# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Huang, Fuping' _publ_contact_author_email gxnuchem312@yahoo.com.cn _publ_author_name 'Fuping Huang' # Attachment '- 5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 801459' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H40 N14 Ni2 O15' _chemical_formula_weight 1098.74 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.368(6) _cell_length_b 11.144(2) _cell_length_c 16.695(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.37(3) _cell_angle_gamma 90.00 _cell_volume 4728.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.845 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12716 _diffrn_reflns_av_R_equivalents 0.1033 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4129 _reflns_number_gt 2689 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+40.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4129 _refine_ls_number_parameters 340 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.1399 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.1712 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.045 _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 Ni1 Ni 0.2500 0.2500 0.0000 0.0188(3) Uani 1 2 d S . . Ni2 Ni 0.2500 -0.2500 0.0000 0.0214(3) Uani 1 2 d S . . C1 C 0.2353(2) -0.0017(6) 0.0717(4) 0.0209(13) Uani 1 1 d . . . C2 C 0.2295(2) -0.0584(6) 0.1500(4) 0.0220(14) Uani 1 1 d . . . C3 C 0.2663(3) -0.1435(6) 0.2077(4) 0.0242(15) Uani 1 1 d . . . C4 C 0.3134(3) -0.1917(6) 0.1970(5) 0.0282(16) Uani 1 1 d . . . C5 C 0.1887(3) -0.0155(6) 0.1672(4) 0.0260(15) Uani 1 1 d . . . H5 H 0.1649 0.0410 0.1300 0.031 Uiso 1 1 calc R . . C6 C 0.1846(2) -0.0605(6) 0.2427(4) 0.0262(15) Uani 1 1 d . . . C7 C 0.2214(3) -0.1424(6) 0.3013(4) 0.0243(15) Uani 1 1 d . . . C8 C 0.2618(3) -0.1859(6) 0.2828(4) 0.0266(16) Uani 1 1 d . . . H8 H 0.2854 -0.2425 0.3201 0.032 Uiso 1 1 calc R . . C9 C 0.1682(3) -0.0937(6) 0.3566(4) 0.0317(17) Uani 1 1 d . . . H9 H 0.1522 -0.0893 0.3947 0.038 Uiso 1 1 calc R . . C10 C 0.3543(3) 0.0894(6) 0.0909(4) 0.0321(17) Uani 1 1 d . . . H10 H 0.3360 0.0502 0.1176 0.038 Uiso 1 1 calc R . . C11 C 0.4058(3) 0.0546(6) 0.1157(4) 0.0331(17) Uani 1 1 d . . . H11 H 0.4210 -0.0059 0.1578 0.040 Uiso 1 1 calc R . . C12 C 0.4346(3) 0.1108(6) 0.0771(4) 0.0284(16) Uani 1 1 d . . . C13 C 0.4093(3) 0.2005(7) 0.0161(5) 0.0372(19) Uani 1 1 d . . . H13 H 0.4269 0.2419 -0.0109 0.045 Uiso 1 1 calc R . . C14 C 0.3576(3) 0.2287(6) -0.0049(4) 0.0359(19) Uani 1 1 d . . . H14 H 0.3416 0.2887 -0.0471 0.043 Uiso 1 1 calc R . . C15 C 0.4896(3) 0.0805(6) 0.0984(5) 0.0332(17) Uani 1 1 d . . . C16 C 0.5635(3) 0.0928(7) 0.0951(5) 0.0354(18) Uani 1 1 d . . . C17 C 0.6084(3) 0.1294(6) 0.0759(4) 0.0286(16) Uani 1 1 d . . . C18 C 0.5993(3) 0.2153(6) 0.0101(5) 0.0371(19) Uani 1 1 d . . . H18 H 0.5663 0.2505 -0.0202 0.045 Uiso 1 1 calc R . . C19 C 0.6402(3) 0.2473(6) -0.0095(4) 0.0319(16) Uani 1 1 d . . . H19 H 0.6338 0.3054 -0.0531 0.038 Uiso 1 1 calc R . . C20 C 0.6966(3) 0.1157(6) 0.0945(4) 0.0323(17) Uani 1 1 d . . . H20 H 0.7299 0.0816 0.1240 0.039 Uiso 1 1 calc R . . C21 C 0.6581(3) 0.0785(6) 0.1176(5) 0.0350(18) Uani 1 1 d . . . H21 H 0.6653 0.0197 0.1610 0.042 Uiso 1 1 calc R . . N1 N 0.3288(2) 0.1761(5) 0.0309(3) 0.0250(13) Uani 1 1 d . . . N2 N 0.5166(2) 0.1469(5) 0.0619(4) 0.0332(14) Uani 1 1 d . . . N3 N 0.5173(2) -0.0104(6) 0.1500(4) 0.0358(14) Uani 1 1 d . . . N4 N 0.5655(2) -0.0025(5) 0.1479(4) 0.0350(14) Uani 1 1 d D . . N5 N 0.6885(2) 0.1989(5) 0.0312(4) 0.0255(13) Uani 1 1 d . . . N6 N 0.1502(2) -0.0317(5) 0.2785(3) 0.0311(14) Uani 1 1 d D . . N7 N 0.2107(2) -0.1617(5) 0.3746(3) 0.0257(13) Uani 1 1 d . . . O1 O 0.23485(17) 0.1113(4) 0.0696(3) 0.0247(10) Uani 1 1 d . . . O2 O 0.23972(17) -0.0684(4) 0.0136(3) 0.0271(11) Uani 1 1 d . . . O3 O 0.30657(17) -0.2570(4) 0.1313(3) 0.0323(11) Uani 1 1 d . . . O4 O 0.3581(2) -0.1677(5) 0.2587(4) 0.0497(15) Uani 1 1 d . . . O5 O 0.4267(3) 0.6480(6) 0.2843(6) 0.108(3) Uani 1 1 d DU . . O6 O 0.5000 0.7702(17) 0.2500 0.205(7) Uani 1 2 d SU . . O7 O 0.0536(17) 0.000(4) 0.381(3) 0.224(8) Uani 0.346(15) 1 d PU A 1 O8 O 0.514(8) 0.489(19) 0.101(12) 0.90(5) Uani 0.346(15) 1 d PU A 1 O7' O 0.5135(8) 0.607(2) 0.0328(16) 0.224(8) Uani 0.654(15) 1 d PU A 2 O8' O 0.9846(16) 0.876(3) 0.2256(14) 0.90(5) Uani 0.654(15) 1 d PU . 2 H6A H 0.5111 0.7290 0.3011 1.082 Uiso 1 1 d R . . H5A H 0.4174 0.6363 0.2301 1.082 Uiso 1 1 d RD . . H5B H 0.4132 0.7195 0.2843 1.082 Uiso 1 1 d RD . . H4 H 0.5857 -0.0700 0.1757 1.082 Uiso 1 1 d RD . . H6 H 0.1228 0.0124 0.2593 1.082 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0237(7) 0.0186(6) 0.0189(6) 0.0004(5) 0.0138(5) 0.0015(6) Ni2 0.0243(7) 0.0192(6) 0.0260(6) -0.0018(6) 0.0160(6) -0.0002(6) C1 0.020(3) 0.020(3) 0.026(3) 0.002(3) 0.013(3) 0.001(3) C2 0.025(4) 0.023(3) 0.021(3) 0.001(3) 0.014(3) 0.000(3) C3 0.027(4) 0.022(4) 0.026(4) -0.004(3) 0.013(3) -0.005(3) C4 0.032(4) 0.026(4) 0.032(4) 0.004(3) 0.018(4) 0.002(3) C5 0.033(4) 0.026(4) 0.025(3) 0.014(3) 0.018(3) 0.007(3) C6 0.028(4) 0.025(4) 0.031(4) 0.003(3) 0.018(3) 0.002(3) C7 0.032(4) 0.027(4) 0.019(3) 0.005(3) 0.015(3) 0.000(3) C8 0.032(4) 0.025(4) 0.028(3) 0.010(3) 0.018(3) 0.010(3) C9 0.039(4) 0.036(4) 0.030(4) 0.000(3) 0.023(4) -0.001(4) C10 0.024(4) 0.047(5) 0.029(4) 0.015(3) 0.016(3) 0.008(3) C11 0.034(4) 0.035(4) 0.035(4) 0.014(3) 0.019(4) 0.006(3) C12 0.028(4) 0.035(4) 0.027(4) -0.001(3) 0.016(3) 0.002(3) C13 0.032(4) 0.050(5) 0.042(4) 0.014(4) 0.027(4) 0.008(4) C14 0.038(5) 0.043(5) 0.033(4) 0.014(3) 0.023(4) 0.013(4) C15 0.028(4) 0.039(4) 0.039(4) 0.000(4) 0.021(4) -0.002(4) C16 0.029(4) 0.043(5) 0.040(4) 0.002(4) 0.021(4) 0.002(4) C17 0.030(4) 0.028(4) 0.034(4) 0.001(3) 0.020(3) 0.000(3) C18 0.024(4) 0.047(5) 0.042(4) 0.016(4) 0.016(4) 0.011(3) C19 0.028(4) 0.034(4) 0.038(4) 0.011(4) 0.019(3) 0.009(4) C20 0.022(4) 0.037(4) 0.036(4) 0.006(3) 0.011(3) 0.001(3) C21 0.031(4) 0.035(4) 0.042(4) 0.014(4) 0.019(4) 0.006(4) N1 0.025(3) 0.028(3) 0.026(3) -0.003(3) 0.016(3) 0.002(3) N2 0.023(3) 0.039(4) 0.044(4) 0.010(3) 0.021(3) 0.007(3) N3 0.023(3) 0.047(4) 0.044(3) 0.014(3) 0.021(3) 0.009(3) N4 0.026(3) 0.045(4) 0.040(3) 0.008(3) 0.020(3) 0.000(3) N5 0.028(3) 0.023(3) 0.034(3) -0.004(3) 0.021(3) -0.001(3) N6 0.033(3) 0.039(4) 0.031(3) 0.005(3) 0.023(3) 0.004(3) N7 0.031(3) 0.033(3) 0.020(3) 0.005(2) 0.017(3) 0.004(3) O1 0.037(3) 0.016(2) 0.033(2) 0.001(2) 0.027(2) 0.000(2) O2 0.041(3) 0.015(2) 0.033(3) 0.001(2) 0.024(2) 0.003(2) O3 0.031(3) 0.039(3) 0.031(3) -0.005(2) 0.017(2) 0.006(2) O4 0.028(3) 0.060(4) 0.054(3) -0.027(3) 0.012(3) -0.005(3) O5 0.079(5) 0.066(5) 0.172(6) -0.018(5) 0.048(5) -0.006(4) O6 0.186(10) 0.206(11) 0.229(11) 0.000 0.098(8) 0.000 O7 0.221(10) 0.220(10) 0.231(10) 0.007(7) 0.099(7) -0.002(7) O8 0.90(5) 0.90(5) 0.90(5) 0.000(7) 0.40(2) 0.001(7) O7' 0.221(10) 0.220(10) 0.231(10) 0.007(7) 0.099(7) -0.002(7) O8' 0.90(5) 0.90(5) 0.90(5) 0.000(7) 0.40(2) 0.001(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 Ni1 O1 2.090(4) 7 y Ni1 O1 2.090(4) . y Ni1 N7 2.126(5) 4 y Ni1 N7 2.126(5) 6 y Ni1 N1 2.217(5) . y Ni1 N1 2.217(5) 7 y Ni2 O3 2.064(4) . y Ni2 O3 2.064(4) 7_545 y Ni2 O2 2.071(4) . y Ni2 O2 2.071(4) 7_545 y Ni2 N5 2.110(5) 5_655 y Ni2 N5 2.110(5) 3_445 y C1 O1 1.260(7) . ? C1 O2 1.272(7) . ? C1 C2 1.524(8) . ? C2 C5 1.397(8) . ? C2 C3 1.423(9) . ? C3 C8 1.398(8) . ? C3 C4 1.521(9) . ? C4 O4 1.257(8) . ? C4 O3 1.259(7) . ? C5 C6 1.409(8) . ? C5 H5 0.9300 . ? C6 N6 1.390(8) . ? C6 C7 1.404(9) . ? C7 C8 1.398(8) . ? C7 N7 1.404(7) . ? C8 H8 0.9300 . ? C9 N7 1.340(8) . ? C9 N6 1.359(8) . ? C9 H9 0.9300 . ? C10 N1 1.347(8) . ? C10 C11 1.386(9) . ? C10 H10 0.9300 . ? C11 C12 1.394(9) . ? C11 H11 0.9300 . ? C12 C13 1.380(9) . ? C12 C15 1.477(9) . ? C13 C14 1.384(9) . ? C13 H13 0.9300 . ? C14 N1 1.344(8) . ? C14 H14 0.9300 . ? C15 N3 1.335(9) . ? C15 N2 1.386(8) . ? C16 N2 1.335(8) . ? C16 N4 1.365(8) . ? C16 C17 1.501(9) . ? C17 C21 1.386(9) . ? C17 C18 1.392(9) . ? C18 C19 1.384(9) . ? C18 H18 0.9300 . ? C19 N5 1.343(8) . ? C19 H19 0.9300 . ? C20 N5 1.347(8) . ? C20 C21 1.375(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? N3 N4 1.387(7) . ? N4 H4 0.9339 . ? N5 Ni2 2.110(5) 3 ? N6 H6 0.8530 . ? N7 Ni1 2.126(5) 4_545 ? O5 H5A 0.8333 . ? O5 H5B 0.8841 . ? O6 H6A 0.8932 . ? O8' O8' 0.89(6) 2_755 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O1 180.0(2) 7 . y O1 Ni1 N7 93.29(18) 7 4 y O1 Ni1 N7 86.71(18) . 4 y O1 Ni1 N7 86.71(18) 7 6 y O1 Ni1 N7 93.29(18) . 6 y N7 Ni1 N7 180.0(4) 4 6 y O1 Ni1 N1 88.23(18) 7 . y O1 Ni1 N1 91.77(18) . . y N7 Ni1 N1 84.76(19) 4 . y N7 Ni1 N1 95.24(19) 6 . y O1 Ni1 N1 91.77(18) 7 7 y O1 Ni1 N1 88.23(18) . 7 y N7 Ni1 N1 95.24(19) 4 7 y N7 Ni1 N1 84.76(19) 6 7 y N1 Ni1 N1 180.0(3) . 7 y O3 Ni2 O3 180.0(5) . 7_545 y O3 Ni2 O2 90.08(18) . . y O3 Ni2 O2 89.92(18) 7_545 . y O3 Ni2 O2 89.92(18) . 7_545 y O3 Ni2 O2 90.08(18) 7_545 7_545 y O2 Ni2 O2 180.0(2) . 7_545 y O3 Ni2 N5 86.22(19) . 5_655 y O3 Ni2 N5 93.78(19) 7_545 5_655 y O2 Ni2 N5 86.29(18) . 5_655 y O2 Ni2 N5 93.71(18) 7_545 5_655 y O3 Ni2 N5 93.78(19) . 3_445 y O3 Ni2 N5 86.22(19) 7_545 3_445 y O2 Ni2 N5 93.71(18) . 3_445 y O2 Ni2 N5 86.29(18) 7_545 3_445 y N5 Ni2 N5 180.0(3) 5_655 3_445 y O1 C1 O2 124.5(5) . . ? O1 C1 C2 115.8(5) . . ? O2 C1 C2 119.8(6) . . ? C5 C2 C3 121.0(5) . . ? C5 C2 C1 116.7(5) . . ? C3 C2 C1 122.1(5) . . ? C8 C3 C2 120.0(6) . . ? C8 C3 C4 114.9(6) . . ? C2 C3 C4 125.0(5) . . ? O4 C4 O3 123.0(6) . . ? O4 C4 C3 116.6(6) . . ? O3 C4 C3 120.2(6) . . ? C2 C5 C6 117.9(6) . . ? C2 C5 H5 121.1 . . ? C6 C5 H5 121.1 . . ? N6 C6 C7 107.4(5) . . ? N6 C6 C5 130.9(6) . . ? C7 C6 C5 121.5(6) . . ? C8 C7 N7 131.0(6) . . ? C8 C7 C6 120.0(5) . . ? N7 C7 C6 108.9(5) . . ? C3 C8 C7 119.5(6) . . ? C3 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? N7 C9 N6 114.8(5) . . ? N7 C9 H9 122.6 . . ? N6 C9 H9 122.6 . . ? N1 C10 C11 124.7(6) . . ? N1 C10 H10 117.6 . . ? C11 C10 H10 117.6 . . ? C10 C11 C12 119.5(6) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 116.6(6) . . ? C13 C12 C15 119.4(6) . . ? C11 C12 C15 124.0(6) . . ? C12 C13 C14 119.7(6) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? N1 C14 C13 125.1(6) . . ? N1 C14 H14 117.5 . . ? C13 C14 H14 117.5 . . ? N3 C15 N2 114.0(6) . . ? N3 C15 C12 125.7(6) . . ? N2 C15 C12 120.2(6) . . ? N2 C16 N4 111.5(6) . . ? N2 C16 C17 124.8(6) . . ? N4 C16 C17 123.6(6) . . ? C21 C17 C18 118.0(6) . . ? C21 C17 C16 123.4(6) . . ? C18 C17 C16 118.5(6) . . ? C19 C18 C17 118.8(6) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? N5 C19 C18 123.4(6) . . ? N5 C19 H19 118.3 . . ? C18 C19 H19 118.3 . . ? N5 C20 C21 123.2(6) . . ? N5 C20 H20 118.4 . . ? C21 C20 H20 118.4 . . ? C20 C21 C17 119.5(6) . . ? C20 C21 H21 120.2 . . ? C17 C21 H21 120.2 . . ? C14 N1 C10 114.3(6) . . ? C14 N1 Ni1 119.0(4) . . ? C10 N1 Ni1 126.3(4) . . ? C16 N2 C15 102.7(6) . . ? C15 N3 N4 103.9(5) . . ? C16 N4 N3 107.9(5) . . ? C16 N4 H4 142.0 . . ? N3 N4 H4 109.2 . . ? C19 N5 C20 117.0(6) . . ? C19 N5 Ni2 122.5(4) . 