . . ? C3 N1 C7 119.9(3) . . ? C4 N1 C7 118.4(3) . . ? C29 N2 C25 118.5(4) . . ? C29 N2 Co1 125.0(3) . . ? C25 N2 Co1 115.8(3) . . ? C24 N3 C20 120.2(3) . . ? C24 N3 Co1 120.0(3) . . ? C20 N3 Co1 119.7(3) . . ? C15 N4 C19 118.5(4) . . ? C15 N4 Co1 124.4(3) . . ? C19 N4 Co1 117.0(3) . . ? C1 O1 Co1 123.5(3) . 4_564 ? C14 O4 Co1 86.7(3) . . ? C14 O5 Co1 93.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 11.9(6) . . . . ? O1 C1 C2 C3 -166.0(4) . . . . ? O2 C1 C2 C6 -171.5(4) . . . . ? O1 C1 C2 C6 10.6(6) . . . . ? C6 C2 C3 N1 -4.2(6) . . . . ? C1 C2 C3 N1 172.6(4) . . . . ? O3 C4 C5 C6 174.3(5) . . . . ? N1 C4 C5 C6 -5.7(7) . . . . ? C4 C5 C6 C2 4.0(8) . . . . ? C3 C2 C6 C5 1.1(7) . . . . ? C1 C2 C6 C5 -175.6(4) . . . . ? N1 C7 C8 C9 -87.9(5) . . . . ? N1 C7 C8 C13 93.5(5) . . . . ? C13 C8 C9 C10 0.7(6) . . . . ? C7 C8 C9 C10 -177.9(4) . . . . ? C8 C9 C10 C11 -0.6(6) . . . . ? C9 C10 C11 C12 -0.5(6) . . . . ? C9 C10 C11 C14 177.9(4) . . . . ? C10 C11 C12 C13 1.6(7) . . . . ? C14 C11 C12 C13 -176.8(4) . . . . ? C9 C8 C13 C12 0.4(7) . . . . ? C7 C8 C13 C12 178.9(4) . . . . ? C11 C12 C13 C8 -1.5(7) . . . . ? C12 C11 C14 O4 -16.7(6) . . . . ? C10 C11 C14 O4 165.0(4) . . . . ? C12 C11 C14 O5 161.4(4) . . . . ? C10 C11 C14 O5 -17.0(6) . . . . ? O1 Co1 C14 O4 163.0(2) 4_465 . . . ? N3 Co1 C14 O4 -9.8(3) . . . . ? O5 Co1 C14 O4 -177.7(4) . . . . ? N2 Co1 C14 O4 -84.1(3) . . . . ? N4 Co1 C14 O4 67.4(3) . . . . ? O1 Co1 C14 O5 -19.3(3) 4_465 . . . ? N3 Co1 C14 O5 167.9(3) . . . . ? N2 Co1 C14 O5 93.6(3) . . . . ? N4 Co1 C14 O5 -114.9(3) . . . . ? O4 Co1 C14 O5 177.7(4) . . . . ? N4 C15 C16 C17 0.0(8) . . . . ? C15 C16 C17 C18 -0.2(8) . . . . ? C16 C17 C18 C19 0.0(7) . . . . ? C17 C18 C19 N4 0.3(7) . . . . ? C17 C18 C19 C20 178.0(4) . . . . ? N4 C19 C20 N3 1.6(5) . . . . ? C18 C19 C20 N3 -176.3(4) . . . . ? N4 C19 C20 C21 179.8(4) . . . . ? C18 C19 C20 C21 1.9(7) . . . . ? N3 C20 C21 C22 2.0(7) . . . . ? C19 C20 C21 C22 -176.0(4) . . . . ? C20 C21 C22 C23 -1.2(6) . . . . ? C20 C21 C22 C30 179.7(4) . . . . ? C21 C22 C23 C24 0.2(6) . . . . ? C30 C22 C23 C24 179.3(4) . . . . ? C22 C23 C24 N3 0.0(6) . . . . ? C22 C23 C24 C25 179.3(4) . . . . ? N3 C24 C25 N2 3.6(6) . . . . ? C23 C24 C25 N2 -175.7(4) . . . . ? N3 C24 C25 C26 -178.2(4) . . . . ? C23 C24 C25 C26 2.5(7) . . . . ? N2 C25 C26 C27 1.0(7) . . . . ? C24 C25 C26 C27 -177.0(4) . . . . ? C25 C26 C27 C28 -0.7(7) . . . . ? C26 C27 C28 C29 -0.9(8) . . . . ? C27 C28 C29 N2 2.5(8) . . . . ? C21 C22 C30 C31 42.4(6) . . . . ? C23 C22 C30 C31 -136.7(5) . . . . ? C21 C22 C30 C35 -137.4(5) . . . . ? C23 C22 C30 C35 43.5(6) . . . . ? C35 C30 C31 C32 -1.0(7) . . . . ? C22 C30 C31 C32 179.3(5) . . . . ? C30 C31 C32 C33 0.1(8) . . . . ? C31 C32 C33 C34 1.5(8) . . . . ? C31 C32 C33 C36 177.2(5) . . . . ? C32 C33 C34 C35 -2.3(7) . . . . ? C36 C33 C34 C35 -178.0(4) . . . . ? C31 C30 C35 C34 0.2(7) . . . . ? C22 C30 C35 C34 180.0(4) . . . . ? C33 C34 C35 C30 1.5(7) . . . . ? C32 C33 C36 C37 -29(3) . . . . ? C34 C33 C36 C37 147(3) . . . . ? C32 C33 C36 C38 -162(3) . . . . ? C34 C33 C36 C38 14(3) . . . . ? C32 C33 C36 C39 94(3) . . . . ? C34 C33 C36 C39 -91(3) . . . . ? C2 C3 N1 C4 2.3(6) . . . . ? C2 C3 N1 C7 -171.2(4) . . . . ? O3 C4 N1 C3 -177.4(4) . . . . ? C5 C4 N1 C3 2.6(6) . . . . ? O3 C4 N1 C7 -3.8(6) . . . . ? C5 C4 N1 C7 176.3(4) . . . . ? C8 C7 N1 C3 -47.0(5) . . . . ? C8 C7 N1 C4 139.3(4) . . . . ? C28 C29 N2 C25 -2.2(7) . . . . ? C28 C29 N2 Co1 -172.4(4) . . . . ? C26 C25 N2 C29 0.5(7) . . . . ? C24 C25 N2 C29 178.7(4) . . . . ? C26 C25 N2 Co1 171.5(3) . . . . ? C24 C25 N2 Co1 -10.3(5) . . . . ? O1 Co1 N2 C29 85.3(4) 4_465 . . . ? N3 Co1 N2 C29 -179.8(4) . . . . ? O5 Co1 N2 C29 -9.7(4) . . . . ? N4 Co1 N2 C29 -158.2(3) . . . . ? O4 Co1 N2 C29 -69.6(4) . . . . ? C14 Co1 N2 C29 -40.0(4) . . . . ? O1 Co1 N2 C25 -85.1(3) 4_465 . . . ? N3 Co1 N2 C25 9.9(3) . . . . ? O5 Co1 N2 C25 179.9(3) . . . . ? N4 Co1 N2 C25 31.4(5) . . . . ? O4 Co1 N2 C25 120.1(3) . . . . ? C14 Co1 N2 C25 149.7(3) . . . . ? C23 C24 N3 C20 0.8(6) . . . . ? C25 C24 N3 C20 -178.5(4) . . . . ? C23 C24 N3 Co1 -175.4(3) . . . . ? C25 C24 N3 Co1 5.3(5) . . . . ? C21 C20 N3 C24 -1.8(6) . . . . ? C19 C20 N3 C24 176.5(4) . . . . ? C21 C20 N3 Co1 174.4(3) . . . . ? C19 C20 N3 Co1 -7.3(5) . . . . ? O1 Co1 N3 C24 96.2(3) 4_465 . . . ? O5 Co1 N3 C24 -60.9(8) . . . . ? N2 Co1 N3 C24 -8.2(3) . . . . ? N4 Co1 N3 C24 -176.4(3) . . . . ? O4 Co1 N3 C24 -95.2(3) . . . . ? C14 Co1 N3 C24 -90.0(4) . . . . ? O1 Co1 N3 C20 -80.1(3) 4_465 . . . ? O5 Co1 N3 C20 122.9(7) . . . . ? N2 Co1 N3 C20 175.6(3) . . . . ? N4 Co1 N3 C20 7.4(3) . . . . ? O4 Co1 N3 C20 88.6(3) . . . . ? C14 Co1 N3 C20 93.8(4) . . . . ? C16 C15 N4 C19 0.3(7) . . . . ? C16 C15 N4 Co1 177.2(4) . . . . ? C18 C19 N4 C15 -0.5(6) . . . . ? C20 C19 N4 C15 -178.4(4) . . . . ? C18 C19 N4 Co1 -177.6(3) . . . . ? C20 C19 N4 Co1 4.5(5) . . . . ? O1 Co1 N4 C15 -84.1(4) 4_465 . . . ? N3 Co1 N4 C15 176.9(4) . . . . ? O5 Co1 N4 C15 8.8(4) . . . . ? N2 Co1 N4 C15 155.2(4) . . . . ? O4 Co1 N4 C15 65.1(4) . . . . ? C14 Co1 N4 C15 37.9(4) . . . . ? O1 Co1 N4 C19 92.7(3) 4_465 . . . ? N3 Co1 N4 C19 -6.3(3) . . . . ? O5 Co1 N4 C19 -174.3(3) . . . . ? N2 Co1 N4 C19 -27.9(5) . . . . ? O4 Co1 N4 C19 -118.0(3) . . . . ? C14 Co1 N4 C19 -145.3(3) . . . . ? O2 C1 O1 Co1 -42.4(6) . . . 4_564 ? C2 C1 O1 Co1 135.3(3) . . . 