Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 --------------------------------------------------------------------- data_global _audit_creation_method SHELXL-97 _journal_coden_Cambridge 186 loop_ _publ_author_name 'Huang, Jian-Quan' 'Lin, Shen' 'Lin, Chi-Chang' 'Liu, Shi-Xiong' # SUBMISSIOPN DETAILS _publ_contact_author_name 'Professor Shi-Xiong Liu' _publ_contact_author_address ; Chemistry Fuzhou University 523 GongYe Road, Fuzhou Fuzhou Fujian 350002 CHINA ; _publ_contact_author_email sxliu@fzu.edu.cn _publ_contact_author_fax '86 591 3729860' _publ_contact_author_phone '86 591 3729860' _publ_requested_journal 'J.Chem.Soc.Dalton Trans.' _publ_section_title ; Four novel nanometer-sized cobalt azametallacrown complexes ; data_1 #C74 H114 Co6 N12 O34 _database_code_CSD 172706 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C74 H114 Co6 N12 O34 _chemical_formula_sum ? _chemical_formula_weight 2069.35 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7567(7) _cell_length_b 14.4971(8) _cell_length_c 16.4840(9) _cell_angle_alpha 65.149(1) _cell_angle_beta 73.935(1) _cell_angle_gamma 74.937(1) _cell_volume 2416.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1076 _exptl_absorpt_coefficient_mu 1.089 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART 1000 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12760 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.1309 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.04 _reflns_number_total 8419 _reflns_number_gt 4419 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL/PC (Sheldrick, 1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8419 _refine_ls_number_parameters 555 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1773 _refine_ls_R_factor_gt 0.0899 _refine_ls_wR_factor_ref 0.2559 _refine_ls_wR_factor_gt 0.2047 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max 0.056 _refine_ls_shift/su_mean 0.005 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 0.17832(10) 0.60634(9) 0.21358(8) 0.0472(4) Uani 1 1 d . . . Co2 Co 0.22838(10) 0.26972(9) 0.38858(8) 0.0438(4) Uani 1 1 d . . . Co3 Co 0.13530(10) 0.18782(9) 0.69008(8) 0.0470(4) Uani 1 1 d . . . N1 N 0.0306(6) 0.6867(5) 0.2323(5) 0.0448(18) Uani 1 1 d . . . N2 N 0.0166(6) 0.7239(5) 0.3031(5) 0.0439(18) Uani 1 1 d . . . N3 N 0.2513(6) 0.4044(5) 0.3149(5) 0.0430(17) Uani 1 1 d . . . N4 N 0.1412(6) 0.4748(5) 0.2998(5) 0.0406(17) Uani 1 1 d . . . N5 N 0.1548(6) 0.1937(5) 0.5736(5) 0.0444(18) Uani 1 1 d . . . N6 N 0.2095(6) 0.2782(5) 0.5049(5) 0.0417(17) Uani 1 1 d . . . O1 O 0.1446(5) 0.5817(5) 0.1210(4) 0.0557(16) Uani 1 1 d . . . O2 O -0.1321(5) 0.8067(4) 0.1956(4) 0.0523(16) Uani 1 1 d . . . O3 O 0.2068(5) 0.6378(4) 0.3060(4) 0.0492(15) Uani 1 1 d . . . O4 O 0.2416(6) 0.7322(5) 0.1241(5) 0.0678(19) Uani 1 1 d . . . O5 O 0.3920(5) 0.2184(4) 0.3853(4) 0.0530(16) Uani 1 1 d . . . O6 O 0.3372(5) 0.5322(4) 0.1987(4) 0.0542(16) Uani 1 1 d . . . O7 O 0.0641(5) 0.3275(4) 0.3872(4) 0.0470(15) Uani 1 1 d . . . O8 O 0.2348(5) 0.2455(5) 0.2791(4) 0.0579(17) Uani 1 1 d . . . O9 O 0.0584(5) 0.0721(4) 0.7456(4) 0.0576(17) Uani 1 1 d . . . O10 O 0.1889(5) 0.1360(4) 0.4600(4) 0.0491(15) Uani 1 1 d . . . O11 O 0.2151(5) 0.3036(4) 0.6293(4) 0.0489(15) Uani 1 1 d . . . O12 O 0.2931(6) 0.1000(5) 0.6983(5) 0.071(2) Uani 1 1 d . . . C1 C 0.0513(9) 0.6331(7) 0.0799(6) 0.050(2) Uani 1 1 d . . . C2 C -0.0398(8) 0.7084(7) 0.1019(6) 0.049(2) Uani 1 1 d . . . C3 C -0.1301(9) 0.7550(7) 0.0524(7) 0.059(3) Uani 1 1 d . . . H3A H -0.1890 0.8049 0.0679 0.071 Uiso 1 1 calc R . . C4 C -0.1382(10) 0.7324(8) -0.0181(7) 0.073(3) Uani 1 1 d . . . H4A H -0.2007 0.7656 -0.0500 0.088 Uiso 1 1 calc R . . C5 C -0.0488(11) 0.6573(8) -0.0403(7) 0.076(3) Uani 1 1 d . . . H5A H -0.0521 0.6395 -0.0876 0.091 Uiso 1 1 calc R . . C6 C 0.0443(10) 0.6092(8) 0.0064(7) 0.067(3) Uani 1 1 d . . . H6A H 0.1035 0.5604 -0.0105 0.080 Uiso 1 1 calc R . . C7 C -0.0476(8) 0.7363(6) 0.1784(6) 0.045(2) Uani 1 1 d . . . C8 C 0.1155(8) 0.6954(6) 0.3363(6) 0.045(2) Uani 1 1 d . . . C9 C 0.1253(8) 0.7282(8) 0.4098(7) 0.066(3) Uani 1 1 d . . . C10A C 0.248(4) 0.758(3) 0.394(3) 0.121(15) Uiso 0.45 1 d P . . C10B C 0.251(3) 0.711(3) 0.429(2) 0.060(9) Uiso 0.35 1 d P . . C10C C 0.201(5) 0.811(4) 0.369(4) 0.057(14) Uiso 0.20 1 d P . . C11 C 0.3043(14) 0.7423(10) 0.0311(9) 0.124(6) Uani 1 1 d . . . C12 C 0.4763(8) 0.2670(8) 0.3199(7) 0.055(3) Uani 1 1 d . . . C13 C 0.4604(8) 0.3711(7) 0.2573(6) 0.050(2) Uani 1 1 d . . . C14 C 0.5591(9) 0.4105(9) 0.1955(8) 0.076(3) Uani 1 1 d . . . H14A H 0.5494 0.4792 0.1562 0.091 Uiso 1 1 calc R . . C15 C 0.6735(9) 0.3501(11) 0.1902(9) 0.095(4) Uani 1 1 d . . . H15A H 0.7386 0.3784 0.1483 0.114 Uiso 1 1 calc R . . C16 C 0.6876(10) 0.2480(11) 0.2484(10) 0.099(4) Uani 1 1 d . . . H16A H 0.7627 0.2069 0.2457 0.119 Uiso 1 1 calc R . . C17 C 0.5911(9) 0.2073(9) 0.3101(8) 0.074(3) Uani 1 1 d . . . H17A H 0.6017 0.1376 0.3469 0.089 Uiso 1 1 calc R . . C18 C 0.3470(8) 0.4388(7) 0.2573(6) 0.045(2) Uani 1 1 d . . . C19 C 0.0502(8) 0.4257(6) 0.3380(6) 0.044(2) Uani 1 1 d . . . C20 C -0.0759(8) 0.4768(7) 0.3281(7) 0.063(3) Uani 1 1 d . . . H20A H -0.1232 0.4711 0.3879 0.076 Uiso 1 1 calc R . . H20B H -0.0758 0.5496 0.2916 0.076 Uiso 1 1 calc R . . C21 C -0.1341(14) 0.4354(12) 0.2867(15) 0.167(9) Uani 1 1 d . . . C22 C 0.2993(9) 0.1486(7) 0.2678(7) 0.071(3) Uani 1 1 d . . . C23 C 0.0601(8) 0.0100(7) 0.7034(7) 0.053(2) Uani 1 1 d . . . C24 C 0.1031(7) 0.0303(6) 0.6088(6) 0.047(2) Uani 1 1 d . . . C25 C 0.0955(8) -0.0419(7) 0.5749(7) 0.061(3) Uani 1 1 d . . . H25A H 0.1265 -0.0303 0.5137 0.073 Uiso 1 1 calc R . . C26 C 0.0445(9) -0.1287(8) 0.6281(8) 0.067(3) Uani 1 1 d . . . H26A H 0.0378 -0.1735 0.6033 0.081 Uiso 1 1 calc R . . C27 C 0.0042(10) -0.1469(7) 0.7182(9) 0.073(3) Uani 1 1 d . . . H27A H -0.0280 -0.2066 0.7554 0.088 Uiso 1 1 calc R . . C28 C 0.0089(8) -0.0805(7) 0.7569(7) 0.064(3) Uani 1 1 d . . . H28A H -0.0217 -0.0953 0.8186 0.077 Uiso 1 1 calc R . . C29 C 0.1520(7) 0.1224(6) 0.5441(7) 0.047(2) Uani 1 1 d . . . C30 C 0.2395(8) 0.3297(6) 0.5427(7) 0.047(2) Uani 1 1 d . . . C31 C 0.3047(10) 0.4188(8) 0.4873(7) 0.068(3) Uani 1 1 d . . . H31A H 0.2940 0.4447 0.4248 0.081 Uiso 1 1 calc R . . H31B H 0.2700 0.4736 0.5103 0.081 Uiso 1 1 calc R . . C32 C 0.4302(15) 0.3924(13) 0.4888(12) 0.169(8) Uani 1 1 d . . . H32A H 0.4816 0.4432 0.4528 0.11(4) Uiso 1 1 d R . . H32B H 0.4603 0.3345 0.4704 0.127 Uiso 1 1 d R . . H32C H 0.4380 0.3689 0.5511 0.127 Uiso 1 1 d R . . C33 C 0.3211(12) 0.0154(11) 0.7783(9) 0.111(5) Uani 1 1 d . . . O13 O 0.2499(6) 0.3955(5) 0.1208(4) 0.0702(19) Uani 1 1 d . . . C34 C 0.3574(11) 0.4012(10) 0.0501(8) 0.101(4) Uani 1 1 d . . . O14 O 0.4433(6) 0.0978(7) 0.5512(5) 0.095(3) Uani 1 1 d . . . C35 C 0.5668(11) 0.0883(12) 0.5524(9) 0.116(5) Uani 1 1 d . . . O15 O 0.1244(9) -0.0899(8) 0.1186(7) 0.128(3) Uiso 1 1 d . . . C36 C 0.060(3) -0.035(2) 0.036(2) 0.285(14) Uiso 1 1 d . . . O16 O 0.432(2) 0.3412(19) 0.7534(17) 0.320(10) Uiso 1 1 d . . . C37A C 0.419(3) 0.240(2) 0.749(2) 0.119(10) Uiso 0.50 1 d P . . C37B C 0.518(4) 0.289(4) 0.821(4) 0.209(19) Uiso 0.50 1 d P . . O17 O 0.601(5) 0.035(4) -0.137(4) 0.38(3) Uiso 0.50 1 d P . . O18 O 0.527(6) -0.112(5) 0.057(4) 0.46(3) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0489(7) 0.0368(7) 0.0467(8) -0.0115(6) -0.0048(6) -0.0036(6) Co2 0.0465(7) 0.0347(7) 0.0465(8) -0.0142(6) -0.0119(6) 0.0011(5) Co3 0.0522(8) 0.0351(7) 0.0475(8) -0.0124(6) -0.0125(6) 0.0010(6) N1 0.057(5) 0.036(4) 0.037(4) -0.011(4) -0.011(4) -0.003(4) N2 0.043(4) 0.031(4) 0.047(5) -0.009(4) -0.008(3) 0.001(3) N3 0.039(4) 0.043(4) 0.042(4) -0.015(4) -0.004(3) -0.005(3) N4 0.035(4) 0.023(3) 0.054(5) -0.011(3) -0.008(3) 0.003(3) N5 0.051(4) 0.033(4) 0.046(5) -0.012(4) -0.009(3) -0.007(3) N6 0.046(4) 0.030(4) 0.044(4) -0.011(4) -0.007(3) -0.005(3) O1 0.065(4) 0.048(4) 0.050(4) -0.022(3) -0.019(3) 0.012(3) O2 0.060(4) 0.040(3) 0.048(4) -0.013(3) -0.016(3) 0.008(3) O3 0.047(3) 0.041(3) 0.058(4) -0.016(3) -0.016(3) 0.000(3) O4 0.069(4) 0.052(4) 0.064(5) -0.011(4) 0.003(4) -0.015(3) O5 0.048(4) 0.046(4) 0.054(4) -0.018(3) -0.011(3) 0.009(3) O6 0.047(4) 0.040(4) 0.061(4) -0.010(3) -0.003(3) -0.006(3) O7 0.044(3) 0.038(3) 0.053(4) -0.013(3) -0.006(3) -0.006(3) O8 0.068(4) 0.057(4) 0.054(4) -0.031(4) -0.014(3) 0.001(3) O9 0.074(4) 0.039(3) 0.054(4) -0.020(3) 0.004(3) -0.015(3) O10 0.061(4) 0.033(3) 0.052(4) -0.018(3) -0.007(3) -0.007(3) O11 0.053(4) 0.042(3) 0.047(4) -0.012(3) -0.010(3) -0.007(3) O12 0.072(4) 0.053(4) 0.061(5) -0.008(4) -0.021(4) 0.020(3) C1 0.073(7) 0.036(5) 0.035(5) -0.001(4) -0.013(5) -0.015(5) C2 0.059(6) 0.040(5) 0.042(5) -0.010(5) -0.011(5) -0.004(5) C3 