3 ? C20 N5 Ni2 120.5(4) . 3 ? C9 N6 C6 105.0(5) . . ? C9 N6 H6 123.0 . . ? C6 N6 H6 131.9 . . ? C9 N7 C7 103.9(5) . . ? C9 N7 Ni1 120.6(4) . 4_545 ? C7 N7 Ni1 135.0(4) . 4_545 ? C1 O1 Ni1 138.8(4) . . ? C1 O2 Ni2 136.1(4) . . ? C4 O3 Ni2 130.6(4) . . ? H5A O5 H5B 102.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C5 48.7(8) . . . . ? O2 C1 C2 C5 -130.7(6) . . . . ? O1 C1 C2 C3 -126.2(6) . . . . ? O2 C1 C2 C3 54.5(8) . . . . ? C5 C2 C3 C8 0.3(10) . . . . ? C1 C2 C3 C8 174.9(6) . . . . ? C5 C2 C3 C4 -177.3(6) . . . . ? C1 C2 C3 C4 -2.7(10) . . . . ? C8 C3 C4 O4 -61.3(8) . . . . ? C2 C3 C4 O4 116.4(7) . . . . ? C8 C3 C4 O3 115.3(7) . . . . ? C2 C3 C4 O3 -67.0(9) . . . . ? C3 C2 C5 C6 -0.9(9) . . . . ? C1 C2 C5 C6 -175.8(6) . . . . ? C2 C5 C6 N6 176.9(7) . . . . ? C2 C5 C6 C7 2.5(10) . . . . ? N6 C6 C7 C8 -178.9(6) . . . . ? C5 C6 C7 C8 -3.4(10) . . . . ? N6 C6 C7 N7 -1.6(7) . . . . ? C5 C6 C7 N7 174.0(6) . . . . ? C2 C3 C8 C7 -1.1(10) . . . . ? C4 C3 C8 C7 176.7(6) . . . . ? N7 C7 C8 C3 -174.1(6) . . . . ? C6 C7 C8 C3 2.6(10) . . . . ? N1 C10 C11 C12 -0.2(11) . . . . ? C10 C11 C12 C13 0.7(10) . . . . ? C10 C11 C12 C15 -179.8(7) . . . . ? C11 C12 C13 C14 -1.1(10) . . . . ? C15 C12 C13 C14 179.4(7) . . . . ? C12 C13 C14 N1 1.1(11) . . . . ? C13 C12 C15 N3 -173.9(7) . . . . ? C11 C12 C15 N3 6.5(11) . . . . ? C13 C12 C15 N2 4.3(10) . . . . ? C11 C12 C15 N2 -175.3(6) . . . . ? N2 C16 C17 C21 173.9(7) . . . . ? N4 C16 C17 C21 -7.5(11) . . . . ? N2 C16 C17 C18 -8.9(11) . . . . ? N4 C16 C17 C18 169.8(7) . . . . ? C21 C17 C18 C19 -1.1(10) . . . . ? C16 C17 C18 C19 -178.5(6) . . . . ? C17 C18 C19 N5 0.7(11) . . . . ? N5 C20 C21 C17 -1.1(11) . . . . ? C18 C17 C21 C20 1.3(10) . . . . ? C16 C17 C21 C20 178.5(7) . . . . ? C13 C14 N1 C10 -0.5(10) . . . . ? C13 C14 N1 Ni1 172.7(6) . . . . ? C11 C10 N1 C14 0.1(10) . . . . ? C11 C10 N1 Ni1 -172.5(5) . . . . ? O1 Ni1 N1 C14 -4.7(5) 7 . . . ? O1 Ni1 N1 C14 175.3(5) . . . . ? N7 Ni1 N1 C14 -98.2(5) 4 . . . ? N7 Ni1 N1 C14 81.8(5) 6 . . . ? N1 Ni1 N1 C14 98(100) 7 . . . ? O1 Ni1 N1 C10 167.6(5) 7 . . . ? O1 Ni1 N1 C10 -12.4(5) . . . . ? N7 Ni1 N1 C10 74.1(5) 4 . . . ? N7 Ni1 N1 C10 -105.9(5) 6 . . . ? N1 Ni1 N1 C10 -90(100) 7 . . . ? N4 C16 N2 C15 0.9(8) . . . . ? C17 C16 N2 C15 179.7(7) . . . . ? N3 C15 N2 C16 -0.9(8) . . . . ? C12 C15 N2 C16 -179.3(6) . . . . ? N2 C15 N3 N4 0.6(8) . . . . ? C12 C15 N3 N4 178.9(6) . . . . ? N2 C16 N4 N3 -0.6(8) . . . . ? C17 C16 N4 N3 -179.4(6) . . . . ? C15 N3 N4 C16 0.0(7) . . . . ? C18 C19 N5 C20 -0.4(10) . . . . ? C18 C19 N5 Ni2 -179.9(5) . . . 3 ? C21 C20 N5 C19 0.7(10) . . . . ? C21 C20 N5 Ni2 -179.9(5) . . . 3 ? N7 C9 N6 C6 -0.9(8) . . . . ? C7 C6 N6 C9 1.5(7) . . . . ? C5 C6 N6 C9 -173.5(7) . . . . ? N6 C9 N7 C7 0.0(8) . . . . ? N6 C9 N7 Ni1 173.0(4) . . . 4_545 ? C8 C7 N7 C9 178.0(7) . . . . ? C6 C7 N7 C9 1.0(7) . . . . ? C8 C7 N7 Ni1 6.4(11) . . . 4_545 ? C6 C7 N7 Ni1 -170.6(5) . . . 4_545 ? O2 C1 O1 Ni1 -11.2(10) . . . . ? C2 C1 O1 Ni1 169.5(4) . . . . ? O1 Ni1 O1 C1 87(100) 7 . . . ? N7 Ni1 O1 C1 -137.4(6) 4 . . . ? N7 Ni1 O1 C1 42.6(6) 6 . . . ? N1 Ni1 O1 C1 -52.7(6) . . . . ? N1 Ni1 O1 C1 127.3(6) 7 . . . ? O1 C1 O2 Ni2 172.0(4) . . . . ? C2 C1 O2 Ni2 -8.8(9) . . . . ? O3 Ni2 O2 C1 -44.3(6) . . . . ? O3 Ni2 O2 C1 135.7(6) 7_545 . . . ? O2 Ni2 O2 C1 106(100) 7_545 . . . ? N5 Ni2 O2 C1 -130.5(6) 5_655 . . . ? N5 Ni2 O2 C1 49.5(6) 3_445 . . . ? O4 C4 O3 Ni2 -146.8(5) . . . . ? C3 C4 O3 Ni2 36.8(9) . . . . ? O3 Ni2 O3 C4 -73(73) 7_545 . . . ? O2 Ni2 O3 C4 25.3(6) . . . . ? O2 Ni2 O3 C4 -154.7(6) 7_545 . . . ? N5 Ni2 O3 C4 111.6(6) 5_655 . . . ? N5 Ni2 O3 C4 -68.4(6) 3_445 . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.547 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.091 # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 852533' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H23 Co2 N5 O13' _chemical_formula_weight 635.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 23.501(5) _cell_length_b 10.181(2) _cell_length_c 10.334(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2472.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 1.417 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.675 _exptl_absorpt_correction_T_max 0.766 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7015 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 25.24 _reflns_number_total 2250 _reflns_number_gt 2131 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+0.8000P] 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 0.02(2) _refine_ls_number_reflns 2250 _refine_ls_number_parameters 173 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.716202(17) 0.98404(4) 0.55535(6) 0.01812(13) Uani 1 1 d . . . C1 C 0.80351(16) 0.9526(3) 0.7653(3) 0.0196(8) Uani 1 1 d . . . C2 C 0.83959(14) 0.8848(4) 0.6635(3) 0.0220(8) Uani 1 1 d . . . H2A H 0.8521 0.9488 0.6002 0.026 Uiso 1 1 calc R . . H2B H 0.8731 0.8476 0.7042 0.026 Uiso 1 1 calc R . . C3 C 0.80673(15) 0.7767(3) 0.5959(3) 0.0192(8) Uani 1 1 d . . . C4 C 0.64692(18) 0.8265(4) 0.7583(4) 0.0390(11) Uani 1 1 d . . . H4 H 0.6737 0.8622 0.8144 0.047 Uiso 1 1 calc R . . C5 C 0.60935(18) 0.7356(4) 0.8070(4) 0.0398(11) Uani 1 1 d . . . H5 H 0.6112 0.7121 0.8938 0.048 Uiso 1 1 calc R . . C6 C 0.56932(15) 0.6796(4) 0.7284(4) 0.0266(9) Uani 1 1 d . . . C7 C 0.56886(18) 0.7216(5) 0.6019(4) 0.0412(11) Uani 1 1 d . . . H7 H 0.5421 0.6882 0.5443 0.049 Uiso 1 1 calc R . . C8 C 0.60792(16) 0.8131(4) 0.5605(5) 0.0403(10) Uani 1 1 d . . . H8 H 0.6067 0.8394 0.4744 0.048 Uiso 1 1 calc R . . C9 C 0.52977(16) 0.5771(4) 0.7713(4) 0.0308(10) Uani 1 1 d . . . N1 N 0.64734(13) 0.8663(3) 0.6366(3) 0.0241(7) Uani 1 1 d . . . N2 N 0.51917(14) 0.5502(3) 0.8952(4) 0.0343(8) Uani 1 1 d . . . N3 N 0.5000 0.5000 0.6906(5) 0.0325(12) Uani 1 2 d S . . O1 O 0.75631(11) 1.0022(2) 0.7325(2) 0.0246(6) Uani 1 1 d . . . O2 O 0.82265(11) 0.9563(3) 0.8777(2) 0.0265(6) Uani 1 1 d . . . O3 O 0.76162(10) 0.8070(2) 0.5371(3) 0.0251(6) Uani 1 1 d . . . O4 O 0.82591(10) 0.6613(2) 0.6005(2) 0.0242(6) Uani 1 1 d . . . O5 O 0.78567(10) 1.0829(3) 0.4613(2) 0.0251(6) Uani 1 1 d . . . O6 O 0.94364(15) 0.6292(4) 0.6478(5) 0.0874(14) Uani 1 1 d U . . O7 O 0.5000 1.0000 0.8576(8) 0.143(4) Uani 1 2 d SU . . H5A H 0.7795 1.1645 0.4772 0.143 Uiso 1 1 d R . . H5B H 0.7793 1.0637 0.3871 0.143 Uiso 1 1 d R . . H6B H 0.9557 0.6001 0.7165 0.143 Uiso 1 1 d R . . H6A H 0.9105 0.6488 0.6647 0.143 Uiso 1 1 d R . . H2C H 0.5436 0.5685 0.9691 0.143 Uiso 0.50 1 d PR . . H7A H 0.4849 0.9498 0.8090 0.143 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0217(2) 0.0152(2) 0.0175(2) -0.0017(3) -0.0010(2) -0.00069(18) C1 0.025(2) 0.0115(18) 0.0218(19) -0.0009(15) 0.0016(17) -0.0049(17) C2 0.0205(17) 0.023(2) 0.0223(19) -0.0047(15) 0.0010(16) -0.0012(16) C3 0.025(2) 0.016(2) 0.0167(16) 0.0000(14) 0.0064(16) 0.0002(15) C4 0.042(3) 0.047(3) 0.028(2) 0.008(2) -0.009(2) -0.023(2) C5 0.049(3) 0.042(3) 0.028(2) 0.0100(19) -0.008(2) -0.024(2) C6 0.0215(19) 0.024(2) 0.034(2) 0.0028(17) 0.0011(19) -0.0054(16) C7 0.038(2) 0.050(3) 0.035(2) 0.002(2) -0.0103(19) -0.022(2) C8 0.039(2) 0.053(2) 0.0297(19) 0.009(3) 0.001(3) -0.018(2) C9 0.022(2) 0.032(2) 0.038(2) 0.002(2) 0.002(2) -0.0044(18) N1 0.0223(15) 0.0233(18) 0.0268(16) 0.0013(15) -0.0013(14) -0.0047(14) N2 0.0294(19) 0.035(2) 0.0381(19) 0.0038(17) -0.0003(16) -0.0154(17) N3 0.029(3) 0.030(3) 0.039(3) 0.000 0.000 -0.015(2) O1 0.0242(13) 0.0308(16) 0.0189(13) -0.0067(12) -0.0024(12) 0.0058(11) O2 0.0295(15) 0.0335(16) 0.0166(13) -0.0012(11) -0.0020(13) 0.0032(13) O3 0.0273(12) 0.0168(12) 0.0311(16) -0.0038(14) -0.0076(14) 0.0020(10) O4 0.0263(13) 0.0151(13) 0.0312(14) -0.0039(11) -0.0039(11) 0.0019(11) O5 0.0276(15) 0.0223(15) 0.0255(13) -0.0012(12) 0.0013(12) -0.0033(12) O6 0.048(2) 0.081(3) 0.133(4) -0.003(3) -0.006(3) 0.004(2) O7 0.123(7) 0.176(8) 0.131(8) 0.000 0.000 -0.034(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.067(2) . y Co1 O2 2.070(3) 8_644 y Co1 O3 2.103(2) . y Co1 O4 2.111(2) 4_655 y Co1 O5 2.150(2) . y Co1 N1 2.182(3) . y C1 O2 1.246(4) . ? C1 O1 1.265(5) . ? C1 C2 1.517(5) . ? C2 C3 1.515(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O4 1.259(4) . ? C3 O3 1.260(4) . ? C4 N1 1.321(5) . ? C4 C5 1.374(5) . ? C4 H4 0.9300 . ? C5 C6 1.367(5) . ? C5 H5 0.9300 . ? C6 C7 1.376(5) . ? C6 C9 1.465(5) . ? C7 C8 1.376(5) . ? C7 H7 0.9300 . ? C8 N1 1.330(5) . ? C8 H8 0.9300 . ? C9 N2 1.333(6) . ? C9 N3 1.342(5) . ? N2 N2 1.363(6) 2_665 ? N2 H2C 0.9734 . ? N3 C9 1.342(5) 2_665 ? O2 Co1 2.070(3) 8_645 ? O4 Co1 2.111(2) 4_645 ? O5 H5A 0.8588 . ? O5 H5B 0.8053 . ? O6 H6B 0.8199 . ? O6 H6A 0.8219 . ? O7 H7A 0.8001 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 177.16(10) . 8_644 y O1 Co1 O3 85.66(10) . . y O2 Co1 O3 91.57(10) 8_644 . y O1 Co1 O4 86.65(10) . 4_655 y O2 Co1 O4 96.09(10) 8_644 4_655 y O3 Co1 O4 172.13(11) . 4_655 y O1 Co1 O5 90.70(10) . . y O2 Co1 O5 89.88(10) 8_644 . y O3 Co1 O5 88.59(10) . . y O4 Co1 O5 93.19(10) 4_655 . y O1 Co1 N1 92.67(11) . . y O2 Co1 N1 86.51(11) 8_644 . y O3 Co1 N1 86.55(11) . . y O4 Co1 N1 92.13(10) 4_655 . y O5 Co1 N1 173.86(11) . . y O2 C1 O1 123.7(3) . . ? O2 C1 C2 117.3(3) . . ? O1 C1 C2 119.1(3) . . ? C3 C2 C1 111.4(3) . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? O4 C3 O3 123.2(3) . . ? O4 C3 C2 118.5(3) . . ? O3 C3 C2 118.3(3) . . ? N1 C4 C5 124.0(4) . . ? N1 C4 H4 118.0 . . ? C5 C4 H4 118.0 . . ? C6 C5 C4 120.4(4) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 116.1(4) . . ? C5 C6 C9 123.7(4) . . ? C7 C6 C9 120.2(4) . . ? C6 C7 C8 120.1(4) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? N1 C8 C7 123.8(4) . . ? N1 C8 H8 118.1 . . ? C7 C8 H8 118.1 . . ? N2 C9 N3 112.3(4) . . ? N2 C9 C6 123.7(4) . . ? N3 C9 C6 124.0(4) . . ? C4 N1 C8 115.6(4) . . ? C4 N1 Co1 122.7(3) . . ? C8 N1 Co1 120.9(3) . . ? C9 N2 N2 106.1(2) . 2_665 ? C9 N2 H2C 127.2 . . ? N2 N2 H2C 122.2 2_665 . ? C9 N3 C9 103.2(5) . 2_665 ? C1 O1 Co1 127.0(2) . . ? C1 O2 Co1 132.2(2) . 