4_564 ? O5 C14 O4 Co1 -2.2(4) . . . . ? C11 C14 O4 Co1 175.8(3) . . . . ? O1 Co1 O4 C14 -29.0(4) 4_465 . . . ? N3 Co1 O4 C14 173.3(2) . . . . ? O5 Co1 O4 C14 1.3(2) . . . . ? N2 Co1 O4 C14 98.1(3) . . . . ? N4 Co1 O4 C14 -114.2(3) . . . . ? O4 C14 O5 Co1 2.4(4) . . . . ? C11 C14 O5 Co1 -175.7(3) . . . . ? O1 Co1 O5 C14 163.7(3) 4_465 . . . ? N3 Co1 O5 C14 -39.0(8) . . . . ? N2 Co1 O5 C14 -89.9(3) . . . . ? N4 Co1 O5 C14 72.8(3) . . . . ? O4 Co1 O5 C14 -1.3(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C7 H7A O3 0.97 2.33 2.753(5) 105.9 . C12 H12 O3 0.93 2.47 3.286(6) 146.7 4_565 C16 H16 O1 0.93 2.45 3.115(5) 128.1 3_455 C27 H27 O2 0.93 2.36 3.263(5) 162.7 1_556 C31 H31 O4 0.93 2.43 3.299(5) 155.5 2_575 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.293 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.048 #=========================END data_Compound-5 _database_code_depnum_ccdc_archive 'CCDC 873954' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H42 Cd2 N6 O14' _chemical_formula_sum 'C52 H42 Cd2 N6 O14' _chemical_formula_weight 1199.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_hall '-p 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.5430(3) _cell_length_b 14.5900(7) _cell_length_c 14.9350(7) _cell_angle_alpha 100.202(4) _cell_angle_beta 94.958(4) _cell_angle_gamma 98.558(4) _cell_volume 1167.58(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3913 _cell_measurement_theta_min 0.95092 _cell_measurement_theta_max 1.00000 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.706 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.835 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6913 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4115 _reflns_number_gt 3670 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In the refienment of the disordered O2W, the PART instructions were used. For O2W and O2W', some anisotropic displacement ellipsoids were rather elongated which led us to use the ISOR restraints. ; _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^)+(0.0327P)^2^+0.2013P] 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 4115 _refine_ls_number_parameters 344 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0708 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.76658(4) 0.215427(16) 0.737220(15) 0.02976(10) Uani 1 1 d . . . C1 C 0.1900(6) 0.7136(2) 0.4163(2) 0.0315(7) Uani 1 1 d . . . C2 C 0.1457(5) 0.6723(2) 0.4996(2) 0.0292(7) Uani 1 1 d . . . C3 C -0.0824(6) 0.6221(2) 0.5068(2) 0.0345(8) Uani 1 1 d . . . H3 H -0.2091 0.6143 0.4597 0.041 Uiso 1 1 calc R . . C4 C -0.1234(6) 0.5837(2) 0.5833(2) 0.0355(8) Uani 1 1 d . . . H4 H -0.2782 0.5511 0.5875 0.043 Uiso 1 1 calc R . . C5 C 0.0635(5) 0.5932(2) 0.6539(2) 0.0288(7) Uani 1 1 d . . . C6 C 0.2907(6) 0.6425(2) 0.6465(2) 0.0343(8) Uani 1 1 d . . . H6 H 0.4179 0.6492 0.6933 0.041 Uiso 1 1 calc R . . C7 C 0.3324(6) 0.6826(2) 0.5703(2) 0.0339(8) Uani 1 1 d . . . H7 H 0.4861 0.7165 0.5667 0.041 Uiso 1 1 calc R . . C8 C 0.0054(5) 0.5499(2) 0.7356(2) 0.0340(8) Uani 1 1 d . . . H8A H -0.1163 0.5815 0.7656 0.041 Uiso 1 1 calc R . . H8B H -0.0673 0.4840 0.7141 0.041 Uiso 1 1 calc R . . C9 C 0.2892(6) 0.6386(2) 0.8673(2) 0.0371(8) Uani 1 1 d . . . C10 C 0.3325(5) 0.4786(2) 0.8013(2) 0.0296(7) Uani 1 1 d . . . H10 H 0.2732 0.4239 0.7581 0.035 Uiso 1 1 calc R . . C11 C 0.5328(5) 0.4808(2) 0.8616(2) 0.0269(7) Uani 1 1 d . . . C12 C 0.6206(6) 0.5653(2) 0.9262(2) 0.0348(8) Uani 1 1 d . . . H12 H 0.7609 0.5692 0.9666 0.042 Uiso 1 1 calc R . . C13 C 0.5024(6) 0.6401(2) 0.9296(2) 0.0407(8) Uani 1 1 d . . . H13 H 0.5609 0.6943 0.9737 0.049 Uiso 1 1 calc R . . C14 C 0.6625(6) 0.3975(2) 0.8567(2) 0.0303(7) Uani 1 1 d . . . C15 C 0.4448(6) 0.0810(3) 0.8531(2) 0.0408(8) Uani 1 1 d . . . H15 H 0.3738 0.1343 0.8706 0.049 Uiso 1 1 calc R . . C16 C 0.3722(7) 0.0022(3) 0.8894(3) 0.0495(10) Uani 1 1 d . . . H16 H 0.2539 0.0024 0.9300 0.059 Uiso 1 1 calc R . . C17 C 0.4762(7) -0.0760(3) 0.8651(3) 0.0538(10) Uani 1 1 d . . . H17 H 0.4296 -0.1296 0.8893 0.065 Uiso 1 1 calc R . . C18 C 0.6527(6) -0.0759(2) 0.8039(2) 0.0427(9) Uani 1 1 d . . . C19 C 0.7683(8) -0.1560(3) 0.7735(3) 0.0583(11) Uani 1 1 d . . . H19 H 0.7274 -0.2109 0.7961 0.070 Uiso 1 1 calc R . . C20 C 0.9332(8) -0.1533(3) 0.7134(3) 0.0593(12) Uani 1 1 d . . . H20 H 1.0047 -0.2063 0.6952 0.071 Uiso 1 1 calc R . . C21 C 1.0014(6) -0.0709(3) 0.6770(3) 0.0451(9) Uani 1 1 d . . . C22 C 1.1809(7) -0.0629(3) 0.6152(3) 0.0592(12) Uani 1 1 d . . . H22 H 1.2542 -0.1146 0.5938 0.071 Uiso 1 1 calc R . . C23 C 1.2455(7) 0.0201(3) 0.5876(3) 0.0549(11) Uani 1 1 d . . . H23 H 1.3642 0.0258 0.5476 0.066 Uiso 1 1 calc R . . C24 C 1.1325(6) 0.0965(3) 0.6195(2) 0.0435(9) Uani 1 1 d . . . H24 H 1.1787 0.1533 0.6005 0.052 Uiso 1 1 calc R . . C25 C 0.8964(6) 0.0101(2) 0.7053(2) 0.0332(8) Uani 1 1 d . . . C26 C 0.7155(6) 0.0065(2) 0.7692(2) 0.0317(7) Uani 1 1 d . . . N1 N 0.2164(5) 0.55501(18) 0.80284(17) 0.0313(6) Uani 1 1 d . . . N2 N 0.6111(5) 0.08453(18) 0.79423(17) 0.0321(6) Uani 1 1 d . . . N3 N 0.9624(4) 0.09167(19) 0.67577(17) 0.0321(6) Uani 1 1 d . . . O1 O 0.3773(4) 0.77370(18) 0.41725(16) 0.0431(6) Uani 1 1 d . . . O2 O 0.0324(4) 0.68659(17) 0.34689(15) 0.0428(6) Uani 1 1 d . . . O3 O 0.1733(5) 0.70480(17) 0.86542(18) 0.0528(7) Uani 1 1 d . . . O4 O 0.8714(4) 0.41030(17) 0.89774(16) 0.0452(6) Uani 1 1 d . . . O5 O 0.5499(4) 0.31914(15) 0.80768(15) 0.0340(5) Uani 1 1 d . . . O1W O 1.0902(4) 0.26493(16) 0.85596(14) 0.0366(5) Uani 1 1 d . . . O2W O 1.030(6) 0.1564(11) 1.0059(12) 0.053(6) Uani 0.45(9) 1 d PU A 1 O2W' O 0.959(7) 0.1578(13) 0.9987(12) 0.080(4) Uani 0.55(9) 1 d PU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03548(15) 0.02632(15) 0.03034(15) 0.00853(10) 0.00841(10) 0.00799(11) C1 0.0364(18) 