0.072(7) 0.050(6) 0.059(7) -0.022(5) -0.020(5) -0.005(5) C4 0.103(9) 0.056(7) 0.066(7) -0.019(6) -0.042(6) 0.000(6) C5 0.124(10) 0.065(7) 0.050(7) -0.019(6) -0.035(7) -0.021(7) C6 0.098(8) 0.054(6) 0.053(6) -0.024(6) -0.010(6) -0.017(6) C7 0.056(6) 0.035(5) 0.034(5) -0.006(4) -0.005(4) -0.007(4) C8 0.045(5) 0.037(5) 0.049(6) -0.015(4) -0.008(4) -0.004(4) C9 0.057(6) 0.080(8) 0.086(8) -0.050(7) -0.023(6) -0.009(6) C11 0.152(13) 0.084(9) 0.077(10) -0.016(8) 0.050(9) -0.027(9) C12 0.037(5) 0.076(7) 0.056(6) -0.037(6) -0.011(5) 0.006(5) C13 0.039(5) 0.056(6) 0.053(6) -0.016(5) -0.016(4) -0.001(5) C14 0.057(7) 0.068(7) 0.080(8) -0.013(7) -0.003(6) -0.008(6) C15 0.046(7) 0.113(11) 0.098(10) -0.031(9) 0.000(6) 0.003(7) C16 0.054(7) 0.100(11) 0.113(11) -0.035(9) -0.006(7) 0.019(7) C17 0.051(6) 0.072(7) 0.079(8) -0.023(7) -0.011(6) 0.013(6) C18 0.044(5) 0.040(5) 0.048(6) -0.019(5) -0.005(4) -0.002(4) C19 0.049(5) 0.030(5) 0.052(6) -0.018(5) -0.006(4) -0.003(4) C20 0.048(6) 0.038(5) 0.090(8) -0.017(6) -0.009(5) -0.003(4) C21 0.124(12) 0.115(12) 0.35(3) -0.129(16) -0.166(15) 0.040(9) C22 0.084(7) 0.050(6) 0.081(8) -0.040(6) -0.015(6) 0.015(5) C23 0.047(5) 0.035(5) 0.058(6) -0.006(5) -0.009(5) 0.002(4) C24 0.047(5) 0.032(5) 0.053(6) -0.011(5) -0.012(4) 0.001(4) C25 0.062(6) 0.045(6) 0.071(7) -0.015(6) -0.024(5) -0.003(5) C26 0.077(7) 0.046(6) 0.075(8) -0.010(6) -0.025(6) -0.013(5) C27 0.084(8) 0.036(6) 0.090(9) -0.006(6) -0.020(7) -0.021(5) C28 0.053(6) 0.039(5) 0.075(7) -0.006(5) 0.000(5) -0.005(5) C29 0.041(5) 0.033(5) 0.063(7) -0.016(5) -0.012(5) 0.000(4) C30 0.053(6) 0.033(5) 0.051(6) -0.007(5) -0.007(5) -0.016(4) C31 0.085(8) 0.068(7) 0.058(7) -0.022(6) -0.015(6) -0.027(6) C32 0.153(16) 0.155(16) 0.191(19) -0.017(15) -0.021(14) -0.107(15) C33 0.126(11) 0.100(10) 0.081(9) -0.026(8) -0.051(8) 0.042(9) O13 0.091(5) 0.059(4) 0.053(4) -0.018(4) -0.019(4) -0.001(4) C34 0.105(10) 0.094(10) 0.070(8) -0.022(8) 0.011(7) -0.005(8) O14 0.057(5) 0.126(7) 0.071(5) -0.031(5) -0.019(4) 0.030(4) C35 0.071(9) 0.160(14) 0.095(10) -0.033(10) -0.033(7) 0.009(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.850(7) . ? Co1 O1 1.866(6) . ? Co1 O3 1.894(6) . ? Co1 O6 1.905(6) . ? Co1 N4 1.912(6) . ? Co1 O4 1.973(6) . ? Co2 N3 1.860(7) . ? Co2 O5 1.868(6) . ? Co2 O7 1.898(5) . ? Co2 O10 1.899(6) . ? Co2 N6 1.921(7) . ? Co2 O8 1.957(6) . ? Co3 N5 1.838(7) . ? Co3 O9 1.874(6) . ? Co3 O11 1.893(6) . ? Co3 O2 1.908(6) 2_566 ? Co3 N2 1.914(7) 2_566 ? Co3 O12 1.962(6) . ? N1 C7 1.314(11) . ? N1 N2 1.432(9) . ? N2 C8 1.318(10) . ? N2 Co3 1.914(7) 2_566 ? N3 C18 1.311(10) . ? N3 N4 1.434(9) . ? N4 C19 1.302(10) . ? N5 C29 1.325(10) . ? N5 N6 1.427(9) . ? N6 C30 1.311(10) . ? O1 C1 1.333(10) . ? O2 C7 1.293(9) . ? O2 Co3 1.908(6) 2_566 ? O3 C8 1.298(9) . ? O4 C11 1.469(13) . ? O5 C12 1.332(10) . ? O6 C18 1.289(10) . ? O7 C19 1.301(9) . ? O8 C22 1.473(10) . ? O9 C23 1.343(10) . ? O10 C29 1.277(10) . ? O11 C30 1.280(10) . ? O12 C33 1.423(13) . ? C1 C2 1.407(12) . ? C1 C6 1.421(12) . ? C2 C3 1.375(12) . ? C2 C7 1.452(12) . ? C3 C4 1.366(13) . ? C3 H3A 0.9300 . ? C4 C5 1.397(14) . ? C4 H4A 0.9300 . ? C5 C6 1.377(14) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C8 C9 1.516(12) . ? C9 C10C 1.49(5) . ? C9 C10A 1.53(4) . ? C9 C10B 1.53(3) . ? C10A C10B 0.68(5) . ? C10A C10C 0.84(6) . ? C10B C10C 1.45(7) . ? C12 C17 1.409(12) . ? C12 C13 1.423(13) . ? C13 C14 1.383(12) . ? C13 C18 1.436(11) . ? C14 C15 1.403(14) . ? C14 H14A 0.9300 . ? C15 C16 1.380(16) . ? C15 H15A 0.9300 . ? C16 C17 1.369(14) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C19 C20 1.495(12) . ? C20 C21 1.453(15) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C23 C28 1.415(12) . ? C23 C24 1.426(12) . ? C24 C25 1.408(12) . ? C24 C29 1.454(12) . ? C25 C26 1.372(12) . ? C25 H25A 0.9300 . ? C26 C27 1.359(14) . ? C26 H26A 0.9300 . ? C27 C28 1.378(13) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C30 C31 1.492(12) . ? C31 C32 1.429(17) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9615 . ? C32 H32B 0.9599 . ? C32 H32C 0.9601 . ? O13 C34 1.456(12) . ? O14 C35 1.427(13) . ? O15 C36 1.55(3) . ? C36 C36 1.91(6) 2 ? O16 C37B 1.53(5) . ? O16 C37A 1.55(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 O1 94.2(3) . . ? N1 Co1 O3 83.1(3) . . ? O1 Co1 O3 177.0(3) . . ? N1 Co1 O6 173.7(3) . . ? O1 Co1 O6 91.3(3) . . ? O3 Co1 O6 91.3(3) . . ? N1 Co1 N4 99.2(3) . . ? O1 Co1 N4 90.7(3) . . ? O3 Co1 N4 91.1(3) . . ? O6 Co1 N4 83.7(3) . . ? N1 Co1 O4 88.9(3) . . ? O1 Co1 O4 90.8(3) . . ? O3 Co1 O4 87.8(3) . . ? O6 Co1 O4 87.9(3) . . ? N4 Co1 O4 171.5(3) . . ? N3 Co2 O5 94.3(3) . . ? N3 Co2 O7 83.1(3) . . ? O5 Co2 O7 177.3(3) . . ? N3 Co2 O10 173.9(3) . . ? O5 Co2 O10 91.3(3) . . ? O7 Co2 O10 91.2(2) . . ? N3 Co2 N6 98.5(3) . . ? O5 Co2 N6 91.5(3) . . ? O7 Co2 N6 89.6(3) . . ? O10 Co2 N6 83.7(3) . . ? N3 Co2 O8 88.8(3) . . ? O5 Co2 O8 91.2(3) . . ? O7 Co2 O8 88.1(2) . . ? O10 Co2 O8 88.8(3) . . ? N6 Co2 O8 172.1(3) . . ? N5 Co3 O9 95.1(3) . . ? N5 Co3 O11 82.5(3) . . ? O9 Co3 O11 177.5(3) . . ? N5 Co3 O2 172.0(3) . 2_566 ? O9 Co3 O2 92.5(3) . 2_566 ? O11 Co3 O2 89.9(3) . 2_566 ? N5 Co3 N2 99.0(3) . 2_566 ? O9 Co3 N2 90.3(3) . 2_566 ? O11 Co3 N2 90.7(3) . 2_566 ? O2 Co3 N2 83.5(3) 2_566 2_566 ? N5 Co3 O12 88.8(3) . . ? O9 Co3 O12 91.2(3) . . ? O11 Co3 O12 88.2(3) . . ? O2 Co3 O12 88.5(3) 2_566 . ? N2 Co3 O12 171.9(3) 2_566 . ? C7 N1 N2 114.0(7) . . ? C7 N1 Co1 130.0(6) . . ? N2 N1 Co1 113.3(5) . . ? C8 N2 N1 111.0(6) . . ? C8 N2 Co3 139.8(6) . 2_566 ? N1 N2 Co3 108.8(5) . 2_566 ? C18 N3 N4 114.4(7) . . ? C18 N3 Co2 129.6(6) . . ? N4 N3 Co2 113.3(5) . . ? C19 N4 N3 110.3(6) . . ? C19 N4 Co1 139.9(6) . . ? N3 N4 Co1 108.7(5) . . ? C29 N5 N6 113.6(7) . . ? C29 N5 Co3 130.4(6) . . ? N6 N5 Co3 114.1(5) . . ? C30 N6 N5 110.0(7) . . ? C30 N6 Co2 141.1(6) . . ? N5 N6 Co2 108.6(5) . . ? C1 O1 Co1 123.9(5) . . ? C7 O2 Co3 111.9(6) . 2_566 ? C8 O3 Co1 112.8(5) . . ? C11 O4 Co1 122.8(7) . . ? C12 O5 Co2 122.4(6) . . ? C18 O6 Co1 112.4(5) . . ? C19 O7 Co2 111.7(5) . . ? C22 O8 Co2 121.4(6) . . ? C23 O9 Co3 123.3(5) . . ? C29 O10 Co2 112.1(5) . . ? C30 O11 Co3 112.7(5) . . ? C33 O12 Co3 124.1(7) . . ? O1 C1 C2 126.6(8) . . ? O1 C1 C6 116.2(9) . . ? C2 C1 C6 117.2(9) . . ? C3 C2 C1 119.6(9) . . ? C3 C2 C7 117.3(8) . . ? C1 C2 C7 123.1(8) . . ? C4 C3 C2 123.9(9) . . ? C4 C3 H3A 118.1 . . ? C2 C3 H3A 118.1 . . ? C3 C4 C5 117.2(10) . . ? C3 C4 H4A 121.4 . . ? C5 C4 H4A 121.4 . . ? C6 C5 C4 121.2(10) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C1 121.0(10) . . ? C5 C6 H6A 119.5 . . ? C1 C6 H6A 119.5 . . ? O2 C7 N1 119.7(8) . . ? O2 C7 C2 121.1(8) . . ? N1 C7 C2 119.2(8) . . ? O3 C8 N2 119.7(8) . . ? O3 C8 C9 118.9(8) . . ? N2 C8 C9 121.3(8) . . ? C10C C9 C8 110(2) . . ? C10C C9 C10A 32(2) . . ? C8 C9 C10A 112.2(17) . . ? C10C C9 C10B 57(3) . . ? C8 C9 C10B 116.7(14) . . ? C10A C9 C10B 25.8(19) . . ? C10B C10A C10C 144(9) . . ? C10B C10A C9 77(5) . . ? C10C C10A C9 72(5) . . ? C10A C10B C10C 20(5) . . ? C10A C10B C9 77(5) . . ? C10C C10B C9 60(2) . . ? C10A C10C C10B 16(4) . . ? C10A C10C C9 76(5) . . ? C10B C10C C9 63(2) . . ? O5 C12 C17 116.0(9) . . ? O5 C12 C13 126.5(8) . . ? C17 C12 C13 117.5(9) . . ? C14 C13 C12 118.9(9) . . ? C14 C13 C18 118.0(9) . . ? C12 C13 C18 123.1(8) . . ? C13 C14 C15 122.1(11) . . ? C13 C14 H14A 118.9 . . ? C15 C14 H14A 118.9 . . ? C16 C15 C14 118.8(11) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C17 C16 C15 120.1(11) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C12 122.4(11) . . ? C16 C17 H17A 118.8 . . ? C12 C17 H17A 118.8 . . ? O6 C18 N3 119.5(8) . . ? O6 C18 C13 120.6(8) . . ? N3 C18 C13 119.9(8) . . ? O7 C19 N4 121.5(8) . . ? O7 C19 C20 115.6(7) . . ? N4 C19 C20 122.9(8) . . ? C21 C20 C19 115.1(9) . . ? C21 C20 H20A 108.5 . . ? C19 C20 H20A 108.5 . . ? C21 C20 H20B 108.5 . . ? C19 C20 H20B 108.5 . . ? H20A C20 H20B 107.5 . . ? O9 C23 C28 116.9(9) . . ? O9 C23 C24 125.5(8) . . ? C28 C23 C24 117.5(9) . . ? C25 C24 C23 118.3(8) . . ? C25 C24 C29 117.6(9) . . ? C23 C24 C29 124.1(8) . . ? C26 C25 C24 123.0(10) . . ? C26 C25 H25A 118.5 . . ? C24 C25 H25A 118.5 . . ? C27 C26 C25 117.8(10) . . ? C27 C26 H26A 121.1 . . ? C25 C26 H26A 121.1 . . ? C26 C27 C28 122.8(10) . . ? C26 C27 H27A 118.6 . . ? C28 C27 H27A 118.6 . . ? C27 C28 C23 120.5(10) . . ? C27 C28 H28A 119.7 . . ? C23 C28 H28A 119.7 . . ? O10 C29 N5 120.3(8) . . ? O10 C29 C24 120.9(8) . . ? N5 C29 C24 118.8(9) . . ? O11 C30 N6 120.6(7) . . ? O11 C30 C31 117.7(8) . . ? N6 C30 C31 121.7(8) . . ? C32 C31 C30 112.8(10) . . ? C32 C31 H31A 109.0 . . ? C30 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? C30 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 119.7 . . ? C31 C32 H32B 106.8 . . ? H32A C32 H32B 107.7 . . ? C31 C32 H32C 107.1 . . ? H32A C32 H32C 107.7 . . ? H32B C32 H32C 107.1 . . ? O15 C36 C36 162(3) . 