8_645 ? C3 O3 Co1 126.4(2) . . ? C3 O4 Co1 128.4(2) . 4_645 ? Co1 O5 H5A 103.7 . . ? Co1 O5 H5B 100.0 . . ? H5A O5 H5B 112.7 . . ? H6B O6 H6A 103.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 124.5(3) . . . . ? O1 C1 C2 C3 -55.7(4) . . . . ? C1 C2 C3 O4 -121.2(3) . . . . ? C1 C2 C3 O3 59.1(4) . . . . ? N1 C4 C5 C6 0.3(7) . . . . ? C4 C5 C6 C7 -1.2(7) . . . . ? C4 C5 C6 C9 176.7(4) . . . . ? C5 C6 C7 C8 1.2(7) . . . . ? C9 C6 C7 C8 -176.8(4) . . . . ? C6 C7 C8 N1 -0.3(7) . . . . ? C5 C6 C9 N2 16.7(7) . . . . ? C7 C6 C9 N2 -165.5(4) . . . . ? C5 C6 C9 N3 -163.5(4) . . . . ? C7 C6 C9 N3 14.3(6) . . . . ? C5 C4 N1 C8 0.6(7) . . . . ? C5 C4 N1 Co1 -169.1(4) . . . . ? C7 C8 N1 C4 -0.6(6) . . . . ? C7 C8 N1 Co1 169.3(4) . . . . ? O1 Co1 N1 C4 -5.1(3) . . . . ? O2 Co1 N1 C4 172.1(3) 8_644 . . . ? O3 Co1 N1 C4 80.3(3) . . . . ? O4 Co1 N1 C4 -91.9(3) 4_655 . . . ? O5 Co1 N1 C4 118.1(10) . . . . ? O1 Co1 N1 C8 -174.4(3) . . . . ? O2 Co1 N1 C8 2.9(3) 8_644 . . . ? O3 Co1 N1 C8 -88.9(3) . . . . ? O4 Co1 N1 C8 98.9(3) 4_655 . . . ? O5 Co1 N1 C8 -51.1(11) . . . . ? N3 C9 N2 N2 0.5(6) . . . 2_665 ? C6 C9 N2 N2 -179.7(4) . . . 2_665 ? N2 C9 N3 C9 -0.2(2) . . . 2_665 ? C6 C9 N3 C9 180.0(5) . . . 2_665 ? O2 C1 O1 Co1 -172.5(2) . . . . ? C2 C1 O1 Co1 7.7(5) . . . . ? O2 Co1 O1 C1 39(2) 8_644 . . . ? O3 Co1 O1 C1 25.7(3) . . . . ? O4 Co1 O1 C1 -156.0(3) 4_655 . . . ? O5 Co1 O1 C1 -62.8(3) . . . . ? N1 Co1 O1 C1 112.1(3) . . . . ? O1 C1 O2 Co1 21.0(5) . . . 8_645 ? C2 C1 O2 Co1 -159.3(2) . . . 8_645 ? O4 C3 O3 Co1 165.8(2) . . . . ? C2 C3 O3 Co1 -14.6(4) . . . . ? O1 Co1 O3 C3 -22.1(3) . . . . ? O2 Co1 O3 C3 158.6(3) 8_644 . . . ? O4 Co1 O3 C3 -34.4(8) 4_655 . . . ? O5 Co1 O3 C3 68.7(3) . . . . ? N1 Co1 O3 C3 -115.0(3) . . . . ? O3 C3 O4 Co1 -15.2(5) . . . 4_645 ? C2 C3 O4 Co1 165.1(2) . . . 4_645 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.491 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.074 # Attachment '- 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 852534' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H38 Co2 N10 O14' _chemical_formula_weight 1036.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.680(4) _cell_length_b 12.222(2) _cell_length_c 20.171(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.86(3) _cell_angle_gamma 90.00 _cell_volume 4335.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max 25.25 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.816 _exptl_absorpt_correction_T_max 0.903 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36048 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.25 _reflns_number_total 7842 _reflns_number_gt 6083 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+20.4736P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7842 _refine_ls_number_parameters 623 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.1627 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.986 _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 N5 N 0.5140(2) 0.2533(3) 0.5260(2) 0.0265(9) Uani 1 1 d . . . C27 C 0.5435(3) 0.2007(4) 0.4764(3) 0.0369(14) Uani 1 1 d . . . H27 H 0.5316 0.1272 0.4693 0.044 Uiso 1 1 calc R . . C28 C 0.5340(3) 0.3578(4) 0.5353(3) 0.0311(12) Uani 1 1 d . . . H28 H 0.5157 0.3954 0.5706 0.037 Uiso 1 1 calc R . . O9 O 0.54492(19) 0.7096(3) 0.34066(16) 0.0277(8) Uani 1 1 d . . . C14 C 0.4886(3) 0.6963(4) 0.2983(2) 0.0243(11) Uani 1 1 d . . . N10 N 0.7587(2) 0.7905(4) -0.1729(2) 0.0353(11) Uani 1 1 d . . . C39 C 0.6965(3) 0.7406(5) -0.1546(3) 0.0487(17) Uani 1 1 d . . . H39 H 0.6796 0.6772 -0.1768 0.058 Uiso 1 1 calc R . . C40 C 0.7805(3) 0.8822(5) -0.1406(3) 0.0404(14) Uani 1 1 d . . . H40 H 0.8234 0.9183 -0.1523 0.049 Uiso 1 1 calc R . . C41 C 0.7425(3) 0.9259(5) -0.0908(3) 0.0400(14) Uani 1 1 d . . . H41 H 0.7592 0.9909 -0.0702 0.048 Uiso 1 1 calc R . . Co1 Co 0.93053(3) 0.32695(5) 0.08514(3) 0.02033(17) Uani 1 1 d . . . Co2 Co 0.31839(4) 0.77128(7) 0.24658(3) 0.0337(2) Uani 1 1 d . . . O2 O 0.84802(18) 0.2268(3) 0.03790(16) 0.0253(7) Uani 1 1 d . . . O5 O 0.8583(2) 0.5153(4) -0.08104(18) 0.0442(11) Uani 1 1 d . . . O4 O 0.91150(19) 0.4365(3) 0.00996(18) 0.0321(9) Uani 1 1 d . . . O10 O 1.01706(19) 0.4267(3) 0.13209(17) 0.0340(9) Uani 1 1 d . . . O8 O 0.42376(18) 0.7352(3) 0.30408(17) 0.0335(9) Uani 1 1 d . . . C13 C 0.5035(3) 0.6316(4) 0.2372(2) 0.0259(11) Uani 1 1 d . . . N1 N 0.8515(2) 0.3879(3) 0.1551(2) 0.0268(9) Uani 1 1 d . . . N2 N 0.6861(3) 0.3659(4) 0.3478(2) 0.0385(12) Uani 1 1 d . . . C4 C 0.7766(3) 0.4558(4) -0.0039(2) 0.0232(10) Uani 1 1 d . . . O6 O 0.3180(2) 0.6134(4) 0.2090(2) 0.0540(12) Uani 1 1 d . . . N6 N 0.3861(2) 0.8400(4) 0.1755(2) 0.0369(11) Uani 1 1 d . . . C19 C 0.7583(3) 0.3338(4) 0.2271(3) 0.0310(12) Uani 1 1 d . . . H19 H 0.7240 0.2812 0.2385 0.037 Uiso 1 1 calc R . . O3 O 0.7425(2) 0.1708(3) -0.0174(2) 0.0512(12) Uani 1 1 d . . . N4 N 0.6739(2) 0.5214(4) 0.3987(2) 0.0318(10) Uani 1 1 d . . . N8 N 0.6502(3) 1.0059(4) 0.0154(2) 0.0386(11) Uani 1 1 d . . . O12 O 0.3065(2) 0.9325(3) 0.28947(19) 0.0429(10) Uani 1 1 d . . . N3 N 0.7181(2) 0.5434(3) 0.3492(2) 0.0321(10) Uani 1 1 d . . . O1 O 0.5109(2) 0.3793(4) 0.0447(2) 0.0558(13) Uani 1 1 d . . . C23 C 0.7238(3) 0.4476(4) 0.3203(3) 0.0294(12) Uani 1 1 d . . . C3 C 0.7451(3) 0.3560(4) 0.0132(2) 0.0207(10) Uani 1 1 d . . . C37 C 0.6799(3) 0.8733(4) -0.0716(3) 0.0300(12) Uani 1 1 d . . . C2 C 0.8547(3) 0.4679(4) -0.0272(2) 0.0239(11) Uani 1 1 d . . . N9 N 0.6019(3) 1.0155(4) 0.0629(2) 0.0429(12) Uani 1 1 d . . . C7 C 0.6330(3) 0.4533(4) 0.0416(2) 0.0272(11) Uani 1 1 d . . . C18 C 0.8008(3) 0.3165(4) 0.1742(2) 0.0282(11) Uani 1 1 d . . . H18 H 0.7937 0.2514 0.1506 0.034 Uiso 1 1 calc R . . C8 C 0.6723(3) 0.3569(4) 0.0341(2) 0.0247(11) Uani 1 1 d . . . H8 H 0.6494 0.2908 0.0433 0.030 Uiso 1 1 calc R . . C35 C 0.5627(3) 0.9234(5) 0.0566(3) 0.0342(13) Uani 1 1 d . . . C15 C 0.4491(3) 0.5672(4) 0.2016(2) 0.0276(11) Uani 1 1 d . . . C25 C 0.6082(3) 0.3607(4) 0.4433(3) 0.0303(12) Uani 1 1 d . . . C6 C 0.6645(3) 0.5516(4) 0.0240(3) 0.0316(12) Uani 1 1 d . . . H6 H 0.6385 0.6169 0.0285 0.038 Uiso 1 1 calc R . . C24 C 0.6555(3) 0.4148(4) 0.3970(3) 0.0314(12) Uani 1 1 d . . . C29 C 0.5799(3) 0.4130(4) 0.4958(3) 0.0333(13) Uani 1 1 d . . . H29 H 0.5920 0.4860 0.5046 0.040 Uiso 1 1 calc R . . N7 N 0.5824(3) 0.8563(4) 0.0078(2) 0.0389(12) Uani 1 1 d . . . C9 C 0.5571(3) 0.4463(5) 0.0682(3) 0.0326(13) Uani 1 1 d . . . C31 C 0.4551(3) 0.8062(5) 0.0817(3) 0.0356(13) Uani 1 1 d . . . H31 H 0.4623 0.7632 0.0448 0.043 Uiso 1 1 calc R . . C20 C 0.7673(3) 0.4298(4) 0.2624(3) 0.0285(12) Uani 1 1 d . . . C21 C 0.8189(3) 0.5056(4) 0.2427(3) 0.0392(14) Uani 1 1 d . . . H21 H 0.8263 0.5719 0.2651 0.047 Uiso 1 1 calc R . . C32 C 0.5014(3) 0.8963(5) 0.0977(3) 0.0344(13) Uani 1 1 d . . . C33 C 0.4870(3) 0.9580(5) 0.1527(3) 0.0469(16) Uani 1 1 d . . . H33 H 0.5157 1.0201 0.1643 0.056 Uiso 1 1 calc R . . C17 C 0.3706(4) 0.5486(5) 0.2231(3) 0.0408(15) Uani 1 1 d . . . C36 C 0.6380(3) 0.9109(4) -0.0170(3) 0.0316(12) Uani 1 1 d . . . C10 C 0.5397(3) 0.5165(4) 0.1254(2) 0.0271(11) Uani 1 1 d . . . C16 C 0.4673(3) 0.5107(4) 0.1462(2) 0.0295(12) Uani 1 1 d . . . H16 H 0.4305 0.4679 0.1224 0.035 Uiso 1 1 calc R . . O11 O 0.2190(2) 0.8060(5) 0.1860(2) 0.0628(14) Uani 1 1 d . . . H11A H 0.2090 0.8803 0.1802 0.075 Uiso 1 1 calc R . . C5 C 0.7349(3) 0.5519(4) -0.0002(3) 0.0310(12) Uani 1 1 d . . . H5 H 0.7548 0.6174 -0.0143 0.037 Uiso 1 1 calc R . . O7 O 0.3644(3) 0.4613(4) 0.2537(3) 0.0762(16) Uani 1 1 d U . . C11 C 0.5940(3) 0.5791(5) 0.1617(3) 0.0377(14) Uani 1 1 d . . . H11 H 0.6430 0.5828 0.1489 0.045 Uiso 1 1 calc R . . C22 C 0.8591(3) 0.4811(4) 0.1894(3) 0.0342(13) Uani 1 1 d . . . H22 H 0.8935 0.5327 0.1767 0.041 Uiso 1 1 calc R . . C1 C 0.7814(3) 0.2442(4) 0.0098(2) 0.0234(11) Uani 1 1 d . . . C12 C 0.5761(3) 0.6361(5) 0.2167(3) 0.0380(14) Uani 1 1 d . . . H12 H 0.6132 0.6783 0.2406 0.046 Uiso 1 1 calc R . . C26 C 0.5908(3) 0.2508(5) 0.4354(3) 0.0408(15) Uani 1 1 d . . . H26 H 0.6111 0.2106 0.4023 0.049 Uiso 1 1 calc R . . C34 C 0.4299(3) 0.9262(6) 0.1897(3) 0.0454(16) Uani 1 1 d . . . H34 H 0.4215 0.9677 0.2269 0.055 Uiso 1 1 calc R . . C38 C 0.6567(3) 0.7789(5) -0.1045(3) 0.0433(15) Uani 1 1 d . . . H38 H 0.6143 0.7412 -0.0929 0.052 Uiso 1 1 calc R . . C30 C 0.3989(3) 0.7821(5) 0.1211(3) 0.0372(13) Uani 1 1 d . . . H30 H 0.3678 0.7223 0.1097 0.045 Uiso 1 1 calc R . . C43 C 0.0947(7) 0.6834(11) 0.1836(6) 0.132(4) Uani 1 1 d U . . H43A H 0.1120 0.6355 0.2197 0.198 Uiso 1 1 calc R . . H43B H 0.0668 0.6420 0.1488 0.198 Uiso 1 1 calc R . . H43C H 0.0624 0.7387 0.1993 0.198 Uiso 1 1 calc R . . C42 C 0.1679(8) 0.7413(13) 0.1547(7) 0.156(5) Uani 1 1 d U . . H42A H 0.1966 0.6817 0.1377 0.187 Uiso 1 1 calc R . . H42B H 0.1471 0.7824 0.1159 0.187 Uiso 1 1 calc R . . O13 O 0.5724(8) 0.2028(11) 0.1415(7) 0.228(5) Uani 1 1 d U . . O14 O 0.5412(10) 0.2421(15) 0.2567(8) 0.348(10) Uani 1 1 d . . . H4A H 0.6617 0.5748 0.4208 0.417 Uiso 1 1 d R . . H8A H 0.6734 1.0552 0.0089 0.417 Uiso 1 1 d R . . H12A H 0.3186 0.9322 0.3296 0.521 Uiso 1 1 d R . . H12B H 0.2722 0.9702 0.2806 0.417 Uiso 1 1 d R . . H10A H 1.0475 0.4550 0.1056 0.417 Uiso 1 1 d R . . H10B H 1.0429 0.3863 0.1594 0.417 Uiso 1 1 d R . . H13B H 0.5795 0.1524 0.1178 0.417 Uiso 1 1 d R . . H13A H 0.5548 0.2521 0.1140 0.417 Uiso 1 1 d R . . H14A H 0.5034 0.2265 0.2733 0.417 Uiso 1 1 d R . . H14B H 0.5506 0.2303 0.2193 0.417 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N5 0.025(2) 0.029(2) 0.027(2) -0.0017(18) 0.0106(17) -0.0022(18) C27 0.045(3) 0.023(3) 0.047(3) -0.006(2) 0.026(3) -0.007(2) C28 0.036(3) 0.030(3) 0.029(3) -0.007(2) 0.016(2) -0.003(2) O9 0.0256(18) 0.036(2) 0.0224(18) -0.0087(15) 0.0049(14) -0.0002(16) C14 0.027(3) 0.025(3) 0.022(2) -0.001(2) 0.008(2) -0.007(2) N10 0.030(2) 0.046(3) 0.033(2) -0.004(2) 0.016(2) -0.010(2) C39 0.038(3) 0.053(4) 0.059(4) -0.025(3) 0.026(3) -0.020(3) C40 0.036(3) 0.048(4) 0.041(3) -0.003(3) 0.021(3) -0.015(3) C41 0.041(3) 0.036(3) 0.046(3) -0.009(3) 0.020(3) -0.015(3) Co1 0.0195(3) 0.0227(3) 0.0199(3) 0.0024(3) 0.0072(2) 0.0008(3) Co2 0.0196(4) 0.0588(5) 0.0239(4) -0.0019(3) 0.0083(3) -0.0003(3) O2 0.0256(18) 0.0209(18) 0.0292(18) -0.0015(15) 0.0019(14) 0.0006(15) O5 0.029(2) 0.070(3) 0.033(2) 0.024(2) 0.0053(17) -0.007(2) O4 0.0231(18) 0.034(2) 0.040(2) 0.0165(17) 0.0093(16) 0.0022(16) O10 0.0271(19) 0.043(2) 0.033(2) -0.0051(17) 0.0099(15) -0.0120(17) O8 0.0200(18) 0.055(2) 0.0262(19) -0.0113(17) 