data_complex-1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H28 Co N4 O4, C3 H7 N O' _chemical_formula_sum 'C30 H35 Co N5 O5' _chemical_formula_weight 604.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.071(3) _cell_length_b 13.885(5) _cell_length_c 17.666(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2960.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 9925 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 24.97 _exptl_crystal_description 'block' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9343 _exptl_absorpt_correction_T_max 0.9516 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21047 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.04 _reflns_number_total 5238 _reflns_number_gt 4060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0808P)^2^+3.2271P] 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 0.01(3) _refine_ls_number_reflns 5238 _refine_ls_number_parameters 348 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1456 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.14250(5) 0.69343(5) 0.26266(4) 0.0341(2) Uani 1 1 d . . . O2 O 0.3772(3) 0.8411(2) 0.3953(2) 0.0345(9) Uani 1 1 d . . . O1 O 0.0543(3) 0.7321(3) 0.3521(2) 0.0397(9) Uani 1 1 d . . . O3 O 0.7612(3) 1.1158(3) 0.3214(2) 0.0392(9) Uani 1 1 d . . . O4 O 0.8025(3) 1.0475(3) 0.2125(2) 0.0447(10) Uani 1 1 d . . . N1 N 0.2788(3) 0.7570(3) 0.3147(3) 0.0384(11) Uani 1 1 d . . . N2 N 0.3867(3) 0.7694(3) 0.2845(3) 0.0389(11) Uani 1 1 d . . . N3 N 0.1251(3) 0.8131(3) 0.1894(2) 0.0375(10) Uani 1 1 d . . . N4 N -0.0108(3) 0.6342(3) 0.2150(3) 0.0342(11) Uani 1 1 d . . . C1 C 0.0804(4) 0.7756(4) 0.4153(3) 0.0349(13) Uani 1 1 d . . . C2 C -0.0026(4) 0.7939(4) 0.4705(3) 0.0364(13) Uani 1 1 d . . . H2 H -0.0757 0.7720 0.4605 0.044 Uiso 1 1 calc R . . C3 C 0.0160(5) 0.8398(4) 0.5353(3) 0.0406(14) Uani 1 1 d . . . H3 H -0.0436 0.8512 0.5693 0.049 Uiso 1 1 calc R . . C4 C 0.1231(5) 0.8717(4) 0.5538(3) 0.0476(15) Uani 1 1 d . . . H4 H 0.1370 0.9034 0.6005 0.057 Uiso 1 1 calc R . . C5 C 0.2075(5) 0.8560(4) 0.5028(3) 0.0410(13) Uani 1 1 d . . . H5 H 0.2802 0.8774 0.5146 0.049 Uiso 1 1 calc R . . C6 C 0.1881(4) 0.8087(4) 0.4334(3) 0.0312(11) Uani 1 1 d . . . C7 C 0.2773(4) 0.7995(4) 0.3799(3) 0.0329(12) Uani 1 1 d . . . C8 C 0.4398(4) 0.8183(4) 0.3333(3) 0.0369(13) Uani 1 1 d . . . C9 C 0.5593(4) 0.8452(4) 0.3331(3) 0.0388(14) Uani 1 1 d . . . H9 H 0.5927 0.8198 0.3809 0.047 Uiso 1 1 calc R . . C10 C 0.6206(5) 0.7993(4) 0.2677(4) 0.0604(18) Uani 1 1 d . . . H10A H 0.5715 0.7931 0.2231 0.072 Uiso 1 1 calc R . . H10B H 0.6477 0.7345 0.2819 0.072 Uiso 1 1 calc R . . C11 C 0.7178(5) 0.8667(4) 0.2504(5) 0.063(2) Uani 1 1 d . . . H11A H 0.7887 0.8311 0.2541 0.075 Uiso 1 1 calc R . . H11B H 0.7109 0.8929 0.1985 0.075 Uiso 1 1 calc R . . C12 C 0.7149(4) 0.9482(4) 0.3083(4) 0.0387(14) Uani 1 1 d . . . C13 C 0.5876(4) 0.9543(4) 0.3285(3) 0.0342(12) Uani 1 1 d . . . C14 C 0.5242(4) 1.0032(4) 0.2649(4) 0.0492(15) Uani 1 1 d . . . H14A H 0.4452 1.0056 0.2777 0.074 Uiso 1 1 calc R . . H14B H 0.5342 0.9666 0.2179 0.074 Uiso 1 1 calc R . . H14C H 0.5522 1.0688 0.2579 0.074 Uiso 1 1 calc R . . C15 C 0.5635(5) 1.0053(5) 0.4028(4) 0.0553(18) Uani 1 1 d . . . H15A H 0.4833 1.0063 0.4116 0.083 Uiso 1 1 calc R . . H15B H 0.5915 1.0715 0.4003 0.083 Uiso 1 1 calc R . . H15C H 0.6001 0.9710 0.4443 0.083 Uiso 1 1 calc R . . C16 C 0.7842(5) 0.9206(5) 0.3762(5) 0.064(2) Uani 1 1 d . . . H16A H 0.8625 0.9186 0.3617 0.096 Uiso 1 1 calc R . . H16B H 0.7612 0.8571 0.3945 0.096 Uiso 1 1 calc R . . H16C H 0.7738 0.9684 0.4165 0.096 Uiso 1 1 calc R . . C17 C 0.7605(4) 1.0421(4) 0.2788(3) 0.0363(13) Uani 1 1 d . . . C18 C 0.2077(4) 0.8418(4) 0.1436(3) 0.0413(14) Uani 1 1 d . . . H18 H 0.2771 0.8098 0.1464 0.050 Uiso 1 1 calc R . . C19 C 0.1945(5) 0.9163(4) 0.0928(4) 0.0492(16) Uani 1 1 d . . . H19 H 0.2542 0.9349 0.0609 0.059 Uiso 1 1 calc R . . C20 C 0.0948(6) 0.9635(5) 0.0884(4) 0.0537(17) Uani 1 1 d . . . H20 H 0.0837 1.0135 0.0525 0.064 Uiso 1 1 calc R . . C21 C 0.0108(5) 0.9369(4) 0.1374(4) 0.0507(16) Uani 1 1 d . . . H21 H -0.0581 0.9701 0.1375 0.061 Uiso 1 1 calc R . . C22 C 0.0293(5) 0.8617(4) 0.1858(4) 0.0467(16) Uani 1 1 d . . . H22 H -0.0291 0.8429 0.2187 0.056 Uiso 1 1 calc R . . C23 C -0.0119(5) 0.6019(5) 0.1436(3) 0.0455(15) Uani 1 1 d . . . H23 H 0.0520 0.6116 0.1131 0.055 Uiso 1 1 calc R . . C24 C -0.1014(5) 0.5553(5) 0.1123(4) 0.0546(17) Uani 1 1 d . . . H24 H -0.0991 0.5324 0.0617 0.066 Uiso 1 1 calc R . . C25 C -0.1947(5) 0.5426(5) 0.1563(4) 0.0521(17) Uani 1 1 d . . . H25 H -0.2582 0.5118 0.1357 0.062 Uiso 1 1 calc R . . C26 C -0.1955(4) 0.5745(4) 0.2297(4) 0.0456(15) Uani 1 1 d . . . H26 H -0.2584 0.5654 0.2612 0.055 Uiso 1 1 calc R . . C27 C -0.1009(4) 0.6206(4) 0.2563(3) 0.0384(13) Uani 1 1 d . . . H27 H -0.1010 0.6436 0.3069 0.046 Uiso 1 1 calc R . . N5 N 0.6315(17) 0.8250(19) 0.0479(7) 0.236(4) Uani 1 1 d . . . O5 O 0.4702(11) 0.8814(12) 0.0681(5) 0.236(4) Uani 1 1 d . . . C28 C 0.572(2) 0.908(2) 0.0563(10) 0.236(4) Uani 1 1 d . . . H28 H 0.6000 0.9720 0.0540 0.283 Uiso 1 1 calc R . . C29 C 0.5771(16) 0.7248(18) 0.0562(9) 0.236(4) Uani 1 1 d . . . H29A H 0.5698 0.6950 0.0062 0.354 Uiso 1 1 calc R . . H29B H 0.5036 0.7319 0.0791 0.354 Uiso 1 1 calc R . . H29C H 0.6234 0.6840 0.0886 0.354 Uiso 1 1 calc R . . C30 C 0.7530(16) 0.8249(17) 0.0403(8) 0.236(4) Uani 1 1 d . . . H30A H 0.7735 0.7973 -0.0089 0.354 Uiso 1 1 calc R . . H30B H 0.7857 0.7861 0.0809 0.354 Uiso 1 1 calc R . . H30C H 0.7808 0.8910 0.0437 0.354 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0199(3) 0.0378(4) 0.0446(4) -0.0044(3) 0.0035(3) -0.0028(3) O2 0.0210(18) 0.033(2) 0.049(2) -0.0026(16) 0.0009(16) -0.0070(15) O1 0.0220(18) 0.049(2) 0.048(2) -0.0111(19) 0.0041(17) -0.0047(17) O3 0.027(2) 0.036(2) 0.054(2) 0.000(2) 0.0019(19) -0.0016(17) O4 0.027(2) 0.050(3) 0.057(3) 0.003(2) 0.0087(19) -0.0018(18) N1 0.017(2) 0.046(3) 0.052(3) -0.006(2) 0.007(2) -0.005(2) N2 0.021(2) 0.040(2) 0.056(3) -0.004(2) 0.009(2) -0.0030(19) N3 0.020(2) 0.042(3) 0.050(3) -0.006(2) 0.0064(19) -0.004(2) N4 0.020(2) 0.033(2) 0.050(3) -0.002(2) 0.001(2) -0.0013(18) C1 0.032(3) 0.029(3) 0.044(3) 0.003(2) 0.001(2) -0.005(2) C2 0.023(2) 0.045(3) 0.041(3) 0.003(3) 0.004(2) -0.004(3) C3 0.035(3) 0.039(3) 0.048(4) 0.004(3) 0.006(3) 0.003(3) C4 0.053(4) 0.045(4) 0.045(3) -0.004(3) 0.009(3) -0.006(3) C5 0.034(3) 0.049(4) 0.040(3) -0.001(3) 0.001(3) -0.006(3) C6 0.025(2) 0.031(3) 0.037(3) 0.003(3) 0.004(2) 0.003(2) C7 0.022(2) 0.027(3) 0.050(3) -0.001(3) -0.003(2) -0.003(2) C8 0.026(3) 0.033(3) 0.052(3) -0.002(3) -0.002(2) -0.001(2) C9 0.018(2) 0.038(3) 0.060(4) -0.002(3) -0.002(2) 0.001(2) C10 0.036(3) 0.041(3) 0.104(5) -0.011(4) 0.020(3) 0.000(3) C11 0.031(3) 0.042(3) 0.115(6) -0.012(4) 0.026(4) -0.003(3) C12 0.018(3) 0.034(3) 0.064(4) 0.006(3) -0.004(3) -0.001(2) C13 0.019(3) 0.035(3) 0.048(3) -0.002(3) -0.002(2) -0.003(2) C14 0.027(3) 0.045(3) 0.075(4) 0.007(4) 0.000(3) 0.001(2) C15 0.040(4) 0.058(4) 0.068(4) -0.013(3) 0.014(3) -0.016(3) C16 0.032(3) 0.058(4) 0.102(6) 0.041(4) -0.017(4) -0.017(3) C17 0.017(3) 0.042(3) 0.050(4) 0.006(3) -0.001(2) 0.001(2) C18 0.022(3) 0.043(3) 0.058(4) -0.001(3) 0.010(3) 0.002(2) C19 0.046(4) 0.045(4) 0.056(4) 0.009(3) 0.011(3) -0.004(3) C20 0.052(4) 0.041(4) 0.068(4) 0.018(3) 0.001(3) 0.002(3) C21 0.033(3) 0.041(4) 0.078(5) 0.004(3) -0.001(3) 0.004(3) C22 0.028(3) 0.044(4) 0.067(4) -0.005(3) 0.016(3) -0.001(3) C23 0.028(3) 0.061(4) 0.048(4) 0.000(3) 0.001(3) -0.009(3) C24 0.039(3) 0.071(5) 0.054(4) -0.013(3) -0.006(3) -0.005(3) C25 0.030(3) 0.050(4) 0.076(5) -0.013(3) -0.010(3) -0.005(3) C26 0.025(3) 0.046(3) 0.066(4) -0.008(3) 0.001(3) -0.003(2) C27 0.031(3) 0.036(3) 0.048(3) -0.005(3) 0.002(3) 0.002(2) N5 0.213(9) 0.405(15) 0.090(3) 0.021(7) 0.013(5) -0.061(9) O5 0.213(9) 0.405(15) 0.090(3) 0.021(7) 0.013(5) -0.061(9) C28 0.213(9) 0.405(15) 0.090(3) 0.021(7) 0.013(5) -0.061(9) C29 0.213(9) 0.405(15) 0.090(3) 0.021(7) 0.013(5) -0.061(9) C30 0.213(9) 0.405(15) 0.090(3) 0.021(7) 0.013(5) -0.061(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.979(4) . ? Co1 N1 2.081(5) . ? Co1 N3 2.117(5) . ? Co1 O3 2.172(4) 4_645 ? Co1 O4 2.177(4) 4_645 ? Co1 N4 2.193(4) . ? Co1 C17 2.514(5) 4_645 ? O2 C7 1.364(6) . ? O2 C8 1.367(6) . ? O1 C1 1.309(6) . ? O3 C17 1.270(7) . ? O3 Co1 2.172(4) 4_655 ? O4 C17 1.278(7) . ? O4 Co1 2.177(4) 4_655 ? N1 C7 1.294(7) . ? N1 N2 1.418(6) . ? N2 C8 1.271(7) . ? N3 C22 1.341(7) . ? N3 C18 1.343(7) . ? N4 C27 1.323(7) . ? N4 C23 1.340(7) . ? C1 C6 1.416(7) . ? C1 C2 1.421(7) . ? C2 C3 1.330(8) . ? C2 H2 0.9500 . ? C3 C4 1.405(8) . ? C3 H3 0.9500 . ? C4 C5 1.377(8) . ? C4 H4 0.9500 . ? C5 C6 1.410(8) . ? C5 H5 0.9500 . ? C6 C7 1.439(7) . ? C8 C9 1.491(7) . ? C9 C10 1.512(8) . ? C9 C13 1.555(8) . ? C9 H9 1.0000 . ? C10 C11 1.532(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.527(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.509(8) . ? C12 C16 1.512(9) . ? C12 C13 1.580(7) . ? C13 C15 1.518(8) . ? C13 C14 1.520(8) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Co1 2.514(5) 4_655 ? C18 C19 1.380(8) . ? C18 H18 0.9500 . ? C19 C20 1.372(9) . ? C19 H19 0.9500 . ? C20 C21 1.384(9) . ? C20 H20 0.9500 . ? C21 C22 1.367(9) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.375(8) . ? C23 H23 0.9500 . ? C24 C25 1.379(9) . ? C24 H24 0.9500 . ? C25 C26 1.370(9) . ? C25 H25 0.9500 . ? C26 C27 1.391(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? N5 C28 1.36(3) . ? N5 C30 1.47(2) . ? N5 C29 1.55(3) . ? O5 C28 1.30(2) . ? C28 H28 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 N1 87.57(16) . . ? O1 Co1 N3 102.82(17) . . ? N1 Co1 N3 90.92(18) . . ? O1 Co1 O3 165.48(16) . 4_645 ? N1 Co1 O3 95.12(17) . 4_645 ? N3 Co1 O3 91.42(16) . 4_645 ? O1 Co1 O4 104.81(16) . 4_645 ? N1 Co1 O4 93.71(17) . 4_645 ? N3 Co1 O4 152.14(16) . 4_645 ? O3 Co1 O4 60.82(15) 4_645 4_645 ? O1 Co1 N4 87.37(16) . . ? N1 Co1 N4 174.69(17) . . ? N3 Co1 N4 88.64(16) . . ? O3 Co1 N4 90.18(16) 4_645 . ? O4 Co1 N4 89.15(16) 4_645 . ? O1 Co1 C17 135.20(18) . 4_645 ? N1 Co1 C17 96.58(17) . 4_645 ? N3 Co1 C17 121.60(18) . 4_645 ? O3 Co1 C17 30.33(16) 4_645 4_645 ? O4 Co1 C17 30.56(17) 4_645 4_645 ? N4 Co1 C17 88.15(16) . 4_645 ? C7 O2 C8 103.3(4) . . ? C1 O1 Co1 132.6(3) . . ? C17 O3 Co1 89.9(3) . 4_655 ? C17 O4 Co1 89.5(3) . 4_655 ? C7 N1 N2 107.0(4) . . ? C7 N1 Co1 125.2(4) . . ? N2 N1 Co1 127.7(3) . . ? C8 N2 N1 105.8(4) . . ? C22 N3 C18 117.6(5) . . ? C22 N3 Co1 120.6(4) . . ? C18 N3 Co1 121.8(4) . . ? C27 N4 C23 117.6(5) . . ? C27 N4 Co1 122.4(4) . . ? C23 N4 Co1 119.7(4) . . ? O1 C1 C6 124.3(5) . . ? O1 C1 C2 119.9(5) . . ? C6 C1 C2 115.8(5) . . ? C3 C2 C1 123.9(5) . . ? C3 C2 H2 118.1 . . ? C1 C2 H2 118.1 . . ? C2 C3 C4 120.4(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 118.6(5) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 121.3(5) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 120.0(5) . . ? C5 C6 C7 119.3(5) . . ? C1 C6 C7 120.7(5) . . ? N1 C7 O2 111.0(4) . . ? N1 C7 C6 129.5(5) . . ? O2 C7 C6 119.5(5) . . ? N2 C8 O2 112.9(4) . . ? N2 C8 C9 128.3(5) . . ? O2 C8 C9 118.6(5) . . ? C8 C9 C10 111.7(5) . . ? C8 C9 C13 117.2(4) . . ? C10 C9 C13 105.3(5) . . ? C8 C9 H9 107.4 . . ? C10 C9 H9 107.4 . . ? C13 C9 H9 107.4 . . ? C9 C10 C11 105.7(5) . . ? C9 C10 H10A 110.6 . . ? C11 C10 H10A 110.6 . . ? C9 C10 H10B 110.6 . . ? C11 C10 H10B 110.6 . . ? H10A C10 H10B 108.7 . . ? C12 C11 C10 107.5(5) . . ? C12 C11 H11A 110.2 . . ? C10 C11 H11A 110.2 . . ? C12 C11 H11B 110.2 . . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C17 C12 C16 107.0(5) . . ? C17 C12 C11 113.6(5) . . ? C16 C12 C11 109.3(6) . . ? C17 C12 C13 112.8(4) . . ? C16 C12 C13 111.9(5) . . ? C11 C12 C13 102.3(4) . . ? C15 C13 C14 109.5(5) . . ? C15 C13 C9 111.6(5) . . ? C14 C13 C9 111.2(4) . . ? C15 C13 C12 114.0(5) . . ? C14 C13 C12 110.3(5) . . ? C9 C13 C12 100.0(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 O4 119.6(5) . . ? O3 C17 C12 119.6(5) . . ? O4 C17 C12 120.8(5) . . ? O3 C17 Co1 59.8(3) . 4_655 ? O4 C17 Co1 60.0(3) . 4_655 ? C12 C17 Co1 173.2(4) . 4_655 ? N3 C18 C19 121.9(5) . . ? N3 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C20 C19 C18 119.7(6) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 118.7(6) . . ? C19 C20 H20 120.7 . . ? C21 C20 H20 120.7 . . ? C22 C21 C20 118.4(6) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? N3 C22 C21 123.7(6) . . ? N3 C22 H22 118.2 . . ? C21 C22 H22 118.2 . . ? N4 C23 C24 122.9(6) . . ? N4 C23 H23 118.5 . . ? C24 C23 H23 118.5 . . ? C23 C24 C25 118.4(6) . . ? C23 C24 H24 120.8 . . ? C25 C24 H24 120.8 . . ? C26 C25 C24 119.8(6) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 117.6(6) . . ? C25 C26 H26 121.2 . . ? C27 C26 H26 121.2 . . ? N4 C27 C26 123.7(6) . . ? N4 C27 H27 118.1 . . ? C26 C27 H27 118.1 . . ? C28 N5 C30 122(3) . . ? C28 N5 C29 122(2) . . ? C30 N5 C29 116(2) . . ? O5 C28 N5 106(3) . . ? O5 C28 H28 127.1 . . ? N5 C28 H28 127.1 . . ? N5 C29 H29A 109.5 . . ? N5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C30 H30A 109.5 . . ? N5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 O1 C1 -2.3(5) . . . . ? N3 Co1 O1 C1 -92.7(5) . . . . ? O3 Co1 O1 C1 98.8(7) 4_645 . . . ? O4 Co1 O1 C1 90.9(5) 4_645 . . . ? N4 Co1 O1 C1 179.3(5) . . . . ? C17 Co1 O1 C1 94.6(5) 4_645 . . . ? O1 Co1 N1 C7 -0.4(5) . . . . ? N3 Co1 N1 C7 102.4(5) . . . . ? O3 Co1 N1 C7 -166.1(5) 4_645 . . . ? O4 Co1 N1 C7 -105.1(5) 4_645 . . . ? C17 Co1 N1 C7 -135.6(5) 4_645 . . . ? O1 Co1 N1 N2 -174.8(4) . . . . ? N3 Co1 N1 N2 -72.0(4) . . . . ? O3 Co1 N1 N2 19.5(4) 4_645 . . . ? O4 Co1 N1 N2 80.5(4) 4_645 . . . ? C17 Co1 N1 N2 50.0(5) 4_645 . . . ? C7 N1 N2 C8 -0.4(6) . . . . ? Co1 N1 N2 C8 174.8(4) . . . . ? O1 Co1 N3 C22 -36.3(5) . . . . ? N1 Co1 N3 C22 -124.0(4) . . . . ? O3 Co1 N3 C22 140.9(4) 4_645 . . . ? O4 Co1 N3 C22 136.3(4) 4_645 . . . ? N4 Co1 N3 C22 50.7(4) . . . . ? C17 Co1 N3 C22 137.7(4) 4_645 . . . ? O1 Co1 N3 C18 145.4(4) . . . . ? N1 Co1 N3 C18 57.6(4) . . . . ? O3 Co1 N3 C18 -37.5(4) 4_645 . . . ? O4 Co1 N3 C18 -42.1(6) 4_645 . . . ? N4 Co1 N3 C18 -127.7(4) . . . . ? C17 Co1 N3 C18 -40.7(5) 4_645 . . . ? O1 Co1 N4 C27 -13.8(4) . . . . ? N3 Co1 N4 C27 -116.7(4) . . . . ? O3 Co1 N4 C27 151.8(4) 4_645 . . . ? O4 Co1 N4 C27 91.0(4) 4_645 . . . ? C17 Co1 N4 C27 121.6(4) 4_645 . . . ? O1 Co1 N4 C23 172.5(4) . . . . ? N3 Co1 N4 C23 69.6(4) . . . . ? O3 Co1 N4 C23 -21.9(4) 4_645 . . . ? O4 Co1 N4 C23 -82.7(4) 4_645 . . . ? C17 Co1 N4 C23 -52.1(5) 4_645 . . . ? Co1 O1 C1 C6 1.4(8) . . . . ? Co1 O1 C1 C2 -179.8(4) . . . . ? O1 C1 C2 C3 -178.2(5) . . . . ? C6 C1 C2 C3 0.7(8) . . . . ? C1 C2 C3 C4 -1.5(9) . . . . ? C2 C3 C4 C5 1.3(9) . . . . ? C3 C4 C5 C6 -0.2(9) . . . . ? C4 C5 C6 C1 -0.6(9) . . . . ? C4 C5 C6 C7 176.0(5) . . . . ? O1 C1 C6 C5 179.2(5) . . . . ? C2 C1 C6 C5 0.4(8) . . . . ? O1 C1 C6 C7 2.6(8) . . . . ? C2 C1 C6 C7 -176.2(5) . . . . ? N2 N1 C7 O2 0.8(6) . . . . ? Co1 N1 C7 O2 -174.6(3) . . . . ? N2 N1 C7 C6 179.6(5) . . . . ? Co1 N1 