0.0293(18) 0.0321(18) 0.0079(15) 0.0084(14) 0.0115(16) C2 0.0351(17) 0.0276(17) 0.0287(17) 0.0083(14) 0.0083(13) 0.0113(15) C3 0.0337(17) 0.037(2) 0.0327(18) 0.0093(15) 0.0009(14) 0.0057(15) C4 0.0312(17) 0.037(2) 0.040(2) 0.0122(16) 0.0081(14) 0.0047(15) C5 0.0330(17) 0.0270(17) 0.0313(17) 0.0098(14) 0.0092(13) 0.0128(14) C6 0.0307(17) 0.044(2) 0.0329(18) 0.0155(16) 0.0034(13) 0.0110(16) C7 0.0271(16) 0.037(2) 0.0395(19) 0.0127(16) 0.0074(14) 0.0027(15) C8 0.0322(17) 0.037(2) 0.0386(19) 0.0179(16) 0.0085(14) 0.0086(15) C9 0.049(2) 0.0286(19) 0.037(2) 0.0094(15) 0.0152(16) 0.0077(17) C10 0.0354(17) 0.0228(17) 0.0322(17) 0.0066(14) 0.0119(14) 0.0045(14) C11 0.0291(16) 0.0268(17) 0.0258(17) 0.0070(13) 0.0078(13) 0.0023(14) C12 0.0387(18) 0.0344(19) 0.0307(18) 0.0064(15) 0.0054(14) 0.0034(16) C13 0.057(2) 0.0298(19) 0.0324(19) -0.0011(15) 0.0087(16) 0.0049(17) C14 0.0332(18) 0.0282(18) 0.0311(17) 0.0047(14) 0.0112(14) 0.0068(15) C15 0.0423(19) 0.039(2) 0.043(2) 0.0117(17) 0.0081(16) 0.0063(17) C16 0.045(2) 0.059(3) 0.046(2) 0.022(2) 0.0088(17) -0.003(2) C17 0.059(2) 0.046(2) 0.054(3) 0.027(2) -0.006(2) -0.012(2) C18 0.048(2) 0.030(2) 0.047(2) 0.0138(17) -0.0098(17) -0.0022(17) C19 0.067(3) 0.024(2) 0.080(3) 0.014(2) -0.014(2) 0.0031(19) C20 0.060(3) 0.032(2) 0.080(3) -0.003(2) -0.011(2) 0.015(2) C21 0.046(2) 0.036(2) 0.048(2) -0.0028(17) -0.0087(17) 0.0118(18) C22 0.053(2) 0.058(3) 0.060(3) -0.016(2) -0.003(2) 0.029(2) C23 0.046(2) 0.069(3) 0.049(2) -0.004(2) 0.0108(18) 0.024(2) C24 0.0393(19) 0.055(2) 0.039(2) 0.0069(18) 0.0091(16) 0.0145(18) C25 0.0360(18) 0.0285(18) 0.0324(18) -0.0002(14) -0.0058(14) 0.0097(15) C26 0.0357(17) 0.0241(17) 0.0328(18) 0.0054(14) -0.0068(14) 0.0036(14) N1 0.0376(15) 0.0294(15) 0.0303(15) 0.0115(12) 0.0085(11) 0.0069(12) N2 0.0359(15) 0.0282(15) 0.0330(15) 0.0081(12) 0.0045(12) 0.0053(12) N3 0.0302(14) 0.0367(16) 0.0292(15) 0.0029(12) 0.0050(11) 0.0080(13) O1 0.0411(13) 0.0503(16) 0.0398(14) 0.0223(12) 0.0050(10) -0.0022(12) O2 0.0532(14) 0.0404(15) 0.0306(13) 0.0114(11) -0.0035(11) -0.0058(12) O3 0.0737(18) 0.0319(14) 0.0594(17) 0.0111(13) 0.0157(13) 0.0226(14) O4 0.0315(13) 0.0465(16) 0.0544(15) 0.0001(12) -0.0029(11) 0.0123(12) O5 0.0308(12) 0.0267(12) 0.0445(13) 0.0024(11) 0.0090(10) 0.0074(10) O1W 0.0357(12) 0.0397(14) 0.0347(13) 0.0101(11) 0.0006(10) 0.0060(11) O2W 0.059(8) 0.052(6) 0.053(6) 0.013(3) 0.011(4) 0.020(4) O2W' 0.082(6) 0.079(5) 0.083(5) 0.024(3) 0.009(4) 0.012(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O5 2.2439(19) . ? Cd1 O2 2.295(2) 2_666 ? Cd1 N2 2.308(3) . ? Cd1 N3 2.335(2) . ? Cd1 O1W 2.344(2) . ? Cd1 O1 2.415(2) 2_666 ? Cd1 C1 2.693(3) 2_666 ? C1 O1 1.253(4) . ? C1 O2 1.261(4) . ? C1 C2 1.499(4) . ? C1 Cd1 2.693(3) 2_666 ? C2 C7 1.383(4) . ? C2 C3 1.386(4) . ? C3 C4 1.380(4) . ? C3 H3 0.9300 . ? C4 C5 1.386(4) . ? C4 H4 0.9300 . ? C5 C6 1.378(4) . ? C5 C8 1.507(4) . ? C6 C7 1.391(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.459(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O3 1.239(4) . ? C9 N1 1.396(4) . ? C9 C13 1.435(5) . ? C10 C11 1.360(4) . ? C10 N1 1.365(4) . ? C10 H10 0.9300 . ? C11 C12 1.416(4) . ? C11 C14 1.495(4) . ? C12 C13 1.351(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O4 1.235(4) . ? C14 O5 1.282(4) . ? C15 N2 1.329(4) . ? C15 C16 1.378(5) . ? C15 H15 0.9300 . ? C16 C17 1.360(5) . ? C16 H16 0.9300 . ? C17 C18 1.396(5) . ? C17 H17 0.9300 . ? C18 C26 1.401(5) . ? C18 C19 1.437(5) . ? C19 C20 1.336(6) . ? C19 H19 0.9300 . ? C20 C21 1.419(6) . ? C20 H20 0.9300 . ? C21 C25 1.409(4) . ? C21 C22 1.420(6) . ? C22 C23 1.356(6) . ? C22 H22 0.9300 . ? C23 C24 1.391(5) . ? C23 H23 0.9300 . ? C24 N3 1.318(4) . ? C24 H24 0.9300 . ? C25 N3 1.353(4) . ? C25 C26 1.444(5) . ? C26 N2 1.362(4) . ? O1 Cd1 2.415(2) 2_666 ? O2 Cd1 2.295(2) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cd1 O2 97.30(8) . 2_666 ? O5 Cd1 N2 99.02(8) . . ? O2 Cd1 N2 163.37(9) 2_666 . ? O5 Cd1 N3 171.49(9) . . ? O2 Cd1 N3 91.21(9) 2_666 . ? N2 Cd1 N3 72.48(9) . . ? O5 Cd1 O1W 90.64(8) . . ? O2 Cd1 O1W 89.59(8) 2_666 . ? N2 Cd1 O1W 93.41(8) . . ? N3 Cd1 O1W 89.56(8) . . ? O5 Cd1 O1 96.36(8) . 2_666 ? O2 Cd1 O1 55.57(8) 2_666 2_666 ? N2 Cd1 O1 119.01(9) . 2_666 ? N3 Cd1 O1 88.31(8) . 2_666 ? O1W Cd1 O1 145.02(8) . 2_666 ? O5 Cd1 C1 98.02(8) . 2_666 ? O2 Cd1 C1 27.86(9) 2_666 2_666 ? N2 Cd1 C1 144.44(10) . 2_666 ? N3 Cd1 C1 89.42(9) . 2_666 ? O1W Cd1 C1 117.38(9) . 2_666 ? O1 Cd1 C1 27.71(9) 2_666 2_666 ? O1 C1 O2 122.0(3) . . ? O1 C1 C2 120.2(3) . . ? O2 C1 C2 117.8(3) . . ? O1 C1 Cd1 63.71(17) . 2_666 ? O2 C1 Cd1 58.25(16) . 2_666 ? C2 C1 Cd1 175.7(2) . 2_666 ? C7 C2 C3 118.8(3) . . ? C7 C2 C1 120.6(3) . . ? C3 C2 C1 120.6(3) . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.7(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 118.7(3) . . ? C6 C5 C8 123.4(3) . . ? C4 C5 C8 117.9(3) . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 120.2(3) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? N1 C8 C5 114.6(3) . . ? N1 C8 H8A 108.6 . . ? C5 C8 H8A 108.6 . . ? N1 C8 H8B 108.6 . . ? C5 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? O3 C9 N1 119.3(3) . . ? O3 C9 C13 125.6(3) . . ? N1 C9 C13 115.0(3) . . ? C11 C10 N1 121.5(3) . . ? C11 C10 H10 119.3 . . ? N1 C10 H10 119.3 . . ? C10 C11 C12 118.2(3) . . ? C10 C11 C14 120.6(3) . . ? C12 C11 C14 121.2(3) . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C9 121.9(3) . . ? C12 C13 H13 119.0 . . ? C9 C13 H13 119.0 . . ? O4 C14 O5 125.3(3) . . ? O4 C14 C11 117.5(3) . . ? O5 C14 C11 117.1(3) . . ? N2 C15 C16 123.3(3) . . ? N2 C15 H15 118.4 . . ? C16 C15 H15 118.4 . . ? C17 C16 C15 119.0(3) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? C16 C17 C18 120.1(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C17 C18 C26 117.6(3) . . ? C17 C18 C19 123.6(4) . . ? C26 C18 C19 118.7(4) . . ? C20 C19 C18 121.6(4) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 121.2(4) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C25 C21 C20 119.7(4) . . ? C25 C21 C22 116.6(4) . . ? C20 C21 C22 123.7(4) . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 119.4(4) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? N3 C24 C23 122.5(4) . . ? N3 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? N3 C25 C21 122.1(3) . . ? N3 C25 C26 118.9(3) . . ? C21 C25 C26 119.0(3) . . ? N2 C26 C18 121.8(3) . . ? N2 C26 C25 118.3(3) . . ? C18 C26 C25 119.8(3) . . ? C10 N1 C9 122.7(3) . . ? C10 N1 C8 119.4(3) . . ? C9 N1 C8 117.8(2) . . ? C15 N2 C26 118.2(3) . . ? C15 N2 Cd1 126.2(2) . . ? C26 N2 Cd1 115.5(2) . . ? C24 N3 C25 119.4(3) . . ? C24 N3 Cd1 125.9(2) . . ? C25 N3 Cd1 114.68(19) . . ? C1 O1 Cd1 88.58(19) . 2_666 ? C1 O2 Cd1 93.9(2) . 2_666 ? C14 O5 Cd1 119.68(17) . . ? 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 C7 -14.7(4) . . . . ? O2 C1 C2 C7 166.0(3) . . . . ? O1 C1 C2 C3 166.0(3) . . . . ? O2 C1 C2 C3 -13.3(4) . . . . ? C7 C2 C3 C4 0.4(5) . . . . ? C1 C2 C3 C4 179.8(3) . . . . ? C2 C3 C4 C5 -1.0(5) . . . . ? C3 C4 C5 C6 0.6(5) . . . . ? C3 C4 C5 C8 179.7(3) . . . . ? C4 C5 C6 C7 0.3(5) . . . . ? C8 C5 C6 C7 -178.7(3) . . . . ? C3 C2 C7 C6 0.5(5) . . . . ? C1 C2 C7 C6 -178.8(3) . . . . ? C5 C6 C7 C2 -0.9(5) . . . . ? C6 C5 C8 N1 -6.5(4) . . . . ? C4 C5 C8 N1 174.5(3) . . . . ? N1 C10 C11 C12 -0.5(4) . . . . ? N1 C10 C11 C14 -177.8(3) . . . . ? C10 C11 C12 C13 2.4(5) . . . . ? C14 C11 C12 C13 179.7(3) . . . . ? C11 C12 C13 C9 -1.7(5) . . . . ? O3 C9 C13 C12 -178.9(3) . . . . ? N1 C9 C13 C12 -0.7(5) . . . . ? C10 C11 C14 O4 163.7(3) . . . . ? C12 C11 C14 O4 -13.6(4) . . . . ? C10 C11 C14 O5 -14.3(4) . . . . ? C12 C11 C14 O5 168.5(3) . . . . ? N2 C15 C16 C17 0.6(6) . . . . ? C15 C16 C17 C18 -0.3(6) . . . . ? C16 C17 C18 C26 -0.2(5) . . . . ? C16 C17 C18 C19 -178.9(3) . . . . ? C17 C18 C19 C20 178.7(4) . . . . ? C26 C18 C19 C20 0.1(6) . . . . ? C18 C19 C20 C21 0.0(6) . . . . ? C19 C20 C21 C25 0.9(6) . . . . ? C19 C20 C21 C22 178.0(4) . . . . ? C25 C21 C22 C23 0.9(5) . . . . ? C20 C21 C22 C23 -176.3(4) . . . . ? C21 C22 C23 C24 -0.6(6) . . . . ? C22 C23 C24 N3 -0.4(6) . . . . ? C20 C21 C25 N3 177.1(3) . . . . ? C22 C21 C25 N3 -0.2(5) . . . . ? C20 C21 C25 C26 -1.8(5) . . . . ? C22 C21 C25 C26 -179.0(3) . . . . ? C17 C18 C26 N2 0.5(5) . . . . ? C19 C18 C26 N2 179.3(3) . . . . ? C17 C18 C26 C25 -179.7(3) . . . . ? C19 C18 C26 C25 -1.0(5) . . . . ? N3 C25 C26 N2 2.7(4) . . . . ? C21 C25 C26 N2 -178.4(3) . . . . ? N3 C25 C26 C18 -177.1(3) . . . . ? C21 C25 C26 C18 1.8(5) . . . . ? C11 C10 N1 C9 -2.1(5) . . . . ? C11 C10 N1 C8 178.7(3) . . . . ? O3 C9 N1 C10 -179.0(3) . . . . ? C13 C9 N1 C10 2.6(4) . . . . ? O3 C9 N1 C8 0.2(4) . . . . ? C13 C9 N1 C8 -178.1(3) . . . . ? C5 C8 N1 C10 -98.0(3) . . . . ? C5 C8 N1 C9 82.8(3) . . . . ? C16 C15 N2 C26 -0.4(5) . . . . ? C16 C15 N2 Cd1 -175.3(3) . . . . ? C18 C26 N2 C15 -0.2(5) . . . . ? C25 C26 N2 C15 -180.0(3) . . . . ? C18 C26 N2 Cd1 175.2(2) . . . . ? C25 C26 N2 Cd1 -4.5(3) . . . . ? O5 Cd1 N2 C15 -1.2(3) . . . . ? O2 Cd1 N2 C15 -169.9(3) 2_666 . . . ? N3 Cd1 N2 C15 178.5(3) . . . . ? O1W Cd1 N2 C15 90.0(3) . . . . ? O1 Cd1 N2 C15 -103.6(3) 2_666 . . . ? C1 Cd1 N2 C15 -118.9(3) 2_666 . . . ? O5 Cd1 N2 C26 -176.2(2) . . . . ? O2 Cd1 N2 C26 15.0(4) 2_666 . . . ? N3 Cd1 N2 C26 3.5(2) . . . . ? O1W Cd1 N2 C26 -85.0(2) . . . . ? O1 Cd1 N2 C26 81.3(2) 2_666 . . . ? C1 Cd1 N2 C26 66.1(3) 2_666 . . . ? C23 C24 N3 C25 1.1(5) . . . . ? C23 C24 N3 Cd1 178.3(2) . . . . ? C21 C25 N3 C24 -0.8(5) . . . . ? C26 C25 N3 C24 178.1(3) . . . . ? C21 C25 N3 Cd1 -178.3(2) . . . . ? C26 C25 N3 Cd1 0.6(4) . . . . ? O2 Cd1 N3 C24 3.9(3) 2_666 . . . ? N2 Cd1 N3 C24 -179.4(3) . . . . ? O1W Cd1 N3 C24 -85.7(3) . . . . ? O1 Cd1 N3 C24 59.4(3) 2_666 . . . ? C1 Cd1 N3 C24 31.7(3) 2_666 . . . ? O2 Cd1 N3 C25 -178.8(2) 2_666 . . . ? N2 Cd1 N3 C25 -2.1(2) . . . . ? O1W Cd1 N3 C25 91.6(2) . . . . ? O1 Cd1 N3 C25 -123.3(2) 2_666 . . . ? C1 Cd1 N3 C25 -151.0(2) 2_666 . . . ? O2 C1 O1 Cd1 1.1(3) . . . 2_666 ? C2 C1 O1 Cd1 -178.1(2) . . . 2_666 ? O1 C1 O2 Cd1 -1.2(3) . . . 2_666 ? C2 C1 O2 Cd1 178.1(2) . . . 2_666 ? O4 C14 O5 Cd1 -28.6(4) . . . . ? C11 C14 O5 Cd1 149.2(2) . . . . ? O2 Cd1 O5 C14 -58.1(2) 2_666 . . . ? N2 Cd1 O5 C14 125.1(2) . . . . ? O1W Cd1 O5 C14 31.6(2) . . . . ? O1 Cd1 O5 C14 -114.1(2) 2_666 . . . ? C1 Cd1 O5 C14 -86.2(2) 2_666 . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.611 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.075 #=========================END data_Compound-6 _database_code_depnum_ccdc_archive 'CCDC 873955' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 Cd3 N8 O14' _chemical_formula_sum 'C34 H30 Cd3 N8 O14' _chemical_formula_weight 1111.