Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Can-Zhong Lu' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Fuzhou 351002 CHINA ; _publ_contact_author_email CZLU@FJIRSM.AC.CN _publ_section_title ; Syntheses, crystal structures, and properties of complexes constructed with polybenzoate and 2,2?-bibenzimidazole ; loop_ _publ_author_name 'Lu Can-Zhong' 'Xiao-Yuan Wu' 'Ding-Ming Wu' 'Chang-Kun Xia' ; Sheng-Chang Xiang ; 'Daqiang Yuan' 'Quan-Zheng Zhang' 'Jian-Jun Zhang' # Attachment 'CIFS.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 286936' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H14 Co N4 O4' _chemical_formula_weight 457.30 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 p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.3278(2) _cell_length_b 21.8954(8) _cell_length_c 11.7204(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.01 _cell_angle_gamma 90.00 _cell_volume 1866.42(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3238 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 25.01 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.817 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Simemens SMART CCD' _diffrn_measurement_method '\w scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 6001 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3238 _reflns_number_gt 2542 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' Simens SMART ' _computing_cell_refinement ' Simens SMART ' _computing_data_reduction ' Simens SMART ' _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^)+(0.0000P)^2^+9.5387P] 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 3238 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1510 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 1.252 _refine_ls_restrained_S_all 1.252 _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 0.23212(11) 0.38156(4) 0.39297(7) 0.0271(2) Uani 1 1 d . . . C1 C -0.5549(8) 0.2008(3) -0.0294(5) 0.0285(14) Uani 1 1 d . . . C2 C -0.4171(8) 0.2432(3) 0.0300(5) 0.0277(13) Uani 1 1 d . . . C3 C -0.4708(8) 0.2847(3) 0.1110(5) 0.0314(14) Uani 1 1 d . . . H3A H -0.5946 0.2889 0.1198 0.038 Uiso 1 1 calc R . . C4 C -0.3406(8) 0.3193(3) 0.1776(5) 0.0315(14) Uani 1 1 d . . . H4A H -0.3765 0.3457 0.2330 0.038 Uiso 1 1 calc R . . C5 C -0.1553(8) 0.3148(3) 0.1617(5) 0.0256(13) Uani 1 1 d . . . C6 C -0.1029(8) 0.2765(3) 0.0760(5) 0.0298(14) Uani 1 1 d . . . H6A H 0.0192 0.2752 0.0619 0.036 Uiso 1 1 calc R . . C7 C -0.2335(8) 0.2402(3) 0.0119(5) 0.0277(13) Uani 1 1 d . . . H7A H -0.1976 0.2138 -0.0434 0.033 Uiso 1 1 calc R . . C8 C -0.0095(9) 0.3468(3) 0.2403(5) 0.0311(14) Uani 1 1 d . . . C9 C 0.3103(8) 0.5131(3) 0.2690(5) 0.0280(13) Uani 1 1 d . . . C10 C 0.3374(9) 0.5010(3) 0.1554(5) 0.0374(15) Uani 1 1 d . . . H10A H 0.3309 0.4614 0.1263 0.045 Uiso 1 1 calc R . . C11 C 0.3741(9) 0.5499(3) 0.0883(6) 0.0424(17) Uani 1 1 d . . . H11A H 0.3936 0.5430 0.0124 0.051 Uiso 1 1 calc R . . C12 C 0.3830(9) 0.6097(3) 0.1307(6) 0.0451(18) Uani 1 1 d . . . H12A H 0.4051 0.6415 0.0818 0.054 Uiso 1 1 calc R . . C13 C 0.3598(9) 0.6226(3) 0.2432(6) 0.0402(16) Uani 1 1 d . . . H13A H 0.3687 0.6622 0.2720 0.048 Uiso 1 1 calc R . . C14 C 0.3222(8) 0.5732(3) 0.3112(5) 0.0326(14) Uani 1 1 d . . . C15 C 0.2616(7) 0.5097(2) 0.4470(5) 0.0252(13) Uani 1 1 d . . . C16 C 0.2245(8) 0.4817(3) 0.5526(5) 0.0254(13) Uani 1 1 d . . . C17 C 0.1804(8) 0.4066(3) 0.6670(5) 0.0307(14) Uani 1 1 d . . . C18 C 0.1607(9) 0.3498(3) 0.7174(6) 0.0408(16) Uani 1 1 d . . . H18A H 0.1706 0.3137 0.6767 0.049 Uiso 1 1 calc R . . C19 C 0.1256(10) 0.3493(4) 0.8310(6) 0.0501(19) Uani 1 1 d . . . H19A H 0.1111 0.3122 0.8675 0.060 Uiso 1 1 calc R . . C20 C 0.1117(10) 0.4043(4) 0.8920(6) 0.0486(19) Uani 1 1 d . . . H20A H 0.0894 0.4024 0.9684 0.058 Uiso 1 1 calc R . . C21 C 0.1296(9) 0.4600(4) 0.8430(6) 0.0452(18) Uani 1 1 d . . . H21A H 0.1181 0.4960 0.8837 0.054 Uiso 1 1 calc R . . C22 C 0.1663(8) 0.4607(3) 0.7285(5) 0.0319(14) Uani 1 1 d . . . N1 N 0.2158(7) 0.4208(2) 0.5564(4) 0.0284(11) Uani 1 1 d . . . N2 N 0.2730(7) 0.4742(2) 0.3564(4) 0.0266(11) Uani 1 1 d . . . N3 N 0.2912(7) 0.5697(2) 0.4255(4) 0.0304(12) Uani 1 1 d . . . H3B H 0.2908 0.5995 0.4732 0.037 Uiso 1 1 calc R . . N4 N 0.1974(7) 0.5075(2) 0.6541(4) 0.0327(12) Uani 1 1 d . . . H4B H 0.1992 0.5459 0.6695 0.039 Uiso 1 1 calc R . . O1 O -0.7246(5) 0.21036(19) -0.0342(4) 0.0347(10) Uani 1 1 d . . . O2 O -0.4970(5) 0.15091(18) -0.0720(3) 0.0287(9) Uani 1 1 d . . . O3 O 0.1551(6) 0.3439(2) 0.2235(4) 0.0398(11) Uani 1 1 d . . . O4 O -0.0555(5) 0.37498(19) 0.3276(3) 0.0326(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0264(4) 0.0250(4) 0.0294(4) -0.0031(4) 0.0017(3) 0.0004(4) C1 0.033(4) 0.026(3) 0.025(3) 0.010(3) 0.001(3) 0.001(3) C2 0.030(3) 0.025(3) 0.028(3) 0.001(3) 0.002(3) -0.002(3) C3 0.026(3) 0.037(4) 0.033(3) 0.001(3) 0.007(3) 0.004(3) C4 0.028(3) 0.036(4) 0.031(3) -0.009(3) 0.007(3) 0.001(3) C5 0.028(3) 0.028(3) 0.020(3) 0.004(2) 0.001(2) -0.001(3) C6 0.027(3) 0.032(3) 0.030(3) -0.001(3) 0.003(3) -0.001(3) C7 0.029(3) 0.026(3) 0.028(3) -0.005(3) 0.005(3) 0.004(3) C8 0.034(4) 0.028(3) 0.031(3) -0.001(3) 0.000(3) 0.000(3) C9 0.021(3) 0.028(3) 0.036(4) 0.002(3) 0.006(3) 0.001(2) C10 0.039(4) 0.038(4) 0.037(4) -0.004(3) 0.012(3) -0.001(3) C11 0.045(4) 0.049(4) 0.036(4) 0.010(3) 0.015(3) 0.001(3) C12 0.044(4) 0.042(4) 0.050(4) 0.016(4) 0.010(3) -0.007(3) C13 0.044(4) 0.029(3) 0.047(4) 0.004(3) 0.002(3) -0.006(3) C14 0.027(3) 0.034(3) 0.036(4) 0.002(3) -0.001(3) -0.003(3) C15 0.020(3) 0.022(3) 0.033(3) 0.001(3) -0.001(2) 0.000(2) C16 0.021(3) 0.027(3) 0.027(3) -0.009(3) -0.002(2) 0.004(2) C17 0.023(3) 0.036(3) 0.034(4) 0.002(3) 0.005(3) -0.001(3) C18 0.043(4) 0.038(4) 0.042(4) 0.003(3) 0.008(3) -0.006(3) C19 0.049(5) 0.056(5) 0.048(5) 0.015(4) 0.015(4) -0.006(4) C20 0.046(4) 0.068(5) 0.034(4) 0.010(4) 0.012(3) 0.000(4) C21 0.041(4) 0.062(5) 0.034(4) -0.009(4) 0.010(3) 0.002(4) C22 0.021(3) 0.043(4) 0.031(3) -0.008(3) 0.001(3) 0.007(3) N1 0.032(3) 0.029(3) 0.025(3) -0.001(2) 0.005(2) 0.000(2) N2 0.030(3) 0.023(3) 0.027(3) -0.003(2) 0.003(2) -0.001(2) N3 0.034(3) 0.021(3) 0.036(3) -0.005(2) 0.004(2) -0.003(2) N4 0.037(3) 0.024(3) 0.036(3) -0.006(2) 0.001(2) 0.005(2) O1 0.024(2) 0.031(2) 0.048(3) -0.002(2) 0.0002(19) -0.0005(18) O2 0.028(2) 0.027(2) 0.030(2) -0.0015(18) 0.0027(18) -0.0019(18) O3 0.023(2) 0.052(3) 0.044(3) -0.018(2) 0.004(2) -0.005(2) O4 0.029(2) 0.036(2) 0.032(2) -0.008(2) 0.0034(18) -0.0050(19) _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 O2 2.101(4) 4_666 ? Co1 N2 2.103(5) . ? Co1 N1 2.115(5) . ? Co1 O4 2.158(4) . ? Co1 O3 2.161(4) . ? Co1 O1 2.194(4) 4_666 ? Co1 C8 2.478(6) . ? Co1 C1 2.483(6) 4_666 ? C1 O1 1.256(7) . ? C1 O2 1.293(7) . ? C1 C2 1.482(8) . ? C1 Co1 2.483(6) 4_465 ? C2 C7 1.389(8) . ? C2 C3 1.404(8) . ? C3 C4 1.383(8) . ? C3 H3A 0.9300 . ? C4 C5 1.397(8) . ? C4 H4A 0.9300 . ? C5 C6 1.397(8) . ? C5 C8 1.497(8) . ? C6 C7 1.391(8) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 O3 1.247(7) . ? C8 O4 1.275(7) . ? C9 N2 1.384(7) . ? C9 C10 1.396(8) . ? C9 C14 1.405(8) . ? C10 C11 1.375(9) . ? C10 H10A 0.9300 . ? C11 C12 1.398(10) . ? C11 H11A 0.9300 . ? C12 C13 1.379(9) . ? C12 H12A 0.9300 . ? C13 C14 1.390(9) . ? C13 H13A 0.9300 . ? C14 N3 1.388(8) . ? C15 N2 1.326(7) . ? C15 N3 1.361(7) . ? C15 C16 1.436(8) . ? C16 N1 1.338(7) . ? C16 N4 1.353(7) . ? C17 N1 1.387(7) . ? C17 C18 1.394(9) . ? C17 C22 1.396(8) . ? C18 C19 1.387(9) . ? C18 H18A 0.9300 . ? C19 C20 1.410(10) . ? C19 H19A 0.9300 . ? C20 C21 1.362(10) . ? C20 H20A 0.9300 . ? C21 C22 1.401(9) . ? C21 H21A 0.9300 . ? C22 N4 1.383(8) . ? N3 O2 2.784(6) 2 ? N3 H3B 0.8600 . ? N4 O4 2.793(6) 3_566 ? N4 H4B 0.8600 . ? O1 Co1 2.194(4) 4_465 ? O2 Co1 2.101(4) 4_465 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 N2 102.22(17) 4_666 . ? O2 Co1 N1 96.72(17) 4_666 . ? N2 Co1 N1 79.53(18) . . ? O2 Co1 O4 154.85(16) 4_666 . ? N2 Co1 O4 98.60(17) . . ? N1 Co1 O4 100.82(17) . . ? O2 Co1 O3 100.65(16) 4_666 . ? N2 Co1 O3 102.03(18) . . ? N1 Co1 O3 161.75(18) . . ? O4 Co1 O3 60.93(15) . . ? O2 Co1 O1 61.67(15) 4_666 4_666 ? N2 Co1 O1 161.27(17) . 4_666 ? N1 Co1 O1 92.37(18) . 4_666 ? O4 Co1 O1 99.51(16) . 4_666 ? O3 Co1 O1 90.96(17) . 4_666 ? O2 Co1 C8 127.70(18) 4_666 . ? N2 Co1 C8 104.86(19) . . ? N1 Co1 C8 131.6(2) . . ? O4 Co1 C8 30.96(17) . . ? O3 Co1 C8 30.22(18) . . ? O1 Co1 C8 93.17(18) 4_666 . ? O2 Co1 C1 31.38(17) 4_666 4_666 ? N2 Co1 C1 132.55(19) . 4_666 ? N1 Co1 C1 93.74(19) . 4_666 ? O4 Co1 C1 128.65(18) . 4_666 ? O3 Co1 C1 98.15(18) . 4_666 ? O1 Co1 C1 30.36(17) 4_666 4_666 ? C8 Co1 C1 113.77(19) . 4_666 ? O1 C1 O2 119.6(5) . . ? O1 C1 C2 122.0(5) . . ? O2 C1 C2 118.3(5) . . ? O1 C1 Co1 62.0(3) . 4_465 ? O2 C1 Co1 57.8(3) . 4_465 ? C2 C1 Co1 171.5(4) . 4_465 ? C7 C2 C3 119.4(5) . . ? C7 C2 C1 121.0(5) . . ? C3 C2 C1 119.5(5) . . ? C4 C3 C2 120.4(6) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 120.0(6) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 119.7(5) . . ? C6 C5 C8 119.0(5) . . ? C4 C5 C8 121.1(5) . . ? C7 C6 C5 120.0(5) . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C2 C7 C6 120.3(5) . . ? C2 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? O3 C8 O4 120.5(5) . . ? O3 C8 C5 120.7(5) . . ? O4 C8 C5 118.8(5) . . ? O3 C8 Co1 60.7(3) . . ? O4 C8 Co1 60.5(3) . . ? C5 C8 Co1 169.0(4) . . ? N2 C9 C10 130.7(6) . . ? N2 C9 C14 109.0(5) . . ? C10 C9 C14 120.3(6) . . ? C11 C10 C9 117.2(6) . . ? C11 C10 H10A 121.4 . . ? C9 C10 H10A 121.4 . . ? C10 C11 C12 122.0(6) . . ? C10 C11 H11A 119.0 . . ? C12 C11 H11A 119.0 . . ? C13 C12 C11 121.7(6) . . ? C13 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? C12 C13 C14 116.4(6) . . ? C12 C13 H13A 121.8 . . ? C14 C13 H13A 121.8 . . ? N3 C14 C13 131.6(6) . . ? N3 C14 C9 106.1(5) . . ? C13 C14 C9 122.3(6) . . ? N2 C15 N3 112.9(5) . . ? N2 C15 C16 118.6(5) . . ? N3 C15 C16 128.5(5) . . ? N1 C16 N4 112.0(5) . . ? N1 C16 C15 117.9(5) . . ? N4 C16 C15 130.0(5) . . ? N1 C17 C18 129.5(6) . . ? N1 C17 C22 109.1(5) . . ? C18 C17 C22 121.3(6) . . ? C19 C18 C17 117.1(7) . . ? C19 C18 H18A 121.5 . . ? C17 C18 H18A 121.5 . . ? C18 C19 C20 120.9(7) . . ? C18 C19 H19A 119.5 . . ? C20 C19 H19A 119.5 . . ? C21 C20 C19 122.3(6) . . ? C21 C20 H20A 118.9 . . ? C19 C20 H20A 118.9 . . ? C20 C21 C22 117.0(7) . . ? C20 C21 H21A 121.5 . . ? C22 C21 H21A 121.5 . . ? N4 C22 C17 106.0(5) . . ? N4 C22 C21 132.6(6) . . ? C17 C22 C21 121.4(6) . . ? C16 N1 C17 105.6(5) . . ? C16 N1 Co1 111.5(4) . . ? C17 N1 Co1 142.5(4) . . ? C15 N2 C9 105.7(5) . . ? C15 N2 Co1 112.1(4) . . ? C9 N2 Co1 142.2(4) . . ? C15 N3 C14 106.3(5) . . ? C15 N3 O2 126.1(4) . 2 ? C14 N3 O2 114.8(4) . 2 ? C15 N3 H3B 126.8 . . ? C14 N3 H3B 126.8 . . ? O2 N3 H3B 32.7 2 . ? C16 N4 C22 107.3(5) . . ? C16 N4 O4 123.2(4) . 3_566 ? C22 N4 O4 122.9(4) . 3_566 ? C16 N4 H4B 126.3 . . ? C22 N4 H4B 126.3 . . ? O4 N4 H4B 23.0 3_566 . ? C1 O1 Co1 87.6(4) . 4_465 ? C1 O2 Co1 90.8(3) . 4_465 ? C8 O3 Co1 89.1(4) . . ? C8 O4 Co1 88.5(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 C7 -164.5(6) . . . . ? O2 C1 C2 C7 19.2(8) . . . . ? Co1 C1 C2 C7 80(3) 4_465 . . . ? O1 C1 C2 C3 19.2(8) . . . . ? O2 C1 C2 C3 -157.1(5) . . . . ? Co1 C1 C2 C3 -97(3) 4_465 . . . ? C7 C2 C3 C4 -4.3(9) . . . . ? C1 C2 C3 C4 172.0(5) . . . . ? C2 C3 C4 C5 2.3(9) . . . . ? C3 C4 C5 C6 1.9(9) . . . . ? C3 C4 C5 C8 -173.7(6) . . . . ? C4 C5 C6 C7 -4.0(9) . . . . ? C8 C5 C6 C7 171.6(5) . . . . ? C3 C2 C7 C6 2.2(9) . . . . ? C1 C2 C7 C6 -174.1(5) . . . . ? C5 C6 C7 C2 2.0(9) . . . . ? C6 C5 C8 O3 6.5(9) . . . . ? C4 C5 C8 O3 -177.9(6) . . . . ? C6 C5 C8 O4 -170.6(5) . . . . ? C4 C5 C8 O4 4.9(9) . . . . ? C6 C5 C8 Co1 -87(2) . . . . ? C4 C5 C8 Co1 88(2) . . . . ? O2 Co1 C8 O3 -30.4(5) 4_666 . . . ? N2 Co1 C8 O3 88.4(4) . . . . ? N1 Co1 C8 O3 177.5(3) . . . . ? O4 Co1 C8 O3 170.3(6) . . . . ? O1 Co1 C8 O3 -86.5(4) 4_666 . . . ? C1 Co1 C8 O3 -63.4(4) 4_666 . . . ? O2 Co1 C8 O4 159.3(3) 4_666 . . . ? N2 Co1 C8 O4 -81.9(4) . . . . ? N1 Co1 C8 O4 7.2(5) . . . . ? O3 Co1 C8 O4 -170.3(6) . . . . ? O1 Co1 C8 O4 103.3(3) 4_666 . . . ? C1 Co1 C8 O4 126.3(3) 4_666 . . . ? O2 Co1 C8 C5 70(2) 4_666 . . . ? N2 Co1 C8 C5 -171(2) . . . . ? N1 Co1 C8 C5 -82(2) . . . . ? O4 Co1 C8 C5 -90(2) . . . . ? O3 Co1 C8 C5 100(2) . . . . ? O1 Co1 C8 C5 14(2) 4_666 . . . ? C1 Co1 C8 C5 37(2) 4_666 . . . ? N2 C9 C10 C11 -179.5(6) . . . . ? C14 C9 C10 C11 -0.5(9) . . . . ? C9 C10 C11 C12 -0.4(10) . . . . ? C10 C11 C12 C13 1.6(11) . . . . ? C11 C12 C13 C14 -1.7(10) . . . . ? C12 C13 C14 N3 -179.8(6) . . . . ? C12 C13 C14 C9 0.7(9) . . . . ? N2 C9 C14 N3 -0.1(6) . . . . ? C10 C9 C14 N3 -179.2(5) . . . . ? N2 C9 C14 C13 179.6(6) . . . . ? C10 C9 C14 C13 0.4(9) . . . . ? N2 C15 C16 N1 4.4(8) . . . . ? N3 C15 C16 N1 -174.2(5) . . . . ? N2 C15 C16 N4 -176.3(6) . . . . ? N3 C15 C16 N4 5.0(10) . . . . ? N1 C17 C18 C19 179.9(6) . . . . ? C22 C17 C18 C19 0.3(10) . . . . ? C17 C18 C19 C20 -0.3(10) . . . . ? C18 C19 C20 C21 0.7(11) . . . . ? C19 C20 C21 C22 -1.1(11) . . . . ? N1 C17 C22 N4 -1.2(7) . . . . ? C18 C17 C22 N4 178.5(6) . . . . ? N1 C17 C22 C21 179.5(5) . . . . ? C18 C17 C22 C21 -0.8(9) . . . . ? C20 C21 C22 N4 -177.9(7) . . . . ? C20 C21 C22 C17 1.1(10) . . . . ? N4 C16 N1 C17 0.2(7) . . . . ? C15 C16 N1 C17 179.5(5) . . . . ? N4 C16 N1 Co1 174.4(4) . . . . ? C15 C16 N1 Co1 -6.2(6) . . . . ? C18 C17 N1 C16 -179.0(6) . . . . ? C22 C17 N1 C16 0.7(6) . . . . ? C18 C17 N1 Co1 9.8(11) . . . . ? C22 C17 N1 Co1 -170.5(5) . . . . ? O2 Co1 N1 C16 105.9(4) 4_666 . . . ? N2 Co1 N1 C16 4.7(4) . . . . ? O4 Co1 N1 C16 -92.2(4) . . . . ? O3 Co1 N1 C16 -92.0(7) . . . . ? O1 Co1 N1 C16 167.7(4) 4_666 . . . ? C8 Co1 N1 C16 -96.0(4) . . . . ? C1 Co1 N1 C16 137.3(4) 4_666 . . . ? O2 Co1 N1 C17 -83.2(7) 4_666 . . . ? N2 Co1 N1 C17 175.5(7) . . . . ? O4 Co1 N1 C17 78.7(7) . . . . ? O3 Co1 N1 C17 78.8(9) . . . . ? O1 Co1 N1 C17 -21.5(7) 4_666 . . . ? C8 Co1 N1 C17 74.9(7) . . . . ? C1 Co1 N1 C17 -51.9(7) 4_666 . . . ? N3 C15 N2 C9 -0.8(6) . . . . ? C16 C15 N2 C9 -179.6(5) . . . . ? N3 C15 N2 Co1 178.8(4) . . . . ? C16 C15 N2 Co1 -0.1(6) . . . . ? C10 C9 N2 C15 179.5(6) . . . . ? C14 C9 N2 C15 0.5(6) . . . . ? C10 C9 N2 Co1 0.2(11) . . . . ? C14 C9 N2 Co1 -178.9(5) . . . . ? O2 Co1 N2 C15 -97.1(4) 4_666 . . . ? N1 Co1 N2 C15 -2.5(4) . . . . ? O4 Co1 N2 C15 97.1(4) . . . . ? O3 Co1 N2 C15 159.0(4) . . . . ? O1 Co1 N2 C15 -68.0(7) 4_666 . . . ? C8 Co1 N2 C15 128.0(4) . . . . ? C1 Co1 N2 C15 -87.9(4) 4_666 . . . ? O2 Co1 N2 C9 82.2(6) 4_666 . . . ? N1 Co1 N2 C9 176.9(6) . . . . ? O4 Co1 N2 C9 -83.6(6) . . . . ? O3 Co1 N2 C9 -21.6(6) . . . . ? O1 Co1 N2 C9 111.3(7) 4_666 . . . ? C8 Co1 N2 C9 -52.6(7) . . . . ? C1 Co1 N2 C9 91.5(7) 4_666 . . . ? N2 C15 N3 C14 0.7(7) . . . . ? C16 C15 N3 C14 179.4(6) . . . . ? N2 C15 N3 O2 -138.3(4) . . . 2 ? C16 C15 N3 O2 40.5(8) . . . 2 ? C13 C14 N3 C15 -180.0(7) . . . . ? C9 C14 N3 C15 -0.3(6) . . . . ? C13 C14 N3 O2 -35.7(8) . . . 2 ? C9 C14 N3 O2 143.9(4) . . . 2 ? N1 C16 N4 C22 -0.9(7) . . . . ? C15 C16 N4 C22 179.8(6) . . . . ? N1 C16 N4 O4 -153.1(4) . . . 3_566 ? C15 C16 N4 O4 27.6(8) . . . 3_566 ? C17 C22 N4 C16 1.3(6) . . . . ? C21 C22 N4 C16 -179.6(7) . . . . ? C17 C22 N4 O4 153.6(4) . . . 3_566 ? C21 C22 N4 O4 -27.3(9) . . . 3_566 ? O2 C1 O1 Co1 4.9(5) . . . 4_465 ? C2 C1 O1 Co1 -171.3(5) . . . 4_465 ? O1 C1 O2 Co1 -5.1(5) . . . 4_465 ? C2 C1 O2 Co1 171.3(4) . . . 4_465 ? O4 C8 O3 Co1 9.8(6) . . . . ? C5 C8 O3 Co1 -167.3(5) . . . . ? O2 Co1 O3 C8 156.0(4) 4_666 . . . ? N2 Co1 O3 C8 -98.9(4) . . . . ? N1 Co1 O3 C8 -5.9(8) . . . . ? O4 Co1 O3 C8 -5.7(3) . . . . ? O1 Co1 O3 C8 94.7(4) 4_666 . . . ? C1 Co1 O3 C8 124.3(4) 4_666 . . . ? O3 C8 O4 Co1 -9.8(6) . . . . ? C5 C8 O4 Co1 167.4(5) . . . . ? O2 Co1 O4 C8 -41.1(5) 4_666 . . . ? N2 Co1 O4 C8 104.6(4) . . . . ? N1 Co1 O4 C8 -174.5(3) . . . . ? O3 Co1 O4 C8 5.6(3) . . . . ? O1 Co1 O4 C8 -80.2(4) 4_666 . . . ? C1 Co1 O4 C8 -70.7(4) 4_666 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B O2 0.86 2.11 2.784(6) 134.6 2 N4 H4B O4 0.86 2.03 2.793(6) 147.5 3_566 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.491 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.098 #===============================END data_2 _database_code_depnum_ccdc_archive 'CCDC 286937' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H14 N4 Ni O4' _chemical_formula_weight 457.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2779(11) _cell_length_b 21.675(3) _cell_length_c 11.786(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.484(7) _cell_angle_gamma 90.00 _cell_volume 1843.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2419 _cell_measurement_theta_min 3.1195 _cell_measurement_theta_max 25.0264 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.5000 _exptl_crystal_size_mid 0.0800 _exptl_crystal_size_min 0.0300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7438 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 CCD _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11638 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_av_sigmaI/netI 0.0877 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3245 _reflns_number_gt 2321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _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^)+(0.0399P)^2^+1.9181P] 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 3245 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.27011(9) 0.38083(3) 0.10570(6) 0.0267(2) Uani 1 1 d . . . C1 C 1.0554(7) 0.1997(2) 0.5299(4) 0.0250(12) Uani 1 1 d . . . C2 C 0.9188(7) 0.2437(2) 0.4690(4) 0.0260(12) Uani 1 1 d . . . C3 C 0.7349(7) 0.2408(2) 0.4885(4) 0.0280(12) Uani 1 1 d . . . H3A H 0.6999 0.2145 0.5443 0.034 Uiso 1 1 calc R . . C4 C 0.6032(7) 0.2774(2) 0.4238(4) 0.0291(13) Uani 1 1 d . . . H4A H 0.4805 0.2765 0.4380 0.035 Uiso 1 1 calc R . . C5 C 0.6545(7) 0.3154(2) 0.3377(4) 0.0243(12) Uani 1 1 d . . . C6 C 0.8413(7) 0.3195(2) 0.3221(4) 0.0289(13) Uani 1 1 d . . . H6A H 0.8771 0.3460 0.2669 0.035 Uiso 1 1 calc R . . C7 C 0.9724(7) 0.2846(2) 0.3880(5) 0.0308(13) Uani 1 1 d . . . H7A H 1.0968 0.2882 0.3785 0.037 Uiso 1 1 calc R . . C8 C 0.5090(8) 0.3474(2) 0.2577(4) 0.0261(12) Uani 1 1 d . . . C9 C 0.3178(7) 0.4047(2) -0.1649(5) 0.0295(13) Uani 1 1 d . . . C10 C 0.3365(8) 0.3474(2) -0.2164(5) 0.0361(14) Uani 1 1 d . . . H10A H 0.3263 0.3109 -0.1763 0.043 Uiso 1 1 calc R . . C11 C 0.3704(9) 0.3470(3) -0.3288(6) 0.0493(17) Uani 1 1 d . . . H11A H 0.3823 0.3095 -0.3657 0.059 Uiso 1 1 calc R . . C12 C 0.3872(8) 0.4020(3) -0.3875(5) 0.0486(17) Uani 1 1 d . . . H12A H 0.4131 0.4000 -0.4626 0.058 Uiso 1 1 calc R . . C13 C 0.3672(8) 0.4590(3) -0.3398(5) 0.0409(15) Uani 1 1 d . . . H13A H 0.3767 0.4953 -0.3805 0.049 Uiso 1 1 calc R . . C14 C 0.3316(7) 0.4587(2) -0.2262(4) 0.0277(12) Uani 1 1 d . . . C15 C 0.2722(7) 0.4805(2) -0.0517(4) 0.0268(12) Uani 1 1 d . . . C16 C 0.2387(7) 0.5083(2) 0.0547(4) 0.0255(12) Uani 1 1 d . . . C17 C 0.1916(7) 0.5109(2) 0.2326(5) 0.0273(12) Uani 1 1 d . . . C18 C 0.1687(8) 0.4978(3) 0.3456(5) 0.0369(14) Uani 1 1 d . . . H18A H 0.1773 0.4578 0.3742 0.044 Uiso 1 1 calc R . . C19 C 0.1323(8) 0.5474(3) 0.4129(5) 0.0390(15) Uani 1 1 d . . . H19A H 0.1160 0.5402 0.4887 0.047 Uiso 1 1 calc R . . C20 C 0.1191(8) 0.6082(3) 0.3718(5) 0.0428(15) Uani 1 1 d . . . H20A H 0.0941 0.6401 0.4202 0.051 Uiso 1 1 calc R . . C21 C 0.1429(7) 0.6207(3) 0.2600(5) 0.0377(14) Uani 1 1 d . . . H21A H 0.1353 0.6608 0.2319 0.045 Uiso 1 1 calc R . . C22 C 0.1784(7) 0.5717(2) 0.1912(5) 0.0287(13) Uani 1 1 d . . . N1 N 0.2819(6) 0.41926(18) -0.0545(3) 0.0261(10) Uani 1 1 d . . . N2 N 0.2312(6) 0.47192(18) 0.1448(4) 0.0270(10) Uani 1 1 d . . . N3 N 0.2086(6) 0.56840(18) 0.0769(4) 0.0299(11) Uani 1 1 d . . . H3B H 0.2083 0.5987 0.0298 0.036 Uiso 1 1 calc R . . N4 N 0.3011(6) 0.50673(18) -0.1523(4) 0.0294(11) Uani 1 1 d . . . H4B H 0.3006 