C7 C6 4.2(8) . . . . ? C8 O2 C7 N1 -0.8(6) . . . . ? C8 O2 C7 C6 -179.8(5) . . . . ? C5 C6 C7 N1 177.7(6) . . . . ? C1 C6 C7 N1 -5.7(9) . . . . ? C5 C6 C7 O2 -3.6(8) . . . . ? C1 C6 C7 O2 173.0(5) . . . . ? N1 N2 C8 O2 -0.1(6) . . . . ? N1 N2 C8 C9 174.8(5) . . . . ? C7 O2 C8 N2 0.6(6) . . . . ? C7 O2 C8 C9 -174.9(5) . . . . ? N2 C8 C9 C10 -5.1(9) . . . . ? O2 C8 C9 C10 169.6(5) . . . . ? N2 C8 C9 C13 116.6(7) . . . . ? O2 C8 C9 C13 -68.8(7) . . . . ? C8 C9 C10 C11 152.8(6) . . . . ? C13 C9 C10 C11 24.5(7) . . . . ? C9 C10 C11 C12 2.7(7) . . . . ? C10 C11 C12 C17 -149.9(5) . . . . ? C10 C11 C12 C16 90.7(6) . . . . ? C10 C11 C12 C13 -28.0(7) . . . . ? C8 C9 C13 C15 73.2(7) . . . . ? C10 C9 C13 C15 -161.9(5) . . . . ? C8 C9 C13 C14 -49.5(7) . . . . ? C10 C9 C13 C14 75.5(6) . . . . ? C8 C9 C13 C12 -166.0(5) . . . . ? C10 C9 C13 C12 -41.0(6) . . . . ? C17 C12 C13 C15 -76.9(7) . . . . ? C16 C12 C13 C15 43.8(7) . . . . ? C11 C12 C13 C15 160.7(5) . . . . ? C17 C12 C13 C14 46.8(7) . . . . ? C16 C12 C13 C14 167.4(5) . . . . ? C11 C12 C13 C14 -75.7(6) . . . . ? C17 C12 C13 C9 164.0(5) . . . . ? C16 C12 C13 C9 -75.4(6) . . . . ? C11 C12 C13 C9 41.6(6) . . . . ? Co1 O3 C17 O4 -5.0(5) 4_655 . . . ? Co1 O3 C17 C12 172.2(4) 4_655 . . . ? Co1 O4 C17 O3 4.9(5) 4_655 . . . ? Co1 O4 C17 C12 -172.2(4) 4_655 . . . ? C16 C12 C17 O3 -60.2(7) . . . . ? C11 C12 C17 O3 179.1(5) . . . . ? C13 C12 C17 O3 63.2(7) . . . . ? C16 C12 C17 O4 116.9(6) . . . . ? C11 C12 C17 O4 -3.8(7) . . . . ? C13 C12 C17 O4 -119.7(5) . . . . ? C22 N3 C18 C19 -2.1(9) . . . . ? Co1 N3 C18 C19 176.3(4) . . . . ? N3 C18 C19 C20 0.4(10) . . . . ? C18 C19 C20 C21 2.2(10) . . . . ? C19 C20 C21 C22 -2.9(10) . . . . ? C18 N3 C22 C21 1.4(9) . . . . ? Co1 N3 C22 C21 -177.0(5) . . . . ? C20 C21 C22 N3 1.1(10) . . . . ? C27 N4 C23 C24 -0.6(9) . . . . ? Co1 N4 C23 C24 173.4(5) . . . . ? N4 C23 C24 C25 1.0(10) . . . . ? C23 C24 C25 C26 -1.3(10) . . . . ? C24 C25 C26 C27 1.2(9) . . . . ? C23 N4 C27 C26 0.4(8) . . . . ? Co1 N4 C27 C26 -173.4(4) . . . . ? C25 C26 C27 N4 -0.7(9) . . . . ? C30 N5 C28 O5 -174.5(12) . . . . ? C29 N5 C28 O5 -3(2) . . . . ? _chemical_absolute_configuration 'rmad' _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.836 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.075 #===END data_compound-2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H28 N4 Ni O4, C3 H7 N O' _chemical_formula_sum 'C30 H35 N5 Ni O5' _chemical_formula_weight 604.34 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' 'Ni' 'Ni' 0.3393 1.1124 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.1844(5) _cell_length_b 12.9184(5) _cell_length_c 18.8908(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2973.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 7808 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 25.04 _exptl_crystal_description 'Block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9146 _exptl_absorpt_correction_T_max 0.9208 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17969 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5176 _reflns_number_gt 4485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1012P)^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 -0.021(19) _refine_ls_number_reflns 5176 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Ni1 Ni 0.13372(4) 0.71863(4) 0.24227(3) 0.03390(17) Uani 1 1 d . . . O2 O 0.3815(2) 0.8329(2) 0.37099(15) 0.0401(7) Uani 1 1 d . . . O1 O 0.0492(2) 0.7708(2) 0.32528(15) 0.0391(7) Uani 1 1 d . . . O3 O 0.7738(2) 1.1244(2) 0.32539(16) 0.0387(7) Uani 1 1 d . . . O4 O 0.8118(2) 1.0712(2) 0.21857(16) 0.0394(7) Uani 1 1 d . . . N1 N 0.2699(3) 0.7847(3) 0.28698(19) 0.0390(8) Uani 1 1 d . . . N2 N 0.3742(3) 0.7993(3) 0.25593(19) 0.0416(8) Uani 1 1 d . . . N3 N 0.1124(3) 0.8416(3) 0.17365(18) 0.0365(8) Uani 1 1 d . . . N4 N -0.0117(3) 0.6474(3) 0.2045(2) 0.0402(9) Uani 1 1 d . . . C1 C 0.0825(3) 0.7849(3) 0.3889(2) 0.0352(9) Uani 1 1 d . . . C2 C 0.0064(3) 0.7880(4) 0.4460(2) 0.0423(10) Uani 1 1 d . . . H2 H -0.0692 0.7777 0.4362 0.051 Uiso 1 1 calc R . . C3 C 0.0380(4) 0.8054(4) 0.5142(2) 0.0506(12) Uani 1 1 d . . . H3 H -0.0156 0.8045 0.5508 0.061 Uiso 1 1 calc R . . C4 C 0.1447(5) 0.8238(5) 0.5308(3) 0.0589(14) Uani 1 1 d . . . H4 H 0.1653 0.8386 0.5782 0.071 Uiso 1 1 calc R . . C5 C 0.2226(4) 0.8208(4) 0.4783(3) 0.0480(12) Uani 1 1 d . . . H5 H 0.2976 0.8316 0.4901 0.058 Uiso 1 1 calc R . . C6 C 0.1938(3) 0.8026(3) 0.4088(2) 0.0367(10) Uani 1 1 d . . . C7 C 0.2775(3) 0.8041(3) 0.3531(2) 0.0361(10) Uani 1 1 d . . . C8 C 0.4356(3) 0.8265(3) 0.3080(3) 0.0395(10) Uani 1 1 d . . . C9 C 0.5571(3) 0.8459(4) 0.3064(3) 0.0465(12) Uani 1 1 d . . . H9 H 0.5900 0.8047 0.3459 0.056 Uiso 1 1 calc R . . C10 C 0.6105(4) 0.8105(4) 0.2399(4) 0.0664(16) Uani 1 1 d . . . H10A H 0.5607 0.8201 0.1991 0.080 Uiso 1 1 calc R . . H10B H 0.6305 0.7364 0.2432 0.080 Uiso 1 1 calc R . . C11 C 0.7139(4) 0.8777(4) 0.2315(4) 0.0605(15) Uani 1 1 d . . . H11A H 0.7805 0.8338 0.2307 0.073 Uiso 1 1 calc R . . H11B H 0.7106 0.9176 0.1868 0.073 Uiso 1 1 calc R . . C12 C 0.7163(3) 0.9509(3) 0.2952(3) 0.0406(10) Uani 1 1 d . . . C13 C 0.5930(3) 0.9603(3) 0.3176(2) 0.0338(9) Uani 1 1 d . . . C14 C 0.5325(4) 1.0302(3) 0.2648(3) 0.0466(11) Uani 1 1 d . . . H14A H 0.4546 1.0338 0.2776 0.070 Uiso 1 1 calc R . . H14B H 0.5398 1.0016 0.2170 0.070 Uiso 1 1 calc R . . H14C H 0.5644 1.0998 0.2662 0.070 Uiso 1 1 calc R . . C15 C 0.5757(4) 0.9966(5) 0.3917(3) 0.0617(15) Uani 1 1 d . . . H15A H 0.4970 0.9982 0.4021 0.093 Uiso 1 1 calc R . . H15B H 0.6065 1.0663 0.3971 0.093 Uiso 1 1 calc R . . H15C H 0.6125 0.9492 0.4245 0.093 Uiso 1 1 calc R . . C16 C 0.7885(4) 0.9054(4) 0.3544(3) 0.0656(17) Uani 1 1 d . . . H16A H 0.8653 0.9048 0.3390 0.098 Uiso 1 1 calc R . . H16B H 0.7648 0.8345 0.3647 0.098 Uiso 1 1 calc R . . H16C H 0.7814 0.9479 0.3971 0.098 Uiso 1 1 calc R . . C17 C 0.7692(3) 1.0558(3) 0.2777(2) 0.0351(10) Uani 1 1 d . . . C18 C 0.1923(4) 0.8668(4) 0.1292(3) 0.0484(12) Uani 1 1 d . . . H18 H 0.2587 0.8283 0.1308 0.058 Uiso 1 1 calc R . . C19 C 0.1835(5) 0.9459(4) 0.0808(3) 0.0588(14) Uani 1 1 d . . . H19 H 0.2430 0.9635 0.0506 0.071 Uiso 1 1 calc R . . C20 C 0.0836(5) 0.9994(5) 0.0776(3) 0.0589(14) Uani 1 1 d . . . H20 H 0.0732 1.0524 0.0434 0.071 Uiso 1 1 calc R . . C21 C 0.0029(4) 0.9758(4) 0.1227(3) 0.0552(14) Uani 1 1 d . . . H21 H -0.0645 1.0129 0.1221 0.066 Uiso 1 1 calc R . . C22 C 0.0200(4) 0.8963(4) 0.1701(3) 0.0445(11) Uani 1 1 d . . . H22 H -0.0375 0.8796 0.2020 0.053 Uiso 1 1 calc R . . C23 C -0.0197(4) 0.6152(4) 0.1382(3) 0.0511(12) Uani 1 1 d . . . H23 H 0.0404 0.6261 0.1071 0.061 Uiso 1 1 calc R . . C24 C -0.1130(4) 0.5661(4) 0.1126(3) 0.0642(15) Uani 1 1 d . . . H24 H -0.1161 0.5432 0.0649 0.077 Uiso 1 1 calc R . . C25 C -0.1983(4) 0.5513(4) 0.1559(3) 0.0569(14) Uani 1 1 d . . . H25 H -0.2634 0.5192 0.1390 0.068 Uiso 1 1 calc R . . C26 C -0.1907(4) 0.5823(4) 0.2226(4) 0.0578(15) Uani 1 1 d . . . H26 H -0.2502 0.5707 0.2541 0.069 Uiso 1 1 calc R . . C27 C -0.0969(3) 0.6313(3) 0.2467(3) 0.0423(10) Uani 1 1 d . . . H27 H -0.0936 0.6539 0.2945 0.051 Uiso 1 1 calc R . . C29 C 0.631(2) 0.965(2) 0.0434(10) 0.267(5) Uani 1 1 d . . . H29A H 0.6203 0.9979 -0.0029 0.401 Uiso 1 1 calc R . . H29B H 0.7023 0.9854 0.0627 0.401 Uiso 1 1 calc R . . H29C H 0.5725 0.9876 0.0757 0.401 Uiso 1 1 calc R . . C30 C 0.729(2) 0.783(2) 0.0273(9) 0.267(5) Uani 1 1 d . . . H30A H 0.7588 0.7671 0.0743 0.401 Uiso 1 1 calc R . . H30B H 0.7836 0.8226 0.0002 0.401 Uiso 1 1 calc R . . H30C H 0.7123 0.7186 0.0023 0.401 Uiso 1 1 calc R . . N5 N 0.626(2) 0.846(2) 0.0350(8) 0.267(5) Uani 1 1 d . . . C28 C 0.518(3) 0.806(3) 0.0491(11) 0.267(5) Uani 1 1 d . . . H28 H 0.5013 0.7342 0.0525 0.321 Uiso 1 1 calc R . . O5 O 0.4519(14) 0.8756(17) 0.0560(7) 0.267(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0185(3) 0.0343(3) 0.0489(3) -0.0031(2) 0.0018(2) -0.00020(19) O2 0.0218(15) 0.0446(16) 0.0540(17) 0.0080(14) -0.0068(13) -0.0053(13) O1 0.0213(13) 0.0494(17) 0.0465(17) -0.0086(15) -0.0021(12) 0.0020(13) O3 0.0313(15) 0.0380(16) 0.0469(17) 0.0007(14) 0.0000(13) -0.0012(13) O4 0.0303(16) 0.0409(16) 0.0471(18) 0.0019(14) 0.0057(13) -0.0016(13) N1 0.0175(16) 0.0416(19) 0.058(2) -0.0012(19) 0.0029(14) -0.0052(16) N2 0.0212(16) 0.0419(18) 0.062(2) -0.0099(17) 0.0079(17) -0.0023(14) N3 0.0261(18) 0.0354(18) 0.048(2) -0.0049(15) 0.0033(14) 0.0008(15) N4 0.0237(18) 0.039(2) 0.058(2) 0.0021(17) -0.0048(16) 0.0034(15) C1 0.0218(19) 0.027(2) 0.057(3) 0.003(2) 0.0013(17) 0.0015(17) C2 0.027(2) 0.051(3) 0.048(2) 0.014(2) 0.0030(17) -0.001(2) C3 0.047(3) 0.063(3) 0.041(3) 0.008(2) 0.007(2) -0.011(2) C4 0.059(3) 0.073(3) 0.045(3) 0.018(2) -0.003(2) -0.016(3) C5 0.043(3) 0.054(3) 0.047(3) 0.014(2) -0.001(2) -0.009(2) C6 0.026(2) 0.033(2) 0.051(2) 0.0122(18) -0.0029(18) -0.0051(17) C7 0.022(2) 0.034(2) 0.052(3) 0.0063(18) -0.0054(17) -0.0016(17) C8 0.0145(19) 0.038(2) 0.066(3) 0.004(2) 0.0015(19) -0.0001(16) C9 0.0152(19) 0.043(3) 0.081(3) 0.017(2) -0.0012(19) -0.0008(18) C10 0.029(2) 0.047(3) 0.123(5) -0.031(3) 0.022(3) -0.0043(19) C11 0.035(3) 0.046(3) 0.100(4) -0.015(3) 0.014(3) -0.006(2) C12 0.023(2) 0.042(2) 0.056(3) 0.005(2) 0.0009(19) -0.0048(18) C13 0.0202(19) 0.035(2) 0.046(2) 0.0019(19) -0.0017(17) 0.0001(16) C14 0.028(2) 0.034(2) 0.077(3) 0.004(2) -0.008(2) 0.0044(17) C15 0.031(3) 0.090(4) 0.064(3) -0.015(3) 0.009(2) -0.023(3) C16 0.030(3) 0.061(3) 0.106(5) 0.042(3) -0.019(3) -0.010(2) C17 0.0195(19) 0.035(2) 0.051(3) 0.0023(19) 0.0007(18) 0.0024(16) C18 0.035(2) 0.043(3) 0.067(3) 0.007(2) 0.016(2) 0.003(2) C19 0.052(3) 0.055(3) 0.070(3) 0.018(3) 0.020(3) 0.008(3) C20 0.061(3) 0.058(3) 0.058(3) 0.014(3) 0.004(3) -0.002(3) C21 0.045(3) 0.053(3) 0.068(4) 0.005(3) 0.007(2) 0.013(3) C22 0.031(2) 0.045(3) 0.058(3) 0.003(2) 0.006(2) 0.006(2) C23 0.039(3) 0.065(3) 0.050(3) -0.005(2) -0.008(2) -0.005(2) C24 0.043(3) 0.066(3) 0.084(4) -0.021(3) -0.014(3) -0.002(3) C25 0.035(3) 0.045(3) 0.092(4) -0.013(3) -0.023(3) -0.003(2) C26 0.024(2) 0.044(3) 0.105(5) 0.001(3) 0.007(3) -0.0056(19) C27 0.028(2) 0.041(2) 0.057(3) 0.003(2) 0.000(2) -0.0039(17) C29 0.301(14) 0.327(16) 0.174(5) 0.024(8) -0.027(8) 0.047(11) C30 0.301(14) 0.327(16) 0.174(5) 0.024(8) -0.027(8) 0.047(11) N5 0.301(14) 0.327(16) 0.174(5) 0.024(8) -0.027(8) 0.047(11) C28 0.301(14) 0.327(16) 0.174(5) 0.024(8) -0.027(8) 0.047(11) O5 0.301(14) 0.327(16) 0.174(5) 0.024(8) -0.027(8) 0.047(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 1.994(3) . ? Ni1 N1 2.048(3) . ? Ni1 N3 2.066(4) . ? Ni1 O3 2.093(3) 4_645 ? Ni1 N4 2.120(4) . ? Ni1 O4 2.148(3) 4_645 ? Ni1 C17 2.443(4) 4_645 ? O2 C8 1.363(6) . ? O2 C7 1.364(5) . ? O1 C1 1.282(5) . ? O3 C17 1.266(5) . ? O3 Ni1 2.093(3) 4_655 ? O4 C17 1.247(5) . ? O4 Ni1 2.148(3) 4_655 ? N1 C7 1.277(5) . ? N1 N2 1.413(4) . ? N2 C8 1.285(6) . ? N3 C18 1.326(6) . ? N3 C22 1.332(6) . ? N4 C23 1.323(6) . ? N4 C27 1.325(6) . ? C1 C2 1.422(6) . ? C1 C6 1.426(5) . ? C2 C3 1.363(7) . ? C2 H2 0.9500 . ? C3 C4 1.359(7) . ? C3 H3 0.9500 . ? C4 C5 1.373(7) . ? C4 H4 0.9500 . ? C5 C6 1.380(7) . ? C5 H5 0.9500 . ? C6 C7 1.465(6) . ? C8 C9 1.502(5) . ? C9 C10 1.486(8) . ? C9 C13 1.555(6) . ? C9 H9 1.0000 . ? C10 C11 1.538(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.531(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C17 1.537(6) . ? C12 C16 1.540(7) . ? C12 C13 1.566(6) . ? C13 C15 1.491(7) . ? C13 C14 1.533(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 Ni1 2.443(4) 4_655 ? C18 C19 1.376(7) . ? C18 H18 0.9500 . ? C19 C20 1.402(8) . ? C19 H19 0.9500 . ? C20 C21 1.337(7) . ? C20 H20 0.9500 . ? C21 C22 1.378(7) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.389(7) . ? C23 H23 0.9500 . ? C24 C25 1.335(8) . ? C24 H24 0.9500 . ? C25 C26 1.325(8) . ? C25 H25 0.9500 . ? C26 C27 1.383(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C29 N5 1.55(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N5 1.50(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? N5 C28 1.44(3) . ? C28 O5 1.22(3) . ? C28 H28 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 N1 87.32(13) . . ? O1 Ni1 N3 99.72(13) . . ? N1 Ni1 N3 92.29(14) . . ? O1 Ni1 O3 162.69(12) . 4_645 ? N1 Ni1 O3 93.34(13) . 4_645 ? N3 Ni1 O3 97.54(12) . 4_645 ? O1 Ni1 N4 88.82(13) . . ? N1 Ni1 N4 175.29(15) . . ? N3 Ni1 N4 91.02(14) . . ? O3 Ni1 N4 89.54(13) 4_645 . ? O1 Ni1 O4 100.85(12) . 4_645 ? N1 Ni1 O4 88.68(13) . 4_645 ? N3 Ni1 O4 159.43(12) . 4_645 ? O3 Ni1 O4 61.89(11) 4_645 4_645 ? N4 Ni1 O4 89.39(13) . 4_645 ? O1 Ni1 C17 131.49(14) . 4_645 ? N1 Ni1 C17 91.74(14) . 4_645 ? N3 Ni1 C17 128.76(14) . 4_645 ? O3 Ni1 C17 31.22(13) 4_645 4_645 ? N4 Ni1 C17 88.79(14) . 4_645 ? O4 Ni1 C17 30.68(13) 4_645 4_645 ? C8 O2 C7 102.5(3) . . ? C1 O1 Ni1 128.5(2) . . ? C17 O3 Ni1 89.8(2) . 4_655 ? C17 O4 Ni1 87.8(2) . 4_655 ? C7 N1 N2 108.3(3) . . ? C7 N1 Ni1 122.9(3) . . ? N2 N1 Ni1 127.8(3) . . ? C8 N2 N1 104.1(3) . . ? C18 N3 C22 117.2(4) . . ? C18 N3 Ni1 119.6(3) . . ? C22 N3 Ni1 123.1(3) . . ? C23 N4 C27 117.5(4) . . ? C23 N4 Ni1 121.1(3) . . ? C27 N4 Ni1 121.4(3) . . ? O1 C1 C2 120.6(3) . . ? O1 C1 C6 124.8(4) . . ? C2 C1 C6 114.5(4) . . ? C3 C2 C1 122.5(4) . . ? C3 C2 H2 118.7 . . ? C1 C2 H2 118.7 . . ? C4 C3 C2 121.1(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.4(5) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 121.0(5) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 121.4(4) . . ? C5 C6 C7 120.3(4) . . ? C1 C6 C7 118.4(4) . . ? N1 C7 O2 111.3(4) . . ? N1 C7 C6 130.5(4) . . ? O2 C7 C6 118.2(4) . . ? N2 C8 O2 113.8(3) . . ? N2 C8 C9 127.2(4) . . ? O2 C8 C9 119.0(4) . . ? C10 C9 C8 113.4(4) . . ? C10 C9 C13 106.5(4) . . ? C8 C9 C13 115.6(4) . . ? C10 C9 H9 106.9 . . ? C8 C9 H9 106.9 . . ? C13 C9 H9 106.9 . . ? C9 C10 C11 105.9(4) . . ? C9 C10 H10A 110.6 . . ? C11 C10 H10A 110.6 . . ? C9 C10 H10B 110.6 . . ? C11 C10 H10B 110.6 . . ? H10A C10 H10B 108.7 . . ? C12 C11 C10 106.4(4) . . ? C12 C11 H11A 110.5 . . ? C10 C11 H11A 110.5 . . ? C12 C11 H11B 110.5 . . ? C10 C11 H11B 110.5 . . ? H11A C11 H11B 108.6 . . ? C11 C12 C17 112.5(4) . . ? C11 C12 C16 110.2(4) . . ? C17 C12 C16 104.6(3) . . ? C11 C12 C13 104.0(4) . . ? C17 C12 C13 113.1(4) . . ? C16 C12 C13 112.4(4) . . ? C15 C13 C14 110.9(4) . . ? C15 C13 C9 112.8(4) . . ? C14 C13 C9 109.6(4) . . ? C15 C13 C12 114.4(4) . . ? C14 C13 C12 109.3(4) . . ? C9 C13 C12 99.1(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C17 O3 120.4(4) . . ? O4 C17 C12 120.6(4) . . ? O3 C17 C12 118.9(4) . . ? O4 C17 Ni1 61.5(2) . 4_655 ? O3 C17 Ni1 59.0(2) . 4_655 ? C12 C17 Ni1 174.8(3) . 