2 ? C37B O16 C37A 95(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 Co1 N1 C7 -20.6(8) . . . . ? O3 Co1 N1 C7 158.1(8) . . . . ? O6 Co1 N1 C7 130(2) . . . . ? N4 Co1 N1 C7 -112.0(8) . . . . ? O4 Co1 N1 C7 70.2(8) . . . . ? O1 Co1 N1 N2 179.5(5) . . . . ? O3 Co1 N1 N2 -1.8(5) . . . . ? O6 Co1 N1 N2 -29(3) . . . . ? N4 Co1 N1 N2 88.1(5) . . . . ? O4 Co1 N1 N2 -89.7(5) . . . . ? C7 N1 N2 C8 -160.5(7) . . . . ? Co1 N1 N2 C8 2.7(8) . . . . ? C7 N1 N2 Co3 13.3(8) . . . 2_566 ? Co1 N1 N2 Co3 176.5(3) . . . 2_566 ? O5 Co2 N3 C18 21.0(8) . . . . ? O7 Co2 N3 C18 -158.3(8) . . . . ? O10 Co2 N3 C18 -136(2) . . . . ? N6 Co2 N3 C18 113.2(8) . . . . ? O8 Co2 N3 C18 -70.1(8) . . . . ? O5 Co2 N3 N4 -179.1(5) . . . . ? O7 Co2 N3 N4 1.6(5) . . . . ? O10 Co2 N3 N4 23(3) . . . . ? N6 Co2 N3 N4 -86.9(5) . . . . ? O8 Co2 N3 N4 89.8(5) . . . . ? C18 N3 N4 C19 159.5(7) . . . . ? Co2 N3 N4 C19 -3.5(8) . . . . ? C18 N3 N4 Co1 -11.0(8) . . . . ? Co2 N3 N4 Co1 -174.1(3) . . . . ? N1 Co1 N4 C19 29.3(9) . . . . ? O1 Co1 N4 C19 -65.1(9) . . . . ? O3 Co1 N4 C19 112.4(9) . . . . ? O6 Co1 N4 C19 -156.3(9) . . . . ? O4 Co1 N4 C19 -165.5(17) . . . . ? N1 Co1 N4 N3 -164.5(5) . . . . ? O1 Co1 N4 N3 101.1(5) . . . . ? O3 Co1 N4 N3 -81.3(5) . . . . ? O6 Co1 N4 N3 9.9(5) . . . . ? O4 Co1 N4 N3 1(2) . . . . ? O9 Co3 N5 C29 -19.3(8) . . . . ? O11 Co3 N5 C29 160.1(8) . . . . ? O2 Co3 N5 C29 141.9(18) 2_566 . . . ? N2 Co3 N5 C29 -110.4(8) 2_566 . . . ? O12 Co3 N5 C29 71.8(8) . . . . ? O9 Co3 N5 N6 177.9(5) . . . . ? O11 Co3 N5 N6 -2.7(5) . . . . ? O2 Co3 N5 N6 -21(2) 2_566 . . . ? N2 Co3 N5 N6 86.7(5) 2_566 . . . ? O12 Co3 N5 N6 -91.1(5) . . . . ? C29 N5 N6 C30 -162.4(7) . . . . ? Co3 N5 N6 C30 3.4(8) . . . . ? C29 N5 N6 Co2 12.1(8) . . . . ? Co3 N5 N6 Co2 177.9(3) . . . . ? N3 Co2 N6 C30 -25.9(10) . . . . ? O5 Co2 N6 C30 68.7(9) . . . . ? O7 Co2 N6 C30 -108.8(9) . . . . ? O10 Co2 N6 C30 159.9(9) . . . . ? O8 Co2 N6 C30 178.7(17) . . . . ? N3 Co2 N6 N5 162.4(5) . . . . ? O5 Co2 N6 N5 -103.0(5) . . . . ? O7 Co2 N6 N5 79.5(5) . . . . ? O10 Co2 N6 N5 -11.8(5) . . . . ? O8 Co2 N6 N5 7(2) . . . . ? N1 Co1 O1 C1 12.6(7) . . . . ? O3 Co1 O1 C1 -13(5) . . . . ? O6 Co1 O1 C1 -164.3(7) . . . . ? N4 Co1 O1 C1 111.9(7) . . . . ? O4 Co1 O1 C1 -76.4(7) . . . . ? N1 Co1 O3 C8 0.6(6) . . . . ? O1 Co1 O3 C8 27(5) . . . . ? O6 Co1 O3 C8 177.7(6) . . . . ? N4 Co1 O3 C8 -98.6(6) . . . . ? O4 Co1 O3 C8 89.8(6) . . . . ? N1 Co1 O4 C11 -127.4(10) . . . . ? O1 Co1 O4 C11 -33.2(10) . . . . ? O3 Co1 O4 C11 149.5(10) . . . . ? O6 Co1 O4 C11 58.1(10) . . . . ? N4 Co1 O4 C11 67(2) . . . . ? N3 Co2 O5 C12 -21.1(7) . . . . ? O7 Co2 O5 C12 -6(6) . . . . ? O10 Co2 O5 C12 156.6(6) . . . . ? N6 Co2 O5 C12 -119.7(6) . . . . ? O8 Co2 O5 C12 67.7(6) . . . . ? N1 Co1 O6 C18 111(3) . . . . ? O1 Co1 O6 C18 -98.3(6) . . . . ? O3 Co1 O6 C18 83.2(6) . . . . ? N4 Co1 O6 C18 -7.7(6) . . . . ? O4 Co1 O6 C18 170.9(6) . . . . ? N3 Co2 O7 C19 0.6(6) . . . . ? O5 Co2 O7 C19 -15(6) . . . . ? O10 Co2 O7 C19 -177.1(6) . . . . ? N6 Co2 O7 C19 99.2(6) . . . . ? O8 Co2 O7 C19 -88.4(6) . . . . ? N3 Co2 O8 C22 138.8(7) . . . . ? O5 Co2 O8 C22 44.5(7) . . . . ? O7 Co2 O8 C22 -138.1(7) . . . . ? O10 Co2 O8 C22 -46.8(7) . . . . ? N6 Co2 O8 C22 -65(2) . . . . ? N5 Co3 O9 C23 15.9(7) . . . . ? O11 Co3 O9 C23 2(7) . . . . ? O2 Co3 O9 C23 -161.5(7) 2_566 . . . ? N2 Co3 O9 C23 115.0(7) 2_566 . . . ? O12 Co3 O9 C23 -73.0(7) . . . . ? N3 Co2 O10 C29 -101(3) . . . . ? O5 Co2 O10 C29 101.5(6) . . . . ? O7 Co2 O10 C29 -79.3(6) . . . . ? N6 Co2 O10 C29 10.1(6) . . . . ? O8 Co2 O10 C29 -167.3(6) . . . . ? N5 Co3 O11 C30 1.6(6) . . . . ? O9 Co3 O11 C30 16(6) . . . . ? O2 Co3 O11 C30 179.1(6) 2_566 . . . ? N2 Co3 O11 C30 -97.4(6) 2_566 . . . ? O12 Co3 O11 C30 90.6(6) . . . . ? N5 Co3 O12 C33 -142.4(9) . . . . ? O9 Co3 O12 C33 -47.4(9) . . . . ? O11 Co3 O12 C33 135.0(9) . . . . ? O2 Co3 O12 C33 45.1(9) 2_566 . . . ? N2 Co3 O12 C33 53(2) 2_566 . . . ? Co1 O1 C1 C2 -4.1(13) . . . . ? Co1 O1 C1 C6 175.6(6) . . . . ? O1 C1 C2 C3 179.6(8) . . . . ? C6 C1 C2 C3 -0.1(13) . . . . ? O1 C1 C2 C7 -3.8(14) . . . . ? C6 C1 C2 C7 176.5(8) . . . . ? C1 C2 C3 C4 0.4(15) . . . . ? C7 C2 C3 C4 -176.3(9) . . . . ? C2 C3 C4 C5 -0.1(16) . . . . ? C3 C4 C5 C6 -0.7(16) . . . . ? C4 C5 C6 C1 1.1(17) . . . . ? O1 C1 C6 C5 179.6(9) . . . . ? C2 C1 C6 C5 -0.7(14) . . . . ? Co3 O2 C7 N1 -7.1(10) 2_566 . . . ? Co3 O2 C7 C2 170.8(6) 2_566 . . . ? N2 N1 C7 O2 -4.3(11) . . . . ? Co1 N1 C7 O2 -164.1(6) . . . . ? N2 N1 C7 C2 177.7(7) . . . . ? Co1 N1 C7 C2 17.9(12) . . . . ? C3 C2 C7 O2 -4.1(13) . . . . ? C1 C2 C7 O2 179.3(8) . . . . ? C3 C2 C7 N1 173.8(8) . . . . ? C1 C2 C7 N1 -2.8(13) . . . . ? Co1 O3 C8 N2 0.9(10) . . . . ? Co1 O3 C8 C9 -179.2(6) . . . . ? N1 N2 C8 O3 -2.4(11) . . . . ? Co3 N2 C8 O3 -173.2(6) 2_566 . . . ? N1 N2 C8 C9 177.8(7) . . . . ? Co3 N2 C8 C9 6.9(14) 2_566 . . . ? O3 C8 C9 C10C 75(2) . . . . ? N2 C8 C9 C10C -105(2) . . . . ? O3 C8 C9 C10A 41(2) . . . . ? N2 C8 C9 C10A -139(2) . . . . ? O3 C8 C9 C10B 13(2) . . . . ? N2 C8 C9 C10B -167.4(17) . . . . ? C10C C9 C10A C10B 162(9) . . . . ? C8 C9 C10A C10B -106(5) . . . . ? C8 C9 C10A C10C 92(5) . . . . ? C10B C9 C10A C10C -162(9) . . . . ? C9 C10A C10B C10C -29(15) . . . . ? C10C C10A C10B C9 29(15) . . . . ? C10C C9 C10B C10A -11(6) . . . . ? C8 C9 C10B C10A 86(5) . . . . ? C8 C9 C10B C10C 97(2) . . . . ? C10A C9 C10B C10C 11(6) . . . . ? C9 C10A C10C C10B 30(15) . . . . ? C10B C10A C10C C9 -30(15) . . . . ? C9 C10B C10C C10A -147(17) . . . . ? C10A C10B C10C C9 147(17) . . . . ? C8 C9 C10C C10A -101(5) . . . . ? C10B C9 C10C C10A 9(5) . . . . ? C8 C9 C10C C10B -109.8(19) . . . . ? C10A C9 C10C C10B -9(5) . . . . ? Co2 O5 C12 C17 -162.0(7) . . . . ? Co2 O5 C12 C13 15.3(12) . . . . ? O5 C12 C13 C14 177.7(9) . . . . ? C17 C12 C13 C14 -5.1(14) . . . . ? O5 C12 C13 C18 0.0(15) . . . . ? C17 C12 C13 C18 177.2(9) . . . . ? C12 C13 C14 C15 2.4(16) . . . . ? C18 C13 C14 C15 -179.8(10) . . . . ? C13 C14 C15 C16 0.3(19) . . . . ? C14 C15 C16 C17 0(2) . . . . ? C15 C16 C17 C12 -3(2) . . . . ? O5 C12 C17 C16 -177.1(10) . . . . ? C13 C12 C17 C16 5.4(16) . . . . ? Co1 O6 C18 N3 3.4(10) . . . . ? Co1 O6 C18 C13 -179.5(6) . . . . ? N4 N3 C18 O6 5.3(11) . . . . ? Co2 N3 C18 O6 165.0(6) . . . . ? N4 N3 C18 C13 -171.8(7) . . . . ? Co2 N3 C18 C13 -12.1(12) . . . . ? C14 C13 C18 O6 2.9(13) . . . . ? C12 C13 C18 O6 -179.4(8) . . . . ? C14 C13 C18 N3 -180.0(9) . . . . ? C12 C13 C18 N3 -2.3(13) . . . . ? Co2 O7 C19 N4 -3.1(10) . . . . ? Co2 O7 C19 C20 176.4(6) . . . . ? N3 N4 C19 O7 4.4(11) . . . . ? Co1 N4 C19 O7 170.5(6) . . . . ? N3 N4 C19 C20 -175.1(7) . . . . ? Co1 N4 C19 C20 -9.0(14) . . . . ? O7 C19 C20 C21 -59.5(15) . . . . ? N4 C19 C20 C21 119.9(13) . . . . ? Co3 O9 C23 C28 173.5(6) . . . . ? Co3 O9 C23 C24 -10.1(12) . . . . ? O9 C23 C24 C25 -178.3(8) . . . . ? C28 C23 C24 C25 -1.9(12) . . . . ? O9 C23 C24 C29 0.2(14) . . . . ? C28 C23 C24 C29 176.6(8) . . . . ? C23 C24 C25 C26 2.5(14) . . . . ? C29 C24 C25 C26 -176.0(9) . . . . ? C24 C25 C26 C27 -2.7(15) . . . . ? C25 C26 C27 C28 2.2(16) . . . . ? C26 C27 C28 C23 -1.7(16) . . . . ? O9 C23 C28 C27 178.2(9) . . . . ? C24 C23 C28 C27 1.5(13) . . . . ? Co2 O10 C29 N5 -5.9(10) . . . . ? Co2 O10 C29 C24 172.3(6) . . . . ? N6 N5 C29 O10 -4.4(11) . . . . ? Co3 N5 C29 O10 -167.3(6) . . . . ? N6 N5 C29 C24 177.4(7) . . . . ? Co3 N5 C29 C24 14.4(12) . . . . ? C25 C24 C29 O10 -1.4(12) . . . . ? C23 C24 C29 O10 -179.9(8) . . . . ? C25 C24 C29 N5 176.8(8) . . . . ? C23 C24 C29 N5 -1.7(13) . . . . ? Co3 O11 C30 N6 0.0(10) . . . . ? Co3 O11 C30 C31 -178.8(7) . . . . ? N5 N6 C30 O11 -2.2(11) . . . . ? Co2 N6 C30 O11 -173.8(6) . . . . ? N5 N6 C30 C31 176.6(8) . . . . ? Co2 N6 C30 C31 4.9(15) . . . . ? O11 C30 C31 C32 77.7(13) . . . . ? N6 C30 C31 C32 -101.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.893 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.107 data_2 #C66 H90 Co6 N12 O30 _database_code_CSD 157264 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H90 Co6 N12 O30' _chemical_formula_sum 'C66 H90 Co6 N12 O30' _chemical_formula_weight 1885.08 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' '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)/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 13.2649(15) _cell_length_b 19.2794(18) _cell_length_c 16.2663(16) _cell_angle_alpha 90.00 _cell_angle_beta 108.264(3) _cell_angle_gamma 90.00 _cell_volume 3950.