0.5455 -0.1676 0.035 Uiso 1 1 calc R . . O1 O 1.2272(5) 0.20958(15) 0.5363(3) 0.0315(9) Uani 1 1 d . . . O2 O 0.9968(5) 0.14953(14) 0.5705(3) 0.0255(8) Uani 1 1 d . . . O3 O 0.5557(5) 0.37477(14) 0.1691(3) 0.0271(8) Uani 1 1 d . . . O4 O 0.3422(5) 0.34453(16) 0.2728(3) 0.0329(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0276(4) 0.0218(3) 0.0298(4) 0.0022(3) 0.0001(3) -0.0005(3) C1 0.029(3) 0.021(3) 0.025(3) -0.006(2) 0.002(2) 0.003(2) C2 0.028(3) 0.021(3) 0.028(3) -0.004(2) 0.001(2) 0.004(2) C3 0.024(3) 0.032(3) 0.027(3) 0.007(2) 0.001(2) 0.000(2) C4 0.028(3) 0.027(3) 0.034(3) -0.001(2) 0.011(3) -0.001(2) C5 0.024(3) 0.022(3) 0.027(3) 0.000(2) 0.001(2) 0.005(2) C6 0.031(3) 0.024(3) 0.033(3) 0.011(2) 0.006(3) 0.004(2) C7 0.026(3) 0.031(3) 0.036(3) 0.002(3) 0.007(3) -0.001(3) C8 0.031(3) 0.020(2) 0.027(3) -0.004(2) 0.000(3) -0.001(2) C9 0.021(3) 0.034(3) 0.033(3) -0.001(3) 0.001(3) 0.001(2) C10 0.037(4) 0.032(3) 0.041(4) -0.004(3) 0.010(3) 0.001(3) C11 0.053(4) 0.046(4) 0.049(4) -0.014(3) 0.008(3) 0.008(3) C12 0.044(4) 0.065(4) 0.037(4) -0.004(3) 0.008(3) 0.005(3) C13 0.029(4) 0.054(4) 0.040(4) 0.010(3) 0.006(3) -0.004(3) C14 0.023(3) 0.031(3) 0.028(3) -0.003(3) -0.001(2) -0.006(2) C15 0.020(3) 0.032(3) 0.027(3) 0.006(2) 0.000(2) -0.001(2) C16 0.024(3) 0.023(3) 0.028(3) 0.002(2) -0.001(2) -0.002(2) C17 0.021(3) 0.025(3) 0.035(3) -0.001(2) -0.001(3) -0.001(2) C18 0.040(4) 0.035(3) 0.037(3) 0.003(3) 0.009(3) 0.001(3) C19 0.039(4) 0.050(4) 0.028(3) -0.002(3) 0.006(3) -0.003(3) C20 0.042(4) 0.041(4) 0.045(4) -0.015(3) 0.003(3) 0.000(3) C21 0.036(4) 0.034(3) 0.042(4) -0.007(3) -0.003(3) 0.007(3) C22 0.028(3) 0.028(3) 0.029(3) -0.004(2) -0.001(2) 0.002(2) N1 0.028(3) 0.024(2) 0.026(2) 0.0024(19) 0.003(2) 0.0006(19) N2 0.028(3) 0.024(2) 0.029(3) 0.000(2) 0.004(2) 0.0009(19) N3 0.034(3) 0.023(2) 0.033(3) 0.004(2) 0.001(2) 0.001(2) N4 0.033(3) 0.023(2) 0.032(3) 0.008(2) 0.004(2) -0.006(2) O1 0.025(2) 0.0267(19) 0.041(2) 0.0004(17) -0.0025(18) 0.0004(17) O2 0.031(2) 0.0198(17) 0.026(2) 0.0009(16) 0.0039(17) 0.0004(16) O3 0.025(2) 0.0297(19) 0.025(2) 0.0054(17) 0.0010(16) 0.0008(16) O4 0.020(2) 0.043(2) 0.034(2) 0.0144(18) 0.0009(17) 0.0039(17) _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 N2 2.055(4) . ? Ni1 N1 2.076(4) . ? Ni1 O2 2.085(3) 4_465 ? Ni1 O3 2.119(3) . ? Ni1 O4 2.123(4) . ? Ni1 O1 2.131(3) 4_465 ? Ni1 C1 2.434(5) 4_465 ? Ni1 C8 2.439(5) . ? C1 O1 1.261(6) . ? C1 O2 1.283(6) . ? C1 C2 1.493(7) . ? C1 Ni1 2.434(5) 4_666 ? C2 C3 1.389(7) . ? C2 C7 1.395(7) . ? C3 C4 1.393(7) . ? C3 H3A 0.9300 . ? C4 C5 1.396(7) . ? C4 H4A 0.9300 . ? C5 C6 1.398(7) . ? C5 C8 1.494(7) . ? C6 C7 1.376(7) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 O4 1.251(6) . ? C8 O3 1.285(6) . ? C9 C14 1.385(7) . ? C9 N1 1.396(6) . ? C9 C10 1.398(7) . ? C10 C11 1.379(8) . ? C10 H10A 0.9300 . ? C11 C12 1.392(8) . ? C11 H11A 0.9300 . ? C12 C13 1.372(8) . ? C12 H12A 0.9300 . ? C13 C14 1.397(7) . ? C13 H13A 0.9300 . ? C14 N4 1.393(6) . ? C15 N1 1.330(6) . ? C15 N4 1.356(6) . ? C15 C16 1.440(7) . ? C16 N2 1.331(6) . ? C16 N3 1.352(6) . ? C17 C18 1.392(7) . ? C17 N2 1.394(6) . ? C17 C22 1.404(7) . ? C18 C19 1.382(7) . ? C18 H18A 0.9300 . ? C19 C20 1.402(7) . ? C19 H19A 0.9300 . ? C20 C21 1.378(8) . ? C20 H20A 0.9300 . ? C21 C22 1.381(7) . ? C21 H21A 0.9300 . ? C22 N3 1.395(6) . ? N3 O2 2.769(5) 2_655 ? N3 H3B 0.8600 . ? N4 O3 2.789(5) 3_665 ? N4 H4B 0.8600 . ? O1 Ni1 2.131(3) 4_666 ? O2 Ni1 2.085(3) 4_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 80.91(16) . . ? N2 Ni1 O2 101.08(15) . 4_465 ? N1 Ni1 O2 95.56(15) . 4_465 ? N2 Ni1 O3 97.93(14) . . ? N1 Ni1 O3 100.98(15) . . ? O2 Ni1 O3 156.51(13) 4_465 . ? N2 Ni1 O4 99.93(15) . . ? N1 Ni1 O4 163.41(15) . . ? O2 Ni1 O4 100.49(13) 4_465 . ? O3 Ni1 O4 62.44(13) . . ? N2 Ni1 O1 162.16(15) . 4_465 ? N1 Ni1 O1 92.36(15) . 4_465 ? O2 Ni1 O1 62.92(13) 4_465 4_465 ? O3 Ni1 O1 99.57(13) . 4_465 ? O4 Ni1 O1 91.23(14) . 4_465 ? N2 Ni1 C1 132.12(17) . 4_465 ? N1 Ni1 C1 93.12(16) . 4_465 ? O2 Ni1 C1 31.81(14) 4_465 4_465 ? O3 Ni1 C1 129.66(15) . 4_465 ? O4 Ni1 C1 98.29(15) . 4_465 ? O1 Ni1 C1 31.17(14) 4_465 4_465 ? N2 Ni1 C8 103.08(16) . . ? N1 Ni1 C8 132.65(18) . . ? O2 Ni1 C8 128.53(15) 4_465 . ? O3 Ni1 C8 31.78(14) . . ? O4 Ni1 C8 30.85(15) . . ? O1 Ni1 C8 93.65(14) 4_465 . ? C1 Ni1 C8 114.76(16) 4_465 . ? O1 C1 O2 119.8(5) . . ? O1 C1 C2 120.9(4) . . ? O2 C1 C2 119.2(5) . . ? O1 C1 Ni1 61.0(3) . 4_666 ? O2 C1 Ni1 58.9(2) . 4_666 ? C2 C1 Ni1 172.1(3) . 4_666 ? C3 C2 C7 120.3(5) . . ? C3 C2 C1 119.2(5) . . ? C7 C2 C1 120.4(5) . . ? C2 C3 C4 119.5(5) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C3 C4 C5 120.3(5) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? C4 C5 C6 119.3(5) . . ? C4 C5 C8 119.9(5) . . ? C6 C5 C8 120.6(5) . . ? C7 C6 C5 120.4(5) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C2 120.0(5) . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? O4 C8 O3 120.2(5) . . ? O4 C8 C5 120.6(5) . . ? O3 C8 C5 119.1(5) . . ? O4 C8 Ni1 60.5(3) . . ? O3 C8 Ni1 60.3(3) . . ? C5 C8 Ni1 168.7(3) . . ? C14 C9 N1 109.3(4) . . ? C14 C9 C10 120.5(5) . . ? N1 C9 C10 130.2(5) . . ? C11 C10 C9 117.6(5) . . ? C11 C10 H10A 121.2 . . ? C9 C10 H10A 121.2 . . ? C10 C11 C12 120.6(6) . . ? C10 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C13 C12 C11 123.2(6) . . ? C13 C12 H12A 118.4 . . ? C11 C12 H12A 118.4 . . ? C12 C13 C14 115.6(5) . . ? C12 C13 H13A 122.2 . . ? C14 C13 H13A 122.2 . . ? C9 C14 N4 106.1(4) . . ? C9 C14 C13 122.5(5) . . ? N4 C14 C13 131.4(5) . . ? N1 C15 N4 112.4(4) . . ? N1 C15 C16 117.1(4) . . ? N4 C15 C16 130.5(5) . . ? N2 C16 N3 113.0(4) . . ? N2 C16 C15 118.5(4) . . ? N3 C16 C15 128.5(5) . . ? C18 C17 N2 130.4(5) . . ? C18 C17 C22 120.8(5) . . ? N2 C17 C22 108.8(4) . . ? C19 C18 C17 116.5(5) . . ? C19 C18 H18A 121.7 . . ? C17 C18 H18A 121.7 . . ? C18 C19 C20 122.8(5) . . ? C18 C19 H19A 118.6 . . ? C20 C19 H19A 118.6 . . ? C21 C20 C19 120.2(5) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C20 C21 C22 117.8(5) . . ? C20 C21 H21A 121.1 . . ? C22 C21 H21A 121.1 . . ? C21 C22 N3 132.2(5) . . ? C21 C22 C17 121.9(5) . . ? N3 C22 C17 106.0(4) . . ? C15 N1 C9 105.4(4) . . ? C15 N1 Ni1 111.7(3) . . ? C9 N1 Ni1 142.4(3) . . ? C16 N2 C17 105.5(4) . . ? C16 N2 Ni1 111.7(3) . . ? C17 N2 Ni1 142.8(3) . . ? C16 N3 C22 106.7(4) . . ? C16 N3 O2 125.3(3) . 2_655 ? C22 N3 O2 115.7(3) . 2_655 ? C16 N3 H3B 126.7 . . ? C22 N3 H3B 126.7 . . ? O2 N3 H3B 32.2 2_655 . ? C15 N4 C14 106.8(4) . . ? C15 N4 O3 123.3(3) . 3_665 ? C14 N4 O3 123.5(3) . 3_665 ? C15 N4 H4B 126.6 . . ? C14 N4 H4B 126.6 . . ? O3 N4 H4B 22.5 3_665 . ? C1 O1 Ni1 87.8(3) . 4_666 ? C1 O2 Ni1 89.3(3) . 4_666 ? C8 O3 Ni1 87.9(3) . . ? C8 O4 Ni1 88.7(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 -163.2(5) . . . . ? O2 C1 C2 C3 20.7(7) . . . . ? Ni1 C1 C2 C3 95(3) 4_666 . . . ? O1 C1 C2 C7 21.1(7) . . . . ? O2 C1 C2 C7 -155.0(5) . . . . ? Ni1 C1 C2 C7 -81(3) 4_666 . . . ? C7 C2 C3 C4 2.1(7) . . . . ? C1 C2 C3 C4 -173.6(4) . . . . ? C2 C3 C4 C5 1.9(7) . . . . ? C3 C4 C5 C6 -4.2(7) . . . . ? C3 C4 C5 C8 171.1(4) . . . . ? C4 C5 C6 C7 2.5(7) . . . . ? C8 C5 C6 C7 -172.8(5) . . . . ? C5 C6 C7 C2 1.5(8) . . . . ? C3 C2 C7 C6 -3.8(8) . . . . ? C1 C2 C7 C6 171.9(5) . . . . ? C4 C5 C8 O4 5.9(7) . . . . ? C6 C5 C8 O4 -178.8(4) . . . . ? C4 C5 C8 O3 -169.8(4) . . . . ? C6 C5 C8 O3 5.5(7) . . . . ? C4 C5 C8 Ni1 -86(2) . . . . ? C6 C5 C8 Ni1 89(2) . . . . ? N2 Ni1 C8 O4 87.5(3) . . . . ? N1 Ni1 C8 O4 177.1(3) . . . . ? O2 Ni1 C8 O4 -28.4(3) 4_465 . . . ? O3 Ni1 C8 O4 171.4(4) . . . . ? O1 Ni1 C8 O4 -86.3(3) 4_465 . . . ? C1 Ni1 C8 O4 -62.4(3) 4_465 . . . ? N2 Ni1 C8 O3 -83.9(3) . . . . ? N1 Ni1 C8 O3 5.7(4) . . . . ? O2 Ni1 C8 O3 160.2(2) 4_465 . . . ? O4 Ni1 C8 O3 -171.4(4) . . . . ? O1 Ni1 C8 O3 102.3(3) 4_465 . . . ? C1 Ni1 C8 O3 126.2(3) 4_465 . . . ? N2 Ni1 C8 C5 -174(2) . . . . ? N1 Ni1 C8 C5 -84(2) . . . . ? O2 Ni1 C8 C5 70(2) 4_465 . . . ? O3 Ni1 C8 C5 -90(2) . . . . ? O4 Ni1 C8 C5 98(2) . . . . ? O1 Ni1 C8 C5 12(2) 4_465 . . . ? C1 Ni1 C8 C5 36(2) 4_465 . . . ? C14 C9 C10 C11 0.6(8) . . . . ? N1 C9 C10 C11 179.3(6) . . . . ? C9 C10 C11 C12 0.6(9) . . . . ? C10 C11 C12 C13 -1.6(10) . . . . ? C11 C12 C13 C14 1.1(9) . . . . ? N1 C9 C14 N4 -0.8(6) . . . . ? C10 C9 C14 N4 178.2(5) . . . . ? N1 C9 C14 C13 180.0(5) . . . . ? C10 C9 C14 C13 -1.1(8) . . . . ? C12 C13 C14 C9 0.2(8) . . . . ? C12 C13 C14 N4 -178.8(5) . . . . ? N1 C15 C16 N2 4.2(7) . . . . ? N4 C15 C16 N2 -174.0(5) . . . . ? N1 C15 C16 N3 -174.3(5) . . . . ? N4 C15 C16 N3 7.6(9) . . . . ? N2 C17 C18 C19 179.1(5) . . . . ? C22 C17 C18 C19 0.1(8) . . . . ? C17 C18 C19 C20 -0.2(9) . . . . ? C18 C19 C20 C21 -0.2(9) . . . . ? C19 C20 C21 C22 0.5(8) . . . . ? C20 C21 C22 N3 -180.0(5) . . . . ? C20 C21 C22 C17 -0.5(8) . . . . ? C18 C17 C22 C21 0.2(8) . . . . ? N2 C17 C22 C21 -179.0(5) . . . . ? C18 C17 C22 N3 179.8(5) . . . . ? N2 C17 C22 N3 0.6(6) . . . . ? N4 C15 N1 C9 -0.6(6) . . . . ? C16 C15 N1 C9 -179.0(4) . . . . ? N4 C15 N1 Ni1 172.9(3) . . . . ? C16 C15 N1 Ni1 -5.6(6) . . . . ? C14 C9 N1 C15 0.8(6) . . . . ? C10 C9 N1 C15 -178.0(6) . . . . ? C14 C9 N1 Ni1 -169.2(4) . . . . ? C10 C9 N1 Ni1 12.0(10) . . . . ? N2 Ni1 N1 C15 4.2(4) . . . . ? O2 Ni1 N1 C15 104.5(4) 4_465 . . . ? O3 Ni1 N1 C15 -92.2(4) . . . . ? O4 Ni1 N1 C15 -90.1(6) . . . . ? O1 Ni1 N1 C15 167.5(4) 4_465 . . . ? C1 Ni1 N1 C15 136.3(4) 4_465 . . . ? C8 Ni1 N1 C15 -95.3(4) . . . . ? N2 Ni1 N1 C9 173.8(6) . . . . ? O2 Ni1 N1 C9 -85.8(6) 4_465 . . . ? O3 Ni1 N1 C9 77.4(6) . . . . ? O4 Ni1 N1 C9 79.5(8) . . . . ? O1 Ni1 N1 C9 -22.8(6) 4_465 . . . ? C1 Ni1 N1 C9 -54.0(6) 4_465 . . . ? C8 Ni1 N1 C9 74.3(6) . . . . ? N3 C16 N2 C17 0.5(6) . . . . ? C15 C16 N2 C17 -178.1(4) . . . . ? N3 C16 N2 Ni1 178.3(3) . . . . ? C15 C16 N2 Ni1 -0.3(6) . . . . ? C18 C17 N2 C16 -179.8(6) . . . . ? C22 C17 N2 C16 -0.7(6) . . . . ? C18 C17 N2 Ni1 3.6(10) . . . . ? C22 C17 N2 Ni1 -177.3(4) . . . . ? N1 Ni1 N2 C16 -2.0(3) . . . . ? O2 Ni1 N2 C16 -96.0(3) 4_465 . . . ? O3 Ni1 N2 C16 97.9(3) . . . . ? O4 Ni1 N2 C16 161.2(3) . . . . ? O1 Ni1 N2 C16 -70.9(6) 4_465 . . . ? C1 Ni1 N2 C16 -88.0(4) 4_465 . . . ? C8 Ni1 N2 C16 129.8(4) . . . . ? N1 Ni1 N2 C17 174.4(6) . . . . ? O2 Ni1 N2 C17 80.5(6) 4_465 . . . ? O3 Ni1 N2 C17 -85.6(6) . . . . ? O4 Ni1 N2 C17 -22.4(6) . . . . ? O1 Ni1 N2 C17 105.6(7) 4_465 . . . ? C1 Ni1 N2 C17 88.5(6) 4_465 . . . ? C8 Ni1 N2 C17 -53.7(6) . . . . ? N2 C16 N3 C22 -0.2(6) . . . . ? C15 C16 N3 C22 178.3(5) . . . . ? N2 C16 N3 O2 -140.1(4) . . . 2_655 ? C15 C16 N3 O2 38.4(7) . . . 2_655 ? C21 C22 N3 C16 179.3(6) . . . . ? C17 C22 N3 C16 -0.3(6) . . . . ? C21 C22 N3 O2 -36.4(7) . . . 2_655 ? C17 C22 N3 O2 144.1(3) . . . 2_655 ? N1 C15 N4 C14 0.1(6) . . . . ? C16 C15 N4 C14 178.3(5) . . . . ? N1 C15 N4 O3 -152.7(3) . . . 3_665 ? C16 C15 N4 O3 25.5(7) . . . 3_665 ? C9 C14 N4 C15 0.4(6) . . . . ? C13 C14 N4 C15 179.6(6) . . . . ? C9 C14 N4 O3 153.2(3) . . . 3_665 ? C13 C14 N4 O3 -27.7(8) . . . 3_665 ? O2 C1 O1 Ni1 4.8(4) . . . 4_666 ? C2 C1 O1 Ni1 -171.2(4) . . . 4_666 ? O1 C1 O2 Ni1 -4.9(5) . . . 4_666 ? C2 C1 O2 Ni1 171.2(4) . . . 4_666 ? O4 C8 O3 Ni1 -8.7(4) . . . . ? C5 C8 O3 Ni1 167.1(4) . . . . ? N2 Ni1 O3 C8 102.1(3) . . . . ? N1 Ni1 O3 C8 -175.7(3) . . . . ? O2 Ni1 O3 C8 -41.8(4) 4_465 . . . ? O4 Ni1 O3 C8 5.0(3) . . . . ? O1 Ni1 O3 C8 -81.4(3) 4_465 . . . ? C1 Ni1 O3 C8 -72.2(3) 4_465 . . . ? O3 C8 O4 Ni1 8.6(4) . . . . ? C5 C8 O4 Ni1 -167.0(4) . . . . ? N2 Ni1 O4 C8 -98.9(3) . . . . ? N1 Ni1 O4 C8 -7.4(7) . . . . ? O2 Ni1 O4 C8 157.7(3) 4_465 . . . ? O3 Ni1 O4 C8 -5.1(3) . . . . ? O1 Ni1 O4 C8 95.1(3) 4_465 . . . ? C1 Ni1 O4 C8 125.6(3) 4_465 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B O2 0.86 2.09 2.769(5) 135.2 2_655 N4 H4B O3 0.86 2.02 2.789(5) 148.2 3_665 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.402 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.089 #===============================END data_3 _database_code_depnum_ccdc_archive 'CCDC 286938' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 Co N8 O5' _chemical_formula_weight 709.58 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 p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4816(5) _cell_length_b 22.1896(8) _cell_length_c 12.2588(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.1960(10) _cell_angle_gamma 90.00 _cell_volume 3290.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5765 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 25.01 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8008 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Simemens SMART CCD' _diffrn_measurement_method '\w scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11624 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5765 _reflns_number_gt 4181 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' Simens SMART ' _computing_cell_refinement ' Simens SMART ' _computing_data_reduction ' Simens SMART ' _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^)+(0.0283P)^2^+4.6297P] 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 5765 _refine_ls_number_parameters 555 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1374 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.236 _refine_ls_restrained_S_all 1.236 _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 0.34309(4) 0.91720(3) 0.56664(5) 0.03768(18) Uani 1 1 d . . . C1 C 0.4691(4) 1.0448(2) 0.7020(4) 0.0459(11) Uani 1 1 d . . . C2 C 0.5219(4) 1.0342(3) 0.8268(5) 0.0607(14) Uani 1 1 d . . . H2 H 0.517(4) 0.994(2) 0.852(4) 0.057(15) Uiso 1 1 d . . . C3 C 0.5751(5) 1.0823(3) 0.9007(6) 0.0725(17) Uani 1 1 d . . . H3 H 0.618(4) 1.073(2) 0.986(5) 0.073(17) Uiso 1 1 d . . . C4 C 0.5748(6) 1.1390(4) 0.8532(7) 0.089(2) Uani 1 1 d . . . H4 H 0.617(5) 1.170(3) 0.907(6) 0.11(2) Uiso 1 1 d . . . C5 C 0.5229(7) 1.1504(3) 0.7314(7) 0.084(2) Uani 1 1 d . . . H5 H 0.513(5) 1.187(3) 0.695(5) 0.08(2) Uiso 1 1 d . . . C6 C 0.4705(4) 1.1020(2) 0.6560(5) 0.0545(13) Uani 1 1 d . . . C7 C 0.2381(4) 0.9388(2) 0.2631(4) 0.0435(11) Uani 1 1 d . . . C8 C 0.1932(5) 0.8845(3) 0.2042(5) 0.0588(14) Uani 1 1 d . . . H8 H 0.207(3) 0.8498(19) 0.248(4) 0.035(12) Uiso 1 1 d . . . C9 C 0.1297(5) 0.8863(3) 0.0810(5) 0.0733(17) Uani 1 1 d . . . H9 H 0.095(4) 0.850(2) 0.033(5) 0.074(17) Uiso 1 1 d . . . C10 C 0.1117(6) 0.9397(3) 0.0154(5) 0.083(2) Uani 1 1 d . . . H10 H 0.067(4) 0.939(2) -0.070(5) 0.078(17) Uiso 1 1 d . . . C11 C 0.1548(5) 0.9935(3) 0.0705(5) 0.0737(18) Uani 1 1 d . . . H11 H 0.138(5) 1.030(3) 0.028(5) 0.084(19) Uiso 1 1 d . . . C12 C 0.2185(4) 0.9919(2) 0.1967(4) 0.0509(12) Uani 1 1 d . . . C13 C 0.3815(4) 1.0389(2) 0.5068(4) 0.0425(11) Uani 1 1 d . . . C14 C 0.3196(3) 1.0103(2) 0.3900(4) 0.0426(11) Uani 1 1 d . . . C15 C 0.2552(4) 0.7835(2) 0.4396(4) 0.0420(10) Uani 1 1 d . . . C16 C 0.3397(4) 0.7582(2) 0.4197(5) 0.0513(13) Uani 1 1 d . . . H16 H 0.406(4) 0.777(2) 0.450(4) 0.059(15) Uiso 1 1 d . . . C17 C 0.3173(5) 0.7051(3) 0.3553(5) 0.0609(14) Uani 1 1 d . . . H17 H 0.372(4) 0.686(2) 0.341(4) 0.051(13) Uiso 1 1 d . . . C18 C 0.2153(5) 0.6767(3) 0.3143(5) 0.0623(14) Uani 1 1 d . . . H18 H 0.198(4) 0.636(2) 0.270(5) 0.080(17) Uiso 1 1 d . . . C19 C 0.1299(5) 0.7009(2) 0.3327(4) 0.0576(13) Uani 1 1 d . . . H19 H 0.054(4) 0.684(2) 0.300(5) 0.077(17) Uiso 1 1 d . . . C20 C 0.1520(4) 0.7551(2) 0.3960(4) 0.0458(11) Uani 1 1 d . . . C21 C 0.1508(3) 0.97539(18) 0.6384(4) 0.0352(9) Uani 1 1 d . . . C22 C 0.1901(4) 1.0294(2) 0.6991(5) 0.0521(12) Uani 1 1 d . . . H22 H 0.251(3) 1.0458(18) 0.704(4) 0.038(12) Uiso 1 1 d . . . C23 C 0.1270(4) 1.0588(3) 0.7452(5) 0.0589(14) Uani 1 1 d . . . H23 H 0.149(4) 1.097(2) 0.784(4) 0.064(15) Uiso 1 1 d . . . C24 C 0.0257(4) 1.0353(2) 0.7308(5) 0.0554(13) Uani 1 1 d . . . H24 H -0.017(4) 1.058(2) 0.765(4) 0.061(14) Uiso 1 1 d . . . C25 C -0.0153(4) 0.9823(2) 0.6703(4) 0.0479(12) Uani 1 1 d . . . H25 H -0.082(3) 0.9658(18) 0.662(4) 0.039(12) Uiso 1 1 d . . . C26 C 0.0488(3) 0.95249(19) 0.6244(4) 0.0378(10) Uani 1 1 d . . . C27 C 0.1504(3) 0.83980(19) 0.4871(4) 0.0380(10) Uani 1 1 d . . . C28 C 0.1232(3) 0.89140(19) 0.5416(4) 0.0368(10) Uani 1 1 d . . . C29 C 0.5131(4) 0.8636(2) 0.7359(4) 0.0488(12) Uani 1 1 d . . . C30 C 0.5993(3) 0.8353(2) 0.8505(4) 0.0408(10) Uani 1 1 d . . . C31 C 0.5979(4) 0.8483(2) 0.9608(4) 0.0513(12) Uani 1 1 d . . . H31 H 0.550(3) 0.8763(18) 0.962(4) 0.038(11) Uiso 1 1 d . . . C32 C 0.6736(4) 0.8224(3) 1.0664(5) 0.0584(14) Uani 1 1 d . . . H32 H 0.678(4) 0.833(2) 1.141(4) 0.058(14) Uiso 1 1 d . . . C33 C 0.7513(4) 0.7829(2) 1.0644(4) 0.0513(12) Uani 1 1 d . . . H33 H 0.806(4) 0.7658(19) 1.139(4) 0.051(13) Uiso 1 1 d . . . C34 C 0.7550(3) 0.7693(2) 0.9554(4) 0.0425(11) Uani 1 1 d . . . C35 C 0.6781(4) 0.7961(2) 0.8483(4) 0.0438(11) Uani 1 1 d . . . H35 H 0.682(3) 0.7858(19) 0.777(4) 0.050(13) Uiso 1 1 d . . . C36 C 0.8425(4) 0.7274(2) 0.9542(4) 0.0506(12) Uani 1 1 d . . . N1 N 0.4115(3) 1.00583(16) 0.6060(3) 0.0429(9) Uani 1 1 d . . . N2 N 0.3029(3) 0.95148(16) 0.3866(3) 0.0407(9) Uani 1 1 d . . . N3 N 0.2520(3) 0.83728(16) 0.4969(3) 0.0398(8) Uani 1 1 d . . . N4 N 0.1960(3) 0.93589(15) 0.5845(3) 0.0359(8) Uani 1 1 d . . . N5 N 0.0872(3) 0.79269(17) 0.4294(3) 0.0440(9) Uani 1 1 d . . . H5A H 0.018(4) 0.787(2) 0.410(4) 0.062(16) Uiso 1 1 d . . . N6 N 0.0330(3) 0.89916(18) 0.5609(3) 0.0414(9) Uani 1 1 d . . . H6A H -0.022(4) 0.873(2) 0.540(5) 0.071(17) Uiso 1 1 d . . . N7 N 0.2725(4) 1.0371(2) 0.2797(4) 0.0535(11) Uani 1 1 d . . . H7A H 0.254(4) 1.073(3) 0.271(5) 0.075(19) Uiso 1 1 d . . . N8 N 0.4128(4) 1.0968(2) 0.5311(5) 0.0569(12) Uani 1 1 d . . . H8A H 0.414(5) 1.119(3) 0.480(5) 0.09(2) Uiso 1 1 d . . . O1 O 0.4344(3) 0.89112(15) 0.7435(3) 0.0594(9) Uani 1 1 d . . . O1W O 0.8358(4) 0.64873(19) 1.2320(5) 0.0780(13) Uani 1 1 d . . . H1C H 0.839(6) 0.660(3) 1.164(7) 0.12(3) Uiso 1 1 d . . . H1B H 0.852(7) 0.676(4) 1.280(8) 0.15(4) Uiso 1 1 d . . . O2 O 0.5205(3) 0.85941(17) 0.6381(3) 0.0656(10) Uani 1 1 d . . . O3 O 0.8772(3) 0.73810(17) 0.8754(3) 0.0650(10) Uani 1 1 d . . . O4 O 0.8780(3) 0.68615(16) 1.0323(3) 0.0612(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0335(3) 0.0403(3) 0.0415(3) 0.0046(3) 0.0186(2) 0.0015(3) C1 0.040(3) 0.052(3) 0.052(3) -0.011(2) 0.027(2) -0.009(2) C2 0.055(3) 0.072(4) 0.058(3) -0.013(3) 0.027(3) -0.011(3) C3 0.065(4) 0.101(5) 0.057(4) -0.024(4) 0.032(3) -0.015(4) C4 0.109(6) 0.090(5) 0.092(6) -0.043(5) 0.069(5) -0.044(4) C5 0.124(6) 0.066(4) 0.094(6) -0.026(4) 0.078(5) -0.029(4) C6 0.063(3) 0.051(3) 0.067(4) -0.014(3) 0.044(3) -0.015(2) C7 0.041(2) 0.053(3) 0.040(3) 0.003(2) 0.021(2) 0.012(2) C8 0.075(4) 0.054(3) 0.046(3) 0.002(3) 0.026(3) 0.015(3) C9 0.080(4) 0.083(4) 0.043(3) -0.012(3) 0.015(3) 0.015(4) C10 0.096(5) 0.102(5) 0.034(3) 0.000(4) 0.011(3) 0.029(4) C11 0.085(4) 0.084(5) 0.044(3) 0.023(3) 0.021(3) 0.033(4) C12 0.053(3) 0.057(3) 0.046(3) 0.010(3) 0.025(2) 0.015(2) C13 0.044(3) 0.044(3) 0.049(3) -0.001(2) 0.030(2) -0.005(2) C14 0.039(2) 0.046(3) 0.051(3) 0.010(2) 0.027(2) 0.007(2) C15 0.047(3) 0.040(3) 0.039(3) 0.007(2) 0.019(2) 0.006(2) C16 0.047(3) 0.058(3) 0.050(3) 0.005(3) 0.023(3) 0.012(3) C17 0.065(4) 0.068(4) 0.053(3) -0.005(3) 0.029(3) 0.021(3) C18 0.076(4) 0.061(4) 0.047(3) -0.013(3) 0.025(3) 0.006(3) C19 0.066(4) 0.058(3) 0.044(3) -0.016(3) 0.020(3) -0.011(3) C20 0.048(3) 0.052(3) 0.043(3) -0.002(2) 0.024(2) -0.007(2) C21 0.034(2) 0.037(2) 0.034(2) 0.0053(19) 0.0152(19) 0.0050(19) C22 0.046(3) 0.048(3) 0.067(3) 0.000(3) 0.030(3) -0.002(2) C23 0.057(3) 0.051(3) 0.072(4) -0.016(3) 0.031(3) 0.001(3) C24 0.053(3) 0.061(3) 0.058(3) -0.002(3) 0.029(3) 0.012(3) C25 0.035(3) 0.067(3) 0.046(3) 0.005(3) 0.023(2) 0.003(2) C26 0.032(2) 0.047(3) 0.035(2) 0.005(2) 0.0149(19) 0.005(2) C27 0.039(2) 0.042(3) 0.035(2) 0.000(2) 0.0178(19) -0.004(2) C28 0.029(2) 0.045(2) 0.035(2) 0.008(2) 0.0129(18) 0.0018(19) C29 0.037(3) 0.050(3) 0.053(3) 