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M p2/n _symmetry_space_group_name_hall '-p 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 11.6400(8) _cell_length_b 7.1420(3) _cell_length_c 22.7780(10) _cell_angle_alpha 90 _cell_angle_beta 91.812(5) _cell_angle_gamma 90 _cell_volume 1892.65(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1505 _cell_measurement_theta_min 3.1519 _cell_measurement_theta_max 29.0682 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 1.750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6130 _exptl_absorpt_correction_T_max 0.7210 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7010 _diffrn_reflns_av_R_equivalents 0.0823 _diffrn_reflns_av_sigmaI/netI 0.1136 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3333 _reflns_number_gt 2409 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. For C15, C16, N2, N3 and N4, some anisotropic displacement ellipsoids were rather elongated which led us to use the SIMU/DELU restraints. In order to give a reasonable O...H distance of water molecule, we used the DFIX restraints. ; _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^)+(0.0260P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3333 _refine_ls_number_parameters 274 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.011 _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 0.0000 0.0000 0.5000 0.0242(2) Uani 1 2 d S . . Cd2 Cd 0.11732(5) 0.44843(7) 0.54369(2) 0.0263(2) Uani 1 1 d . . . C1 C -0.0257(7) 0.1866(11) 0.6296(3) 0.0282(19) Uani 1 1 d . . . C2 C -0.0583(7) 0.1651(10) 0.6916(3) 0.0259(18) Uani 1 1 d . . . C3 C -0.0815(8) -0.0104(10) 0.7142(3) 0.032(2) Uani 1 1 d . . . H3 H -0.0756 -0.1149 0.6901 0.039 Uiso 1 1 calc R . . C4 C -0.1128(8) -0.0335(11) 0.7708(3) 0.036(2) Uani 1 1 d . . . H4 H -0.1272 -0.1530 0.7850 0.043 Uiso 1 1 calc R . . C5 C -0.1233(7) 0.1216(12) 0.8078(3) 0.033(2) Uani 1 1 d . . . C6 C -0.0995(9) 0.2963(12) 0.7863(3) 0.045(2) Uani 1 1 d . . . H6 H -0.1058 0.4008 0.8103 0.054 Uiso 1 1 calc R . . C7 C -0.0661(9) 0.3170(11) 0.7288(3) 0.043(2) Uani 1 1 d . . . H7 H -0.0486 0.4357 0.7149 0.051 Uiso 1 1 calc R . . C8 C -0.1581(8) 0.0989(13) 0.8701(3) 0.041(2) Uani 1 1 d . . . H8A H -0.2321 0.0369 0.8711 0.049 Uiso 1 1 calc R . . H8B H -0.1652 0.2209 0.8883 0.049 Uiso 1 1 calc R . . C9 C -0.0916(8) -0.2045(12) 0.9138(3) 0.036(2) Uani 1 1 d . . . C10 C -0.0006(8) -0.2975(11) 0.9444(3) 0.039(2) Uani 1 1 d . . . H10 H -0.0104 -0.4231 0.9537 0.046 Uiso 1 1 calc R . . C11 C 0.1001(7) -0.2140(10) 0.9610(3) 0.0276(19) Uani 1 1 d . . . H11 H 0.1564 -0.2821 0.9815 0.033 Uiso 1 1 calc R . . C12 C 0.1196(7) -0.0227(10) 0.9470(3) 0.0287(19) Uani 1 1 d . . . C13 C 0.0307(7) 0.0679(10) 0.9187(3) 0.0253(18) Uani 1 1 d . . . H13 H 0.0399 0.1938 0.9095 0.030 Uiso 1 1 calc R . . C14 C 0.2309(7) 0.0750(11) 0.9611(3) 0.0296(19) Uani 1 1 d . . . C15 C 0.1918(8) 0.7663(11) 0.6439(3) 0.0366(9) Uani 1 1 d U . . H15 H 0.1349 0.8484 0.6303 0.044 Uiso 1 1 calc R . . C16 C 0.3375(8) 0.6558(11) 0.6961(3) 0.0364(9) Uani 1 1 d U . . H16 H 0.3990 0.6445 0.7229 0.044 Uiso 1 1 calc R . . C17 C 0.2848(8) 0.9736(10) 0.7222(3) 0.037(2) Uani 1 1 d . . . H17A H 0.2625 1.0809 0.6984 0.045 Uiso 1 1 calc R . . H17B H 0.3656 0.9867 0.7330 0.045 Uiso 1 1 calc R . . N1 N -0.0696(6) -0.0151(8) 0.9035(3) 0.0297(16) Uani 1 1 d . . . N2 N 0.2086(6) 0.5978(9) 0.6235(3) 0.0365(9) Uani 1 1 d U . . N3 N 0.2685(6) 0.8026(9) 0.6871(3) 0.0365(9) Uani 1 1 d U . . N4 N 0.2981(7) 0.5302(9) 0.6581(3) 0.0372(9) Uani 1 1 d U . . O1 O -0.0049(5) 0.0421(7) 0.6006(2) 0.0386(15) Uani 1 1 d . . . O2 O -0.0230(5) 0.3537(7) 0.6089(2) 0.0365(14) Uani 1 1 d . . . O3 O -0.1819(6) -0.2764(9) 0.8949(3) 0.0553(18) Uani 1 1 d . . . O4 O 0.2425(5) 0.2358(8) 0.9393(2) 0.0456(16) Uani 1 1 d . . . O5 O 0.3005(5) -0.0108(8) 0.9936(2) 0.0396(15) Uani 1 1 d . . . O6 O 0.0042(5) 0.3027(6) 0.4733(2) 0.0260(12) Uani 1 1 d . . . O1W O 0.2180(6) 0.5431(8) 0.4592(2) 0.0363(15) Uani 1 1 d D . . H1A H 0.164(9) 0.582(12) 0.437(4) 0.054 Uiso 1 1 d . . . H1B H 0.256(7) 0.468(10) 0.435(3) 0.054 Uiso 1 1 d 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 0.0293(6) 0.0173(4) 0.0257(4) 0.0004(3) -0.0035(3) -0.0002(3) Cd2 0.0296(4) 0.0219(3) 0.0271(3) -0.0007(2) -0.0037(2) 0.0004(3) C1 0.021(5) 0.037(5) 0.027(4) 0.005(4) -0.001(3) -0.002(4) C2 0.025(5) 0.032(4) 0.022(4) 0.009(3) 0.005(3) 0.006(4) C3 0.036(6) 0.029(4) 0.032(4) 0.000(4) 0.001(4) 0.001(4) C4 0.043(6) 0.033(5) 0.030(4) 0.007(4) 0.002(4) -0.008(4) C5 0.021(5) 0.051(5) 0.028(4) 0.013(4) -0.001(3) 0.002(4) C6 0.066(8) 0.042(5) 0.028(5) -0.002(4) 0.011(4) 0.002(5) C7 0.062(8) 0.027(5) 0.039(5) 0.010(4) 0.012(5) -0.003(4) C8 0.031(6) 0.057(6) 0.036(5) 0.006(4) -0.004(4) 0.004(5) C9 0.029(6) 0.051(6) 0.027(4) 0.008(4) 0.000(4) -0.013(5) C10 0.050(7) 0.031(5) 0.034(4) 0.000(4) 0.001(4) -0.011(4) C11 0.026(5) 0.033(4) 0.024(4) 0.001(3) 0.000(3) 0.011(4) C12 0.032(6) 0.030(4) 0.024(4) -0.002(3) 0.006(3) 0.007(4) C13 0.023(5) 0.029(4) 0.024(4) -0.002(3) 0.000(3) -0.008(4) C14 0.020(5) 0.041(5) 0.028(4) -0.008(4) 0.005(4) -0.011(4) C15 0.040(2) 0.0385(19) 0.0310(18) 0.0020(15) -0.0087(15) 0.0039(16) C16 0.040(2) 0.0383(19) 0.0307(18) 0.0019(15) -0.0089(15) 0.0040(16) C17 0.049(7) 0.026(4) 0.036(4) -0.007(4) -0.009(4) -0.009(4) N1 0.030(5) 0.032(4) 0.027(3) 0.005(3) 0.001(3) -0.005(3) N2 0.040(2) 0.0383(19) 0.0309(18) 0.0020(15) -0.0087(15) 0.0039(16) N3 0.040(2) 0.0384(19) 0.0308(18) 0.0020(15) -0.0087(15) 0.0038(16) N4 0.040(2) 0.0392(19) 0.0316(18) 0.0020(15) -0.0086(15) 0.0039(16) O1 0.056(5) 0.034(3) 0.026(3) 0.002(3) 0.006(3) 0.010(3) O2 0.037(4) 0.037(3) 0.036(3) 0.007(3) 0.011(3) -0.001(3) O3 0.050(5) 0.063(4) 0.052(4) 0.019(3) -0.011(3) -0.026(4) O4 0.040(4) 0.041(4) 0.055(4) 0.015(3) -0.014(3) -0.014(3) O5 0.028(4) 0.047(3) 0.043(3) 0.011(3) -0.010(3) -0.002(3) O6 0.033(4) 0.011(2) 0.033(3) 0.000(2) -0.007(2) 0.001(2) O1W 0.040(5) 0.035(3) 0.033(3) -0.005(3) 0.001(3) 0.006(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O6 2.247(4) 