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.374 _exptl_crystal_size_mid 0.319 _exptl_crystal_size_min 0.268 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.321 _exptl_absorpt_correction_type psi _exptl_absorpt_correction_T_min 0.6836 _exptl_absorpt_correction_T_max 0.9988 _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 Rigaku Weissenberg _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8944 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8944 _reflns_number_gt 5776 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8944 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1532 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 0.71831(4) 0.16238(3) 0.13305(3) 0.03222(14) Uani 1 1 d . . . Co2 Co 0.47247(4) 0.08248(3) 0.24481(3) 0.03352(14) Uani 1 1 d . . . Co3 Co 0.32983(4) -0.12419(3) 0.14807(3) 0.03404(14) Uani 1 1 d . . . O1 O 0.6816(2) 0.25414(14) 0.14780(18) 0.0405(6) Uani 1 1 d . . . O2 O 0.6748(2) 0.21946(15) -0.11355(17) 0.0415(7) Uani 1 1 d . . . O3 O 0.7548(2) 0.07053(14) 0.11211(17) 0.0367(6) Uani 1 1 d . . . O4 O 0.8613(2) 0.19298(19) 0.1429(2) 0.0542(9) Uani 1 1 d . . . H04 H 0.8895 0.1837 0.0940 0.09(2) Uiso 1 1 d R . . O5 O 0.5410(2) 0.05011(17) 0.35694(17) 0.0452(7) Uani 1 1 d . . . O6 O 0.7647(2) 0.14694(15) 0.25423(16) 0.0366(6) Uani 1 1 d . . . O7 O 0.4121(2) 0.11760(15) 0.13092(17) 0.0370(6) Uani 1 1 d . . . O8 O 0.4638(3) 0.17662(17) 0.2882(2) 0.0517(8) Uani 1 1 d . . . H08 H 0.5375 0.2056 0.2934 0.076(17) Uiso 1 1 d R . . O9 O 0.1851(2) -0.12239(15) 0.13757(19) 0.0438(7) Uani 1 1 d . . . O10 O 0.3357(2) 0.06533(15) 0.25514(19) 0.0411(7) Uani 1 1 d . . . O11 O 0.4780(2) -0.12094(14) 0.16358(17) 0.0376(6) Uani 1 1 d . . . O12 O 0.3614(3) -0.15420(17) 0.26719(19) 0.0548(8) Uani 1 1 d . . . H012 H 0.3923 -0.1203 0.3192 0.12(3) Uiso 1 1 d R . . N1 N 0.6846(2) 0.17003(16) 0.0142(2) 0.0323(7) Uani 1 1 d . . . N2 N 0.6998(2) 0.10796(16) -0.0272(2) 0.0331(7) Uani 1 1 d . . . N3 N 0.5982(2) 0.10578(17) 0.22550(19) 0.0335(7) Uani 1 1 d . . . N4 N 0.5847(2) 0.13178(17) 0.14079(19) 0.0333(7) Uani 1 1 d . . . N5 N 0.3529(2) -0.03341(17) 0.1863(2) 0.0329(7) Uani 1 1 d . . . N6 N 0.4576(2) -0.00965(17) 0.1999(2) 0.0339(7) Uani 1 1 d . . . C1 C 0.6615(3) 0.3035(2) 0.0867(3) 0.0367(8) Uani 1 1 d . . . C2 C 0.6590(3) 0.2929(2) 0.0002(3) 0.0370(9) Uani 1 1 d . . . C3 C 0.6385(4) 0.3496(2) -0.0565(3) 0.0479(11) Uani 1 1 d . . . H3A H 0.6365 0.3428 -0.1135 0.058 Uiso 1 1 calc R . . C4 C 0.6214(4) 0.4151(2) -0.0301(3) 0.0574(13) Uani 1 1 d . . . H4A H 0.6090 0.4523 -0.0684 0.069 Uiso 1 1 calc R . . C5 C 0.6229(4) 0.4245(2) 0.0552(3) 0.0554(12) Uani 1 1 d . . . H5A H 0.6100 0.4683 0.0737 0.067 Uiso 1 1 calc R . . C6 C 0.6430(4) 0.3701(2) 0.1120(3) 0.0484(10) Uani 1 1 d . . . H6A H 0.6445 0.3778 0.1688 0.058 Uiso 1 1 calc R . . C7 C 0.6749(3) 0.2253(2) -0.0349(2) 0.0340(8) Uani 1 1 d . . . C8 C 0.7390(3) 0.0592(2) 0.0297(2) 0.0336(8) Uani 1 1 d . . . C9 C 0.7662(4) -0.0106(2) 0.0049(3) 0.0484(11) Uani 1 1 d . . . H9A H 0.6981 -0.0344 -0.0262 0.081(19) Uiso 1 1 d R . . H9B H 0.8044 -0.0366 0.0555 0.097 Uiso 1 1 d R . . H9C H 0.8099 -0.0067 -0.0320 0.097 Uiso 1 1 d R . . C10 C 0.9310(5) 0.2257(3) 0.2144(4) 0.0764(18) Uani 1 1 d . . . H10A H 1.0003 0.2267 0.2048 0.078(18) Uiso 1 1 d R . . H10B H 0.9354 0.2006 0.2664 0.094 Uiso 1 1 d R . . H10C H 0.9071 0.2720 0.2197 0.094 Uiso 1 1 d R . . C11 C 0.6382(3) 0.0708(2) 0.4043(2) 0.0400(9) Uani 1 1 d . . . C12 C 0.7141(3) 0.1011(2) 0.3721(2) 0.0359(8) Uani 1 1 d . . . C13 C 0.8144(3) 0.1189(2) 0.4299(3) 0.0453(10) Uani 1 1 d . . . H13A H 0.8651 0.1384 0.4083 0.054 Uiso 1 1 calc R . . C14 C 0.8386(4) 0.1082(3) 0.5172(3) 0.0545(12) Uani 1 1 d . . . H14A H 0.9048 0.1208 0.5546 0.065 Uiso 1 1 calc R . . C15 C 0.7638(4) 0.0787(3) 0.5491(3) 0.0558(13) Uani 1 1 d . . . H15A H 0.7799 0.0712 0.6083 0.067 Uiso 1 1 calc R . . C16 C 0.6666(4) 0.0603(3) 0.4948(3) 0.0502(11) Uani 1 1 d . . . H16A H 0.6176 0.0403 0.5179 0.060 Uiso 1 1 calc R . . C17 C 0.6926(3) 0.1184(2) 0.2804(2) 0.0334(8) Uani 1 1 d . . . C18 C 0.4830(3) 0.1379(2) 0.0980(2) 0.0357(8) Uani 1 1 d . . . C19 C 0.4463(3) 0.1689(3) 0.0094(3) 0.0540(12) Uani 1 1 d . . . H19A H 0.3734 0.1620 -0.0158 0.076(18) Uiso 1 1 d R . . H19B H 0.4836 0.1480 -0.0262 0.091 Uiso 1 1 d R . . H19C H 0.4615 0.2177 0.0132 0.091 Uiso 1 1 d R . . C20 C 0.4326(5) 0.1911(3) 0.3613(4) 0.0763(18) Uani 1 1 d . . . H20A H 0.3686 0.1678 0.3504 0.13(3) Uiso 1 1 d R . . H20B H 0.4235 0.2400 0.3676 0.154 Uiso 1 1 d R . . H20C H 0.4840 0.1739 0.4130 0.154 Uiso 1 1 d R . . C21 C 0.1411(3) -0.0759(2) 0.1768(2) 0.0382(9) Uani 1 1 d . . . C22 C 0.1879(3) -0.0124(2) 0.2136(2) 0.0373(9) Uani 1 1 d . . . C23 C 0.1296(3) 0.0334(2) 0.2484(3) 0.0431(10) Uani 1 1 d . . . H23A H 0.1606 0.0751 0.2724 0.052 Uiso 1 1 calc R . . C24 C 0.0281(3) 0.0186(3) 0.2479(3) 0.0513(12) Uani 1 1 d . . . H24A H -0.0103 0.0506 0.2688 0.062 Uiso 1 1 calc R . . C25 C -0.0159(4) -0.0447(3) 0.2158(3) 0.0540(12) Uani 1 1 d . . . H25A H -0.0830 -0.0564 0.2179 0.065 Uiso 1 1 calc R . . C26 C 0.0389(3) -0.0906(3) 0.1806(3) 0.0497(11) Uani 1 1 d . . . H26A H 0.0074 -0.1326 0.1588 0.060 Uiso 1 1 calc R . . C27 C 0.2965(3) 0.0073(2) 0.2190(2) 0.0343(8) Uani 1 1 d . . . C28 C 0.5184(3) -0.0610(2) 0.1887(2) 0.0361(8) Uani 1 1 d . . . C29 C 0.6342(3) -0.0522(3) 0.2058(3) 0.0514(11) Uani 1 1 d . . . H29A H 0.6695 -0.0365 0.2633 0.056(14) Uiso 1 1 d R . . H29B H 0.6458 -0.0193 0.1654 0.068 Uiso 1 1 d R . . H29C H 0.6645 -0.0956 0.1967 0.068 Uiso 1 1 d R . . C30 C 0.3027(6) -0.2049(4) 0.2999(4) 0.0848(19) Uani 1 1 d . . . H30A H 0.3425 -0.2062 0.3640 0.9(3) Uiso 1 1 d R . . H30B H 0.3032 -0.2494 0.2737 1.105 Uiso 1 1 d R . . H30C H 0.2305 -0.1904 0.2894 1.105 Uiso 1 1 d R . . O31 O 0.6046(3) 0.26877(16) 0.2806(2) 0.0509(8) Uani 1 1 d . . . H031 H 0.6386 0.2670 0.2386 0.080(19) Uiso 1 1 d R . . C31 C 0.6908(4) 0.2873(3) 0.3530(3) 0.0607(13) Uani 1 1 d . . . H31A H 0.7575 0.2666 0.3542 0.10(2) Uiso 1 1 d R . . H31B H 0.6746 0.2735 0.4042 0.115 Uiso 1 1 d R . . H31C H 0.6984 0.3368 0.3546 0.115 Uiso 1 1 d R . . O32 O 0.4971(3) -0.0837(2) 0.3839(2) 0.0677(10) Uani 1 1 d . . . H032 H 0.5071 -0.0331 0.3764 0.12(3) Uiso 1 1 d R . . C32 C 0.5869(5) -0.1167(4) 0.4366(5) 0.100(2) Uani 1 1 d . . . H32A H 0.5536 -0.1586 0.4567 0.11(3) Uiso 1 1 d R . . H32B H 0.6250 -0.0879 0.4844 0.134 Uiso 1 1 d R . . H32C H 0.6336 -0.1306 0.4049 0.134 Uiso 1 1 d R . . O33 O -0.0570(3) 0.1719(2) 0.0186(2) 0.0693(11) Uani 1 1 d . . . H033 H -0.1080 0.1588 -0.0352 0.053(14) Uiso 1 1 d R . . C33 C 0.0290(6) 0.1256(5) 0.0444(5) 0.121(3) Uani 1 1 d . . . H33A H 0.0591 0.1209 -0.0022 0.29(7) Uiso 1 1 d R . . H33B H 0.0050 0.0813 0.0576 0.353 Uiso 1 1 d R . . H33C H 0.0818 0.1426 0.0953 0.353 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0320(3) 0.0357(3) 0.0288(3) -0.0013(2) 0.0093(2) -0.0014(2) Co2 0.0334(3) 0.0371(3) 0.0319(3) -0.0037(2) 0.0127(2) -0.0009(2) Co3 0.0393(3) 0.0343(3) 0.0297(3) 0.0003(2) 0.0127(2) -0.0003(2) O1 0.0520(17) 0.0351(15) 0.0372(15) -0.0020(12) 0.0179(13) -0.0001(13) O2 0.0579(18) 0.0360(15) 0.0348(14) 0.0013(12) 0.0203(13) -0.0011(13) O3 0.0378(14) 0.0392(15) 0.0328(13) 0.0040(11) 0.0107(11) 0.0101(12) O4 0.0399(16) 0.077(2) 0.0504(18) -0.0169(17) 0.0214(14) -0.0218(16) O5 0.0481(16) 0.0590(19) 0.0302(14) 0.0026(13) 0.0146(12) -0.0077(15) O6 0.0284(13) 0.0492(17) 0.0287(13) -0.0001(12) 0.0039(11) -0.0035(12) O7 0.0287(13) 0.0435(16) 0.0381(14) 0.0020(12) 0.0094(11) 0.0003(12) O8 0.0584(19) 0.0472(18) 0.060(2) -0.0205(15) 0.0339(16) -0.0110(15) O9 0.0456(16) 0.0432(17) 0.0469(16) -0.0063(13) 0.0208(13) -0.0079(13) O10 0.0402(15) 0.0410(16) 0.0476(16) -0.0093(13) 0.0218(13) -0.0022(12) O11 0.0417(15) 0.0349(15) 0.0367(14) -0.0003(11) 0.0128(12) 0.0052(12) O12 0.079(2) 0.053(2) 0.0328(15) 0.0067(14) 0.0185(15) -0.0089(17) N1 0.0367(16) 0.0305(16) 0.0309(15) -0.0032(13) 0.0122(13) -0.0036(13) N2 0.0372(17) 0.0301(16) 0.0315(16) -0.0025(13) 0.0101(13) -0.0005(13) N3 0.0374(16) 0.0386(17) 0.0242(14) 0.0008(13) 0.0095(13) 0.0040(14) N4 0.0339(16) 0.0386(18) 0.0253(15) 0.0013(13) 0.0061(12) 0.0046(14) N5 0.0298(15) 0.0393(18) 0.0326(16) 0.0000(13) 0.0140(13) 0.0018(14) N6 0.0340(16) 0.0375(18) 0.0334(16) -0.0020(14) 0.0150(13) -0.0017(14) C1 0.035(2) 0.035(2) 0.039(2) -0.0028(16) 0.0097(16) -0.0034(17) C2 0.041(2) 0.0292(19) 0.039(2) 0.0002(16) 0.0110(17) -0.0071(16) C3 0.060(3) 0.036(2) 0.043(2) 0.0023(18) 0.010(2) -0.007(2) C4 0.073(3) 0.034(2) 0.056(3) 0.004(2) 0.008(2) 0.001(2) C5 0.065(3) 0.034(2) 0.062(3) -0.007(2) 0.013(2) 0.002(2) C6 0.058(3) 0.038(2) 0.046(2) -0.0079(19) 0.013(2) -0.001(2) C7 0.0358(19) 0.034(2) 0.0334(19) 0.0028(15) 0.0118(15) -0.0024(16) C8 0.0263(17) 0.035(2) 0.039(2) 0.0000(16) 0.0095(15) -0.0012(15) C9 0.061(3) 0.038(2) 