0.012(2) 0.015(2) -0.012(2) C30 0.032(2) 0.047(3) 0.043(3) 0.008(2) 0.016(2) 0.000(2) C31 0.040(3) 0.059(3) 0.054(3) 0.005(3) 0.020(2) 0.017(2) C32 0.066(3) 0.072(4) 0.041(3) 0.003(3) 0.027(3) 0.021(3) C33 0.048(3) 0.063(3) 0.038(3) 0.005(2) 0.015(2) 0.016(2) C34 0.037(2) 0.050(3) 0.040(3) 0.005(2) 0.017(2) 0.009(2) C35 0.039(2) 0.058(3) 0.041(3) 0.005(2) 0.023(2) 0.002(2) C36 0.038(3) 0.069(3) 0.044(3) -0.001(3) 0.017(2) 0.010(2) N1 0.039(2) 0.047(2) 0.046(2) 0.0006(19) 0.0217(18) -0.0037(17) N2 0.041(2) 0.046(2) 0.039(2) 0.0030(17) 0.0217(17) 0.0042(17) N3 0.0342(19) 0.042(2) 0.045(2) -0.0002(17) 0.0193(17) -0.0001(16) N4 0.0297(18) 0.038(2) 0.040(2) 0.0057(16) 0.0156(16) 0.0016(15) N5 0.036(2) 0.053(2) 0.046(2) -0.0095(19) 0.0205(19) -0.0090(19) N6 0.0307(19) 0.052(2) 0.044(2) 0.0009(18) 0.0186(17) -0.0031(18) N7 0.064(3) 0.050(3) 0.054(3) 0.015(2) 0.032(2) 0.012(2) N8 0.073(3) 0.049(3) 0.065(3) 0.000(2) 0.046(3) -0.012(2) O1 0.0375(18) 0.062(2) 0.068(2) 0.0212(18) 0.0139(16) 0.0126(16) O1W 0.106(3) 0.057(3) 0.100(4) -0.013(3) 0.071(3) -0.019(2) O2 0.056(2) 0.089(3) 0.047(2) 0.0236(19) 0.0178(17) -0.0056(19) O3 0.054(2) 0.094(3) 0.058(2) 0.019(2) 0.0344(18) 0.029(2) O4 0.060(2) 0.069(2) 0.061(2) 0.0182(19) 0.0325(18) 0.0288(19) _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 2.048(3) . ? Co1 N3 2.111(3) . ? Co1 N4 2.129(3) . ? Co1 N1 2.135(4) . ? Co1 N2 2.165(3) . ? C1 N1 1.390(5) . ? C1 C6 1.391(6) . ? C1 C2 1.393(7) . ? C2 C3 1.379(8) . ? C2 H2 0.95(5) . ? C3 C4 1.387(9) . ? C3 H3 0.97(5) . ? C4 C5 1.364(10) . ? C4 H4 0.96(7) . ? C5 C6 1.391(7) . ? C5 H5 0.90(5) . ? C6 N8 1.382(7) . ? C7 C12 1.389(6) . ? C7 C8 1.398(7) . ? C7 N2 1.402(5) . ? C8 C9 1.369(7) . ? C8 H8 0.91(4) . ? C9 C10 1.391(9) . ? C9 H9 0.97(5) . ? C10 C11 1.368(9) . ? C10 H10 0.95(5) . ? C11 C12 1.400(7) . ? C11 H11 0.93(6) . ? C12 N7 1.384(6) . ? C13 N1 1.321(5) . ? C13 N8 1.345(6) . ? C13 C14 1.448(6) . ? C14 N2 1.321(5) . ? C14 N7 1.352(6) . ? C15 C16 1.385(6) . ? C15 N3 1.395(5) . ? C15 C20 1.400(6) . ? C16 C17 1.375(7) . ? C16 H16 0.90(5) . ? C17 C18 1.390(8) . ? C17 H17 0.94(4) . ? C18 C19 1.376(7) . ? C18 H18 1.03(5) . ? C19 C20 1.391(6) . ? C19 H19 1.00(5) . ? C20 N5 1.394(6) . ? C21 C22 1.388(6) . ? C21 N4 1.390(5) . ? C21 C26 1.404(6) . ? C22 C23 1.374(7) . ? C22 H22 0.88(4) . ? C23 C24 1.398(7) . ? C23 H23 0.96(5) . ? C24 C25 1.371(7) . ? C24 H24 0.98(5) . ? C25 C26 1.389(6) . ? C25 H25 0.93(4) . ? C26 N6 1.380(5) . ? C27 N3 1.322(5) . ? C27 N5 1.336(5) . ? C27 C28 1.452(6) . ? C28 N4 1.327(5) . ? C28 N6 1.349(5) . ? C29 O2 1.249(5) . ? C29 O1 1.262(5) . ? C29 C30 1.509(6) . ? C30 C35 1.384(6) . ? C30 C31 1.389(6) . ? C31 C32 1.371(7) . ? C31 H31 0.90(4) . ? C32 C33 1.375(7) . ? C32 H32 0.92(5) . ? C33 C34 1.392(6) . ? C33 H33 0.97(4) . ? C34 C35 1.397(6) . ? C34 C36 1.506(6) . ? C35 H35 0.92(4) . ? C36 O4 1.257(5) 1 ? C36 O4 1.257(5) . ? C36 O3 1.268(5) . ? N5 O3 2.695(5) 4_475 ? N5 H5A 0.86(5) . ? N6 O4 2.725(5) 4_475 ? N6 H6A 0.89(5) . ? N7 O1W 2.848(6) 2_656 ? N7 H7A 0.83(5) . ? N8 O2 2.776(6) 3_676 ? N8 H8A 0.79(6) . ? O1W O4 2.870(6) 1 ? O1W O3 2.973(6) 4_576 ? O1W H1C 0.89(8) . ? O1W H1B 0.82(9) . ? O4 O4 0.000(7) 1 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N3 99.31(14) . . ? O1 Co1 N4 95.64(13) . . ? N3 Co1 N4 78.67(13) . . ? O1 Co1 N1 91.33(14) . . ? N3 Co1 N1 168.90(14) . . ? N4 Co1 N1 97.24(13) . . ? O1 Co1 N2 160.28(13) . . ? N3 Co1 N2 92.47(14) . . ? N4 Co1 N2 102.18(13) . . ? N1 Co1 N2 78.21(14) . . ? N1 C1 C6 109.0(4) . . ? N1 C1 C2 130.4(5) . . ? C6 C1 C2 120.6(5) . . ? C3 C2 C1 117.1(6) . . ? C3 C2 H2 126(3) . . ? C1 C2 H2 116(3) . . ? C2 C3 C4 121.5(6) . . ? C2 C3 H3 116(3) . . ? C4 C3 H3 122(3) . . ? C5 C4 C3 122.3(7) . . ? C5 C4 H4 119(4) . . ? C3 C4 H4 119(4) . . ? C4 C5 C6 116.6(7) . . ? C4 C5 H5 127(4) . . ? C6 C5 H5 116(4) . . ? N8 C6 C1 105.8(4) . . ? N8 C6 C5 132.3(6) . . ? C1 C6 C5 121.9(6) . . ? C12 C7 C8 120.1(4) . . ? C12 C7 N2 109.2(4) . . ? C8 C7 N2 130.7(4) . . ? C9 C8 C7 117.5(6) . . ? C9 C8 H8 123(3) . . ? C7 C8 H8 119(3) . . ? C8 C9 C10 121.9(6) . . ? C8 C9 H9 122(3) . . ? C10 C9 H9 116(3) . . ? C11 C10 C9 121.9(6) . . ? C11 C10 H10 119(3) . . ? C9 C10 H10 119(3) . . ? C10 C11 C12 116.3(6) . . ? C10 C11 H11 122(4) . . ? C12 C11 H11 121(4) . . ? N7 C12 C7 106.4(4) . . ? N7 C12 C11 131.3(5) . . ? C7 C12 C11 122.3(5) . . ? N1 C13 N8 112.8(4) . . ? N1 C13 C14 118.4(4) . . ? N8 C13 C14 128.8(4) . . ? N2 C14 N7 113.8(4) . . ? N2 C14 C13 118.7(4) . . ? N7 C14 C13 127.4(4) . . ? C16 C15 N3 130.3(4) . . ? C16 C15 C20 120.3(5) . . ? N3 C15 C20 109.4(4) . . ? C17 C16 C15 117.4(5) . . ? C17 C16 H16 124(3) . . ? C15 C16 H16 119(3) . . ? C16 C17 C18 121.8(5) . . ? C16 C17 H17 121(3) . . ? C18 C17 H17 117(3) . . ? C19 C18 C17 122.0(5) . . ? C19 C18 H18 115(3) . . ? C17 C18 H18 123(3) . . ? C18 C19 C20 116.1(5) . . ? C18 C19 H19 125(3) . . ? C20 C19 H19 119(3) . . ? C19 C20 N5 132.4(4) . . ? C19 C20 C15 122.4(5) . . ? N5 C20 C15 105.3(4) . . ? C22 C21 N4 131.0(4) . . ? C22 C21 C26 120.0(4) . . ? N4 C21 C26 109.0(4) . . ? C23 C22 C21 118.1(5) . . ? C23 C22 H22 120(3) . . ? C21 C22 H22 121(3) . . ? C22 C23 C24 121.2(5) . . ? C22 C23 H23 121(3) . . ? C24 C23 H23 118(3) . . ? C25 C24 C23 121.8(5) . . ? C25 C24 H24 120(3) . . ? C23 C24 H24 119(3) . . ? C24 C25 C26 116.9(4) . . ? C24 C25 H25 122(3) . . ? C26 C25 H25 121(3) . . ? N6 C26 C25 131.9(4) . . ? N6 C26 C21 106.1(4) . . ? C25 C26 C21 122.0(4) . . ? N3 C27 N5 114.1(4) . . ? N3 C27 C28 117.0(4) . . ? N5 C27 C28 129.0(4) . . ? N4 C28 N6 113.7(4) . . ? N4 C28 C27 118.5(4) . . ? N6 C28 C27 127.7(4) . . ? O2 C29 O1 122.1(4) . . ? O2 C29 C30 120.5(4) . . ? O1 C29 C30 117.3(4) . . ? C35 C30 C31 119.3(4) . . ? C35 C30 C29 121.7(4) . . ? C31 C30 C29 119.0(4) . . ? C32 C31 C30 120.5(4) . . ? C32 C31 H31 121(3) . . ? C30 C31 H31 119(3) . . ? C31 C32 C33 120.3(5) . . ? C31 C32 H32 122(3) . . ? C33 C32 H32 118(3) . . ? C32 C33 C34 120.4(5) . . ? C32 C33 H33 120(3) . . ? C34 C33 H33 119(3) . . ? C33 C34 C35 118.9(4) . . ? C33 C34 C36 120.3(4) . . ? C35 C34 C36 120.8(4) . . ? C30 C35 C34 120.5(4) . . ? C30 C35 H35 122(3) . . ? C34 C35 H35 117(3) . . ? O4 C36 O4 0.0(3) 1 . ? O4 C36 O3 124.9(4) 1 . ? O4 C36 O3 124.9(4) . . ? O4 C36 C34 118.5(4) 1 . ? O4 C36 C34 118.5(4) . . ? O3 C36 C34 116.5(4) . . ? C13 N1 C1 105.3(4) . . ? C13 N1 Co1 112.2(3) . . ? C1 N1 Co1 142.1(3) . . ? C14 N2 C7 104.4(4) . . ? C14 N2 Co1 110.6(3) . . ? C7 N2 Co1 141.8(3) . . ? C27 N3 C15 104.6(3) . . ? C27 N3 Co1 113.3(3) . . ? C15 N3 Co1 141.3(3) . . ? C28 N4 C21 104.7(3) . . ? C28 N4 Co1 112.0(3) . . ? C21 N4 Co1 142.7(3) . . ? C27 N5 C20 106.7(4) . . ? C27 N5 O3 133.1(3) . 4_475 ? C20 N5 O3 120.2(3) . 4_475 ? C27 N5 H5A 128(3) . . ? C20 N5 H5A 125(3) . . ? O3 N5 H5A 7(3) 4_475 . ? C28 N6 C26 106.4(4) . . ? C28 N6 O4 126.0(3) . 4_475 ? C26 N6 O4 125.9(3) . 4_475 ? C28 N6 H6A 125(3) . . ? C26 N6 H6A 128(3) . . ? O4 N6 H6A 9(3) 4_475 . ? C14 N7 C12 106.2(4) . . ? C14 N7 O1W 115.9(3) . 2_656 ? C12 N7 O1W 120.1(3) . 2_656 ? C14 N7 H7A 122(4) . . ? C12 N7 H7A 125(4) . . ? O1W N7 H7A 16(4) 2_656 . ? C13 N8 C6 107.0(4) . . ? C13 N8 O2 110.0(3) . 3_676 ? C6 N8 O2 126.1(3) . 3_676 ? C13 N8 H8A 121(4) . . ? C6 N8 H8A 129(5) . . ? O2 N8 H8A 23(4) 3_676 . ? C29 O1 Co1 101.0(3) . . ? O4 O1W O3 101.75(16) 1 4_576 ? O4 O1W H1C 8(5) 1 . ? O3 O1W H1C 104(5) 4_576 . ? O4 O1W H1B 108(6) 1 . ? O3 O1W H1B 9(6) 4_576 . ? H1C O1W H1B 111(7) . . ? O4 O4 C36 0(10) 1 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 178.6(5) . . . . ? C6 C1 C2 C3 -0.4(7) . . . . ? C1 C2 C3 C4 1.0(8) . . . . ? C2 C3 C4 C5 -0.5(10) . . . . ? C3 C4 C5 C6 -0.5(10) . . . . ? N1 C1 C6 N8 0.1(5) . . . . ? C2 C1 C6 N8 179.3(4) . . . . ? N1 C1 C6 C5 -179.8(5) . . . . ? C2 C1 C6 C5 -0.6(8) . . . . ? C4 C5 C6 N8 -178.8(6) . . . . ? C4 C5 C6 C1 1.1(9) . . . . ? C12 C7 C8 C9 -0.4(7) . . . . ? N2 C7 C8 C9 178.1(5) . . . . ? C7 C8 C9 C10 1.2(9) . . . . ? C8 C9 C10 C11 -1.1(10) . . . . ? C9 C10 C11 C12 0.2(10) . . . . ? C8 C7 C12 N7 179.6(4) . . . . ? N2 C7 C12 N7 0.7(5) . . . . ? C8 C7 C12 C11 -0.4(7) . . . . ? N2 C7 C12 C11 -179.3(4) . . . . ? C10 C11 C12 N7 -179.5(5) . . . . ? C10 C11 C12 C7 0.5(8) . . . . ? N1 C13 C14 N2 -5.1(6) . . . . ? N8 C13 C14 N2 176.4(4) . . . . ? N1 C13 C14 N7 173.1(4) . . . . ? N8 C13 C14 N7 -5.4(7) . . . . ? N3 C15 C16 C17 -177.3(4) . . . . ? C20 C15 C16 C17 0.6(7) . . . . ? C15 C16 C17 C18 -1.7(8) . . . . ? C16 C17 C18 C19 1.9(9) . . . . ? C17 C18 C19 C20 -0.7(8) . . . . ? C18 C19 C20 N5 178.7(5) . . . . ? C18 C19 C20 C15 -0.4(7) . . . . ? C16 C15 C20 C19 0.5(7) . . . . ? N3 C15 C20 C19 178.8(4) . . . . ? C16 C15 C20 N5 -178.8(4) . . . . ? N3 C15 C20 N5 -0.6(5) . . . . ? N4 C21 C22 C23 -179.1(4) . . . . ? C26 C21 C22 C23 0.7(7) . . . . ? C21 C22 C23 C24 -0.5(8) . . . . ? C22 C23 C24 C25 -0.1(8) . . . . ? C23 C24 C25 C26 0.5(7) . . . . ? C24 C25 C26 N6 179.6(5) . . . . ? C24 C25 C26 C21 -0.3(7) . . . . ? C22 C21 C26 N6 179.8(4) . . . . ? N4 C21 C26 N6 -0.4(4) . . . . ? C22 C21 C26 C25 -0.3(6) . . . . ? N4 C21 C26 C25 179.5(4) . . . . ? N3 C27 C28 N4 7.8(6) . . . . ? N5 C27 C28 N4 -173.8(4) . . . . ? N3 C27 C28 N6 -168.2(4) . . . . ? N5 C27 C28 N6 10.1(7) . . . . ? O2 C29 C30 C35 -10.7(7) . . . . ? O1 C29 C30 C35 169.2(4) . . . . ? O2 C29 C30 C31 170.5(4) . . . . ? O1 C29 C30 C31 -9.6(6) . . . . ? C35 C30 C31 C32 -0.2(7) . . . . ? C29 C30 C31 C32 178.6(5) . . . . ? C30 C31 C32 C33 -0.5(8) . . . . ? C31 C32 C33 C34 0.7(8) . . . . ? C32 C33 C34 C35 -0.3(7) . . . . ? C32 C33 C34 C36 178.1(5) . . . . ? C31 C30 C35 C34 0.6(7) . . . . ? C29 C30 C35 C34 -178.2(4) . . . . ? C33 C34 C35 C30 -0.4(7) . . . . ? C36 C34 C35 C30 -178.8(4) . . . . ? C33 C34 C36 O4 31.0(7) . . . 1 ? C35 C34 C36 O4 -150.6(5) . . . 1 ? C33 C34 C36 O4 31.0(7) . . . . ? C35 C34 C36 O4 -150.6(5) . . . . ? C33 C34 C36 O3 -146.8(5) . . . . ? C35 C34 C36 O3 31.6(7) . . . . ? N8 C13 N1 C1 -1.7(5) . . . . ? C14 C13 N1 C1 179.6(4) . . . . ? N8 C13 N1 Co1 172.5(3) . . . . ? C14 C13 N1 Co1 -6.2(5) . . . . ? C6 C1 N1 C13 0.9(5) . . . . ? C2 C1 N1 C13 -178.2(5) . . . . ? C6 C1 N1 Co1 -170.2(4) . . . . ? C2 C1 N1 Co1 10.7(8) . . . . ? O1 Co1 N1 C13 173.0(3) . . . . ? N3 Co1 N1 C13 -23.5(8) . . . . ? N4 Co1 N1 C13 -91.2(3) . . . . ? N2 Co1 N1 C13 9.8(3) . . . . ? O1 Co1 N1 C1 -16.2(5) . . . . ? N3 Co1 N1 C1 147.2(6) . . . . ? N4 Co1 N1 C1 79.6(5) . . . . ? N2 Co1 N1 C1 -179.4(5) . . . . ? N7 C14 N2 C7 -0.6(5) . . . . ? C13 C14 N2 C7 177.8(4) . . . . ? N7 C14 N2 Co1 -165.2(3) . . . . ? C13 C14 N2 Co1 13.3(5) . . . . ? C12 C7 N2 C14 -0.1(5) . . . . ? C8 C7 N2 C14 -178.8(5) . . . . ? C12 C7 N2 Co1 156.1(4) . . . . ? C8 C7 N2 Co1 -22.6(8) . . . . ? O1 Co1 N2 C14 -71.5(5) . . . . ? N3 Co1 N2 C14 161.6(3) . . . . ? N4 Co1 N2 C14 82.7(3) . . . . ? N1 Co1 N2 C14 -12.3(3) . . . . ? O1 Co1 N2 C7 133.2(5) . . . . ? N3 Co1 N2 C7 6.3(4) . . . . ? N4 Co1 N2 C7 -72.6(4) . . . . ? N1 Co1 N2 C7 -167.6(5) . . . . ? N5 C27 N3 C15 0.3(5) . . . . ? C28 C27 N3 C15 178.9(4) . . . . ? N5 C27 N3 Co1 172.2(3) . . . . ? C28 C27 N3 Co1 -9.2(5) . . . . ? C16 C15 N3 C27 178.2(5) . . . . ? C20 C15 N3 C27 0.2(5) . . . . ? C16 C15 N3 Co1 10.2(8) . . . . ? C20 C15 N3 Co1 -167.9(3) . . . . ? O1 Co1 N3 C27 100.1(3) . . . . ? N4 Co1 N3 C27 6.2(3) . . . . ? N1 Co1 N3 C27 -63.2(8) . . . . ? N2 Co1 N3 C27 -95.8(3) . . . . ? O1 Co1 N3 C15 -92.5(5) . . . . ? N4 Co1 N3 C15 173.6(5) . . . . ? N1 Co1 N3 C15 104.2(8) . . . . ? N2 Co1 N3 C15 71.6(5) . . . . ? N6 C28 N4 C21 1.2(4) . . . . ? C27 C28 N4 C21 -175.4(3) . . . . ? N6 C28 N4 Co1 174.5(3) . . . . ? C27 C28 N4 Co1 -2.1(4) . . . . ? C22 C21 N4 C28 179.3(5) . . . . ? C26 C21 N4 C28 -0.5(4) . . . . ? C22 C21 N4 Co1 9.6(8) . . . . ? C26 C21 N4 Co1 -170.1(3) . . . . ? O1 Co1 N4 C28 -100.4(3) . . . . ? N3 Co1 N4 C28 -2.0(3) . . . . ? N1 Co1 N4 C28 167.5(3) . . . . ? N2 Co1 N4 C28 88.1(3) . . . . ? O1 Co1 N4 C21 68.8(4) . . . . ? N3 Co1 N4 C21 167.2(4) . . . . ? N1 Co1 N4 C21 -23.3(4) . . . . ? N2 Co1 N4 C21 -102.7(4) . . . . ? N3 C27 N5 C20 -0.6(5) . . . . ? C28 C27 N5 C20 -179.0(4) . . . . ? N3 C27 N5 O3 178.7(3) . . . 4_475 ? C28 C27 N5 O3 0.3(7) . . . 4_475 ? C19 C20 N5 C27 -178.6(5) . . . . ? C15 C20 N5 C27 0.7(5) . . . . ? C19 C20 N5 O3 2.0(7) . . . 4_475 ? C15 C20 N5 O3 -178.8(3) . . . 4_475 ? N4 C28 N6 C26 -1.5(5) . . . . ? C27 C28 N6 C26 174.7(4) . . . . ? N4 C28 N6 O4 -167.5(3) . . . 4_475 ? C27 C28 N6 O4 8.8(6) . . . 4_475 ? C25 C26 N6 C28 -178.8(5) . . . . ? C21 C26 N6 C28 1.1(4) . . . . ? C25 C26 N6 O4 -12.8(7) . . . 4_475 ? C21 C26 N6 O4 167.1(3) . . . 4_475 ? N2 C14 N7 C12 1.1(5) . . . . ? C13 C14 N7 C12 -177.2(4) . . . . ? N2 C14 N7 O1W 137.3(3) . . . 2_656 ? C13 C14 N7 O1W -41.0(6) . . . 2_656 ? C7 C12 N7 C14 -1.1(5) . . . . ? C11 C12 N7 C14 178.9(5) . . . . ? C7 C12 N7 O1W -135.0(3) . . . 2_656 ? C11 C12 N7 O1W 45.0(7) . . . 2_656 ? N1 C13 N8 C6 1.7(5) . . . . ? C14 C13 N8 C6 -179.7(4) . . . . ? N1 C13 N8 O2 141.8(3) . . . 3_676 ? C14 C13 N8 O2 -39.6(6) . . . 3_676 ? C1 C6 N8 C13 -1.0(5) . . . . ? C5 C6 N8 C13 178.8(6) . . . . ? C1 C6 N8 O2 -132.8(4) . . . 3_676 ? C5 C6 N8 O2 47.1(8) . . . 3_676 ? O2 C29 O1 Co1 1.5(5) . . . . ? C30 C29 O1 Co1 -178.4(3) . . . . ? N3 Co1 O1 C29 83.5(3) . . . . ? N4 Co1 O1 C29 162.9(3) . . . . ? N1 Co1 O1 C29 -99.7(3) . . . . ? N2 Co1 O1 C29 -42.4(6) . . . . ? O3 C36 O4 O4 0.0(9) . . . 1 ? C34 C36 O4 O4 0.0(7) . . . 1 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5A O3 0.86(5) 1.85(5) 2.695(5) 170(5) 4_475 N6 H6A O4 0.89(5) 1.85(5) 2.725(5) 167(5) 4_475 N7 H7A O1W 0.83(5) 2.06(6) 2.848(6) 158(5) 2_656 N8 H8A O2 0.79(6) 2.07(6) 2.776(6) 149(6) 3_676 O1W H1B O3 0.82(9) 2.17(9) 2.973(6) 168(8) 4_576 O1W H1C O4 0.89(8) 2.00(8) 2.870(6) 169(7) 1 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.312 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.066 #===============================END data_4 _database_code_depnum_ccdc_archive 'CCDC 286939' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H69 Co4 N20 O19' _chemical_formula_weight 1946.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.5096(4) _cell_length_b 33.7329(7) _cell_length_c 15.2861(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.1210(10) _cell_angle_gamma 90.00 _cell_volume 8938.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9592 _cell_measurement_theta_min 1.21 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3988 _exptl_absorpt_coefficient_mu 0.810 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.864 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Simemens SMART CCD' _diffrn_measurement_method '\w scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13840 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9592 _reflns_number_gt 8011 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' Simens SMART ' _computing_cell_refinement ' Simens SMART ' _computing_data_reduction ' Simens SMART ' _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^)+(0.0394P)^2^+77.2231P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 9592 _refine_ls_number_parameters 1134 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1711 _refine_ls_wR_factor_gt 0.1500 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.28481(9) 0.60079(4) 1.06756(11) 0.0494(4) Uani 1 1 d . . . Co2 Co 0.97908(8) 0.63625(4) 0.50082(10) 0.0419(3) Uani 1 1 d . . . Co3 Co 0.66418(8) 0.64588(4) 0.28171(10) 0.0439(4) Uani 1 1 d . . . Co4 Co 0.57508(9) 0.61766(4) -0.11093(11) 0.0483(4) Uani 1 1 d . . . C1 C 1.1108(8) 0.5814(4) 1.1312(10) 0.062(3) Uani 1 1 d . . . C2 C 1.0715(11) 0.6174(5) 1.1365(12) 0.086(5) Uani 1 1 d . . . H2A H 1.097(6) 0.638(3) 1.141(7) 0.04(3) Uiso 1 1 d . . . C3 C 0.9970(11) 0.6156(6) 1.1617(15) 0.106(7) Uani 1 1 d . . . H3A H 0.9688 0.6387 1.1657 0.128 Uiso 1 1 calc R . . C4 C 0.9673(11) 0.5805(7) 1.1798(14) 0.110(6) Uani 1 1 d . . . H4A H 0.9185 0.5807 1.1972 0.132 Uiso 1 1 calc R . . C5 C 1.0015(10) 0.5448(6) 1.1751(12) 0.093(5) Uani 1 1 d . . . H5A H 0.9782 0.5212 1.1883 0.112 Uiso 1 1 calc R . . C6 C 1.0757(8) 0.5462(4) 1.1485(10) 0.064(3) Uani 1 1 d . . . C7 C 1.3866(8) 0.5173(3) 1.0862(8) 0.056(3) Uani 1 1 d . . . C8 C 1.4642(8) 0.5260(4) 1.0840(10) 0.075(4) Uani 1 1 d . . . H8A H 1.4817 0.5520 1.0820 0.090 Uiso 1 1 calc R . . C9 C 1.5147(10) 0.4934(6) 1.0850(14) 0.107(6) Uani 1 1 d . . . H9A H 1.5672 0.4981 1.0866 0.129 Uiso 1 1 calc R . . C10 C 1.4889(11) 0.4543(6) 1.0836(15) 0.110(7) Uani 1 1 d . . . H10A H 1.5237 0.4339 1.0788 0.131 Uiso 1 1 calc R . . C11 C 1.4123(12) 0.4453(5) 1.0892(13) 0.104(6) Uani 1 1 d . . . H11A H 1.3950 0.4193 1.0916 0.124 Uiso 1 1 calc R . . C12 C 1.3630(8) 0.4778(4) 1.0909(11) 0.070(4) Uani 1 1 d . . . C13 C 1.1899(7) 0.5348(3) 1.1118(9) 0.053(3) Uani 1 1 d . . . C14 C 1.2641(7) 0.5178(3) 1.0979(8) 0.050(3) Uani 1 1 d . . . C15 C 1.2055(7) 0.6422(3) 0.9486(7) 0.049(3) Uani 1 1 d . . . C16 C 1.1634(6) 0.6684(3) 0.8794(7) 0.041(2) Uani 1 1 d . . . C17 C 1.1678(7) 0.7095(3) 0.8894(7) 0.043(3) Uani 1 1 d . . . H17A H 1.1941 0.7205 0.9408 0.052 Uiso 1 1 calc R . . C18 C 1.1323(6) 0.7341(3) 0.8216(8) 0.042(3) Uani 1 1 d . . . C19 C 1.1409(7) 0.7778(3) 0.8306(8) 0.049(3) Uiso 1 1 d . . . C20 C 1.0909(6) 0.7173(3) 0.7453(7) 0.039(2) Uani 1 1 d . . . H20A H 1.0669 0.7337 0.7007 0.047 Uiso 1 1 calc R . . C21 C 1.0854(6) 0.6760(3) 0.7358(8) 0.043(3) Uani 1 1 d . . . C22 C 1.0410(6) 0.6593(3) 0.6532(8) 0.041(2) Uani 1 1 d . . . C23 C 1.1230(7) 0.6518(3) 0.8040(8) 0.045(3) Uani 1 1 d . . . H23A H 1.1205 0.6244 0.7982 0.054 Uiso 1 1 calc R . . C24 C 1.1303(6) 0.6861(3) 0.4393(8) 0.045(3) Uani 1 1 d . . . C25 C 1.1226(7) 0.7256(3) 0.4629(10) 0.067(4) Uani 1 1 d . . . H25A H 1.0813 0.7339 0.4903 0.081 Uiso 1 1 calc R . . C26 C 1.1785(10) 0.7521(4) 0.4442(12) 0.081(5) Uani 1 1 d . . . H26A H 1.1750 0.7786 0.4599 0.097 Uiso 1 1 calc R . . C27 C 1.2403(9) 0.7397(4) 0.4020(12) 0.082(5) Uani 1 1 d . . . H27A H 1.2770 0.7582 0.3904 0.099 Uiso 1 1 calc R . . C28 C 1.2479(7) 0.7005(4) 0.3772(10) 0.064(4) Uani 1 1 d . . . H28A H 1.2891 0.6924 0.3492 0.076 Uiso 1 1 calc R . . C29 C 1.1915(7) 0.6736(3) 0.3958(8) 0.053(3) Uani 1 1 d . . . C30 C 0.9982(7) 0.5407(3) 0.4453(8) 0.048(3) Uani 1 1 d . . . C31 C 0.9348(8) 0.5192(4) 0.4671(9) 0.062(4) Uani 1 1 d . . . H31A H 0.8946 0.5320 0.4893 0.075 Uiso 1 1 calc R . . C32 C 0.9335(9) 0.4788(4) 0.4547(11) 0.076(4) Uani 1 1 d . . . H32A H 0.8920 0.4642 0.4693 0.092 Uiso 1 1 calc R . . C33 C 0.9935(9) 0.4591(4) 0.4207(11) 0.073(4) Uani 1 1 d . . . H33A H 0.9905 0.4318 0.4123 0.088 Uiso 1 1 calc R . . C34 C 1.0558(8) 0.4791(3) 0.3995(10) 0.068(4) Uani 1 1 d . . . H34A H 1.0958 0.4659 0.3777 0.082 Uiso 1 1 calc R . . C35 C 1.0577(7) 0.5203(3) 0.4118(9) 0.057(3) Uani 1 1 d . . . C36 C 1.1180(6) 0.6231(3) 0.4173(8) 0.045(3) Uani 1 1 d . . . C37 C 1.0828(6) 0.5839(3) 0.4190(8) 0.043(3) Uani 1 1 d . . . C38 C 0.8382(7) 0.5995(3) 0.6032(8) 0.048(3) Uani 1 1 d . . . C39 C 0.8718(8) 0.5863(3) 0.6891(8) 0.055(3) Uani 1 1 d . . . H39A H 0.9247 0.5876 0.7072 0.066 Uiso 1 1 calc R . . C40 C 0.8220(9) 0.5714(4) 0.7440(9) 0.065(3) Uani 1 1 d . . . H40A H 0.8421 0.5637 0.8010 0.077 Uiso 1 1 calc R . . C41 C 0.7425(9) 0.5676(4) 0.7165(10) 0.071(4) Uani 1 1 d . . . H41A H 0.7114 0.5570 0.7552 0.085 Uiso 1 1 calc R . . C42 C 0.7093(8) 0.5795(3) 0.6324(10) 0.060(3) Uani 1 1 d . . . H42A H 0.6566 0.5769 0.6135 0.072 Uiso 1 1 calc R . . C43 C 0.7599(6) 0.5959(3) 0.5772(8) 0.050(3) Uani 1 1 d . . . C44 C 0.9008(7) 0.6772(3) 0.3139(7) 0.048(3) Uani 1 1 d . . . C45 C 0.9559(7) 0.7001(4) 0.2783(9) 0.064(3) Uani 1 1 d . . . H45A H 1.0057 0.7027 0.3083 0.077 Uiso 1 1 calc R . . C46 C 0.9351(9) 0.7185(4) 0.1984(10) 0.077(4) Uani 1 1 d . . . H46A H 0.9716 0.7335 0.1742 0.092 Uiso 1 1 calc R . . C47 C 0.8606(9) 0.7153(4) 0.1526(11) 0.084(5) Uani 1 1 d . . . H47A H 0.8485 0.7279 0.0983 0.101 Uiso 1 1 calc R . . C48 C 0.8048(9) 0.6940(4) 0.1861(10) 0.075(4) Uani 1 1 d . . . H48A