4_655 ? N3 C18 C19 123.2(5) . . ? N3 C18 H18 118.4 . . ? C19 C18 H18 118.4 . . ? C18 C19 C20 117.5(5) . . ? C18 C19 H19 121.2 . . ? C20 C19 H19 121.2 . . ? C21 C20 C19 119.9(5) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 118.2(5) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? N3 C22 C21 123.9(4) . . ? N3 C22 H22 118.1 . . ? C21 C22 H22 118.1 . . ? N4 C23 C24 122.3(5) . . ? N4 C23 H23 118.9 . . ? C24 C23 H23 118.9 . . ? C25 C24 C23 119.3(5) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C26 C25 C24 119.0(5) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C25 C26 C27 120.6(5) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? N4 C27 C26 121.5(5) . . ? N4 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? N5 C29 H29A 109.5 . . ? N5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N5 C30 H30A 109.5 . . ? N5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 N5 C30 126(3) . . ? C28 N5 C29 112(3) . . ? C30 N5 C29 121(2) . . ? O5 C28 N5 111(4) . . ? O5 C28 H28 124.5 . . ? N5 C28 H28 124.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 O1 C1 -30.6(4) . . . . ? N3 Ni1 O1 C1 -122.4(4) . . . . ? O3 Ni1 O1 C1 62.1(6) 4_645 . . . ? N4 Ni1 O1 C1 146.7(4) . . . . ? O4 Ni1 O1 C1 57.6(4) 4_645 . . . ? C17 Ni1 O1 C1 59.4(4) 4_645 . . . ? O1 Ni1 N1 C7 22.8(4) . . . . ? N3 Ni1 N1 C7 122.5(4) . . . . ? O3 Ni1 N1 C7 -139.8(4) 4_645 . . . ? O4 Ni1 N1 C7 -78.1(4) 4_645 . . . ? C17 Ni1 N1 C7 -108.6(4) 4_645 . . . ? O1 Ni1 N1 N2 -169.2(3) . . . . ? N3 Ni1 N1 N2 -69.6(3) . . . . ? O3 Ni1 N1 N2 28.1(3) 4_645 . . . ? O4 Ni1 N1 N2 89.8(3) 4_645 . . . ? C17 Ni1 N1 N2 59.3(3) 4_645 . . . ? C7 N1 N2 C8 0.2(5) . . . . ? Ni1 N1 N2 C8 -169.2(3) . . . . ? O1 Ni1 N3 C18 146.1(3) . . . . ? N1 Ni1 N3 C18 58.4(4) . . . . ? O3 Ni1 N3 C18 -35.3(4) 4_645 . . . ? N4 Ni1 N3 C18 -124.9(4) . . . . ? O4 Ni1 N3 C18 -33.9(6) 4_645 . . . ? C17 Ni1 N3 C18 -35.7(4) 4_645 . . . ? O1 Ni1 N3 C22 -35.9(4) . . . . ? N1 Ni1 N3 C22 -123.6(4) . . . . ? O3 Ni1 N3 C22 142.7(3) 4_645 . . . ? N4 Ni1 N3 C22 53.1(4) . . . . ? O4 Ni1 N3 C22 144.1(4) 4_645 . . . ? C17 Ni1 N3 C22 142.3(3) 4_645 . . . ? O1 Ni1 N4 C23 164.1(4) . . . . ? N3 Ni1 N4 C23 64.3(4) . . . . ? O3 Ni1 N4 C23 -33.2(4) 4_645 . . . ? O4 Ni1 N4 C23 -95.1(4) 4_645 . . . ? C17 Ni1 N4 C23 -64.4(4) 4_645 . . . ? O1 Ni1 N4 C27 -17.5(3) . . . . ? N3 Ni1 N4 C27 -117.2(3) . . . . ? O3 Ni1 N4 C27 145.3(3) 4_645 . . . ? O4 Ni1 N4 C27 83.4(3) 4_645 . . . ? C17 Ni1 N4 C27 114.1(3) 4_645 . . . ? Ni1 O1 C1 C2 -158.3(3) . . . . ? Ni1 O1 C1 C6 24.4(6) . . . . ? O1 C1 C2 C3 -178.3(5) . . . . ? C6 C1 C2 C3 -0.7(7) . . . . ? C1 C2 C3 C4 2.0(8) . . . . ? C2 C3 C4 C5 -2.6(9) . . . . ? C3 C4 C5 C6 2.0(8) . . . . ? C4 C5 C6 C1 -0.8(7) . . . . ? C4 C5 C6 C7 177.4(4) . . . . ? O1 C1 C6 C5 177.6(4) . . . . ? C2 C1 C6 C5 0.1(6) . . . . ? O1 C1 C6 C7 -0.6(7) . . . . ? C2 C1 C6 C7 -178.1(4) . . . . ? N2 N1 C7 O2 0.6(5) . . . . ? Ni1 N1 C7 O2 170.6(3) . . . . ? N2 N1 C7 C6 178.7(4) . . . . ? Ni1 N1 C7 C6 -11.3(7) . . . . ? C8 O2 C7 N1 -1.1(4) . . . . ? C8 O2 C7 C6 -179.5(4) . . . . ? C5 C6 C7 N1 176.3(5) . . . . ? C1 C6 C7 N1 -5.5(7) . . . . ? C5 C6 C7 O2 -5.7(6) . . . . ? C1 C6 C7 O2 172.5(4) . . . . ? N1 N2 C8 O2 -0.9(5) . . . . ? N1 N2 C8 C9 176.0(4) . . . . ? C7 O2 C8 N2 1.3(5) . . . . ? C7 O2 C8 C9 -175.9(4) . . . . ? N2 C8 C9 C10 -11.7(7) . . . . ? O2 C8 C9 C10 165.1(4) . . . . ? N2 C8 C9 C13 111.7(5) . . . . ? O2 C8 C9 C13 -71.5(6) . . . . ? C8 C9 C10 C11 154.2(5) . . . . ? C13 C9 C10 C11 25.9(5) . . . . ? C9 C10 C11 C12 0.2(6) . . . . ? C10 C11 C12 C17 -148.5(4) . . . . ? C10 C11 C12 C16 95.1(5) . . . . ? C10 C11 C12 C13 -25.7(5) . . . . ? C10 C9 C13 C15 -162.1(4) . . . . ? C8 C9 C13 C15 70.9(5) . . . . ? C10 C9 C13 C14 73.7(5) . . . . ? C8 C9 C13 C14 -53.3(6) . . . . ? C10 C9 C13 C12 -40.7(5) . . . . ? C8 C9 C13 C12 -167.7(4) . . . . ? C11 C12 C13 C15 159.9(5) . . . . ? C17 C12 C13 C15 -77.7(5) . . . . ? C16 C12 C13 C15 40.6(6) . . . . ? C11 C12 C13 C14 -75.0(5) . . . . ? C17 C12 C13 C14 47.4(5) . . . . ? C16 C12 C13 C14 165.7(4) . . . . ? C11 C12 C13 C9 39.6(5) . . . . ? C17 C12 C13 C9 162.1(4) . . . . ? C16 C12 C13 C9 -79.7(5) . . . . ? Ni1 O4 C17 O3 1.9(4) 4_655 . . . ? Ni1 O4 C17 C12 -174.5(3) 4_655 . . . ? Ni1 O3 C17 O4 -2.0(4) 4_655 . . . ? Ni1 O3 C17 C12 174.5(3) 4_655 . . . ? C11 C12 C17 O4 -5.2(6) . . . . ? C16 C12 C17 O4 114.5(5) . . . . ? C13 C12 C17 O4 -122.8(4) . . . . ? C11 C12 C17 O3 178.3(4) . . . . ? C16 C12 C17 O3 -62.0(5) . . . . ? C13 C12 C17 O3 60.7(5) . . . . ? C22 N3 C18 C19 0.3(7) . . . . ? Ni1 N3 C18 C19 178.4(4) . . . . ? N3 C18 C19 C20 -2.0(8) . . . . ? C18 C19 C20 C21 2.9(9) . . . . ? C19 C20 C21 C22 -1.9(9) . . . . ? C18 N3 C22 C21 0.7(7) . . . . ? Ni1 N3 C22 C21 -177.3(4) . . . . ? C20 C21 C22 N3 0.1(8) . . . . ? C27 N4 C23 C24 -0.1(7) . . . . ? Ni1 N4 C23 C24 178.4(4) . . . . ? N4 C23 C24 C25 0.6(9) . . . . ? C23 C24 C25 C26 -1.3(8) . . . . ? C24 C25 C26 C27 1.5(8) . . . . ? C23 N4 C27 C26 0.3(6) . . . . ? Ni1 N4 C27 C26 -178.2(3) . . . . ? C25 C26 C27 N4 -1.0(8) . . . . ? C30 N5 C28 O5 176.7(15) . . . . ? C29 N5 C28 O5 8(3) . . . . ? _chemical_absolute_configuration 'rmad' _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.838 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.071 #===END data_compound-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H23 Cu N3 O4' _chemical_formula_sum 'C22 H23 Cu N3 O4' _chemical_formula_weight 456.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.4795(6) _cell_length_b 11.4662(9) _cell_length_c 23.901(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.773(2) _cell_angle_gamma 90.00 _cell_volume 2025.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 3284 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 23.49 _exptl_crystal_description 'block' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 1.113 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9262 _exptl_absorpt_correction_T_max 0.9362 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12319 _diffrn_reflns_av_R_equivalents 0.1010 _diffrn_reflns_av_sigmaI/netI 0.1758 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.86 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6568 _reflns_number_gt 3563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+0.9026P] 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 -0.01(3) _refine_ls_number_reflns 6568 _refine_ls_number_parameters 541 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1490 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.11144(16) 0.42469(11) 0.83089(5) 0.0349(4) Uani 1 1 d . . . Cu2 Cu 0.42026(16) 0.97719(10) 0.66159(5) 0.0333(4) Uani 1 1 d . . . O1 O 0.1480(10) 0.4549(8) 0.7557(3) 0.043(3) Uani 1 1 d . . . O2 O 0.5906(10) 0.6039(8) 0.8585(3) 0.036(2) Uani 1 1 d . . . O3 O 0.9128(9) 0.8668(8) 1.0926(3) 0.037(2) Uani 1 1 d . . . O4 O 0.7944(10) 0.7209(8) 1.1354(3) 0.044(2) Uani 1 1 d . . . O5 O 0.3893(9) 0.9435(8) 0.7377(3) 0.045(3) Uani 1 1 d . . . O6 O -0.0638(10) 0.8025(8) 0.6354(3) 0.038(2) Uani 1 1 d . . . O7 O -0.4370(9) 0.5423(8) 0.4149(3) 0.034(2) Uani 1 1 d . . . O8 O -0.3282(10) 0.6744(8) 0.3628(3) 0.036(2) Uani 1 1 d . . . N1 N 0.3411(11) 0.5062(8) 0.8588(3) 0.029(3) Uani 1 1 d . . . N2 N 0.4332(13) 0.5065(10) 0.9148(4) 0.043(3) Uani 1 1 d . . . N3 N 0.1938(11) 0.8951(9) 0.6346(4) 0.034(3) Uani 1 1 d . . . N4 N 0.0992(11) 0.8966(9) 0.5794(3) 0.031(3) Uani 1 1 d . . . N5 N -0.1485(11) 0.3791(9) 0.8017(4) 0.033(3) Uani 1 1 d . . . N6 N 0.6801(11) 1.0255(9) 0.6909(4) 0.034(3) Uani 1 1 d . . . C1 C 0.2607(14) 0.5219(11) 0.7348(4) 0.037(3) Uani 1 1 d . . . C2 C 0.2392(17) 0.5394(12) 0.6755(5) 0.048(4) Uani 1 1 d . . . H2A H 0.1417 0.5038 0.6514 0.058 Uiso 1 1 calc R . . C3 C 0.3617(18) 0.6089(13) 0.6531(5) 0.050(4) Uani 1 1 d . . . H3A H 0.3476 0.6173 0.6132 0.060 Uiso 1 1 calc R . . C4 C 0.5031(18) 0.6667(14) 0.6853(6) 0.053(4) Uani 1 1 d . . . H4A H 0.5815 0.7161 0.6683 0.063 Uiso 1 1 calc R . . C5 C 0.5259(16) 0.6502(13) 0.7423(5) 0.043(4) Uani 1 1 d . . . H5A H 0.6225 0.6885 0.7656 0.052 Uiso 1 1 calc R . . C6 C 0.4105(15) 0.5782(11) 0.7674(5) 0.033(3) Uani 1 1 d . . . C7 C 0.4424(15) 0.5615(11) 0.8266(4) 0.032(3) Uani 1 1 d . . . C8 C 0.5781(17) 0.5666(13) 0.9130(5) 0.037(3) Uani 1 1 d . . . C9 C 0.7336(15) 0.5913(13) 0.9583(5) 0.042(4) Uani 1 1 d . . . H9A H 0.7927 0.5142 0.9682 0.051 Uiso 1 1 calc R . . C10 C 0.8770(15) 0.6678(12) 0.9440(4) 0.071(4) Uani 1 1 d . . . H10A H 0.8284 0.7199 0.9122 0.086 Uiso 1 1 calc R . . H10B H 0.9760 0.6207 0.9324 0.086 Uiso 1 1 calc R . . C11 C 0.5542(16) 0.7394(13) 1.0022(6) 0.063(4) Uani 1 1 d . . . H11A H 0.4351 0.7106 0.9850 0.094 Uiso 1 1 calc R . . H11B H 0.6006 0.7934 0.9760 0.094 Uiso 1 1 calc R . . H11C H 0.5434 0.7800 1.0376 0.094 Uiso 1 1 calc R . . C12 C 0.5967(17) 0.5443(10) 1.0462(4) 0.069(4) Uani 1 1 d . . . H12A H 0.4779 0.5234 1.0254 0.103 Uiso 1 1 calc R . . H12B H 0.5825 0.5730 1.0839 0.103 Uiso 1 1 calc R . . H12C H 0.6752 0.4755 1.0500 0.103 Uiso 1 1 calc R . . C13 C 0.6812(13) 0.6393(10) 1.0142(4) 0.033(3) Uani 1 1 d . . . C14 C 0.8685(15) 0.6857(13) 1.0437(5) 0.039(3) Uani 1 1 d . . . C15 C 0.9498(15) 0.7416(13) 0.9978(5) 0.069(4) Uani 1 1 d . . . H15A H 1.0835 0.7388 1.0059 0.083 Uiso 1 1 calc R . . H15B H 0.9109 0.8240 0.9927 0.083 Uiso 1 1 calc R . . C16 C 0.9927(16) 0.5776(12) 1.0669(5) 0.079(5) Uani 1 1 d . . . H16A H 1.1122 0.6059 1.0841 0.118 Uiso 1 1 calc R . . H16B H 1.0059 0.5249 1.0355 0.118 Uiso 1 1 calc R . . H16C H 0.9363 0.5356 1.0954 0.118 Uiso 1 1 calc R . . C17 C 0.8551(15) 0.7632(14) 1.0944(5) 0.035(3) Uani 1 1 d . . . C18 C 0.2742(15) 0.8773(11) 0.7590(5) 0.034(3) Uani 1 1 d . . . C19 C 0.2943(15) 0.8611(11) 0.8190(5) 0.042(3) Uani 1 1 d . . . H19A H 0.3909 0.8990 0.8424 0.051 Uiso 1 1 calc R . . C20 C 0.1799(16) 0.7935(13) 0.8431(5) 0.044(4) Uani 1 1 d . . . H20A H 0.1984 0.7841 0.8831 0.053 Uiso 1 1 calc R . . C21 C 0.0362(17) 0.7377(13) 0.8108(4) 0.048(4) Uani 1 1 d . . . H21A H -0.0436 0.6904 0.8283 0.057 Uiso 1 1 calc R . . C22 C 0.0103(15) 0.7512(11) 0.7539(6) 0.043(4) Uani 1 1 d . . . H22A H -0.0896 0.7135 0.7319 0.052 Uiso 1 1 calc R . . C23 C 0.1265(14) 0.8192(11) 0.7264(4) 0.029(3) Uani 1 1 d . . . C24 C 0.0958(14) 0.8400(10) 0.6665(4) 0.025(3) Uani 1 1 d . . . C25 C -0.0508(16) 0.8445(11) 0.5821(5) 0.031(3) Uani 1 1 d . . . C26 C -0.2115(15) 0.8263(12) 0.5387(5) 0.033(3) Uani 1 1 d . . . H26A H -0.3200 0.8318 0.5584 0.040 Uiso 1 1 calc R . . C27 C -0.2367(14) 0.9155(9) 0.4914(4) 0.049(3) Uani 1 1 d . . . H27A H -0.3061 0.9832 0.5022 0.059 Uiso 1 1 calc R . . H27B H -0.1176 0.9435 0.4837 0.059 Uiso 1 1 calc R . . C28 C -0.2238(13) 0.7059(10) 0.5067(4) 0.030(3) Uani 1 1 d . . . C29 C -0.0466(12) 0.6836(12) 0.4839(5) 0.038(3) Uani 1 1 d . . . H29A H -0.0213 0.7492 0.4600 0.056 Uiso 1 1 calc R . . H29B H -0.0573 0.6117 0.4614 0.056 Uiso 1 1 calc R . . H29C H 0.0523 0.6755 0.5156 0.056 Uiso 1 1 calc R . . C30 C -0.2597(14) 0.6027(9) 0.5445(4) 0.051(3) Uani 1 1 d . . . H30A H -0.1560 0.5924 0.5745 0.076 Uiso 1 1 calc R . . H30B H -0.2776 0.5316 0.5216 0.076 Uiso 1 1 calc R . . H30C H -0.3685 0.6184 0.5615 0.076 Uiso 1 1 calc R . . C31 C -0.3379(14) 0.8571(9) 0.4396(4) 0.044(3) Uani 1 1 d . . . H31A H -0.2627 0.8552 0.4090 0.052 Uiso 1 1 calc R . . H31B H -0.4508 0.9002 0.4259 0.052 Uiso 1 1 calc R . . C32 C -0.5680(13) 0.7320(10) 0.4744(5) 0.050(3) Uani 1 1 d . . . H32A H -0.6598 0.7496 0.4417 0.076 Uiso 1 1 calc R . . H32B H -0.5740 0.7902 0.5041 0.076 Uiso 1 1 calc R . . H32C H -0.5904 0.6543 0.4889 0.076 Uiso 1 1 calc R . . C33 C -0.3810(14) 0.7349(11) 0.4565(5) 0.027(3) Uani 1 1 d . . . C34 C -0.3767(14) 0.6444(11) 0.4078(5) 0.024(3) Uani 1 1 d . . . C35 C -0.2596(15) 0.3333(13) 0.8351(5) 0.044(4) Uani 1 1 d . . . H35A H -0.2199 0.3329 0.8747 0.053 Uiso 1 1 calc R . . C36 C -0.4220(18) 0.2886(14) 0.8161(6) 0.049(4) Uani 1 1 d . . . H36A H -0.4946 0.2576 0.8418 0.058 Uiso 1 1 calc R . . C37 C -0.4817(18) 0.2878(14) 0.7604(8) 0.069(5) Uani 1 1 d . . . H37A H -0.5975 0.2568 0.7461 0.083 Uiso 1 1 calc R . . C38 C -0.3724(17) 0.3327(14) 0.7241(5) 0.056(4) Uani 1 1 d . . . H38A H -0.4094 0.3313 0.6843 0.067 Uiso 1 1 calc R . . C39 C -0.2113(15) 0.3787(12) 0.7467(5) 0.044(4) Uani 1 1 d . . . H39A H -0.1386 0.4127 0.7217 0.053 Uiso 1 1 calc R . . C40 C 0.7455(14) 1.0238(11) 0.7473(4) 0.035(3) Uani 1 1 d . . . H40A H 0.6750 0.9886 0.7726 0.042 Uiso 1 1 calc R . . C41 C 0.9104(15) 1.0716(14) 0.7689(6) 0.049(4) Uani 1 1 d . . . H41A H 0.9518 1.0691 0.8084 0.059 Uiso 1 1 calc R . . C42 C 1.0118(16) 1.1210(13) 0.7346(5) 0.043(4) Uani 1 1 d . . . H42A H 1.1233 1.1568 0.7496 0.051 Uiso 1 1 calc R . . C43 C 0.9547(18) 1.1200(15) 0.6776(6) 0.057(4) Uani 1 1 d U . . H43A H 1.0264 1.1537 0.6523 0.068 Uiso 1 1 calc R . . C44 C 0.7862(16) 1.0675(12) 0.6572(5) 0.044(4) Uani 1 1 d . . . H44A H 0.7488 1.0627 0.6174 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0381(8) 0.0353(10) 0.0293(8) 0.0003(7) -0.0016(7) -0.0047(7) Cu2 0.0359(7) 0.0360(10) 0.0260(7) 0.0043(7) -0.0014(6) -0.0063(7) O1 0.048(4) 0.050(8) 0.030(4) 0.000(4) 0.004(4) -0.030(5) O2 0.045(5) 0.040(6) 0.020(4) -0.004(4) -0.006(4) -0.004(4) O3 0.038(5) 0.037(6) 0.033(4) 0.001(4) -0.008(4) -0.001(4) O4 0.046(5) 0.049(7) 0.033(5) -0.006(5) -0.003(4) -0.001(5) O5 0.047(4) 0.062(8) 0.023(4) 0.001(4) -0.004(4) -0.019(5) O6 0.037(5) 0.038(6) 0.038(5) 0.001(5) -0.002(4) -0.019(4) O7 0.030(4) 0.040(6) 0.034(4) -0.004(4) 0.012(4) 0.004(4) O8 0.033(4) 0.040(6) 0.036(5) 0.001(4) 0.007(4) -0.003(4) N1 0.039(5) 0.027(7) 0.021(5) 0.005(5) 0.004(4) -0.008(5) N2 0.053(6) 0.047(9) 0.028(5) -0.007(5) 0.003(5) -0.014(6) N3 0.040(5) 0.029(7) 0.032(5) 0.002(5) 0.005(5) -0.005(5) N4 0.034(5) 0.039(8) 0.018(5) 0.009(5) -0.006(4) -0.009(5) N5 0.034(5) 0.032(7) 0.031(5) -0.003(5) 0.003(5) 0.002(5) N6 0.022(5) 0.046(8) 0.033(5) -0.002(5) 0.004(5) 0.002(5) C1 0.035(7) 0.044(9) 0.026(6) 0.000(6) -0.010(6) 0.000(6) C2 0.053(8) 0.063(11) 0.026(7) -0.010(7) -0.001(7) 0.009(7) C3 0.060(9) 0.069(12) 0.026(7) 0.008(8) 0.022(7) 0.004(8) C4 0.045(8) 0.063(12) 0.051(9) -0.004(8) 0.011(7) -0.009(8) C5 0.039(7) 0.075(12) 0.016(6) 0.016(6) 0.003(6) 0.003(7) C6 0.039(7) 0.032(8) 0.028(7) 0.001(6) 0.011(6) -0.004(6) C7 0.037(7) 0.044(9) 0.011(6) -0.001(6) -0.005(5) -0.014(6) C8 0.045(8) 0.049(10) 0.015(6) -0.002(6) 0.001(6) -0.004(7) C9 0.034(7) 0.059(11) 0.033(7) -0.023(7) 0.001(6) 0.003(7) C10 0.052(8) 0.126(13) 0.039(7) -0.034(8) 0.017(6) -0.032(8) C11 0.055(9) 0.056(11) 0.073(9) -0.025(8) 0.000(8) 0.007(8) C12 0.100(10) 0.071(10) 0.035(7) -0.001(6) 0.012(7) -0.048(8) C13 0.030(6) 0.044(8) 0.025(6) -0.007(6) 0.007(5) -0.001(6) C14 0.031(7) 0.048(10) 0.038(7) -0.019(7) 0.002(6) -0.009(6) C15 0.054(9) 0.122(13) 0.035(7) -0.033(8) 0.021(7) -0.038(8) C16 0.061(9) 0.103(13) 0.064(9) -0.041(9) -0.021(7) 0.041(8) C17 0.025(6) 0.050(11) 0.026(7) -0.013(7) -0.003(6) 0.006(7) C18 0.041(7) 0.027(8) 0.035(7) 0.000(6) 0.015(6) -0.001(6) C19 0.046(7) 0.045(10) 0.033(7) 0.006(6) -0.002(6) -0.010(7) C20 0.036(7) 0.063(12) 0.033(7) -0.009(8) 0.002(6) -0.009(7) C21 0.057(8) 0.074(12) 0.011(6) 0.016(7) 0.002(6) -0.014(8) C22 0.033(7) 0.027(8) 0.067(10) -0.017(7) -0.001(7) -0.014(6) C23 0.029(6) 0.034(8) 0.023(6) 0.002(6) 0.001(5) 0.000(6) C24 0.033(6) 0.016(7) 0.026(6) -0.001(6) 0.007(6) 0.005(5) C25 0.039(7) 0.028(9) 0.024(6) -0.005(6) -0.003(6) 0.010(6) C26 0.032(6) 0.037(9) 0.029(6) -0.008(6) -0.001(6) 0.001(6) C27 0.060(7) 0.022(6) 0.056(7) -0.007(6) -0.021(6) 