0.045(2) 0.0010(19) 0.015(2) 0.014(2) C10 0.064(3) 0.101(5) 0.063(3) -0.019(3) 0.017(3) -0.040(3) C11 0.046(2) 0.044(2) 0.0308(19) -0.0009(17) 0.0127(17) 0.0077(19) C12 0.036(2) 0.038(2) 0.0305(19) -0.0019(16) 0.0057(15) 0.0010(17) C13 0.046(2) 0.047(3) 0.039(2) 0.0029(19) 0.0067(18) 0.004(2) C14 0.053(3) 0.062(3) 0.036(2) -0.004(2) -0.003(2) 0.006(2) C15 0.073(3) 0.064(3) 0.025(2) 0.003(2) 0.009(2) 0.010(3) C16 0.062(3) 0.054(3) 0.037(2) 0.004(2) 0.018(2) -0.001(2) C17 0.0343(19) 0.034(2) 0.0301(18) -0.0021(15) 0.0078(15) 0.0013(16) C18 0.0338(19) 0.036(2) 0.0345(19) -0.0019(16) 0.0071(16) 0.0007(16) C19 0.036(2) 0.076(3) 0.045(2) 0.016(2) 0.0047(19) 0.004(2) C20 0.086(4) 0.073(4) 0.088(4) -0.027(3) 0.054(4) -0.012(3) C21 0.039(2) 0.045(2) 0.0334(19) 0.0008(17) 0.0155(16) -0.0012(18) C22 0.040(2) 0.044(2) 0.0309(19) 0.0014(16) 0.0143(16) 0.0007(18) C23 0.040(2) 0.051(3) 0.039(2) -0.0033(19) 0.0144(18) -0.0010(19) C24 0.037(2) 0.074(3) 0.048(3) -0.004(2) 0.021(2) 0.007(2) C25 0.039(2) 0.075(3) 0.054(3) -0.002(3) 0.024(2) -0.008(2) C26 0.044(2) 0.058(3) 0.050(3) -0.001(2) 0.019(2) -0.013(2) C27 0.038(2) 0.038(2) 0.0281(17) 0.0025(15) 0.0125(16) 0.0012(17) C28 0.039(2) 0.039(2) 0.0317(18) 0.0015(16) 0.0132(16) 0.0045(17) C29 0.039(2) 0.050(3) 0.066(3) -0.008(2) 0.018(2) 0.003(2) C30 0.106(5) 0.088(5) 0.067(4) 0.018(3) 0.036(4) -0.008(4) O31 0.0538(18) 0.0501(19) 0.0527(18) -0.0145(15) 0.0222(15) -0.0091(15) C31 0.064(3) 0.054(3) 0.058(3) -0.014(2) 0.010(2) -0.002(3) O32 0.064(2) 0.076(3) 0.052(2) 0.0139(18) 0.0027(17) -0.017(2) C32 0.072(4) 0.086(5) 0.120(6) 0.024(4) -0.003(4) -0.008(4) O33 0.050(2) 0.105(3) 0.053(2) -0.014(2) 0.0169(17) -0.004(2) C33 0.102(6) 0.190(10) 0.064(4) 0.002(5) 0.015(4) 0.069(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.849(3) . ? Co1 O1 1.870(3) . ? Co1 O3 1.894(3) . ? Co1 O6 1.895(3) . ? Co1 N4 1.909(3) . ? Co1 O4 1.945(3) . ? Co2 N3 1.847(3) . ? Co2 O5 1.872(3) . ? Co2 O7 1.898(3) . ? Co2 O10 1.902(3) . ? Co2 N6 1.907(3) . ? Co2 O8 1.964(3) . ? Co3 N5 1.850(3) . ? Co3 O9 1.874(3) . ? Co3 O11 1.902(3) . ? Co3 N2 1.906(3) 3_655 ? Co3 O2 1.916(3) 3_655 ? Co3 O12 1.938(3) . ? O1 C1 1.341(5) . ? O2 C7 1.284(5) . ? O2 Co3 1.916(3) 3_655 ? O3 C8 1.308(5) . ? O4 C10 1.390(6) . ? O4 H04 0.9943 . ? O5 C11 1.339(5) . ? O6 C17 1.285(5) . ? O7 C18 1.281(5) . ? O8 C20 1.404(6) . ? O8 H08 1.1061 . ? O9 C21 1.336(5) . ? O10 C27 1.295(5) . ? O11 C28 1.285(5) . ? O12 C30 1.450(7) . ? O12 H012 1.0466 . ? N1 C7 1.313(5) . ? N1 N2 1.418(4) . ? N2 C8 1.307(5) . ? N2 Co3 1.906(3) 3_655 ? N3 C17 1.313(5) . ? N3 N4 1.424(4) . ? N4 C18 1.316(5) . ? N5 C27 1.306(5) . ? N5 N6 1.413(4) . ? N6 C28 1.325(5) . ? C1 C6 1.394(6) . ? C1 C2 1.411(6) . ? C2 C3 1.402(6) . ? C2 C7 1.464(5) . ? C3 C4 1.375(6) . ? C3 H3A 0.9300 . ? C4 C5 1.393(7) . ? C4 H4A 0.9300 . ? C5 C6 1.367(7) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C8 C9 1.483(6) . ? C9 H9A 0.9980 . ? C9 H9B 0.9600 . ? C9 H9C 0.9602 . ? C10 H10A 0.9802 . ? C10 H10B 0.9600 . ? C10 H10C 0.9601 . ? C11 C12 1.400(6) . ? C11 C16 1.416(6) . ? C12 C13 1.410(6) . ? C12 C17 1.467(5) . ? C13 C14 1.371(6) . ? C13 H13A 0.9300 . ? C14 C15 1.379(7) . ? C14 H14A 0.9300 . ? C15 C16 1.361(7) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C18 C19 1.493(6) . ? C19 H19A 0.9335 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9274 . ? C20 H20B 0.9600 . ? C20 H20C 0.9601 . ? C21 C26 1.405(6) . ? C21 C22 1.416(6) . ? C22 C23 1.406(6) . ? C22 C27 1.466(5) . ? C23 C24 1.373(6) . ? C23 H23A 0.9300 . ? C24 C25 1.383(7) . ? C24 H24A 0.9300 . ? C25 C26 1.379(7) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C28 C29 1.483(5) . ? C29 H29A 0.9545 . ? C29 H29B 0.9600 . ? C29 H29C 0.9602 . ? C30 H30A 1.0107 . ? C30 H30B 0.9599 . ? C30 H30C 0.9599 . ? O31 C31 1.406(5) . ? O31 H031 0.9302 . ? C31 H31A 0.9648 . ? C31 H31B 0.9600 . ? C31 H31C 0.9599 . ? O32 C32 1.385(7) . ? O32 H032 0.9982 . ? C32 H32A 1.0231 . ? C32 H32B 0.9601 . ? C32 H32C 0.9601 . ? O33 C33 1.406(8) . ? O33 H033 0.9569 . ? C33 H33A 0.9647 . ? C33 H33B 0.9599 . ? C33 H33C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 O1 94.09(13) . . ? N1 Co1 O3 83.00(13) . . ? O1 Co1 O3 177.06(12) . . ? N1 Co1 O6 173.43(13) . . ? O1 Co1 O6 91.60(12) . . ? O3 Co1 O6 91.27(12) . . ? N1 Co1 N4 99.68(13) . . ? O1 Co1 N4 89.96(13) . . ? O3 Co1 N4 91.00(13) . . ? O6 Co1 N4 83.58(12) . . ? N1 Co1 O4 88.39(14) . . ? O1 Co1 O4 89.38(14) . . ? O3 Co1 O4 90.05(14) . . ? O6 Co1 O4 88.39(13) . . ? N4 Co1 O4 171.92(13) . . ? N3 Co2 O5 93.34(13) . . ? N3 Co2 O7 82.78(12) . . ? O5 Co2 O7 176.08(12) . . ? N3 Co2 O10 173.86(13) . . ? O5 Co2 O10 92.36(13) . . ? O7 Co2 O10 91.49(12) . . ? N3 Co2 N6 98.72(14) . . ? O5 Co2 N6 91.34(14) . . ? O7 Co2 N6 89.82(13) . . ? O10 Co2 N6 83.42(13) . . ? N3 Co2 O8 89.65(13) . . ? O5 Co2 O8 91.33(14) . . ? O7 Co2 O8 88.09(13) . . ? O10 Co2 O8 87.94(12) . . ? N6 Co2 O8 171.05(13) . . ? N5 Co3 O9 94.00(13) . . ? N5 Co3 O11 82.48(13) . . ? O9 Co3 O11 176.28(12) . . ? N5 Co3 N2 98.64(13) . 3_655 ? O9 Co3 N2 91.64(13) . 3_655 ? O11 Co3 N2 90.11(12) . 3_655 ? N5 Co3 O2 172.70(13) . 3_655 ? O9 Co3 O2 93.06(13) . 3_655 ? O11 Co3 O2 90.41(12) . 3_655 ? N2 Co3 O2 82.98(12) 3_655 3_655 ? N5 Co3 O12 89.16(14) . . ? O9 Co3 O12 89.47(14) . . ? O11 Co3 O12 89.25(14) . . ? N2 Co3 O12 172.02(14) 3_655 . ? O2 Co3 O12 89.08(13) 3_655 . ? C1 O1 Co1 125.1(2) . . ? C7 O2 Co3 111.5(2) . 3_655 ? C8 O3 Co1 111.8(2) . . ? C10 O4 Co1 125.6(3) . . ? C10 O4 H04 115.6 . . ? Co1 O4 H04 118.8 . . ? C11 O5 Co2 123.2(3) . . ? C17 O6 Co1 112.3(2) . . ? C18 O7 Co2 112.2(2) . . ? C20 O8 Co2 123.7(3) . . ? C20 O8 H08 108.8 . . ? Co2 O8 H08 110.2 . . ? C21 O9 Co3 123.9(3) . . ? C27 O10 Co2 111.6(2) . . ? C28 O11 Co3 112.5(2) . . ? C30 O12 Co3 126.5(3) . . ? C30 O12 H012 104.1 . . ? Co3 O12 H012 121.9 . . ? C7 N1 N2 113.4(3) . . ? C7 N1 Co1 130.2(3) . . ? N2 N1 Co1 113.9(2) . . ? C8 N2 N1 110.8(3) . . ? C8 N2 Co3 139.2(3) . 3_655 ? N1 N2 Co3 109.7(2) . 3_655 ? C17 N3 N4 113.3(3) . . ? C17 N3 Co2 130.5(3) . . ? N4 N3 Co2 113.8(2) . . ? C18 N4 N3 109.9(3) . . ? C18 N4 Co1 139.2(3) . . ? N3 N4 Co1 109.6(2) . . ? C27 N5 N6 113.7(3) . . ? C27 N5 Co3 130.5(3) . . ? N6 N5 Co3 114.2(2) . . ? C28 N6 N5 110.3(3) . . ? C28 N6 Co2 139.0(3) . . ? N5 N6 Co2 109.9(2) . . ? O1 C1 C6 116.6(4) . . ? O1 C1 C2 125.0(4) . . ? C6 C1 C2 118.4(4) . . ? C3 C2 C1 118.8(4) . . ? C3 C2 C7 117.4(4) . . ? C1 C2 C7 123.8(4) . . ? C4 C3 C2 121.9(4) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C3 C4 C5 118.5(4) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C5 C6 C1 121.5(4) . . ? C5 C6 H6A 119.2 . . ? C1 C6 H6A 119.2 . . ? O2 C7 N1 120.3(4) . . ? O2 C7 C2 120.7(3) . . ? N1 C7 C2 118.9(3) . . ? N2 C8 O3 120.4(3) . . ? N2 C8 C9 122.5(4) . . ? O3 C8 C9 117.1(3) . . ? C8 C9 H9A 107.3 . . ? C8 C9 H9B 110.4 . . ? H9A C9 H9B 110.2 . . ? C8 C9 H9C 110.1 . . ? H9A C9 H9C 110.2 . . ? H9B C9 H9C 108.5 . . ? O4 C10 H10A 106.6 . . ? O4 C10 H10B 110.5 . . ? H10A C10 H10B 110.4 . . ? O4 C10 H10C 110.2 . . ? H10A C10 H10C 110.4 . . ? H10B C10 H10C 108.6 . . ? O5 C11 C12 125.8(3) . . ? O5 C11 C16 116.7(4) . . ? C12 C11 C16 117.5(4) . . ? C11 C12 C13 119.4(4) . . ? C11 C12 C17 122.8(3) . . ? C13 C12 C17 117.7(4) . . ? C14 C13 C12 121.4(4) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C13 C14 C15 119.3(4) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C16 C15 C14 120.7(4) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C15 C16 C11 121.8(4) . . ? C15 C16 H16A 119.1 . . ? C11 C16 H16A 119.1 . . ? O6 C17 N3 120.3(3) . . ? O6 C17 C12 120.4(3) . . ? N3 C17 C12 119.3(3) . . ? O7 C18 N4 121.1(4) . . ? O7 C18 C19 117.8(3) . . ? N4 C18 C19 121.1(4) . . ? C18 C19 H19A 110.3 . . ? C18 C19 H19B 109.9 . . ? H19A C19 H19B 109.6 . . ? C18 C19 H19C 109.4 . . ? H19A C19 H19C 109.6 . . ? H19B C19 H19C 108.1 . . ? O8 C20 H20A 103.7 . . ? O8 C20 H20B 111.5 . . ? H20A C20 H20B 110.9 . . ? O8 C20 H20C 110.8 . . ? H20A C20 H20C 110.9 . . ? H20B C20 H20C 108.9 . . ? O9 C21 C26 117.2(4) . . ? O9 C21 C22 125.6(4) . . ? C26 C21 C22 117.2(4) . . ? C23 C22 C21 119.3(4) . . ? C23 C22 C27 117.9(4) . . ? C21 C22 C27 122.8(4) . . ? C24 C23 C22 121.9(4) . . ? C24 C23 H23A 119.0 . . ? C22 C23 H23A 119.0 . . ? C23 C24 C25 118.8(4) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? C26 C25 C24 120.5(4) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C21 122.0(4) . . ? C25 C26 H26A 119.0 . . ? C21 C26 H26A 119.0 . . ? O10 C27 N5 120.3(4) . . ? O10 C27 C22 119.9(3) . . ? N5 C27 C22 119.8(4) . . ? O11 C28 N6 120.3(4) . . ? O11 C28 C29 117.9(4) . . ? N6 C28 C29 121.8(4) . . ? C28 C29 H29A 112.4 . . ? C28 C29 H29B 109.0 . . ? H29A C29 H29B 109.1 . . ? C28 C29 H29C 109.2 . . ? H29A C29 H29C 109.1 . . ? H29B C29 H29C 107.9 . . ? O12 C30 H30A 103.2 . . ? O12 C30 H30B 111.2 . . ? H30A C30 H30B 111.1 . . ? O12 C30 H30C 111.1 . . ? H30A C30 H30C 111.1 . . ? H30B C30 H30C 109.1 . . ? C31 O31 H031 99.9 . . ? O31 C31 H31A 114.3 . . ? O31 C31 H31B 108.2 . . ? H31A C31 H31B 108.8 . . ? O31 C31 H31C 109.0 . . ? H31A C31 H31C 108.8 . . ? H31B C31 H31C 107.6 . . ? C32 O32 H032 113.8 . . ? O32 C32 H32A 100.7 . . ? O32 C32 H32B 111.6 . . ? H32A C32 H32B 111.6 . . ? O32 C32 H32C 111.8 . . ? H32A C32 H32C 111.6 . . ? H32B C32 H32C 109.4 . . ? C33 O33 H033 112.3 . . ? O33 C33 H33A 108.8 . . ? O33 C33 H33B 109.7 . . ? H33A C33 H33B 109.9 . . ? O33 C33 H33C 110.2 . . ? H33A C33 H33C 109.9 . . ? H33B C33 H33C 108.3 . . ? 