H 0.7549 0.6923 0.1562 0.090 Uiso 1 1 calc R . . C49 C 0.8265(7) 0.6745(3) 0.2686(8) 0.048(3) Uani 1 1 d . . . C50 C 0.8144(6) 0.6233(3) 0.4713(7) 0.041(2) Uani 1 1 d . . . C51 C 0.8293(7) 0.6435(3) 0.3942(8) 0.041(2) Uani 1 1 d . . . C52 C 0.7007(7) 0.5871(3) 0.1462(9) 0.051(3) Uani 1 1 d . . . C53 C 0.7498(7) 0.5633(3) 0.2070(11) 0.068(4) Uani 1 1 d . . . H53A H 0.7589 0.5699 0.2666 0.082 Uiso 1 1 calc R . . C54 C 0.7831(9) 0.5308(4) 0.1761(12) 0.074(4) Uani 1 1 d . . . H54A H 0.8172 0.5155 0.2144 0.089 Uiso 1 1 calc R . . C55 C 0.7662(8) 0.5199(4) 0.0855(12) 0.075(5) Uani 1 1 d . . . H55A H 0.7879 0.4967 0.0670 0.090 Uiso 1 1 calc R . . C56 C 0.7187(8) 0.5421(3) 0.0233(10) 0.064(4) Uani 1 1 d . . . H56A H 0.7092 0.5349 -0.0360 0.077 Uiso 1 1 calc R . . C57 C 0.6855(7) 0.5769(3) 0.0565(9) 0.048(3) Uani 1 1 d . . . C58 C 0.4723(7) 0.7052(3) 0.0520(8) 0.051(3) Uani 1 1 d . . . C59 C 0.4206(8) 0.7340(4) 0.0699(11) 0.072(4) Uani 1 1 d . . . H59A H 0.4200 0.7433 0.1271 0.087 Uiso 1 1 calc R . . C60 C 0.3705(8) 0.7481(4) 0.0004(12) 0.075(4) Uani 1 1 d . . . H60A H 0.3342 0.7670 0.0110 0.090 Uiso 1 1 calc R . . C61 C 0.3720(8) 0.7353(4) -0.0849(11) 0.069(4) Uani 1 1 d . . . H61A H 0.3366 0.7456 -0.1303 0.083 Uiso 1 1 calc R . . C62 C 0.4246(8) 0.7077(3) -0.1045(11) 0.067(4) Uani 1 1 d . . . H62A H 0.4259 0.6994 -0.1623 0.080 Uiso 1 1 calc R . . C63 C 0.4761(6) 0.6926(3) -0.0342(8) 0.046(3) Uani 1 1 d . . . C64 C 0.6204(6) 0.6292(3) 0.0787(8) 0.044(3) Uani 1 1 d . . . C65 C 0.5621(6) 0.6600(3) 0.0516(7) 0.041(3) Uani 1 1 d . . . C66 C 0.4448(9) 0.6440(4) -0.2836(10) 0.070(4) Uani 1 1 d . . . C67 C 0.3737(9) 0.6304(4) -0.2645(11) 0.080(4) Uani 1 1 d . . . H67A H 0.3693 0.6148 -0.2153 0.096 Uiso 1 1 calc R . . C68 C 0.3091(10) 0.6419(4) -0.3244(13) 0.093(5) Uani 1 1 d . . . H68A H 0.2602 0.6341 -0.3143 0.111 Uiso 1 1 calc R . . C69 C 0.3168(14) 0.6647(5) -0.3980(14) 0.117(8) Uani 1 1 d . . . H69A H 0.2723 0.6719 -0.4353 0.140 Uiso 1 1 calc R . . C70 C 0.3888(13) 0.6776(5) -0.4197(14) 0.110(6) Uani 1 1 d . . . H70A H 0.3933 0.6923 -0.4702 0.132 Uiso 1 1 calc R . . C71 C 0.4522(12) 0.6665(4) -0.3594(9) 0.084(5) Uani 1 1 d . . . C72 C 0.7494(9) 0.6514(4) -0.1468(10) 0.063(4) Uani 1 1 d . . . C73 C 0.8044(9) 0.6427(4) -0.0741(11) 0.074(4) Uani 1 1 d . . . H73A H 0.7901 0.6299 -0.0250 0.089 Uiso 1 1 calc R . . C74 C 0.8784(9) 0.6530(5) -0.0758(15) 0.099(6) Uani 1 1 d . . . H74A H 0.9149 0.6474 -0.0272 0.119 Uiso 1 1 calc R . . C75 C 0.9019(12) 0.6723(6) -0.150(2) 0.122(9) Uani 1 1 d . . . H75A H 0.9537 0.6786 -0.1490 0.147 Uiso 1 1 calc R . . C76 C 0.8513(11) 0.6817(5) -0.2203(15) 0.096(6) Uani 1 1 d . . . H76A H 0.8661 0.6949 -0.2685 0.115 Uiso 1 1 calc R . . C77 C 0.7748(10) 0.6706(4) -0.2179(12) 0.075(4) Uani 1 1 d . . . C78 C 0.5665(9) 0.6588(3) -0.2807(8) 0.061(3) Uani 1 1 d . . . C79 C 0.6493(9) 0.6602(3) -0.2426(9) 0.060(4) Uani 1 1 d . . . C80 C 0.5195(7) 0.5495(3) -0.1363(8) 0.047(3) Uiso 1 1 d . . . C81 C 0.4890(6) 0.5074(3) -0.1466(8) 0.045(3) Uiso 1 1 d . . . C82 C 0.5409(6) 0.4764(3) -0.1561(8) 0.046(3) Uani 1 1 d . . . H82A H 0.5931 0.4813 -0.1567 0.055 Uiso 1 1 calc R . . C83 C 0.5118(6) 0.4381(3) -0.1646(7) 0.043(3) Uani 1 1 d . . . C84 C 0.5605(7) 0.4017(3) -0.1798(9) 0.053(3) Uani 1 1 d . . . C85 C 0.4329(6) 0.4306(3) -0.1643(8) 0.045(3) Uani 1 1 d . . . H85A H 0.4146 0.4047 -0.1696 0.054 Uiso 1 1 calc R . . C86 C 0.3820(6) 0.4616(3) -0.1563(8) 0.043(3) Uani 1 1 d . . . C87 C 0.2978(6) 0.4520(3) -0.1594(8) 0.044(3) Uani 1 1 d . . . C88 C 0.4117(6) 0.5002(3) -0.1471(8) 0.044(3) Uani 1 1 d . . . H88A H 0.3786 0.5213 -0.1412 0.053 Uiso 1 1 calc R . . N1 N 1.1839(5) 0.5739(3) 1.1090(7) 0.051(2) Uani 1 1 d . . . N2 N 1.3234(6) 0.5417(2) 1.0893(7) 0.051(2) Uani 1 1 d . . . N3 N 1.2844(6) 0.4785(3) 1.0979(8) 0.063(3) Uani 1 1 d . . . H3B H 1.2547 0.4585 1.1014 0.075 Uiso 1 1 calc R . . N4 N 1.1278(6) 0.5165(3) 1.1344(7) 0.059(3) Uani 1 1 d . . . H4B H 1.1213 0.4914 1.1392 0.071 Uiso 1 1 calc R . . N5 N 1.0839(5) 0.6532(2) 0.4524(7) 0.048(2) Uani 1 1 d . . . N6 N 1.0167(6) 0.5812(3) 0.4505(6) 0.049(2) Uani 1 1 d . . . N7 N 1.1119(5) 0.5491(2) 0.3959(7) 0.053(3) Uani 1 1 d . . . H7A H 1.1547 0.5453 0.3757 0.063 Uiso 1 1 calc R . . N8 N 1.1819(5) 0.6338(2) 0.3832(7) 0.051(2) Uani 1 1 d . . . H8B H 1.2112 0.6183 0.3581 0.061 Uiso 1 1 calc R . . N9 N 0.8715(5) 0.6171(2) 0.5370(6) 0.0378(19) Uani 1 1 d . . . N10 N 0.9022(5) 0.6571(3) 0.3935(6) 0.047(2) Uani 1 1 d . . . N11 N 0.7795(5) 0.6533(2) 0.3196(6) 0.047(2) Uani 1 1 d . . . N12 N 0.7450(6) 0.6107(3) 0.4937(7) 0.056(3) Uani 1 1 d . . . H12A H 0.7008 0.6120 0.4613 0.068 Uiso 1 1 calc R . . N13 N 0.6586(5) 0.6210(2) 0.1597(6) 0.043(2) Uani 1 1 d . . . N14 N 0.5295(6) 0.6847(3) 0.1050(7) 0.059(3) Uani 1 1 d . . . H14A H 0.5419 0.6872 0.1612 0.071 Uiso 1 1 calc R . . N15 N 0.5342(5) 0.6630(2) -0.0314(6) 0.045(2) Uani 1 1 d . . . N16 N 0.6348(5) 0.6040(3) 0.0134(7) 0.050(2) Uani 1 1 d . . . N17 N 0.5193(7) 0.6390(3) -0.2346(7) 0.059(3) Uani 1 1 d . . . N18 N 0.6701(6) 0.6453(3) -0.1642(7) 0.054(3) Uani 1 1 d . . . N19 N 0.7079(8) 0.6758(3) -0.2795(10) 0.079(4) Uani 1 1 d . . . H19A H 0.7051 0.6867 -0.3306 0.094 Uiso 1 1 calc R . . N20 N 0.5300(9) 0.6753(3) -0.3549(8) 0.083(4) Uani 1 1 d . . . H20B H 0.5511 0.6889 -0.3928 0.099 Uiso 1 1 calc R . . O1W O 1.3204(7) 0.6257(3) 1.1893(6) 0.080(3) Uani 1 1 d . . . O1 O 1.2128(5) 0.6052(2) 0.9361(6) 0.060(2) Uani 1 1 d . . . O2W O 1.3849(5) 0.6135(2) 1.0057(7) 0.070(3) Uani 1 1 d . . . O2 O 1.2396(5) 0.6576(2) 1.0207(6) 0.057(2) Uani 1 1 d . . . O3W O 0.6438(9) 0.7197(4) -0.4303(10) 0.126(4) Uiso 1 1 d . . . O3 O 1.1274(4) 0.7985(2) 0.7598(6) 0.0496(18) Uiso 1 1 d . . . O4W O 1.1972(10) 0.7122(4) 1.1401(12) 0.149(6) Uiso 1 1 d . . . O4 O 1.1629(5) 0.7939(2) 0.9037(6) 0.065(2) Uiso 1 1 d . . . O5W O 0.4248(13) 0.6826(6) 0.2788(15) 0.196(8) Uiso 1 1 d . . . O5 O 0.9996(4) 0.6815(2) 0.6005(5) 0.0504(19) Uani 1 1 d . . . O6W O 1.1553(6) 0.5648(2) 0.6452(7) 0.080(3) Uani 1 1 d . . . O6 O 1.0473(5) 0.62289(19) 0.6351(6) 0.054(2) Uani 1 1 d . . . O7W O 1.2363(7) 0.5560(3) 0.8033(7) 0.085(3) Uani 1 1 d . . . O7 O 0.5849(5) 0.5572(2) -0.1555(6) 0.054(2) Uiso 1 1 d . . . O8 O 0.4793(4) 0.5758(2) -0.1054(5) 0.0495(18) Uiso 1 1 d . . . O9 O 0.2523(5) 0.4785(2) -0.1398(7) 0.064(3) Uani 1 1 d . . . O10 O 0.2763(4) 0.4171(2) -0.1813(6) 0.055(2) Uani 1 1 d . . . O11 O 0.6324(5) 0.4036(2) -0.1504(6) 0.062(2) Uani 1 1 d . . . O12 O 0.5324(5) 0.3723(2) -0.2213(8) 0.076(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0540(9) 0.0422(7) 0.0497(10) 0.0120(7) -0.0010(8) -0.0016(7) Co2 0.0316(7) 0.0487(7) 0.0431(9) -0.0069(7) -0.0022(6) 0.0003(6) Co3 0.0413(8) 0.0348(6) 0.0506(9) 0.0020(7) -0.0105(7) -0.0039(6) Co4 0.0572(10) 0.0429(7) 0.0451(9) -0.0046(7) 0.0089(7) -0.0102(7) C1 0.058(8) 0.056(7) 0.069(9) -0.003(7) -0.006(7) -0.009(6) C2 0.084(12) 0.070(10) 0.104(14) -0.024(9) 0.011(10) -0.008(9) C3 0.071(12) 0.102(13) 0.15(2) -0.009(13) 0.033(12) 0.014(10) C4 0.074(12) 0.143(16) 0.116(18) -0.018(14) 0.023(12) 0.017(12) C5 0.072(11) 0.115(13) 0.092(14) 0.004(11) 0.012(10) -0.010(10) C6 0.047(8) 0.074(8) 0.067(9) 0.010(7) 0.000(7) 0.000(6) C7 0.065(8) 0.056(7) 0.049(8) 0.015(6) 0.011(6) 0.013(6) C8 0.053(8) 0.095(10) 0.076(11) 0.019(8) 0.011(7) 0.005(7) C9 0.062(10) 0.141(16) 0.123(17) 0.025(13) 0.027(10) 0.033(11) C10 0.091(14) 0.097(12) 0.15(2) 0.030(12) 0.039(13) 0.038(10) C11 0.120(16) 0.082(10) 0.118(16) 0.038(10) 0.049(13) 0.041(10) C12 0.055(8) 0.071(8) 0.085(11) 0.029(8) 0.016(8) 0.033(7) C13 0.049(7) 0.044(6) 0.062(8) 0.004(6) -0.004(6) -0.008(5) C14 0.044(7) 0.054(6) 0.053(8) 0.015(6) 0.006(6) -0.001(5) C15 0.064(8) 0.040(6) 0.039(7) -0.002(5) -0.002(6) -0.013(5) C16 0.045(6) 0.037(5) 0.039(6) -0.004(5) -0.004(5) -0.001(4) C17 0.061(7) 0.033(5) 0.031(6) -0.010(4) -0.003(5) 0.003(5) C18 0.045(6) 0.026(4) 0.054(7) -0.004(5) 0.003(5) 0.006(4) C20 0.040(6) 0.036(5) 0.039(6) 0.000(5) -0.001(5) 0.008(4) C21 0.037(6) 0.027(5) 0.063(8) 0.009(5) 0.006(5) 0.007(4) C22 0.033(6) 0.041(5) 0.046(7) -0.007(5) -0.006(5) 0.002(4) C23 0.049(7) 0.039(5) 0.047(7) 0.000(5) 0.005(5) 0.010(5) C24 0.040(6) 0.043(5) 0.051(7) 0.004(5) 0.002(5) 0.001(5) C25 0.046(8) 0.057(7) 0.100(12) -0.009(7) 0.015(8) 0.000(6) C26 0.094(12) 0.037(6) 0.112(14) -0.010(7) 0.016(10) -0.008(7) C27 0.082(11) 0.059(8) 0.102(13) 0.020(8) 0.002(10) -0.018(7) C28 0.043(7) 0.066(8) 0.084(10) 0.012(7) 0.014(7) -0.007(6) C29 0.044(7) 0.053(6) 0.059(8) 0.008(6) 0.004(6) 0.005(5) C30 0.045(7) 0.057(6) 0.043(7) -0.006(5) 0.005(5) -0.005(5) C31 0.062(8) 0.060(8) 0.068(9) -0.017(6) 0.021(7) -0.018(6) C32 0.074(10) 0.069(9) 0.091(12) -0.009(8) 0.028(9) -0.021(7) C33 0.088(11) 0.048(6) 0.087(11) -0.015(7) 0.028(9) -0.026(7) C34 0.077(10) 0.057(7) 0.071(10) -0.014(7) 0.018(8) 0.000(7) C35 0.053(7) 0.046(6) 0.070(9) 0.005(6) -0.003(6) 0.003(5) C36 0.038(6) 0.034(5) 0.061(8) 0.004(5) 0.002(6) 0.004(5) C37 0.036(6) 0.042(5) 0.050(7) -0.010(5) 0.007(5) -0.002(5) C38 0.050(7) 0.038(5) 0.055(8) 0.000(5) 0.000(6) 0.001(5) C39 0.059(8) 0.062(7) 0.042(7) 0.006(6) -0.004(6) 0.000(6) C40 0.079(10) 0.066(8) 0.048(8) 0.012(6) 0.006(7) -0.002(7) C41 0.090(11) 0.061(7) 0.069(10) 0.002(7) 0.036(9) -0.002(7) C42 0.053(8) 0.057(7) 0.071(10) 0.004(7) 0.012(7) -0.001(6) C43 0.040(7) 0.053(6) 0.056(8) 0.005(6) 0.003(6) -0.003(5) C44 0.054(7) 0.054(6) 0.034(6) -0.010(5) -0.005(5) 0.000(5) C45 0.047(7) 0.086(8) 0.059(9) -0.008(7) 0.009(6) -0.025(6) C46 0.089(12) 0.084(9) 0.060(9) 0.021(8) 0.018(9) -0.024(8) C47 0.085(12) 0.096(10) 0.064(10) 0.024(9) -0.012(9) -0.023(9) C48 0.070(10) 0.081(9) 0.066(10) 0.017(8) -0.013(8) -0.019(8) C49 0.056(7) 0.050(6) 0.036(6) 0.004(5) -0.004(6) -0.009(5) C50 0.036(6) 0.046(5) 0.041(7) -0.003(5) 0.005(5) -0.002(5) C51 0.037(6) 0.045(5) 0.039(6) -0.006(5) -0.003(5) -0.002(5) C52 0.041(6) 0.041(6) 0.070(9) 0.007(6) 0.003(6) -0.002(5) C53 0.055(8) 0.038(6) 0.106(12) 0.005(7) -0.005(8) 0.004(6) C54 0.075(10) 0.053(7) 0.099(13) 0.025(8) 0.024(9) 0.027(7) C55 0.069(9) 0.047(7) 0.116(14) -0.004(8) 0.041(10) 0.015(6) C56 0.081(10) 0.043(6) 0.076(10) -0.015(6) 0.037(8) 0.009(6) C57 0.048(7) 0.039(5) 0.059(8) -0.002(5) 0.017(6) 0.004(5) C58 0.044(7) 0.048(6) 0.054(8) -0.014(5) -0.016(6) 0.003(5) C59 0.068(9) 0.059(7) 0.083(11) -0.018(7) -0.015(8) 0.019(7) C60 0.048(8) 0.055(7) 0.116(14) 0.000(8) -0.014(8) 0.012(6) C61 0.063(9) 0.056(7) 0.078(11) 0.019(7) -0.023(8) 0.001(6) C62 0.058(8) 0.050(7) 0.085(11) 0.013(7) -0.022(7) 0.001(6) C63 0.040(6) 0.033(5) 0.062(8) 0.005(5) -0.009(6) -0.009(4) C64 0.039(6) 0.041(5) 0.049(7) -0.006(5) -0.002(5) 0.000(4) C65 0.045(6) 0.036(5) 0.041(7) 0.001(5) -0.002(5) -0.010(5) C66 0.091(11) 0.063(8) 0.051(8) -0.005(7) -0.005(8) -0.008(7) C67 0.064(10) 0.090(10) 0.083(11) 0.010(9) 0.000(8) -0.020(8) C68 0.081(12) 0.076(9) 0.112(15) -0.019(10) -0.022(10) 0.009(8) C69 0.126(18) 0.103(13) 0.100(15) 0.030(12) -0.060(14) 0.016(12) C70 0.118(17) 0.102(13) 0.097(15) 0.015(11) -0.029(13) -0.003(12) C71 0.142(17) 0.064(8) 0.040(8) -0.007(7) -0.009(9) -0.018(10) C72 0.066(9) 0.059(7) 0.068(10) -0.012(7) 0.021(8) -0.009(7) C73 0.076(10) 0.063(8) 0.088(12) -0.024(8) 0.029(9) -0.025(7) C74 0.051(10) 0.105(12) 0.144(19) -0.022(12) 0.025(11) -0.008(8) C75 0.066(13) 0.099(13) 0.21(3) -0.040(16) 0.067(16) -0.029(11) C76 0.088(14) 0.077(10) 0.137(19) -0.023(11) 0.070(13) -0.030(10) C77 0.077(11) 0.062(8) 0.092(12) -0.017(8) 0.030(10) -0.012(7) C78 0.095(11) 0.047(6) 0.040(7) 0.003(6) 0.008(7) -0.009(7) C79 0.089(11) 0.039(6) 0.057(8) -0.009(6) 0.026(8) -0.011(6) C82 0.031(6) 0.043(5) 0.062(8) -0.012(5) 0.003(5) -0.014(4) C83 0.037(6) 0.053(6) 0.034(6) -0.006(5) -0.010(5) 0.010(5) C84 0.049(7) 0.057(7) 0.055(8) 0.011(6) 0.011(6) 0.015(6) C85 0.045(6) 0.032(5) 0.055(7) -0.009(5) -0.004(5) 0.001(4) C86 0.036(6) 0.043(5) 0.048(7) -0.008(5) 0.000(5) -0.003(4) C87 0.044(6) 0.040(5) 0.049(7) -0.003(5) 0.008(5) -0.005(5) C88 0.037(6) 0.046(5) 0.050(7) -0.013(5) 0.004(5) -0.002(5) N1 0.041(6) 0.048(5) 0.062(7) 0.012(5) 0.000(5) -0.002(4) N2 0.052(6) 0.048(5) 0.051(6) 0.013(4) 0.002(5) 0.001(4) N3 0.071(7) 0.040(5) 0.079(8) 0.017(5) 0.017(6) 0.003(5) N4 0.052(6) 0.052(5) 0.070(8) 0.009(5) -0.004(5) -0.002(5) N5 0.030(5) 0.051(5) 0.063(7) -0.006(5) 0.003(4) 0.001(4) N6 0.053(6) 0.050(5) 0.045(6) -0.005(4) 0.009(5) -0.002(4) N7 0.043(5) 0.045(5) 0.072(7) -0.008(5) 0.012(5) -0.007(4) N8 0.033(5) 0.045(5) 0.075(8) 0.005(5) 0.011(5) 0.002(4) N9 0.029(4) 0.049(5) 0.036(5) -0.002(4) 0.005(4) 0.003(4) N10 0.039(5) 0.059(5) 0.041(6) 0.004(4) -0.003(4) -0.001(4) N11 0.046(5) 0.046(5) 0.043(6) 0.009(4) -0.015(4) -0.012(4) N12 0.040(6) 0.069(6) 0.053(7) 0.012(5) -0.016(5) -0.004(5) N13 0.040(5) 0.034(4) 0.052(6) -0.007(4) -0.002(4) 0.005(4) N14 0.068(7) 0.062(6) 0.041(6) -0.019(5) -0.017(5) 0.017(5) N15 0.047(5) 0.039(4) 0.046(6) 0.006(4) -0.008(5) -0.008(4) N16 0.051(6) 0.042(5) 0.059(7) -0.001(5) 0.010(5) -0.002(4) N17 0.077(7) 0.064(6) 0.036(6) 0.002(5) 0.006(5) -0.015(5) N18 0.061(7) 0.044(5) 0.060(7) -0.003(5) 0.015(6) -0.008(4) N19 0.107(11) 0.055(6) 0.087(10) -0.013(6) 0.059(9) -0.021(6) N20 0.129(12) 0.069(7) 0.050(7) 0.017(6) 0.015(8) -0.028(8) O1W 0.114(8) 0.071(6) 0.052(6) 0.004(5) -0.002(6) -0.031(6) O1 0.084(6) 0.038(4) 0.053(5) -0.001(4) -0.013(5) 0.007(4) O2W 0.070(6) 0.056(5) 0.089(7) 0.013(5) 0.024(6) -0.006(4) O2 0.078(6) 0.036(4) 0.051(5) 0.004(4) -0.012(4) 0.002(4) O5 0.052(5) 0.048(4) 0.046(5) -0.005(4) -0.013(4) 0.009(4) O6W 0.077(7) 0.060(5) 0.098(8) -0.017(5) -0.002(6) 0.028(5) O6 0.054(5) 0.034(4) 0.068(6) -0.014(4) -0.013(4) 0.001(3) O7W 0.115(9) 0.063(5) 0.076(7) 0.000(5) 0.008(6) 0.032(5) O9 0.038(4) 0.052(4) 0.105(8) -0.003(5) 0.018(5) 0.002(4) O10 0.045(5) 0.055(4) 0.068(6) -0.011(4) 0.015(4) -0.013(4) O11 0.043(5) 0.075(5) 0.065(6) 0.001(5) -0.005(4) 0.021(4) O12 0.059(6) 0.044(4) 0.126(9) -0.026(5) 0.021(6) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1W 2.056(10) . ? Co1 N2 2.115(9) . ? Co1 O2W 2.149(9) . ? Co1 O2 2.156(7) . ? Co1 N1 2.161(9) . ? Co1 O1 2.220(8) . ? Co2 N10 2.092(9) . ? Co2 N9 2.137(8) . ? Co2 O5 2.149(7) . ? Co2 N6 2.149(9) . ? Co2 N5 2.152(9) . ? Co2 O6 2.269(8) . ? Co3 O3 1.996(7) 4_464 ? Co3 N13 2.035(9) . ? Co3 N11 2.037(9) . ? Co3 O11 2.083(8) 2_565 ? Co3 O12 2.382(9) 2_565 ? Co4 N16 2.087(11) . ? Co4 N17 2.128(11) . ? Co4 N15 2.140(9) . ? Co4 N18 2.165(10) . ? Co4 O7 2.166(7) . ? Co4 O8 2.202(7) . ? Co4 C80 2.505(11) . ? C1 C6 1.379(17) . ? C1 N1 1.392(16) . ? C1 C2 1.40(2) . ? C2 C3 1.41(2) . ? C2 H2A 0.84(10) . ? C3 C4 1.34(2) . ? C3 H3A 0.9300 . ? C4 C5 1.35(2) . ? C4 H4A 0.9300 . ? C5 C6 1.42(2) . ? C5 H5A 0.9300 . ? C6 N4 1.394(16) . ? C7 N2 1.386(15) . ? C7 C8 1.396(18) . ? C7 C12 1.399(17) . ? C8 C9 1.41(2) . ? C8 H8A 0.9300 . ? C9 C10 1.39(3) . ? C9 H9A 0.9300 . ? C10 C11 1.39(2) . ? C10 H10A 0.9300 . ? C11 C12 1.398(18) . ? C11 H11A 0.9300 . ? C12 N3 1.395(16) . ? C13 N1 1.320(13) . ? C13 N4 1.338(15) . ? C13 C14 1.465(16) . ? C14 N2 1.337(14) . ? C14 N3 1.370(13) . ? C15 O1 1.271(12) . ? C15 O2 1.285(13) . ? C15 C16 1.492(15) . ? C16 C23 1.383(15) . ? C16 C17 1.393(13) . ? C17 C18 1.403(14) . ? C17 H17A 0.9300 . ? C18 C20 1.403(15) . ? C18 C19 1.488(14) . ? C19 O4 1.252(14) . ? C19 O3 1.280(13) . ? C20 C21 1.402(13) . ? C20 H20A 0.9300 . ? C21 C23 1.413(15) . ? C21 C22 1.496(15) . ? C22 O5 1.253(12) . ? C22 O6 1.267(11) . ? C23 H23A 0.9300 . ? C24 C25 1.391(15) . ? C24 C29 1.403(16) . ? C24 N5 1.407(13) . ? C25 C26 1.385(19) . ? C25 H25A 0.9300 . ? C26 C27 1.40(2) . ? C26 H26A 0.9300 . ? C27 C28 1.388(18) . ? C27 H27A 0.9300 . ? C28 C29 1.400(16) . ? C28 H28A 0.9300 . ? C29 N8 1.364(14) . ? C30 N6 1.403(13) . ? C30 C35 1.404(16) . ? C30 C31 1.405(16) . ? C31 C32 1.375(17) . ? C31 H31A 0.9300 . ? C32 C33 1.40(2) . ? C32 H32A 0.9300 . ? C33 C34 1.360(18) . ? C33 H33A 0.9300 . ? C34 C35 1.402(16) . ? C34 H34A 0.9300 . ? C35 N7 1.403(15) . ? C36 N5 1.327(13) . ? C36 N8 1.348(14) . ? C36 C37 1.462(14) . ? C37 N6 1.318(14) . ? C37 N7 1.347(13) . ? C38 N9 1.373(14) . ? C38 C43 1.378(16) . ? C38 C39 1.432(16) . ? C39 C40 1.386(18) . ? C39 H39A 0.9300 . ? C40 C41 1.40(2) . ? C40 H40A 0.9300 . ? C41 C42 1.39(2) . ? C41 H41A 0.9300 . ? C42 C43 1.419(17) . ? C42 H42A 0.9300 . ? C43 N12 1.361(15) . ? C44 C49 1.388(16) . ? C44 N10 1.389(14) . ? C44 C45 1.405(16) . ? C45 C46 1.373(19) . ? C45 H45A 0.9300 . ? C46 C47 1.40(2) . ? C46 H46A 0.9300 . ? C47 C48 1.368(19) . ? C47 H47A 0.9300 . ? C48 C49 1.426(17) . ? C48 H48A 0.9300 . ? C49 N11 1.405(14) . ? C50 N9 1.329(13) . ? C50 N12 1.374(14) . ? C50 C51 1.418(16) . ? C51 N10 1.359(14) . ? C51 N11 1.374(14) . ? C52 N13 1.390(14) . ? C52 C57 1.402(17) . ? C52 C53 1.422(18) . ? C53 C54 1.359(18) . ? C53 H53A 0.9300 . ? C54 C55 1.42(2) . ? C54 H54A 0.9300 . ? C55 C56 1.39(2) . ? C55 H55A 0.9300 . ? C56 C57 1.435(15) . ? C56 H56A 0.9300 . ? C57 N16 1.374(14) . ? C58 C59 1.380(16) . ? C58 N14 1.381(14) . ? C58 C63 1.395(17) . ? C59 C60 1.365(19) . ? C59 H59A 0.9300 . ? C60 C61 1.38(2) . ? C60 H60A 0.9300 . ? C61 C62 1.372(19) . ? C61 H61A 0.9300 . ? C62 C63 1.399(16) . ? C62 H62A 0.9300 . ? C63 N15 1.420(14) . ? C64 N13 1.351(14) . ? C64 N16 1.363(14) . ? C64 C65 1.473(15) . ? C65 N15 1.298(14) . ? C65 N14 1.349(14) . ? C66 C67 1.40(2) . ? C66 C71 1.41(2) . ? C66 N17 1.419(18) . ? C67 C68 1.40(2) . ? C67 H67A 0.9300 . ? C68 C69 1.38(3) . ? C68 H68A 0.9300 . ? C69 C70 1.42(3) . ? C69 H69A 0.9300 . ? C70 C71 1.39(2) . ? C70 H70A 0.9300 . ? C71 N20 1.39(2) . ? C72 N18 1.391(17) . ? C72 C77 1.39(2) . ? C72 C73 1.39(2) . ? C73 C74 1.34(2) . ? C73 H73A 0.9300 . ? C74 C75 1.41(3) . ? C74 H74A 0.9300 . ? C75 C76 1.33(3) . ? C75 H75A 0.9300 . ? C76 C77 1.40(2) . ? C76 H76A 0.9300 . ? C77 N19 1.40(2) . ? C78 N17 1.337(16) . ? C78 N20 1.342(17) . ? C78 C79 1.485(19) . ? C79 N18 1.303(16) . ? C79 N19 1.346(16) . ? C80 O7 1.249(13) . ? C80 O8 1.266(13) . ? C80 C81 1.518(14) . ? C81 C88 1.373(15) . ? C81 C82 1.408(14) . ? C82 C83 1.388(14) . ? C82 H82A 0.9300 . ? C83 C85 1.404(15) . ? C83 C84 1.530(14) . ? C84 O12 1.241(14) . ? C84 O11 1.276(14) . ? C85 C86 1.392(14) . ? C85 H85A 0.9300 . ? C86 C88 1.402(14) . ? C86 C87 1.503(14) . ? C87 O9 1.262(12) . ? C87 O10 1.268(12) . ? C88 H88A 0.9300 . ? N3 O6W 2.869(14) 2_565 ? N3 H3B 0.8600 . ? N4 O6W 2.785(13) 2_565 ? N4 H4B 0.8600 . ? N7 O9 2.755(12) 2_665 ? N7 H7A 0.8600 . ? N8 O10 2.666(12) 2_665 ? N8 H8B 0.8600 . ? N12 O11 2.785(13) 2_565 ? N12 H12A 0.8600 . ? N14 O3 2.778(12) 4_464 ? N14 H14A 0.8600 . ? N19 O3W 2.84(2) 1 ? N19 H19A 0.8600 . ? N20 O3W 2.861(19) 1 ? N20 H20B 0.8600 . ? O3W O3W 0.00(4) 1 ? O3 Co3 1.996(7) 4_565 ? O11 Co3 2.083(8) 2_564 ? O12 Co3 2.382(9) 2_564 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Co1 N2 101.1(4) . . ? O1W Co1 O2W 98.9(4) . . ? N2 Co1 O2W 89.7(4) . . ? O1W Co1 O2 89.3(4) . . ? N2 Co1 O2 169.5(4) . . ? O2W Co1 O2 87.8(3) . . ? O1W Co1 N1 93.6(4) . . ? N2 Co1 N1 79.3(4) . . ? O2W Co1 N1 164.7(4) . . ? O2 Co1 N1 101.2(3) . . ? O1W Co1 O1 148.4(4) . . ? N2 Co1 O1 109.5(3) . . ? O2W Co1 O1 89.0(4) . . ? O2 Co1 O1 60.3(3) . . ? N1 Co1 O1 84.9(4) . . ? N10 Co2 N9 79.1(3) . . ? N10 Co2 O5 110.0(3) . . ? N9 Co2 O5 95.5(3) . . ? N10 Co2 N6 101.9(4) . . ? N9 Co2 N6 99.0(3) . . ? O5 Co2 N6 146.9(3) . . ? N10 Co2 N5 97.3(4) . . ? N9 Co2 N5 174.6(4) . . ? O5 Co2 N5 89.4(3) . . ? N6 Co2 N5 77.7(3) . . ? N10 Co2 O6 167.0(3) . . ? N9 Co2 O6 94.4(3) . . ? O5 Co2 O6 59.1(3) . . ? N6 Co2 O6 90.2(3) . . ? N5 Co2 O6 89.9(3) . . ? O3 Co3 N13 105.2(3) 4_464 . ? O3 Co3 N11 102.4(3) 4_464 . ? N13 Co3 N11 103.2(4) . . ? O3 Co3 O11 137.3(3) 4_464 2_565 ? N13 Co3 O11 98.3(3) . 2_565 ? N11 Co3 O11 106.4(3) . 2_565 ? O3 Co3 O12 87.2(3) 4_464 2_565 ? N13 Co3 O12 87.4(4) . 2_565 ? N11 Co3 O12 163.0(4) . 