0.008(6) C28 0.020(6) 0.050(8) 0.020(6) -0.009(5) 0.005(5) 0.006(5) C29 0.020(6) 0.045(9) 0.042(7) -0.009(6) -0.012(5) 0.003(6) C30 0.067(8) 0.045(8) 0.034(6) 0.017(6) -0.009(6) -0.019(6) C31 0.045(7) 0.047(8) 0.038(6) -0.001(6) 0.002(6) 0.003(6) C32 0.036(7) 0.051(8) 0.063(8) -0.012(7) 0.002(6) 0.010(6) C33 0.026(6) 0.029(8) 0.026(6) 0.005(6) 0.006(5) 0.008(5) C34 0.020(6) 0.022(8) 0.029(7) -0.001(6) -0.003(5) 0.002(5) C35 0.030(7) 0.066(12) 0.035(8) -0.018(8) -0.002(7) 0.004(7) C36 0.047(9) 0.050(10) 0.046(8) 0.018(8) 0.002(7) -0.002(7) C37 0.029(8) 0.050(12) 0.133(16) -0.022(12) 0.027(10) -0.003(7) C38 0.043(8) 0.071(12) 0.047(8) -0.014(8) -0.016(7) -0.001(8) C39 0.033(7) 0.047(10) 0.053(9) 0.010(7) 0.006(7) -0.001(6) C40 0.033(6) 0.048(10) 0.023(6) -0.002(6) 0.000(6) 0.002(6) C41 0.023(7) 0.062(11) 0.057(9) -0.016(8) -0.007(7) 0.006(7) C42 0.027(7) 0.050(10) 0.044(8) -0.005(7) -0.017(6) 0.005(6) C43 0.036(6) 0.062(8) 0.074(8) -0.004(7) 0.016(6) -0.005(6) C44 0.037(8) 0.054(11) 0.042(8) 0.004(7) 0.006(7) 0.016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.891(7) . ? Cu1 O3 1.979(7) 2_647 ? Cu1 N1 1.980(9) . ? Cu1 N5 2.032(9) . ? Cu1 O4 2.537(9) 2_647 ? Cu2 O5 1.909(7) . ? Cu2 N3 1.959(9) . ? Cu2 O7 1.996(7) 2_556 ? Cu2 N6 2.039(9) . ? Cu2 O8 2.409(9) 2_556 ? Cu2 C34 2.524(12) 2_556 ? O1 C1 1.295(12) . ? O2 C7 1.338(12) . ? O2 C8 1.387(12) . ? O3 C17 1.267(15) . ? O3 Cu1 1.979(7) 2_657 ? O4 C17 1.239(13) . ? O4 Cu1 2.537(9) 2_657 ? O5 C18 1.308(12) . ? O6 C24 1.375(12) . ? O6 C25 1.380(12) . ? O7 C34 1.275(13) . ? O7 Cu2 1.996(7) 2_546 ? O8 C34 1.235(12) . ? O8 Cu2 2.409(9) 2_546 ? N1 C7 1.322(12) . ? N1 N2 1.410(11) . ? N2 C8 1.291(15) . ? N3 C24 1.299(12) . ? N3 N4 1.398(11) . ? N4 C25 1.281(13) . ? N5 C39 1.327(13) . ? N5 C35 1.343(13) . ? N6 C44 1.306(13) . ? N6 C40 1.363(12) . ? C1 C2 1.416(14) . ? C1 C6 1.419(15) . ? C2 C3 1.381(17) . ? C2 H2A 0.9500 . ? C3 C4 1.379(17) . ? C3 H3A 0.9500 . ? C4 C5 1.361(16) . ? C4 H4A 0.9500 . ? C5 C6 1.393(16) . ? C5 H5A 0.9500 . ? C6 C7 1.412(14) . ? C8 C9 1.492(15) . ? C9 C10 1.466(16) . ? C9 C13 1.549(13) . ? C9 H9A 1.0000 . ? C10 C15 1.566(14) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C13 1.489(16) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.523(14) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.562(14) . ? C14 C15 1.479(16) . ? C14 C17 1.520(16) . ? C14 C16 1.597(17) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C18 C23 1.417(15) . ? C18 C19 1.430(14) . ? C19 C20 1.348(15) . ? C19 H19A 0.9500 . ? C20 C21 1.382(16) . ? C20 H20A 0.9500 . ? C21 C22 1.352(16) . ? C21 H21A 0.9500 . ? C22 C23 1.403(16) . ? C22 H22A 0.9500 . ? C23 C24 1.435(13) . ? C25 C26 1.478(14) . ? C26 C27 1.514(15) . ? C26 C28 1.575(16) . ? C26 H26A 1.0000 . ? C27 C31 1.506(12) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.529(13) . ? C28 C30 1.537(13) . ? C28 C33 1.582(14) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.506(15) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.524(13) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.564(16) . ? C34 Cu2 2.524(12) 2_546 ? C35 C36 1.333(16) . ? C35 H35A 0.9500 . ? C36 C37 1.337(19) . ? C36 H36A 0.9500 . ? C37 C38 1.380(18) . ? C37 H37A 0.9500 . ? C38 C39 1.350(15) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C41 1.375(15) . ? C40 H40A 0.9500 . ? C41 C42 1.325(16) . ? C41 H41A 0.9500 . ? C42 C43 1.365(17) . ? C42 H42A 0.9500 . ? C43 C44 1.415(17) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 O3 170.5(4) . 2_647 ? O1 Cu1 N1 89.4(3) . . ? O3 Cu1 N1 92.5(3) 2_647 . ? O1 Cu1 N5 89.4(3) . . ? O3 Cu1 N5 90.8(3) 2_647 . ? N1 Cu1 N5 166.7(4) . . ? O1 Cu1 O4 113.4(3) . 2_647 ? O3 Cu1 O4 57.1(3) 2_647 2_647 ? N1 Cu1 O4 98.2(3) . 2_647 ? N5 Cu1 O4 94.4(3) . 2_647 ? O5 Cu2 N3 89.6(3) . . ? O5 Cu2 O7 169.2(4) . 2_556 ? N3 Cu2 O7 92.9(3) . 2_556 ? O5 Cu2 N6 88.6(3) . . ? N3 Cu2 N6 167.0(4) . . ? O7 Cu2 N6 91.3(3) 2_556 . ? O5 Cu2 O8 110.4(3) . 2_556 ? N3 Cu2 O8 99.8(3) . 2_556 ? O7 Cu2 O8 58.9(3) 2_556 2_556 ? N6 Cu2 O8 92.9(3) . 2_556 ? O5 Cu2 C34 139.3(4) . 2_556 ? N3 Cu2 C34 97.5(4) . 2_556 ? O7 Cu2 C34 30.0(3) 2_556 2_556 ? N6 Cu2 C34 92.3(4) . 2_556 ? O8 Cu2 C34 28.9(3) 2_556 2_556 ? C1 O1 Cu1 132.2(7) . . ? C7 O2 C8 104.7(9) . . ? C17 O3 Cu1 101.7(7) . 2_657 ? C17 O4 Cu1 76.8(8) . 2_657 ? C18 O5 Cu2 132.1(7) . . ? C24 O6 C25 102.3(9) . . ? C34 O7 Cu2 98.6(7) . 2_546 ? C34 O8 Cu2 80.7(7) . 2_546 ? C7 N1 N2 108.1(8) . . ? C7 N1 Cu1 125.1(7) . . ? N2 N1 Cu1 126.5(7) . . ? C8 N2 N1 105.1(9) . . ? C24 N3 N4 108.1(8) . . ? C24 N3 Cu2 125.2(7) . . ? N4 N3 Cu2 126.3(7) . . ? C25 N4 N3 105.6(8) . . ? C39 N5 C35 115.5(10) . . ? C39 N5 Cu1 121.1(8) . . ? C35 N5 Cu1 122.9(8) . . ? C44 N6 C40 117.1(10) . . ? C44 N6 Cu2 121.7(8) . . ? C40 N6 Cu2 121.0(7) . . ? O1 C1 C2 119.2(11) . . ? O1 C1 C6 124.4(10) . . ? C2 C1 C6 116.4(11) . . ? C3 C2 C1 119.3(12) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C4 C3 C2 124.0(12) . . ? C4 C3 H3A 118.0 . . ? C2 C3 H3A 118.0 . . ? C5 C4 C3 117.4(13) . . ? C5 C4 H4A 121.3 . . ? C3 C4 H4A 121.3 . . ? C4 C5 C6 121.4(13) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C5 C6 C7 119.3(11) . . ? C5 C6 C1 121.5(11) . . ? C7 C6 C1 119.1(10) . . ? N1 C7 O2 110.0(9) . . ? N1 C7 C6 128.6(11) . . ? O2 C7 C6 121.4(10) . . ? N2 C8 O2 112.0(11) . . ? N2 C8 C9 129.9(11) . . ? O2 C8 C9 117.9(10) . . ? C10 C9 C8 117.4(11) . . ? C10 C9 C13 106.2(10) . . ? C8 C9 C13 115.0(9) . . ? C10 C9 H9A 105.8 . . ? C8 C9 H9A 105.8 . . ? C13 C9 H9A 105.8 . . ? C9 C10 C15 107.8(9) . . ? C9 C10 H10A 110.1 . . ? C15 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? C15 C10 H10B 110.1 . . ? H10A C10 H10B 108.5 . . ? C13 C11 H11A 109.5 . . ? C13 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C13 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 C12 110.3(10) . . ? C11 C13 C9 110.2(10) . . ? C12 C13 C9 111.0(10) . . ? C11 C13 C14 109.1(10) . . ? C12 C13 C14 115.4(9) . . ? C9 C13 C14 100.5(8) . . ? C15 C14 C17 115.0(12) . . ? C15 C14 C13 104.8(9) . . ? C17 C14 C13 113.3(9) . . ? C15 C14 C16 108.1(10) . . ? C17 C14 C16 106.4(10) . . ? C13 C14 C16 109.1(11) . . ? C14 C15 C10 104.1(10) . . ? C14 C15 H15A 110.9 . . ? C10 C15 H15A 110.9 . . ? C14 C15 H15B 110.9 . . ? C10 C15 H15B 110.9 . . ? H15A C15 H15B 109.0 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C17 O3 124.2(11) . . ? O4 C17 C14 118.5(13) . . ? O3 C17 C14 117.2(11) . . ? O5 C18 C23 124.3(10) . . ? O5 C18 C19 119.4(11) . . ? C23 C18 C19 116.3(10) . . ? C20 C19 C18 121.8(12) . . ? C20 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? C19 C20 C21 121.1(12) . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? C22 C21 C20 119.3(12) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C21 C22 C23 122.0(12) . . ? C21 C22 H22A 119.0 . . ? C23 C22 H22A 119.0 . . ? C22 C23 C18 119.4(10) . . ? C22 C23 C24 122.9(11) . . ? C18 C23 C24 117.5(11) . . ? N3 C24 O6 110.8(9) . . ? N3 C24 C23 130.4(11) . . ? O6 C24 C23 118.7(10) . . ? N4 C25 O6 113.2(10) . . ? N4 C25 C26 131.0(10) . . ? O6 C25 C26 115.8(10) . . ? C25 C26 C27 115.1(10) . . ? C25 C26 C28 116.4(10) . . ? C27 C26 C28 103.8(8) . . ? C25 C26 H26A 107.0 . . ? C27 C26 H26A 107.0 . . ? C28 C26 H26A 107.0 . . ? C31 C27 C26 107.6(9) . . ? C31 C27 H27A 110.2 . . ? C26 C27 H27A 110.2 . . ? C31 C27 H27B 110.2 . . ? C26 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? C29 C28 C30 108.6(10) . . ? C29 C28 C26 109.3(9) . . ? C30 C28 C26 113.1(8) . . ? C29 C28 C33 110.5(8) . . ? C30 C28 C33 115.5(8) . . ? C26 C28 C33 99.5(9) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C31 C33 107.1(9) . . ? C27 C31 H31A 110.3 . . ? C33 C31 H31A 110.3 . . ? C27 C31 H31B 110.3 . . ? C33 C31 H31B 110.3 . . ? H31A C31 H31B 108.5 . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 C32 109.8(9) . . ? C31 C33 C34 112.8(9) . . ? C32 C33 C34 108.6(10) . . ? C31 C33 C28 103.5(9) . . ? C32 C33 C28 113.0(8) . . ? C34 C33 C28 109.1(9) . . ? O8 C34 O7 121.9(11) . . ? O8 C34 C33 120.4(11) . . ? O7 C34 C33 117.5(10) . . ? O8 C34 Cu2 70.4(6) . 2_546 ? O7 C34 Cu2 51.5(6) . 2_546 ? C33 C34 Cu2 168.1(8) . 2_546 ? C36 C35 N5 124.2(11) . . ? C36 C35 H35A 117.9 . . ? N5 C35 H35A 117.9 . . ? C35 C36 C37 119.4(13) . . ? C35 C36 H36A 120.3 . . ? C37 C36 H36A 120.3 . . ? C36 C37 C38 118.9(14) . . ? C36 C37 H37A 120.6 . . ? C38 C37 H37A 120.6 . . ? C39 C38 C37 118.3(13) . . ? C39 C38 H38A 120.9 . . ? C37 C38 H38A 120.9 . . ? N5 C39 C38 123.8(12) . . ? N5 C39 H39A 118.1 . . ? C38 C39 H39A 118.1 . . ? N6 C40 C41 122.1(11) . . ? N6 C40 H40A 119.0 . . ? C41 C40 H40A 119.0 . . ? C42 C41 C40 120.2(13) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C41 C42 C43 119.5(13) . . ? C41 C42 H42A 120.3 . . ? C43 C42 H42A 120.3 . . ? C42 C43 C44 118.3(13) . . ? C42 C43 H43A 120.8 . . ? C44 C43 H43A 120.8 . . ? N6 C44 C43 122.5(12) . . ? N6 C44 H44A 118.7 . . ? C43 C44 H44A 118.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cu1 O1 C1 -114(2) 2_647 . . . ? N1 Cu1 O1 C1 -11.7(10) . . . . ? N5 Cu1 O1 C1 155.1(11) . . . . ? O4 Cu1 O1 C1 -110.4(10) 2_647 . . . ? N3 Cu2 O5 C18 8.5(11) . . . . ? O7 Cu2 O5 C18 111.7(19) 2_556 . . . ? N6 Cu2 O5 C18 -158.6(11) . . . . ? O8 Cu2 O5 C18 108.8(10) 2_556 . . . ? C34 Cu2 O5 C18 109.5(11) 2_556 . . . ? O1 Cu1 N1 C7 5.2(10) . . . . ? O3 Cu1 N1 C7 175.9(10) 2_647 . . . ? N5 Cu1 N1 C7 -79.9(18) . . . . ? O4 Cu1 N1 C7 118.7(9) 2_647 . . . ? O1 Cu1 N1 N2 -168.6(9) . . . . ? O3 Cu1 N1 N2 2.1(9) 2_647 . . . ? N5 Cu1 N1 N2 106.3(17) . . . . ? O4 Cu1 N1 N2 -55.0(9) 2_647 . . . ? C7 N1 N2 C8 3.1(14) . . . . ? Cu1 N1 N2 C8 177.7(8) . . . . ? O5 Cu2 N3 C24 -3.9(9) . . . . ? O7 Cu2 N3 C24 -173.4(9) 2_556 . . . ? N6 Cu2 N3 C24 78.0(19) . . . . ? O8 Cu2 N3 C24 -114.5(9) 2_556 . . . ? C34 Cu2 N3 C24 -143.6(9) 2_556 . . . ? O5 Cu2 N3 N4 168.2(9) . . . . ? O7 Cu2 N3 N4 -1.3(9) 2_556 . . . ? N6 Cu2 N3 N4 -110.0(17) . . . . ? O8 Cu2 N3 N4 57.6(9) 2_556 . . . ? C34 Cu2 N3 N4 28.4(9) 2_556 . . . ? C24 N3 N4 C25 1.2(12) . . . . ? Cu2 N3 N4 C25 -171.9(8) . . . . ? O1 Cu1 N5 C39 2.1(10) . . . . ? O3 Cu1 N5 C39 -168.5(10) 2_647 . . . ? N1 Cu1 N5 C39 87.1(17) . . . . ? O4 Cu1 N5 C39 -111.4(10) 2_647 . . . ? O1 Cu1 N5 C35 173.1(10) . . . . ? O3 Cu1 N5 C35 2.5(10) 2_647 . . . ? N1 Cu1 N5 C35 -101.8(17) . . . . ? O4 Cu1 N5 C35 59.7(9) 2_647 . . . ? O5 Cu2 N6 C44 -176.5(10) . . . . ? N3 Cu2 N6 C44 101.6(18) . . . . ? O7 Cu2 N6 C44 -7.2(10) 2_556 . . . ? O8 Cu2 N6 C44 -66.1(10) 2_556 . . . ? C34 Cu2 N6 C44 -37.2(10) 2_556 . . . ? O5 Cu2 N6 C40 -1.8(9) . . . . ? N3 Cu2 N6 C40 -83.7(18) . . . . ? O7 Cu2 N6 C40 167.4(9) 2_556 . . . ? O8 Cu2 N6 C40 108.6(9) 2_556 . . . ? C34 Cu2 N6 C40 137.5(9) 2_556 . . . ? Cu1 O1 C1 C2 -171.0(8) . . . . ? Cu1 O1 C1 C6 10.7(18) . . . . ? O1 C1 C2 C3 -178.6(12) . . . . ? C6 C1 C2 C3 -0.2(18) . . . . ? C1 C2 C3 C4 -2(2) . . . . ? C2 C3 C4 C5 3(2) . . . . ? C3 C4 C5 C6 0(2) . . . . ? C4 C5 C6 C7 178.4(13) . . . . ? C4 C5 C6 C1 -2(2) . . . . ? O1 C1 C6 C5 -179.4(12) . . . . ? C2 C1 C6 C5 2.3(18) . . . . ? O1 C1 C6 C7 0.1(19) . . . . ? C2 C1 C6 C7 -178.2(11) . . . . ? N2 N1 C7 O2 -3.4(13) . . . . ? Cu1 N1 C7 O2 -178.2(7) . . . . ? N2 N1 C7 C6 176.7(12) . . . . ? Cu1 N1 C7 C6 1.9(18) . . . . ? C8 O2 C7 N1 2.4(13) . . . . ? C8 O2 C7 C6 -177.7(12) . . . . ? C5 C6 C7 N1 173.3(12) . . . . ? C1 C6 C7 N1 -6(2) . . . . ? C5 C6 C7 O2 -6.6(18) . . . . ? C1 C6 C7 O2 173.8(11) . . . . ? N1 N2 C8 O2 -1.6(14) . . . . ? N1 N2 C8 C9 -175.9(12) . . . . ? C7 O2 C8 N2 -0.4(14) . . . . ? C7 O2 C8 C9 174.7(11) . . . . ? N2 C8 C9 C10 -177.3(14) . . . . ? O2 C8 C9 C10 8.7(17) . . . . ? N2 C8 C9 C13 -51(2) . . . . ? O2 C8 C9 C13 134.8(12) . . . . ? C8 C9 C10 C15 145.1(11) . . . . ? C13 C9 C10 C15 14.9(14) . . . . ? C10 C9 C13 C11 81.4(12) . . . . ? C8 C9 C13 C11 -50.3(15) . . . . ? C10 C9 C13 C12 -156.2(11) . . . . ? C8 C9 C13 C12 72.2(14) . . . . ? C10 C9 C13 C14 -33.6(13) . . . . ? C8 C9 C13 C14 -165.2(12) . . . . ? C11 C13 C14 C15 -74.9(12) . . . . ? C12 C13 C14 C15 160.3(11) . . . . ? C9 C13 C14 C15 40.9(12) . . . . ? C11 C13 C14 C17 51.3(14) . . . . ? C12 C13 C14 C17 -73.5(14) . . . . ? C9 C13 C14 C17 167.1(12) . . . . ? C11 C13 C14 C16 169.6(10) . . . . ? C12 C13 C14 C16 44.8(12) . . . . ? C9 C13 C14 C16 -74.6(11) . . . . ? C17 C14 C15 C10 -157.4(10) . . . . ? C13 C14 C15 C10 -32.4(13) . . . . ? C16 C14 C15 C10 83.8(12) . . . . ? C9 C10 C15 C14 11.2(15) . . . . ? Cu1 O4 C17 O3 -2.3(11) 2_657 . . . ? Cu1 O4 C17 C14 175.3(10) 2_657 . . . ? Cu1 O3 C17 O4 2.9(14) 2_657 . . . ? Cu1 O3 C17 C14 -174.8(8) 2_657 . . . ? C15 C14 C17 O4 -177.4(10) . . . . ? C13 C14 C17 O4 62.1(15) . . . . ? C16 C14 C17 O4 -57.7(13) . . . . ? C15 C14 C17 O3 0.3(16) . . . . ? C13 C14 C17 O3 -120.1(12) . . . . ? C16 C14 C17 O3 120.0(12) . . . . ? Cu2 O5 C18 C23 -5.8(18) . . . . ? Cu2 O5 C18 C19 174.5(8) . . . . ? O5 C18 C19 C20 -179.8(12) . . . . ? C23 C18 C19 C20 0.5(18) . . . . ? C18 C19 C20 C21 -1(2) . . . . ? C19 C20 C21 C22 0(2) . . . . ? C20 C21 C22 C23 1(2) . . . . ? C21 C22 C23 C18 -1.0(19) . . . . ? C21 C22 C23 C24 -176.4(12) . . . . ? O5 C18 C23 C22 -179.4(11) . . . . ? C19 C18 C23 C22 0.3(17) . . . . ? O5 C18 C23 C24 -3.8(18) . . . . ? C19 C18 C23 C24 175.9(10) . . . . ? N4 N3 C24 O6 0.3(12) . . . . ? Cu2 N3 C24 O6 173.6(7) . . . . ? N4 N3 C24 C23 -176.7(11) . . . . ? Cu2 N3 C24 C23 -3.4(18) . . . . ? C25 O6 C24 N3 -1.6(12) . . . . ? C25 O6 C24 C23 175.8(10) . . . . ? C22 C23 C24 N3 -176.0(12) . . . . ? C18 C23 C24 N3 8.6(19) . . . . ? C22 C23 C24 O6 7.2(17) . . . . ? C18 C23 C24 O6 -168.3(10) . . . . ? N3 N4 C25 O6 -2.4(13) . . . . ? N3 N4 C25 C26 175.0(12) . . . . ? C24 O6 C25 N4 2.5(12) . . . . ? C24 O6 C25 C26 -175.3(10) . . . . ? N4 C25 C26 C27 -25.0(18) . . . . ? O6 C25 C26 C27 152.4(10) . . . . ? N4 C25 C26 C28 96.8(15) . . . . ? O6 C25 C26 C28 -85.9(11) . . . . ? C25 C26 C27 C31 152.3(9) . . . . ? C28 C26 C27 C31 23.9(11) . . . . ? C25 C26 C28 C29 -51.2(12) . . . . ? C27 C26 C28 C29 76.4(11) . . . . ? C25 C26 C28 C30 70.0(12) . . . . ? C27 C26 C28 C30 -162.5(9) . . . . ? C25 C26 C28 C33 -166.9(9) . . . . ? C27 C26 C28 C33 -39.4(10) . . . . ? C26 C27 C31 C33 2.6(12) . . . . ? C27 C31 C33 C32 93.0(11) . . . . ? C27 C31 C33 C34 -145.7(9) . . . . ? C27 C31 C33 C28 -27.9(10) . . . . ? C29 C28 C33 C31 -73.8(11) . . . . ? C30 C28 C33 C31 162.4(9) . . . . ? C26 C28 C33 C31 41.1(9) . . . . ? C29 C28 C33 C32 167.5(10) . . . . ? C30 C28 C33 C32 43.7(13) . . . . ? C26 C28 C33 C32 -77.7(11) . . . . ? C29 C28 C33 C34 46.6(12) . . . . ? C30 C28 C33 C34 -77.2(10) . . . . ? C26 C28 C33 C34 161.4(9) . . . . ? Cu2 O8 C34 O7 0.5(10) 2_546 . . . ? Cu2 O8 C34 C33 -174.4(9) 2_546 . . . ? Cu2 O7 C34 O8 -0.5(12) 2_546 . . . ? Cu2 O7 C34 C33 174.4(7) 2_546 . . . ? C31 C33 C34 O8 5.2(14) . . . . ? C32 C33 C34 O8 127.1(11) . . . . ? C28 C33 C34 O8 -109.3(11) . . . . ? C31 C33 C34 O7 -169.9(9) . . . . ? C32 C33 C34 O7 -47.9(13) . . . . ? C28 C33 C34 O7 75.6(12) . . . . ? C31 C33 C34 Cu2 -148(3) . . . 2_546 ? C32 C33 C34 Cu2 -26(4) . . . 2_546 ? C28 C33 C34 Cu2 97(4) . . . 