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 N1 Co1 O1 C1 -11.5(3) . . . . ? O3 Co1 O1 C1 -2(3) . . . . ? O6 Co1 O1 C1 165.2(3) . . . . ? N4 Co1 O1 C1 -111.2(3) . . . . ? O4 Co1 O1 C1 76.8(3) . . . . ? N1 Co1 O3 C8 0.0(2) . . . . ? O1 Co1 O3 C8 -9(3) . . . . ? O6 Co1 O3 C8 -176.8(2) . . . . ? N4 Co1 O3 C8 99.7(3) . . . . ? O4 Co1 O3 C8 -88.4(3) . . . . ? N1 Co1 O4 C10 154.7(5) . . . . ? O1 Co1 O4 C10 60.6(5) . . . . ? O3 Co1 O4 C10 -122.3(5) . . . . ? O6 Co1 O4 C10 -31.0(5) . . . . ? N4 Co1 O4 C10 -24.8(13) . . . . ? N3 Co2 O5 C11 23.8(3) . . . . ? O7 Co2 O5 C11 15(2) . . . . ? O10 Co2 O5 C11 -154.0(3) . . . . ? N6 Co2 O5 C11 122.6(3) . . . . ? O8 Co2 O5 C11 -66.0(3) . . . . ? N1 Co1 O6 C17 -113.7(11) . . . . ? O1 Co1 O6 C17 96.3(3) . . . . ? O3 Co1 O6 C17 -84.4(3) . . . . ? N4 Co1 O6 C17 6.5(3) . . . . ? O4 Co1 O6 C17 -174.4(3) . . . . ? N3 Co2 O7 C18 0.9(3) . . . . ? O5 Co2 O7 C18 9(2) . . . . ? O10 Co2 O7 C18 178.7(3) . . . . ? N6 Co2 O7 C18 -97.9(3) . . . . ? O8 Co2 O7 C18 90.8(3) . . . . ? N3 Co2 O8 C20 -138.2(4) . . . . ? O5 Co2 O8 C20 -44.9(4) . . . . ? O7 Co2 O8 C20 139.0(4) . . . . ? O10 Co2 O8 C20 47.5(4) . . . . ? N6 Co2 O8 C20 62.5(11) . . . . ? N5 Co3 O9 C21 -19.0(3) . . . . ? O11 Co3 O9 C21 0(2) . . . . ? N2 Co3 O9 C21 -117.7(3) 3_655 . . . ? O2 Co3 O9 C21 159.2(3) 3_655 . . . ? O12 Co3 O9 C21 70.2(3) . . . . ? N3 Co2 O10 C27 103.0(12) . . . . ? O5 Co2 O10 C27 -98.8(3) . . . . ? O7 Co2 O10 C27 81.9(3) . . . . ? N6 Co2 O10 C27 -7.7(3) . . . . ? O8 Co2 O10 C27 169.9(3) . . . . ? N5 Co3 O11 C28 -1.8(3) . . . . ? O9 Co3 O11 C28 -21(2) . . . . ? N2 Co3 O11 C28 96.9(3) 3_655 . . . ? O2 Co3 O11 C28 179.8(3) 3_655 . . . ? O12 Co3 O11 C28 -91.1(3) . . . . ? N5 Co3 O12 C30 135.6(5) . . . . ? O9 Co3 O12 C30 41.6(5) . . . . ? O11 Co3 O12 C30 -141.9(5) . . . . ? N2 Co3 O12 C30 -56.5(12) 3_655 . . . ? O2 Co3 O12 C30 -51.5(5) 3_655 . . . ? O1 Co1 N1 C7 20.0(4) . . . . ? O3 Co1 N1 C7 -159.5(4) . . . . ? O6 Co1 N1 C7 -129.9(11) . . . . ? N4 Co1 N1 C7 110.7(4) . . . . ? O4 Co1 N1 C7 -69.2(4) . . . . ? O1 Co1 N1 N2 -179.1(2) . . . . ? O3 Co1 N1 N2 1.4(2) . . . . ? O6 Co1 N1 N2 30.9(13) . . . . ? N4 Co1 N1 N2 -88.4(3) . . . . ? O4 Co1 N1 N2 91.6(3) . . . . ? C7 N1 N2 C8 161.6(3) . . . . ? Co1 N1 N2 C8 -2.5(4) . . . . ? C7 N1 N2 Co3 -12.5(4) . . . 3_655 ? Co1 N1 N2 Co3 -176.69(14) . . . 3_655 ? O5 Co2 N3 C17 -21.4(4) . . . . ? O7 Co2 N3 C17 158.1(4) . . . . ? O10 Co2 N3 C17 136.8(11) . . . . ? N6 Co2 N3 C17 -113.2(4) . . . . ? O8 Co2 N3 C17 69.9(4) . . . . ? O5 Co2 N3 N4 177.4(3) . . . . ? O7 Co2 N3 N4 -3.2(2) . . . . ? O10 Co2 N3 N4 -24.5(14) . . . . ? N6 Co2 N3 N4 85.5(3) . . . . ? O8 Co2 N3 N4 -91.3(3) . . . . ? C17 N3 N4 C18 -159.7(3) . . . . ? Co2 N3 N4 C18 4.8(4) . . . . ? C17 N3 N4 Co1 9.7(4) . . . . ? Co2 N3 N4 Co1 174.26(15) . . . . ? N1 Co1 N4 C18 -29.7(4) . . . . ? O1 Co1 N4 C18 64.4(4) . . . . ? O3 Co1 N4 C18 -112.8(4) . . . . ? O6 Co1 N4 C18 156.0(4) . . . . ? O4 Co1 N4 C18 149.8(9) . . . . ? N1 Co1 N4 N3 165.6(2) . . . . ? O1 Co1 N4 N3 -100.3(2) . . . . ? O3 Co1 N4 N3 82.5(2) . . . . ? O6 Co1 N4 N3 -8.6(2) . . . . ? O4 Co1 N4 N3 -14.9(12) . . . . ? O9 Co3 N5 C27 18.3(4) . . . . ? O11 Co3 N5 C27 -160.4(4) . . . . ? N2 Co3 N5 C27 110.6(3) 3_655 . . . ? O2 Co3 N5 C27 -147.1(9) 3_655 . . . ? O12 Co3 N5 C27 -71.1(4) . . . . ? O9 Co3 N5 N6 -177.3(2) . . . . ? O11 Co3 N5 N6 4.0(2) . . . . ? N2 Co3 N5 N6 -85.0(2) 3_655 . . . ? O2 Co3 N5 N6 17.3(11) 3_655 . . . ? O12 Co3 N5 N6 93.3(3) . . . . ? C27 N5 N6 C28 161.7(3) . . . . ? Co3 N5 N6 C28 -5.3(4) . . . . ? C27 N5 N6 Co2 -9.9(4) . . . . ? Co3 N5 N6 Co2 -176.93(15) . . . . ? N3 Co2 N6 C28 27.3(4) . . . . ? O5 Co2 N6 C28 -66.3(4) . . . . ? O7 Co2 N6 C28 110.0(4) . . . . ? O10 Co2 N6 C28 -158.5(4) . . . . ? O8 Co2 N6 C28 -173.6(8) . . . . ? N3 Co2 N6 N5 -164.8(2) . . . . ? O5 Co2 N6 N5 101.6(2) . . . . ? O7 Co2 N6 N5 -82.1(2) . . . . ? O10 Co2 N6 N5 9.4(2) . . . . ? O8 Co2 N6 N5 -5.7(10) . . . . ? Co1 O1 C1 C6 -175.4(3) . . . . ? Co1 O1 C1 C2 3.9(6) . . . . ? O1 C1 C2 C3 -179.0(4) . . . . ? C6 C1 C2 C3 0.3(6) . . . . ? O1 C1 C2 C7 2.0(6) . . . . ? C6 C1 C2 C7 -178.7(4) . . . . ? C1 C2 C3 C4 0.2(7) . . . . ? C7 C2 C3 C4 179.3(4) . . . . ? C2 C3 C4 C5 -1.0(8) . . . . ? C3 C4 C5 C6 1.3(8) . . . . ? C4 C5 C6 C1 -0.8(8) . . . . ? O1 C1 C6 C5 179.3(4) . . . . ? C2 C1 C6 C5 0.0(7) . . . . ? Co3 O2 C7 N1 8.0(5) 3_655 . . . ? Co3 O2 C7 C2 -169.0(3) 3_655 . . . ? N2 N1 C7 O2 3.1(5) . . . . ? Co1 N1 C7 O2 164.0(3) . . . . ? N2 N1 C7 C2 -179.9(3) . . . . ? Co1 N1 C7 C2 -18.9(5) . . . . ? C3 C2 C7 O2 3.1(6) . . . . ? C1 C2 C7 O2 -177.9(4) . . . . ? C3 C2 C7 N1 -173.9(4) . . . . ? C1 C2 C7 N1 5.1(6) . . . . ? N1 N2 C8 O3 2.7(5) . . . . ? Co3 N2 C8 O3 174.3(3) 3_655 . . . ? N1 N2 C8 C9 -178.0(4) . . . . ? Co3 N2 C8 C9 -6.4(6) 3_655 . . . ? Co1 O3 C8 N2 -1.6(4) . . . . ? Co1 O3 C8 C9 179.1(3) . . . . ? Co2 O5 C11 C12 -20.2(6) . . . . ? Co2 O5 C11 C16 160.6(3) . . . . ? O5 C11 C12 C13 -178.6(4) . . . . ? C16 C11 C12 C13 0.6(6) . . . . ? O5 C11 C12 C17 4.4(7) . . . . ? C16 C11 C12 C17 -176.4(4) . . . . ? C11 C12 C13 C14 -1.0(7) . . . . ? C17 C12 C13 C14 176.1(4) . . . . ? C12 C13 C14 C15 0.8(7) . . . . ? C13 C14 C15 C16 -0.2(8) . . . . ? C14 C15 C16 C11 -0.2(8) . . . . ? O5 C11 C16 C15 179.3(4) . . . . ? C12 C11 C16 C15 0.0(7) . . . . ? Co1 O6 C17 N3 -2.6(5) . . . . ? Co1 O6 C17 C12 178.8(3) . . . . ? N4 N3 C17 O6 -4.9(5) . . . . ? Co2 N3 C17 O6 -166.3(3) . . . . ? N4 N3 C17 C12 173.7(3) . . . . ? Co2 N3 C17 C12 12.4(6) . . . . ? C11 C12 C17 O6 179.1(4) . . . . ? C13 C12 C17 O6 2.1(6) . . . . ? C11 C12 C17 N3 0.5(6) . . . . ? C13 C12 C17 N3 -176.5(4) . . . . ? Co2 O7 C18 N4 1.9(5) . . . . ? Co2 O7 C18 C19 -178.1(3) . . . . ? N3 N4 C18 O7 -4.4(5) . . . . ? Co1 N4 C18 O7 -169.0(3) . . . . ? N3 N4 C18 C19 175.6(4) . . . . ? Co1 N4 C18 C19 10.9(7) . . . . ? Co3 O9 C21 C26 -164.7(3) . . . . ? Co3 O9 C21 C22 16.3(6) . . . . ? O9 C21 C22 C23 176.3(4) . . . . ? C26 C21 C22 C23 -2.7(6) . . . . ? O9 C21 C22 C27 -5.1(6) . . . . ? C26 C21 C22 C27 175.9(4) . . . . ? C21 C22 C23 C24 0.1(6) . . . . ? C27 C22 C23 C24 -178.6(4) . . . . ? C22 C23 C24 C25 3.0(7) . . . . ? C23 C24 C25 C26 -3.4(7) . . . . ? C24 C25 C26 C21 0.8(8) . . . . ? O9 C21 C26 C25 -176.8(4) . . . . ? C22 C21 C26 C25 2.3(7) . . . . ? Co2 O10 C27 N5 4.2(4) . . . . ? Co2 O10 C27 C22 -174.8(3) . . . . ? N6 N5 C27 O10 3.9(5) . . . . ? Co3 N5 C27 O10 168.3(3) . . . . ? N6 N5 C27 C22 -177.1(3) . . . . ? Co3 N5 C27 C22 -12.6(5) . . . . ? C23 C22 C27 O10 0.1(6) . . . . ? C21 C22 C27 O10 -178.5(4) . . . . ? C23 C22 C27 N5 -178.9(4) . . . . ? C21 C22 C27 N5 2.4(6) . . . . ? Co3 O11 C28 N6 -0.9(4) . . . . ? Co3 O11 C28 C29 178.2(3) . . . . ? N5 N6 C28 O11 4.0(5) . . . . ? Co2 N6 C28 O11 171.9(3) . . . . ? N5 N6 C28 C29 -175.0(4) . . . . ? Co2 N6 C28 C29 -7.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.877 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.091 data_3 #C59 H74 Co6 N12 O29 _database_code_CSD 157263 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C59 H74 Co6 N12 O29' _chemical_formula_sum 'C59 H74 Co6 N12 O29' _chemical_formula_weight 1768.