0.0064(14) 0.0039(17) C13 0.022(2) 0.031(3) 0.025(3) -0.007(2) 0.006(2) -0.001(2) N1 0.026(2) 0.027(2) 0.028(2) 0.0045(18) 0.0094(18) -0.0006(19) N2 0.052(3) 0.026(2) 0.043(3) -0.007(2) 0.031(2) -0.004(2) C4 0.023(2) 0.025(3) 0.023(2) 0.001(2) 0.007(2) 0.001(2) O6 0.021(2) 0.091(4) 0.052(3) -0.028(3) 0.0122(18) -0.005(2) N6 0.027(2) 0.058(3) 0.026(2) -0.004(2) 0.0049(19) 0.000(2) C19 0.032(3) 0.029(3) 0.035(3) 0.002(2) 0.017(2) -0.006(2) O3 0.038(2) 0.023(2) 0.089(3) -0.014(2) -0.010(2) -0.0053(18) N4 0.036(2) 0.028(2) 0.034(3) -0.0025(19) 0.018(2) -0.008(2) N8 0.036(3) 0.039(3) 0.044(3) -0.012(2) 0.018(2) -0.005(2) O12 0.033(2) 0.058(3) 0.040(2) 0.005(2) 0.0114(17) 0.0081(19) N3 0.037(3) 0.026(2) 0.037(3) -0.002(2) 0.023(2) -0.008(2) O1 0.028(2) 0.069(3) 0.073(3) -0.045(3) 0.020(2) -0.016(2) C23 0.034(3) 0.024(3) 0.033(3) -0.004(2) 0.017(2) -0.004(2) C3 0.020(2) 0.024(3) 0.018(2) -0.0012(19) 0.0023(18) 0.000(2) C37 0.027(3) 0.033(3) 0.032(3) 0.001(2) 0.014(2) -0.004(2) C2 0.023(3) 0.022(3) 0.028(3) 0.002(2) 0.011(2) -0.004(2) N9 0.040(3) 0.043(3) 0.049(3) -0.018(2) 0.022(2) -0.009(2) C7 0.023(3) 0.037(3) 0.023(3) -0.011(2) 0.006(2) -0.001(2) C18 0.031(3) 0.029(3) 0.027(3) -0.002(2) 0.011(2) -0.003(2) C8 0.020(2) 0.030(3) 0.025(3) -0.004(2) 0.008(2) -0.006(2) C35 0.030(3) 0.044(3) 0.031(3) -0.012(3) 0.013(2) -0.008(3) C15 0.024(3) 0.032(3) 0.029(3) -0.006(2) 0.011(2) -0.004(2) C25 0.031(3) 0.026(3) 0.037(3) -0.002(2) 0.015(2) -0.006(2) C6 0.027(3) 0.029(3) 0.039(3) -0.006(2) 0.005(2) 0.007(2) C24 0.036(3) 0.026(3) 0.036(3) -0.006(2) 0.018(2) -0.005(2) C29 0.040(3) 0.027(3) 0.036(3) -0.008(2) 0.018(2) -0.008(2) N7 0.041(3) 0.039(3) 0.040(3) -0.012(2) 0.021(2) -0.013(2) C9 0.020(3) 0.041(3) 0.038(3) -0.014(3) 0.009(2) 0.001(2) C31 0.035(3) 0.046(4) 0.027(3) -0.007(2) 0.010(2) -0.006(3) C20 0.033(3) 0.022(3) 0.034(3) 0.000(2) 0.018(2) -0.002(2) C21 0.047(3) 0.023(3) 0.052(4) -0.012(3) 0.026(3) -0.009(3) C32 0.030(3) 0.046(3) 0.029(3) -0.006(2) 0.013(2) -0.002(3) C33 0.045(4) 0.054(4) 0.045(4) -0.020(3) 0.019(3) -0.015(3) C17 0.047(4) 0.039(3) 0.040(3) -0.027(3) 0.024(3) -0.027(3) C36 0.032(3) 0.028(3) 0.038(3) -0.006(2) 0.017(2) -0.009(2) C10 0.022(3) 0.032(3) 0.028(3) -0.011(2) 0.008(2) -0.002(2) C16 0.021(3) 0.037(3) 0.031(3) -0.012(2) 0.009(2) -0.009(2) O11 0.034(2) 0.087(4) 0.063(3) 0.013(3) -0.015(2) -0.008(2) C5 0.030(3) 0.022(3) 0.042(3) 0.004(2) 0.007(2) 0.002(2) O7 0.087(3) 0.056(3) 0.095(3) -0.014(3) 0.058(3) -0.019(3) C11 0.021(3) 0.055(4) 0.039(3) -0.019(3) 0.012(2) -0.010(3) C22 0.034(3) 0.024(3) 0.048(3) -0.002(2) 0.023(3) -0.009(2) C1 0.023(3) 0.023(3) 0.025(3) 0.004(2) 0.008(2) -0.003(2) C12 0.025(3) 0.057(4) 0.033(3) -0.021(3) 0.005(2) -0.007(3) C26 0.050(4) 0.031(3) 0.047(3) -0.010(3) 0.032(3) -0.007(3) C34 0.041(3) 0.064(4) 0.034(3) -0.015(3) 0.019(3) -0.001(3) C38 0.038(3) 0.046(4) 0.051(4) -0.016(3) 0.025(3) -0.017(3) C30 0.035(3) 0.051(4) 0.027(3) -0.004(3) 0.008(2) -0.011(3) C43 0.129(6) 0.134(6) 0.135(6) -0.007(4) 0.021(4) 0.000(4) C42 0.159(7) 0.152(7) 0.158(7) -0.007(5) 0.022(5) -0.002(5) O13 0.235(7) 0.221(7) 0.232(7) 0.000(5) 0.040(5) -0.007(5) O14 0.40(3) 0.36(2) 0.30(2) -0.055(18) 0.12(2) -0.05(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N5 C28 1.333(7) . ? N5 C27 1.340(6) . ? N5 Co1 2.218(4) 4_566 ? C27 C26 1.377(7) . ? C27 H27 0.9300 . ? C28 C29 1.373(7) . ? C28 H28 0.9300 . ? O9 C14 1.255(6) . ? O9 Co1 2.086(3) 2_655 ? C14 O8 1.258(6) . ? C14 C13 1.510(7) . ? N10 C40 1.334(7) . ? N10 C39 1.342(7) . ? N10 Co2 2.161(4) 4_675 ? C39 C38 1.370(8) . ? C39 H39 0.9300 . ? C40 C41 1.371(7) . ? C40 H40 0.9300 . ? C41 C37 1.369(7) . ? C41 H41 0.9300 . ? Co1 O4 2.025(3) . y Co1 O2 2.062(3) . y Co1 O9 2.086(3) 2_645 y Co1 O10 2.104(4) . y Co1 N1 2.213(4) . y Co1 N5 2.218(4) 4_665 y Co2 O6 2.072(5) . y Co2 O11 2.078(4) . y Co2 N6 2.132(5) . y Co2 O8 2.138(4) . y Co2 N10 2.161(4) 4_576 y Co2 O12 2.170(4) . y O2 C1 1.271(6) . ? O5 C2 1.238(6) . ? O4 C2 1.250(6) . ? O10 H10A 0.8689 . ? O10 H10B 0.8396 . ? C13 C15 1.385(7) . ? C13 C12 1.389(7) . ? N1 C22 1.333(7) . ? N1 C18 1.337(6) . ? N2 C24 1.321(6) . ? N2 C23 1.351(6) . ? C4 C5 1.393(7) . ? C4 C3 1.399(7) . ? C4 C2 1.510(6) . ? O6 C17 1.233(8) . ? N6 C34 1.322(8) . ? N6 C30 1.343(7) . ? C19 C20 1.374(7) . ? C19 C18 1.381(7) . ? C19 H19 0.9300 . ? O3 C1 1.226(6) . ? N4 C24 1.343(7) . ? N4 N3 1.357(6) . ? N4 H4A 0.8307 . ? N8 C36 1.339(7) . ? N8 N9 1.351(6) . ? N8 H8A 0.7482 . ? O12 H12A 0.8151 . ? O12 H12B 0.7685 . ? N3 C23 1.316(6) . ? O1 C9 1.217(6) . ? C23 C20 1.478(7) . ? C3 C8 1.396(6) . ? C3 C1 1.514(7) . ? C37 C38 1.372(8) . ? C37 C36 1.463(7) . ? N9 C35 1.322(7) . ? C7 C6 1.386(7) . ? C7 C8 1.384(7) . ? C7 C9 1.497(7) . ? C18 H18 0.9300 . ? C8 H8 0.9300 . ? C35 N7 1.355(7) . ? C35 C32 1.468(7) . ? C15 C16 1.380(7) . ? C15 C17 1.512(7) . ? C25 C29 1.374(7) . ? C25 C26 1.383(7) . ? C25 C24 1.472(7) . ? C6 C5 1.384(7) . ? C6 H6 0.9300 . ? C29 H29 0.9300 . ? N7 C36 1.327(6) . ? C9 C10 1.495(7) . ? C31 C30 1.367(7) . ? C31 C32 1.390(8) . ? C31 H31 0.9300 . ? C20 C21 1.386(7) . ? C21 C22 1.381(7) . ? C21 H21 0.9300 . ? C32 C33 1.385(8) . ? C33 C34 1.371(8) . ? C33 H33 0.9300 . ? C17 O7 1.242(8) . ? C10 C11 1.378(7) . ? C10 C16 1.389(7) . ? C16 H16 0.9300 . ? O11 C42 1.314(14) . ? O11 H11A 0.9300 . ? C5 H5 0.9300 . ? C11 C12 1.374(7) . ? C11 H11 0.9300 . ? C22 H22 0.9300 . ? C12 H12 0.9300 . ? C26 H26 0.9300 . ? C34 H34 0.9300 . ? C38 H38 0.9300 . ? C30 H30 0.9300 . ? C43 C42 1.634(16) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? O13 H13B 0.7973 . ? O13 H13A 0.8560 . ? O14 H14A 0.8000 . ? O14 H14B 0.8000 . ? 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 C28 N5 C27 116.5(4) . . ? C28 N5 Co1 121.9(3) . 4_566 ? C27 N5 Co1 121.4(3) . 4_566 ? N5 C27 C26 122.8(5) . . ? N5 C27 H27 118.6 . . ? C26 C27 H27 118.6 . . ? N5 C28 C29 123.6(5) . . ? N5 C28 H28 118.2 . . ? C29 C28 H28 118.2 . . ? C14 O9 Co1 132.1(3) . 2_655 ? O9 C14 O8 123.7(4) . . ? O9 C14 C13 115.6(4) . . ? O8 C14 C13 120.7(4) . . ? C40 N10 C39 116.8(5) . . ? C40 N10 Co2 121.5(3) . 4_675 ? C39 N10 Co2 121.7(4) . 4_675 ? N10 C39 C38 123.0(5) . . ? N10 C39 H39 118.5 . . ? C38 C39 H39 118.5 . . ? N10 C40 C41 123.2(5) . . ? N10 C40 H40 118.4 . . ? C41 C40 H40 118.4 . . ? C37 C41 C40 119.6(5) . . ? C37 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? O4 Co1 O2 89.48(14) . . y O4 Co1 O9 176.52(14) . 2_645 y O2 Co1 O9 90.52(13) . 2_645 y O4 Co1 O10 90.65(15) . . y O2 Co1 O10 178.39(14) . . y O9 Co1 O10 89.25(14) 2_645 . y O4 Co1 N1 100.78(15) . . y O2 Co1 N1 91.82(14) . . y O9 Co1 N1 82.70(14) 2_645 . y O10 Co1 N1 89.73(15) . . y O4 Co1 N5 87.63(15) . 4_665 y O2 Co1 N5 88.11(14) . 4_665 y O9 Co1 N5 88.88(14) 2_645 4_665 y O10 Co1 N5 90.29(15) . 4_665 y N1 Co1 N5 171.58(15) . 4_665 y O6 Co2 O11 90.3(2) . . y O6 Co2 N6 95.84(18) . . y O11 Co2 N6 91.33(18) . . y O6 Co2 O8 88.65(16) . . y O11 Co2 O8 176.89(16) . . y N6 Co2 O8 85.89(16) . . y O6 Co2 N10 88.05(18) . 4_576 y O11 Co2 N10 93.69(18) . 4_576 y N6 Co2 N10 173.64(18) . 4_576 y O8 Co2 N10 89.18(16) . 4_576 y O6 Co2 O12 173.65(15) . . y O11 Co2 O12 86.47(19) . . y N6 Co2 O12 89.68(17) . . y O8 Co2 O12 94.89(14) . . y N10 Co2 O12 86.73(16) 4_576 . y C1 O2 Co1 133.3(3) . . ? C2 O4 Co1 135.5(3) . . ? Co1 O10 H10A 115.0 . . ? Co1 O10 H10B 106.1 . . ? H10A O10 H10B 107.9 . . ? C14 O8 Co2 141.2(3) . . ? C15 C13 C12 118.9(4) . . ? C15 C13 C14 123.4(4) . . ? C12 C13 C14 117.7(4) . . ? C22 N1 C18 116.3(4) . . ? C22 N1 Co1 125.6(3) . . ? C18 N1 Co1 116.8(3) . . ? C24 N2 C23 103.4(4) . . ? C5 C4 C3 119.7(4) . . ? C5 C4 C2 116.1(4) . . ? C3 C4 C2 124.2(4) . . ? C17 O6 Co2 122.7(4) . . ? C34 N6 C30 116.9(5) . . ? C34 N6 Co2 121.6(4) . . ? C30 N6 Co2 119.7(4) . . ? C20 C19 C18 119.2(5) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C24 N4 N3 109.2(4) . . ? C24 N4 H4A 134.4 . . ? N3 N4 H4A 116.1 . . ? C36 N8 N9 109.9(4) . . ? C36 N8 H8A 132.5 . . ? N9 N8 H8A 116.8 . . ? Co2 O12 H12A 111.5 . . ? Co2 O12 H12B 123.9 . . ? H12A O12 H12B 110.8 . . ? C23 N3 N4 103.1(4) . . ? N3 C23 N2 114.4(4) . . ? N3 C23 C20 123.4(4) . . ? N2 C23 C20 122.3(4) . . ? C8 C3 C4 118.1(4) . . ? C8 C3 C1 115.4(4) . . ? C4 C3 C1 126.4(4) . . ? C41 C37 C38 117.9(5) . . ? C41 C37 C36 123.5(5) . . ? C38 C37 C36 118.6(5) . . ? O5 C2 O4 124.0(4) . . ? O5 C2 C4 116.7(4) . . ? O4 C2 C4 119.1(4) . . ? C35 N9 N8 102.8(4) . . ? C6 C7 C8 119.4(4) . . ? C6 C7 C9 122.6(5) . . ? C8 C7 C9 117.9(5) . . ? N1 C18 C19 123.9(5) . . ? N1 C18 H18 118.1 . . ? C19 C18 H18 118.1 . . ? C7 C8 C3 121.9(5) . . ? C7 C8 H8 119.0 . . ? C3 C8 H8 119.0 . . ? N9 C35 N7 114.4(5) . . ? N9 C35 C32 123.3(5) . . ? N7 C35 C32 122.3(5) . . ? C16 C15 C13 119.7(4) . . ? C16 C15 C17 117.0(4) . . ? C13 C15 C17 123.1(4) . . ? C29 C25 C26 116.5(5) . . ? C29 C25 C24 123.6(5) . . ? C26 C25 C24 119.8(5) . . ? C7 C6 C5 119.5(5) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? N2 C24 N4 109.9(4) . . ? N2 C24 C25 125.2(5) . . ? N4 C24 C25 124.9(4) . . ? C28 C29 C25 120.1(5) . . ? C28 C29 H29 119.9 . . ? C25 C29 H29 119.9 . . ? C36 N7 C35 103.1(4) . . ? O1 C9 C10 120.2(4) . . ? O1 C9 C7 119.4(4) . . ? C10 C9 C7 120.4(4) . . ? C30 C31 C32 118.7(5) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? C19 C20 C21 117.8(5) . . ? C19 C20 C23 119.6(4) . . ? C21 C20 C23 122.6(5) . . ? C22 C21 C20 119.0(5) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C33 C32 C31 117.7(5) . . ? C33 C32 C35 122.4(5) . . ? C31 C32 C35 119.9(5) . . ? C34 C33 C32 119.2(6) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? O6 C17 O7 124.3(6) . . ? O6 C17 C15 122.0(6) . . ? O7 C17 C15 113.7(6) . . ? N7 C36 N8 109.8(4) . . ? N7 C36 C37 125.3(5) . . ? N8 C36 C37 124.9(5) . . ? C11 C10 C16 118.7(4) . . ? C11 C10 C9 122.8(4) . . ? C16 C10 C9 118.2(4) . . ? C15 C16 C10 121.2(5) . . ? C15 C16 H16 119.4 . . ? C10 C16 H16 119.4 . . ? C42 O11 Co2 131.2(8) . . ? C42 O11 H11A 114.4 . . ? Co2 O11 H11A 114.4 . . ? C6 C5 C4 121.2(5) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C12 C11 C10 120.4(5) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? N1 C22 C21 123.9(5) . . ? N1 C22 H22 118.1 . . ? C21 C22 H22 118.1 . . ? O3 C1 O2 122.0(5) . . ? O3 C1 C3 117.4(4) . . ? O2 C1 C3 120.5(4) . . ? C11 C12 C13 121.0(5) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C27 C26 C25 120.2(5) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? N6 C34 C33 123.7(5) . . ? N6 C34 H34 118.2 . . ? C33 C34 H34 118.2 . . ? C39 C38 C37 119.5(5) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? N6 C30 C31 123.7(5) . . ? N6 C30 H30 118.1 . . ? C31 C30 H30 118.1 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O11 C42 C43 128.2(12) . . ? O11 C42 H42A 105.2 . . ? C43 C42 H42A 105.2 . . ? O11 C42 H42B 105.2 . . ? C43 C42 H42B 105.2 . . ? H42A C42 H42B 106.0 . . ? H13B O13 H13A 103.0 . . ? H14A O14 H14B 127.9 . . ? 