2_546 ? C39 N5 C35 C36 0.7(19) . . . . ? Cu1 N5 C35 C36 -170.8(11) . . . . ? N5 C35 C36 C37 0(2) . . . . ? C35 C36 C37 C38 0(2) . . . . ? C36 C37 C38 C39 -2(2) . . . . ? C35 N5 C39 C38 -2.2(19) . . . . ? Cu1 N5 C39 C38 169.5(11) . . . . ? C37 C38 C39 N5 3(2) . . . . ? C44 N6 C40 C41 4.5(18) . . . . ? Cu2 N6 C40 C41 -170.4(10) . . . . ? N6 C40 C41 C42 0(2) . . . . ? C40 C41 C42 C43 -3(2) . . . . ? C41 C42 C43 C44 1(2) . . . . ? C40 N6 C44 C43 -6.1(19) . . . . ? Cu2 N6 C44 C43 168.8(11) . . . . ? C42 C43 C44 N6 3(2) . . . . ? _chemical_absolute_configuration 'rmad' _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.497 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.091 #===END data_compound-4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H46 N6 O8 Zn2' _chemical_formula_sum 'C44 H46 N6 O8 Zn2' _chemical_formula_weight 917.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.0633(5) _cell_length_b 13.4316(7) _cell_length_c 15.0358(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.9244(9) _cell_angle_gamma 90.00 _cell_volume 2024.83(17) _cell_formula_units_Z 2 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 5464 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 25.01 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 1.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7709 _exptl_absorpt_correction_T_max 0.8159 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12250 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7050 _reflns_number_gt 5697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+0.6577P] 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 0.010(17) _refine_ls_number_reflns 7050 _refine_ls_number_parameters 547 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1053 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.25680(6) 0.56774(4) 0.19456(4) 0.02968(19) Uani 1 1 d . . . Zn2 Zn 0.23829(6) 0.76401(4) 0.31326(4) 0.03001(19) Uani 1 1 d . . . C1 C 0.3855(5) 0.7658(6) 0.1448(3) 0.0311(13) Uani 1 1 d . . . C2 C 0.4354(6) 0.7135(5) 0.0738(4) 0.0344(15) Uani 1 1 d . . . H2 H 0.4002 0.6493 0.0594 0.041 Uiso 1 1 calc R . . C3 C 0.5315(6) 0.7505(7) 0.0249(4) 0.048(2) Uani 1 1 d . . . H3 H 0.5598 0.7127 -0.0234 0.057 Uiso 1 1 calc R . . C4 C 0.5882(7) 0.8415(6) 0.0445(4) 0.050(2) Uani 1 1 d . . . H4 H 0.6607 0.8649 0.0138 0.060 Uiso 1 1 calc R . . C5 C 0.5369(7) 0.8984(6) 0.1100(4) 0.0430(18) Uani 1 1 d . . . H5 H 0.5703 0.9638 0.1206 0.052 Uiso 1 1 calc R . . C6 C 0.4386(6) 0.8631(5) 0.1606(4) 0.0326(15) Uani 1 1 d . . . C7 C 0.3932(6) 0.9256(5) 0.2284(4) 0.0288(15) Uani 1 1 d . . . C8 C 0.3768(6) 1.0593(6) 0.3078(4) 0.0355(15) Uani 1 1 d . . . C9 C 0.4151(6) 1.1597(5) 0.3396(4) 0.0382(16) Uani 1 1 d . . . H9 H 0.4240 1.2031 0.2864 0.046 Uiso 1 1 calc R . . C10 C 0.3072(6) 1.2055(5) 0.3952(5) 0.0631(19) Uani 1 1 d . . . H10A H 0.2469 1.2489 0.3570 0.076 Uiso 1 1 calc R . . H10B H 0.2534 1.1520 0.4198 0.076 Uiso 1 1 calc R . . C11 C 0.3744(6) 1.2630(6) 0.4673(4) 0.0549(16) Uani 1 1 d . . . H11A H 0.3603 1.2320 0.5255 0.066 Uiso 1 1 calc R . . H11B H 0.3381 1.3316 0.4669 0.066 Uiso 1 1 calc R . . C12 C 0.5243(6) 1.2655(6) 0.4535(3) 0.0339(14) Uani 1 1 d . . . C13 C 0.5477(5) 1.1662(4) 0.4014(3) 0.0330(12) Uani 1 1 d . . . C14 C 0.6089(7) 1.2674(6) 0.5428(4) 0.0424(16) Uani 1 1 d . . . C15 C 0.5552(6) 1.3579(4) 0.3991(3) 0.0470(15) Uani 1 1 d . . . H15A H 0.5406 1.4179 0.4341 0.071 Uiso 1 1 calc R . . H15B H 0.4963 1.3593 0.3437 0.071 Uiso 1 1 calc R . . H15C H 0.6483 1.3556 0.3848 0.071 Uiso 1 1 calc R . . C16 C 0.6666(5) 1.1681(4) 0.3477(4) 0.0489(15) Uani 1 1 d . . . H16A H 0.7464 1.1854 0.3866 0.073 Uiso 1 1 calc R . . H16B H 0.6525 1.2178 0.3001 0.073 Uiso 1 1 calc R . . H16C H 0.6784 1.1023 0.3213 0.073 Uiso 1 1 calc R . . C17 C 0.5565(6) 1.0769(5) 0.4668(4) 0.0504(17) Uani 1 1 d . . . H17A H 0.5634 1.0149 0.4332 0.076 Uiso 1 1 calc R . . H17B H 0.4762 1.0750 0.4993 0.076 Uiso 1 1 calc R . . H17C H 0.6353 1.0844 0.5093 0.076 Uiso 1 1 calc R . . C18 C -0.0047(7) 0.8727(5) 0.3524(4) 0.0417(17) Uani 1 1 d . . . H18 H 0.0600 0.9071 0.3905 0.050 Uiso 1 1 calc R . . C19 C -0.1362(7) 0.8963(6) 0.3547(5) 0.052(2) Uani 1 1 d . . . H19 H -0.1630 0.9456 0.3948 0.063 Uiso 1 1 calc R . . C20 C -0.2307(7) 0.8471(7) 0.2972(5) 0.055(2) Uani 1 1 d . . . H20 H -0.3230 0.8613 0.2984 0.066 Uiso 1 1 calc R . . C21 C -0.1891(7) 0.7793(6) 0.2402(4) 0.0475(18) Uani 1 1 d . . . H21 H -0.2510 0.7466 0.1987 0.057 Uiso 1 1 calc R . . C22 C -0.0555(6) 0.7582(6) 0.2429(3) 0.0364(15) Uani 1 1 d . . . H22 H -0.0272 0.7091 0.2031 0.044 Uiso 1 1 calc R . . C23 C 0.4980(7) 0.4606(7) 0.1515(5) 0.056(2) Uani 1 1 d . . . H23 H 0.4337 0.4271 0.1123 0.068 Uiso 1 1 calc R . . C24 C 0.6294(7) 0.4346(8) 0.1479(5) 0.068(3) Uani 1 1 d . . . H24 H 0.6547 0.3866 0.1062 0.082 Uiso 1 1 calc R . . C25 C 0.7208(7) 0.4783(6) 0.2045(5) 0.052(2) Uani 1 1 d . . . H25 H 0.8124 0.4612 0.2043 0.063 Uiso 1 1 calc R . . C26 C 0.6803(7) 0.5490(6) 0.2636(4) 0.050(2) Uani 1 1 d . . . H26 H 0.7437 0.5810 0.3046 0.060 Uiso 1 1 calc R . . C27 C 0.5467(6) 0.5723(6) 0.2621(3) 0.0371(15) Uani 1 1 d . . . H27 H 0.5187 0.6209 0.3024 0.045 Uiso 1 1 calc R . . C28 C 0.1008(5) 0.5672(6) 0.3599(3) 0.0276(12) Uani 1 1 d . . . C29 C 0.0533(6) 0.6193(5) 0.4324(4) 0.0381(16) Uani 1 1 d . . . H29 H 0.0919 0.6817 0.4494 0.046 Uiso 1 1 calc R . . C30 C -0.0467(6) 0.5822(6) 0.4786(4) 0.0417(17) Uani 1 1 d . . . H30 H -0.0777 0.6205 0.5258 0.050 Uiso 1 1 calc R . . C31 C -0.1039(6) 0.4907(5) 0.4587(4) 0.0391(16) Uani 1 1 d . . . H31 H -0.1758 0.4672 0.4899 0.047 Uiso 1 1 calc R . . C32 C -0.0548(6) 0.4349(5) 0.3934(4) 0.0357(16) Uani 1 1 d . . . H32 H -0.0899 0.3702 0.3812 0.043 Uiso 1 1 calc R . . C33 C 0.0475(6) 0.4717(5) 0.3433(4) 0.0270(14) Uani 1 1 d . . . C34 C 0.0977(6) 0.4063(5) 0.2782(4) 0.0337(16) Uani 1 1 d . . . C35 C 0.1125(6) 0.2756(6) 0.1977(4) 0.0362(15) Uani 1 1 d . . . C36 C 0.0827(7) 0.1739(5) 0.1596(4) 0.0413(18) Uani 1 1 d . . . H36 H 0.1707 0.1397 0.1578 0.050 Uiso 1 1 calc R . . C37 C -0.0014(9) 0.1068(5) 0.2105(4) 0.085(3) Uani 1 1 d . . . H37A H -0.0666 0.1454 0.2422 0.102 Uiso 1 1 calc R . . H37B H 0.0544 0.0666 0.2545 0.102 Uiso 1 1 calc R . . C38 C -0.0732(10) 0.0394(6) 0.1375(5) 0.094(3) Uani 1 1 d . . . H38A H -0.0537 -0.0315 0.1511 0.113 Uiso 1 1 calc R . . H38B H -0.1709 0.0494 0.1355 0.113 Uiso 1 1 calc R . . C39 C -0.0231(6) 0.0671(6) 0.0476(3) 0.0339(14) Uani 1 1 d . . . C40 C 0.0201(6) 0.1774(4) 0.0629(4) 0.0399(14) Uani 1 1 d . . . C41 C -0.1213(8) 0.0559(6) -0.0344(5) 0.055(2) Uani 1 1 d . . . C42 C 0.0940(8) 0.0020(7) 0.0318(7) 0.121(5) Uani 1 1 d . . . H42A H 0.1714 0.0225 0.0716 0.182 Uiso 1 1 calc R . . H42B H 0.1149 0.0088 -0.0304 0.182 Uiso 1 1 calc R . . H42C H 0.0722 -0.0675 0.0438 0.182 Uiso 1 1 calc R . . C43 C -0.1079(8) 0.2418(5) 0.0633(5) 0.077(3) Uani 1 1 d . . . H43A H -0.0839 0.3090 0.0844 0.115 Uiso 1 1 calc R . . H43B H -0.1688 0.2116 0.1030 0.115 Uiso 1 1 calc R . . H43C H -0.1518 0.2456 0.0026 0.115 Uiso 1 1 calc R . . C44 C 0.1049(10) 0.2220(7) 0.0004(5) 0.129(5) Uani 1 1 d . . . H44A H 0.0559 0.2264 -0.0587 0.193 Uiso 1 1 calc R . . H44B H 0.1846 0.1807 -0.0034 0.193 Uiso 1 1 calc R . . H44C H 0.1316 0.2889 0.0210 0.193 Uiso 1 1 calc R . . N1 N 0.3042(5) 0.9106(4) 0.2832(3) 0.0323(12) Uani 1 1 d . . . N2 N 0.2929(6) 0.9973(4) 0.3369(4) 0.0398(14) Uani 1 1 d . . . N3 N 0.0359(5) 0.8018(4) 0.2974(3) 0.0295(13) Uani 1 1 d . . . N4 N 0.4548(5) 0.5281(4) 0.2049(3) 0.0317(13) Uani 1 1 d . . . N5 N 0.1970(5) 0.4204(4) 0.2279(3) 0.0376(13) Uani 1 1 d . . . N6 N 0.2085(6) 0.3336(5) 0.1770(4) 0.0432(15) Uani 1 1 d . . . O1 O 0.2993(4) 0.7242(3) 0.1931(2) 0.0304(10) Uani 1 1 d . . . O2 O 0.4459(4) 1.0186(3) 0.2391(3) 0.0364(11) Uani 1 1 d . . . O3 O 0.7300(5) 1.2902(4) 0.5430(3) 0.0528(13) Uani 1 1 d . . . O4 O 0.5609(6) 1.2458(5) 0.6127(3) 0.0708(18) Uani 1 1 d . . . O5 O 0.1925(4) 0.6080(3) 0.3140(2) 0.0321(10) Uani 1 1 d . . . O6 O 0.0405(4) 0.3149(3) 0.2597(3) 0.0331(11) Uani 1 1 d . . . O7 O -0.2357(5) 0.0251(4) -0.0251(5) 0.094(2) Uani 1 1 d . . . O8 O -0.0886(6) 0.0817(5) -0.1067(3) 0.0798(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0297(4) 0.0306(4) 0.0287(3) -0.0053(3) 0.0024(3) -0.0011(3) Zn2 0.0317(4) 0.0292(4) 0.0293(4) -0.0031(3) 0.0034(3) -0.0019(4) C1 0.028(3) 0.042(4) 0.021(3) 0.003(3) -0.007(2) -0.005(3) C2 0.034(4) 0.041(4) 0.029(3) 0.003(3) 0.006(3) -0.005(3) C3 0.036(4) 0.077(6) 0.029(3) 0.000(4) -0.001(3) 0.003(4) C4 0.036(4) 0.082(6) 0.031(4) 0.017(4) 0.002(3) -0.001(4) C5 0.053(5) 0.042(5) 0.032(3) 0.007(3) -0.003(3) -0.008(4) C6 0.026(3) 0.045(4) 0.026(3) 0.005(3) 0.000(3) -0.008(3) C7 0.031(4) 0.022(4) 0.033(3) 0.008(3) -0.001(3) -0.008(3) C8 0.028(3) 0.037(4) 0.040(3) -0.003(3) -0.006(3) 0.002(4) C9 0.039(4) 0.023(4) 0.050(4) 0.001(3) -0.012(3) 0.000(3) C10 0.030(3) 0.048(4) 0.109(6) -0.026(4) -0.013(3) 0.001(3) C11 0.037(3) 0.090(5) 0.038(3) -0.007(4) 0.002(2) 0.001(4) C12 0.038(4) 0.030(4) 0.033(3) 0.006(3) 0.001(3) 0.004(4) C13 0.033(3) 0.023(3) 0.042(3) 0.002(2) -0.004(2) 0.002(2) C14 0.057(4) 0.024(3) 0.042(4) -0.002(4) -0.014(3) -0.003(4) C15 0.083(5) 0.024(3) 0.033(3) -0.001(2) -0.006(3) -0.002(3) C16 0.046(3) 0.037(3) 0.065(4) -0.013(3) 0.014(3) -0.008(3) C17 0.052(4) 0.029(3) 0.066(4) 0.022(3) -0.019(3) -0.008(3) C18 0.041(4) 0.040(4) 0.044(4) -0.018(3) 0.003(3) 0.003(4) C19 0.053(5) 0.050(5) 0.053(4) -0.012(4) -0.001(4) 0.021(4) C20 0.036(4) 0.079(6) 0.049(4) 0.010(4) 0.003(3) 0.007(4) C21 0.041(4) 0.050(5) 0.049(4) -0.003(4) -0.011(3) 0.002(4) C22 0.039(4) 0.040(4) 0.029(3) -0.010(3) 0.000(3) 0.000(4) C23 0.043(5) 0.079(6) 0.046(4) -0.026(4) -0.006(4) 0.014(5) C24 0.044(5) 0.110(8) 0.049(4) -0.030(5) -0.003(4) 0.023(5) C25 0.032(4) 0.068(6) 0.057(5) -0.007(4) 0.001(3) 0.015(4) C26 0.045(4) 0.055(6) 0.046(4) 0.008(4) -0.016(3) -0.009(4) C27 0.046(4) 0.033(4) 0.031(3) 0.009(3) -0.003(3) 0.003(4) C28 0.024(3) 0.033(3) 0.026(3) 0.003(3) 0.004(2) 0.004(3) C29 0.047(4) 0.039(4) 0.029(3) -0.007(3) 0.003(3) -0.002(3) C30 0.045(4) 0.052(5) 0.030(3) 0.002(3) 0.012(3) -0.004(4) C31 0.034(4) 0.049(4) 0.035(4) 0.003(3) 0.008(3) -0.009(3) C32 0.028(3) 0.042(4) 0.037(3) 0.012(3) 0.001(3) -0.006(3) C33 0.030(3) 0.026(3) 0.024(3) 0.001(2) -0.004(2) 0.001(3) C34 0.031(4) 0.036(4) 0.033(3) 0.007(3) -0.005(3) -0.003(3) C35 0.047(4) 0.026(4) 0.035(3) 0.001(3) 0.002(3) 0.003(4) C36 0.054(5) 0.036(5) 0.032(3) -0.003(3) -0.006(3) -0.001(4) C37 0.163(8) 0.053(4) 0.040(4) -0.002(3) 0.009(4) -0.046(5) C38 0.160(8) 0.061(5) 0.061(5) -0.002(4) 0.008(5) -0.070(5) C39 0.040(4) 0.025(3) 0.034(3) -0.001(3) -0.013(3) -0.002(4) C40 0.043(3) 0.040(3) 0.036(3) 0.000(3) -0.001(3) -0.015(3) C41 0.067(5) 0.028(4) 0.063(5) 0.013(4) -0.031(4) -0.012(4) C42 0.091(7) 0.104(7) 0.154(9) -0.088(7) -0.080(6) 0.047(6) C43 0.082(6) 0.031(4) 0.107(6) -0.001(4) -0.049(5) 0.003(4) C44 0.175(10) 0.162(9) 0.058(5) -0.041(5) 0.054(6) -0.132(8) N1 0.033(3) 0.027(3) 0.036(3) -0.005(2) -0.001(2) -0.005(3) N2 0.044(3) 0.026(3) 0.049(3) -0.011(2) 0.005(3) -0.006(3) N3 0.030(3) 0.029(3) 0.030(3) 0.000(2) 0.003(2) 0.000(2) N4 0.033(3) 0.036(3) 0.026(3) -0.007(2) 0.001(2) -0.004(2) N5 0.045(3) 0.028(3) 0.040(3) -0.006(2) 0.005(3) -0.002(3) N6 0.051(4) 0.040(4) 0.039(3) -0.005(2) 0.006(3) -0.003(3) O1 0.027(2) 0.037(3) 0.027(2) 0.0010(17) 0.0035(17) -0.005(2) O2 0.035(2) 0.036(3) 0.037(2) 0.006(2) -0.0032(19) -0.009(2) O3 0.046(3) 0.034(3) 0.073(3) -0.012(2) -0.024(2) 0.008(2) O4 0.101(4) 0.073(4) 0.035(3) 0.017(3) -0.016(3) -0.038(3) O5 0.044(3) 0.021(2) 0.031(2) -0.0082(16) 0.0036(18) -0.005(2) O6 0.039(3) 0.025(3) 0.035(2) -0.0035(19) 0.000(2) -0.006(2) O7 0.040(3) 0.053(4) 0.178(6) -0.026(4) -0.043(3) -0.006(3) O8 0.139(5) 0.051(4) 0.043(3) 0.004(3) -0.030(3) -0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 2.034(4) . ? Zn1 N4 2.055(5) . ? Zn1 O8 2.064(5) 2 ? Zn1 N5 2.141(5) . ? Zn1 O1 2.145(4) . ? Zn1 O7 2.602(7) 2 ? Zn2 O1 2.030(4) . ? Zn2 N3 2.093(5) . ? Zn2 N1 2.139(5) . ? Zn2 O5 2.146(4) . ? Zn2 O3 2.186(5) 2_646 ? Zn2 O4 2.235(5) 2_646 ? Zn2 C14 2.545(6) 2_646 ? C1 O1 1.304(7) . ? C1 C2 1.406(8) . ? C1 C6 1.424(10) . ? C2 C3 1.358(8) . ? C2 H2 0.9500 . ? C3 C4 1.370(11) . ? C3 H3 0.9500 . ? C4 C5 1.381(10) . ? C4 H4 0.9500 . ? C5 C6 1.383(8) . ? C5 H5 0.9500 . ? C6 C7 1.425(8) . ? C7 N1 1.284(7) . ? C7 O2 1.362(7) . ? C8 N2 1.289(8) . ? C8 O2 1.405(7) . ? C8 C9 1.471(10) . ? C9 C10 1.554(9) . ? C9 C13 1.562(7) . ? C9 H9 1.0000 . ? C10 C11 1.450(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.541(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C14 1.527(8) . ? C12 C15 1.532(8) . ? C12 C13 1.575(9) . ? C13 C16 1.500(7) . ? C13 C17 1.548(7) . ? C14 O4 1.228(7) . ? C14 O3 1.256(8) . ? C14 Zn2 2.545(6) 2_656 ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N3 1.346(8) . ? C18 C19 1.364(9) . ? C18 H18 0.9500 . ? C19 C20 1.396(10) . ? C19 H19 0.9500 . ? C20 C21 1.341(10) . ? C20 H20 0.9500 . ? C21 C22 1.371(8) . ? C21 H21 0.9500 . ? C22 N3 1.316(8) . ? C22 H22 0.9500 . ? C23 N4 1.311(8) . ? C23 C24 1.373(9) . ? C23 H23 0.9500 . ? C24 C25 1.334(10) . ? C24 H24 0.9500 . ? C25 C26 1.386(10) . ? C25 H25 0.9500 . ? C26 C27 1.379(8) . ? C26 H26 0.9500 . ? C27 N4 1.346(8) . ? C27 H27 0.9500 . ? C28 O5 1.318(7) . ? C28 C33 1.405(9) . ? C28 C29 1.413(8) . ? C29 C30 1.365(8) . ? C29 H29 0.9500 . ? C30 C31 1.379(9) . ? C30 H30 0.9500 . ? C31 C32 1.361(8) . ? C31 H31 0.9500 . ? C32 C33 1.415(8) . ? C32 H32 0.9500 . ? C33 C34 1.439(8) . ? C34 N5 1.317(7) . ? C34 O6 1.374(8) . ? C35 N6 1.300(8) . ? C35 O6 1.338(7) . ? C35 C36 1.501(10) . ? C36 C37 1.492(9) . ? C36 C40 1.535(7) . ? C36 H36 1.0000 . ? C37 C38 1.553(9) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.528(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C42 1.502(9) . ? C39 C41 1.521(8) . ? C39 C40 1.556(9) . ? C40 C44 1.453(9) . ? C40 C43 1.552(9) . ? C41 O8 1.213(8) . ? C41 O7 1.242(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? N1 N2 1.427(7) . ? N5 N6 1.404(7) . ? O3 Zn2 2.186(5) 2_656 ? O4 Zn2 2.235(5) 2_656 ? O7 Zn1 2.602(7) 2_545 ? O8 Zn1 2.064(5) 2_545 ? 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 N4 112.47(18) . . ? O5 Zn1 O8 103.6(2) . 2 ? N4 Zn1 O8 143.9(2) . 2 ? O5 Zn1 N5 85.50(18) . . ? N4 Zn1 N5 91.9(2) . . ? O8 Zn1 N5 90.1(2) 2 . ? O5 Zn1 O1 80.08(15) . . ? N4 Zn1 O1 93.55(19) . . ? O8 Zn1 O1 93.3(2) 2 . ? N5 Zn1 O1 165.58(17) . . ? O5 Zn1 O7 156.60(18) . 2 ? N4 Zn1 O7 90.79(18) . 2 ? O8 Zn1 O7 53.14(19) 2 2 ? N5 Zn1 O7 91.44(18) . 2 ? O1 Zn1 O7 101.81(16) . 2 ? O1 Zn2 N3 109.17(17) . . ? O1 Zn2 N1 86.06(18) . . ? N3 Zn2 N1 94.0(2) . . ? O1 Zn2 O5 80.16(15) . . ? N3 Zn2 O5 91.74(19) . . ? N1 Zn2 O5 166.16(16) . . ? O1 Zn2 O3 153.27(18) . 2_646 ? N3 Zn2 O3 97.56(18) . 2_646 ? N1 Zn2 O3 92.25(18) . 2_646 ? O5 Zn2 O3 99.49(16) . 2_646 ? O1 Zn2 O4 94.88(17) . 2_646 ? N3 Zn2 O4 155.87(18) . 2_646 ? N1 Zn2 O4 85.5(2) . 2_646 ? O5 Zn2 O4 94.4(2) . 2_646 ? O3 Zn2 O4 58.41(17) 2_646 2_646 ? O1 Zn2 C14 123.7(2) . 2_646 ? N3 Zn2 C14 127.1(2) . 2_646 ? N1 Zn2 C14 89.3(2) . 