2_565 ? O11 Co3 O12 58.4(3) 2_565 2_565 ? N16 Co4 N17 172.8(4) . . ? N16 Co4 N15 78.8(3) . . ? N17 Co4 N15 96.6(4) . . ? N16 Co4 N18 97.2(4) . . ? N17 Co4 N18 78.5(4) . . ? N15 Co4 N18 104.0(3) . . ? N16 Co4 O7 91.5(3) . . ? N17 Co4 O7 94.9(4) . . ? N15 Co4 O7 154.2(3) . . ? N18 Co4 O7 100.8(3) . . ? N16 Co4 O8 96.3(3) . . ? N17 Co4 O8 89.7(4) . . ? N15 Co4 O8 96.8(3) . . ? N18 Co4 O8 157.0(3) . . ? O7 Co4 O8 60.2(3) . . ? N16 Co4 C80 94.1(4) . . ? N17 Co4 C80 93.1(4) . . ? N15 Co4 C80 126.2(4) . . ? N18 Co4 C80 129.8(4) . . ? O7 Co4 C80 29.9(3) . . ? O8 Co4 C80 30.3(3) . . ? C6 C1 N1 109.9(11) . . ? C6 C1 C2 119.8(14) . . ? N1 C1 C2 130.4(13) . . ? C1 C2 C3 117.3(16) . . ? C1 C2 H2A 118(8) . . ? C3 C2 H2A 122(8) . . ? C4 C3 C2 119.7(17) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C3 C4 C5 126.1(18) . . ? C3 C4 H4A 117.0 . . ? C5 C4 H4A 117.0 . . ? C4 C5 C6 114.5(17) . . ? C4 C5 H5A 122.7 . . ? C6 C5 H5A 122.7 . . ? C1 C6 N4 105.7(12) . . ? C1 C6 C5 122.5(14) . . ? N4 C6 C5 131.8(14) . . ? N2 C7 C8 131.2(11) . . ? N2 C7 C12 108.8(11) . . ? C8 C7 C12 119.9(12) . . ? C7 C8 C9 116.4(15) . . ? C7 C8 H8A 121.8 . . ? C9 C8 H8A 121.8 . . ? C10 C9 C8 122.5(17) . . ? C10 C9 H9A 118.7 . . ? C8 C9 H9A 118.7 . . ? C9 C10 C11 121.3(16) . . ? C9 C10 H10A 119.3 . . ? C11 C10 H10A 119.3 . . ? C10 C11 C12 115.7(16) . . ? C10 C11 H11A 122.2 . . ? C12 C11 H11A 122.2 . . ? N3 C12 C11 129.4(14) . . ? N3 C12 C7 106.8(10) . . ? C11 C12 C7 123.9(14) . . ? N1 C13 N4 114.0(11) . . ? N1 C13 C14 117.1(10) . . ? N4 C13 C14 128.7(10) . . ? N2 C14 N3 112.3(10) . . ? N2 C14 C13 119.6(9) . . ? N3 C14 C13 127.9(10) . . ? O1 C15 O2 118.7(10) . . ? O1 C15 C16 121.7(10) . . ? O2 C15 C16 119.4(9) . . ? C23 C16 C17 120.5(10) . . ? C23 C16 C15 119.6(9) . . ? C17 C16 C15 119.8(9) . . ? C16 C17 C18 119.7(10) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C17 C18 C20 119.8(8) . . ? C17 C18 C19 119.4(10) . . ? C20 C18 C19 120.7(10) . . ? O4 C19 O3 121.0(10) . . ? O4 C19 C18 121.7(11) . . ? O3 C19 C18 117.3(10) . . ? C21 C20 C18 120.5(10) . . ? C21 C20 H20A 119.8 . . ? C18 C20 H20A 119.8 . . ? C20 C21 C23 118.7(11) . . ? C20 C21 C22 118.8(9) . . ? C23 C21 C22 122.5(9) . . ? O5 C22 O6 119.9(10) . . ? O5 C22 C21 120.1(9) . . ? O6 C22 C21 119.9(9) . . ? C16 C23 C21 120.7(9) . . ? C16 C23 H23A 119.6 . . ? C21 C23 H23A 119.6 . . ? C25 C24 C29 121.3(10) . . ? C25 C24 N5 129.7(11) . . ? C29 C24 N5 108.9(9) . . ? C26 C25 C24 117.8(12) . . ? C26 C25 H25A 121.1 . . ? C24 C25 H25A 121.1 . . ? C25 C26 C27 121.2(12) . . ? C25 C26 H26A 119.4 . . ? C27 C26 H26A 119.4 . . ? C28 C27 C26 121.4(13) . . ? C28 C27 H27A 119.3 . . ? C26 C27 H27A 119.3 . . ? C27 C28 C29 117.7(13) . . ? C27 C28 H28A 121.2 . . ? C29 C28 H28A 121.2 . . ? N8 C29 C28 133.3(11) . . ? N8 C29 C24 106.1(10) . . ? C28 C29 C24 120.6(11) . . ? N6 C30 C35 108.8(10) . . ? N6 C30 C31 132.3(11) . . ? C35 C30 C31 118.9(10) . . ? C32 C31 C30 118.6(12) . . ? C32 C31 H31A 120.7 . . ? C30 C31 H31A 120.7 . . ? C31 C32 C33 121.3(12) . . ? C31 C32 H32A 119.3 . . ? C33 C32 H32A 119.3 . . ? C34 C33 C32 121.5(12) . . ? C34 C33 H33A 119.2 . . ? C32 C33 H33A 119.2 . . ? C33 C34 C35 117.5(12) . . ? C33 C34 H34A 121.2 . . ? C35 C34 H34A 121.2 . . ? C34 C35 N7 131.8(12) . . ? C34 C35 C30 122.1(11) . . ? N7 C35 C30 106.1(9) . . ? N5 C36 N8 113.4(9) . . ? N5 C36 C37 118.1(10) . . ? N8 C36 C37 128.5(10) . . ? N6 C37 N7 114.8(9) . . ? N6 C37 C36 117.6(9) . . ? N7 C37 C36 127.5(10) . . ? N9 C38 C43 109.5(11) . . ? N9 C38 C39 130.4(11) . . ? C43 C38 C39 120.0(12) . . ? C40 C39 C38 117.1(12) . . ? C40 C39 H39A 121.4 . . ? C38 C39 H39A 121.4 . . ? C39 C40 C41 122.3(13) . . ? C39 C40 H40A 118.9 . . ? C41 C40 H40A 118.9 . . ? C42 C41 C40 121.2(13) . . ? C42 C41 H41A 119.4 . . ? C40 C41 H41A 119.4 . . ? C41 C42 C43 116.5(13) . . ? C41 C42 H42A 121.8 . . ? C43 C42 H42A 121.8 . . ? N12 C43 C38 106.8(10) . . ? N12 C43 C42 130.4(11) . . ? C38 C43 C42 122.8(12) . . ? C49 C44 N10 107.7(10) . . ? C49 C44 C45 119.4(11) . . ? N10 C44 C45 132.7(11) . . ? C46 C45 C44 118.9(12) . . ? C46 C45 H45A 120.6 . . ? C44 C45 H45A 120.6 . . ? C45 C46 C47 121.5(13) . . ? C45 C46 H46A 119.2 . . ? C47 C46 H46A 119.2 . . ? C48 C47 C46 121.3(14) . . ? C48 C47 H47A 119.3 . . ? C46 C47 H47A 119.3 . . ? C47 C48 C49 117.3(13) . . ? C47 C48 H48A 121.3 . . ? C49 C48 H48A 121.3 . . ? C44 C49 N11 109.7(10) . . ? C44 C49 C48 121.6(11) . . ? N11 C49 C48 128.5(11) . . ? N9 C50 N12 111.2(10) . . ? N9 C50 C51 119.7(10) . . ? N12 C50 C51 128.9(10) . . ? N10 C51 N11 113.5(10) . . ? N10 C51 C50 116.9(10) . . ? N11 C51 C50 129.5(10) . . ? N13 C52 C57 108.4(10) . . ? N13 C52 C53 130.6(13) . . ? C57 C52 C53 120.9(11) . . ? C54 C53 C52 118.6(15) . . ? C54 C53 H53A 120.7 . . ? C52 C53 H53A 120.7 . . ? C53 C54 C55 120.4(14) . . ? C53 C54 H54A 119.8 . . ? C55 C54 H54A 119.8 . . ? C56 C55 C54 123.3(11) . . ? C56 C55 H55A 118.4 . . ? C54 C55 H55A 118.4 . . ? C55 C56 C57 115.6(13) . . ? C55 C56 H56A 122.2 . . ? C57 C56 H56A 122.2 . . ? N16 C57 C52 109.1(9) . . ? N16 C57 C56 129.8(12) . . ? C52 C57 C56 121.1(12) . . ? C59 C58 N14 132.6(12) . . ? C59 C58 C63 121.5(11) . . ? N14 C58 C63 105.9(9) . . ? C60 C59 C58 117.3(14) . . ? C60 C59 H59A 121.4 . . ? C58 C59 H59A 121.4 . . ? C59 C60 C61 122.1(13) . . ? C59 C60 H60A 119.0 . . ? C61 C60 H60A 119.0 . . ? C62 C61 C60 121.6(13) . . ? C62 C61 H61A 119.2 . . ? C60 C61 H61A 119.2 . . ? C61 C62 C63 117.3(14) . . ? C61 C62 H62A 121.3 . . ? C63 C62 H62A 121.3 . . ? C58 C63 C62 120.2(11) . . ? C58 C63 N15 108.4(10) . . ? C62 C63 N15 131.3(12) . . ? N13 C64 N16 115.1(9) . . ? N13 C64 C65 129.5(10) . . ? N16 C64 C65 115.3(10) . . ? N15 C65 N14 114.1(10) . . ? N15 C65 C64 118.7(10) . . ? N14 C65 C64 127.0(10) . . ? C67 C66 C71 122.5(16) . . ? C67 C66 N17 129.2(14) . . ? C71 C66 N17 108.2(14) . . ? C66 C67 C68 115.6(16) . . ? C66 C67 H67A 122.2 . . ? C68 C67 H67A 122.2 . . ? C69 C68 C67 121.4(18) . . ? C69 C68 H68A 119.3 . . ? C67 C68 H68A 119.3 . . ? C68 C69 C70 123.6(17) . . ? C68 C69 H69A 118.2 . . ? C70 C69 H69A 118.2 . . ? C71 C70 C69 114.6(19) . . ? C71 C70 H70A 122.7 . . ? C69 C70 H70A 122.7 . . ? N20 C71 C70 131.5(17) . . ? N20 C71 C66 106.2(14) . . ? C70 C71 C66 122(2) . . ? N18 C72 C77 109.8(14) . . ? N18 C72 C73 132.9(13) . . ? C77 C72 C73 117.3(14) . . ? C74 C73 C72 119.3(17) . . ? C74 C73 H73A 120.3 . . ? C72 C73 H73A 120.3 . . ? C73 C74 C75 122(2) . . ? C73 C74 H74A 119.2 . . ? C75 C74 H74A 119.2 . . ? C76 C75 C74 121.3(18) . . ? C76 C75 H75A 119.3 . . ? C74 C75 H75A 119.3 . . ? C75 C76 C77 116.4(19) . . ? C75 C76 H76A 121.8 . . ? C77 C76 H76A 121.8 . . ? C72 C77 C76 124.0(18) . . ? C72 C77 N19 104.7(13) . . ? C76 C77 N19 131.3(17) . . ? N17 C78 N20 113.4(14) . . ? N17 C78 C79 116.8(11) . . ? N20 C78 C79 129.8(13) . . ? N18 C79 N19 113.8(14) . . ? N18 C79 C78 118.7(11) . . ? N19 C79 C78 127.5(14) . . ? O7 C80 O8 121.3(10) . . ? O7 C80 C81 119.4(10) . . ? O8 C80 C81 119.3(10) . . ? O7 C80 Co4 59.8(6) . . ? O8 C80 Co4 61.5(5) . . ? C81 C80 Co4 176.5(9) . . ? C88 C81 C82 121.2(9) . . ? C88 C81 C80 119.9(9) . . ? C82 C81 C80 118.9(9) . . ? C83 C82 C81 117.9(10) . . ? C83 C82 H82A 121.1 . . ? C81 C82 H82A 121.1 . . ? C82 C83 C85 121.1(9) . . ? C82 C83 C84 123.7(10) . . ? C85 C83 C84 115.2(9) . . ? O12 C84 O11 121.3(10) . . ? O12 C84 C83 121.9(11) . . ? O11 C84 C83 116.7(11) . . ? C86 C85 C83 120.5(9) . . ? C86 C85 H85A 119.8 . . ? C83 C85 H85A 119.8 . . ? C85 C86 C88 118.3(10) . . ? C85 C86 C87 118.3(9) . . ? C88 C86 C87 123.4(9) . . ? O9 C87 O10 123.2(10) . . ? O9 C87 C86 119.3(9) . . ? O10 C87 C86 117.4(9) . . ? C81 C88 C86 121.1(10) . . ? C81 C88 H88A 119.4 . . ? C86 C88 H88A 119.4 . . ? C13 N1 C1 104.2(9) . . ? C13 N1 Co1 111.3(8) . . ? C1 N1 Co1 144.3(8) . . ? C14 N2 C7 106.1(9) . . ? C14 N2 Co1 110.5(7) . . ? C7 N2 Co1 142.7(8) . . ? C14 N3 C12 106.0(10) . . ? C14 N3 O6W 106.2(8) . 2_565 ? C12 N3 O6W 146.1(8) . 2_565 ? C14 N3 H3B 127.0 . . ? C12 N3 H3B 127.0 . . ? O6W N3 H3B 22.8 2_565 . ? C13 N4 C6 106.3(10) . . ? C13 N4 O6W 109.3(8) . 2_565 ? C6 N4 O6W 144.2(8) . 2_565 ? C13 N4 H4B 126.9 . . ? C6 N4 H4B 126.9 . . ? O6W N4 H4B 17.8 2_565 . ? C36 N5 C24 104.1(9) . . ? C36 N5 Co2 112.9(7) . . ? C24 N5 Co2 142.8(7) . . ? C37 N6 C30 104.7(9) . . ? C37 N6 Co2 113.6(7) . . ? C30 N6 Co2 141.4(8) . . ? C37 N7 C35 105.6(9) . . ? C37 N7 O9 136.7(7) . 2_665 ? C35 N7 O9 116.4(7) . 2_665 ? C37 N7 H7A 127.2 . . ? C35 N7 H7A 127.2 . . ? O9 N7 H7A 14.3 2_665 . ? C36 N8 C29 107.4(9) . . ? C36 N8 O10 124.3(7) . 2_665 ? C29 N8 O10 128.0(7) . 2_665 ? C36 N8 H8B 126.3 . . ? C29 N8 H8B 126.3 . . ? O10 N8 H8B 4.9 2_665 . ? C50 N9 C38 105.8(9) . . ? C50 N9 Co2 110.8(7) . . ? C38 N9 Co2 143.5(8) . . ? C51 N10 C44 105.7(9) . . ? C51 N10 Co2 112.4(7) . . ? C44 N10 Co2 141.4(8) . . ? C51 N11 C49 103.4(9) . . ? C51 N11 Co3 133.9(8) . . ? C49 N11 Co3 122.6(7) . . ? C43 N12 C50 106.8(9) . . ? C43 N12 O11 134.3(8) . 2_565 ? C50 N12 O11 114.1(8) . 2_565 ? C43 N12 H12A 126.6 . . ? C50 N12 H12A 126.6 . . ? O11 N12 H12A 21.9 2_565 . ? C64 N13 C52 103.7(9) . . ? C64 N13 Co3 135.2(7) . . ? C52 N13 Co3 121.1(8) . . ? C65 N14 C58 106.8(10) . . ? C65 N14 O3 112.2(7) . 4_464 ? C58 N14 O3 134.9(7) . 4_464 ? C65 N14 H14A 126.6 . . ? C58 N14 H14A 126.6 . . ? O3 N14 H14A 24.6 4_464 . ? C65 N15 C63 104.8(10) . . ? C65 N15 Co4 112.9(7) . . ? C63 N15 Co4 141.3(8) . . ? C64 N16 C57 103.7(10) . . ? C64 N16 Co4 114.1(7) . . ? C57 N16 Co4 142.2(8) . . ? C78 N17 C66 104.7(11) . . ? C78 N17 Co4 113.4(9) . . ? C66 N17 Co4 141.3(9) . . ? C79 N18 C72 105.2(11) . . ? C79 N18 Co4 112.4(9) . . ? C72 N18 Co4 142.3(10) . . ? C79 N19 C77 106.5(13) . . ? C79 N19 O3W 107.8(11) . 1 ? C77 N19 O3W 143.7(9) . 1 ? C79 N19 H19A 126.8 . . ? C77 N19 H19A 126.8 . . ? O3W N19 H19A 21.7 1 . ? C78 N20 C71 107.5(12) . . ? C78 N20 O3W 106.4(11) . 1 ? C71 N20 O3W 145.8(10) . 1 ? C78 N20 H20B 126.3 . . ? C71 N20 H20B 126.3 . . ? O3W N20 H20B 20.3 1 . ? C15 O1 Co1 89.2(7) . . ? C15 O2 Co1 91.7(6) . . ? C19 O3 Co3 110.7(7) . 4_565 ? C22 O5 Co2 93.2(6) . . ? C22 O6 Co2 87.4(6) . . ? C80 O7 Co4 90.3(6) . . ? C80 O8 Co4 88.2(6) . . ? C84 O11 Co3 96.0(7) . 2_564 ? C84 O12 Co3 83.3(7) . 2_564 ? 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 C6 C1 C2 C3 1(2) . . . . ? N1 C1 C2 C3 -179.6(17) . . . . ? C1 C2 C3 C4 0(3) . . . . ? C2 C3 C4 C5 -1(4) . . . . ? C3 C4 C5 C6 0(3) . . . . ? N1 C1 C6 N4 -1.4(16) . . . . ? C2 C1 C6 N4 177.8(14) . . . . ? N1 C1 C6 C5 178.3(14) . . . . ? C2 C1 C6 C5 -3(2) . . . . ? C4 C5 C6 C1 2(2) . . . . ? C4 C5 C6 N4 -178.6(16) . . . . ? N2 C7 C8 C9 177.3(15) . . . . ? C12 C7 C8 C9 1(2) . . . . ? C7 C8 C9 C10 3(3) . . . . ? C8 C9 C10 C11 -6(3) . . . . ? C9 C10 C11 C12 4(3) . . . . ? C10 C11 C12 N3 -178.6(18) . . . . ? C10 C11 C12 C7 1(3) . . . . ? N2 C7 C12 N3 -0.6(16) . . . . ? C8 C7 C12 N3 176.2(13) . . . . ? N2 C7 C12 C11 179.8(15) . . . . ? C8 C7 C12 C11 -3(2) . . . . ? N1 C13 C14 N2 4.6(18) . . . . ? N4 C13 C14 N2 -169.4(13) . . . . ? N1 C13 C14 N3 179.9(12) . . . . ? N4 C13 C14 N3 6(2) . . . . ? O1 C15 C16 C23 8.3(17) . . . . ? O2 C15 C16 C23 -176.3(11) . . . . ? O1 C15 C16 C17 -169.0(11) . . . . ? O2 C15 C16 C17 6.4(17) . . . . ? C23 C16 C17 C18 -1.4(17) . . . . ? C15 C16 C17 C18 175.9(11) . . . . ? C16 C17 C18 C20 1.7(17) . . . . ? C16 C17 C18 C19 -176.6(10) . . . . ? C17 C18 C19 O4 -16.9(17) . . . . ? C20 C18 C19 O4 164.8(11) . . . . ? C17 C18 C19 O3 160.7(10) . . . . ? C20 C18 C19 O3 -17.6(16) . . . . ? C17 C18 C20 C21 -0.7(16) . . . . ? C19 C18 C20 C21 177.6(10) . . . . ? C18 C20 C21 C23 -0.7(16) . . . . ? C18 C20 C21 C22 -179.7(10) . . . . ? C20 C21 C22 O5 -11.2(16) . . . . ? C23 C21 C22 O5 169.8(10) . . . . ? C20 C21 C22 O6 166.3(10) . . . . ? C23 C21 C22 O6 -12.7(17) . . . . ? C17 C16 C23 C21 0.0(17) . . . . ? C15 C16 C23 C21 -177.3(10) . . . . ? C20 C21 C23 C16 1.1(16) . . . . ? C22 C21 C23 C16 -179.9(11) . . . . ? C29 C24 C25 C26 -2(2) . . . . ? N5 C24 C25 C26 178.0(14) . . . . ? C24 C25 C26 C27 1(2) . . . . ? C25 C26 C27 C28 0(3) . . . . ? C26 C27 C28 C29 0(2) . . . . ? C27 C28 C29 N8 -178.1(14) . . . . ? C27 C28 C29 C24 -1(2) . . . . ? C25 C24 C29 N8 179.7(12) . . . . ? N5 C24 C29 N8 -0.1(14) . . . . ? C25 C24 C29 C28 1.8(19) . . . . ? N5 C24 C29 C28 -177.9(11) . . . . ? N6 C30 C31 C32 -179.5(14) . . . . ? C35 C30 C31 C32 0(2) . . . . ? C30 C31 C32 C33 0(2) . . . . ? C31 C32 C33 C34 1(3) . . . . ? C32 C33 C34 C35 -1(2) . . . . ? C33 C34 C35 N7 -179.1(15) . . . . ? C33 C34 C35 C30 1(2) . . . . ? N6 C30 C35 C34 179.6(12) . . . . ? C31 C30 C35 C34 0(2) . . . . ? N6 C30 C35 N7 -0.7(14) . . . . ? C31 C30 C35 N7 179.6(12) . . . . ? N5 C36 C37 N6 4.1(17) . . . . ? N8 C36 C37 N6 -175.2(11) . . . . ? N5 C36 C37 N7 -172.3(12) . . . . ? N8 C36 C37 N7 8(2) . . . . ? N9 C38 C39 C40 176.5(11) . . . . ? C43 C38 C39 C40 -2.3(17) . . . . ? C38 C39 C40 C41 2.8(19) . . . . ? C39 C40 C41 C42 -1(2) . . . . ? C40 C41 C42 C43 -0.6(19) . . . . ? N9 C38 C43 N12 1.1(13) . . . . ? C39 C38 C43 N12 -179.9(10) . . . . ? N9 C38 C43 C42 -178.7(10) . . . . ? C39 C38 C43 C42 0.4(18) . . . . ? C41 C42 C43 N12 -178.6(12) . . . . ? C41 C42 C43 C38 1.1(18) . . . . ? C49 C44 C45 C46 -1.3(19) . . . . ? N10 C44 C45 C46 -176.0(13) . . . . ? C44 C45 C46 C47 1(2) . . . . ? C45 C46 C47 C48 1(3) . . . . ? C46 C47 C48 C49 -1(2) . . . . ? N10 C44 C49 N11 1.3(13) . . . . ? C45 C44 C49 N11 -174.7(10) . . . . ? N10 C44 C49 C48 176.6(11) . . . . ? C45 C44 C49 C48 0.6(18) . . . . ? C47 C48 C49 C44 1(2) . . . . ? C47 C48 C49 N11 175.0(13) . . . . ? N9 C50 C51 N10 -2.5(15) . . . . ? N12 C50 C51 N10 171.6(10) . . . . ? N9 C50 C51 N11 -179.3(10) . . . . ? N12 C50 C51 N11 -5.2(19) . . . . ? N13 C52 C53 C54 178.5(12) . . . . ? C57 C52 C53 C54 1.3(19) . . . . ? C52 C53 C54 C55 -3(2) . . . . ? C53 C54 C55 C56 3(2) . . . . ? C54 C55 C56 C57 -2(2) . . . . ? N13 C52 C57 N16 0.3(13) . . . . ? C53 C52 C57 N16 178.1(10) . . . . ? N13 C52 C57 C56 -177.6(10) . . . . ? C53 C52 C57 C56 0.2(18) . . . . ? C55 C56 C57 N16 -177.5(12) . . . . ? C55 C56 C57 C52 -0.1(18) . . . . ? N14 C58 C59 C60 -179.7(14) . . . . ? C63 C58 C59 C60 3(2) . . . . ? C58 C59 C60 C61 -2(2) . . . . ? C59 C60 C61 C62 0(2) . . . . ? C60 C61 C62 C63 1(2) . . . . ? C59 C58 C63 C62 -2.9(18) . . . . ? N14 C58 C63 C62 179.4(10) . . . . ? C59 C58 C63 N15 -179.9(11) . . . . ? N14 C58 C63 N15 2.4(12) . . . . ? C61 C62 C63 C58 0.7(17) . . . . ? C61 C62 C63 N15 176.9(11) . . . . ? N13 C64 C65 N15 178.4(11) . . . . ? N16 C64 C65 N15 -5.6(15) . . . . ? N13 C64 C65 N14 -6.2(19) . . . . ? N16 C64 C65 N14 169.7(11) . . . . ? C71 C66 C67 C68 -2(2) . . . . ? N17 C66 C67 C68 177.0(13) . . . . ? C66 C67 C68 C69 1(2) . . . . ? C67 C68 C69 C70 1(3) . . . . ? C68 C69 C70 C71 -2(3) . . . . ? C69 C70 C71 N20 -175.7(17) . . . . ? C69 C70 C71 C66 1(3) . . . . ? C67 C66 C71 N20 178.5(13) . . . . ? N17 C66 C71 N20 -0.8(15) . . . . ? C67 C66 C71 C70 1(2) . . . . ? N17 C66 C71 C70 -177.9(15) . . . . ? N18 C72 C73 C74 -178.7(14) . . . . ? C77 C72 C73 C74 -0.1(19) . . . . ? C72 C73 C74 C75 0(2) . . . . ? C73 C74 C75 C76 1(3) . . . . ? C74 C75 C76 C77 -2(3) . . . . ? N18 C72 C77 C76 178.6(13) . . . . ? C73 C72 C77 C76 0(2) . . . . ? N18 C72 C77 N19 -0.4(14) . . . . ? C73 C72 C77 N19 -179.3(11) . . . . ? C75 C76 C77 C72 1(2) . . . . ? C75 C76 C77 N19 179.8(16) . . . . ? N17 C78 C79 N18 -5.7(17) . . . . ? N20 C78 C79 N18 172.6(13) . . . . ? N17 C78 C79 N19 174.9(11) . . . . ? N20 C78 C79 N19 -7(2) . . . . ? N16 Co4 C80 O7 -85.9(7) . . . . ? N17 Co4 C80 O7 94.6(7) . . . . ? N15 Co4 C80 O7 -165.0(6) . . . . ? N18 Co4 C80 O7 17.0(9) . . . . ? O8 Co4 C80 O7 178.6(11) . . . . ? N16 Co4 C80 O8 95.5(7) . . . . ? N17 Co4 C80 O8 -84.1(7) . . . . ? N15 Co4 C80 O8 16.4(8) . . . . ? N18 Co4 C80 O8 -161.7(6) . . . . ? O7 Co4 C80 O8 -178.6(11) . . . . ? N16 Co4 C80 C81 -7(14) . . . . ? N17 Co4 C80 C81 173(14) . . . . ? N15 Co4 C80 C81 -86(14) . . . . ? N18 Co4 C80 C81 95(14) . . . . ? O7 Co4 C80 C81 79(14) . . . . ? O8 Co4 C80 C81 -103(14) . . . . ? O7 C80 C81 C88 -163.9(11) . . . . ? O8 C80 C81 C88 18.5(17) . . . . ? Co4 C80 C81 C88 119(13) . . . . ? O7 C80 C81 C82 15.6(17) . . . . ? O8 C80 C81 C82 -161.9(11) . . . . ? Co4 C80 C81 C82 -61(14) . . . . ? C88 C81 C82 C83 -1.0(18) . . . . ? C80 C81 C82 C83 179.5(11) . . . . ? C81 C82 C83 C85 0.4(17) . . . . ? C81 C82 C83 C84 177.0(11) . . . . ? C82 C83 C84 O12 -150.1(12) . . . . ? C85 C83 C84 O12 26.7(17) . . . . ? C82 C83 C84 O11 27.4(17) . . . . ? C85 C83 C84 O11 -155.8(11) . . . . ? C82 C83 C85 C86 0.6(18) . . . . ? C84 C83 C85 C86 -176.3(11) . . . . ? C83 C85 C86 C88 -1.0(17) . . . . ? C83 C85 C86 C87 178.0(11) . . . . ? C85 C86 C87 O9 169.9(11) . . . . ? C88 C86 C87 O9 -11.1(18) . . . . ? C85 C86 C87 O10 -9.4(17) . . . . ? C88 C86 C87 O10 169.5(11) . . . . ? C82 C81 C88 C86 0.6(18) . . . . ? C80 C81 C88 C86 -179.9(11) . . . . ? C85 C86 C88 C81 0.5(17) . . . . ? C87 C86 C88 C81 -178.5(11) . . . . ? N4 C13 N1 C1 -0.5(15) . . . . ? C14 C13 N1 C1 -175.4(11) . . . . ? N4 C13 N1 Co1 -177.9(9) . . . . ? C14 C13 N1 Co1 7.2(14) . . . . ? C6 C1 N1 C13 1.2(15) . . . . ? C2 C1 N1 C13 -177.9(16) . . . . ? C6 C1 N1 Co1 177.1(11) . . . . ? C2 C1 N1 Co1 -2(3) . . . . ? O1W Co1 N1 C13 -111.6(9) . . . . ? N2 Co1 N1 C13 -10.9(9) . . . . ? O2W Co1 N1 C13 33.4(19) . . . . ? O2 Co1 N1 C13 158.4(8) . . . . ? O1 Co1 N1 C13 100.0(9) . . . . ? O1W Co1 N1 C1 72.6(15) . . . . ? N2 Co1 N1 C1 173.3(16) . . . . ? O2W Co1 N1 C1 -142.3(16) . . . . ? O2 Co1 N1 C1 -17.4(16) . . . . ? O1 Co1 N1 C1 -75.7(15) . . . . ? N3 C14 N2 C7 -2.0(14) . . . . ? C13 C14 N2 C7 174.0(11) . . . . ? N3 C14 N2 Co1 170.2(8) . . . . ? C13 C14 N2 Co1 -13.8(14) . . . . ? C8 C7 N2 C14 -174.8(15) . . . . ? C12 C7 N2 C14 1.6(15) . . . . ? C8 C7 N2 Co1 17(2) . . . . ? C12 C7 N2 Co1 -166.3(11) . . . . ? O1W Co1 N2 C14 104.5(9) . . . . ? O2W Co1 N2 C14 -156.4(9) . . . . ? O2 Co1 N2 C14 -81(2) . . . . ? N1 Co1 N2 C14 12.9(8) . . . . ? O1 Co1 N2 C14 -67.7(9) . . . . ? O1W Co1 N2 C7 -88.0(14) . . . . ? O2W Co1 N2 C7 11.1(14) . . . . ? O2 Co1 N2 C7 87(2) . . . . ? N1 Co1 N2 C7 -179.5(14) . . . . ? O1 Co1 N2 C7 99.9(14) . . . . ? N2 C14 N3 C12 1.6(15) . . . . ? C13 C14 N3 C12 -174.0(13) . . . . ? N2 C14 N3 O6W 171.0(9) . . . 2_565 ? C13 C14 N3 O6W -4.6(16) . . . 2_565 ? C11 C12 N3 C14 179.0(17) . . . . ? C7 C12 N3 C14 -0.5(16) . . . . ? C11 C12 N3 O6W 18(3) . . . 2_565 ? C7 C12 N3 O6W -162.1(12) . . . 2_565 ? N1 C13 N4 C6 -0.4(16) . . . . ? C14 C13 N4 C6 173.8(13) . . . . ? N1 C13 N4 O6W -177.0(9) . . . 2_565 ? C14 C13 N4 O6W -2.8(17) . . . 2_565 ? C1 C6 N4 C13 1.1(15) . . . . ? C5 C6 N4 C13 -178.6(16) . . . . ? C1 C6 N4 O6W 175.6(11) . . . 2_565 ? C5 C6 N4 O6W -4(3) . . . 2_565 ? N8 C36 N5 C24 0.2(13) . . . . ? C37 C36 N5 C24 -179.2(10) . . . . ? N8 C36 N5 Co2 177.2(8) . . . . ? C37 C36 N5 Co2 -2.2(13) . . . . ? C25 C24 N5 C36 -179.8(13) . . . . ? C29 C24 N5 C36 -0.1(13) . . . . ? C25 C24 N5 Co2 5(2) . . . . ? C29 C24 N5 Co2 -175.5(10) . . . . ? N10 Co2 N5 C36 -100.5(8) . . . . ? N9 Co2 N5 C36 -53(4) . . . . ? O5 Co2 N5 C36 149.4(8) . . . . ? N6 Co2 N5 C36 0.2(8) . . . . ? O6 Co2 N5 C36 90.4(8) . . . . ? N10 Co2 N5 C24 74.7(13) . . . . ? N9 Co2 N5 C24 122(3) . . . . ? O5 Co2 N5 C24 -35.3(13) . . . . ? N6 Co2 N5 C24 175.4(14) . . . . ? O6 Co2 N5 C24 -94.4(13) . . . . ? N7 C37 N6 C30 -2.2(14) . . . . ? C36 C37 N6 C30 -179.0(10) . . . . ? N7 C37 N6 Co2 173.1(8) . . . . ? C36 C37 N6 Co2 -3.7(13) . . . . ? C35 C30 N6 C37 1.7(13) . . . . ? C31 C30 N6 C37 -178.7(14) . . . . ? C35 C30 N6 Co2 -171.4(10) . . . . ? C31 C30 N6 Co2 8(2) . . . . ? N10 Co2 N6 C37 96.9(8) . . . . ? N9 Co2 N6 C37 177.6(8) . . . . ? O5 Co2 N6 C37 -67.4(11) . . . . ? N5 Co2 N6 C37 2.0(8) . . . . ? O6 Co2 N6 C37 -87.9(8) . . . . ? N10 Co2 N6 C30 -90.4(13) . . . . ? N9 Co2 N6 C30 -9.7(13) . . . . ? O5 Co2 N6 C30 105.4(13) . . . . ? N5 Co2 N6 C30 174.7(13) . . . . ? O6 Co2 N6 C30 84.8(13) . . . . ? N6 C37 N7 C35 1.8(15) . . . . ? C36 C37 N7 C35 178.3(12) . . . . ? N6 C37 N7 O9 -163.8(9) . . . 2_665 ? C36 C37 N7 O9 13(2) . . . 2_665 ? C34 C35 N7 C37 179.1(15) . . . . ? C30 C35 N7 C37 -0.6(14) . . . . ? C34 C35 N7 O9 -11.8(19) . . . 