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 C28 N5 C27 C26 -1.5(9) . . . . ? Co1 N5 C27 C26 174.8(5) 4_566 . . . ? C27 N5 C28 C29 2.4(8) . . . . ? Co1 N5 C28 C29 -173.8(4) 4_566 . . . ? Co1 O9 C14 O8 -21.7(7) 2_655 . . . ? Co1 O9 C14 C13 156.8(3) 2_655 . . . ? C40 N10 C39 C38 -1.0(10) . . . . ? Co2 N10 C39 C38 -178.8(5) 4_675 . . . ? C39 N10 C40 C41 -0.1(9) . . . . ? Co2 N10 C40 C41 177.7(5) 4_675 . . . ? N10 C40 C41 C37 1.3(10) . . . . ? O4 Co1 O2 C1 -45.1(4) . . . . ? O9 Co1 O2 C1 138.4(4) 2_645 . . . ? O10 Co1 O2 C1 -140(5) . . . . ? N1 Co1 O2 C1 55.7(4) . . . . ? N5 Co1 O2 C1 -132.7(4) 4_665 . . . ? O2 Co1 O4 C2 34.7(5) . . . . ? O9 Co1 O4 C2 125(2) 2_645 . . . ? O10 Co1 O4 C2 -146.9(5) . . . . ? N1 Co1 O4 C2 -57.0(5) . . . . ? N5 Co1 O4 C2 122.9(5) 4_665 . . . ? O9 C14 O8 Co2 162.7(4) . . . . ? C13 C14 O8 Co2 -15.8(8) . . . . ? O6 Co2 O8 C14 50.5(6) . . . . ? O11 Co2 O8 C14 -19(4) . . . . ? N6 Co2 O8 C14 -45.5(6) . . . . ? N10 Co2 O8 C14 138.5(6) 4_576 . . . ? O12 Co2 O8 C14 -134.8(6) . . . . ? O9 C14 C13 C15 149.6(5) . . . . ? O8 C14 C13 C15 -31.8(8) . . . . ? O9 C14 C13 C12 -29.3(7) . . . . ? O8 C14 C13 C12 149.3(5) . . . . ? O4 Co1 N1 C22 -69.1(4) . . . . ? O2 Co1 N1 C22 -158.9(4) . . . . ? O9 Co1 N1 C22 110.8(4) 2_645 . . . ? O10 Co1 N1 C22 21.5(4) . . . . ? N5 Co1 N1 C22 111.7(11) 4_665 . . . ? O4 Co1 N1 C18 124.7(4) . . . . ? O2 Co1 N1 C18 34.9(4) . . . . ? O9 Co1 N1 C18 -55.4(4) 2_645 . . . ? O10 Co1 N1 C18 -144.7(4) . . . . ? N5 Co1 N1 C18 -54.5(12) 4_665 . . . ? O11 Co2 O6 C17 173.9(5) . . . . ? N6 Co2 O6 C17 82.5(5) . . . . ? O8 Co2 O6 C17 -3.2(5) . . . . ? N10 Co2 O6 C17 -92.4(5) 4_576 . . . ? O12 Co2 O6 C17 -127.2(14) . . . . ? O6 Co2 N6 C34 -152.1(5) . . . . ? O11 Co2 N6 C34 117.5(5) . . . . ? O8 Co2 N6 C34 -63.9(5) . . . . ? N10 Co2 N6 C34 -24.6(19) 4_576 . . . ? O12 Co2 N6 C34 31.1(5) . . . . ? O6 Co2 N6 C30 12.4(4) . . . . ? O11 Co2 N6 C30 -78.0(4) . . . . ? O8 Co2 N6 C30 100.6(4) . . . . ? N10 Co2 N6 C30 139.8(15) 4_576 . . . ? O12 Co2 N6 C30 -164.5(4) . . . . ? C24 N4 N3 C23 -0.1(6) . . . . ? N4 N3 C23 N2 0.3(6) . . . . ? N4 N3 C23 C20 179.9(5) . . . . ? C24 N2 C23 N3 -0.3(7) . . . . ? C24 N2 C23 C20 180.0(5) . . . . ? C5 C4 C3 C8 -0.4(7) . . . . ? C2 C4 C3 C8 179.9(4) . . . . ? C5 C4 C3 C1 177.8(5) . . . . ? C2 C4 C3 C1 -1.9(8) . . . . ? C40 C41 C37 C38 -1.3(9) . . . . ? C40 C41 C37 C36 177.0(6) . . . . ? Co1 O4 C2 O5 -160.5(4) . . . . ? Co1 O4 C2 C4 24.3(7) . . . . ? C5 C4 C2 O5 -54.1(6) . . . . ? C3 C4 C2 O5 125.6(5) . . . . ? C5 C4 C2 O4 121.4(5) . . . . ? C3 C4 C2 O4 -58.9(7) . . . . ? C36 N8 N9 C35 0.4(6) . . . . ? C22 N1 C18 C19 -1.2(8) . . . . ? Co1 N1 C18 C19 166.4(4) . . . . ? C20 C19 C18 N1 0.5(8) . . . . ? C6 C7 C8 C3 4.1(7) . . . . ? C9 C7 C8 C3 -176.4(4) . . . . ? C4 C3 C8 C7 -3.6(7) . . . . ? C1 C3 C8 C7 178.0(4) . . . . ? N8 N9 C35 N7 -0.6(7) . . . . ? N8 N9 C35 C32 -179.2(5) . . . . ? C12 C13 C15 C16 -1.1(8) . . . . ? C14 C13 C15 C16 180.0(5) . . . . ? C12 C13 C15 C17 174.4(6) . . . . ? C14 C13 C15 C17 -4.6(8) . . . . ? C8 C7 C6 C5 -0.5(8) . . . . ? C9 C7 C6 C5 -179.9(5) . . . . ? C23 N2 C24 N4 0.3(6) . . . . ? C23 N2 C24 C25 -179.7(5) . . . . ? N3 N4 C24 N2 -0.1(7) . . . . ? N3 N4 C24 C25 179.9(5) . . . . ? C29 C25 C24 N2 177.1(6) . . . . ? C26 C25 C24 N2 -2.1(9) . . . . ? C29 C25 C24 N4 -2.9(9) . . . . ? C26 C25 C24 N4 177.9(6) . . . . ? N5 C28 C29 C25 -0.1(9) . . . . ? C26 C25 C29 C28 -3.1(8) . . . . ? C24 C25 C29 C28 177.7(5) . . . . ? N9 C35 N7 C36 0.5(7) . . . . ? C32 C35 N7 C36 179.2(5) . . . . ? C6 C7 C9 O1 131.9(6) . . . . ? C8 C7 C9 O1 -47.5(8) . . . . ? C6 C7 C9 C10 -51.4(7) . . . . ? C8 C7 C9 C10 129.2(5) . . . . ? C18 C19 C20 C21 0.4(8) . . . . ? C18 C19 C20 C23 -178.2(5) . . . . ? N3 C23 C20 C19 -167.1(5) . . . . ? N2 C23 C20 C19 12.6(8) . . . . ? N3 C23 C20 C21 14.4(9) . . . . ? N2 C23 C20 C21 -165.9(6) . . . . ? C19 C20 C21 C22 -0.7(9) . . . . ? C23 C20 C21 C22 177.9(5) . . . . ? C30 C31 C32 C33 -1.0(9) . . . . ? C30 C31 C32 C35 179.4(5) . . . . ? N9 C35 C32 C33 -9.4(9) . . . . ? N7 C35 C32 C33 172.1(6) . . . . ? N9 C35 C32 C31 170.2(6) . . . . ? N7 C35 C32 C31 -8.3(9) . . . . ? C31 C32 C33 C34 1.9(9) . . . . ? C35 C32 C33 C34 -178.5(6) . . . . ? Co2 O6 C17 O7 116.6(6) . . . . ? Co2 O6 C17 C15 -66.1(6) . . . . ? C16 C15 C17 O6 -99.7(6) . . . . ? C13 C15 C17 O6 84.7(7) . . . . ? C16 C15 C17 O7 77.8(7) . . . . ? C13 C15 C17 O7 -97.8(6) . . . . ? C35 N7 C36 N8 -0.2(6) . . . . ? C35 N7 C36 C37 179.7(5) . . . . ? N9 N8 C36 N7 -0.1(7) . . . . ? N9 N8 C36 C37 180.0(5) . . . . ? C41 C37 C36 N7 -172.3(6) . . . . ? C38 C37 C36 N7 6.1(9) . . . . ? C41 C37 C36 N8 7.6(9) . . . . ? C38 C37 C36 N8 -174.0(6) . . . . ? O1 C9 C10 C11 167.9(6) . . . . ? C7 C9 C10 C11 -8.7(8) . . . . ? O1 C9 C10 C16 -6.3(8) . . . . ? C7 C9 C10 C16 177.1(5) . . . . ? C13 C15 C16 C10 0.3(8) . . . . ? C17 C15 C16 C10 -175.5(5) . . . . ? C11 C10 C16 C15 0.9(8) . . . . ? C9 C10 C16 C15 175.3(5) . . . . ? O6 Co2 O11 C42 17.9(10) . . . . ? N6 Co2 O11 C42 113.8(10) . . . . ? O8 Co2 O11 C42 87(4) . . . . ? N10 Co2 O11 C42 -70.1(10) 4_576 . . . ? O12 Co2 O11 C42 -156.6(10) . . . . ? C7 C6 C5 C4 -3.5(8) . . . . ? C3 C4 C5 C6 4.0(8) . . . . ? C2 C4 C5 C6 -176.3(5) . . . . ? C16 C10 C11 C12 -1.2(9) . . . . ? C9 C10 C11 C12 -175.4(6) . . . . ? C18 N1 C22 C21 0.9(8) . . . . ? Co1 N1 C22 C21 -165.4(5) . . . . ? C20 C21 C22 N1 0.0(9) . . . . ? Co1 O2 C1 O3 177.7(4) . . . . ? Co1 O2 C1 C3 -6.7(7) . . . . ? C8 C3 C1 O3 46.7(6) . . . . ? C4 C3 C1 O3 -131.6(5) . . . . ? C8 C3 C1 O2 -129.0(5) . . . . ? C4 C3 C1 O2 52.7(7) . . . . ? C10 C11 C12 C13 0.4(9) . . . . ? C15 C13 C12 C11 0.8(9) . . . . ? C14 C13 C12 C11 179.8(5) . . . . ? N5 C27 C26 C25 -1.7(10) . . . . ? C29 C25 C26 C27 3.9(9) . . . . ? C24 C25 C26 C27 -176.8(6) . . . . ? C30 N6 C34 C33 -0.7(9) . . . . ? Co2 N6 C34 C33 164.2(5) . . . . ? C32 C33 C34 N6 -1.1(10) . . . . ? N10 C39 C38 C37 1.0(11) . . . . ? C41 C37 C38 C39 0.3(9) . . . . ? C36 C37 C38 C39 -178.2(6) . . . . ? C34 N6 C30 C31 1.7(9) . . . . ? Co2 N6 C30 C31 -163.5(5) . . . . ? C32 C31 C30 N6 -0.8(9) . . . . ? Co2 O11 C42 C43 84.8(16) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.993 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.085 # Attachment '- 4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 852535' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H18 N5 Ni O8' _chemical_formula_weight 479.05 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7520(18) _cell_length_b 10.915(2) _cell_length_c 11.035(2) _cell_angle_alpha 76.85(3) _cell_angle_beta 77.91(3) _cell_angle_gamma 67.61(3) _cell_volume 940.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 494 _exptl_absorpt_coefficient_mu 1.092 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8182 _exptl_absorpt_correction_T_max 0.9496 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6610 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4193 _reflns_number_gt 3446 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4193 _refine_ls_number_parameters 283 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.082 _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 Ni1 Ni 0.5000 0.5000 0.5000 0.01555(15) Uani 1 2 d S . . Ni2 Ni 0.5000 0.0000 0.5000 0.01710(15) Uani 1 2 d S . . O4 O 0.8911(3) 0.0000(4) 0.1981(2) 0.0467(8) Uani 1 1 d . . . O5 O 0.3231(3) 0.4212(2) 0.6079(2) 0.0250(5) Uani 1 1 d . . . O1 O 0.6679(3) 0.3128(2) 0.4810(2) 0.0189(5) Uani 1 1 d . . . O3 O 0.6756(3) -0.0067(2) 0.3415(2) 0.0265(5) Uani 1 1 d . . . O2 O 0.5311(3) 0.1686(2) 0.5327(2) 0.0226(5) Uani 1 1 d . . . C1 C 0.6626(4) 0.1961(3) 0.5044(3) 0.0152(6) Uani 1 1 d . . . C2 C 0.8337(3) 0.0875(3) 0.5012(3) 0.0142(6) Uani 1 1 d . . . C4 C 0.8170(4) 0.0045(3) 0.3079(3) 0.0211(7) Uani 1 1 d . . . C15 C -0.2016(4) 0.7656(3) -0.4112(3) 0.0224(7) Uani 1 1 d . . . H15A H -0.1948 0.7426 -0.4888 0.027 Uiso 1 1 calc R . . C14 C -0.0789(4) 0.6883(3) -0.3369(3) 0.0233(7) Uani 1 1 d . . . H14A H 0.0097 0.6159 -0.3648 0.028 Uiso 1 1 calc R . . N5 N -0.3297(3) 0.8721(3) -0.3767(2) 0.0190(5) Uani 1 1 d . . . C16 C -0.3390(4) 0.9016(3) -0.2633(3) 0.0245(7) Uani 1 1 d . . . H16A H -0.4285 0.9749 -0.2379 0.029 Uiso 1 1 calc R . . C17 C -0.2239(4) 0.8296(4) -0.1830(3) 0.0263(7) Uani 1 1 d . . . H17A H -0.2355 0.8537 -0.1050 0.032 Uiso 1 1 calc R . . C13 C -0.0892(4) 0.7200(3) -0.2196(3) 0.0198(6) Uani 1 1 d . . . N1 N 0.3863(3) 0.5023(3) 0.3466(2) 0.0194(5) Uani 1 1 d . . . C10 C 0.2331(4) 0.5888(3) 0.3319(3) 0.0245(7) Uani 1 1 d . . . H10A H 0.1732 0.6375 0.3962 0.029 Uiso 1 1 calc R . . C6 C 0.4657(4) 0.4253(3) 0.2575(3) 0.0228(7) Uani 1 1 d . . . H6 H 0.5695 0.3596 0.2687 0.027 Uiso 1 1 calc R . . N4 N 0.1655(3) 0.5319(3) -0.1734(2) 0.0229(6) Uani 1 1 d . . . N3 N 0.2522(3) 0.4838(3) -0.0748(2) 0.0235(6) Uani 1 1 d . . . C5 C 1.0739(4) -0.0754(3) 0.4059(3) 0.0163(6) Uani 1 1 d . . . N2 N 0.0398(3) 0.6586(3) -0.0216(2) 0.0222(6) Uani 1 1 d . . . C11 C 0.1774(4) 0.5597(3) 0.0149(3) 0.0210(7) Uani 1 1 d . . . C8 C 0.2456(4) 0.5353(3) 0.1318(3) 0.0212(7) Uani 1 1 d . . . C9 C 0.1582(4) 0.6103(3) 0.2276(3) 0.0249(7) Uani 1 1 d . . . H9A H 0.0518 0.6734 0.2209 0.030 Uiso 1 1 calc R . . C3 C 0.9093(4) 0.0092(3) 0.4058(3) 0.0158(6) Uani 1 1 d . . . C7 C 0.3999(4) 0.4394(3) 0.1502(3) 0.0245(7) Uani 1 1 d . . . H7 H 0.4592 0.3845 0.0903 0.029 Uiso 1 1 calc R . . C12 C 0.0391(4) 0.6372(3) -0.1383(3) 0.0208(7) Uani 1 1 d . . . O8 O 0.2023(4) 0.9106(4) 0.0455(3) 0.0735(12) Uani 1 1 d . . . O7 O 0.4954(4) 0.7432(4) 0.1132(4) 0.0720(11) Uani 1 1 d . . . O6 O 0.2524(5) 0.1956(3) 0.8431(4) 0.0683(10) Uani 1 1 d D . . H7B H 0.5111 0.7928 0.1554 0.082 Uiso 1 1 d R . . H5A H 0.3693 0.3321 0.6210 0.082 Uiso 1 1 d R . . H5 H 1.1187 -0.1278 0.3466 0.082 Uiso 1 1 d R . . H8A H 0.1191 0.9316 0.0959 0.082 Uiso 1 1 d R . . H6A H 0.1711 0.1930 0.8946 0.082 Uiso 1 1 d RD . . H8B H 0.1837 0.9217 -0.0153 0.082 Uiso 1 1 d R . . H3 H 0.3372 0.4112 -0.0774 0.082 Uiso 1 1 d R . . H7A H 0.4099 0.7957 0.0885 0.082 Uiso 1 1 d R . . H5B H 0.2737 0.4478 0.6749 0.082 Uiso 1 1 d R . . H6B H 0.2377 0.1975 0.7649 0.082 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0156(3) 