2_646 ? O5 Zn2 C14 97.3(2) . 2_646 ? O3 Zn2 C14 29.57(19) 2_646 2_646 ? O4 Zn2 C14 28.85(19) 2_646 2_646 ? O1 C1 C2 120.4(7) . . ? O1 C1 C6 123.9(5) . . ? C2 C1 C6 115.6(5) . . ? C3 C2 C1 123.0(7) . . ? C3 C2 H2 118.5 . . ? C1 C2 H2 118.5 . . ? C2 C3 C4 120.8(7) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C3 C4 C5 118.2(6) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? C4 C5 C6 122.1(7) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C1 119.9(6) . . ? C5 C6 C7 118.7(6) . . ? C1 C6 C7 121.4(5) . . ? N1 C7 O2 110.7(5) . . ? N1 C7 C6 130.6(6) . . ? O2 C7 C6 118.6(5) . . ? N2 C8 O2 112.2(6) . . ? N2 C8 C9 130.0(6) . . ? O2 C8 C9 117.6(6) . . ? C8 C9 C10 111.2(5) . . ? C8 C9 C13 115.6(5) . . ? C10 C9 C13 104.9(5) . . ? C8 C9 H9 108.3 . . ? C10 C9 H9 108.3 . . ? C13 C9 H9 108.3 . . ? C11 C10 C9 108.1(5) . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? C11 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 C11 C12 108.1(5) . . ? C10 C11 H11A 110.1 . . ? C12 C11 H11A 110.1 . . ? C10 C11 H11B 110.1 . . ? C12 C11 H11B 110.1 . . ? H11A C11 H11B 108.4 . . ? C14 C12 C15 109.4(6) . . ? C14 C12 C11 111.1(5) . . ? C15 C12 C11 109.6(6) . . ? C14 C12 C13 110.8(5) . . ? C15 C12 C13 112.0(4) . . ? C11 C12 C13 103.8(5) . . ? C16 C13 C17 110.5(5) . . ? C16 C13 C9 111.1(5) . . ? C17 C13 C9 109.5(5) . . ? C16 C13 C12 114.4(4) . . ? C17 C13 C12 110.1(5) . . ? C9 C13 C12 100.8(4) . . ? O4 C14 O3 120.6(6) . . ? O4 C14 C12 121.2(6) . . ? O3 C14 C12 118.2(6) . . ? O4 C14 Zn2 61.4(3) . 2_656 ? O3 C14 Zn2 59.2(3) . 2_656 ? C12 C14 Zn2 176.1(5) . 2_656 ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C19 121.7(7) . . ? N3 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C18 C19 C20 119.0(7) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 118.9(7) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C20 C21 C22 118.7(7) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? N3 C22 C21 123.8(6) . . ? N3 C22 H22 118.1 . . ? C21 C22 H22 118.1 . . ? N4 C23 C24 124.8(7) . . ? N4 C23 H23 117.6 . . ? C24 C23 H23 117.6 . . ? C25 C24 C23 118.5(7) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 C25 C26 119.1(6) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 C25 119.0(7) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? N4 C27 C26 121.8(7) . . ? N4 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? O5 C28 C33 124.1(5) . . ? O5 C28 C29 119.7(7) . . ? C33 C28 C29 116.1(5) . . ? C30 C29 C28 121.7(7) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 121.8(6) . . ? C29 C30 H30 119.1 . . ? C31 C30 H30 119.1 . . ? C32 C31 C30 118.5(6) . . ? C32 C31 H31 120.8 . . ? C30 C31 H31 120.8 . . ? C31 C32 C33 121.2(7) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C28 C33 C32 120.5(5) . . ? C28 C33 C34 121.8(5) . . ? C32 C33 C34 117.6(6) . . ? N5 C34 O6 109.8(5) . . ? N5 C34 C33 129.1(6) . . ? O6 C34 C33 121.1(5) . . ? N6 C35 O6 112.8(6) . . ? N6 C35 C36 125.6(6) . . ? O6 C35 C36 121.5(6) . . ? C37 C36 C35 117.2(5) . . ? C37 C36 C40 107.4(5) . . ? C35 C36 C40 112.7(5) . . ? C37 C36 H36 106.3 . . ? C35 C36 H36 106.3 . . ? C40 C36 H36 106.3 . . ? C36 C37 C38 103.9(5) . . ? C36 C37 H37A 111.0 . . ? C38 C37 H37A 111.0 . . ? C36 C37 H37B 111.0 . . ? C38 C37 H37B 111.0 . . ? H37A C37 H37B 109.0 . . ? C39 C38 C37 108.3(5) . . ? C39 C38 H38A 110.0 . . ? C37 C38 H38A 110.0 . . ? C39 C38 H38B 110.0 . . ? C37 C38 H38B 110.0 . . ? H38A C38 H38B 108.4 . . ? C42 C39 C41 106.1(6) . . ? C42 C39 C38 108.8(7) . . ? C41 C39 C38 116.9(6) . . ? C42 C39 C40 111.4(6) . . ? C41 C39 C40 111.6(5) . . ? C38 C39 C40 102.1(5) . . ? C44 C40 C36 114.2(6) . . ? C44 C40 C43 107.9(7) . . ? C36 C40 C43 106.7(5) . . ? C44 C40 C39 118.0(6) . . ? C36 C40 C39 101.4(5) . . ? C43 C40 C39 108.1(5) . . ? O8 C41 O7 121.5(7) . . ? O8 C41 C39 119.4(7) . . ? O7 C41 C39 119.0(7) . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 H44A 109.5 . . ? C40 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C40 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C7 N1 N2 109.3(5) . . ? C7 N1 Zn2 121.7(4) . . ? N2 N1 Zn2 126.2(4) . . ? C8 N2 N1 104.4(5) . . ? C22 N3 C18 117.7(6) . . ? C22 N3 Zn2 125.7(4) . . ? C18 N3 Zn2 116.4(5) . . ? C23 N4 C27 116.8(6) . . ? C23 N4 Zn1 120.3(5) . . ? C27 N4 Zn1 122.8(4) . . ? C34 N5 N6 107.2(5) . . ? C34 N5 Zn1 120.6(4) . . ? N6 N5 Zn1 126.9(4) . . ? C35 N6 N5 105.6(5) . . ? C1 O1 Zn2 130.5(4) . . ? C1 O1 Zn1 124.6(4) . . ? Zn2 O1 Zn1 99.95(16) . . ? C7 O2 C8 103.4(5) . . ? C14 O3 Zn2 91.2(4) . 2_656 ? C14 O4 Zn2 89.7(4) . 2_656 ? C28 O5 Zn1 129.9(4) . . ? C28 O5 Zn2 124.7(4) . . ? Zn1 O5 Zn2 99.79(17) . . ? C35 O6 C34 104.5(5) . . ? C41 O7 Zn1 79.3(5) . 2_545 ? C41 O8 Zn1 106.0(5) . 2_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -175.7(6) . . . . ? C6 C1 C2 C3 2.4(9) . . . . ? C1 C2 C3 C4 1.8(10) . . . . ? C2 C3 C4 C5 -5.6(10) . . . . ? C3 C4 C5 C6 5.3(10) . . . . ? C4 C5 C6 C1 -1.1(10) . . . . ? C4 C5 C6 C7 178.6(6) . . . . ? O1 C1 C6 C5 175.3(6) . . . . ? C2 C1 C6 C5 -2.7(8) . . . . ? O1 C1 C6 C7 -4.4(9) . . . . ? C2 C1 C6 C7 177.7(6) . . . . ? C5 C6 C7 N1 179.7(6) . . . . ? C1 C6 C7 N1 -0.7(10) . . . . ? C5 C6 C7 O2 1.7(9) . . . . ? C1 C6 C7 O2 -178.6(5) . . . . ? N2 C8 C9 C10 -20.5(10) . . . . ? O2 C8 C9 C10 164.3(5) . . . . ? N2 C8 C9 C13 99.0(8) . . . . ? O2 C8 C9 C13 -76.2(7) . . . . ? C8 C9 C10 C11 143.4(6) . . . . ? C13 C9 C10 C11 17.7(7) . . . . ? C9 C10 C11 C12 6.4(8) . . . . ? C10 C11 C12 C14 -146.9(6) . . . . ? C10 C11 C12 C15 92.0(7) . . . . ? C10 C11 C12 C13 -27.8(7) . . . . ? C8 C9 C13 C16 82.1(6) . . . . ? C10 C9 C13 C16 -155.0(5) . . . . ? C8 C9 C13 C17 -40.3(7) . . . . ? C10 C9 C13 C17 82.6(6) . . . . ? C8 C9 C13 C12 -156.2(5) . . . . ? C10 C9 C13 C12 -33.4(6) . . . . ? C14 C12 C13 C16 -84.4(6) . . . . ? C15 C12 C13 C16 38.2(6) . . . . ? C11 C12 C13 C16 156.3(5) . . . . ? C14 C12 C13 C17 40.8(6) . . . . ? C15 C12 C13 C17 163.3(5) . . . . ? C11 C12 C13 C17 -78.6(5) . . . . ? C14 C12 C13 C9 156.4(5) . . . . ? C15 C12 C13 C9 -81.1(5) . . . . ? C11 C12 C13 C9 37.0(5) . . . . ? C15 C12 C14 O4 136.8(7) . . . . ? C11 C12 C14 O4 15.7(11) . . . . ? C13 C12 C14 O4 -99.2(8) . . . . ? C15 C12 C14 O3 -44.4(9) . . . . ? C11 C12 C14 O3 -165.5(7) . . . . ? C13 C12 C14 O3 79.7(8) . . . . ? C15 C12 C14 Zn2 -91(8) . . . 2_656 ? C11 C12 C14 Zn2 148(8) . . . 2_656 ? C13 C12 C14 Zn2 33(8) . . . 2_656 ? N3 C18 C19 C20 -1.3(11) . . . . ? C18 C19 C20 C21 -1.3(12) . . . . ? C19 C20 C21 C22 2.5(12) . . . . ? C20 C21 C22 N3 -1.2(12) . . . . ? N4 C23 C24 C25 2.2(14) . . . . ? C23 C24 C25 C26 -0.9(13) . . . . ? C24 C25 C26 C27 -0.2(12) . . . . ? C25 C26 C27 N4 0.1(11) . . . . ? O5 C28 C29 C30 176.4(6) . . . . ? C33 C28 C29 C30 -5.3(9) . . . . ? C28 C29 C30 C31 1.9(10) . . . . ? C29 C30 C31 C32 2.6(10) . . . . ? C30 C31 C32 C33 -3.5(10) . . . . ? O5 C28 C33 C32 -177.4(5) . . . . ? C29 C28 C33 C32 4.4(8) . . . . ? O5 C28 C33 C34 5.3(9) . . . . ? C29 C28 C33 C34 -173.0(5) . . . . ? C31 C32 C33 C28 -0.1(9) . . . . ? C31 C32 C33 C34 177.3(6) . . . . ? C28 C33 C34 N5 2.2(10) . . . . ? C32 C33 C34 N5 -175.2(6) . . . . ? C28 C33 C34 O6 -177.0(5) . . . . ? C32 C33 C34 O6 5.6(8) . . . . ? N6 C35 C36 C37 161.3(7) . . . . ? O6 C35 C36 C37 -17.4(10) . . . . ? N6 C35 C36 C40 -73.2(9) . . . . ? O6 C35 C36 C40 108.1(6) . . . . ? C35 C36 C37 C38 151.1(7) . . . . ? C40 C36 C37 C38 23.1(8) . . . . ? C36 C37 C38 C39 2.5(10) . . . . ? C37 C38 C39 C42 91.7(8) . . . . ? C37 C38 C39 C41 -148.2(8) . . . . ? C37 C38 C39 C40 -26.2(8) . . . . ? C37 C36 C40 C44 -167.4(7) . . . . ? C35 C36 C40 C44 62.0(8) . . . . ? C37 C36 C40 C43 73.6(7) . . . . ? C35 C36 C40 C43 -57.0(7) . . . . ? C37 C36 C40 C39 -39.4(7) . . . . ? C35 C36 C40 C39 -170.1(5) . . . . ? C42 C39 C40 C44 48.3(9) . . . . ? C41 C39 C40 C44 -70.1(8) . . . . ? C38 C39 C40 C44 164.3(7) . . . . ? C42 C39 C40 C36 -77.1(7) . . . . ? C41 C39 C40 C36 164.5(6) . . . . ? C38 C39 C40 C36 38.8(6) . . . . ? C42 C39 C40 C43 170.9(6) . . . . ? C41 C39 C40 C43 52.5(7) . . . . ? C38 C39 C40 C43 -73.1(6) . . . . ? C42 C39 C41 O8 -62.2(10) . . . . ? C38 C39 C41 O8 176.3(7) . . . . ? C40 C39 C41 O8 59.3(10) . . . . ? C42 C39 C41 O7 121.3(9) . . . . ? C38 C39 C41 O7 -0.2(11) . . . . ? C40 C39 C41 O7 -117.2(8) . . . . ? O2 C7 N1 N2 -0.5(7) . . . . ? C6 C7 N1 N2 -178.6(6) . . . . ? O2 C7 N1 Zn2 -162.5(4) . . . . ? C6 C7 N1 Zn2 19.4(9) . . . . ? O1 Zn2 N1 C7 -24.0(5) . . . . ? N3 Zn2 N1 C7 -133.0(5) . . . . ? O5 Zn2 N1 C7 -18.9(10) . . . . ? O3 Zn2 N1 C7 129.3(5) 2_646 . . . ? O4 Zn2 N1 C7 71.2(5) 2_646 . . . ? C14 Zn2 N1 C7 99.9(5) 2_646 . . . ? O1 Zn2 N1 N2 177.2(5) . . . . ? N3 Zn2 N1 N2 68.2(5) . . . . ? O5 Zn2 N1 N2 -177.7(6) . . . . ? O3 Zn2 N1 N2 -29.5(5) 2_646 . . . ? O4 Zn2 N1 N2 -87.6(5) 2_646 . . . ? C14 Zn2 N1 N2 -59.0(5) 2_646 . . . ? O2 C8 N2 N1 -1.3(7) . . . . ? C9 C8 N2 N1 -176.6(6) . . . . ? C7 N1 N2 C8 1.1(7) . . . . ? Zn2 N1 N2 C8 162.1(4) . . . . ? C21 C22 N3 C18 -1.3(11) . . . . ? C21 C22 N3 Zn2 174.0(5) . . . . ? C19 C18 N3 C22 2.6(10) . . . . ? C19 C18 N3 Zn2 -173.2(5) . . . . ? O1 Zn2 N3 C22 36.6(6) . . . . ? N1 Zn2 N3 C22 123.8(5) . . . . ? O5 Zn2 N3 C22 -43.5(5) . . . . ? O3 Zn2 N3 C22 -143.4(5) 2_646 . . . ? O4 Zn2 N3 C22 -148.2(6) 2_646 . . . ? C14 Zn2 N3 C22 -144.1(5) 2_646 . . . ? O1 Zn2 N3 C18 -148.0(4) . . . . ? N1 Zn2 N3 C18 -60.8(5) . . . . ? O5 Zn2 N3 C18 131.8(5) . . . . ? O3 Zn2 N3 C18 32.0(5) 2_646 . . . ? O4 Zn2 N3 C18 27.2(8) 2_646 . . . ? C14 Zn2 N3 C18 31.3(6) 2_646 . . . ? C24 C23 N4 C27 -2.2(12) . . . . ? C24 C23 N4 Zn1 174.5(7) . . . . ? C26 C27 N4 C23 1.0(10) . . . . ? C26 C27 N4 Zn1 -175.6(5) . . . . ? O5 Zn1 N4 C23 148.4(5) . . . . ? O8 Zn1 N4 C23 -30.3(8) 2 . . . ? N5 Zn1 N4 C23 62.5(6) . . . . ? O1 Zn1 N4 C23 -130.8(6) . . . . ? O7 Zn1 N4 C23 -28.9(6) 2 . . . ? O5 Zn1 N4 C27 -35.1(5) . . . . ? O8 Zn1 N4 C27 146.2(5) 2 . . . ? N5 Zn1 N4 C27 -121.0(5) . . . . ? O1 Zn1 N4 C27 45.7(5) . . . . ? O7 Zn1 N4 C27 147.6(5) 2 . . . ? O6 C34 N5 N6 -2.2(7) . . . . ? C33 C34 N5 N6 178.6(6) . . . . ? O6 C34 N5 Zn1 154.0(4) . . . . ? C33 C34 N5 Zn1 -25.2(9) . . . . ? O5 Zn1 N5 C34 30.0(5) . . . . ? N4 Zn1 N5 C34 142.4(5) . . . . ? O8 Zn1 N5 C34 -73.6(5) 2 . . . ? O1 Zn1 N5 C34 30.2(11) . . . . ? O7 Zn1 N5 C34 -126.8(5) 2 . . . ? O5 Zn1 N5 N6 -178.9(6) . . . . ? N4 Zn1 N5 N6 -66.5(6) . . . . ? O8 Zn1 N5 N6 77.5(6) 2 . . . ? O1 Zn1 N5 N6 -178.7(6) . . . . ? O7 Zn1 N5 N6 24.4(6) 2 . . . ? O6 C35 N6 N5 -1.8(8) . . . . ? C36 C35 N6 N5 179.4(6) . . . . ? C34 N5 N6 C35 2.4(7) . . . . ? Zn1 N5 N6 C35 -151.8(5) . . . . ? C2 C1 O1 Zn2 165.1(4) . . . . ? C6 C1 O1 Zn2 -12.8(8) . . . . ? C2 C1 O1 Zn1 15.1(7) . . . . ? C6 C1 O1 Zn1 -162.8(4) . . . . ? N3 Zn2 O1 C1 115.3(5) . . . . ? N1 Zn2 O1 C1 22.5(5) . . . . ? O5 Zn2 O1 C1 -156.3(5) . . . . ? O3 Zn2 O1 C1 -64.7(7) 2_646 . . . ? O4 Zn2 O1 C1 -62.7(5) 2_646 . . . ? C14 Zn2 O1 C1 -64.0(6) 2_646 . . . ? N3 Zn2 O1 Zn1 -89.3(2) . . . . ? N1 Zn2 O1 Zn1 177.82(19) . . . . ? O5 Zn2 O1 Zn1 -0.9(2) . . . . ? O3 Zn2 O1 Zn1 90.6(4) 2_646 . . . ? O4 Zn2 O1 Zn1 92.6(2) 2_646 . . . ? C14 Zn2 O1 Zn1 91.3(3) 2_646 . . . ? O5 Zn1 O1 C1 158.3(4) . . . . ? N4 Zn1 O1 C1 46.1(4) . . . . ? O8 Zn1 O1 C1 -98.5(4) 2 . . . ? N5 Zn1 O1 C1 158.1(7) . . . . ? O7 Zn1 O1 C1 -45.5(4) 2 . . . ? O5 Zn1 O1 Zn2 1.0(2) . . . . ? N4 Zn1 O1 Zn2 -111.21(19) . . . . ? O8 Zn1 O1 Zn2 104.2(2) 2 . . . ? N5 Zn1 O1 Zn2 0.8(8) . . . . ? O7 Zn1 O1 Zn2 157.23(16) 2 . . . ? N1 C7 O2 C8 -0.2(6) . . . . ? C6 C7 O2 C8 178.2(5) . . . . ? N2 C8 O2 C7 1.0(7) . . . . ? C9 C8 O2 C7 177.0(5) . . . . ? O4 C14 O3 Zn2 2.1(8) . . . 2_656 ? C12 C14 O3 Zn2 -176.7(6) . . . 2_656 ? O3 C14 O4 Zn2 -2.0(8) . . . 2_656 ? C12 C14 O4 Zn2 176.8(7) . . . 2_656 ? C33 C28 O5 Zn1 14.8(8) . . . . ? C29 C28 O5 Zn1 -167.1(4) . . . . ? C33 C28 O5 Zn2 162.9(4) . . . . ? C29 C28 O5 Zn2 -18.9(7) . . . . ? N4 Zn1 O5 C28 -117.3(5) . . . . ? O8 Zn1 O5 C28 61.9(5) 2 . . . ? N5 Zn1 O5 C28 -27.1(5) . . . . ? O1 Zn1 O5 C28 152.9(5) . . . . ? O7 Zn1 O5 C28 56.1(7) 2 . . . ? N4 Zn1 O5 Zn2 88.8(2) . . . . ? O8 Zn1 O5 Zn2 -92.0(2) 2 . . . ? N5 Zn1 O5 Zn2 179.0(2) . . . . ? O1 Zn1 O5 Zn2 -0.9(2) . . . . ? O7 Zn1 O5 Zn2 -97.8(4) 2 . . . ? O1 Zn2 O5 C28 -154.7(4) . . . . ? N3 Zn2 O5 C28 -45.6(4) . . . . ? N1 Zn2 O5 C28 -159.9(7) . . . . ? O3 Zn2 O5 C28 52.4(4) 2_646 . . . ? O4 Zn2 O5 C28 111.0(4) 2_646 . . . ? C14 Zn2 O5 C28 82.2(4) 2_646 . . . ? O1 Zn2 O5 Zn1 1.0(2) . . . . ? N3 Zn2 O5 Zn1 110.15(19) . . . . ? N1 Zn2 O5 Zn1 -4.2(8) . . . . ? O3 Zn2 O5 Zn1 -151.89(18) 2_646 . . . ? O4 Zn2 O5 Zn1 -93.22(19) 2_646 . . . ? C14 Zn2 O5 Zn1 -122.1(2) 2_646 . . . ? N6 C35 O6 C34 0.5(7) . . . . ? C36 C35 O6 C34 179.4(6) . . . . ? N5 C34 O6 C35 1.1(6) . . . . ? C33 C34 O6 C35 -179.6(6) . . . . ? O8 C41 O7 Zn1 -1.8(8) . . . 2_545 ? C39 C41 O7 Zn1 174.5(7) . . . 2_545 ? O7 C41 O8 Zn1 2.4(10) . . . 2_545 ? C39 C41 O8 Zn1 -174.0(6) . . . 2_545 ? _chemical_absolute_configuration rmad _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.573 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.066 # start Validation Reply Form _vrf_PLAT111 ; PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry ..... 83 PerFi RESPONSE: According to this alert, we tried to solve this structure using space group P2(1)/c suggested by the program Platon.In this situation, the camphoric group is disordered. Each chiral carbon atom in the camphoric group is disordered over two positions with oposite charilities. This does not agree with the experimental fact that the ligand used is enantiomeric pure. Chiral molecules are incompatible with an inversion centre. Furthermore, this kind of model for solving the structure can not achieve the convergence of the refinement.Thus, we think the centre mentioned in this level is not the real centre of symmtry, just a pseudo centre. ; # end Validation Reply Form #===END data_compound-5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H46 Cd2 N6 O8' _chemical_formula_sum 'C44 H46 Cd2 N6 O8' _chemical_formula_weight 1011.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.2397(5) _cell_length_b 13.5650(7) _cell_length_c 15.0505(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.3840(10) _cell_angle_gamma 90.00 _cell_volume 2086.89(19) _cell_formula_units_Z 2 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 5142 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.05 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8129 _exptl_absorpt_correction_T_max 0.8461 _exptl_absorpt_process_details sadabs _exptl_special_details ; CHECKCIF shows that there is a Alert level B "PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry ..... 