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 10.157(2) _cell_length_b 13.025(3) _cell_length_c 14.969(5) _cell_angle_alpha 85.22(2) _cell_angle_beta 85.599(16) _cell_angle_gamma 68.239(16) _cell_volume 1830.5(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour 'dark violet-red' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 906 _exptl_absorpt_coefficient_mu 1.418 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Siemens SMART 1000 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8892 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6032 _reflns_number_gt 3600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction 'SAINT (Siemens, 1996)' _computing_structure_solution 'SHELXS 97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL 97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL/PC (Sheldrick, 1993)' _computing_publication_material 'SHELXL 97 (Sheldrick, 1997)' _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^)+(0.1485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6032 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1191 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.2135 _refine_ls_wR_factor_gt 0.1763 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.459 _refine_ls_shift/su_mean 0.019 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 0.30578(10) -0.12063(8) 0.23078(6) 0.0388(3) Uani 1 1 d . . . Co2 Co 0.56928(11) 0.08027(8) 0.25536(6) 0.0385(3) Uani 1 1 d . . . Co3 Co 0.52314(10) 0.30874(8) 0.01283(6) 0.0362(3) Uani 1 1 d . . . O1 O 0.3778(6) -0.2123(4) 0.3332(3) 0.0482(13) Uani 1 1 d . . . O2 O 0.5460(5) -0.3888(4) 0.0967(3) 0.0408(12) Uani 1 1 d . . . O3 O 0.2342(5) -0.0345(4) 0.1225(3) 0.0435(12) Uani 1 1 d . . . O4 O 0.1338(6) -0.1558(5) 0.2446(4) 0.0676(17) Uani 1 1 d . . . O5 O 0.4693(6) 0.2009(4) 0.3222(3) 0.0532(14) Uani 1 1 d . . . O6 O 0.2185(5) 0.0040(4) 0.3034(3) 0.0443(12) Uani 1 1 d . . . O7 O 0.6685(5) -0.0485(4) 0.1895(3) 0.0468(13) Uani 1 1 d . . . O8 O 0.6567(6) 0.0009(5) 0.3653(4) 0.0628(16) Uani 1 1 d . . . H08 H 0.6830 0.0223 0.4212 0.26(9) Uiso 1 1 d R . . O9 O 0.6632(5) 0.3703(4) 0.0087(3) 0.0426(12) Uani 1 1 d . . . O10 O 0.7194(5) 0.1348(4) 0.2336(3) 0.0448(13) Uani 1 1 d . . . O11 O 0.3805(5) 0.2446(4) 0.0240(3) 0.0421(12) Uani 1 1 d . . . O12 O 0.3943(6) 0.4344(4) 0.0760(3) 0.0533(14) Uani 1 1 d . . . H012 H 0.3652 0.5054 0.0386 0.12(4) Uiso 1 1 d R . . N1 N 0.3916(6) -0.2332(5) 0.1534(4) 0.0384(14) Uani 1 1 d . . . N2 N 0.3663(6) -0.1979(5) 0.0628(4) 0.0379(14) Uani 1 1 d . . . N3 N 0.4278(6) 0.0230(5) 0.2682(4) 0.0368(14) Uani 1 1 d . . . N4 N 0.4595(6) -0.0727(5) 0.2213(4) 0.0360(14) Uani 1 1 d . . . N5 N 0.5851(6) 0.2249(4) 0.1172(4) 0.0336(13) Uani 1 1 d . . . N6 N 0.5017(6) 0.1631(5) 0.1486(4) 0.0391(14) Uani 1 1 d . . . C1 C 0.4782(9) -0.3133(6) 0.3328(5) 0.047(2) Uani 1 1 d . . . C2 C 0.5330(9) -0.3738(6) 0.2553(5) 0.049(2) Uani 1 1 d . . . C3 C 0.6376(11) -0.4803(7) 0.2645(6) 0.072(3) Uani 1 1 d . . . H3A H 0.6743 -0.5200 0.2136 0.086 Uiso 1 1 calc R . . C4 C 0.6873(12) -0.5275(9) 0.3473(6) 0.089(4) Uani 1 1 d . . . H4A H 0.7563 -0.5983 0.3526 0.106 Uiso 1 1 calc R . . C5 C 0.6320(13) -0.4671(9) 0.4220(6) 0.095(4) Uani 1 1 d . . . H5A H 0.6634 -0.4986 0.4782 0.114 Uiso 1 1 calc R . . C6 C 0.5323(11) -0.3621(8) 0.4153(6) 0.073(3) Uani 1 1 d . . . H6A H 0.5000 -0.3226 0.4666 0.087 Uiso 1 1 calc R . . C7 C 0.4896(8) -0.3316(6) 0.1647(5) 0.0398(17) Uani 1 1 d . . . C8 C 0.2862(8) -0.0941(6) 0.0542(5) 0.0446(19) Uani 1 1 d . . . H8A H 0.2653 -0.0613 -0.0031 0.054 Uiso 1 1 calc R . . C9A C -0.004(4) -0.087(3) 0.285(2) 0.121(11) Uiso 0.45 1 d P . . C9B C 0.043(3) -0.145(3) 0.326(2) 0.093(9) Uiso 0.40 1 d P . . C9C C 0.108(8) -0.239(7) 0.296(5) 0.09(2) Uiso 0.15 1 d P . . C10 C 0.3380(9) 0.2258(6) 0.3572(5) 0.0465(19) Uani 1 1 d . . . C11 C 0.2528(8) 0.1612(6) 0.3540(5) 0.0436(19) Uani 1 1 d . . . C12 C 0.1182(9) 0.1958(8) 0.3965(6) 0.062(2) Uani 1 1 d . . . H12A H 0.0625 0.1530 0.3959 0.074 Uiso 1 1 calc R . . C13 C 0.0667(11) 0.2947(9) 0.4401(7) 0.079(3) Uani 1 1 d . . . H13A H -0.0236 0.3189 0.4681 0.094 Uiso 1 1 calc R . . C14 C 0.1506(12) 0.3552(8) 0.4411(7) 0.084(3) Uani 1 1 d . . . H14A H 0.1160 0.4206 0.4708 0.101 Uiso 1 1 calc R . . C15 C 0.2815(11) 0.3249(8) 0.4008(6) 0.068(3) Uani 1 1 d . . . H15A H 0.3343 0.3697 0.4021 0.082 Uiso 1 1 calc R . . C16 C 0.2989(8) 0.0586(6) 0.3079(4) 0.0379(17) Uani 1 1 d . . . C17 C 0.5852(8) -0.1027(6) 0.1828(5) 0.0440(19) Uani 1 1 d . . . H17A H 0.6171 -0.1650 0.1492 0.053 Uiso 1 1 calc R . . C18 C 0.6512(13) -0.0979(9) 0.4061(8) 0.090(4) Uani 1 1 d . . . H18A H 0.6613 -0.1486 0.3599 0.38(16) Uiso 1 1 d R . . H18B H 0.5630 -0.0849 0.4400 0.460 Uiso 1 1 d R . . H18C H 0.7270 -0.1296 0.4464 0.460 Uiso 1 1 d R . . C19 C 0.7723(8) 0.3403(6) 0.0626(5) 0.0400(17) Uani 1 1 d . . . C20 C 0.7946(8) 0.2621(6) 0.1366(5) 0.0400(17) Uani 1 1 d . . . C21 C 0.9130(8) 0.2395(7) 0.1873(5) 0.051(2) Uani 1 1 d . . . H21A H 0.9282 0.1876 0.2357 0.061 Uiso 1 1 calc R . . C22 C 1.0063(9) 0.2912(8) 0.1679(7) 0.074(3) Uani 1 1 d . . . H22A H 1.0833 0.2762 0.2033 0.089 Uiso 1 1 calc R . . C23 C 0.9858(10) 0.3668(9) 0.0945(7) 0.078(3) Uani 1 1 d . . . H23A H 1.0513 0.4005 0.0790 0.094 Uiso 1 1 calc R . . C24 C 0.8688(9) 0.3918(7) 0.0450(6) 0.058(2) Uani 1 1 d . . . H24A H 0.8540 0.4454 -0.0022 0.069 Uiso 1 1 calc R . . C25 C 0.6973(8) 0.2044(6) 0.1639(4) 0.0357(16) Uani 1 1 d . . . C26 C 0.3993(7) 0.1792(6) 0.0952(4) 0.0389(17) Uani 1 1 d . . . H26A H 0.3373 0.1420 0.1092 0.047 Uiso 1 1 calc R . . C27 C 0.3523(12) 0.4446(9) 0.1678(6) 0.090(3) Uani 1 1 d . . . H27A H 0.3015 0.3799 0.1942 0.15(5) Uiso 1 1 d R . . H27B H 0.2846 0.5180 0.1765 0.176 Uiso 1 1 d R . . H27C H 0.4332 0.4340 0.2018 0.176 Uiso 1 1 d R . . C28 C 0.7964(19) 0.1546(18) 0.4651(11) 0.186(10) Uani 1 1 d . . . H28A H 0.8610 0.1038 0.4280 1.5(8) Uiso 1 1 d R . . H28B H 0.7510 0.2235 0.4317 1.788 Uiso 1 1 d R . . H28C H 0.8440 0.1680 0.5132 1.788 Uiso 1 1 d R . . O13 O 0.6964(9) 0.1130(7) 0.4979(5) 0.101(2) Uani 1 1 d . . . C29 C 0.038(2) 0.1609(17) -0.0560(14) 0.206(11) Uani 1 1 d . . . O14 O 0.0634(11) 0.0802(12) -0.1194(10) 0.203(6) Uani 1 1 d . . . C30 C 0.076(5) 0.375(3) -0.269(3) 0.20(2) Uani 0.50 1 d P . . O15A O 0.133(4) 0.355(3) -0.160(6) 0.24(3) Uani 0.25 1 d P . . O15B O -0.139(8) 0.373(3) -0.320(5) 0.29(5) Uani 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0444(6) 0.0393(6) 0.0355(6) -0.0019(4) 0.0004(4) -0.0190(5) Co2 0.0496(6) 0.0386(6) 0.0315(5) 0.0078(4) -0.0077(4) -0.0221(5) Co3 0.0478(6) 0.0322(6) 0.0290(5) 0.0035(4) -0.0068(4) -0.0155(5) O1 0.069(4) 0.046(3) 0.035(3) 0.001(2) 0.004(2) -0.029(3) O2 0.054(3) 0.034(3) 0.030(3) 0.007(2) -0.011(2) -0.012(2) O3 0.049(3) 0.031(3) 0.046(3) 0.000(2) -0.010(2) -0.008(2) O4 0.059(4) 0.087(5) 0.071(4) -0.013(4) 0.015(3) -0.044(4) O5 0.078(4) 0.053(4) 0.040(3) -0.006(3) -0.003(3) -0.036(3) O6 0.044(3) 0.046(3) 0.045(3) -0.008(2) 0.005(2) -0.019(3) O7 0.043(3) 0.049(3) 0.052(3) 0.000(3) 0.002(2) -0.022(3) O8 0.093(4) 0.059(4) 0.046(3) 0.026(3) -0.028(3) -0.041(4) O9 0.056(3) 0.036(3) 0.041(3) 0.012(2) -0.010(2) -0.025(3) O10 0.051(3) 0.050(3) 0.041(3) 0.016(2) -0.015(2) -0.028(3) O11 0.049(3) 0.043(3) 0.038(3) 0.008(2) -0.014(2) -0.021(3) O12 0.079(4) 0.038(3) 0.033(3) 0.004(2) 0.003(3) -0.012(3) N1 0.056(4) 0.032(3) 0.029(3) 0.001(3) -0.003(3) -0.019(3) N2 0.050(4) 0.035(4) 0.027(3) 0.007(3) -0.009(3) -0.014(3) N3 0.046(4) 0.032(3) 0.033(3) -0.002(3) 0.001(3) -0.016(3) N4 0.044(4) 0.034(3) 0.033(3) 0.000(3) -0.001(3) -0.018(3) N5 0.036(3) 0.035(3) 0.032(3) 0.005(3) -0.004(3) -0.017(3) N6 0.045(4) 0.038(3) 0.037(3) 0.003(3) -0.005(3) -0.020(3) C1 0.071(6) 0.031(4) 0.038(4) 0.009(3) -0.010(4) -0.018(4) C2 0.071(5) 0.034(4) 0.037(4) 0.009(3) -0.015(4) -0.012(4) C3 0.110(8) 0.052(6) 0.041(5) 0.005(4) -0.015(5) -0.015(6) C4 0.121(9) 0.062(6) 0.050(6) 0.003(5) -0.027(6) 0.007(6) C5 0.148(11) 0.070(7) 0.043(6) 0.008(5) -0.030(6) -0.009(7) C6 0.103(8) 0.060(6) 0.042(5) 0.003(4) -0.012(5) -0.014(6) C7 0.059(5) 0.031(4) 0.035(4) 0.003(3) -0.001(4) -0.023(4) C8 0.053(5) 0.041(5) 0.035(4) 0.004(4) -0.011(4) -0.012(4) C10 0.068(6) 0.043(5) 0.030(4) 0.005(3) -0.012(4) -0.021(4) C11 0.050(5) 0.044(5) 0.028(4) -0.003(3) -0.004(3) -0.006(4) C12 0.050(5) 0.068(6) 0.060(6) -0.019(5) -0.004(4) -0.010(5) C13 0.058(6) 0.082(8) 0.073(7) -0.023(6) 0.001(5) 0.003(6) C14 0.092(8) 0.054(6) 0.095(8) -0.034(6) -0.010(7) -0.008(6) C15 0.077(7) 0.052(6) 0.076(7) -0.026(5) -0.001(5) -0.019(5) C16 0.046(5) 0.040(4) 0.027(4) 0.006(3) -0.007(3) -0.017(4) C17 0.049(5) 0.041(5) 0.036(4) -0.002(3) 0.008(4) -0.012(4) C18 0.127(10) 0.070(7) 0.075(7) 0.034(6) -0.045(7) -0.038(7) C19 0.046(4) 0.036(4) 0.039(4) 0.003(3) -0.002(3) -0.017(4) C20 0.045(4) 0.039(4) 0.039(4) 0.000(3) -0.006(3) -0.018(4) C21 0.048(5) 0.056(5) 0.053(5) 0.022(4) -0.019(4) -0.025(4) C22 0.053(6) 0.088(7) 0.087(7) 0.030(6) -0.024(5) -0.037(6) C23 0.066(6) 0.092(8) 0.091(7) 0.033(6) -0.010(5) -0.053(6) C24 0.060(5) 0.061(6) 0.057(5) 0.024(4) -0.018(4) -0.032(5) C25 0.045(4) 0.033(4) 0.027(4) -0.002(3) -0.001(3) -0.011(3) C26 0.042(4) 0.043(4) 0.034(4) 0.007(3) -0.008(3) -0.019(4) C27 0.117(9) 0.076(7) 0.067(7) 0.002(6) 0.014(6) -0.028(7) C28 0.185(16) 0.30(2) 0.172(16) -0.108(16) 0.100(14) -0.200(18) O13 0.145(7) 0.122(6) 0.061(5) -0.010(4) -0.014(4) -0.076(6) C29 0.21(2) 0.187(18) 0.20(2) -0.153(17) 0.087(15) -0.043(15) O14 0.108(8) 0.232(15) 0.257(16) 0.034(13) 0.003(9) -0.062(9) C30 0.34(6) 0.19(4) 0.17(4) 