0.0135(3) 0.0168(3) -0.0031(2) -0.0060(2) -0.0020(2) Ni2 0.0152(3) 0.0168(3) 0.0204(3) -0.0023(2) -0.0080(2) -0.0043(2) O4 0.0298(14) 0.095(2) 0.0191(13) -0.0173(14) -0.0012(11) -0.0228(16) O5 0.0251(12) 0.0244(12) 0.0230(12) -0.0046(10) -0.0004(9) -0.0068(10) O1 0.0188(11) 0.0120(10) 0.0247(11) -0.0022(8) -0.0065(9) -0.0025(9) O3 0.0209(12) 0.0395(14) 0.0241(12) -0.0075(10) -0.0067(9) -0.0129(11) O2 0.0143(11) 0.0171(11) 0.0372(13) -0.0084(10) -0.0046(9) -0.0038(9) C1 0.0161(14) 0.0165(14) 0.0137(13) -0.0069(11) -0.0076(11) -0.0013(12) C2 0.0120(13) 0.0121(13) 0.0192(14) -0.0026(11) -0.0042(11) -0.0037(11) C4 0.0188(15) 0.0246(16) 0.0199(15) -0.0066(13) -0.0060(12) -0.0042(13) C15 0.0243(16) 0.0264(17) 0.0179(15) -0.0018(13) -0.0092(12) -0.0082(14) C14 0.0196(16) 0.0234(17) 0.0221(16) -0.0017(13) -0.0079(13) -0.0008(13) N5 0.0176(13) 0.0198(13) 0.0200(13) -0.0010(10) -0.0095(10) -0.0046(11) C16 0.0218(16) 0.0257(17) 0.0240(17) -0.0059(13) -0.0089(13) -0.0021(14) C17 0.0276(18) 0.0308(18) 0.0211(16) -0.0081(14) -0.0082(13) -0.0060(15) C13 0.0192(15) 0.0220(16) 0.0182(15) 0.0027(12) -0.0087(12) -0.0074(13) N1 0.0212(13) 0.0189(13) 0.0192(13) -0.0017(10) -0.0088(10) -0.0058(11) C10 0.0246(17) 0.0243(17) 0.0257(17) -0.0076(14) -0.0100(13) -0.0046(14) C6 0.0185(15) 0.0239(16) 0.0232(16) -0.0018(13) -0.0079(12) -0.0030(13) N4 0.0198(13) 0.0280(15) 0.0176(13) -0.0018(11) -0.0097(11) -0.0021(12) N3 0.0190(13) 0.0310(15) 0.0192(13) -0.0046(11) -0.0082(11) -0.0041(12) C5 0.0154(14) 0.0159(14) 0.0180(14) -0.0040(11) -0.0049(11) -0.0039(12) N2 0.0224(14) 0.0247(14) 0.0201(13) -0.0033(11) -0.0089(11) -0.0060(11) C11 0.0204(16) 0.0243(16) 0.0186(15) -0.0018(12) -0.0064(12) -0.0069(13) C8 0.0234(16) 0.0230(16) 0.0189(15) 0.0004(12) -0.0081(12) -0.0094(13) C9 0.0198(16) 0.0243(17) 0.0281(17) -0.0055(14) -0.0117(13) 0.0001(13) C3 0.0151(14) 0.0136(14) 0.0192(15) -0.0023(11) -0.0041(11) -0.0049(11) C7 0.0240(17) 0.0278(18) 0.0197(16) -0.0047(13) -0.0062(13) -0.0049(14) C12 0.0204(15) 0.0276(17) 0.0161(15) 0.0006(13) -0.0075(12) -0.0098(14) O8 0.0355(17) 0.114(3) 0.0417(19) -0.007(2) -0.0138(14) 0.0070(19) O7 0.0400(19) 0.052(2) 0.111(3) -0.016(2) -0.0223(19) 0.0049(16) O6 0.078(3) 0.057(2) 0.085(3) -0.0218(19) -0.038(2) -0.020(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 2.039(2) 2_666 y Ni1 O1 2.039(2) . y Ni1 O5 2.081(2) 2_666 y Ni1 O5 2.081(2) . y Ni1 N1 2.127(3) 2_666 y Ni1 N1 2.127(3) . y Ni2 O3 2.068(2) 2_656 y Ni2 O3 2.068(2) . y Ni2 O2 2.077(2) . y Ni2 O2 2.077(2) 2_656 y Ni2 N5 2.103(3) 2_565 y Ni2 N5 2.103(3) 1_646 y O4 C4 1.251(4) . ? O5 H5A 0.8895 . ? O5 H5B 0.8280 . ? O1 C1 1.258(4) . ? O3 C4 1.259(4) . ? O2 C1 1.258(4) . ? C1 C2 1.515(4) . ? C2 C5 1.389(4) 2_756 ? C2 C3 1.401(4) . ? C4 C3 1.499(4) . ? C15 N5 1.335(4) . ? C15 C14 1.379(4) . ? C15 H15A 0.9300 . ? C14 C13 1.390(5) . ? C14 H14A 0.9300 . ? N5 C16 1.340(4) . ? N5 Ni2 2.103(3) 1_464 ? C16 C17 1.369(5) . ? C16 H16A 0.9300 . ? C17 C13 1.390(5) . ? C17 H17A 0.9300 . ? C13 C12 1.471(4) . ? N1 C10 1.331(4) . ? N1 C6 1.343(4) . ? C10 C9 1.373(5) . ? C10 H10A 0.9300 . ? C6 C7 1.376(5) . ? C6 H6 0.9300 . ? N4 C12 1.322(4) . ? N4 N3 1.348(4) . ? N3 C11 1.335(4) . ? N3 H3 0.8574 . ? C5 C3 1.384(4) . ? C5 C2 1.389(4) 2_756 ? C5 H5 0.8946 . ? N2 C11 1.339(4) . ? N2 C12 1.362(4) . ? C11 C8 1.463(4) . ? C8 C7 1.379(5) . ? C8 C9 1.396(5) . ? C9 H9A 0.9300 . ? C7 H7 0.9300 . ? O8 H8A 0.8077 . ? O8 H8B 0.6968 . ? O7 H7B 0.8522 . ? O7 H7A 0.8072 . ? O6 H6A 0.8183 . ? O6 H6B 0.8932 . ? 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 O1 180.000(1) 2_666 . y O1 Ni1 O5 91.66(9) 2_666 2_666 y O1 Ni1 O5 88.34(9) . 2_666 y O1 Ni1 O5 88.34(9) 2_666 . y O1 Ni1 O5 91.66(9) . . y O5 Ni1 O5 180.00(11) 2_666 . y O1 Ni1 N1 90.83(10) 2_666 2_666 y O1 Ni1 N1 89.17(10) . 2_666 y O5 Ni1 N1 84.13(10) 2_666 2_666 y O5 Ni1 N1 95.87(10) . 2_666 y O1 Ni1 N1 89.17(10) 2_666 . y O1 Ni1 N1 90.83(10) . . y O5 Ni1 N1 95.87(10) 2_666 . y O5 Ni1 N1 84.13(10) . . y N1 Ni1 N1 180.000(1) 2_666 . y O3 Ni2 O3 180.0 2_656 . y O3 Ni2 O2 90.01(10) 2_656 . y O3 Ni2 O2 89.99(10) . . y O3 Ni2 O2 89.99(10) 2_656 2_656 y O3 Ni2 O2 90.01(10) . 2_656 y O2 Ni2 O2 180.0 . 2_656 y O3 Ni2 N5 95.55(10) 2_656 2_565 y O3 Ni2 N5 84.45(10) . 2_565 y O2 Ni2 N5 88.34(10) . 2_565 y O2 Ni2 N5 91.66(10) 2_656 2_565 y O3 Ni2 N5 84.45(10) 2_656 1_646 y O3 Ni2 N5 95.55(10) . 1_646 y O2 Ni2 N5 91.66(10) . 1_646 y O2 Ni2 N5 88.34(10) 2_656 1_646 y N5 Ni2 N5 180.0 2_565 1_646 y Ni1 O5 H5A 108.4 . . ? Ni1 O5 H5B 119.8 . . ? H5A O5 H5B 109.9 . . ? C1 O1 Ni1 135.37(19) . . ? C4 O3 Ni2 138.9(2) . . ? C1 O2 Ni2 126.49(19) . . ? O2 C1 O1 125.0(3) . . ? O2 C1 C2 121.9(3) . . ? O1 C1 C2 113.1(2) . . ? C5 C2 C3 118.6(3) 2_756 . ? C5 C2 C1 116.3(3) 2_756 . ? C3 C2 C1 124.8(3) . . ? O4 C4 O3 123.1(3) . . ? O4 C4 C3 117.8(3) . . ? O3 C4 C3 118.8(3) . . ? N5 C15 C14 122.9(3) . . ? N5 C15 H15A 118.6 . . ? C14 C15 H15A 118.6 . . ? C15 C14 C13 119.2(3) . . ? C15 C14 H14A 120.4 . . ? C13 C14 H14A 120.4 . . ? C15 N5 C16 117.5(3) . . ? C15 N5 Ni2 121.8(2) . 1_464 ? C16 N5 Ni2 120.4(2) . 1_464 ? N5 C16 C17 123.5(3) . . ? N5 C16 H16A 118.3 . . ? C17 C16 H16A 118.3 . . ? C16 C17 C13 119.0(3) . . ? C16 C17 H17A 120.5 . . ? C13 C17 H17A 120.5 . . ? C17 C13 C14 117.9(3) . . ? C17 C13 C12 122.2(3) . . ? C14 C13 C12 119.9(3) . . ? C10 N1 C6 117.1(3) . . ? C10 N1 Ni1 119.8(2) . . ? C6 N1 Ni1 123.0(2) . . ? N1 C10 C9 124.0(3) . . ? N1 C10 H10A 118.0 . . ? C9 C10 H10A 118.0 . . ? N1 C6 C7 122.7(3) . . ? N1 C6 H6 118.6 . . ? C7 C6 H6 118.6 . . ? C12 N4 N3 103.7(3) . . ? C11 N3 N4 109.8(3) . . ? C11 N3 H3 132.0 . . ? N4 N3 H3 118.1 . . ? C3 C5 C2 122.2(3) . 2_756 ? C3 C5 H5 118.0 . . ? C2 C5 H5 119.7 2_756 . ? C11 N2 C12 102.9(3) . . ? N3 C11 N2 109.9(3) . . ? N3 C11 C8 122.6(3) . . ? N2 C11 C8 127.5(3) . . ? C7 C8 C9 117.8(3) . . ? C7 C8 C11 121.1(3) . . ? C9 C8 C11 121.1(3) . . ? C10 C9 C8 118.5(3) . . ? C10 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? C5 C3 C2 119.1(3) . . ? C5 C3 C4 117.6(3) . . ? C2 C3 C4 123.1(3) . . ? C6 C7 C8 119.7(3) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? N4 C12 N2 113.7(3) . . ? N4 C12 C13 121.7(3) . . ? N2 C12 C13 124.6(3) . . ? H8A O8 H8B 112.1 . . ? H7B O7 H7A 98.2 . . ? H6A O6 H6B 112.7 . . ? 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 O1 Ni1 O1 C1 122(100) 2_666 . . . ? O5 Ni1 O1 C1 -169.1(3) 2_666 . . . ? O5 Ni1 O1 C1 10.9(3) . . . . ? N1 Ni1 O1 C1 106.8(3) 2_666 . . . ? N1 Ni1 O1 C1 -73.2(3) . . . . ? O3 Ni2 O3 C4 -70(100) 2_656 . . . ? O2 Ni2 O3 C4 44.1(3) . . . . ? O2 Ni2 O3 C4 -135.9(3) 2_656 . . . ? N5 Ni2 O3 C4 132.4(4) 2_565 . . . ? N5 Ni2 O3 C4 -47.6(4) 1_646 . . . ? O3 Ni2 O2 C1 149.4(3) 2_656 . . . ? O3 Ni2 O2 C1 -30.6(3) . . . . ? O2 Ni2 O2 C1 31(100) 2_656 . . . ? N5 Ni2 O2 C1 -115.0(3) 2_565 . . . ? N5 Ni2 O2 C1 65.0(3) 1_646 . . . ? Ni2 O2 C1 O1 152.2(2) . . . . ? Ni2 O2 C1 C2 -30.6(4) . . . . ? Ni1 O1 C1 O2 11.4(5) . . . . ? Ni1 O1 C1 C2 -165.98(19) . . . . ? O2 C1 C2 C5 -110.8(3) . . . 2_756 ? O1 C1 C2 C5 66.7(3) . . . 2_756 ? O2 C1 C2 C3 75.7(4) . . . . ? O1 C1 C2 C3 -106.8(3) . . . . ? Ni2 O3 C4 O4 -177.1(3) . . . . ? Ni2 O3 C4 C3 9.4(5) . . . . ? N5 C15 C14 C13 1.3(5) . . . . ? C14 C15 N5 C16 -1.6(5) . . . . ? C14 C15 N5 Ni2 173.2(2) . . . 1_464 ? C15 N5 C16 C17 0.8(5) . . . . ? Ni2 N5 C16 C17 -174.0(3) 1_464 . . . ? N5 C16 C17 C13 0.1(5) . . . . ? C16 C17 C13 C14 -0.4(5) . . . . ? C16 C17 C13 C12 -179.6(3) . . . . ? C15 C14 C13 C17 -0.3(5) . . . . ? C15 C14 C13 C12 179.0(3) . . . . ? O1 Ni1 N1 C10 -18.4(2) 2_666 . . . ? O1 Ni1 N1 C10 161.6(2) . . . . ? O5 Ni1 N1 C10 -110.0(2) 2_666 . . . ? O5 Ni1 N1 C10 70.0(2) . . . . ? N1 Ni1 N1 C10 122(100) 2_666 . . . ? O1 Ni1 N1 C6 157.4(3) 2_666 . . . ? O1 Ni1 N1 C6 -22.6(3) . . . . ? O5 Ni1 N1 C6 65.8(3) 2_666 . . . ? O5 Ni1 N1 C6 -114.2(3) . . . . ? N1 Ni1 N1 C6 -63(100) 2_666 . . . ? C6 N1 C10 C9 -5.1(5) . . . . ? Ni1 N1 C10 C9 171.0(3) . . . . ? C10 N1 C6 C7 4.6(5) . . . . ? Ni1 N1 C6 C7 -171.3(2) . . . . ? C12 N4 N3 C11 0.0(4) . . . . ? N4 N3 C11 N2 0.3(4) . . . . ? N4 N3 C11 C8 -177.8(3) . . . . ? C12 N2 C11 N3 -0.5(3) . . . . ? C12 N2 C11 C8 177.4(3) . . . . ? N3 C11 C8 C7 6.1(5) . . . . ? N2 C11 C8 C7 -171.7(3) . . . . ? N3 C11 C8 C9 -175.3(3) . . . . ? N2 C11 C8 C9 6.9(5) . . . . ? N1 C10 C9 C8 1.5(5) . . . . ? C7 C8 C9 C10 2.7(5) . . . . ? C11 C8 C9 C10 -175.9(3) . . . . ? C2 C5 C3 C2 1.2(5) 2_756 . . . ? C2 C5 C3 C4 -174.3(3) 2_756 . . . ? C5 C2 C3 C5 -1.2(5) 2_756 . . . ? C1 C2 C3 C5 172.2(3) . . . . ? C5 C2 C3 C4 174.1(3) 2_756 . . . ? C1 C2 C3 C4 -12.5(5) . . . . ? O4 C4 C3 C5 -43.4(4) . . . . ? O3 C4 C3 C5 130.5(3) . . . . ? O4 C4 C3 C2 141.3(3) . . . . ? O3 C4 C3 C2 -44.9(4) . . . . ? N1 C6 C7 C8 -0.5(5) . . . . ? C9 C8 C7 C6 -3.2(5) . . . . ? C11 C8 C7 C6 175.5(3) . . . . ? N3 N4 C12 N2 -0.4(4) . . . . ? N3 N4 C12 C13 -179.6(3) . . . . ? C11 N2 C12 N4 0.6(4) . . . . ? C11 N2 C12 C13 179.8(3) . . . . ? C17 C13 C12 N4 179.0(3) . . . . ? C14 C13 C12 N4 -0.2(5) . . . . ? C17 C13 C12 N2 -0.1(5) . . . . ? C14 C13 C12 N2 -179.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.496 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.110 data_1 _database_code_depnum_ccdc_archive 'CCDC 860287' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H30 Co2 N10 O12' _chemical_formula_weight 864.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P21/C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2800(17) _cell_length_b 28.059(6) _cell_length_c 16.424(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.02(3) _cell_angle_gamma 90.00 _cell_volume 3806.4(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.845 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30746 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6685 _reflns_number_gt 5530 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+22.