83 PerFi". According to this alert, we tried to solve this structure using space group P2(1)/c suggested by the program Platon.In this situation, the camphoric group is disordered. Each chiral carbon atom in the camphoric group is disordered over two positions with oposite charilities. This does not agree with the experimental fact that the ligand used is enantiomeric pure. Chiral molecules are incompatible with an inversion centre. Furthermore, this kind of model for solving the structure can not achieve the convergence of the refinement.Thus, we think the centre mentioned in this level is not the real centre of symmtry, just a pseudo centre. ; _diffrn_ambient_temperature 185(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11887 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.06 _reflns_number_total 6439 _reflns_number_gt 5174 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^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 0.03(3) _refine_ls_number_reflns 6439 _refine_ls_number_parameters 547 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.009 _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 0.26077(4) 0.56369(3) 0.18202(3) 0.03212(17) Uani 1 1 d . . . Cd2 Cd 0.23041(4) 0.76676(2) 0.32008(3) 0.03225(17) Uani 1 1 d . . . C1 C 0.3833(6) 0.7741(8) 0.1352(5) 0.0328(18) Uani 1 1 d . . . C2 C 0.4332(7) 0.7250(7) 0.0633(5) 0.038(2) Uani 1 1 d . . . H2 H 0.3977 0.6627 0.0460 0.046 Uiso 1 1 calc R . . C3 C 0.5312(7) 0.7637(9) 0.0174(5) 0.044(2) Uani 1 1 d . . . H3 H 0.5618 0.7267 -0.0308 0.053 Uiso 1 1 calc R . . C4 C 0.5884(8) 0.8529(7) 0.0364(6) 0.045(2) Uani 1 1 d . . . H4 H 0.6599 0.8768 0.0052 0.055 Uiso 1 1 calc R . . C5 C 0.5359(7) 0.9062(8) 0.1038(5) 0.045(2) Uani 1 1 d . . . H5 H 0.5700 0.9700 0.1172 0.054 Uiso 1 1 calc R . . C6 C 0.4346(7) 0.8701(7) 0.1531(5) 0.031(2) Uani 1 1 d . . . C7 C 0.3866(7) 0.9343(6) 0.2220(5) 0.0299(19) Uani 1 1 d . . . C8 C 0.3744(6) 1.0636(9) 0.3016(5) 0.0335(18) Uani 1 1 d . . . C9 C 0.4098(7) 1.1651(7) 0.3339(5) 0.040(2) Uani 1 1 d . . . H9 H 0.4187 1.2093 0.2815 0.048 Uiso 1 1 calc R . . C10 C 0.3073(6) 1.2082(5) 0.3929(5) 0.060(2) Uani 1 1 d . . . H10A H 0.2439 1.2487 0.3565 0.071 Uiso 1 1 calc R . . H10B H 0.2589 1.1543 0.4206 0.071 Uiso 1 1 calc R . . C11 C 0.3753(6) 1.2709(6) 0.4639(4) 0.0479(16) Uani 1 1 d . . . H11A H 0.3608 1.2439 0.5236 0.057 Uiso 1 1 calc R . . H11B H 0.3411 1.3392 0.4608 0.057 Uiso 1 1 calc R . . C12 C 0.5235(6) 1.2698(9) 0.4468(5) 0.0309(18) Uani 1 1 d . . . C13 C 0.5422(6) 1.1689(4) 0.3957(4) 0.0343(14) Uani 1 1 d . . . C14 C 0.6098(6) 1.2731(8) 0.5322(5) 0.0308(18) Uani 1 1 d . . . C15 C 0.5556(7) 1.3587(5) 0.3888(4) 0.0491(18) Uani 1 1 d . . . H15A H 0.5373 1.4197 0.4206 0.074 Uiso 1 1 calc R . . H15B H 0.5017 1.3562 0.3329 0.074 Uiso 1 1 calc R . . H15C H 0.6483 1.3568 0.3760 0.074 Uiso 1 1 calc R . . C16 C 0.6609(5) 1.1663(5) 0.3410(4) 0.0455(16) Uani 1 1 d . . . H16A H 0.7390 1.1827 0.3789 0.068 Uiso 1 1 calc R . . H16B H 0.6502 1.2144 0.2925 0.068 Uiso 1 1 calc R . . H16C H 0.6705 1.1002 0.3161 0.068 Uiso 1 1 calc R . . C17 C 0.5467(8) 1.0809(8) 0.4588(6) 0.053(3) Uani 1 1 d . . . H17A H 0.5547 1.0200 0.4246 0.080 Uiso 1 1 calc R . . H17B H 0.4662 1.0788 0.4909 0.080 Uiso 1 1 calc R . . H17C H 0.6222 1.0874 0.5016 0.080 Uiso 1 1 calc R . . C18 C -0.0409(9) 0.8647(8) 0.3590(6) 0.051(3) Uani 1 1 d . . . H18 H 0.0144 0.8944 0.4043 0.062 Uiso 1 1 calc R . . C19 C -0.1710(8) 0.8851(8) 0.3561(6) 0.065(3) Uani 1 1 d . . . H19 H -0.2056 0.9275 0.3991 0.078 Uiso 1 1 calc R . . C20 C -0.2511(8) 0.8441(9) 0.2909(8) 0.069(3) Uani 1 1 d . . . H20 H -0.3422 0.8577 0.2876 0.083 Uiso 1 1 calc R . . C21 C -0.1994(9) 0.7839(10) 0.2313(6) 0.064(3) Uani 1 1 d . . . H21 H -0.2539 0.7547 0.1853 0.076 Uiso 1 1 calc R . . C22 C -0.0678(7) 0.7649(10) 0.2373(5) 0.045(2) Uani 1 1 d . . . H22 H -0.0323 0.7220 0.1950 0.054 Uiso 1 1 calc R . . C23 C 0.5306(10) 0.4761(10) 0.1438(7) 0.080(4) Uani 1 1 d . . . H23 H 0.4724 0.4443 0.1014 0.096 Uiso 1 1 calc R . . C24 C 0.6602(10) 0.4560(12) 0.1396(7) 0.099(5) Uani 1 1 d . . . H24 H 0.6909 0.4127 0.0957 0.119 Uiso 1 1 calc R . . C25 C 0.7406(10) 0.4982(10) 0.1979(8) 0.084(4) Uani 1 1 d . . . H25 H 0.8321 0.4880 0.1953 0.101 Uiso 1 1 calc R . . C26 C 0.6943(8) 0.5577(11) 0.2637(7) 0.069(3) Uani 1 1 d . . . H26 H 0.7511 0.5861 0.3088 0.082 Uiso 1 1 calc R . . C27 C 0.5592(8) 0.5737(9) 0.2601(6) 0.050(2) Uani 1 1 d . . . H27 H 0.5240 0.6153 0.3035 0.060 Uiso 1 1 calc R . . C28 C 0.1002(6) 0.5593(8) 0.3631(5) 0.0295(17) Uani 1 1 d . . . C29 C 0.0502(8) 0.6112(7) 0.4357(5) 0.043(2) Uani 1 1 d . . . H29 H 0.0892 0.6726 0.4522 0.051 Uiso 1 1 calc R . . C30 C -0.0501(7) 0.5784(8) 0.4828(6) 0.047(2) Uani 1 1 d . . . H30 H -0.0807 0.6163 0.5304 0.056 Uiso 1 1 calc R . . C31 C -0.1079(8) 0.4867(7) 0.4599(6) 0.048(3) Uani 1 1 d . . . H31 H -0.1813 0.4641 0.4898 0.058 Uiso 1 1 calc R . . C32 C -0.0578(7) 0.4303(7) 0.3944(5) 0.036(2) Uani 1 1 d . . . H32 H -0.0947 0.3674 0.3810 0.044 Uiso 1 1 calc R . . C33 C 0.0475(7) 0.4644(7) 0.3464(5) 0.0307(19) Uani 1 1 d . . . C34 C 0.0984(7) 0.4017(7) 0.2805(6) 0.039(2) Uani 1 1 d . . . C35 C 0.1099(7) 0.2658(8) 0.2018(5) 0.038(2) Uani 1 1 d . . . C36 C 0.0771(7) 0.1671(6) 0.1672(5) 0.035(2) Uani 1 1 d . . . H36 H 0.1588 0.1266 0.1725 0.042 Uiso 1 1 calc R . . C37 C -0.0280(7) 0.1117(5) 0.2162(4) 0.058(2) Uani 1 1 d . . . H37A H -0.0855 0.1586 0.2458 0.070 Uiso 1 1 calc R . . H37B H 0.0127 0.0668 0.2617 0.070 Uiso 1 1 calc R . . C38 C -0.1063(8) 0.0530(6) 0.1434(4) 0.067(2) Uani 1 1 d . . . H38A H -0.1134 -0.0172 0.1606 0.080 Uiso 1 1 calc R . . H38B H -0.1955 0.0805 0.1330 0.080 Uiso 1 1 calc R . . C39 C -0.0288(6) 0.0635(10) 0.0598(5) 0.037(2) Uani 1 1 d . . . C40 C 0.0298(6) 0.1681(5) 0.0696(4) 0.0392(15) Uani 1 1 d . . . C41 C -0.1143(7) 0.0563(9) -0.0277(5) 0.037(2) Uani 1 1 d . . . C42 C 0.0738(9) -0.0176(6) 0.0571(5) 0.081(3) Uani 1 1 d . . . H42A H 0.1347 -0.0124 0.1096 0.121 Uiso 1 1 calc R . . H42B H 0.1220 -0.0105 0.0031 0.121 Uiso 1 1 calc R . . H42C H 0.0306 -0.0821 0.0568 0.121 Uiso 1 1 calc R . . C43 C -0.0770(8) 0.2448(7) 0.0516(6) 0.059(3) Uani 1 1 d . . . H43A H -0.0451 0.3095 0.0722 0.088 Uiso 1 1 calc R . . H43B H -0.1542 0.2267 0.0835 0.088 Uiso 1 1 calc R . . H43C H -0.1005 0.2476 -0.0124 0.088 Uiso 1 1 calc R . . C44 C 0.1431(7) 0.1869(7) 0.0123(4) 0.080(3) Uani 1 1 d . . . H44A H 0.1147 0.1771 -0.0504 0.120 Uiso 1 1 calc R . . H44B H 0.2144 0.1411 0.0289 0.120 Uiso 1 1 calc R . . H44C H 0.1738 0.2548 0.0211 0.120 Uiso 1 1 calc R . . N1 N 0.2940(6) 0.9199(5) 0.2757(4) 0.0352(17) Uani 1 1 d . . . N2 N 0.2859(6) 1.0074(5) 0.3278(5) 0.0388(18) Uani 1 1 d . . . N3 N 0.0126(6) 0.8051(5) 0.3011(5) 0.0345(19) Uani 1 1 d . . . N4 N 0.4798(6) 0.5338(6) 0.1994(5) 0.038(2) Uani 1 1 d . . . N5 N 0.1990(6) 0.4089(5) 0.2317(5) 0.0391(18) Uani 1 1 d . . . N6 N 0.2090(7) 0.3229(6) 0.1817(5) 0.047(2) Uani 1 1 d . . . O1 O 0.2944(5) 0.7329(4) 0.1820(3) 0.0323(14) Uani 1 1 d . . . O2 O 0.4421(5) 1.0253(4) 0.2345(4) 0.0359(15) Uani 1 1 d . . . O3 O 0.7299(4) 1.2901(4) 0.5276(3) 0.0325(14) Uani 1 1 d . . . O4 O 0.5608(5) 1.2544(6) 0.6060(3) 0.0444(16) Uani 1 1 d . . . O5 O 0.1908(5) 0.6005(4) 0.3170(3) 0.0392(16) Uani 1 1 d . . . O6 O 0.0372(5) 0.3110(4) 0.2645(4) 0.0356(15) Uani 1 1 d . . . O7 O -0.2337(5) 0.0360(5) -0.0263(4) 0.0448(18) Uani 1 1 d . . . O8 O -0.0608(5) 0.0704(7) -0.0988(3) 0.0454(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0341(3) 0.0292(4) 0.0329(4) -0.0009(3) -0.0002(3) -0.0038(3) Cd2 0.0359(3) 0.0291(4) 0.0316(4) -0.0007(3) 0.0003(3) -0.0049(3) C1 0.028(3) 0.034(5) 0.036(4) -0.001(5) 0.000(3) -0.004(4) C2 0.045(4) 0.034(5) 0.035(5) -0.001(4) -0.004(4) -0.005(4) C3 0.039(4) 0.056(6) 0.038(5) 0.000(5) 0.006(3) 0.007(5) C4 0.039(4) 0.047(6) 0.052(6) 0.008(5) 0.005(4) -0.014(4) C5 0.043(4) 0.043(6) 0.047(6) -0.002(5) -0.003(4) -0.010(4) C6 0.038(4) 0.027(5) 0.028(5) 0.004(4) 0.003(3) -0.002(3) C7 0.038(4) 0.019(5) 0.030(5) 0.002(4) -0.018(4) -0.009(3) C8 0.028(3) 0.034(5) 0.037(4) -0.011(5) -0.013(3) 0.001(4) C9 0.039(4) 0.040(6) 0.040(5) 0.005(5) -0.016(4) -0.002(4) C10 0.038(4) 0.051(4) 0.088(6) -0.024(4) -0.009(4) 0.002(3) C11 0.037(3) 0.060(5) 0.045(4) -0.003(4) -0.004(3) 0.009(4) C12 0.037(3) 0.024(5) 0.032(4) 0.000(5) 0.000(3) -0.006(5) C13 0.038(3) 0.029(3) 0.036(4) 0.001(3) 0.000(3) -0.004(3) C14 0.034(4) 0.024(5) 0.034(5) 0.005(5) 0.000(3) 0.005(5) C15 0.073(5) 0.028(4) 0.045(4) 0.002(3) -0.011(4) -0.001(3) C16 0.040(3) 0.046(4) 0.052(4) -0.016(3) 0.016(3) -0.005(3) C17 0.050(4) 0.043(6) 0.064(6) 0.011(5) -0.013(4) 0.001(4) C18 0.052(5) 0.054(6) 0.048(6) -0.020(5) 0.002(4) 0.007(5) C19 0.064(6) 0.060(6) 0.073(7) 0.003(6) 0.025(6) 0.027(5) C20 0.035(5) 0.094(9) 0.075(7) 0.036(7) -0.020(5) -0.002(5) C21 0.060(5) 0.064(8) 0.064(7) 0.002(6) -0.023(5) -0.011(6) C22 0.043(4) 0.040(5) 0.050(6) 0.009(6) -0.007(4) 0.005(5) C23 0.061(6) 0.110(11) 0.068(8) -0.017(8) -0.008(6) 0.026(7) C24 0.071(7) 0.162(14) 0.063(7) -0.028(8) -0.009(6) 0.042(8) C25 0.057(6) 0.107(11) 0.090(9) 0.026(8) 0.019(6) 0.029(6) C26 0.053(5) 0.067(7) 0.081(8) 0.035(7) -0.036(5) -0.012(6) C27 0.061(5) 0.041(6) 0.046(6) 0.003(6) -0.012(4) -0.008(5) C28 0.032(3) 0.030(5) 0.027(4) 0.010(5) -0.001(3) -0.003(4) C29 0.056(5) 0.034(6) 0.039(5) -0.004(4) 0.006(4) -0.007(4) C30 0.060(5) 0.035(6) 0.047(5) -0.002(4) 0.019(4) -0.001(4) C31 0.044(4) 0.057(7) 0.043(6) 0.012(5) 0.004(4) 0.003(4) C32 0.039(4) 0.032(5) 0.038(5) 0.012(4) -0.002(4) -0.008(3) C33 0.035(4) 0.025(5) 0.032(5) 0.000(4) 0.000(3) -0.004(4) C34 0.030(4) 0.036(6) 0.050(6) 0.011(5) 0.000(4) -0.008(4) C35 0.041(4) 0.033(5) 0.040(5) 0.019(5) 0.009(3) -0.007(5) C36 0.044(4) 0.017(5) 0.044(5) -0.005(4) -0.001(4) -0.003(4) C37 0.088(6) 0.040(4) 0.046(4) -0.004(3) -0.001(4) -0.022(4) C38 0.092(6) 0.056(5) 0.052(4) 0.001(4) 0.006(4) -0.038(5) C39 0.040(4) 0.039(5) 0.032(4) -0.002(5) -0.010(3) 0.008(5) C40 0.049(4) 0.035(4) 0.033(4) -0.001(3) -0.001(3) -0.003(3) C41 0.045(4) 0.026(5) 0.038(5) -0.002(5) -0.008(4) 0.000(5) C42 0.109(7) 0.053(5) 0.074(6) -0.034(5) -0.038(6) 0.037(5) C43 0.072(6) 0.017(5) 0.083(7) -0.001(5) -0.032(5) -0.003(4) C44 0.074(5) 0.129(8) 0.039(4) -0.006(5) 0.011(4) -0.058(6) N1 0.028(3) 0.042(5) 0.035(4) -0.002(4) 0.000(3) -0.004(3) N2 0.039(4) 0.034(5) 0.042(4) 0.002(3) -0.004(3) -0.007(3) N3 0.032(3) 0.034(5) 0.037(5) 0.001(4) -0.004(3) -0.005(3) N4 0.039(4) 0.042(5) 0.035(5) -0.004(4) 0.006(3) 0.002(3) N5 0.051(4) 0.016(4) 0.051(4) 0.000(3) 0.009(4) -0.011(3) N6 0.048(4) 0.038(5) 0.056(5) -0.018(4) 0.012(4) -0.006(4) O1 0.043(3) 0.023(4) 0.032(3) -0.004(2) 0.006(2) -0.010(2) O2 0.036(3) 0.033(4) 0.038(3) -0.001(3) -0.002(2) -0.010(2) O3 0.039(3) 0.025(4) 0.033(3) 0.001(3) -0.002(2) -0.008(2) O4 0.044(3) 0.052(4) 0.037(3) 0.010(4) 0.000(3) -0.010(4) O5 0.048(3) 0.039(4) 0.031(3) 0.002(3) 0.002(2) -0.010(3) O6 0.040(3) 0.026(3) 0.040(4) 0.001(3) 0.001(3) -0.005(2) O7 0.033(3) 0.052(5) 0.049(4) 0.008(3) -0.004(3) -0.001(3) O8 0.040(3) 0.064(4) 0.031(3) -0.003(4) -0.005(2) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O5 2.250(5) . ? Cd1 N4 2.279(7) . ? Cd1 O1 2.321(5) . ? Cd1 N5 2.328(6) . ? Cd1 O8 2.338(5) 2 ? Cd1 O7 2.374(5) 2 ? Cd1 C41 2.690(8) 2 ? Cd1 Cd2 3.4755(5) . ? Cd2 O1 2.263(5) . ? Cd2 N1 2.288(7) . ? Cd2 O5 2.291(6) . ? Cd2 N3 2.292(6) . ? Cd2 O3 2.326(5) 2_646 ? Cd2 O4 2.357(5) 2_646 ? Cd2 C14 2.683(7) 2_646 ? C1 O1 1.309(9) . ? C1 C2 1.394(11) . ? C1 C6 1.424(13) . ? C2 C3 1.357(11) . ? C2 H2 0.9500 . ? C3 C4 1.368(14) . ? C3 H3 0.9500 . ? C4 C5 1.379(12) . ? C4 H4 0.9500 . ? C5 C6 1.399(10) . ? C5 H5 0.9500 . ? C6 C7 1.460(11) . ? C7 N1 1.297(9) . ? C7 O2 1.367(9) . ? C8 N2 1.264(11) . ? C8 O2 1.362(9) . ? C8 C9 1.499(14) . ? C9 C10 1.530(10) . ? C9 C13 1.599(8) . ? C9 H9 1.0000 . ? C10 C11 1.504(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.555(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C14 1.517(9) . ? C12 C15 1.535(12) . ? C12 C13 1.586(12) . ? C13 C16 1.508(8) . ? C13 C17 1.525(11) . ? C14 O3 1.258(8) . ? C14 O4 1.271(8) . ? C14 Cd2 2.683(7) 2_656 ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N3 1.330(10) . ? C18 C19 1.359(11) . ? C18 H18 0.9500 . ? C19 C20 1.360(13) . ? C19 H19 0.9500 . ? C20 C21 1.344(16) . ? C20 H20 0.9500 . ? C21 C22 1.370(11) . ? C21 H21 0.9500 . ? C22 N3 1.343(10) . ? C22 H22 0.9500 . ? C23 N4 1.280(12) . ? C23 C24 1.360(13) . ? C23 H23 0.9500 . ? C24 C25 1.301(14) . ? C24 H24 0.9500 . ? C25 C26 1.382(17) . ? C25 H25 0.9500 . ? C26 C27 1.398(11) . ? C26 H26 0.9500 . ? C27 N4 1.304(10) . ? C27 H27 0.9500 . ? C28 O5 1.315(8) . ? C28 C33 1.412(13) . ? C28 C29 1.421(11) . ? C29 C30 1.357(11) . ? C29 H29 0.9500 . ? C30 C31 1.411(13) . ? C30 H30 0.9500 . ? C31 C32 1.371(12) . ? C31 H31 0.9500 . ? C32 C33 1.410(10) . ? C32 H32 0.9500 . ? C33 C34 1.428(12) . ? C34 N5 1.304(9) . ? C34 O6 1.395(10) . ? C35 N6 1.326(10) . ? C35 O6 1.379(10) . ? C35 C36 1.469(13) . ? C36 C40 1.519(9) . ? C36 C37 1.537(10) . ? C36 H36 1.0000 . ? C37 C38 1.542(9) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.533(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C42 1.523(12) . ? C39 C41 1.542(10) . ? C39 C40 1.544(14) . ? C40 C44 1.507(9) . ? C40 C43 1.523(10) . ? C41 O8 1.246(9) . ? C41 O7 1.254(8) . ? C41 Cd1 2.690(8) 2_545 ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? N1 N2 1.428(9) . ? N5 N6 1.395(9) . ? O3 Cd2 2.326(5) 2_656 ? O4 Cd2 2.357(5) 2_656 ? O7 Cd1 2.374(5) 2_545 ? O8 Cd1 2.338(5) 2_545 ? 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 N4 107.4(2) . . ? O5 Cd1 O1 80.54(19) . . ? N4 Cd1 O1 91.8(2) . . ? O5 Cd1 N5 78.7(2) . . ? N4 Cd1 N5 95.0(3) . . ? O1 Cd1 N5 159.2(2) . . ? O5 Cd1 O8 99.17(19) . 2 ? N4 Cd1 O8 153.3(2) . 2 ? O1 Cd1 O8 95.0(3) . 2 ? N5 Cd1 O8 87.8(3) . 2 ? O5 Cd1 O7 154.40(19) . 2 ? N4 Cd1 O7 98.2(2) . 2 ? O1 Cd1 O7 99.5(2) . 2 ? N5 Cd1 O7 99.0(2) . 2 ? O8 Cd1 O7 55.24(17) 2 2 ? O5 Cd1 C41 126.6(2) . 2 ? N4 Cd1 C41 126.0(2) . 2 ? O1 Cd1 C41 96.4(3) . 2 ? N5 Cd1 C41 95.5(3) . 2 ? O8 Cd1 C41 27.56(19) 2 2 ? O7 Cd1 C41 27.8(2) 2 2 ? O5 Cd1 Cd2 40.51(15) . . ? N4 Cd1 Cd2 101.20(19) . . ? O1 Cd1 Cd2 40.07(12) . . ? N5 Cd1 Cd2 119.15(17) . . ? O8 Cd1 Cd2 100.52(19) 2 . ? O7 Cd1 Cd2 134.95(15) 2 . ? C41 Cd1 Cd2 118.7(2) 2 . ? O1 Cd2 N1 79.3(2) . . ? O1 Cd2 O5 80.92(18) . . ? N1 Cd2 O5 160.2(2) . . ? O1 Cd2 N3 105.3(2) . . ? N1 Cd2 N3 92.8(2) . . ? O5 Cd2 N3 92.9(2) . . ? O1 Cd2 O3 152.83(18) . 2_646 ? N1 Cd2 O3 97.4(2) . 2_646 ? O5 Cd2 O3 100.01(19) . 2_646 ? N3 Cd2 O3 101.8(2) . 2_646 ? O1 Cd2 O4 96.61(19) . 2_646 ? N1 Cd2 O4 86.4(2) . 2_646 ? O5 Cd2 O4 95.4(2) . 2_646 ? N3 Cd2 O4 157.5(2) . 2_646 ? O3 Cd2 O4 56.21(16) 2_646 2_646 ? O1 Cd2 C14 124.9(2) . 2_646 ? N1 Cd2 C14 92.5(3) . 2_646 ? O5 Cd2 C14 98.4(3) . 2_646 ? N3 Cd2 C14 129.6(2) . 