2_665 ? C30 C35 N7 O9 168.4(8) . . . 2_665 ? N5 C36 N8 C29 -0.2(14) . . . . ? C37 C36 N8 C29 179.1(12) . . . . ? N5 C36 N8 O10 174.3(8) . . . 2_665 ? C37 C36 N8 O10 -6.4(18) . . . 2_665 ? C28 C29 N8 C36 177.6(14) . . . . ? C24 C29 N8 C36 0.2(13) . . . . ? C28 C29 N8 O10 3(2) . . . 2_665 ? C24 C29 N8 O10 -174.1(8) . . . 2_665 ? N12 C50 N9 C38 0.9(11) . . . . ? C51 C50 N9 C38 176.1(9) . . . . ? N12 C50 N9 Co2 179.5(7) . . . . ? C51 C50 N9 Co2 -5.4(12) . . . . ? C43 C38 N9 C50 -1.2(12) . . . . ? C39 C38 N9 C50 179.9(11) . . . . ? C43 C38 N9 Co2 -179.0(9) . . . . ? C39 C38 N9 Co2 2(2) . . . . ? N10 Co2 N9 C50 7.7(7) . . . . ? O5 Co2 N9 C50 117.0(7) . . . . ? N6 Co2 N9 C50 -92.8(7) . . . . ? N5 Co2 N9 C50 -40(4) . . . . ? O6 Co2 N9 C50 176.3(7) . . . . ? N10 Co2 N9 C38 -174.6(12) . . . . ? O5 Co2 N9 C38 -65.3(12) . . . . ? N6 Co2 N9 C38 84.9(12) . . . . ? N5 Co2 N9 C38 137(3) . . . . ? O6 Co2 N9 C38 -6.0(12) . . . . ? N11 C51 N10 C44 0.2(12) . . . . ? C50 C51 N10 C44 -177.1(9) . . . . ? N11 C51 N10 Co2 -173.4(7) . . . . ? C50 C51 N10 Co2 9.2(12) . . . . ? C49 C44 N10 C51 -0.9(12) . . . . ? C45 C44 N10 C51 174.3(13) . . . . ? C49 C44 N10 Co2 169.7(9) . . . . ? C45 C44 N10 Co2 -15(2) . . . . ? N9 Co2 N10 C51 -9.1(7) . . . . ? O5 Co2 N10 C51 -101.1(8) . . . . ? N6 Co2 N10 C51 88.0(8) . . . . ? N5 Co2 N10 C51 166.9(7) . . . . ? O6 Co2 N10 C51 -70.1(17) . . . . ? N9 Co2 N10 C44 -179.2(12) . . . . ? O5 Co2 N10 C44 88.8(12) . . . . ? N6 Co2 N10 C44 -82.1(12) . . . . ? N5 Co2 N10 C44 -3.2(12) . . . . ? O6 Co2 N10 C44 119.8(16) . . . . ? N10 C51 N11 C49 0.6(12) . . . . ? C50 C51 N11 C49 177.5(11) . . . . ? N10 C51 N11 Co3 -175.4(8) . . . . ? C50 C51 N11 Co3 1.5(18) . . . . ? C44 C49 N11 C51 -1.1(12) . . . . ? C48 C49 N11 C51 -176.0(13) . . . . ? C44 C49 N11 Co3 175.4(7) . . . . ? C48 C49 N11 Co3 0.5(17) . . . . ? O3 Co3 N11 C51 121.5(10) 4_464 . . . ? N13 Co3 N11 C51 -129.4(10) . . . . ? O11 Co3 N11 C51 -26.5(11) 2_565 . . . ? O12 Co3 N11 C51 -2(2) 2_565 . . . ? O3 Co3 N11 C49 -53.8(9) 4_464 . . . ? N13 Co3 N11 C49 55.3(9) . . . . ? O11 Co3 N11 C49 158.2(8) 2_565 . . . ? O12 Co3 N11 C49 -177.0(10) 2_565 . . . ? C38 C43 N12 C50 -0.5(13) . . . . ? C42 C43 N12 C50 179.2(12) . . . . ? C38 C43 N12 O11 152.4(9) . . . 2_565 ? C42 C43 N12 O11 -28(2) . . . 2_565 ? N9 C50 N12 C43 -0.3(12) . . . . ? C51 C50 N12 C43 -174.8(11) . . . . ? N9 C50 N12 O11 -159.3(7) . . . 2_565 ? C51 C50 N12 O11 26.1(14) . . . 2_565 ? N16 C64 N13 C52 -0.9(13) . . . . ? C65 C64 N13 C52 175.1(11) . . . . ? N16 C64 N13 Co3 179.5(7) . . . . ? C65 C64 N13 Co3 -4.6(19) . . . . ? C57 C52 N13 C64 0.3(12) . . . . ? C53 C52 N13 C64 -177.2(12) . . . . ? C57 C52 N13 Co3 -180.0(7) . . . . ? C53 C52 N13 Co3 2.5(17) . . . . ? O3 Co3 N13 C64 -20.2(11) 4_464 . . . ? N11 Co3 N13 C64 -127.3(11) . . . . ? O11 Co3 N13 C64 123.7(11) 2_565 . . . ? O12 Co3 N13 C64 66.1(11) 2_565 . . . ? O3 Co3 N13 C52 160.1(8) 4_464 . . . ? N11 Co3 N13 C52 53.1(8) . . . . ? O11 Co3 N13 C52 -55.9(8) 2_565 . . . ? O12 Co3 N13 C52 -113.5(8) 2_565 . . . ? N15 C65 N14 C58 2.2(14) . . . . ? C64 C65 N14 C58 -173.4(10) . . . . ? N15 C65 N14 O3 -154.8(7) . . . 4_464 ? C64 C65 N14 O3 29.6(14) . . . 4_464 ? C59 C58 N14 C65 179.9(14) . . . . ? C63 C58 N14 C65 -2.7(13) . . . . ? C59 C58 N14 O3 -31(2) . . . 4_464 ? C63 C58 N14 O3 146.5(9) . . . 4_464 ? N14 C65 N15 C63 -0.6(12) . . . . ? C64 C65 N15 C63 175.3(9) . . . . ? N14 C65 N15 Co4 -171.4(7) . . . . ? C64 C65 N15 Co4 4.6(12) . . . . ? C58 C63 N15 C65 -1.1(11) . . . . ? C62 C63 N15 C65 -177.7(12) . . . . ? C58 C63 N15 Co4 165.1(9) . . . . ? C62 C63 N15 Co4 -11.4(19) . . . . ? N16 Co4 N15 C65 -2.0(7) . . . . ? N17 Co4 N15 C65 -176.4(8) . . . . ? N18 Co4 N15 C65 -96.6(8) . . . . ? O7 Co4 N15 C65 67.7(12) . . . . ? O8 Co4 N15 C65 93.2(8) . . . . ? C80 Co4 N15 C65 84.9(8) . . . . ? N16 Co4 N15 C63 -167.6(11) . . . . ? N17 Co4 N15 C63 18.0(11) . . . . ? N18 Co4 N15 C63 97.8(11) . . . . ? O7 Co4 N15 C63 -97.9(12) . . . . ? O8 Co4 N15 C63 -72.4(11) . . . . ? C80 Co4 N15 C63 -80.7(12) . . . . ? N13 C64 N16 C57 1.1(13) . . . . ? C65 C64 N16 C57 -175.5(9) . . . . ? N13 C64 N16 Co4 -179.9(7) . . . . ? C65 C64 N16 Co4 3.6(12) . . . . ? C52 C57 N16 C64 -0.8(12) . . . . ? C56 C57 N16 C64 176.9(12) . . . . ? C52 C57 N16 Co4 -179.4(9) . . . . ? C56 C57 N16 Co4 -2(2) . . . . ? N17 Co4 N16 C64 49(4) . . . . ? N15 Co4 N16 C64 -1.0(8) . . . . ? N18 Co4 N16 C64 101.9(8) . . . . ? O7 Co4 N16 C64 -156.9(8) . . . . ? O8 Co4 N16 C64 -96.7(8) . . . . ? C80 Co4 N16 C64 -127.1(8) . . . . ? N17 Co4 N16 C57 -132(3) . . . . ? N15 Co4 N16 C57 177.5(13) . . . . ? N18 Co4 N16 C57 -79.6(13) . . . . ? O7 Co4 N16 C57 21.6(13) . . . . ? O8 Co4 N16 C57 81.7(12) . . . . ? C80 Co4 N16 C57 51.4(13) . . . . ? N20 C78 N17 C66 -1.1(15) . . . . ? C79 C78 N17 C66 177.5(10) . . . . ? N20 C78 N17 Co4 -174.3(9) . . . . ? C79 C78 N17 Co4 4.3(14) . . . . ? C67 C66 N17 C78 -178.1(15) . . . . ? C71 C66 N17 C78 1.2(14) . . . . ? C67 C66 N17 Co4 -8(2) . . . . ? C71 C66 N17 Co4 171.1(10) . . . . ? N16 Co4 N17 C78 52(4) . . . . ? N15 Co4 N17 C78 101.3(9) . . . . ? N18 Co4 N17 C78 -1.7(8) . . . . ? O7 Co4 N17 C78 -101.8(9) . . . . ? O8 Co4 N17 C78 -161.9(9) . . . . ? C80 Co4 N17 C78 -131.7(9) . . . . ? N16 Co4 N17 C66 -118(3) . . . . ? N15 Co4 N17 C66 -68.2(13) . . . . ? N18 Co4 N17 C66 -171.2(14) . . . . ? O7 Co4 N17 C66 88.7(13) . . . . ? O8 Co4 N17 C66 28.7(13) . . . . ? C80 Co4 N17 C66 58.8(13) . . . . ? N19 C79 N18 C72 0.1(14) . . . . ? C78 C79 N18 C72 -179.4(10) . . . . ? N19 C79 N18 Co4 -176.6(7) . . . . ? C78 C79 N18 Co4 3.9(13) . . . . ? C77 C72 N18 C79 0.2(14) . . . . ? C73 C72 N18 C79 178.9(14) . . . . ? C77 C72 N18 Co4 175.2(10) . . . . ? C73 C72 N18 Co4 -6(2) . . . . ? N16 Co4 N18 C79 -175.4(8) . . . . ? N17 Co4 N18 C79 -1.2(8) . . . . ? N15 Co4 N18 C79 -95.2(8) . . . . ? O7 Co4 N18 C79 91.7(8) . . . . ? O8 Co4 N18 C79 59.1(13) . . . . ? C80 Co4 N18 C79 83.1(9) . . . . ? N16 Co4 N18 C72 9.8(13) . . . . ? N17 Co4 N18 C72 -176.1(13) . . . . ? N15 Co4 N18 C72 89.9(13) . . . . ? O7 Co4 N18 C72 -83.2(13) . . . . ? O8 Co4 N18 C72 -115.7(14) . . . . ? C80 Co4 N18 C72 -91.7(14) . . . . ? N18 C79 N19 C77 -0.3(14) . . . . ? C78 C79 N19 C77 179.1(12) . . . . ? N18 C79 N19 O3W -168.3(9) . . . 1 ? C78 C79 N19 O3W 11.1(14) . . . 1 ? C72 C77 N19 C79 0.4(14) . . . . ? C76 C77 N19 C79 -178.5(14) . . . . ? C72 C77 N19 O3W 160.8(11) . . . 1 ? C76 C77 N19 O3W -18(3) . . . 1 ? N17 C78 N20 C71 0.7(16) . . . . ? C79 C78 N20 C71 -177.7(12) . . . . ? N17 C78 N20 O3W 175.9(9) . . . 1 ? C79 C78 N20 O3W -2.5(17) . . . 1 ? C70 C71 N20 C78 176.8(17) . . . . ? C66 C71 N20 C78 0.1(16) . . . . ? C70 C71 N20 O3W 5(3) . . . 1 ? C66 C71 N20 O3W -171.7(13) . . . 1 ? O2 C15 O1 Co1 1.1(12) . . . . ? C16 C15 O1 Co1 176.6(10) . . . . ? O1W Co1 O1 C15 16.8(11) . . . . ? N2 Co1 O1 C15 -177.9(7) . . . . ? O2W Co1 O1 C15 -88.7(7) . . . . ? O2 Co1 O1 C15 -0.7(7) . . . . ? N1 Co1 O1 C15 105.3(7) . . . . ? O1 C15 O2 Co1 -1.1(12) . . . . ? C16 C15 O2 Co1 -176.7(10) . . . . ? O1W Co1 O2 C15 -170.3(8) . . . . ? N2 Co1 O2 C15 15(2) . . . . ? O2W Co1 O2 C15 90.7(8) . . . . ? N1 Co1 O2 C15 -76.8(8) . . . . ? O1 Co1 O2 C15 0.6(7) . . . . ? O4 C19 O3 Co3 10.1(14) . . . 4_565 ? C18 C19 O3 Co3 -167.5(8) . . . 4_565 ? O6 C22 O5 Co2 -6.8(11) . . . . ? C21 C22 O5 Co2 170.7(9) . . . . ? N10 Co2 O5 C22 176.1(7) . . . . ? N9 Co2 O5 C22 95.7(7) . . . . ? N6 Co2 O5 C22 -20.3(10) . . . . ? N5 Co2 O5 C22 -86.4(7) . . . . ? O6 Co2 O5 C22 3.9(6) . . . . ? O5 C22 O6 Co2 6.5(11) . . . . ? C21 C22 O6 Co2 -171.1(10) . . . . ? N10 Co2 O6 C22 -38.2(17) . . . . ? N9 Co2 O6 C22 -97.6(7) . . . . ? O5 Co2 O6 C22 -3.8(6) . . . . ? N6 Co2 O6 C22 163.3(7) . . . . ? N5 Co2 O6 C22 85.6(7) . . . . ? O8 C80 O7 Co4 1.4(12) . . . . ? C81 C80 O7 Co4 -176.1(10) . . . . ? N16 Co4 O7 C80 95.6(7) . . . . ? N17 Co4 O7 C80 -87.6(7) . . . . ? N15 Co4 O7 C80 28.7(12) . . . . ? N18 Co4 O7 C80 -166.8(7) . . . . ? O8 Co4 O7 C80 -0.8(7) . . . . ? O7 C80 O8 Co4 -1.4(11) . . . . ? C81 C80 O8 Co4 176.1(10) . . . . ? N16 Co4 O8 C80 -87.3(7) . . . . ? N17 Co4 O8 C80 96.7(7) . . . . ? N15 Co4 O8 C80 -166.8(7) . . . . ? N18 Co4 O8 C80 38.2(12) . . . . ? O7 Co4 O8 C80 0.8(6) . . . . ? O12 C84 O11 Co3 10.6(13) . . . 2_564 ? C83 C84 O11 Co3 -166.9(9) . . . 2_564 ? O11 C84 O12 Co3 -9.3(12) . . . 2_564 ? C83 C84 O12 Co3 168.1(11) . . . 2_564 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B O6W 0.86 2.10 2.869(14) 148.1 2_565 N4 H4B O6W 0.86 1.98 2.785(13) 154.6 2_565 N7 H7A O9 0.86 1.93 2.755(12) 159.4 2_665 N8 H8B O10 0.86 1.81 2.666(12) 172.8 2_665 N12 H12A O11 0.86 2.01 2.785(13) 148.9 2_565 N14 H14A O3 0.86 2.03 2.778(12) 145.3 4_464 N19 H19A O3W 0.86 2.06 2.84(2) 149.4 1 N20 H20B O3W 0.86 2.08 2.861(19) 151.5 1 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.662 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.087 #===============================END data_5 _database_code_depnum_ccdc_archive 'CCDC 286940' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H42 Co2 N16 O8' _chemical_formula_weight 1305.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 11.3758(18) _cell_length_b 11.982(2) _cell_length_c 12.6203(19) _cell_angle_alpha 104.568(6) _cell_angle_beta 97.853(2) _cell_angle_gamma 108.063(6) _cell_volume 1539.2(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3103 _cell_measurement_theta_min 3.0494 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3800 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.609 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8035 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 CCD _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12042 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6982 _reflns_number_gt 5151 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _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^)+(0.0527P)^2^+0.6248P] 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 6982 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 0.76239(4) 0.75475(3) 0.71302(3) 0.02986(13) Uani 1 1 d . . . C1 C 0.4723(3) 0.7417(3) 0.7397(2) 0.0326(6) Uani 1 1 d . . . C2 C 0.4780(4) 0.8609(3) 0.7923(3) 0.0499(8) Uani 1 1 d . . . H2A H 0.5536 0.9285 0.8123 0.060 Uiso 1 1 calc R . . C3 C 0.3661(4) 0.8745(4) 0.8136(3) 0.0626(10) Uani 1 1 d . . . H3A H 0.3668 0.9529 0.8487 0.075 Uiso 1 1 calc R . . C4 C 0.2517(4) 0.7730(4) 0.7836(3) 0.0564(10) Uani 1 1 d . . . H4A H 0.1785 0.7859 0.7989 0.068 Uiso 1 1 calc R . . C5 C 0.2453(3) 0.6558(3) 0.7325(3) 0.0443(8) Uani 1 1 d . . . H5A H 0.1696 0.5885 0.7130 0.053 Uiso 1 1 calc R . . C6 C 0.3570(3) 0.6417(3) 0.7109(2) 0.0321(6) Uani 1 1 d . . . C7 C 0.7462(3) 0.4646(3) 0.5902(2) 0.0324(6) Uani 1 1 d . . . C8 C 0.8691(3) 0.4677(3) 0.5836(3) 0.0415(8) Uani 1 1 d . . . H8A H 0.9381 0.5420 0.6077 0.050 Uiso 1 1 calc R . . C9 C 0.8837(4) 0.3569(4) 0.5400(3) 0.0514(9) Uani 1 1 d . . . H9A H 0.9645 0.3565 0.5352 0.062 Uiso 1 1 calc R . . C10 C 0.7809(4) 0.2447(3) 0.5028(3) 0.0522(9) Uani 1 1 d . . . H10A H 0.7949 0.1718 0.4732 0.063 Uiso 1 1 calc R . . C11 C 0.6592(3) 0.2393(3) 0.5087(3) 0.0445(8) Uani 1 1 d . . . H11A H 0.5907 0.1647 0.4843 0.053 Uiso 1 1 calc R . . C12 C 0.6440(3) 0.3509(3) 0.5530(2) 0.0328(6) Uani 1 1 d . . . C13 C 0.5068(3) 0.5779(3) 0.6602(2) 0.0282(6) Uani 1 1 d . . . C14 C 0.5783(3) 0.5031(2) 0.6182(2) 0.0276(6) Uani 1 1 d . . . C15 C 0.7460(3) 0.6260(3) 0.9225(2) 0.0426(8) Uani 1 1 d . . . C16 C 0.7076(4) 0.4988(3) 0.8751(3) 0.0587(10) Uani 1 1 d . . . H16A H 0.7050 0.4636 0.7998 0.070 Uiso 1 1 calc R . . C17 C 0.6736(5) 0.4267(4) 0.9426(3) 0.0801(15) Uani 1 1 d . . . H17A H 0.6455 0.3412 0.9120 0.096 Uiso 1 1 calc R . . C18 C 0.6803(6) 0.4787(4) 1.0565(4) 0.0915(17) Uani 1 1 d . . . H18A H 0.6568 0.4268 1.0999 0.110 Uiso 1 1 calc R . . C19 C 0.7208(5) 0.6048(4) 1.1067(3) 0.0774(14) Uani 1 1 d . . . H19A H 0.7260 0.6395 1.1827 0.093 Uiso 1 1 calc R . . C20 C 0.7535(4) 0.6772(3) 1.0368(3) 0.0482(9) Uani 1 1 d . . . C21 C 0.8498(3) 1.0649(3) 0.8377(2) 0.0334(6) Uani 1 1 d . . . C22 C 0.8507(4) 1.1208(3) 0.7537(3) 0.0520(9) Uani 1 1 d . . . H22A H 0.8252 1.0745 0.6779 0.062 Uiso 1 1 calc R . . C23 C 0.8911(5) 1.2476(4) 0.7877(3) 0.0706(13) Uani 1 1 d . . . H23A H 0.8937 1.2877 0.7334 0.085 Uiso 1 1 calc R . . C24 C 0.9279(5) 1.3174(3) 0.9005(3) 0.0680(12) Uani 1 1 d . . . H24A H 0.9542 1.4030 0.9195 0.082 Uiso 1 1 calc R . . C25 C 0.9266(4) 1.2639(3) 0.9853(3) 0.0522(9) Uani 1 1 d . . . H25A H 0.9515 1.3108 1.0609 0.063 Uiso 1 1 calc R . . C26 C 0.8862(3) 1.1366(3) 0.9514(2) 0.0362(7) Uani 1 1 d . . . C27 C 0.8339(3) 0.9401(3) 0.9362(2) 0.0310(6) Uani 1 1 d . . . C28 C 0.8065(3) 0.8235(3) 0.9585(2) 0.0342(7) Uani 1 1 d . . . C29 C 1.0172(3) 0.9025(3) 0.6901(2) 0.0279(6) Uani 1 1 d . . . C30 C 0.7887(3) 0.7804(3) 0.4841(2) 0.0381(7) Uani 1 1 d . . . C31 C 1.0053(3) 0.9512(2) 0.5906(2) 0.0272(6) Uani 1 1 d . . . C32 C 0.9017(3) 0.8943(2) 0.4980(2) 0.0276(6) Uani 1 1 d . . . C33 C 0.8981(3) 0.9439(3) 0.4089(2) 0.0292(6) Uani 1 1 d . . . H33A H 0.8287 0.9053 0.3474 0.035 Uiso 1 1 calc R . . N1 N 0.5650(2) 0.6989(2) 0.70598(19) 0.0297(5) Uani 1 1 d . . . N2 N 0.7025(2) 0.5590(2) 0.62994(18) 0.0283(5) Uani 1 1 d . . . N3 N 0.5382(2) 0.3791(2) 0.57250(19) 0.0325(5) Uani 1 1 d . . . H3B H 0.4616 0.3276 0.5583 0.039 Uiso 1 1 calc R . . N4 N 0.3824(2) 0.5386(2) 0.66097(19) 0.0314(5) Uani 1 1 d . . . H4B H 0.3294 0.4637 0.6352 0.038 Uiso 1 1 calc R . . N5 N 0.7807(2) 0.7215(2) 0.87545(18) 0.0348(6) Uani 1 1 d . . . N6 N 0.8173(2) 0.9406(2) 0.83004(18) 0.0317(5) Uani 1 1 d . . . N7 N 0.8741(2) 1.0534(2) 1.01169(19) 0.0351(6) Uani 1 1 d . . . H7A H 0.8895 1.0709 1.0838 0.042 Uiso 1 1 calc R . . N8 N 0.7930(3) 0.8031(2) 1.0576(2) 0.0450(7) Uani 1 1 d . . . H8B H 0.8065 0.8581 1.1212 0.054 Uiso 1 1 calc R . . O1 O 0.94205(18) 0.79625(18) 0.68138(16) 0.0326(5) Uani 1 1 d . . . O2 O 1.10428(19) 0.97040(19) 0.77589(15) 0.0369(5) Uani 1 1 d . . . O3 O 0.71557(18) 0.7838(2) 0.55011(17) 0.0407(5) Uani 1 1 d . . . O4 O 0.7730(3) 0.6900(2) 0.4015(2) 0.0759(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0313(2) 0.0258(2) 0.0242(2) 0.00827(15) 0.00531(15) -0.00086(16) C1 0.0394(16) 0.0298(15) 0.0270(14) 0.0082(12) 0.0089(12) 0.0106(13) C2 0.059(2) 0.0359(19) 0.049(2) 0.0064(16) 0.0139(17) 0.0136(17) C3 0.078(3) 0.050(2) 0.066(3) 0.010(2) 0.025(2) 0.035(2) C4 0.057(2) 0.072(3) 0.056(2) 0.023(2) 0.0266(19) 0.037(2) C5 0.0418(18) 0.055(2) 0.0429(18) 0.0208(17) 0.0159(15) 0.0195(16) C6 0.0351(15) 0.0347(16) 0.0296(14) 0.0137(13) 0.0108(12) 0.0125(13) C7 0.0369(15) 0.0363(17) 0.0229(13) 0.0124(12) 0.0082(11) 0.0087(13) C8 0.0342(16) 0.052(2) 0.0415(17) 0.0217(16) 0.0122(14) 0.0131(15) C9 0.055(2) 0.070(3) 0.053(2) 0.031(2) 0.0282(18) 0.039(2) C10 0.072(3) 0.052(2) 0.049(2) 0.0206(18) 0.0259(19) 0.037(2) C11 0.059(2) 0.0339(18) 0.0417(18) 0.0105(14) 0.0141(16) 0.0177(16) C12 0.0370(15) 0.0335(16) 0.0267(14) 0.0101(12) 0.0086(12) 0.0101(13) C13 0.0297(14) 0.0272(15) 0.0231(13) 0.0086(11) 0.0068(11) 0.0030(12) C14 0.0308(14) 0.0240(14) 0.0222(12) 0.0081(11) 0.0062(11) 0.0012(11) C15 0.059(2) 0.0360(18) 0.0293(15) 0.0146(14) 0.0044(14) 0.0113(16) C16 0.099(3) 0.040(2) 0.0320(17) 0.0139(16) 0.0099(18) 0.018(2) C17 0.142(4) 0.039(2) 0.051(2) 0.0233(19) 0.016(3) 0.017(3) C18 0.167(5) 0.055(3) 0.053(3) 0.036(2) 0.031(3) 0.023(3) C19 0.138(4) 0.056(3) 0.0339(19) 0.0246(19) 0.022(2) 0.021(3) C20 0.070(2) 0.040(2) 0.0301(16) 0.0145(15) 0.0084(15) 0.0125(17) C21 0.0392(16) 0.0277(15) 0.0268(14) 0.0066(12) 0.0045(12) 0.0062(13) C22 0.080(3) 0.047(2) 0.0306(17) 0.0172(16) 0.0105(17) 0.0206(19) C23 0.121(4) 0.039(2) 0.047(2) 0.0222(18) 0.015(2) 0.018(2) C24 0.110(4) 0.031(2) 0.055(2) 0.0136(17) 0.016(2) 0.015(2) C25 0.076(3) 0.0317(18) 0.0371(18) 0.0049(15) 0.0092(17) 0.0103(17) C26 0.0407(16) 0.0309(16) 0.0327(15) 0.0091(13) 0.0078(13) 0.0078(13) C27 0.0336(15) 0.0324(16) 0.0224(13) 0.0052(12) 0.0062(11) 0.0086(13) C28 0.0379(16) 0.0327(16) 0.0249(14) 0.0095(12) 0.0027(12) 0.0048(13) C29 0.0311(14) 0.0291(15) 0.0213(13) 0.0090(11) 0.0078(11) 0.0061(12) C30 0.0406(16) 0.0312(16) 0.0264(14) 0.0127(13) 0.0020(12) -0.0094(13) C31 0.0318(14) 0.0221(14) 0.0232(13) 0.0085(11) 0.0081(11) 0.0016(11) C32 0.0289(14) 0.0234(14) 0.0236(13) 0.0083(11) 0.0062(10) -0.0007(11) C33 0.0260(13) 0.0288(15) 0.0222(13) 0.0075(11) 0.0010(10) -0.0023(11) N1 0.0306(12) 0.0250(12) 0.0288(12) 0.0065(10) 0.0077(10) 0.0048(10) N2 0.0255(11) 0.0283(13) 0.0253(11) 0.0080(10) 0.0060(9) 0.0020(10) N3 0.0316(13) 0.0250(13) 0.0354(13) 0.0098(10) 0.0090(10) 0.0019(10) N4 0.0289(12) 0.0263(13) 0.0331(13) 0.0103(10) 0.0094(10) 0.0004(10) N5 0.0479(15) 0.0276(13) 0.0235(12) 0.0094(10) 0.0062(11) 0.0060(11) N6 0.0355(13) 0.0275(13) 0.0245(11) 0.0064(10) 0.0028(10) 0.0040(10) N7 0.0455(14) 0.0317(14) 0.0217(11) 0.0055(10) 0.0052(10) 0.0085(12) N8 0.0684(19) 0.0378(16) 0.0207(12) 0.0081(11) 0.0096(12) 0.0093(14) O1 0.0313(10) 0.0298(11) 0.0350(11) 0.0170(9) 0.0094(8) 0.0025(9) O2 0.0421(12) 0.0341(12) 0.0235(10) 0.0097(9) 0.0009(9) 0.0009(9) O3 0.0307(11) 0.0488(14) 0.0390(12) 0.0253(11) 0.0081(9) 0.0001(10) O4 0.097(2) 0.0396(15) 0.0432(14) -0.0056(12) 0.0268(14) -0.0298(14) _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 2.0680(19) . ? Co1 N1 2.117(2) . ? Co1 N2 2.154(2) . ? Co1 N5 2.179(2) . ? Co1 N6 2.182(2) . ? Co1 O3 2.1927(19) . ? C1 N1 1.379(4) . ? C1 C2 1.393(4) . ? C1 C6 1.401(4) . ? C2 C3 1.385(5) . ? C2 H2A 0.9300 . ? C3 C4 1.403(5) . ? C3 H3A 0.9300 . ? C4 C5 1.364(5) . ? C4 H4A 0.9300 . ? C5 C6 1.386(4) . ? C5 H5A 0.9300 . ? C6 N4 1.374(4) . ? C7 N2 1.383(4) . ? C7 C8 1.401(4) . ? C7 C12 1.406(4) . ? C8 C9 1.375(5) . ? C8 H8A 0.9300 . ? C9 C10 1.397(5) . ? C9 H9A 0.9300 . ? C10 C11 1.380(5) . ? C10 H10A 0.9300 . ? C11 C12 1.387(4) . ? C11 H11A 0.9300 . ? C12 N3 1.384(4) . ? C13 N1 1.324(3) . ? C13 N4 1.348(3) . ? C13 C14 1.441(4) . ? C14 N2 1.331(3) . ? C14 N3 1.351(4) . ? C15 C16 1.389(5) . ? C15 N5 1.394(4) . ? C15 C20 1.398(4) . ? C16 C17 1.370(5) . ? C16 H16A 0.9300 . ? C17 C18 1.397(6) . ? C17 H17A 0.9300 . ? C18 C19 1.380(6) . ? C18 H18A 0.9300 . ? C19 C20 1.395(4) . ? C19 H19A 0.9300 . ? C20 N8 1.376(4) . ? C21 C22 1.389(4) . ? C21 N6 1.393(4) . ? C21 C26 1.401(4) . ? C22 C23 1.374(5) . ? C22 H22A 0.9300 . ? C23 C24 1.387(5) . ? C23 H23A 0.9300 . ? C24 C25 1.379(5) . ? C24 H24A 0.9300 . ? C25 C26 1.380(4) . ? C25 H25A 0.9300 . ? C26 N7 1.385(4) . ? C27 N6 1.329(3) . ? C27 N7 1.344(4) . ? C27 C28 1.441(4) . ? C28 N5 1.314(4) . ? C28 N8 1.353(3) . ? C29 O2 1.257(3) . ? C29 O1 1.262(3) . ? C29 C31 1.518(3) . ? C30 O4 1.246(4) . ? C30 O3 1.257(4) . ? C30 C32 1.509(4) . ? C31 C33 1.388(4) 2_776 ? C31 C32 1.395(4) . ? C32 C33 1.399(3) . ? C33 C31 1.388(4) 2_776 ? C33 H33A 0.9300 . ? N3 O3 2.881(3) 2_666 ? N3 H3B 0.8600 . ? N4 O4 2.604(3) 2_666 ? N4 H4B 0.8600 . ? N7 O2 2.753(3) 2_777 ? N7 H7A 0.8600 . ? N8 O2 2.764(3) 2_777 ? N8 H8B 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 N1 167.26(8) . . ? O1 Co1 N2 95.13(8) . . ? N1 Co1 N2 79.13(9) . . ? O1 Co1 N5 105.80(9) . . ? N1 Co1 N5 85.66(9) . . ? N2 Co1 N5 89.57(9) . . ? O1 Co1 N6 90.66(8) . . ? N1 Co1 N6 97.28(9) . . ? N2 Co1 N6 167.35(8) . . ? N5 Co1 N6 78.02(9) . . ? O1 Co1 O3 82.34(7) . . ? N1 Co1 O3 86.27(8) . . ? N2 Co1 O3 90.01(8) . . ? N5 Co1 O3 171.85(9) . . ? N6 Co1 O3 101.92(9) . . ? N1 C1 C2 130.9(3) . . ? N1 C1 C6 109.0(2) . . ? C2 C1 C6 120.1(3) . . ? C3 C2 C1 117.1(3) . . ? C3 C2 H2A 121.5 . . ? C1 C2 H2A 121.5 . . ? C2 C3 C4 121.7(4) . . ? C2 C3 H3A 119.1 . . ? C4 C3 H3A 119.1 . . ? C5 C4 C3 121.6(3) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C4 C5 C6 116.9(3) . . ? C4 C5 H5A 121.6 . . ? C6 C5 H5A 121.6 . . ? N4 C6 C5 131.3(3) . . ? N4 C6 C1 106.1(2) . . ? C5 C6 C1 122.6(3) . . ? N2 C7 C8 130.6(3) . . ? N2 C7 C12 109.4(2) . . ? C8 C7 C12 119.9(3) . . ? C9 C8 C7 117.4(3) . . ? C9 C8 H8A 121.3 . . ? C7 C8 H8A 121.3 . . ? C8 C9 C10 122.0(3) . . ? C8 C9 H9A 119.0 . . ? C10 C9 H9A 119.0 . . ? C11 C10 C9 121.6(3) . . ? C11 C10 H10A 119.2 . . ? C9 C10 H10A 119.2 . . ? C10 C11 C12 116.6(3) . . ? C10 C11 H11A 121.7 . . ? C12 C11 H11A 121.7 . . ? N3 C12 C11 131.9(3) . . ? N3 C12 C7 105.6(3) . . ? C11 C12 C7 122.5(3) . . ? N1 C13 N4 113.3(3) . . ? N1 C13 C14 119.6(2) . . ? N4 C13 C14 127.1(3) . . ? N2 C14 N3 113.2(3) . . ? N2 C14 C13 118.0(2) . . ? N3 C14 C13 128.7(2) . . ? C16 C15 N5 131.4(3) . . ? C16 C15 C20 120.1(3) . . ? N5 C15 C20 108.5(3) . . ? C17 C16 C15 118.0(3) . . ? C17 C16 H16A 121.0 . . ? C15 C16 H16A 121.0 . . ? C16 C17 C18 121.4(4) . . ? C16 C17 H17A 119.3 . . ? C18 C17 H17A 119.3 . . ? C19 C18 C17 122.0(3) . . ? C19 C18 H18A 119.0 . . ? C17 C18 H18A 119.0 . . ? C18 C19 C20 116.1(3) . . ? C18 C19 H19A 122.0 . . ? C20 C19 H19A 122.0 . . ? N8 C20 C19 131.4(3) . . ? N8 C20 C15 106.2(3) . . ? C19 C20 C15 122.4(3) . . ? C22 C21 N6 130.3(3) . . ? C22 C21 C26 120.4(3) . . ? N6 C21 C26 109.3(2) . . ? C23 C22 C21 117.0(3) . . ? C23 C22 H22A 121.5 . . ? C21 C22 H22A 121.5 . . ? C22 C23 C24 122.0(3) . . ? C22 C23 H23A 119.0 . . ? C24 C23 H23A 119.0 . . ? C25 C24 C23 122.0(3) . . ? C25 C24 H24A 119.0 . . ? C23 C24 H24A 119.0 . . ? C26 C25 C24 116.1(3) . . ? C26 C25 H25A 122.0 . . ? C24 C25 H25A 122.0 . . ? C25 C26 N7 131.9(3) . . ? C25 C26 C21 122.5(3) . . ? N7 C26 C21 105.6(3) . . ? N6 C27 N7 113.5(2) . . ? N6 C27 C28 119.0(3) . . ? N7 C27 C28 127.6(2) . . ? N5 C28 N8 113.2(3) . . ? N5 C28 C27 119.9(2) . . ? N8 C28 C27 126.7(3) . . ? O2 C29 O1 123.9(2) . . ? O2 C29 C31 117.3(2) . . ? O1 C29 C31 118.8(2) . . ? O4 C30 O3 125.1(3) . . ? O4 C30 C32 114.9(3) . . ? O3 C30 C32 119.9(3) . . ? C33 C31 C32 118.4(2) 2_776 . ? C33 C31 C29 118.9(2) 2_776 . ? C32 C31 C29 122.8(2) . . ? C31 C32 C33 119.5(2) . . ? C31 C32 C30 125.3(2) . . ? C33 C32 C30 115.2(2) . . ? C31 C33 C32 122.1(2) 2_776 . ? C31 C33 H33A 118.9 2_776 . ? C32 C33 H33A 118.9 . . ? C13 N1 C1 105.1(2) . . ? C13 N1 Co1 111.90(19) . . ? C1 N1 Co1 142.78(19) . . ? C14 N2 C7 105.0(2) . . ? C14 N2 Co1 111.28(19) . . ? C7 N2 Co1 143.47(19) . . ? C14 N3 C12 106.8(2) . . ? C14 N3 O3 126.56(19) . 