3_556 ? Cd1 O6 2.247(4) . ? Cd1 O1 2.313(5) . ? Cd1 O1 2.313(5) 3_556 ? Cd1 O5 2.323(6) 2_556 ? Cd1 O5 2.323(6) 4 ? Cd2 O4 2.253(6) 2_556 ? Cd2 O6 2.292(5) . ? Cd2 O6 2.297(5) 3_566 ? Cd2 N2 2.334(6) . ? Cd2 O2 2.342(5) . ? Cd2 O1W 2.382(6) . ? Cd2 Cd2 3.4086(12) 3_566 ? C1 O1 1.254(9) . ? C1 O2 1.284(9) . ? C1 C2 1.482(10) . ? C2 C7 1.380(10) . ? C2 C3 1.385(10) . ? C3 C4 1.361(10) . ? C3 H3 0.9300 . ? C4 C5 1.399(11) . ? C4 H4 0.9300 . ? C5 C6 1.372(11) . ? C5 C8 1.497(10) . ? C6 C7 1.386(11) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.500(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O3 1.235(10) . ? C9 N1 1.397(10) . ? C9 C10 1.415(12) . ? C10 C11 1.359(11) . ? C10 H10 0.9300 . ? C11 C12 1.423(10) . ? C11 H11 0.9300 . ? C12 C13 1.366(11) . ? C12 C14 1.498(11) . ? C13 N1 1.345(10) . ? C13 H13 0.9300 . ? C14 O5 1.241(9) . ? C14 O4 1.260(9) . ? C15 N2 1.307(10) . ? C15 N3 1.334(10) . ? C15 H15 0.9300 . ? C16 N4 1.319(9) . ? C16 N3 1.332(10) . ? C16 H16 0.9300 . ? C17 N3 1.468(9) . ? C17 C17 1.525(16) 2_556 ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? N2 N4 1.373(9) . ? O4 Cd2 2.253(6) 2_556 ? O5 Cd1 2.323(6) 2_556 ? O6 Cd2 2.297(5) 3_566 ? O1W H1A 0.84(9) . ? O1W H1B 0.897(10) . ? 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 O6 Cd1 O6 180.0(2) 3_556 . ? O6 Cd1 O1 81.70(17) 3_556 . ? O6 Cd1 O1 98.30(17) . . ? O6 Cd1 O1 98.30(17) 3_556 3_556 ? O6 Cd1 O1 81.70(17) . 3_556 ? O1 Cd1 O1 180.000(1) . 3_556 ? O6 Cd1 O5 88.94(19) 3_556 2_556 ? O6 Cd1 O5 91.06(19) . 2_556 ? O1 Cd1 O5 89.9(2) . 2_556 ? O1 Cd1 O5 90.1(2) 3_556 2_556 ? O6 Cd1 O5 91.06(19) 3_556 4 ? O6 Cd1 O5 88.94(19) . 4 ? O1 Cd1 O5 90.1(2) . 4 ? O1 Cd1 O5 89.9(2) 3_556 4 ? O5 Cd1 O5 180.000(1) 2_556 4 ? O4 Cd2 O6 102.17(18) 2_556 . ? O4 Cd2 O6 171.6(2) 2_556 3_566 ? O6 Cd2 O6 84.05(16) . 3_566 ? O4 Cd2 N2 82.2(2) 2_556 . ? O6 Cd2 N2 171.7(2) . . ? O6 Cd2 N2 92.3(2) 3_566 . ? O4 Cd2 O2 102.2(2) 2_556 . ? O6 Cd2 O2 85.16(19) . . ? O6 Cd2 O2 83.82(19) 3_566 . ? N2 Cd2 O2 87.0(2) . . ? O4 Cd2 O1W 87.6(2) 2_556 . ? O6 Cd2 O1W 81.40(19) . . ? O6 Cd2 O1W 87.73(19) 3_566 . ? N2 Cd2 O1W 106.0(2) . . ? O2 Cd2 O1W 164.8(2) . . ? O4 Cd2 Cd2 143.93(14) 2_556 3_566 ? O6 Cd2 Cd2 42.08(12) . 3_566 ? O6 Cd2 Cd2 41.97(12) 3_566 3_566 ? N2 Cd2 Cd2 133.83(17) . 3_566 ? O2 Cd2 Cd2 82.57(14) . 3_566 ? O1W Cd2 Cd2 82.69(16) . 3_566 ? O1 C1 O2 124.3(7) . . ? O1 C1 C2 118.5(7) . . ? O2 C1 C2 117.2(7) . . ? C7 C2 C3 117.8(7) . . ? C7 C2 C1 121.8(7) . . ? C3 C2 C1 120.4(7) . . ? C4 C3 C2 121.5(7) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 120.4(7) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 118.8(7) . . ? C6 C5 C8 120.1(8) . . ? C4 C5 C8 121.1(8) . . ? C5 C6 C7 120.0(8) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C2 C7 C6 121.4(7) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C5 C8 N1 109.7(7) . . ? C5 C8 H8A 109.7 . . ? N1 C8 H8A 109.7 . . ? C5 C8 H8B 109.7 . . ? N1 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O3 C9 N1 120.2(8) . . ? O3 C9 C10 126.2(8) . . ? N1 C9 C10 113.5(8) . . ? C11 C10 C9 123.8(8) . . ? C11 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? C10 C11 C12 120.1(7) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 115.9(8) . . ? C13 C12 C14 121.2(7) . . ? C11 C12 C14 122.9(7) . . ? N1 C13 C12 123.5(7) . . ? N1 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? O5 C14 O4 127.5(8) . . ? O5 C14 C12 116.2(7) . . ? O4 C14 C12 116.3(7) . . ? N2 C15 N3 109.7(8) . . ? N2 C15 H15 125.1 . . ? N3 C15 H15 125.1 . . ? N4 C16 N3 103.8(7) . . ? N4 C16 H16 128.1 . . ? N3 C16 H16 128.1 . . ? N3 C17 C17 112.9(6) . 2_556 ? N3 C17 H17A 109.0 . . ? C17 C17 H17A 109.0 2_556 . ? N3 C17 H17B 109.0 . . ? C17 C17 H17B 109.0 2_556 . ? H17A C17 H17B 107.8 . . ? C13 N1 C9 123.0(7) . . ? C13 N1 C8 117.9(6) . . ? C9 N1 C8 118.9(7) . . ? C15 N2 N4 103.8(6) . . ? C15 N2 Cd2 128.9(6) . . ? N4 N2 Cd2 127.2(5) . . ? C16 N3 C15 110.3(7) . . ? C16 N3 C17 120.3(7) . . ? C15 N3 C17 129.4(7) . . ? C16 N4 N2 112.3(6) . . ? C1 O1 Cd1 129.9(5) . . ? C1 O2 Cd2 121.8(5) . . ? C14 O4 Cd2 129.2(5) . 2_556 ? C14 O5 Cd1 130.8(5) . 2_556 ? Cd1 O6 Cd2 105.36(19) . . ? Cd1 O6 Cd2 140.5(3) . 3_566 ? Cd2 O6 Cd2 95.95(16) . 3_566 ? Cd2 O1W H1A 101(7) . . ? Cd2 O1W H1B 127(5) . . ? H1A O1W H1B 101(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 170.4(8) . . . . ? O2 C1 C2 C7 -10.9(12) . . . . ? O1 C1 C2 C3 -9.3(12) . . . . ? O2 C1 C2 C3 169.3(8) . . . . ? C7 C2 C3 C4 0.9(13) . . . . ? C1 C2 C3 C4 -179.3(8) . . . . ? C2 C3 C4 C5 0.6(13) . . . . ? C3 C4 C5 C6 -1.2(13) . . . . ? C3 C4 C5 C8 179.8(8) . . . . ? C4 C5 C6 C7 0.3(14) . . . . ? C8 C5 C6 C7 179.3(8) . . . . ? C3 C2 C7 C6 -1.9(14) . . . . ? C1 C2 C7 C6 178.3(8) . . . . ? C5 C6 C7 C2 1.4(15) . . . . ? C6 C5 C8 N1 -116.4(9) . . . . ? C4 C5 C8 N1 62.6(11) . . . . ? O3 C9 C10 C11 175.7(8) . . . . ? N1 C9 C10 C11 -1.8(12) . . . . ? C9 C10 C11 C12 -0.9(12) . . . . ? C10 C11 C12 C13 2.3(10) . . . . ? C10 C11 C12 C14 -176.7(7) . . . . ? C11 C12 C13 N1 -1.1(10) . . . . ? C14 C12 C13 N1 178.0(7) . . . . ? C13 C12 C14 O5 170.7(7) . . . . ? C11 C12 C14 O5 -10.3(10) . . . . ? C13 C12 C14 O4 -8.4(10) . . . . ? C11 C12 C14 O4 170.6(7) . . . . ? C12 C13 N1 C9 -1.8(11) . . . . ? C12 C13 N1 C8 -177.3(7) . . . . ? O3 C9 N1 C13 -174.5(8) . . . . ? C10 C9 N1 C13 3.2(11) . . . . ? O3 C9 N1 C8 0.9(11) . . . . ? C10 C9 N1 C8 178.6(7) . . . . ? C5 C8 N1 C13 74.7(9) . . . . ? C5 C8 N1 C9 -101.0(9) . . . . ? N3 C15 N2 N4 1.9(9) . . . . ? N3 C15 N2 Cd2 -174.9(5) . . . . ? O4 Cd2 N2 C15 170.3(7) 2_556 . . . ? O6 Cd2 N2 C15 -3.2(7) 