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6685 _refine_ls_number_parameters 558 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.1490 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.964 _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 0.23010(7) 0.42683(2) 0.84811(4) 0.02131(17) Uani 1 1 d . . . Co2 Co -0.11951(7) 0.42146(2) 0.68869(4) 0.02192(18) Uani 1 1 d . . . C1 C 0.2244(6) 0.40240(16) 0.6604(3) 0.0235(10) Uani 1 1 d . . . C2 C 0.3440(6) 0.39913(19) 0.5990(3) 0.0298(12) Uani 1 1 d . . . H2 H 0.3068 0.3935 0.5451 0.036 Uiso 1 1 calc R . . C3 C 0.4978(6) 0.40359(19) 0.6153(3) 0.0293(11) Uani 1 1 d . . . H3 H 0.5352 0.4078 0.6696 0.035 Uiso 1 1 calc R . . C4 C 0.6189(6) 0.40243(18) 0.5529(3) 0.0280(11) Uani 1 1 d . . . C5 C -0.1499(6) 0.45626(16) 0.8287(3) 0.0237(10) Uani 1 1 d . . . C6 C -0.1648(6) 0.48387(18) 0.9031(3) 0.0269(11) Uani 1 1 d . . . H6 H -0.0871 0.4804 0.9464 0.032 Uiso 1 1 calc R . . C7 C -0.2849(6) 0.51327(19) 0.9100(3) 0.0338(12) Uani 1 1 d . . . H7 H -0.3608 0.5154 0.8656 0.041 Uiso 1 1 calc R . . C8 C -0.3125(7) 0.5436(2) 0.9814(3) 0.0345(13) Uani 1 1 d . . . C9 C 0.0767(7) 0.34418(18) 0.9358(4) 0.0389(14) Uani 1 1 d . . . H9 H 0.0253 0.3687 0.9620 0.047 Uiso 1 1 calc R . . C10 C 0.0401(7) 0.29859(19) 0.9552(4) 0.0433(15) Uani 1 1 d . . . H10 H -0.0343 0.2924 0.9938 0.052 Uiso 1 1 calc R . . C11 C 0.1134(6) 0.26184(17) 0.9177(3) 0.0293(11) Uani 1 1 d . . . C12 C 0.2242(8) 0.27377(19) 0.8638(4) 0.0450(15) Uani 1 1 d . . . H12 H 0.2797 0.2500 0.8378 0.054 Uiso 1 1 calc R . . C13 C 0.2537(7) 0.32001(19) 0.8480(4) 0.0426(15) Uani 1 1 d . . . H13 H 0.3302 0.3271 0.8110 0.051 Uiso 1 1 calc R . . C14 C 0.0723(7) 0.21239(18) 0.9343(3) 0.0322(12) Uani 1 1 d . . . C15 C 0.0567(6) 0.13867(17) 0.9235(3) 0.0290(11) Uani 1 1 d . . . C16 C 0.0725(6) 0.08947(18) 0.8998(3) 0.0309(12) Uani 1 1 d . . . C17 C 0.1922(8) 0.0754(2) 0.8534(4) 0.0547(18) Uani 1 1 d . . . H17 H 0.2677 0.0974 0.8372 0.066 Uiso 1 1 calc R . . C18 C 0.2020(8) 0.0292(2) 0.8303(4) 0.0544(19) Uani 1 1 d . . . H18 H 0.2851 0.0206 0.7980 0.065 Uiso 1 1 calc R . . C19 C -0.0315(7) 0.05524(19) 0.9220(4) 0.0411(14) Uani 1 1 d . . . H19 H -0.1158 0.0630 0.9542 0.049 Uiso 1 1 calc R . . C20 C -0.0117(7) 0.00962(19) 0.8969(3) 0.0397(14) Uani 1 1 d . . . H20 H -0.0837 -0.0132 0.9136 0.048 Uiso 1 1 calc R . . C21 C 0.2104(8) 0.5333(2) 0.8435(4) 0.0459(15) Uani 1 1 d . . . H21 H 0.1550 0.5270 0.8897 0.055 Uiso 1 1 calc R . . C22 C 0.2176(8) 0.5791(2) 0.8171(4) 0.0521(17) Uani 1 1 d . . . H22 H 0.1702 0.6035 0.8454 0.063 Uiso 1 1 calc R . . C23 C 0.2955(7) 0.58894(18) 0.7481(3) 0.0341(12) Uani 1 1 d . . . C24 C 0.3681(7) 0.55249(19) 0.7109(4) 0.0381(13) Uani 1 1 d . . . H24 H 0.4244 0.5578 0.6647 0.046 Uiso 1 1 calc R . . C25 C 0.3568(6) 0.50759(18) 0.7427(3) 0.0332(12) Uani 1 1 d . . . H25 H 0.4082 0.4828 0.7173 0.040 Uiso 1 1 calc R . . C26 C 0.2999(7) 0.63777(18) 0.7199(3) 0.0358(13) Uani 1 1 d . . . C27 C 0.2767(7) 0.71078(18) 0.7108(3) 0.0376(13) Uani 1 1 d . . . C28 C 0.2359(7) 0.75953(19) 0.7305(3) 0.0362(13) Uani 1 1 d . . . C29 C 0.2908(8) 0.7967(2) 0.6887(4) 0.0515(17) Uani 1 1 d . . . H29 H 0.3546 0.7916 0.6451 0.062 Uiso 1 1 calc R . . C30 C 0.2525(8) 0.8417(2) 0.7105(4) 0.0488(17) Uani 1 1 d . . . H30 H 0.2919 0.8669 0.6809 0.059 Uiso 1 1 calc R . . C31 C 0.1416(9) 0.7695(2) 0.7926(4) 0.0548(18) Uani 1 1 d . . . H31 H 0.1009 0.7448 0.8230 0.066 Uiso 1 1 calc R . . C32 C 0.1069(8) 0.81514(19) 0.8103(4) 0.0481(16) Uani 1 1 d . . . H32 H 0.0400 0.8210 0.8523 0.058 Uiso 1 1 calc R . . H9A H 0.549(6) 0.426(2) 0.850(3) 0.06(2) Uiso 1 1 d D . . H9B H 0.485(7) 0.420(2) 0.9225(14) 0.05(2) Uiso 1 1 d D . . H4C H -0.083(7) 0.1346(18) 1.015(3) 0.054(19) Uiso 1 1 d D . . H9C H 0.387(8) 0.633(2) 0.613(3) 0.07(2) Uiso 1 1 d D . . N1 N 0.1800(5) 0.35570(14) 0.8823(3) 0.0276(9) Uani 1 1 d . . . N2 N 0.1273(5) 0.17525(15) 0.8922(3) 0.0340(10) Uani 1 1 d . . . N3 N -0.0240(6) 0.20036(15) 0.9905(3) 0.0427(12) Uani 1 1 d . . . N4 N -0.0339(6) 0.15302(16) 0.9819(3) 0.0402(12) Uani 1 1 d D . . N5 N 0.1019(5) -0.00429(15) 0.8508(3) 0.0303(10) Uani 1 1 d . . . N6 N 0.2771(5) 0.49756(14) 0.8075(3) 0.0293(10) Uani 1 1 d . . . N7 N 0.2471(6) 0.67428(16) 0.7596(3) 0.0409(12) Uani 1 1 d . . . N8 N 0.3408(7) 0.69943(16) 0.6436(3) 0.0496(14) Uani 1 1 d . . . N9 N 0.3541(7) 0.65184(16) 0.6501(3) 0.0469(13) Uani 1 1 d D . . N10 N 0.1629(5) 0.85164(14) 0.7710(3) 0.0294(10) Uani 1 1 d . . . O1 O 0.2735(4) 0.40393(13) 0.7327(2) 0.0297(8) Uani 1 1 d . . . O2 O 0.0809(4) 0.40511(12) 0.6336(2) 0.0295(8) Uani 1 1 d . . . O3 O 0.7639(4) 0.40526(13) 0.5783(2) 0.0295(8) Uani 1 1 d . . . O4 O 0.5716(5) 0.39875(16) 0.4806(2) 0.0461(11) Uani 1 1 d . . . O5 O -0.0155(4) 0.44022(11) 0.8111(2) 0.0258(7) Uani 1 1 d . . . O6 O -0.2699(4) 0.44972(11) 0.7799(2) 0.0260(8) Uani 1 1 d . . . O7 O -0.2051(4) 0.54663(12) 1.0374(2) 0.0278(8) Uani 1 1 d . . . O8 O -0.4462(6) 0.5629(2) 0.9795(3) 0.086(2) Uani 1 1 d . . . O9 O 0.4742(4) 0.41221(13) 0.8726(2) 0.0321(8) Uani 1 1 d D . . O10 O 0.716(3) 0.3726(10) 0.0059(16) 0.189(13) Uani 0.443(19) 1 d PU A 1 O11 O 0.482(4) 0.2309(11) 0.0622(19) 0.211(14) Uani 0.443(19) 1 d PU A 1 O10' O 0.699(4) 0.3161(14) 0.054(2) 0.307(18) Uani 0.557(19) 1 d PU A 2 O11' O 0.599(3) 0.2624(10) 0.0211(15) 0.220(12) Uani 0.557(19) 1 d PU A 2 O12A O 0.308(3) 0.1722(8) 0.7367(15) 0.120(7) Uani 0.33 1 d PU B 2 O12B O 0.322(4) 0.1313(11) 0.6736(17) 0.155(10) Uani 0.33 1 d PU C 3 O12C O 0.181(3) 0.1607(10) 0.6694(15) 0.138(9) Uani 0.33 1 d PU D 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0227(3) 0.0180(3) 0.0238(3) -0.0024(3) 0.0061(3) -0.0003(3) Co2 0.0209(3) 0.0199(3) 0.0257(4) -0.0036(3) 0.0072(3) -0.0006(3) C1 0.022(3) 0.020(2) 0.030(3) -0.003(2) 0.008(2) -0.0035(19) C2 0.023(3) 0.044(3) 0.023(3) -0.009(2) 0.005(2) 0.002(2) C3 0.026(3) 0.039(3) 0.023(3) -0.006(2) 0.003(2) 0.002(2) C4 0.027(3) 0.031(3) 0.026(3) -0.010(2) 0.007(2) -0.001(2) C5 0.027(3) 0.021(2) 0.024(3) -0.002(2) 0.008(2) -0.004(2) C6 0.025(3) 0.034(3) 0.022(2) -0.006(2) 0.003(2) -0.001(2) C7 0.032(3) 0.040(3) 0.029(3) -0.012(2) -0.001(2) 0.004(2) C8 0.037(3) 0.038(3) 0.029(3) -0.005(2) 0.002(2) 0.013(2) C9 0.049(4) 0.020(3) 0.051(4) -0.002(2) 0.024(3) 0.003(2) C10 0.055(4) 0.026(3) 0.052(4) 0.002(3) 0.026(3) -0.001(3) C11 0.036(3) 0.019(2) 0.033(3) -0.001(2) 0.003(2) -0.003(2) C12 0.059(4) 0.020(3) 0.059(4) -0.001(3) 0.028(3) 0.003(3) C13 0.053(4) 0.025(3) 0.053(4) -0.001(3) 0.027(3) 0.003(3) C14 0.042(3) 0.022(3) 0.034(3) 0.002(2) 0.011(2) -0.002(2) C15 0.033(3) 0.024(3) 0.030(3) 0.000(2) 0.005(2) -0.002(2) C16 0.036(3) 0.024(3) 0.033(3) 0.000(2) 0.005(2) -0.003(2) C17 0.051(4) 0.030(3) 0.087(5) -0.015(3) 0.034(4) -0.018(3) C18 0.045(4) 0.041(4) 0.082(5) -0.021(3) 0.037(4) -0.015(3) C19 0.046(3) 0.029(3) 0.052(4) -0.005(3) 0.030(3) -0.006(2) C20 0.050(4) 0.028(3) 0.044(3) 0.001(3) 0.024(3) -0.009(3) C21 0.064(4) 0.031(3) 0.045(4) 0.004(3) 0.026(3) 0.009(3) C22 0.082(5) 0.023(3) 0.056(4) -0.003(3) 0.033(4) 0.012(3) C23 0.044(3) 0.023(3) 0.036(3) 0.000(2) 0.006(2) -0.002(2) C24 0.045(3) 0.030(3) 0.041(3) 0.000(3) 0.015(3) -0.001(2) C25 0.038(3) 0.023(3) 0.040(3) -0.004(2) 0.012(2) 0.001(2) C26 0.048(3) 0.026(3) 0.035(3) 0.001(2) 0.012(3) 0.004(2) C27 0.058(4) 0.020(3) 0.036(3) 0.000(2) 0.010(3) 0.003(2) C28 0.046(3) 0.027(3) 0.036(3) 0.002(2) 0.007(3) 0.005(2) C29 0.077(5) 0.028(3) 0.055(4) 0.003(3) 0.040(4) 0.004(3) C30 0.071(4) 0.023(3) 0.057(4) 0.006(3) 0.035(3) 0.000(3) C31 0.086(5) 0.023(3) 0.060(4) 0.010(3) 0.034(4) 0.001(3) C32 0.077(5) 0.027(3) 0.045(4) 0.006(3) 0.035(3) 0.004(3) N1 0.029(2) 0.020(2) 0.035(2) -0.0004(18) 0.0084(19) -0.0001(17) N2 0.042(3) 0.023(2) 0.038(3) -0.001(2) 0.012(2) -0.0055(19) N3 0.063(3) 0.021(2) 0.047(3) -0.001(2) 0.023(3) -0.003(2) N4 0.059(3) 0.022(2) 0.042(3) 0.002(2) 0.022(2) -0.005(2) N5 0.029(2) 0.028(2) 0.034(2) -0.0008(19) 0.0064(19) -0.0009(18) N6 0.032(2) 0.022(2) 0.034(2) -0.0008(19) 0.0055(19) 0.0003(18) N7 0.062(3) 0.025(2) 0.038(3) 0.003(2) 0.016(2) 0.004(2) N8 0.085(4) 0.025(3) 0.041(3) 0.001(2) 0.020(3) 0.006(2) N9 0.087(4) 0.021(2) 0.036(3) -0.003(2) 0.020(3) 0.006(2) N10 0.034(2) 0.024(2) 0.031(2) 0.0051(19) 0.0045(19) 0.0027(18) O1 0.0303(19) 0.038(2) 0.0214(18) -0.0039(16) 0.0073(15) 0.0015(16) O2 0.0203(18) 0.036(2) 0.0324(19) -0.0037(16) 0.0066(15) 0.0009(15) O3 0.0188(18) 0.041(2) 0.0294(19) -0.0048(16) 0.0052(14) -0.0024(15) O4 0.034(2) 0.079(3) 0.026(2) -0.012(2) 0.0066(17) 0.002(2) O5 0.0206(17) 0.0275(18) 0.0300(19) -0.0103(15) 0.0075(14) 0.0018(14) O6 0.0211(17) 0.0259(18) 0.0312(19) -0.0083(15) 0.0038(15) -0.0003(14) O7 0.0290(19) 0.0295(19) 0.0250(18) -0.0061(15) 0.0028(15) 0.0023(15) O8 0.066(3) 0.140(5) 0.049(3) -0.048(3) -0.018(2) 0.062(3) O9 0.0241(19) 0.038(2) 0.035(2) -0.0056(18) 0.0077(16) 0.0010(16) O10 0.187(15) 0.200(16) 0.179(15) -0.009(9) 0.012(9) 0.028(9) O11 0.206(16) 0.207(16) 0.217(16) 0.005(10) -0.005(9) -0.001(9) O10' 0.313(19) 0.31(2) 0.298(19) -0.010(10) 0.049(10) 0.005(10) O11' 0.232(14) 0.213(14) 0.212(14) 0.004(9) 0.006(9) -0.008(9) O12A 0.115(10) 0.114(10) 0.137(11) -0.011(9) 0.038(9) -0.014(8) O12B 0.168(13) 0.157(13) 0.141(12) -0.009(9) 0.024(9) -0.021(9) O12C 0.144(12) 0.153(12) 0.117(11) 0.015(9) 0.010(9) 0.005(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 O9 2.074(4) . Y Co1 O7 2.046(3) 3_567 Y Co1 O1 2.057(3) . Y Co1 N1 2.122(4) . Y Co1 N6 2.138(4) . Y Co1 O5 2.115(3) . Y Co2 O2 1.998(3) . Y Co2 O3 2.045(3) 1_455 Y Co2 N10 2.107(4) 2_546 Y Co2 O5 2.195(3) . Y Co2 N5 2.190(4) 2_556 Y Co2 O6 2.164(3) . Y Co2 C5 2.528(5) . Y C1 O1 1.229(6) . ? C1 O2 1.240(6) . ? C1 C2 1.464(7) . ? C2 C3 1.289(7) . ? C2 H2 0.9300 . ? C3 C4 1.484(7) . ? C3 H3 0.9300 . ? C4 O4 1.229(6) . ? C4 O3 1.246(6) . ? C5 O6 1.246(6) . ? C5 O5 1.253(6) . ? C5 C6 1.458(7) . ? C6 C7 1.303(7) . ? C6 H6 0.9300 . ? C7 C8 1.480(7) . ? C7 H7 0.9300 . ? C8 O8 1.230(7) . ? C8 O7 1.237(6) . ? C9 N1 1.309(7) . ? C9 C10 1.358(7) . ? C9 H9 0.9300 . ? C10 C11 1.365(7) . ? C10 H10 0.9300 . ? C11 C12 1.361(8) . ? C11 C14 1.459(7) . ? C12 C13 1.349(7) . ? C12 H12 0.9300 . ? C13 N1 1.319(6) . ? C13 H13 0.9300 . ? C14 N3 1.305(7) . ? C14 N2 1.347(7) . ? C15 N2 1.304(6) . ? C15 N4 1.321(7) . ? C15 C16 1.443(7) . ? C16 C17 1.351(8) . ? C16 C19 1.357(7) . ? C17 C18 1.357(8) . ? C17 H17 0.9300 . ? C18 N5 1.312(7) . ? C18 H18 0.9300 . ? C19 C20 1.358(7) . ? C19 H19 0.9300 . ? C20 N5 1.307(7) . ? C20 H20 0.9300 . ? C21 N6 1.305(7) . ? C21 C22 1.360(8) . ? C21 H21 0.9300 . ? C22 C23 1.370(8) . ? C22 H22 0.9300 . ? C23 C24 1.354(7) . ? C23 C26 1.448(7) . ? C24 C25 1.370(7) . ? C24 H24 0.9300 . ? C25 N6 1.321(7) . ? C25 H25 0.9300 . ? C26 N9 1.321(7) . ? C26 N7 1.307(7) . ? C27 N8 1.298(7) . ? C27 N7 1.334(7) . ? C27 C28 1.451(7) . ? C28 C31 1.356(8) . ? C28 C29 1.346(8) . ? C29 C30 1.356(8) . ? C29 H29 0.9300 . ? C30 N10 1.312(7) . ? C30 H30 0.9300 . ? C31 C32 1.349(8) . ? C31 H31 0.9300 . ? C32 N10 1.312(7) . ? C32 H32 0.9300 . ? N3 N4 1.338(6) . ? N4 H4C 0.87(2) . ? N5 Co2 2.190(4) 2_546 ? N8 N9 1.344(6) . ? N9 H9C 0.87(2) . ? N10 Co2 2.107(4) 2_556 ? O3 Co2 2.045(3) 1_655 ? O7 Co1 2.046(3) 3_567 ? O9 H9A 0.84(2) . ? O9 H9B 0.845(19) . ? 