2_666 ? C12 N3 O3 121.82(19) . 2_666 ? C14 N3 H3B 126.6 . . ? C12 N3 H3B 126.6 . . ? O3 N3 H3B 19.7 2_666 . ? C13 N4 C6 106.5(2) . . ? C13 N4 O4 126.5(2) . 2_666 ? C6 N4 O4 126.71(19) . 2_666 ? C13 N4 H4B 126.7 . . ? C6 N4 H4B 126.7 . . ? O4 N4 H4B 4.5 2_666 . ? C28 N5 C15 105.4(2) . . ? C28 N5 Co1 111.35(18) . . ? C15 N5 Co1 140.9(2) . . ? C27 N6 C21 104.6(2) . . ? C27 N6 Co1 111.30(19) . . ? C21 N6 Co1 143.92(18) . . ? C27 N7 C26 107.0(2) . . ? C27 N7 O2 108.42(17) . 2_777 ? C26 N7 O2 144.59(19) . 2_777 ? C27 N7 H7A 126.5 . . ? C26 N7 H7A 126.5 . . ? O2 N7 H7A 18.1 2_777 . ? C28 N8 C20 106.6(3) . . ? C28 N8 O2 107.50(19) . 2_777 ? C20 N8 O2 144.51(19) . 2_777 ? C28 N8 H8B 126.7 . . ? C20 N8 H8B 126.7 . . ? O2 N8 H8B 21.1 2_777 . ? C29 O1 Co1 125.82(19) . . ? C30 O3 Co1 120.09(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 178.7(3) . . . . ? C6 C1 C2 C3 -0.2(5) . . . . ? C1 C2 C3 C4 -0.1(6) . . . . ? C2 C3 C4 C5 0.4(6) . . . . ? C3 C4 C5 C6 -0.4(5) . . . . ? C4 C5 C6 N4 -179.5(3) . . . . ? C4 C5 C6 C1 0.1(4) . . . . ? N1 C1 C6 N4 0.7(3) . . . . ? C2 C1 C6 N4 179.9(3) . . . . ? N1 C1 C6 C5 -179.0(3) . . . . ? C2 C1 C6 C5 0.2(4) . . . . ? N2 C7 C8 C9 179.5(3) . . . . ? C12 C7 C8 C9 0.0(4) . . . . ? C7 C8 C9 C10 0.4(5) . . . . ? C8 C9 C10 C11 -0.6(5) . . . . ? C9 C10 C11 C12 0.3(5) . . . . ? C10 C11 C12 N3 -178.9(3) . . . . ? C10 C11 C12 C7 0.1(4) . . . . ? N2 C7 C12 N3 -0.6(3) . . . . ? C8 C7 C12 N3 179.0(2) . . . . ? N2 C7 C12 C11 -179.9(3) . . . . ? C8 C7 C12 C11 -0.3(4) . . . . ? N1 C13 C14 N2 1.7(4) . . . . ? N4 C13 C14 N2 -176.8(2) . . . . ? N1 C13 C14 N3 177.6(2) . . . . ? N4 C13 C14 N3 -1.0(4) . . . . ? N5 C15 C16 C17 -177.1(4) . . . . ? C20 C15 C16 C17 2.2(6) . . . . ? C15 C16 C17 C18 -1.7(8) . . . . ? C16 C17 C18 C19 0.2(9) . . . . ? C17 C18 C19 C20 0.6(8) . . . . ? C18 C19 C20 N8 177.7(5) . . . . ? C18 C19 C20 C15 0.0(7) . . . . ? C16 C15 C20 N8 -179.7(3) . . . . ? N5 C15 C20 N8 -0.2(4) . . . . ? C16 C15 C20 C19 -1.5(6) . . . . ? N5 C15 C20 C19 178.1(4) . . . . ? N6 C21 C22 C23 -178.4(4) . . . . ? C26 C21 C22 C23 1.3(5) . . . . ? C21 C22 C23 C24 -0.8(7) . . . . ? C22 C23 C24 C25 0.2(8) . . . . ? C23 C24 C25 C26 -0.2(7) . . . . ? C24 C25 C26 N7 179.2(4) . . . . ? C24 C25 C26 C21 0.7(5) . . . . ? C22 C21 C26 C25 -1.4(5) . . . . ? N6 C21 C26 C25 178.4(3) . . . . ? C22 C21 C26 N7 179.8(3) . . . . ? N6 C21 C26 N7 -0.4(3) . . . . ? N6 C27 C28 N5 8.2(4) . . . . ? N7 C27 C28 N5 -172.8(3) . . . . ? N6 C27 C28 N8 -165.7(3) . . . . ? N7 C27 C28 N8 13.4(5) . . . . ? O2 C29 C31 C33 10.8(4) . . . 2_776 ? O1 C29 C31 C33 -167.5(3) . . . 2_776 ? O2 C29 C31 C32 -169.7(3) . . . . ? O1 C29 C31 C32 11.9(4) . . . . ? C33 C31 C32 C33 0.1(5) 2_776 . . . ? C29 C31 C32 C33 -179.3(3) . . . . ? C33 C31 C32 C30 -179.7(3) 2_776 . . . ? C29 C31 C32 C30 0.8(5) . . . . ? O4 C30 C32 C31 -118.7(3) . . . . ? O3 C30 C32 C31 64.8(4) . . . . ? O4 C30 C32 C33 61.4(4) . . . . ? O3 C30 C32 C33 -115.1(3) . . . . ? C31 C32 C33 C31 -0.1(5) . . . 2_776 ? C30 C32 C33 C31 179.7(3) . . . 2_776 ? N4 C13 N1 C1 0.3(3) . . . . ? C14 C13 N1 C1 -178.4(2) . . . . ? N4 C13 N1 Co1 176.07(17) . . . . ? C14 C13 N1 Co1 -2.7(3) . . . . ? C2 C1 N1 C13 -179.7(3) . . . . ? C6 C1 N1 C13 -0.6(3) . . . . ? C2 C1 N1 Co1 6.9(5) . . . . ? C6 C1 N1 Co1 -174.1(2) . . . . ? O1 Co1 N1 C13 66.2(4) . . . . ? N2 Co1 N1 C13 2.04(17) . . . . ? N5 Co1 N1 C13 -88.36(18) . . . . ? N6 Co1 N1 C13 -165.67(18) . . . . ? O3 Co1 N1 C13 92.76(18) . . . . ? O1 Co1 N1 C1 -120.7(4) . . . . ? N2 Co1 N1 C1 175.2(3) . . . . ? N5 Co1 N1 C1 84.8(3) . . . . ? N6 Co1 N1 C1 7.5(3) . . . . ? O3 Co1 N1 C1 -94.1(3) . . . . ? N3 C14 N2 C7 -0.6(3) . . . . ? C13 C14 N2 C7 175.8(2) . . . . ? N3 C14 N2 Co1 -176.27(17) . . . . ? C13 C14 N2 Co1 0.2(3) . . . . ? C8 C7 N2 C14 -178.8(3) . . . . ? C12 C7 N2 C14 0.8(3) . . . . ? C8 C7 N2 Co1 -5.6(5) . . . . ? C12 C7 N2 Co1 173.9(2) . . . . ? O1 Co1 N2 C14 -169.68(17) . . . . ? N1 Co1 N2 C14 -1.17(17) . . . . ? N5 Co1 N2 C14 84.49(18) . . . . ? N6 Co1 N2 C14 73.4(5) . . . . ? O3 Co1 N2 C14 -87.37(17) . . . . ? O1 Co1 N2 C7 17.4(3) . . . . ? N1 Co1 N2 C7 -174.1(3) . . . . ? N5 Co1 N2 C7 -88.4(3) . . . . ? N6 Co1 N2 C7 -99.5(5) . . . . ? O3 Co1 N2 C7 99.7(3) . . . . ? N2 C14 N3 C12 0.3(3) . . . . ? C13 C14 N3 C12 -175.7(3) . . . . ? N2 C14 N3 O3 -155.18(17) . . . 2_666 ? C13 C14 N3 O3 28.8(4) . . . 2_666 ? C11 C12 N3 C14 179.4(3) . . . . ? C7 C12 N3 C14 0.2(3) . . . . ? C11 C12 N3 O3 -23.7(4) . . . 2_666 ? C7 C12 N3 O3 157.09(16) . . . 2_666 ? N1 C13 N4 C6 0.1(3) . . . . ? C14 C13 N4 C6 178.7(2) . . . . ? N1 C13 N4 O4 -174.33(18) . . . 2_666 ? C14 C13 N4 O4 4.3(4) . . . 2_666 ? C5 C6 N4 C13 179.1(3) . . . . ? C1 C6 N4 C13 -0.5(3) . . . . ? C5 C6 N4 O4 -6.4(4) . . . 2_666 ? C1 C6 N4 O4 173.92(18) . . . 2_666 ? N8 C28 N5 C15 0.8(4) . . . . ? C27 C28 N5 C15 -173.9(3) . . . . ? N8 C28 N5 Co1 167.2(2) . . . . ? C27 C28 N5 Co1 -7.4(3) . . . . ? C16 C15 N5 C28 179.1(4) . . . . ? C20 C15 N5 C28 -0.4(4) . . . . ? C16 C15 N5 Co1 19.3(6) . . . . ? C20 C15 N5 Co1 -160.1(3) . . . . ? O1 Co1 N5 C28 91.1(2) . . . . ? N1 Co1 N5 C28 -94.6(2) . . . . ? N2 Co1 N5 C28 -173.7(2) . . . . ? N6 Co1 N5 C28 3.8(2) . . . . ? O3 Co1 N5 C28 -86.6(7) . . . . ? O1 Co1 N5 C15 -109.9(3) . . . . ? N1 Co1 N5 C15 64.5(4) . . . . ? N2 Co1 N5 C15 -14.7(4) . . . . ? N6 Co1 N5 C15 162.9(4) . . . . ? O3 Co1 N5 C15 72.4(8) . . . . ? N7 C27 N6 C21 0.0(3) . . . . ? C28 C27 N6 C21 179.2(3) . . . . ? N7 C27 N6 Co1 176.79(19) . . . . ? C28 C27 N6 Co1 -4.0(3) . . . . ? C22 C21 N6 C27 180.0(3) . . . . ? C26 C21 N6 C27 0.3(3) . . . . ? C22 C21 N6 Co1 5.1(6) . . . . ? C26 C21 N6 Co1 -174.6(2) . . . . ? O1 Co1 N6 C27 -105.85(19) . . . . ? N1 Co1 N6 C27 84.1(2) . . . . ? N2 Co1 N6 C27 11.5(5) . . . . ? N5 Co1 N6 C27 0.17(19) . . . . ? O3 Co1 N6 C27 171.84(19) . . . . ? O1 Co1 N6 C21 68.8(3) . . . . ? N1 Co1 N6 C21 -101.2(3) . . . . ? N2 Co1 N6 C21 -173.8(4) . . . . ? N5 Co1 N6 C21 174.8(3) . . . . ? O3 Co1 N6 C21 -13.5(3) . . . . ? N6 C27 N7 C26 -0.3(3) . . . . ? C28 C27 N7 C26 -179.4(3) . . . . ? N6 C27 N7 O2 178.6(2) . . . 2_777 ? C28 C27 N7 O2 -0.5(4) . . . 2_777 ? C25 C26 N7 C27 -178.2(4) . . . . ? C21 C26 N7 C27 0.4(3) . . . . ? C25 C26 N7 O2 3.6(6) . . . 2_777 ? C21 C26 N7 O2 -177.7(3) . . . 2_777 ? N5 C28 N8 C20 -0.9(4) . . . . ? C27 C28 N8 C20 173.3(3) . . . . ? N5 C28 N8 O2 169.3(2) . . . 2_777 ? C27 C28 N8 O2 -16.5(4) . . . 2_777 ? C19 C20 N8 C28 -177.4(4) . . . . ? C15 C20 N8 C28 0.6(4) . . . . ? C19 C20 N8 O2 18.9(8) . . . 2_777 ? C15 C20 N8 O2 -163.1(3) . . . 2_777 ? O2 C29 O1 Co1 95.9(3) . . . . ? C31 C29 O1 Co1 -85.9(3) . . . . ? N1 Co1 O1 C29 102.2(4) . . . . ? N2 Co1 O1 C29 164.7(2) . . . . ? N5 Co1 O1 C29 -104.3(2) . . . . ? N6 Co1 O1 C29 -26.5(2) . . . . ? O3 Co1 O1 C29 75.4(2) . . . . ? O4 C30 O3 Co1 99.5(4) . . . . ? C32 C30 O3 Co1 -84.3(3) . . . . ? O1 Co1 O3 C30 18.5(2) . . . . ? N1 Co1 O3 C30 -155.8(2) . . . . ? N2 Co1 O3 C30 -76.7(2) . . . . ? N5 Co1 O3 C30 -163.8(6) . . . . ? N6 Co1 O3 C30 107.5(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B O3 0.86 2.09 2.881(3) 152.4 2_666 N4 H4B O4 0.86 1.75 2.604(3) 173.3 2_666 N7 H7A O2 0.86 1.95 2.753(3) 154.0 2_777 N8 H8B O2 0.86 1.99 2.764(3) 150.0 2_777 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.444 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.065 #===============================END data_6 _database_code_depnum_ccdc_archive 'CCDC 286941' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H40 N12 Ni O7' _chemical_formula_weight 979.65 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 p2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.1901(2) _cell_length_b 28.2433(4) _cell_length_c 14.470 _cell_angle_alpha 90.00 _cell_angle_beta 92.3040(10) _cell_angle_gamma 90.00 _cell_volume 4977.93(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8707 _cell_measurement_theta_min 1.58 _cell_measurement_theta_max 25.04 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.453 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.909 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Simemens SMART CCD' _diffrn_measurement_method '\w scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 15973 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.04 _reflns_number_total 8707 _reflns_number_gt 6326 _reflns_threshold_expression >2sigma(I) _computing_data_collection ' Simens SMART ' _computing_cell_refinement ' Simens SMART ' _computing_data_reduction ' Simens SMART ' _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^)+(0.0000P)^2^+19.9041P] 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 8707 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1515 _refine_ls_R_factor_gt 0.1049 _refine_ls_wR_factor_ref 0.2101 _refine_ls_wR_factor_gt 0.1843 _refine_ls_goodness_of_fit_ref 1.321 _refine_ls_restrained_S_all 1.321 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.40386(7) 0.65292(3) 0.88499(5) 0.0383(2) Uani 1 1 d . . . C1 C 0.2380(6) 0.7436(2) 0.8101(5) 0.0503(18) Uani 1 1 d . . . C2 C 0.1404(7) 0.7259(3) 0.7706(6) 0.070(2) Uani 1 1 d . . . H2A H 0.1291 0.6935 0.7640 0.084 Uiso 1 1 calc R . . C3 C 0.0612(8) 0.7579(4) 0.7417(8) 0.099(4) Uani 1 1 d . . . H3A H -0.0048 0.7467 0.7157 0.119 Uiso 1 1 calc R . . C4 C 0.0769(8) 0.8064(3) 0.7503(7) 0.091(3) Uani 1 1 d . . . H4A H 0.0216 0.8269 0.7294 0.109 Uiso 1 1 calc R . . C5 C 0.1710(8) 0.8244(3) 0.7884(6) 0.077(3) Uani 1 1 d . . . H5A H 0.1813 0.8569 0.7943 0.092 Uiso 1 1 calc R . . C6 C 0.2528(6) 0.7923(3) 0.8189(5) 0.0522(18) Uani 1 1 d . . . C7 C 0.6324(5) 0.7020(2) 0.9808(5) 0.0459(16) Uani 1 1 d . . . C8 C 0.7046(6) 0.6659(3) 1.0097(6) 0.062(2) Uani 1 1 d . . . H8A H 0.6890 0.6343 0.9969 0.074 Uiso 1 1 calc R . . C9 C 0.7982(7) 0.6788(3) 1.0570(7) 0.085(3) Uani 1 1 d . . . H9A H 0.8466 0.6554 1.0781 0.102 Uiso 1 1 calc R . . C10 C 0.8240(8) 0.7264(4) 1.0749(8) 0.104(4) Uani 1 1 d . . . H10A H 0.8893 0.7337 1.1071 0.125 Uiso 1 1 calc R . . C11 C 0.7565(7) 0.7620(3) 1.0466(7) 0.089(3) Uani 1 1 d . . . H11A H 0.7736 0.7936 1.0587 0.107 Uiso 1 1 calc R . . C12 C 0.6604(6) 0.7490(3) 0.9987(5) 0.057(2) Uani 1 1 d . . . C13 C 0.3969(6) 0.7562(2) 0.8780(4) 0.0412(15) Uani 1 1 d . . . C14 C 0.4999(5) 0.7451(2) 0.9235(4) 0.0404(15) Uani 1 1 d . . . C15 C 0.5666(5) 0.5600(2) 0.9307(5) 0.0439(16) Uani 1 1 d . . . C16 C 0.6158(6) 0.5464(2) 0.8500(5) 0.0540(19) Uani 1 1 d . . . H16A H 0.5946 0.5596 0.7931 0.065 Uiso 1 1 calc R . . C17 C 0.6975(6) 0.5126(3) 0.8574(6) 0.063(2) Uani 1 1 d . . . H17A H 0.7309 0.5023 0.8044 0.075 Uiso 1 1 calc R . . C18 C 0.7310(6) 0.4936(3) 0.9433(6) 0.063(2) Uani 1 1 d . . . H18A H 0.7886 0.4720 0.9459 0.075 Uiso 1 1 calc R . . C19 C 0.6822(6) 0.5057(3) 1.0234(6) 0.0558(19) Uani 1 1 d . . . H19A H 0.7031 0.4920 1.0798 0.067 Uiso 1 1 calc R . . C20 C 0.5992(5) 0.5397(2) 1.0157(5) 0.0459(17) Uani 1 1 d . . . C21 C 0.2641(5) 0.6775(2) 1.0700(4) 0.0438(16) Uani 1 1 d . . . C22 C 0.1920(6) 0.7143(3) 1.0489(5) 0.0542(19) Uani 1 1 d . . . H22A H 0.1872 0.7274 0.9899 0.065 Uiso 1 1 calc R . . C23 C 0.1280(7) 0.7306(3) 1.1177(6) 0.074(2) Uani 1 1 d . . . H23A H 0.0790 0.7552 1.1047 0.089 Uiso 1 1 calc R . . C24 C 0.1343(8) 0.7116(4) 1.2063(6) 0.089(3) Uani 1 1 d . . . H24A H 0.0899 0.7239 1.2512 0.107 Uiso 1 1 calc R . . C25 C 0.2049(8) 0.6749(3) 1.2291(6) 0.081(3) Uani 1 1 d . . . H25A H 0.2090 0.6620 1.2883 0.097 Uiso 1 1 calc R . . C26 C 0.2696(6) 0.6581(3) 1.1595(4) 0.0502(17) Uani 1 1 d . . . C27 C 0.4674(5) 0.5915(2) 1.0355(4) 0.0372(14) Uani 1 1 d . . . C28 C 0.3858(5) 0.6218(2) 1.0724(4) 0.0412(15) Uani 1 1 d . . . C29 C 0.5597(6) 0.6489(3) 0.7038(5) 0.0516(18) Uani 1 1 d . . . C30 C 0.6658(6) 0.6602(3) 0.7339(6) 0.066(2) Uani 1 1 d . . . H30A H 0.6833 0.6672 0.7955 0.080 Uiso 1 1 calc R . . C31 C 0.7449(8) 0.6606(4) 0.6668(7) 0.091(3) Uani 1 1 d . . . H31A H 0.8173 0.6678 0.6841 0.109 Uiso 1 1 calc R . . C32 C 0.7175(9) 0.6503(4) 0.5739(7) 0.092(3) Uani 1 1 d . . . H32A H 0.7725 0.6514 0.5312 0.110 Uiso 1 1 calc R . . C33 C 0.6136(9) 0.6388(3) 0.5437(6) 0.082(3) Uani 1 1 d . . . H33A H 0.5964 0.6320 0.4819 0.098 Uiso 1 1 calc R . . C34 C 0.5339(7) 0.6377(3) 0.6111(5) 0.058(2) Uani 1 1 d . . . C35 C 0.1617(6) 0.6057(2) 0.8284(5) 0.0514(18) Uani 1 1 d . . . C36 C 0.1030(6) 0.6018(3) 0.9087(6) 0.062(2) Uani 1 1 d . . . H36A H 0.1369 0.6064 0.9667 0.074 Uiso 1 1 calc R . . C37 C -0.0069(7) 0.5908(3) 0.8990(7) 0.084(3) Uani 1 1 d . . . H37A H -0.0475 0.5871 0.9516 0.101 Uiso 1 1 calc R . . C38 C -0.0588(8) 0.5853(4) 0.8112(8) 0.092(3) Uani 1 1 d . . . H38A H -0.1336 0.5788 0.8071 0.110 Uiso 1 1 calc R . . C39 C -0.0025(8) 0.5891(3) 0.7317(7) 0.083(3) Uani 1 1 d . . . H39A H -0.0368 0.5851 0.6736 0.100 Uiso 1 1 calc R . . C40 C 0.1085(6) 0.5992(3) 0.7425(6) 0.060(2) Uani 1 1 d . . . C41 C 0.3878(6) 0.6292(2) 0.6918(4) 0.0437(16) Uani 1 1 d . . . C42 C 0.2811(6) 0.6177(2) 0.7252(5) 0.0489(17) Uani 1 1 d . . . C43 C 0.4756(8) 0.5463(3) 1.3205(5) 0.061(2) Uani 1 1 d . . . C44 C 0.4892(7) 0.5210(3) 1.4130(5) 0.057(2) Uani 1 1 d . . . C45 C 0.3978(7) 0.5048(3) 1.4574(5) 0.069(2) Uani 1 1 d . . . H45A H 0.3284 0.5079 1.4290 0.082 Uiso 1 1 calc R . . C46 C 0.5906(7) 0.5161(3) 1.4561(5) 0.069(2) Uani 1 1 d . . . H46A H 0.6524 0.5269 1.4269 0.083 Uiso 1 1 calc R . . C47 C 0.5079(7) 0.8991(3) 0.9644(6) 0.060(2) Uani 1 1 d . . . C48 C 0.5055(6) 0.9515(2) 0.9830(5) 0.0517(18) Uani 1 1 d . . . C49 C 0.4076(6) 0.9753(3) 0.9742(6) 0.068(2) Uani 1 1 d . . . H49A H 0.3441 0.9588 0.9568 0.081 Uiso 1 1 calc R . . C50 C 0.5983(7) 0.9766(3) 1.0093(6) 0.068(2) Uani 1 1 d . . . H50A H 0.6654 0.9611 1.0160 0.082 Uiso 1 1 calc R . . O1 O 0.5535(5) 0.5454(2) 1.2676(4) 0.0818(19) Uani 1 1 d . . . O1W O 0.993(4) 0.5594(16) 1.195(3) 0.31(2) Uani 0.50 1 d P . . O2 O 0.3854(5) 0.5668(2) 1.3036(3) 0.0702(16) Uani 1 1 d . . . O2W O 0.908(4) 0.5494(16) 1.196(3) 0.35(4) Uani 0.50 1 d P . . O3 O 0.4278(6) 0.88162(19) 0.9219(5) 0.093(2) Uani 1 1 d . . . O3W O 0.7840(19) 0.5222(11) 1.2462(10) 0.50(2) Uani 1 1 d . . . O4W O 0.3035(5) 0.6168(2) 1.4454(4) 0.0809(17) Uani 1 1 d . . . O4 O 0.5918(5) 0.87558(18) 0.9929(4) 0.0733(16) Uani 1 1 d . . . N1 N 0.3317(4) 0.72130(18) 0.8476(4) 0.0424(13) Uani 1 1 d . . . N2 N 0.5309(4) 0.70025(19) 0.9331(4) 0.0430(13) Uani 1 1 d . . . N3 N 0.5742(5) 0.7760(2) 0.9611(4) 0.0554(16) Uani 1 1 d . . . H3B H 0.5691 0.8063 0.9616 0.066 Uiso 1 1 calc R . . N4 N 0.3535(5) 0.79928(19) 0.8616(4) 0.0488(14) Uani 1 1 d . . . H4B H 0.3834 0.8261 0.8753 0.059 Uiso 1 1 calc R . . N5 N 0.4840(4) 0.59310(18) 0.9455(3) 0.0388(12) Uani 1 1 d . . . N6 N 0.3385(4) 0.65376(18) 1.0165(3) 0.0388(12) Uani 1 1 d . . . N7 N 0.3474(5) 0.6224(2) 1.1585(4) 0.0500(15) Uani 1 1 d . . . H7A H 0.3673 0.6043 1.2038 0.060 Uiso 1 1 calc R . . N8 N 0.5341(4) 0.56024(19) 1.0808(4) 0.0451(14) Uani 1 1 d . . . H8B H 0.5357 0.5542 1.1391 0.054 Uiso 1 1 calc R . . N9 N 0.4648(4) 0.64327(19) 0.7531(3) 0.0425(13) Uani 1 1 d . . . N10 N 0.2706(4) 0.61810(18) 0.8166(4) 0.0405(13) Uani 1 1 d . . . N11 N 0.4253(6) 0.6258(2) 0.6055(4) 0.0597(17) Uani 1 1 d . . . H11B H 0.3879 0.6177 0.5564 0.072 Uiso 1 1 calc R . . N12 N 0.1875(5) 0.6072(2) 0.6776(4) 0.0600(17) Uani 1 1 d . . . H12A H 0.1781 0.6057 0.6184 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0474(5) 0.0354(4) 0.0320(4) 0.0041(4) 0.0000(3) -0.0023(4) C1 0.054(4) 0.048(4) 0.048(4) 0.007(3) -0.006(3) 0.004(3) C2 0.068(6) 0.056(5) 0.083(6) 0.006(4) -0.025(5) 0.000(4) C3 0.079(7) 0.087(8) 0.126(9) 0.018(7) -0.051(6) 0.009(6) C4 0.078(7) 0.072(7) 0.119(9) 0.017(6) -0.032(6) 0.018(5) C5 0.085(7) 0.054(5) 0.090(7) 0.018(5) -0.008(5) 0.012(5) C6 0.061(5) 0.048(4) 0.047(4) 0.011(3) 0.000(4) 0.008(4) C7 0.043(4) 0.044(4) 0.050(4) -0.001(3) 0.000(3) -0.009(3) C8 0.048(4) 0.059(5) 0.077(6) 0.003(4) -0.009(4) 0.004(4) C9 0.066(6) 0.077(6) 0.110(8) 0.003(6) -0.032(5) 0.010(5) C10 0.063(6) 0.092(8) 0.153(11) -0.018(7) -0.046(7) -0.009(6) C11 0.065(6) 0.065(6) 0.133(9) -0.019(6) -0.028(6) -0.010(5) C12 0.052(5) 0.050(5) 0.068(5) -0.010(4) -0.004(4) 0.000(4) C13 0.055(4) 0.030(3) 0.039(4) 0.004(3) 0.005(3) -0.006(3) C14 0.050(4) 0.036(4) 0.036(3) 0.001(3) 0.006(3) -0.007(3) C15 0.046(4) 0.037(4) 0.049(4) 0.001(3) 0.005(3) -0.003(3) C16 0.066(5) 0.046(4) 0.052(4) 0.001(3) 0.020(4) -0.002(4) C17 0.062(5) 0.056(5) 0.072(6) -0.005(4) 0.026(4) -0.003(4) C18 0.049(5) 0.052(5) 0.088(6) 0.000(4) 0.010(4) 0.003(4) C19 0.049(4) 0.049(4) 0.069(5) 0.009(4) 0.003(4) 0.008(3) C20 0.040(4) 0.048(4) 0.050(4) 0.008(3) 0.001(3) -0.003(3) C21 0.048(4) 0.045(4) 0.039(4) 0.000(3) 0.000(3) 0.001(3) C22 0.057(5) 0.054(5) 0.052(4) 0.005(4) 0.009(4) 0.010(4) C23 0.076(6) 0.081(6) 0.066(5) 0.009(5) 0.012(5) 0.027(5) C24 0.100(7) 0.102(8) 0.068(6) 0.006(5) 0.039(5) 0.038(6) C25 0.103(7) 0.097(7) 0.046(5) 0.011(5) 0.024(5) 0.035(6) C26 0.062(5) 0.055(4) 0.034(4) 0.003(3) 0.000(3) 0.006(4) C27 0.040(4) 0.030(3) 0.041(4) 0.007(3) -0.002(3) -0.002(3) C28 0.046(4) 0.045(4) 0.033(3) 0.002(3) 0.006(3) -0.001(3) C29 0.056(5) 0.047(4) 0.052(4) 0.012(3) 0.007(4) 0.004(4) C30 0.062(5) 0.080(6) 0.059(5) 0.018(4) 0.018(4) 0.010(4) C31 0.068(6) 0.108(8) 0.098(8) 0.023(6) 0.016(6) -0.002(6) C32 0.084(7) 0.106(8) 0.087(7) 0.004(6) 0.039(6) 0.009(6) C33 0.097(8) 0.086(7) 0.065(6) 0.003(5) 0.025(5) -0.002(6) C34 0.064(5) 0.061(5) 0.050(5) 0.001(4) 0.016(4) -0.004(4) C35 0.061(5) 0.039(4) 0.054(4) 0.001(3) -0.003(4) -0.004(3) C36 0.061(5) 0.061(5) 0.064(5) -0.001(4) 0.007(4) -0.005(4) C37 0.061(6) 0.098(7) 0.094(7) 0.008(6) 0.021(5) -0.019(5) C38 0.057(6) 0.108(8) 0.110(9) 0.003(7) -0.003(6) -0.022(5) C39 0.073(6) 0.090(7) 0.085(7) -0.002(5) -0.015(5) -0.024(5) C40 0.055(5) 0.058(5) 0.065(5) -0.004(4) -0.012(4) -0.014(4) C41 