3_566 . . . ? O2 Cd2 N2 C15 -86.9(7) . . . . ? O1W Cd2 N2 C15 85.1(7) . . . . ? Cd2 Cd2 N2 C15 -10.2(8) 3_566 . . . ? O4 Cd2 N2 N4 -5.7(6) 2_556 . . . ? O6 Cd2 N2 N4 -179.2(6) 3_566 . . . ? O2 Cd2 N2 N4 97.1(7) . . . . ? O1W Cd2 N2 N4 -90.9(7) . . . . ? Cd2 Cd2 N2 N4 173.8(5) 3_566 . . . ? N4 C16 N3 C15 -1.4(9) . . . . ? N4 C16 N3 C17 179.5(7) . . . . ? N2 C15 N3 C16 -0.4(10) . . . . ? N2 C15 N3 C17 178.6(7) . . . . ? C17 C17 N3 C16 -90.6(11) 2_556 . . . ? C17 C17 N3 C15 90.5(11) 2_556 . . . ? N3 C16 N4 N2 2.6(9) . . . . ? C15 N2 N4 C16 -2.8(9) . . . . ? Cd2 N2 N4 C16 174.0(5) . . . . ? O2 C1 O1 Cd1 -17.0(12) . . . . ? C2 C1 O1 Cd1 161.5(5) . . . . ? O6 Cd1 O1 C1 -165.6(7) 3_556 . . . ? O6 Cd1 O1 C1 14.4(7) . . . . ? O5 Cd1 O1 C1 105.5(7) 2_556 . . . ? O5 Cd1 O1 C1 -74.5(7) 4 . . . ? O1 C1 O2 Cd2 -39.2(10) . . . . ? C2 C1 O2 Cd2 142.3(6) . . . . ? O4 Cd2 O2 C1 -21.0(6) 2_556 . . . ? O6 Cd2 O2 C1 80.4(6) . . . . ? O6 Cd2 O2 C1 165.0(6) 3_566 . . . ? N2 Cd2 O2 C1 -102.4(6) . . . . ? O1W Cd2 O2 C1 108.3(8) . . . . ? Cd2 Cd2 O2 C1 122.7(6) 3_566 . . . ? O5 C14 O4 Cd2 -7.1(12) . . . 2_556 ? C12 C14 O4 Cd2 172.0(5) . . . 2_556 ? O4 C14 O5 Cd1 -29.6(12) . . . 2_556 ? C12 C14 O5 Cd1 151.4(5) . . . 2_556 ? O1 Cd1 O6 Cd2 37.4(2) . . . . ? O1 Cd1 O6 Cd2 -142.6(2) 3_556 . . . ? O5 Cd1 O6 Cd2 -52.7(2) 2_556 . . . ? O5 Cd1 O6 Cd2 127.3(2) 4 . . . ? O1 Cd1 O6 Cd2 -82.8(4) . . . 3_566 ? O1 Cd1 O6 Cd2 97.2(4) 3_556 . . 3_566 ? O5 Cd1 O6 Cd2 -172.8(3) 2_556 . . 3_566 ? O5 Cd1 O6 Cd2 7.2(3) 4 . . 3_566 ? O4 Cd2 O6 Cd1 39.3(3) 2_556 . . . ? O6 Cd2 O6 Cd1 -146.4(3) 3_566 . . . ? O2 Cd2 O6 Cd1 -62.2(2) . . . . ? O1W Cd2 O6 Cd1 125.0(2) . . . . ? Cd2 Cd2 O6 Cd1 -146.4(3) 3_566 . . . ? O4 Cd2 O6 Cd2 -174.2(2) 2_556 . . 3_566 ? O6 Cd2 O6 Cd2 0.0 3_566 . . 3_566 ? O2 Cd2 O6 Cd2 84.28(19) . . . 3_566 ? O1W Cd2 O6 Cd2 -88.6(2) . . . 3_566 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1A O2 0.84(9) 1.97(10) 2.807(8) 172(10) 3_566 O1W H1B O3 0.897(10) 1.81(2) 2.690(8) 167(8) 4_655 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.852 _refine_diff_density_min -1.538 _refine_diff_density_rms 0.163 #=========================END data_Compound-7 _database_code_depnum_ccdc_archive 'CCDC 873956' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H20 N2 O11 Pb2' _chemical_formula_sum 'C28 H20 N2 O11 Pb2' _chemical_formula_weight 974.84 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' Pb Pb -3.3944 10.1111 '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/n _symmetry_space_group_name_hall '-p 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 4.8640(3) _cell_length_b 9.6450(6) _cell_length_c 27.5870(17) _cell_angle_alpha 90 _cell_angle_beta 92.265(6) _cell_angle_gamma 90 _cell_volume 1293.19(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1945 _cell_measurement_theta_min 4.1844 _cell_measurement_theta_max 29.1782 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 13.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.835 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5931 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 4.23 _diffrn_reflns_theta_max 29.24 _reflns_number_total 2977 _reflns_number_gt 2252 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0256P)^2^+2.6959P] 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 2977 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.006 _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 Pb1 Pb 0.71985(6) 1.16282(3) 0.074268(12) 0.02817(13) Uani 1 1 d . . . C1 C 0.3082(18) 0.6481(9) 0.3512(3) 0.031(2) Uani 1 1 d . . . C2 C 0.1656(15) 0.6494(9) 0.3021(3) 0.0240(18) Uani 1 1 d . . . C3 C 0.2455(17) 0.5585(9) 0.2662(3) 0.030(2) Uani 1 1 d . . . H3 H 0.3832 0.4935 0.2728 0.036 Uiso 1 1 calc R . . C4 C 0.1196(17) 0.5658(9) 0.2213(3) 0.030(2) Uani 1 1 d . . . H4 H 0.1733 0.5037 0.1977 0.036 Uiso 1 1 calc R . . C5 C -0.0855(15) 0.6615(8) 0.2091(3) 0.0238(18) Uani 1 1 d . . . C6 C -0.1645(18) 0.7497(9) 0.2458(3) 0.032(2) Uani 1 1 d . . . H6 H -0.3044 0.8136 0.2394 0.038 Uiso 1 1 calc R . . C7 C -0.0389(17) 0.7444(9) 0.2920(3) 0.029(2) Uani 1 1 d . . . H7 H -0.0934 0.8052 0.3159 0.034 Uiso 1 1 calc R . . C8 C -0.2249(17) 0.6719(10) 0.1607(3) 0.032(2) Uani 1 1 d . . . H8A H -0.3029 0.7641 0.1569 0.039 Uiso 1 1 calc R . . H8B H -0.3756 0.6060 0.1588 0.039 Uiso 1 1 calc R . . C9 C -0.0462(16) 0.5137(8) 0.0980(3) 0.0241(18) Uani 1 1 d . . . C10 C 0.1333(17) 0.4980(9) 0.0593(3) 0.032(2) Uani 1 1 d . . . H10 H 0.1397 0.4138 0.0429 0.038 Uiso 1 1 calc R . . C11 C 0.2949(18) 0.6033(9) 0.0457(3) 0.030(2) Uani 1 1 d . . . H11 H 0.4060 0.5903 0.0194 0.036 Uiso 1 1 calc R . . C12 C 0.3025(16) 0.7323(9) 0.0697(3) 0.0233(18) Uani 1 1 d . . . C13 C 0.1274(16) 0.7495(9) 0.1072(3) 0.0261(19) Uani 1 1 d . . . H13 H 0.1252 0.8334 0.1238 0.031 Uiso 1 1 calc R . . C14 C 0.4886(16) 0.8439(9) 0.0554(3) 0.028(2) Uani 1 1 d . . . N1 N -0.0422(14) 0.6454(7) 0.1202(2) 0.0249(16) Uani 1 1 d . . . O1 O 0.5391(12) 0.5855(8) 0.3552(2) 0.0418(17) Uani 1 1 d . . . O2 O 0.2065(13) 0.7109(7) 0.3865(2) 0.0372(15) Uani 1 1 d . . . O3 O -0.2001(13) 0.4224(7) 0.1134(2) 0.0429(17) Uani 1 1 d . . . O4 O 0.5267(13) 0.9424(7) 0.0858(2) 0.0431(17) Uani 1 1 d . . . O5 O 0.6050(13) 0.8347(7) 0.0160(3) 0.0443(17) Uani 1 1 d . . . O1W O 1.007(4) 1.015(2) 0.0205(6) 0.074(6) 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 Pb1 0.03397(19) 0.02728(19) 0.02332(19) 0.00099(15) 0.00185(13) -0.00818(16) C1 0.039(5) 0.031(5) 0.021(5) 0.001(4) -0.001(4) -0.008(4) C2 0.019(4) 0.028(4) 0.026(5) -0.001(4) 0.004(3) -0.004(4) C3 0.033(4) 