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 O9 Co1 O7 93.06(14) . 3_567 Y O9 Co1 O1 83.48(15) . . Y O7 Co1 O1 174.84(14) 3_567 . Y O9 Co1 N1 88.20(15) . . Y O7 Co1 N1 93.72(15) 3_567 . Y O1 Co1 N1 90.00(15) . . Y O9 Co1 N6 92.74(16) . . Y O7 Co1 N6 88.90(15) 3_567 . Y O1 Co1 N6 87.45(15) . . Y N1 Co1 N6 177.16(16) . . Y O9 Co1 O5 174.44(14) . . Y O7 Co1 O5 92.42(13) 3_567 . Y O1 Co1 O5 90.99(13) . . Y N1 Co1 O5 92.36(15) . . Y N6 Co1 O5 86.44(15) . . Y O2 Co2 O3 84.44(13) . 1_455 Y O2 Co2 N10 95.39(15) . 2_546 Y O3 Co2 N10 89.51(15) 1_455 2_546 Y O2 Co2 O5 100.63(13) . . Y O3 Co2 O5 174.93(12) 1_455 . Y N10 Co2 O5 90.00(14) 2_546 . Y O2 Co2 N5 90.55(15) . 2_556 Y O3 Co2 N5 89.20(15) 1_455 2_556 Y N10 Co2 N5 173.78(16) 2_546 2_556 Y O5 Co2 N5 90.75(14) . 2_556 Y O2 Co2 O6 159.01(14) . . Y O3 Co2 O6 115.87(13) 1_455 . Y N10 Co2 O6 90.26(14) 2_546 . Y O5 Co2 O6 59.08(12) . . Y N5 Co2 O6 84.83(14) 2_556 . Y O2 Co2 C5 129.74(15) . . Y O3 Co2 C5 145.29(15) 1_455 . Y N10 Co2 C5 92.49(15) 2_546 . Y O5 Co2 C5 29.72(13) . . Y N5 Co2 C5 85.12(15) 2_556 . Y O6 Co2 C5 29.53(14) . . Y O1 C1 O2 125.7(4) . . ? O1 C1 C2 118.3(4) . . ? O2 C1 C2 115.9(4) . . ? C3 C2 C1 123.8(5) . . ? C3 C2 H2 118.1 . . ? C1 C2 H2 118.1 . . ? C2 C3 C4 124.0(5) . . ? C2 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? O4 C4 O3 124.3(5) . . ? O4 C4 C3 119.0(5) . . ? O3 C4 C3 116.7(4) . . ? O6 C5 O5 118.6(4) . . ? O6 C5 C6 120.4(4) . . ? O5 C5 C6 120.9(4) . . ? O6 C5 Co2 58.8(2) . . ? O5 C5 Co2 60.3(2) . . ? C6 C5 Co2 170.6(4) . . ? C7 C6 C5 121.3(5) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 126.5(5) . . ? C6 C7 H7 116.8 . . ? C8 C7 H7 116.8 . . ? O8 C8 O7 126.0(5) . . ? O8 C8 C7 114.9(5) . . ? O7 C8 C7 119.1(5) . . ? N1 C9 C10 123.9(5) . . ? N1 C9 H9 118.1 . . ? C10 C9 H9 118.1 . . ? C9 C10 C11 119.5(5) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 116.7(5) . . ? C12 C11 C14 122.2(5) . . ? C10 C11 C14 121.1(5) . . ? C11 C12 C13 120.1(5) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? N1 C13 C12 123.6(5) . . ? N1 C13 H13 118.2 . . ? C12 C13 H13 118.2 . . ? N3 C14 N2 114.1(5) . . ? N3 C14 C11 122.7(5) . . ? N2 C14 C11 123.2(5) . . ? N2 C15 N4 109.8(4) . . ? N2 C15 C16 126.5(5) . . ? N4 C15 C16 123.7(5) . . ? C17 C16 C19 116.8(5) . . ? C17 C16 C15 121.0(5) . . ? C19 C16 C15 122.2(5) . . ? C16 C17 C18 119.8(5) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? N5 C18 C17 124.2(5) . . ? N5 C18 H18 117.9 . . ? C17 C18 H18 117.9 . . ? C16 C19 C20 119.5(5) . . ? C16 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? N5 C20 C19 124.4(5) . . ? N5 C20 H20 117.8 . . ? C19 C20 H20 117.8 . . ? N6 C21 C22 123.5(5) . . ? N6 C21 H21 118.3 . . ? C22 C21 H21 118.3 . . ? C21 C22 C23 119.2(5) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C22 C23 C24 118.1(5) . . ? C22 C23 C26 118.6(5) . . ? C24 C23 C26 123.3(5) . . ? C23 C24 C25 118.5(5) . . ? C23 C24 H24 120.7 . . ? C25 C24 H24 120.7 . . ? N6 C25 C24 123.7(5) . . ? N6 C25 H25 118.2 . . ? C24 C25 H25 118.2 . . ? N9 C26 N7 110.2(5) . . ? N9 C26 C23 125.4(5) . . ? N7 C26 C23 124.4(5) . . ? N8 C27 N7 115.2(5) . . ? N8 C27 C28 122.4(5) . . ? N7 C27 C28 122.3(5) . . ? C31 C28 C29 117.3(5) . . ? C31 C28 C27 121.1(5) . . ? C29 C28 C27 121.6(5) . . ? C30 C29 C28 119.5(5) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? N10 C30 C29 123.6(5) . . ? N10 C30 H30 118.2 . . ? C29 C30 H30 118.2 . . ? C28 C31 C32 120.0(5) . . ? C28 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? N10 C32 C31 123.2(5) . . ? N10 C32 H32 118.4 . . ? C31 C32 H32 118.4 . . ? C9 N1 C13 116.3(5) . . ? C9 N1 Co1 124.0(3) . . ? C13 N1 Co1 119.7(4) . . ? C15 N2 C14 103.3(4) . . ? C14 N3 N4 102.6(4) . . ? C15 N4 N3 110.2(4) . . ? C15 N4 H4C 126(4) . . ? N3 N4 H4C 123(4) . . ? C20 N5 C18 115.4(5) . . ? C20 N5 Co2 121.4(4) . 2_546 ? C18 N5 Co2 123.2(4) . 2_546 ? C25 N6 C21 116.9(5) . . ? C25 N6 Co1 124.1(3) . . ? C21 N6 Co1 118.6(4) . . ? C26 N7 C27 102.7(5) . . ? C27 N8 N9 102.3(5) . . ? C26 N9 N8 109.6(5) . . ? C26 N9 H9C 125(5) . . ? N8 N9 H9C 125(5) . . ? C32 N10 C30 116.4(5) . . ? C32 N10 Co2 119.9(4) . 2_556 ? C30 N10 Co2 123.6(4) . 2_556 ? C1 O1 Co1 146.5(3) . . ? C1 O2 Co2 131.3(3) . . ? C4 O3 Co2 134.0(3) . 1_655 ? C5 O5 Co1 148.1(3) . . ? C5 O5 Co2 90.0(3) . . ? Co1 O5 Co2 121.89(14) . . ? C5 O6 Co2 91.6(3) . . ? C8 O7 Co1 126.5(3) . 3_567 ? Co1 O9 H9A 124(5) . . ? Co1 O9 H9B 100(4) . . ? H9A O9 H9B 106(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -8.8(8) . . . . ? O2 C1 C2 C3 168.7(5) . . . . ? C1 C2 C3 C4 -177.2(5) . . . . ? C2 C3 C4 O4 2.8(8) . . . . ? C2 C3 C4 O3 -177.1(5) . . . . ? O2 Co2 C5 O6 174.8(2) . . . . ? O3 Co2 C5 O6 6.6(4) 1_455 . . . ? N10 Co2 C5 O6 -86.1(3) 2_546 . . . ? O5 Co2 C5 O6 -171.8(4) . . . . ? N5 Co2 C5 O6 88.1(3) 2_556 . . . ? O2 Co2 C5 O5 -13.5(3) . . . . ? O3 Co2 C5 O5 178.4(3) 1_455 . . . ? N10 Co2 C5 O5 85.6(3) 2_546 . . . ? N5 Co2 C5 O5 -100.1(3) 2_556 . . . ? O6 Co2 C5 O5 171.8(4) . . . . ? O2 Co2 C5 C6 86(2) . . . . ? O3 Co2 C5 C6 -82(2) 1_455 . . . ? N10 Co2 C5 C6 -175(2) 2_546 . . . ? O5 Co2 C5 C6 100(2) . . . . ? N5 Co2 C5 C6 0(2) 2_556 . . . ? O6 Co2 C5 C6 -89(2) . . . . ? O6 C5 C6 C7 -19.9(8) . . . . ? O5 C5 C6 C7 157.3(5) . . . . ? Co2 C5 C6 C7 63(2) . . . . ? C5 C6 C7 C8 -179.2(5) . . . . ? C6 C7 C8 O8 -169.2(6) . . . . ? C6 C7 C8 O7 9.2(9) . . . . ? N1 C9 C10 C11 -0.1(10) . . . . ? C9 C10 C11 C12 1.9(9) . . . . ? C9 C10 C11 C14 -177.4(6) . . . . ? C10 C11 C12 C13 -1.8(9) . . . . ? C14 C11 C12 C13 177.4(6) . . . . ? C11 C12 C13 N1 -0.1(10) . . . . ? C12 C11 C14 N3 174.4(6) . . . . ? C10 C11 C14 N3 -6.4(9) . . . . ? C12 C11 C14 N2 -7.0(9) . . . . ? C10 C11 C14 N2 172.2(6) . . . . ? N2 C15 C16 C17 14.7(9) . . . . ? N4 C15 C16 C17 -165.1(6) . . . . ? N2 C15 C16 C19 -164.7(6) . . . . ? N4 C15 C16 C19 15.4(9) . . . . ? C19 C16 C17 C18 1.0(10) . . . . ? C15 C16 C17 C18 -178.5(6) . . . . ? C16 C17 C18 N5 -0.6(12) . . . . ? C17 C16 C19 C20 -0.4(9) . . . . ? C15 C16 C19 C20 179.1(6) . . . . ? C16 C19 C20 N5 -0.9(10) . . . . ? N6 C21 C22 C23 1.4(11) . . . . ? C21 C22 C23 C24 -2.6(10) . . . . ? C21 C22 C23 C26 179.0(6) . . . . ? C22 C23 C24 C25 1.5(9) . . . . ? C26 C23 C24 C25 179.9(5) . . . . ? C23 C24 C25 N6 0.9(9) . . . . ? C22 C23 C26 N9 -172.0(6) . . . . ? C24 C23 C26 N9 9.7(10) . . . . ? C22 C23 C26 N7 6.5(9) . . . . ? C24 C23 C26 N7 -171.9(6) . . . . ? N8 C27 C28 C31 167.1(7) . . . . ? N7 C27 C28 C31 -11.1(10) . . . . ? N8 C27 C28 C29 -13.4(10) . . . . ? N7 C27 C28 C29 168.3(6) . . . . ? C31 C28 C29 C30 1.0(10) . . . . ? C27 C28 C29 C30 -178.5(6) . . . . ? C28 C29 C30 N10 -0.2(12) . . . . ? C29 C28 C31 C32 -0.2(11) . . . . ? C27 C28 C31 C32 179.3(6) . . . . ? C28 C31 C32 N10 -1.4(11) . . . . ? C10 C9 N1 C13 -1.8(9) . . . . ? C10 C9 N1 Co1 177.3(5) . . . . ? C12 C13 N1 C9 1.9(9) . . . . ? C12 C13 N1 Co1 -177.3(5) . . . . ? O9 Co1 N1 C9 128.2(5) . . . . ? O7 Co1 N1 C9 35.2(5) 3_567 . . . ? O1 Co1 N1 C9 -148.4(5) . . . . ? N6 Co1 N1 C9 -122(3) . . . . ? O5 Co1 N1 C9 -57.4(5) . . . . ? O9 Co1 N1 C13 -52.7(4) . . . . ? O7 Co1 N1 C13 -145.7(4) 3_567 . . . ? O1 Co1 N1 C13 30.7(4) . . . . ? N6 Co1 N1 C13 57(3) . . . . ? O5 Co1 N1 C13 121.7(4) . . . . ? N4 C15 N2 C14 -0.8(6) . . . . ? C16 C15 N2 C14 179.4(5) . . . . ? N3 C14 N2 C15 1.6(7) . . . . ? C11 C14 N2 C15 -177.1(5) . . . . ? N2 C14 N3 N4 -1.7(7) . . . . ? C11 C14 N3 N4 177.0(5) . . . . ? N2 C15 N4 N3 -0.2(7) . . . . ? C16 C15 N4 N3 179.6(5) . . . . ? C14 N3 N4 C15 1.1(7) . . . . ? C19 C20 N5 C18 1.3(9) . . . . ? C19 C20 N5 Co2 -178.5(5) . . . 2_546 ? C17 C18 N5 C20 -0.6(10) . . . . ? C17 C18 N5 Co2 179.2(6) . . . 2_546 ? C24 C25 N6 C21 -2.0(8) . . . . ? C24 C25 N6 Co1 171.0(4) . . . . ? C22 C21 N6 C25 0.9(9) . . . . ? C22 C21 N6 Co1 -172.6(6) . . . . ? O9 Co1 N6 C25 63.9(4) . . . . ? O7 Co1 N6 C25 157.0(4) 3_567 . . . ? O1 Co1 N6 C25 -19.4(4) . . . . ? N1 Co1 N6 C25 -45(3) . . . . ? O5 Co1 N6 C25 -110.6(4) . . . . ? O9 Co1 N6 C21 -123.1(5) . . . . ? O7 Co1 N6 C21 -30.1(5) 3_567 . . . ? O1 Co1 N6 C21 153.6(5) . . . . ? N1 Co1 N6 C21 128(3) . . . . ? O5 Co1 N6 C21 62.4(4) . . . . ? N9 C26 N7 C27 -1.6(7) . . . . ? C23 C26 N7 C27 179.8(6) . . . . ? N8 C27 N7 C26 1.2(7) . . . . ? C28 C27 N7 C26 179.6(6) . . . . ? N7 C27 N8 N9 -0.3(8) . . . . ? C28 C27 N8 N9 -178.7(6) . . . . ? N7 C26 N9 N8 1.5(8) . . . . ? C23 C26 N9 N8 -179.9(6) . . . . ? C27 N8 N9 C26 -0.7(7) . . . . ? C31 C32 N10 C30 2.1(10) . . . . ? C31 C32 N10 Co2 -174.0(6) . . . 2_556 ? C29 C30 N10 C32 -1.3(10) . . . . ? C29 C30 N10 Co2 174.6(6) . . . 2_556 ? O2 C1 O1 Co1 -25.2(9) . . . . ? C2 C1 O1 Co1 152.0(5) . . . . ? O9 Co1 O1 C1 -164.3(6) . . . . ? O7 Co1 O1 C1 -116.3(15) 3_567 . . . ? N1 Co1 O1 C1 107.5(6) . . . . ? N6 Co1 O1 C1 -71.3(6) . . . . ? O5 Co1 O1 C1 15.1(6) . . . . ? O1 C1 O2 Co2 9.6(8) . . . . ? C2 C1 O2 Co2 -167.7(3) . . . . ? O3 Co2 O2 C1 -175.2(4) 1_455 . . . ? N10 Co2 O2 C1 -86.2(4) 2_546 . . . ? O5 Co2 O2 C1 4.8(4) . . . . ? N5 Co2 O2 C1 95.7(4) 2_556 . . . ? O6 Co2 O2 C1 18.8(7) . . . . ? C5 Co2 O2 C1 11.6(5) . . . . ? O4 C4 O3 Co2 169.0(4) . . . 1_655 ? C3 C4 O3 Co2 -11.1(7) . . . 1_655 ? O6 C5 O5 Co1 -172.0(4) . . . . ? C6 C5 O5 Co1 10.7(9) . . . . ? Co2 C5 O5 Co1 179.9(6) . . . . ? O6 C5 O5 Co2 8.0(4) . . . . ? C6 C5 O5 Co2 -169.2(4) . . . . ? O9 Co1 O5 C5 -169.1(13) . . . . ? O7 Co1 O5 C5 1.4(6) 3_567 . . . ? O1 Co1 O5 C5 -174.7(6) . . . . ? N1 Co1 O5 C5 95.2(6) . . . . ? N6 Co1 O5 C5 -87.3(6) . . . . ? O9 Co1 O5 Co2 10.8(16) . . . . ? O7 Co1 O5 Co2 -178.66(18) 3_567 . . . ? O1 Co1 O5 Co2 5.21(19) . . . . ? N1 Co1 O5 Co2 -84.8(2) . . . . ? N6 Co1 O5 Co2 92.6(2) . . . . ? O2 Co2 O5 C5 169.5(3) . . . . ? O3 Co2 O5 C5 -10.6(17) 1_455 . . . ? N10 Co2 O5 C5 -95.0(3) 2_546 . . . ? N5 Co2 O5 C5 78.8(3) 2_556 . . . ? O6 Co2 O5 C5 -4.7(3) . . . . ? O2 Co2 O5 Co1 -10.5(2) . . . . ? O3 Co2 O5 Co1 169.5(14) 1_455 . . . ? N10 Co2 O5 Co1 85.0(2) 2_546 . . . ? N5 Co2 O5 Co1 -101.17(19) 2_556 . . . ? O6 Co2 O5 Co1 175.3(2) . . . . ? C5 Co2 O5 Co1 -180.0(4) . . . . ? O5 C5 O6 Co2 -8.2(4) . . . . ? C6 C5 O6 Co2 169.1(4) . . . . ? O2 Co2 O6 C5 -11.3(5) . . . . ? O3 Co2 O6 C5 -175.8(3) 1_455 . . . ? N10 Co2 O6 C5 94.6(3) 2_546 . . . ? O5 Co2 O6 C5 4.8(3) . . . . ? N5 Co2 O6 C5 -89.2(3) 2_556 . . . ? O8 C8 O7 Co1 12.8(9) . . . 3_567 ? C7 C8 O7 Co1 -165.4(4) . . . 3_567 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.556 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.082