2_646 ? O3 Cd2 C14 27.94(18) 2_646 2_646 ? O4 Cd2 C14 28.28(18) 2_646 2_646 ? O1 Cd2 Cd1 41.31(14) . . ? N1 Cd2 Cd1 120.53(16) . . ? O5 Cd2 Cd1 39.64(13) . . ? N3 Cd2 Cd1 103.06(18) . . ? O3 Cd2 Cd1 132.88(14) 2_646 . ? O4 Cd2 Cd1 96.62(17) 2_646 . ? C14 Cd2 Cd1 116.7(2) 2_646 . ? O1 C1 C2 120.8(9) . . ? O1 C1 C6 123.4(7) . . ? C2 C1 C6 115.8(7) . . ? C3 C2 C1 121.8(9) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 123.8(9) . . ? C2 C3 H3 118.1 . . ? C4 C3 H3 118.1 . . ? C3 C4 C5 115.9(8) . . ? C3 C4 H4 122.0 . . ? C5 C4 H4 122.0 . . ? C4 C5 C6 122.7(9) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 119.8(8) . . ? C5 C6 C7 117.3(8) . . ? C1 C6 C7 122.9(7) . . ? N1 C7 O2 111.3(7) . . ? N1 C7 C6 129.9(8) . . ? O2 C7 C6 118.8(7) . . ? N2 C8 O2 114.0(9) . . ? N2 C8 C9 128.1(7) . . ? O2 C8 C9 117.9(8) . . ? C8 C9 C10 112.2(6) . . ? C8 C9 C13 113.5(7) . . ? C10 C9 C13 103.7(6) . . ? C8 C9 H9 109.1 . . ? C10 C9 H9 109.1 . . ? C13 C9 H9 109.1 . . ? C11 C10 C9 108.9(6) . . ? C11 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? C11 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C10 C11 C12 106.9(6) . . ? C10 C11 H11A 110.3 . . ? C12 C11 H11A 110.3 . . ? C10 C11 H11B 110.3 . . ? C12 C11 H11B 110.3 . . ? H11A C11 H11B 108.6 . . ? C14 C12 C15 109.0(7) . . ? C14 C12 C11 112.6(5) . . ? C15 C12 C11 109.3(7) . . ? C14 C12 C13 110.8(8) . . ? C15 C12 C13 111.5(5) . . ? C11 C12 C13 103.6(6) . . ? C16 C13 C17 109.0(6) . . ? C16 C13 C12 114.1(5) . . ? C17 C13 C12 111.9(6) . . ? C16 C13 C9 111.4(5) . . ? C17 C13 C9 109.3(6) . . ? C12 C13 C9 100.8(5) . . ? O3 C14 O4 121.5(7) . . ? O3 C14 C12 118.8(6) . . ? O4 C14 C12 119.7(6) . . ? O3 C14 Cd2 60.1(4) . 2_656 ? O4 C14 Cd2 61.4(4) . 2_656 ? C12 C14 Cd2 175.9(7) . 2_656 ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C19 122.9(9) . . ? N3 C18 H18 118.5 . . ? C19 C18 H18 118.5 . . ? C18 C19 C20 119.2(10) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C21 C20 C19 119.0(9) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 119.7(10) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? N3 C22 C21 122.0(10) . . ? N3 C22 H22 119.0 . . ? C21 C22 H22 119.0 . . ? N4 C23 C24 126.1(11) . . ? N4 C23 H23 117.0 . . ? C24 C23 H23 117.0 . . ? C25 C24 C23 117.4(12) . . ? C25 C24 H24 121.3 . . ? C23 C24 H24 121.3 . . ? C24 C25 C26 120.7(10) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C27 116.4(10) . . ? C25 C26 H26 121.8 . . ? C27 C26 H26 121.8 . . ? N4 C27 C26 122.5(10) . . ? N4 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? O5 C28 C33 124.6(8) . . ? O5 C28 C29 119.5(9) . . ? C33 C28 C29 115.9(7) . . ? C30 C29 C28 123.9(9) . . ? C30 C29 H29 118.1 . . ? C28 C29 H29 118.1 . . ? C29 C30 C31 118.7(9) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? C32 C31 C30 119.9(8) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 121.0(9) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C32 C33 C28 120.2(7) . . ? C32 C33 C34 118.8(8) . . ? C28 C33 C34 121.0(7) . . ? N5 C34 O6 109.3(8) . . ? N5 C34 C33 132.8(8) . . ? O6 C34 C33 117.8(7) . . ? N6 C35 O6 110.3(9) . . ? N6 C35 C36 127.9(8) . . ? O6 C35 C36 121.8(7) . . ? C35 C36 C40 112.8(7) . . ? C35 C36 C37 115.3(6) . . ? C40 C36 C37 106.0(6) . . ? C35 C36 H36 107.4 . . ? C40 C36 H36 107.4 . . ? C37 C36 H36 107.4 . . ? C36 C37 C38 105.1(5) . . ? C36 C37 H37A 110.7 . . ? C38 C37 H37A 110.7 . . ? C36 C37 H37B 110.7 . . ? C38 C37 H37B 110.7 . . ? H37A C37 H37B 108.8 . . ? C39 C38 C37 105.2(6) . . ? C39 C38 H38A 110.7 . . ? C37 C38 H38A 110.7 . . ? C39 C38 H38B 110.7 . . ? C37 C38 H38B 110.7 . . ? H38A C38 H38B 108.8 . . ? C42 C39 C38 110.2(8) . . ? C42 C39 C41 106.8(8) . . ? C38 C39 C41 113.5(6) . . ? C42 C39 C40 113.7(6) . . ? C38 C39 C40 103.0(7) . . ? C41 C39 C40 109.8(8) . . ? C44 C40 C36 110.0(5) . . ? C44 C40 C43 110.6(7) . . ? C36 C40 C43 111.3(6) . . ? C44 C40 C39 114.1(6) . . ? C36 C40 C39 100.6(6) . . ? C43 C40 C39 109.9(6) . . ? O8 C41 O7 121.8(7) . . ? O8 C41 C39 117.9(6) . . ? O7 C41 C39 120.3(7) . . ? O8 C41 Cd1 60.3(4) . 2_545 ? O7 C41 Cd1 61.9(4) . 2_545 ? C39 C41 Cd1 174.2(9) . 2_545 ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 H44A 109.5 . . ? C40 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C40 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C7 N1 N2 106.6(7) . . ? C7 N1 Cd2 123.3(6) . . ? N2 N1 Cd2 124.6(5) . . ? C8 N2 N1 105.3(7) . . ? C18 N3 C22 117.2(7) . . ? C18 N3 Cd2 119.5(6) . . ? C22 N3 Cd2 123.2(6) . . ? C23 N4 C27 116.8(8) . . ? C23 N4 Cd1 118.0(7) . . ? C27 N4 Cd1 125.2(6) . . ? C34 N5 N6 109.1(7) . . ? C34 N5 Cd1 119.1(6) . . ? N6 N5 Cd1 123.5(5) . . ? C35 N6 N5 106.6(7) . . ? C1 O1 Cd2 130.9(5) . . ? C1 O1 Cd1 122.1(6) . . ? Cd2 O1 Cd1 98.62(19) . . ? C8 O2 C7 102.7(7) . . ? C14 O3 Cd2 92.0(4) . 2_656 ? C14 O4 Cd2 90.3(4) . 2_656 ? C28 O5 Cd1 130.8(5) . . ? C28 O5 Cd2 122.5(6) . . ? Cd1 O5 Cd2 99.8(2) . . ? C35 O6 C34 104.8(7) . . ? C41 O7 Cd1 90.3(5) . 2_545 ? C41 O8 Cd1 92.2(4) . 2_545 ? 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 O5 Cd1 Cd2 O1 -177.0(4) . . . . ? N4 Cd1 Cd2 O1 79.2(3) . . . . ? N5 Cd1 Cd2 O1 -178.5(3) . . . . ? O8 Cd1 Cd2 O1 -85.2(3) 2 . . . ? O7 Cd1 Cd2 O1 -34.5(3) 2 . . . ? C41 Cd1 Cd2 O1 -63.0(3) 2 . . . ? O5 Cd1 Cd2 N1 -179.8(3) . . . . ? N4 Cd1 Cd2 N1 76.4(3) . . . . ? O1 Cd1 Cd2 N1 -2.8(3) . . . . ? N5 Cd1 Cd2 N1 178.7(3) . . . . ? O8 Cd1 Cd2 N1 -88.0(2) 2 . . . ? O7 Cd1 Cd2 N1 -37.3(2) 2 . . . ? C41 Cd1 Cd2 N1 -65.9(3) 2 . . . ? N4 Cd1 Cd2 O5 -103.8(3) . . . . ? O1 Cd1 Cd2 O5 177.0(4) . . . . ? N5 Cd1 Cd2 O5 -1.5(3) . . . . ? O8 Cd1 Cd2 O5 91.8(3) 2 . . . ? O7 Cd1 Cd2 O5 142.5(3) 2 . . . ? C41 Cd1 Cd2 O5 114.0(3) 2 . . . ? O5 Cd1 Cd2 N3 -78.6(3) . . . . ? N4 Cd1 Cd2 N3 177.7(3) . . . . ? O1 Cd1 Cd2 N3 98.4(3) . . . . ? N5 Cd1 Cd2 N3 -80.1(3) . . . . ? O8 Cd1 Cd2 N3 13.3(2) 2 . . . ? O7 Cd1 Cd2 N3 63.9(2) 2 . . . ? C41 Cd1 Cd2 N3 35.4(3) 2 . . . ? O5 Cd1 Cd2 O3 41.5(3) . . . 2_646 ? N4 Cd1 Cd2 O3 -62.2(2) . . . 2_646 ? O1 Cd1 Cd2 O3 -141.5(3) . . . 2_646 ? N5 Cd1 Cd2 O3 40.0(2) . . . 2_646 ? O8 Cd1 Cd2 O3 133.3(2) 2 . . 2_646 ? O7 Cd1 Cd2 O3 -176.0(3) 2 . . 2_646 ? C41 Cd1 Cd2 O3 155.5(3) 2 . . 2_646 ? O5 Cd1 Cd2 O4 90.5(3) . . . 2_646 ? N4 Cd1 Cd2 O4 -13.3(2) . . . 2_646 ? O1 Cd1 Cd2 O4 -92.5(3) . . . 2_646 ? N5 Cd1 Cd2 O4 89.0(2) . . . 2_646 ? O8 Cd1 Cd2 O4 -177.7(3) 2 . . 2_646 ? O7 Cd1 Cd2 O4 -127.0(2) 2 . . 2_646 ? C41 Cd1 Cd2 O4 -155.5(3) 2 . . 2_646 ? O5 Cd1 Cd2 C14 69.5(3) . . . 2_646 ? N4 Cd1 Cd2 C14 -34.2(3) . . . 2_646 ? O1 Cd1 Cd2 C14 -113.4(3) . . . 2_646 ? N5 Cd1 Cd2 C14 68.0(3) . . . 2_646 ? O8 Cd1 Cd2 C14 161.4(3) 2 . . 2_646 ? O7 Cd1 Cd2 C14 -148.0(3) 2 . . 2_646 ? C41 Cd1 Cd2 C14 -176.5(4) 2 . . 2_646 ? O1 C1 C2 C3 -175.8(7) . . . . ? C6 C1 C2 C3 4.4(12) . . . . ? C1 C2 C3 C4 -0.5(14) . . . . ? C2 C3 C4 C5 -3.3(13) . . . . ? C3 C4 C5 C6 3.0(13) . . . . ? C4 C5 C6 C1 1.0(13) . . . . ? C4 C5 C6 C7 -179.3(8) . . . . ? O1 C1 C6 C5 175.6(7) . . . . ? C2 C1 C6 C5 -4.6(12) . . . . ? O1 C1 C6 C7 -4.1(13) . . . . ? C2 C1 C6 C7 175.6(7) . . . . ? C5 C6 C7 N1 179.0(8) . . . . ? C1 C6 C7 N1 -1.2(14) . . . . ? C5 C6 C7 O2 0.1(11) . . . . ? C1 C6 C7 O2 179.9(7) . . . . ? N2 C8 C9 C10 -11.9(12) . . . . ? O2 C8 C9 C10 166.7(6) . . . . ? N2 C8 C9 C13 105.3(9) . . . . ? O2 C8 C9 C13 -76.1(9) . . . . ? C8 C9 C10 C11 145.4(7) . . . . ? C13 C9 C10 C11 22.5(9) . . . . ? C9 C10 C11 C12 2.0(9) . . . . ? C10 C11 C12 C14 -145.6(8) . . . . ? C10 C11 C12 C15 93.2(8) . . . . ? C10 C11 C12 C13 -25.8(8) . . . . ? C14 C12 C13 C16 -81.3(7) . . . . ? C15 C12 C13 C16 40.3(7) . . . . ? C11 C12 C13 C16 157.7(5) . . . . ? C14 C12 C13 C17 43.1(7) . . . . ? C15 C12 C13 C17 164.7(6) . . . . ? C11 C12 C13 C17 -77.9(7) . . . . ? C14 C12 C13 C9 159.2(6) . . . . ? C15 C12 C13 C9 -79.2(6) . . . . ? C11 C12 C13 C9 38.2(7) . . . . ? C8 C9 C13 C16 79.4(8) . . . . ? C10 C9 C13 C16 -158.5(6) . . . . ? C8 C9 C13 C17 -41.1(9) . . . . ? C10 C9 C13 C17 81.0(8) . . . . ? C8 C9 C13 C12 -159.2(7) . . . . ? C10 C9 C13 C12 -37.1(7) . . . . ? C15 C12 C14 O3 -46.2(12) . . . . ? C11 C12 C14 O3 -167.6(9) . . . . ? C13 C12 C14 O3 76.9(11) . . . . ? C15 C12 C14 O4 137.0(9) . . . . ? C11 C12 C14 O4 15.6(14) . . . . ? C13 C12 C14 O4 -100.0(10) . . . . ? C15 C12 C14 Cd2 -118(8) . . . 2_656 ? C11 C12 C14 Cd2 121(8) . . . 2_656 ? C13 C12 C14 Cd2 5(8) . . . 2_656 ? N3 C18 C19 C20 -0.8(17) . . . . ? C18 C19 C20 C21 0.4(18) . . . . ? C19 C20 C21 C22 0.1(19) . . . . ? C20 C21 C22 N3 -0.3(19) . . . . ? N4 C23 C24 C25 1(2) . . . . ? C23 C24 C25 C26 3(2) . . . . ? C24 C25 C26 C27 -4(2) . . . . ? C25 C26 C27 N4 1.3(18) . . . . ? O5 C28 C29 C30 174.8(8) . . . . ? C33 C28 C29 C30 -5.8(13) . . . . ? C28 C29 C30 C31 0.9(14) . . . . ? C29 C30 C31 C32 3.6(13) . . . . ? C30 C31 C32 C33 -2.8(13) . . . . ? C31 C32 C33 C28 -2.4(12) . . . . ? C31 C32 C33 C34 178.3(7) . . . . ? O5 C28 C33 C32 -174.2(7) . . . . ? C29 C28 C33 C32 6.4(11) . . . . ? O5 C28 C33 C34 5.1(12) . . . . ? C29 C28 C33 C34 -174.3(7) . . . . ? C32 C33 C34 N5 -173.7(9) . . . . ? C28 C33 C34 N5 7.0(15) . . . . ? C32 C33 C34 O6 2.5(12) . . . . ? C28 C33 C34 O6 -176.8(7) . . . . ? N6 C35 C36 C40 -69.1(11) . . . . ? O6 C35 C36 C40 112.4(8) . . . . ? N6 C35 C36 C37 168.9(8) . . . . ? O6 C35 C36 C37 -9.7(11) . . . . ? C35 C36 C37 C38 144.5(7) . . . . ? C40 C36 C37 C38 18.9(8) . . . . ? C36 C37 C38 C39 9.3(9) . . . . ? C37 C38 C39 C42 88.2(9) . . . . ? C37 C38 C39 C41 -152.0(9) . . . . ? C37 C38 C39 C40 -33.4(8) . . . . ? C35 C36 C40 C44 73.1(8) . . . . ? C37 C36 C40 C44 -159.8(6) . . . . ? C35 C36 C40 C43 -49.8(8) . . . . ? C37 C36 C40 C43 77.3(8) . . . . ? C35 C36 C40 C39 -166.2(6) . . . . ? C37 C36 C40 C39 -39.1(7) . . . . ? C42 C39 C40 C44 42.9(8) . . . . ? C38 C39 C40 C44 162.2(6) . . . . ? C41 C39 C40 C44 -76.6(7) . . . . ? C42 C39 C40 C36 -74.8(7) . . . . ? C38 C39 C40 C36 44.4(7) . . . . ? C41 C39 C40 C36 165.6(6) . . . . ? C42 C39 C40 C43 167.8(7) . . . . ? C38 C39 C40 C43 -73.0(7) . . . . ? C41 C39 C40 C43 48.2(8) . . . . ? C42 C39 C41 O8 -62.9(14) . . . . ? C38 C39 C41 O8 175.4(10) . . . . ? C40 C39 C41 O8 60.8(12) . . . . ? C42 C39 C41 O7 116.6(10) . . . . ? C38 C39 C41 O7 -5.2(16) . . . . ? C40 C39 C41 O7 -119.8(10) . . . . ? C42 C39 C41 Cd1 -133(5) . . . 2_545 ? C38 C39 C41 Cd1 106(5) . . . 2_545 ? C40 C39 C41 Cd1 -9(5) . . . 2_545 ? O2 C7 N1 N2 0.3(8) . . . . ? C6 C7 N1 N2 -178.7(7) . . . . ? O2 C7 N1 Cd2 -154.5(5) . . . . ? C6 C7 N1 Cd2 26.5(11) . . . . ? O1 Cd2 N1 C7 -31.3(6) . . . . ? O5 Cd2 N1 C7 -29.7(10) . . . . ? N3 Cd2 N1 C7 -136.3(6) . . . . ? O3 Cd2 N1 C7 121.4(6) 2_646 . . . ? O4 Cd2 N1 C7 66.2(6) 2_646 . . . ? C14 Cd2 N1 C7 93.8(6) 2_646 . . . ? Cd1 Cd2 N1 C7 -29.4(6) . . . . ? O1 Cd2 N1 N2 178.4(6) . . . . ? O5 Cd2 N1 N2 -180.0(5) . . . . ? N3 Cd2 N1 N2 73.4(5) . . . . ? O3 Cd2 N1 N2 -28.9(6) 2_646 . . . ? O4 Cd2 N1 N2 -84.1(5) 2_646 . . . ? C14 Cd2 N1 N2 -56.5(6) 2_646 . . . ? Cd1 Cd2 N1 N2 -179.7(5) . . . . ? O2 C8 N2 N1 1.5(9) . . . . ? C9 C8 N2 N1 -179.8(7) . . . . ? C7 N1 N2 C8 -1.1(9) . . . . ? Cd2 N1 N2 C8 153.3(5) . . . . ? C19 C18 N3 C22 0.6(14) . . . . ? C19 C18 N3 Cd2 -175.0(8) . . . . ? C21 C22 N3 C18 0.0(15) . . . . ? C21 C22 N3 Cd2 175.3(8) . . . . ? O1 Cd2 N3 C18 -152.9(7) . . . . ? N1 Cd2 N3 C18 -73.3(7) . . . . ? O5 Cd2 N3 C18 125.7(7) . . . . ? O3 Cd2 N3 C18 24.8(7) 2_646 . . . ? O4 Cd2 N3 C18 14.0(11) 2_646 . . . ? C14 Cd2 N3 C18 22.2(8) 2_646 . . . ? Cd1 Cd2 N3 C18 164.5(6) . . . . ? O1 Cd2 N3 C22 31.8(8) . . . . ? N1 Cd2 N3 C22 111.4(7) . . . . ? O5 Cd2 N3 C22 -49.6(7) . . . . ? O3 Cd2 N3 C22 -150.4(7) 2_646 . . . ? O4 Cd2 N3 C22 -161.3(8) 2_646 . . . ? C14 Cd2 N3 C22 -153.0(7) 2_646 . . . ? Cd1 Cd2 N3 C22 -10.8(8) . . . . ? C24 C23 N4 C27 -3.1(18) . . . . ? C24 C23 N4 Cd1 174.5(11) . . . . ? C26 C27 N4 C23 1.9(16) . . . . ? C26 C27 N4 Cd1 -175.5(8) . . . . ? O5 Cd1 N4 C23 152.9(8) . . . . ? O1 Cd1 N4 C23 -126.5(8) . . . . ? N5 Cd1 N4 C23 73.2(8) . . . . ? O8 Cd1 N4 C23 -21.8(12) 2 . . . ? O7 Cd1 N4 C23 -26.6(9) 2 . . . ? C41 Cd1 N4 C23 -27.2(10) 2 . . . ? Cd2 Cd1 N4 C23 -165.7(8) . . . . ? O5 Cd1 N4 C27 -29.7(8) . . . . ? O1 Cd1 N4 C27 51.0(8) . . . . ? N5 Cd1 N4 C27 -109.3(8) . . . . ? O8 Cd1 N4 C27 155.7(8) 2 . . . ? O7 Cd1 N4 C27 150.8(8) 2 . . . ? C41 Cd1 N4 C27 150.2(8) 2 . . . ? Cd2 Cd1 N4 C27 11.7(8) . . . . ? O6 C34 N5 N6 -0.4(10) . . . . ? C33 C34 N5 N6 176.0(9) . . . . ? O6 C34 N5 Cd1 149.0(5) . . . . ? C33 C34 N5 Cd1 -34.6(13) . . . . ? O5 Cd1 N5 C34 35.1(6) . . . . ? N4 Cd1 N5 C34 141.9(7) . . . . ? O1 Cd1 N5 C34 33.4(10) . . . . ? O8 Cd1 N5 C34 -64.7(7) 2 . . . ? O7 Cd1 N5 C34 -119.0(6) 2 . . . ? C41 Cd1 N5 C34 -91.2(7) 2 . . . ? Cd2 Cd1 N5 C34 36.1(7) . . . . ? O5 Cd1 N5 N6 179.8(7) . . . . ? N4 Cd1 N5 N6 -73.4(6) . . . . ? O1 Cd1 N5 N6 178.1(5) . . . . ? O8 Cd1 N5 N6 80.0(6) 2 . . . ? O7 Cd1 N5 N6 25.7(6) 2 . . . ? C41 Cd1 N5 N6 53.5(6) 2 . . . ? Cd2 Cd1 N5 N6 -179.2(5) . . . . ? O6 C35 N6 N5 -1.2(9) . . . . ? C36 C35 N6 N5 -179.8(8) . . . . ? C34 N5 N6 C35 1.0(10) . . . . ? Cd1 N5 N6 C35 -146.8(6) . . . . ? C2 C1 O1 Cd2 161.2(5) . . . . ? C6 C1 O1 Cd2 -19.0(12) . . . . ? C2 C1 O1 Cd1 20.2(10) . . . . ? C6 C1 O1 Cd1 -160.1(6) . . . . ? N1 Cd2 O1 C1 30.1(7) . . . . ? O5 Cd2 O1 C1 -149.3(7) . . . . ? N3 Cd2 O1 C1 120.1(7) . . . . ? O3 Cd2 O1 C1 -55.1(9) 2_646 . . . ? O4 Cd2 O1 C1 -54.9(7) 2_646 . . . ? C14 Cd2 O1 C1 -55.3(8) 2_646 . . . ? Cd1 Cd2 O1 C1 -147.4(8) . . . . ? N1 Cd2 O1 Cd1 177.5(2) . . . . ? O5 Cd2 O1 Cd1 -1.9(2) . . . . ? N3 Cd2 O1 Cd1 -92.5(2) . . . . ? O3 Cd2 O1 Cd1 92.3(4) 2_646 . . . ? O4 Cd2 O1 Cd1 92.5(2) 2_646 . . . ? C14 Cd2 O1 Cd1 92.1(3) 2_646 . . . ? O5 Cd1 O1 C1 153.3(5) . . . . ? N4 Cd1 O1 C1 45.9(5) . . . . ? N5 Cd1 O1 C1 155.0(6) . . . . ? O8 Cd1 O1 C1 -108.2(5) 2 . . . ? O7 Cd1 O1 C1 -52.7(5) 2 . . . ? C41 Cd1 O1 C1 -80.6(5) 2 . . . ? Cd2 Cd1 O1 C1 151.3(6) . . . . ? O5 Cd1 O1 Cd2 2.0(2) . . . . ? N4 Cd1 O1 Cd2 -105.4(2) . . . . ? N5 Cd1 O1 Cd2 3.7(7) . . . . ? O8 Cd1 O1 Cd2 100.47(19) 2 . . . ? O7 Cd1 O1 Cd2 156.01(17) 2 . . . ? C41 Cd1 O1 Cd2 128.1(2) 2 . . . ? N2 C8 O2 C7 -1.3(8) . . . . ? C9 C8 O2 C7 179.9(7) . . . . ? N1 C7 O2 C8 0.5(8) . . . . ? C6 C7 O2 C8 179.6(6) . . . . ? O4 C14 O3 Cd2 1.2(11) . . . 2_656 ? C12 C14 O3 Cd2 -175.6(9) . . . 2_656 ? O3 C14 O4 Cd2 -1.2(11) . . . 2_656 ? C12 C14 O4 Cd2 175.5(9) . . . 2_656 ? C33 C28 O5 Cd1 17.2(12) . . . . ? C29 C28 O5 Cd1 -163.4(5) . . . . ? C33 C28 O5 Cd2 162.1(6) . . . . ? C29 C28 O5 Cd2 -18.5(9) . . . . ? N4 Cd1 O5 C28 -122.5(7) . . . . ? O1 Cd1 O5 C28 148.6(6) . . . . ? N5 Cd1 O5 C28 -30.8(7) . . . . ? O8 Cd1 O5 C28 55.0(7) 2 . . . ? O7 Cd1 O5 C28 56.3(10) 2 . . . ? C41 Cd1 O5 C28 57.6(8) 2 . . . ? Cd2 Cd1 O5 C28 150.5(8) . . . . ? N4 Cd1 O5 Cd2 86.9(3) . . . . ? O1 Cd1 O5 Cd2 -2.0(2) . . . . ? N5 Cd1 O5 Cd2 178.7(3) . . . . ? O8 Cd1 O5 Cd2 -95.5(3) 2 . . . ? O7 Cd1 O5 Cd2 -94.3(5) 2 . . . ? C41 Cd1 O5 Cd2 -93.0(4) 2 . . . ? O1 Cd2 O5 C28 -151.8(5) . . . . ? N1 Cd2 O5 C28 -153.4(6) . . . . ? N3 Cd2 O5 C28 -46.7(5) . . . . ? O3 Cd2 O5 C28 55.8(5) 2_646 . . . ? O4 Cd2 O5 C28 112.4(5) 2_646 . . . ? C14 Cd2 O5 C28 84.0(5) 2_646 . . . ? Cd1 Cd2 O5 C28 -153.8(6) . . . . ? O1 Cd2 O5 Cd1 2.0(3) . . . . ? N1 Cd2 O5 Cd1 0.4(7) . . . . ? N3 Cd2 O5 Cd1 107.0(2) . . . . ? O3 Cd2 O5 Cd1 -150.45(18) 2_646 . . . ? O4 Cd2 O5 Cd1 -93.9(2) 2_646 . . . ? C14 Cd2 O5 Cd1 -122.2(2) 2_646 . . . ? N6 C35 O6 C34 0.9(9) . . . . ? C36 C35 O6 C34 179.7(7) . . . . ? N5 C34 O6 C35 -0.3(9) . . . . ? C33 C34 O6 C35 -177.3(7) . . . . ? O8 C41 O7 Cd1 -6.8(11) . . . 2_545 ? C39 C41 O7 Cd1 173.8(10) . . . 2_545 ? O7 C41 O8 Cd1 6.9(12) . . . 2_545 ? C39 C41 O8 Cd1 -173.7(9) . . . 2_545 ? _chemical_absolute_configuration rmad _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.369 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.071 #===END