0.033(5) 0.025(5) 0.001(4) 0.006(4) 0.009(4) C4 0.039(5) 0.032(5) 0.019(4) -0.002(4) 0.002(4) 0.008(4) C5 0.021(4) 0.023(4) 0.027(5) 0.007(4) 0.002(3) -0.005(4) C6 0.034(5) 0.023(4) 0.039(6) 0.003(4) 0.002(4) 0.003(4) C7 0.035(4) 0.034(5) 0.017(4) -0.003(4) 0.006(4) 0.004(4) C8 0.027(4) 0.046(6) 0.023(5) 0.004(4) 0.001(4) 0.004(4) C9 0.032(4) 0.020(4) 0.020(4) 0.007(4) -0.006(3) -0.003(4) C10 0.043(5) 0.022(4) 0.030(5) -0.006(4) 0.008(4) -0.012(4) C11 0.039(5) 0.033(5) 0.018(4) 0.000(4) 0.005(4) 0.002(4) C12 0.024(4) 0.023(4) 0.023(4) 0.009(4) -0.001(3) -0.010(4) C13 0.034(4) 0.024(4) 0.019(4) 0.009(4) -0.009(4) -0.005(4) C14 0.026(4) 0.033(5) 0.025(5) 0.010(4) 0.000(4) 0.001(4) N1 0.032(4) 0.024(4) 0.019(4) -0.004(3) 0.002(3) -0.003(3) O1 0.035(3) 0.061(5) 0.029(4) -0.002(3) 0.000(3) 0.006(3) O2 0.047(4) 0.034(4) 0.030(4) -0.011(3) -0.001(3) 0.002(3) O3 0.048(4) 0.030(4) 0.051(4) 0.005(3) 0.014(3) -0.012(3) O4 0.053(4) 0.030(4) 0.047(4) -0.010(3) 0.009(3) -0.022(3) O5 0.045(4) 0.042(4) 0.048(4) 0.006(3) 0.019(3) -0.016(3) O1W 0.050(8) 0.059(11) 0.111(18) 0.030(15) -0.032(12) -0.032(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O4 2.350(6) . ? Pb1 O1 2.352(6) 2_655 ? Pb1 O2 2.422(6) 2 ? Pb1 O1W 2.52(2) . ? Pb1 O3 2.748(7) 1_665 ? C1 O2 1.263(10) . ? C1 O1 1.276(10) . ? C1 C2 1.498(11) . ? C2 C7 1.373(11) . ? C2 C3 1.389(11) . ? C3 C4 1.363(11) . ? C3 H3 0.9300 . ? C4 C5 1.391(11) . ? C4 H4 0.9300 . ? C5 C6 1.389(12) . ? C5 C8 1.476(11) . ? C6 C7 1.391(11) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 N1 1.478(10) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O3 1.241(9) . ? C9 N1 1.409(10) . ? C9 C10 1.415(11) . ? C10 C11 1.346(12) . ? C10 H10 0.9300 . ? C11 C12 1.410(12) . ? C11 H11 0.9300 . ? C12 C13 1.374(11) . ? C12 C14 1.471(11) . ? C13 N1 1.357(10) . ? C13 H13 0.9300 . ? C14 O5 1.247(10) . ? C14 O4 1.277(11) . ? O1 Pb1 2.352(6) 2_645 ? O2 Pb1 2.422(6) 2_545 ? O3 Pb1 2.748(7) 1_445 ? O1W O1W 1.16(3) 3_775 ? 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 Pb1 O1 77.9(2) . 2_655 ? O4 Pb1 O2 76.1(2) . 2 ? O1 Pb1 O2 95.6(2) 2_655 2 ? O4 Pb1 O1W 78.5(4) . . ? O1 Pb1 O1W 92.2(4) 2_655 . ? O2 Pb1 O1W 151.1(4) 2 . ? O4 Pb1 O3 145.3(2) . 1_665 ? O1 Pb1 O3 84.6(2) 2_655 1_665 ? O2 Pb1 O3 76.1(2) 2 1_665 ? O1W Pb1 O3 132.4(4) . 1_665 ? O2 C1 O1 122.0(8) . . ? O2 C1 C2 120.7(8) . . ? O1 C1 C2 117.2(8) . . ? C7 C2 C3 119.8(8) . . ? C7 C2 C1 119.7(8) . . ? C3 C2 C1 120.4(8) . . ? C4 C3 C2 119.1(8) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 123.1(8) . . ? C3 C4 H4 118.4 . . ? C5 C4 H4 118.4 . . ? C6 C5 C4 116.5(8) . . ? C6 C5 C8 119.2(8) . . ? C4 C5 C8 124.3(8) . . ? C5 C6 C7 121.4(8) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C2 C7 C6 119.9(8) . . ? C2 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C5 C8 N1 113.8(7) . . ? C5 C8 H8A 108.8 . . ? N1 C8 H8A 108.8 . . ? C5 C8 H8B 108.8 . . ? N1 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? O3 C9 N1 119.3(8) . . ? O3 C9 C10 125.5(8) . . ? N1 C9 C10 115.2(7) . . ? C11 C10 C9 121.0(8) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 122.6(8) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C13 C12 C11 117.1(7) . . ? C13 C12 C14 121.3(8) . . ? C11 C12 C14 121.6(8) . . ? N1 C13 C12 120.7(8) . . ? N1 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? O5 C14 O4 124.5(8) . . ? O5 C14 C12 119.2(8) . . ? O4 C14 C12 116.3(8) . . ? C13 N1 C9 123.4(7) . . ? C13 N1 C8 117.5(7) . . ? C9 N1 C8 119.0(7) . . ? C1 O1 Pb1 109.3(5) . 2_645 ? C1 O2 Pb1 128.4(6) . 2_545 ? C9 O3 Pb1 126.1(6) . 1_445 ? C14 O4 Pb1 129.3(6) . . ? O1W O1W Pb1 134(2) 3_775 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 15.5(12) . . . . ? O1 C1 C2 C7 -162.1(8) . . . . ? O2 C1 C2 C3 -166.8(8) . . . . ? O1 C1 C2 C3 15.6(12) . . . . ? C7 C2 C3 C4 0.3(13) . . . . ? C1 C2 C3 C4 -177.4(8) . . . . ? C2 C3 C4 C5 0.7(14) . . . . ? C3 C4 C5 C6 -1.7(13) . . . . ? C3 C4 C5 C8 179.9(8) . . . . ? C4 C5 C6 C7 1.7(12) . . . . ? C8 C5 C6 C7 -179.7(8) . . . . ? C3 C2 C7 C6 -0.3(13) . . . . ? C1 C2 C7 C6 177.5(8) . . . . ? C5 C6 C7 C2 -0.8(13) . . . . ? C6 C5 C8 N1 144.9(8) . . . . ? C4 C5 C8 N1 -36.7(12) . . . . ? O3 C9 C10 C11 -179.2(8) . . . . ? N1 C9 C10 C11 0.5(12) . . . . ? C9 C10 C11 C12 2.1(13) . . . . ? C10 C11 C12 C13 -2.6(12) . . . . ? C10 C11 C12 C14 177.6(8) . . . . ? C11 C12 C13 N1 0.5(11) . . . . ? C14 C12 C13 N1 -179.7(7) . . . . ? C13 C12 C14 O5 -166.5(8) . . . . ? C11 C12 C14 O5 13.2(12) . . . . ? C13 C12 C14 O4 16.0(11) . . . . ? C11 C12 C14 O4 -164.2(8) . . . . ? C12 C13 N1 C9 2.1(11) . . . . ? C12 C13 N1 C8 -179.9(7) . . . . ? O3 C9 N1 C13 177.1(7) . . . . ? C10 C9 N1 C13 -2.6(11) . . . . ? O3 C9 N1 C8 -0.9(11) . . . . ? C10 C9 N1 C8 179.4(7) . . . . ? C5 C8 N1 C13 -78.6(10) . . . . ? C5 C8 N1 C9 99.5(9) . . . . ? O2 C1 O1 Pb1 -16.9(10) . . . 2_645 ? C2 C1 O1 Pb1 160.7(6) . . . 2_645 ? O1 C1 O2 Pb1 -117.5(8) . . . 2_545 ? C2 C1 O2 Pb1 65.0(10) . . . 2_545 ? N1 C9 O3 Pb1 175.5(5) . . . 1_445 ? C10 C9 O3 Pb1 -4.8(11) . . . 1_445 ? O5 C14 O4 Pb1 17.4(13) . . . . ? C12 C14 O4 Pb1 -165.3(5) . . . . ? O1 Pb1 O4 C14 -130.8(8) 2_655 . . . ? O2 Pb1 O4 C14 130.2(8) 2 . . . ? O1W Pb1 O4 C14 -36.1(8) . . . . ? O3 Pb1 O4 C14 167.8(6) 1_665 . . . ? O4 Pb1 O1W O1W 93(3) . . . 3_775 ? O1 Pb1 O1W O1W 170(3) 2_655 . . 3_775 ? O2 Pb1 O1W O1W 65(3) 2 . . 3_775 ? O3 Pb1 O1W O1W -105(3) 1_665 . . 3_775 ? _diffrn_measured_fraction_theta_max 0.846 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.932 _refine_diff_density_min -1.760 _refine_diff_density_rms 0.264 #=========================END