0.061(4) 0.038(4) 0.032(3) 0.003(3) -0.002(3) 0.002(3) C42 0.067(5) 0.042(4) 0.037(4) -0.001(3) -0.003(3) -0.013(4) C43 0.080(6) 0.066(5) 0.037(4) 0.015(4) -0.006(4) -0.004(5) C44 0.075(5) 0.061(5) 0.034(4) 0.012(3) -0.003(4) -0.004(4) C45 0.065(5) 0.088(6) 0.052(5) 0.020(4) -0.012(4) 0.004(5) C46 0.060(5) 0.096(7) 0.052(5) 0.027(5) -0.005(4) -0.012(5) C47 0.067(5) 0.047(5) 0.066(5) 0.000(4) 0.002(4) -0.006(4) C48 0.060(5) 0.036(4) 0.058(5) -0.003(3) -0.009(4) -0.002(3) C49 0.053(5) 0.043(4) 0.105(7) -0.002(4) -0.025(5) -0.005(4) C50 0.063(5) 0.036(4) 0.105(7) -0.001(4) -0.008(5) 0.008(4) O1 0.081(4) 0.119(5) 0.046(3) 0.029(3) 0.004(3) 0.011(4) O1W 0.34(5) 0.35(6) 0.25(4) -0.12(4) 0.05(4) 0.12(4) O2 0.089(4) 0.082(4) 0.040(3) 0.019(3) 0.001(3) 0.023(3) O2W 0.43(7) 0.28(4) 0.31(5) 0.13(4) -0.16(5) -0.25(5) O3 0.104(5) 0.045(3) 0.127(6) -0.019(3) -0.032(4) -0.006(3) O3W 0.46(3) 0.88(5) 0.151(12) -0.18(2) -0.133(16) 0.52(3) O4W 0.088(4) 0.103(5) 0.050(3) -0.012(3) -0.007(3) 0.001(4) O4 0.082(4) 0.046(3) 0.092(4) -0.004(3) -0.005(3) 0.006(3) N1 0.054(3) 0.037(3) 0.037(3) 0.007(2) 0.004(3) -0.001(3) N2 0.047(3) 0.044(3) 0.038(3) -0.005(2) 0.002(3) -0.004(3) N3 0.057(4) 0.041(3) 0.068(4) -0.008(3) 0.003(3) -0.006(3) N4 0.063(4) 0.032(3) 0.052(4) 0.005(3) -0.002(3) 0.000(3) N5 0.046(3) 0.036(3) 0.035(3) 0.007(2) 0.003(2) -0.002(2) N6 0.045(3) 0.040(3) 0.032(3) 0.006(2) 0.002(2) 0.006(3) N7 0.066(4) 0.055(4) 0.030(3) 0.006(3) 0.004(3) 0.013(3) N8 0.052(3) 0.047(3) 0.037(3) 0.010(3) 0.005(3) -0.001(3) N9 0.048(3) 0.046(3) 0.034(3) 0.006(2) 0.000(3) -0.006(3) N10 0.043(3) 0.039(3) 0.039(3) 0.007(2) -0.003(2) -0.009(2) N11 0.083(5) 0.060(4) 0.036(3) -0.006(3) 0.002(3) -0.010(3) N12 0.063(4) 0.063(4) 0.054(4) -0.005(3) -0.011(3) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N9 2.093(5) . ? Ni1 N6 2.093(5) . ? Ni1 N10 2.111(5) . ? Ni1 N5 2.123(5) . ? Ni1 N2 2.141(5) . ? Ni1 N1 2.182(5) . ? C1 C2 1.391(10) . ? C1 C6 1.394(10) . ? C1 N1 1.395(8) . ? C2 C3 1.375(11) . ? C2 H2A 0.9300 . ? C3 C4 1.388(13) . ? C3 H3A 0.9300 . ? C4 C5 1.352(12) . ? C4 H4A 0.9300 . ? C5 C6 1.405(10) . ? C5 H5A 0.9300 . ? C6 N4 1.366(9) . ? C7 N2 1.393(8) . ? C7 C12 1.394(9) . ? C7 C8 1.399(10) . ? C8 C9 1.356(11) . ? C8 H8A 0.9300 . ? C9 C10 1.403(12) . ? C9 H9A 0.9300 . ? C10 C11 1.353(12) . ? C10 H10A 0.9300 . ? C11 C12 1.387(10) . ? C11 H11A 0.9300 . ? C12 N3 1.390(9) . ? C13 N1 1.330(8) . ? C13 N4 1.344(8) . ? C13 C14 1.429(9) . ? C14 N2 1.327(8) . ? C14 N3 1.356(8) . ? C15 C16 1.387(9) . ? C15 N5 1.397(8) . ? C15 C20 1.400(9) . ? C16 C17 1.381(10) . ? C16 H16A 0.9300 . ? C17 C18 1.399(11) . ? C17 H17A 0.9300 . ? C18 C19 1.367(10) . ? C18 H18A 0.9300 . ? C19 C20 1.398(9) . ? C19 H19A 0.9300 . ? C20 N8 1.383(8) . ? C21 C22 1.388(9) . ? C21 N6 1.388(8) . ? C21 C26 1.405(9) . ? C22 C23 1.369(10) . ? C22 H22A 0.9300 . ? C23 C24 1.389(11) . ? C23 H23A 0.9300 . ? C24 C25 1.380(11) . ? C24 H24A 0.9300 . ? C25 C26 1.387(10) . ? C25 H25A 0.9300 . ? C26 N7 1.384(8) . ? C27 N5 1.327(8) . ? C27 N8 1.352(8) . ? C27 C28 1.431(9) . ? C28 N6 1.329(8) . ? C28 N7 1.349(8) . ? C29 C30 1.385(10) . ? C29 N9 1.393(8) . ? C29 C34 1.402(10) . ? C30 C31 1.395(11) . ? C30 H30A 0.9300 . ? C31 C32 1.403(13) . ? C31 H31A 0.9300 . ? C32 C33 1.363(13) . ? C32 H32A 0.9300 . ? C33 C34 1.404(11) . ? C33 H33A 0.9300 . ? C34 N11 1.365(9) . ? C35 N10 1.390(9) . ? C35 C40 1.390(10) . ? C35 C36 1.393(10) . ? C36 C37 1.376(11) . ? C36 H36A 0.9300 . ? C37 C38 1.405(13) . ? C37 H37A 0.9300 . ? C38 C39 1.368(13) . ? C38 H38A 0.9300 . ? C39 C40 1.386(11) . ? C39 H39A 0.9300 . ? C40 N12 1.390(10) . ? C41 N9 1.326(8) . ? C41 N11 1.350(8) . ? C41 C42 1.443(9) . ? C42 N10 1.334(8) . ? C42 N12 1.343(8) . ? C43 O1 1.244(9) 1 ? C43 O1 1.244(9) . ? C43 O2 1.258(9) 1 ? C43 O2 1.258(9) . ? C43 C44 1.521(9) . ? C44 C46 1.368(10) . ? C44 C45 1.387(10) . ? C45 C46 1.386(10) 3_668 ? C45 H45A 0.9300 . ? C46 C45 1.386(10) 3_668 ? C46 H46A 0.9300 . ? C47 O3 1.236(9) 1 ? C47 O3 1.236(9) . ? C47 O4 1.274(9) 1 ? C47 O4 1.274(9) . ? C47 C48 1.505(10) . ? C48 C49 1.371(10) . ? C48 C50 1.375(10) . ? C49 C50 1.382(10) 3_677 ? C49 H49A 0.9300 . ? C50 C49 1.382(10) 3_677 ? C50 H50A 0.9300 . ? O1 O1 0.000(13) 1 ? O1W O2W 1.08(6) . ? O2 O2 0.0000 1 ? O3 O3 0.000(11) 1 ? O4 O4 0.00(2) 1 ? N3 O4 2.857(8) 1 ? N3 H3B 0.8600 . ? N4 O3 2.632(8) 1 ? N4 H4B 0.8600 . ? N7 O2 2.648(7) 1 ? N7 H7A 0.8600 . ? N8 O1 2.737(7) 1 ? N8 H8B 0.8600 . ? N11 H11B 0.8600 . ? N12 O4 2.913(9) 4_575 ? N12 H12A 0.8600 . ? 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 N9 Ni1 N6 173.0(2) . . ? N9 Ni1 N10 78.9(2) . . ? N6 Ni1 N10 96.8(2) . . ? N9 Ni1 N5 95.6(2) . . ? N6 Ni1 N5 79.63(19) . . ? N10 Ni1 N5 98.9(2) . . ? N9 Ni1 N2 95.7(2) . . ? N6 Ni1 N2 89.7(2) . . ? N10 Ni1 N2 167.5(2) . . ? N5 Ni1 N2 92.8(2) . . ? N9 Ni1 N1 92.5(2) . . ? N6 Ni1 N1 92.92(19) . . ? N10 Ni1 N1 90.1(2) . . ? N5 Ni1 N1 168.9(2) . . ? N2 Ni1 N1 78.9(2) . . ? C2 C1 C6 119.8(7) . . ? C2 C1 N1 132.2(7) . . ? C6 C1 N1 108.0(6) . . ? C3 C2 C1 117.8(8) . . ? C3 C2 H2A 121.1 . . ? C1 C2 H2A 121.1 . . ? C2 C3 C4 122.0(9) . . ? C2 C3 H3A 119.0 . . ? C4 C3 H3A 119.0 . . ? C5 C4 C3 121.2(8) . . ? C5 C4 H4A 119.4 . . ? C3 C4 H4A 119.4 . . ? C4 C5 C6 117.8(8) . . ? C4 C5 H5A 121.1 . . ? C6 C5 H5A 121.1 . . ? N4 C6 C1 107.1(6) . . ? N4 C6 C5 131.5(7) . . ? C1 C6 C5 121.4(8) . . ? N2 C7 C12 109.3(6) . . ? N2 C7 C8 131.2(6) . . ? C12 C7 C8 119.5(7) . . ? C9 C8 C7 117.5(8) . . ? C9 C8 H8A 121.2 . . ? C7 C8 H8A 121.2 . . ? C8 C9 C10 121.9(8) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C11 C10 C9 121.9(8) . . ? C11 C10 H10A 119.1 . . ? C9 C10 H10A 119.1 . . ? C10 C11 C12 116.4(8) . . ? C10 C11 H11A 121.8 . . ? C12 C11 H11A 121.8 . . ? C11 C12 N3 131.3(7) . . ? C11 C12 C7 122.7(8) . . ? N3 C12 C7 105.9(6) . . ? N1 C13 N4 112.8(6) . . ? N1 C13 C14 119.4(6) . . ? N4 C13 C14 127.8(6) . . ? N2 C14 N3 112.9(6) . . ? N2 C14 C13 120.0(6) . . ? N3 C14 C13 127.1(6) . . ? C16 C15 N5 130.7(6) . . ? C16 C15 C20 120.7(7) . . ? N5 C15 C20 108.6(6) . . ? C17 C16 C15 117.4(7) . . ? C17 C16 H16A 121.3 . . ? C15 C16 H16A 121.3 . . ? C16 C17 C18 121.2(7) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C19 C18 C17 122.4(7) . . ? C19 C18 H18A 118.8 . . ? C17 C18 H18A 118.8 . . ? C18 C19 C20 116.2(7) . . ? C18 C19 H19A 121.9 . . ? C20 C19 H19A 121.9 . . ? N8 C20 C19 131.9(7) . . ? N8 C20 C15 106.1(6) . . ? C19 C20 C15 122.0(7) . . ? C22 C21 N6 131.4(6) . . ? C22 C21 C26 120.1(6) . . ? N6 C21 C26 108.5(6) . . ? C23 C22 C21 117.8(7) . . ? C23 C22 H22A 121.1 . . ? C21 C22 H22A 121.1 . . ? C22 C23 C24 121.9(8) . . ? C22 C23 H23A 119.0 . . ? C24 C23 H23A 119.0 . . ? C25 C24 C23 121.5(8) . . ? C25 C24 H24A 119.3 . . ? C23 C24 H24A 119.3 . . ? C24 C25 C26 116.7(8) . . ? C24 C25 H25A 121.6 . . ? C26 C25 H25A 121.6 . . ? N7 C26 C25 131.7(7) . . ? N7 C26 C21 106.3(6) . . ? C25 C26 C21 121.9(7) . . ? N5 C27 N8 112.7(6) . . ? N5 C27 C28 118.8(6) . . ? N8 C27 C28 128.5(6) . . ? N6 C28 N7 113.2(6) . . ? N6 C28 C27 118.1(5) . . ? N7 C28 C27 128.7(6) . . ? C30 C29 N9 130.5(7) . . ? C30 C29 C34 121.5(7) . . ? N9 C29 C34 107.8(6) . . ? C29 C30 C31 116.5(8) . . ? C29 C30 H30A 121.7 . . ? C31 C30 H30A 121.7 . . ? C30 C31 C32 121.3(9) . . ? C30 C31 H31A 119.3 . . ? C32 C31 H31A 119.3 . . ? C33 C32 C31 122.6(9) . . ? C33 C32 H32A 118.7 . . ? C31 C32 H32A 118.7 . . ? C32 C33 C34 116.2(9) . . ? C32 C33 H33A 121.9 . . ? C34 C33 H33A 121.9 . . ? N11 C34 C29 106.9(6) . . ? N11 C34 C33 131.3(8) . . ? C29 C34 C33 121.7(8) . . ? N10 C35 C40 109.7(6) . . ? N10 C35 C36 130.3(7) . . ? C40 C35 C36 119.9(7) . . ? C37 C36 C35 117.6(8) . . ? C37 C36 H36A 121.2 . . ? C35 C36 H36A 121.2 . . ? C36 C37 C38 121.2(9) . . ? C36 C37 H37A 119.4 . . ? C38 C37 H37A 119.4 . . ? C39 C38 C37 122.0(9) . . ? C39 C38 H38A 119.0 . . ? C37 C38 H38A 119.0 . . ? C38 C39 C40 116.2(9) . . ? C38 C39 H39A 121.9 . . ? C40 C39 H39A 121.9 . . ? C39 C40 N12 131.1(8) . . ? C39 C40 C35 123.1(8) . . ? N12 C40 C35 105.8(6) . . ? N9 C41 N11 112.5(6) . . ? N9 C41 C42 117.8(6) . . ? N11 C41 C42 129.6(6) . . ? N10 C42 N12 113.4(6) . . ? N10 C42 C41 117.0(6) . . ? N12 C42 C41 129.6(6) . . ? O1 C43 O1 0.0(8) 1 . ? O1 C43 O2 125.0(7) 1 1 ? O1 C43 O2 125.0(7) . 1 ? O1 C43 O2 125.0(7) 1 . ? O1 C43 O2 125.0(7) . . ? O2 C43 O2 0.0(3) 1 . ? O1 C43 C44 118.2(8) 1 . ? O1 C43 C44 118.2(8) . . ? O2 C43 C44 116.9(7) 1 . ? O2 C43 C44 116.9(7) . . ? C46 C44 C45 118.9(7) . . ? C46 C44 C43 120.9(7) . . ? C45 C44 C43 120.1(7) . . ? C46 C45 C44 120.3(7) 3_668 . ? C46 C45 H45A 119.9 3_668 . ? C44 C45 H45A 119.9 . . ? C44 C46 C45 120.8(7) . 3_668 ? C44 C46 H46A 119.6 . . ? C45 C46 H46A 119.6 3_668 . ? O3 C47 O3 0.0(6) 1 . ? O3 C47 O4 124.1(8) 1 1 ? O3 C47 O4 124.1(8) . 1 ? O3 C47 O4 124.1(8) 1 . ? O3 C47 O4 124.1(8) . . ? O4 C47 O4 0.0(7) 1 . ? O3 C47 C48 117.4(7) 1 . ? O3 C47 C48 117.4(7) . . ? O4 C47 C48 118.4(7) 1 . ? O4 C47 C48 118.4(7) . . ? C49 C48 C50 118.4(7) . . ? C49 C48 C47 119.3(7) . . ? C50 C48 C47 122.3(7) . . ? C48 C49 C50 121.2(7) . 3_677 ? C48 C49 H49A 119.4 . . ? C50 C49 H49A 119.4 3_677 . ? C48 C50 C49 120.4(7) . 3_677 ? C48 C50 H50A 119.8 . . ? C49 C50 H50A 119.8 3_677 . ? O1 O1 C43 0(10) 1 . ? O2 O2 C43 0(10) 1 . ? O3 O3 C47 0(10) 1 . ? O4 O4 C47 0(10) 1 . ? C13 N1 C1 105.3(6) . . ? C13 N1 Ni1 110.2(4) . . ? C1 N1 Ni1 144.2(5) . . ? C14 N2 C7 105.2(5) . . ? C14 N2 Ni1 111.3(4) . . ? C7 N2 Ni1 143.0(4) . . ? C14 N3 C12 106.7(6) . . ? C14 N3 O4 138.0(5) . 1 ? C12 N3 O4 115.2(4) . 1 ? C14 N3 H3B 126.7 . . ? C12 N3 H3B 126.7 . . ? O4 N3 H3B 12.0 1 . ? C13 N4 C6 106.8(6) . . ? C13 N4 O3 127.9(5) . 1 ? C6 N4 O3 124.6(5) . 1 ? C13 N4 H4B 126.6 . . ? C6 N4 H4B 126.6 . . ? O3 N4 H4B 7.5 1 . ? C27 N5 C15 105.5(5) . . ? C27 N5 Ni1 110.2(4) . . ? C15 N5 Ni1 142.4(4) . . ? C28 N6 C21 105.5(5) . . ? C28 N6 Ni1 111.9(4) . . ? C21 N6 Ni1 142.5(4) . . ? C28 N7 C26 106.5(5) . . ? C28 N7 O2 131.9(5) . 1 ? C26 N7 O2 121.4(4) . 1 ? C28 N7 H7A 126.8 . . ? C26 N7 H7A 126.8 . . ? O2 N7 H7A 6.5 1 . ? C27 N8 C20 107.1(5) . . ? C27 N8 O1 127.3(4) . 1 ? C20 N8 O1 125.4(4) . 1 ? C27 N8 H8B 126.5 . . ? C20 N8 H8B 126.5 . . ? O1 N8 H8B 4.4 1 . ? C41 N9 C29 105.7(6) . . ? C41 N9 Ni1 112.4(4) . . ? C29 N9 Ni1 141.7(5) . . ? C42 N10 C35 104.4(6) . . ? C42 N10 Ni1 111.5(4) . . ? C35 N10 Ni1 141.4(5) . . ? C41 N11 C34 107.0(6) . . ? C41 N11 H11B 126.5 . . ? C34 N11 H11B 126.5 . . ? C42 N12 C40 106.7(6) . . ? C42 N12 O4 137.3(5) . 4_575 ? C40 N12 O4 112.6(5) . 4_575 ? C42 N12 H12A 126.7 . . ? C40 N12 H12A 126.7 . . ? O4 N12 H12A 20.5 4_575 . ? 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 C6 C1 C2 C3 -0.2(13) . . . . ? N1 C1 C2 C3 178.4(9) . . . . ? C1 C2 C3 C4 0.6(16) . . . . ? C2 C3 C4 C5 -0.6(18) . . . . ? C3 C4 C5 C6 0.2(16) . . . . ? C2 C1 C6 N4 178.5(7) . . . . ? N1 C1 C6 N4 -0.4(8) . . . . ? C2 C1 C6 C5 -0.2(12) . . . . ? N1 C1 C6 C5 -179.1(7) . . . . ? C4 C5 C6 N4 -178.1(9) . . . . ? C4 C5 C6 C1 0.2(13) . . . . ? N2 C7 C8 C9 -179.0(8) . . . . ? C12 C7 C8 C9 2.1(12) . . . . ? C7 C8 C9 C10 -1.5(15) . . . . ? C8 C9 C10 C11 0.5(19) . . . . ? C9 C10 C11 C12 -0.2(18) . . . . ? C10 C11 C12 N3 179.5(10) . . . . ? C10 C11 C12 C7 0.8(15) . . . . ? N2 C7 C12 C11 179.0(8) . . . . ? C8 C7 C12 C11 -1.8(12) . . . . ? N2 C7 C12 N3 0.1(8) . . . . ? C8 C7 C12 N3 179.2(7) . . . . ? N1 C13 C14 N2 1.7(9) . . . . ? N4 C13 C14 N2 -179.2(6) . . . . ? N1 C13 C14 N3 -177.8(6) . . . . ? N4 C13 C14 N3 1.3(11) . . . . ? N5 C15 C16 C17 179.2(7) . . . . ? C20 C15 C16 C17 -0.2(10) . . . . ? C15 C16 C17 C18 -1.4(11) . . . . ? C16 C17 C18 C19 2.9(12) . . . . ? C17 C18 C19 C20 -2.5(11) . . . . ? C18 C19 C20 N8 -179.5(7) . . . . ? C18 C19 C20 C15 0.9(11) . . . . ? C16 C15 C20 N8 -179.3(6) . . . . ? N5 C15 C20 N8 1.2(7) . . . . ? C16 C15 C20 C19 0.5(10) . . . . ? N5 C15 C20 C19 -179.0(6) . . . . ? N6 C21 C22 C23 -179.8(7) . . . . ? C26 C21 C22 C23 0.3(11) . . . . ? C21 C22 C23 C24 0.2(13) . . . . ? C22 C23 C24 C25 -0.6(16) . . . . ? C23 C24 C25 C26 0.3(16) . . . . ? C24 C25 C26 N7 -179.9(9) . . . . ? C24 C25 C26 C21 0.1(14) . . . . ? C22 C21 C26 N7 179.6(6) . . . . ? N6 C21 C26 N7 -0.4(8) . . . . ? C22 C21 C26 C25 -0.5(12) . . . . ? N6 C21 C26 C25 179.6(7) . . . . ? N5 C27 C28 N6 -7.1(9) . . . . ? N8 C27 C28 N6 172.3(6) . . . . ? N5 C27 C28 N7 172.2(6) . . . . ? N8 C27 C28 N7 -8.4(11) . . . . ? N9 C29 C30 C31 176.6(8) . . . . ? C34 C29 C30 C31 0.9(12) . . . . ? C29 C30 C31 C32 0.4(14) . . . . ? C30 C31 C32 C33 -0.9(17) . . . . ? C31 C32 C33 C34 0.1(15) . . . . ? C30 C29 C34 N11 176.7(7) . . . . ? N9 C29 C34 N11 0.1(8) . . . . ? C30 C29 C34 C33 -1.7(12) . . . . ? N9 C29 C34 C33 -178.4(7) . . . . ? C32 C33 C34 N11 -176.8(9) . . . . ? C32 C33 C34 C29 1.2(13) . . . . ? N10 C35 C36 C37 177.0(8) . . . . ? C40 C35 C36 C37 0.8(12) . . . . ? C35 C36 C37 C38 -1.9(14) . . . . ? C36 C37 C38 C39 1.9(16) . . . . ? C37 C38 C39 C40 -0.7(16) . . . . ? C38 C39 C40 N12 -177.2(9) . . . . ? C38 C39 C40 C35 -0.4(14) . . . . ? N10 C35 C40 C39 -176.5(8) . . . . ? C36 C35 C40 C39 0.3(12) . . . . ? N10 C35 C40 N12 0.9(8) . . . . ? C36 C35 C40 N12 177.8(7) . . . . ? N9 C41 C42 N10 -5.6(9) . . . . ? N11 C41 C42 N10 170.8(7) . . . . ? N9 C41 C42 N12 172.8(7) . . . . ? N11 C41 C42 N12 -10.8(13) . . . . ? O1 C43 C44 C46 28.8(12) 1 . . . ? O1 C43 C44 C46 28.8(12) . . . . ? O2 C43 C44 C46 -150.9(8) 1 . . . ? O2 C43 C44 C46 -150.9(8) . . . . ? O1 C43 C44 C45 -154.8(8) 1 . . . ? O1 C43 C44 C45 -154.8(8) . . . . ? O2 C43 C44 C45 25.5(12) 1 . . . ? O2 C43 C44 C45 25.5(12) . . . . ? C46 C44 C45 C46 -0.1(15) . . . 3_668 ? C43 C44 C45 C46 -176.6(8) . . . 3_668 ? C45 C44 C46 C45 0.1(15) . . . 3_668 ? C43 C44 C46 C45 176.6(8) . . . 3_668 ? O3 C47 C48 C49 16.3(12) 1 . . . ? O3 C47 C48 C49 16.3(12) . . . . ? O4 C47 C48 C49 -164.0(8) 1 . . . ? O4 C47 C48 C49 -164.0(8) . . . . ? O3 C47 C48 C50 -164.1(8) 1 . . . ? O3 C47 C48 C50 -164.1(8) . . . . ? O4 C47 C48 C50 15.6(12) 1 . . . ? O4 C47 C48 C50 15.6(12) . . . . ? C50 C48 C49 C50 0.3(15) . . . 3_677 ? C47 C48 C49 C50 179.9(8) . . . 3_677 ? C49 C48 C50 C49 -0.3(15) . . . 3_677 ? C47 C48 C50 C49 -179.9(8) . . . 3_677 ? O2 C43 O1 O1 0.0(13) 1 . . 1 ? O2 C43 O1 O1 0.0(13) . . . 1 ? C44 C43 O1 O1 0.0(11) . . . 1 ? O1 C43 O2 O2 0.0(9) 1 . . 1 ? O1 C43 O2 O2 0.0(9) . . . 1 ? C44 C43 O2 O2 0.0(8) . . . 1 ? O4 C47 O3 O3 0.0(6) 1 . . 1 ? O4 C47 O3 O3 0.0(6) . . . 1 ? C48 C47 O3 O3 0.0(6) . . . 1 ? O3 C47 O4 O4 0.0(7) 1 . . 1 ? O3 C47 O4 O4 0.0(7) . . . 1 ? C48 C47 O4 O4 0.0(10) . . . 1 ? N4 C13 N1 C1 -1.2(7) . . . . ? C14 C13 N1 C1 178.1(6) . . . . ? N4 C13 N1 Ni1 -176.4(4) . . . . ? C14 C13 N1 Ni1 2.8(7) . . . . ? C2 C1 N1 C13 -177.8(8) . . . . ? C6 C1 N1 C13 0.9(7) . . . . ? C2 C1 N1 Ni1 -5.5(14) . . . . ? C6 C1 N1 Ni1 173.2(5) . . . . ? N9 Ni1 N1 C13 -99.4(4) . . . . ? N6 Ni1 N1 C13 84.9(4) . . . . ? N10 Ni1 N1 C13 -178.3(4) . . . . ? N5 Ni1 N1 C13 37.4(12) . . . . ? N2 Ni1 N1 C13 -4.1(4) . . . . ? N9 Ni1 N1 C1 88.4(8) . . . . ? N6 Ni1 N1 C1 -87.2(8) . . . . ? N10 Ni1 N1 C1 9.6(8) . . . . ? N5 Ni1 N1 C1 -134.7(10) . . . . ? N2 Ni1 N1 C1 -176.3(8) . . . . ? N3 C14 N2 C7 0.5(7) . . . . ? C13 C14 N2 C7 -179.1(6) . . . . ? N3 C14 N2 Ni1 174.2(4) . . . . ? C13 C14 N2 Ni1 -5.3(7) . . . . ? C12 C7 N2 C14 -0.3(8) . . . . ? C8 C7 N2 C14 -179.3(8) . . . . ? C12 C7 N2 Ni1 -170.7(6) . . . . ? C8 C7 N2 Ni1 10.3(13) . . . . ? N9 Ni1 N2 C14 96.4(4) . . . . ? N6 Ni1 N2 C14 -88.1(4) . . . . ? N10 Ni1 N2 C14 33.1(12) . . . . ? N5 Ni1 N2 C14 -167.7(4) . . . . ? N1 Ni1 N2 C14 5.0(4) . . . . ? N9 Ni1 N2 C7 -93.6(7) . . . . ? N6 Ni1 N2 C7 81.9(7) . . . . ? N10 Ni1 N2 C7 -156.9(9) . . . . ? N5 Ni1 N2 C7 2.3(7) . . . . ? N1 Ni1 N2 C7 175.0(7) . . . . ? N2 C14 N3 C12 -0.4(8) . . . . ? C13 C14 N3 C12 179.1(6) . . . . ? N2 C14 N3 O4 -174.9(5) . . . 1 ? C13 C14 N3 O4 4.6(11) . . . 1 ? C11 C12 N3 C14 -178.6(9) . . . . ? C7 C12 N3 C14 0.2(8) . . . . ? C11 C12 N3 O4 -2.7(12) . . . 1 ? C7 C12 N3 O4 176.1(5) . . . 1 ? N1 C13 N4 C6 0.9(8) . . . . ? C14 C13 N4 C6 -178.2(6) . . . . ? N1 C13 N4 O3 171.6(4) . . . 1 ? C14 C13 N4 O3 -7.5(10) . . . 1 ? C1 C6 N4 C13 -0.3(8) . . . . ? C5 C6 N4 C13 178.2(8) . . . . ? C1 C6 N4 O3 -171.4(5) . . . 1 ? C5 C6 N4 O3 7.1(11) . . . 1 ? N8 C27 N5 C15 0.8(7) . . . . ? C28 C27 N5 C15 -179.7(6) . . . . ? N8 C27 N5 Ni1 -167.2(4) . . . . ? C28 C27 N5 Ni1 12.3(7) . . . . ? C16 C15 N5 C27 179.3(7) . . . . ? C20 C15 N5 C27 -1.2(7) . . . . ? C16 C15 N5 Ni1 -19.3(12) . . . . ? C20 C15 N5 Ni1 160.2(5) . . . . ? N9 Ni1 N5 C27 175.1(4) . . . . ? N6 Ni1 N5 C27 -10.1(4) . . . . ? N10 Ni1 N5 C27 -105.4(4) . . . . ? N2 Ni1 N5 C27 79.1(4) . . . . ? N1 Ni1 N5 C27 38.4(12) . . . . ? N9 Ni1 N5 C15 14.2(7) . . . . ? N6 Ni1 N5 C15 -171.0(7) . . . . ? N10 Ni1 N5 C15 93.7(7) . . . . ? N2 Ni1 N5 C15 -81.8(7) . . . . ? N1 Ni1 N5 C15 -122.5(11) . . . . ? N7 C28 N6 C21 0.5(8) . . . . ? C27 C28 N6 C21 179.9(6) . . . . ? N7 C28 N6 Ni1 178.2(4) . . . . ? C27 C28 N6 Ni1 -2.4(7) . . . . ? C22 C21 N6 C28 180.0(7) . . . . ? C26 C21 N6 C28 0.0(7) . . . . ? C22 C21 N6 Ni1 3.4(13) . . . . ? C26 C21 N6 Ni1 -176.6(6) . . . . ? N9 Ni1 N6 C28 54.0(19) . . . . ? N10 Ni1 N6 C28 104.5(5) . . . . ? N5 Ni1 N6 C28 6.6(4) . . . . ? N2 Ni1 N6 C28 -86.2(5) . . . . ? N1 Ni1 N6 C28 -165.0(5) . . . . ? N9 Ni1 N6 C21 -129.6(16) . . . . ? N10 Ni1 N6 C21 -79.0(7) . . . . ? N5 Ni1 N6 C21 -176.9(7) . . . . ? N2 Ni1 N6 C21 90.2(7) . . . . ? N1 Ni1 N6 C21 11.4(7) . . . . ? N6 C28 N7 C26 -0.8(8) . . . . ? C27 C28 N7 C26 179.9(7) . . . . ? N6 C28 N7 O2 174.2(5) . . . 1 ? C27 C28 N7 O2 -5.1(11) . . . 1 ? C25 C26 N7 C28 -179.3(9) . . . . ? C21 C26 N7 C28 0.7(8) . . . . ? C25 C26 N7 O2 5.1(12) . . . 1 ? C21 C26 N7 O2 -174.9(5) . . . 1 ? N5 C27 N8 C20 -0.1(7) . . . . ? C28 C27 N8 C20 -179.5(6) . . . . ? N5 C27 N8 O1 174.5(4) . . . 1 ? C28 C27 N8 O1 -5.0(9) . . . 1 ? C19 C20 N8 C27 179.6(7) . . . . ? C15 C20 N8 C27 -0.7(7) . . . . ? C19 C20 N8 O1 4.9(11) . . . 1 ? C15 C20 N8 O1 -175.4(4) . . . 1 ? N11 C41 N9 C29 -0.8(8) . . . . ? C42 C41 N9 C29 176.1(6) . . . . ? N11 C41 N9 Ni1 176.1(4) . . . . ? C42 C41 N9 Ni1 -6.9(7) . . . . ? C30 C29 N9 C41 -175.8(8) . . . . ? C34 C29 N9 C41 0.4(8) . . . . ? C30 C29 N9 Ni1 8.8(13) . . . . ? C34 C29 N9 Ni1 -175.1(6) . . . . ? N6 Ni1 N9 C41 62.6(19) . . . . ? N10 Ni1 N9 C41 11.1(4) . . . . ? N5 Ni1 N9 C41 109.2(4) . . . . ? N2 Ni1 N9 C41 -157.5(4) . . . . ? N1 Ni1 N9 C41 -78.4(5) . . . . ? N6 Ni1 N9 C29 -122.1(17) . . . . ? N10 Ni1 N9 C29 -173.6(7) . . . . ? N5 Ni1 N9 C29 -75.5(7) . . . . ? N2 Ni1 N9 C29 17.8(7) . . . . ? N1 Ni1 N9 C29 96.9(7) . . . . ? N12 C42 N10 C35 1.6(8) . . . . ? C41 C42 N10 C35 -179.8(6) . . . . ? N12 C42 N10 Ni1 -163.9(5) . . . . ? C41 C42 N10 Ni1 14.8(7) . . . . ? C40 C35 N10 C42 -1.5(8) . . . . ? C36 C35 N10 C42 -177.9(8) . . . . ? C40 C35 N10 Ni1 156.5(6) . . . . ? C36 C35 N10 Ni1 -19.9(12) . . . . ? N9 Ni1 N10 C42 -13.9(5) . . . . ? N6 Ni1 N10 C42 171.5(5) . . . . ? N5 Ni1 N10 C42 -107.9(5) . . . . ? N2 Ni1 N10 C42 51.1(12) . . . . ? N1 Ni1 N10 C42 78.6(5) . . . . ? N9 Ni1 N10 C35 -171.0(7) . . . . ? N6 Ni1 N10 C35 14.5(7) . . . . ? N5 Ni1 N10 C35 95.0(7) . . . . ? N2 Ni1 N10 C35 -106.0(11) . . . . ? N1 Ni1 N10 C35 -78.5(7) . . . . ? N9 C41 N11 C34 0.9(8) . . . . ? C42 C41 N11 C34 -175.5(7) . . . . ? C29 C34 N11 C41 -0.6(8) . . . . ? C33 C34 N11 C41 177.7(9) . . . . ? N10 C42 N12 C40 -1.0(8) . . . . ? C41 C42 N12 C40 -179.5(7) . . . . ? N10 C42 N12 O4 155.2(5) . . . 4_575 ? C41 C42 N12 O4 -23.2(12) . . . 4_575 ? C39 C40 N12 C42 177.2(9) . . . . ? C35 C40 N12 C42 0.0(8) . . . . ? C39 C40 N12 O4 14.4(11) . . . 4_575 ? C35 C40 N12 O4 -162.8(5) . . . 4_575 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3B O4 0.86 2.02 2.857(8) 162.9 1 N4 H4B O3 0.86 1.78 2.632(8) 168.9 1 N7 H7A O2 0.86 1.80 2.648(7) 170.4 1 N8 H8B O1 0.86 1.88 2.737(7) 173.5 1 N12 H12A O4 0.86 2.13 2.913(9) 151.4 4_575 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.788 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.083