0.04(3) -0.03(4) -0.21(4) O15A 0.09(3) 0.10(3) 0.54(10) -0.14(5) 0.15(4) -0.07(2) O15B 0.42(10) 0.04(2) 0.34(8) -0.02(3) 0.21(8) -0.07(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 N1 1.852(6) . ? Co1 N4 1.876(6) . ? Co1 O1 1.879(5) . ? Co1 O6 1.919(5) . ? Co1 O3 1.920(5) . ? Co1 O4 1.956(5) . ? Co2 N3 1.840(6) . ? Co2 O5 1.850(5) . ? Co2 N6 1.876(6) . ? Co2 O10 1.904(5) . ? Co2 O7 1.916(5) . ? Co2 O8 1.956(5) . ? Co3 N5 1.840(5) . ? Co3 O9 1.869(5) . ? Co3 N2 1.872(6) 2_655 ? Co3 O2 1.902(4) 2_655 ? Co3 O11 1.914(5) . ? Co3 O12 1.941(5) . ? O1 C1 1.333(9) . ? O2 C7 1.281(8) . ? O2 Co3 1.902(4) 2_655 ? O3 C8 1.293(8) . ? O4 C9C 1.37(8) . ? O4 C9B 1.46(3) . ? O4 C9A 1.47(3) . ? O5 C10 1.327(9) . ? O6 C16 1.275(8) . ? O7 C17 1.300(8) . ? O8 C18 1.397(11) . ? O8 H08 0.9876 . ? O9 C19 1.340(8) . ? O10 C25 1.299(8) . ? O11 C26 1.287(8) . ? O12 C27 1.410(10) . ? O12 H012 0.9961 . ? N1 C7 1.307(9) . ? N1 N2 1.406(7) . ? N2 C8 1.295(9) . ? N2 Co3 1.872(6) 2_655 ? N3 C16 1.327(9) . ? N3 N4 1.401(8) . ? N4 C17 1.292(9) . ? N5 C25 1.314(8) . ? N5 N6 1.404(7) . ? N6 C26 1.304(8) . ? C1 C6 1.394(11) . ? C1 C2 1.416(10) . ? C2 C3 1.403(11) . ? C2 C7 1.457(10) . ? C3 C4 1.382(12) . ? C3 H3A 0.9300 . ? C4 C5 1.381(13) . ? C4 H4A 0.9300 . ? C5 C6 1.369(13) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C8 H8A 0.9300 . ? C9A C9B 0.94(4) . ? C9A C9C 1.89(9) . ? C9B C9C 1.26(8) . ? C9C O15B 1.67(9) 2 ? C10 C15 1.398(11) . ? C10 C11 1.419(11) . ? C11 C12 1.391(11) . ? C11 C16 1.456(10) . ? C12 C13 1.396(12) . ? C12 H12A 0.9300 . ? C13 C14 1.360(13) . ? C13 H13A 0.9300 . ? C14 C15 1.347(13) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C17 H17A 0.9300 . ? C18 H18A 0.9692 . ? C18 H18B 0.9599 . ? C18 H18C 0.9599 . ? C19 C24 1.378(10) . ? C19 C20 1.412(9) . ? C20 C21 1.397(10) . ? C20 C25 1.465(9) . ? C21 C22 1.354(11) . ? C21 H21A 0.9300 . ? C22 C23 1.386(12) . ? C22 H22A 0.9300 . ? C23 C24 1.369(12) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C26 H26A 0.9300 . ? C27 H27A 1.1699 . ? C27 H27B 0.9600 . ? C27 H27C 0.9601 . ? C28 O13 1.361(13) . ? C28 H28A 0.9267 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O14 1.415(18) . ? C30 O15A 1.74(8) . ? O15B C9C 1.67(9) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N4 93.7(2) . . ? N1 Co1 O1 93.4(2) . . ? N4 Co1 O1 91.2(2) . . ? N1 Co1 O6 175.5(2) . . ? N4 Co1 O6 83.9(2) . . ? O1 Co1 O6 90.5(2) . . ? N1 Co1 O3 83.5(2) . . ? N4 Co1 O3 90.1(2) . . ? O1 Co1 O3 176.7(2) . . ? O6 Co1 O3 92.6(2) . . ? N1 Co1 O4 91.6(3) . . ? N4 Co1 O4 174.3(3) . . ? O1 Co1 O4 90.6(2) . . ? O6 Co1 O4 90.7(2) . . ? O3 Co1 O4 88.4(2) . . ? N3 Co2 O5 94.1(2) . . ? N3 Co2 N6 93.8(2) . . ? O5 Co2 N6 91.0(2) . . ? N3 Co2 O10 175.7(2) . . ? O5 Co2 O10 89.6(2) . . ? N6 Co2 O10 84.0(2) . . ? N3 Co2 O7 83.7(2) . . ? O5 Co2 O7 177.3(2) . . ? N6 Co2 O7 90.5(2) . . ? O10 Co2 O7 92.7(2) . . ? N3 Co2 O8 92.7(2) . . ? O5 Co2 O8 88.5(2) . . ? N6 Co2 O8 173.5(2) . . ? O10 Co2 O8 89.5(2) . . ? O7 Co2 O8 90.3(2) . . ? N5 Co3 O9 93.1(2) . . ? N5 Co3 N2 94.7(2) . 2_655 ? O9 Co3 N2 91.9(2) . 2_655 ? N5 Co3 O2 176.4(2) . 2_655 ? O9 Co3 O2 90.2(2) . 2_655 ? N2 Co3 O2 83.7(2) 2_655 2_655 ? N5 Co3 O11 84.1(2) . . ? O9 Co3 O11 176.9(2) . . ? N2 Co3 O11 89.7(2) 2_655 . ? O2 Co3 O11 92.6(2) 2_655 . ? N5 Co3 O12 93.3(2) . . ? O9 Co3 O12 89.5(2) . . ? N2 Co3 O12 171.8(2) 2_655 . ? O2 Co3 O12 88.2(2) 2_655 . ? O11 Co3 O12 89.3(2) . . ? C1 O1 Co1 125.5(4) . . ? C7 O2 Co3 111.7(4) . 2_655 ? C8 O3 Co1 109.5(4) . . ? C9C O4 C9B 53(3) . . ? C9C O4 C9A 83(3) . . ? C9B O4 C9A 37.4(15) . . ? C9C O4 Co1 129(3) . . ? C9B O4 Co1 125.3(13) . . ? C9A O4 Co1 126.3(13) . . ? C10 O5 Co2 126.0(5) . . ? C16 O6 Co1 111.5(4) . . ? C17 O7 Co2 109.2(4) . . ? C18 O8 Co2 128.2(6) . . ? C18 O8 H08 92.6 . . ? Co2 O8 H08 135.2 . . ? C19 O9 Co3 126.1(4) . . ? C25 O10 Co2 111.2(4) . . ? C26 O11 Co3 109.1(4) . . ? C27 O12 Co3 130.7(6) . . ? C27 O12 H012 115.1 . . ? Co3 O12 H012 113.6 . . ? C7 N1 N2 113.7(6) . . ? C7 N1 Co1 132.1(5) . . ? N2 N1 Co1 112.9(4) . . ? C8 N2 N1 111.5(6) . . ? C8 N2 Co3 137.0(5) . 2_655 ? N1 N2 Co3 110.9(4) . 2_655 ? C16 N3 N4 114.1(6) . . ? C16 N3 Co2 132.5(5) . . ? N4 N3 Co2 113.2(4) . . ? C17 N4 N3 111.5(6) . . ? C17 N4 Co1 137.7(5) . . ? N3 N4 Co1 110.8(4) . . ? C25 N5 N6 113.6(5) . . ? C25 N5 Co3 133.1(5) . . ? N6 N5 Co3 113.0(4) . . ? C26 N6 N5 111.0(6) . . ? C26 N6 Co2 138.0(5) . . ? N5 N6 Co2 111.0(4) . . ? O1 C1 C6 117.0(7) . . ? O1 C1 C2 124.8(6) . . ? C6 C1 C2 118.2(7) . . ? C3 C2 C1 119.1(7) . . ? C3 C2 C7 116.9(7) . . ? C1 C2 C7 124.0(7) . . ? C4 C3 C2 121.5(8) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C5 C4 C3 118.4(9) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? C6 C5 C4 121.6(9) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C5 C6 C1 121.1(8) . . ? C5 C6 H6A 119.4 . . ? C1 C6 H6A 119.4 . . ? O2 C7 N1 119.9(6) . . ? O2 C7 C2 121.3(7) . . ? N1 C7 C2 118.8(6) . . ? O3 C8 N2 122.4(7) . . ? O3 C8 H8A 118.8 . . ? N2 C8 H8A 118.8 . . ? C9B C9A O4 70(3) . . ? C9B C9A C9C 36(3) . . ? O4 C9A C9C 46(3) . . ? C9A C9B C9C 118(5) . . ? C9A C9B O4 72(3) . . ? C9C C9B O4 60(4) . . ? C9B C9C O4 67(4) . . ? C9B C9C O15B 142(7) . 2 ? O4 C9C O15B 151(6) . 2 ? C9B C9C C9A 26(3) . . ? O4 C9C C9A 51(3) . . ? O15B C9C C9A 156(6) 2 . ? O5 C10 C15 115.7(8) . . ? O5 C10 C11 125.7(7) . . ? C15 C10 C11 118.6(8) . . ? C12 C11 C10 119.5(7) . . ? C12 C11 C16 117.3(8) . . ? C10 C11 C16 123.3(7) . . ? C11 C12 C13 120.0(9) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 119.0(9) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C15 C14 C13 123.1(9) . . ? C15 C14 H14A 118.5 . . ? C13 C14 H14A 118.5 . . ? C14 C15 C10 119.9(9) . . ? C14 C15 H15A 120.0 . . ? C10 C15 H15A 120.1 . . ? O6 C16 N3 119.6(6) . . ? O6 C16 C11 122.0(7) . . ? N3 C16 C11 118.3(7) . . ? N4 C17 O7 122.2(7) . . ? N4 C17 H17A 118.9 . . ? O7 C17 H17A 118.9 . . ? O8 C18 H18A 108.7 . . ? O8 C18 H18B 110.8 . . ? H18A C18 H18B 109.8 . . ? O8 C18 H18C 109.5 . . ? H18A C18 H18C 109.8 . . ? H18B C18 H18C 108.3 . . ? O9 C19 C24 117.0(6) . . ? O9 C19 C20 125.3(6) . . ? C24 C19 C20 117.7(7) . . ? C21 C20 C19 119.0(7) . . ? C21 C20 C25 118.0(7) . . ? C19 C20 C25 123.0(6) . . ? C22 C21 C20 121.7(7) . . ? C22 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? C21 C22 C23 119.3(8) . . ? C21 C22 H22A 120.3 . . ? C23 C22 H22A 120.3 . . ? C24 C23 C22 119.8(8) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C23 C24 C19 122.3(8) . . ? C23 C24 H24A 118.9 . . ? C19 C24 H24A 118.9 . . ? O10 C25 N5 119.8(6) . . ? O10 C25 C20 121.3(6) . . ? N5 C25 C20 118.8(6) . . ? O11 C26 N6 122.8(7) . . ? O11 C26 H26A 118.6 . . ? N6 C26 H26A 118.6 . . ? O12 C27 H27A 111.3 . . ? O12 C27 H27B 109.3 . . ? H27A C27 H27B 109.4 . . ? O12 C27 H27C 109.5 . . ? H27A C27 H27C 109.4 . . ? H27B C27 H27C 108.0 . . ? O13 C28 H28A 108.4 . . ? O13 C28 H28B 109.1 . . ? H28A C28 H28B 110.2 . . ? O13 C28 H28C 110.5 . . ? H28A C28 H28C 110.2 . . ? H28B C28 H28C 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 O1 C1 11.7(6) . . . . ? N4 Co1 O1 C1 -82.1(6) . . . . ? O6 Co1 O1 C1 -166.0(6) . . . . ? O3 Co1 O1 C1 31(4) . . . . ? O4 Co1 O1 C1 103.3(6) . . . . ? N1 Co1 O3 C8 -3.4(5) . . . . ? N4 Co1 O3 C8 90.3(5) . . . . ? O1 Co1 O3 C8 -23(4) . . . . ? O6 Co1 O3 C8 174.2(5) . . . . ? O4 Co1 O3 C8 -95.2(5) . . . . ? N1 Co1 O4 C9C 78(4) . . . . ? N4 Co1 O4 C9C -123(5) . . . . ? O1 Co1 O4 C9C -15(4) . . . . ? O6 Co1 O4 C9C -105(4) . . . . ? O3 Co1 O4 C9C 162(4) . . . . ? N1 Co1 O4 C9B 146.3(18) . . . . ? N4 Co1 O4 C9B -55(3) . . . . ? O1 Co1 O4 C9B 52.9(18) . . . . ? O6 Co1 O4 C9B -37.6(18) . . . . ? O3 Co1 O4 C9B -130.2(18) . . . . ? N1 Co1 O4 C9A -167.2(18) . . . . ? N4 Co1 O4 C9A -9(3) . . . . ? O1 Co1 O4 C9A 99.4(18) . . . . ? O6 Co1 O4 C9A 8.9(18) . . . . ? O3 Co1 O4 C9A -83.7(18) . . . . ? N3 Co2 O5 C10 -3.2(6) . . . . ? N6 Co2 O5 C10 90.6(6) . . . . ? O10 Co2 O5 C10 174.6(6) . . . . ? O7 Co2 O5 C10 -35(5) . . . . ? O8 Co2 O5 C10 -95.9(6) . . . . ? N1 Co1 O6 C16 -56(3) . . . . ? N4 Co1 O6 C16 2.1(4) . . . . ? O1 Co1 O6 C16 93.2(5) . . . . ? O3 Co1 O6 C16 -87.7(5) . . . . ? O4 Co1 O6 C16 -176.2(5) . . . . ? N3 Co2 O7 C17 4.3(5) . . . . ? O5 Co2 O7 C17 36(5) . . . . ? N6 Co2 O7 C17 -89.4(5) . . . . ? O10 Co2 O7 C17 -173.4(4) . . . . ? O8 Co2 O7 C17 97.0(5) . . . . ? N3 Co2 O8 C18 26.3(9) . . . . ? O5 Co2 O8 C18 120.3(9) . . . . ? N6 Co2 O8 C18 -154(2) . . . . ? O10 Co2 O8 C18 -150.0(9) . . . . ? O7 Co2 O8 C18 -57.4(9) . . . . ? N5 Co3 O9 C19 7.6(6) . . . . ? N2 Co3 O9 C19 -87.2(6) 2_655 . . . ? O2 Co3 O9 C19 -170.9(6) 2_655 . . . ? O11 Co3 O9 C19 34(4) . . . . ? O12 Co3 O9 C19 100.9(6) . . . . ? N3 Co2 O10 C25 63(3) . . . . ? O5 Co2 O10 C25 -86.6(5) . . . . ? N6 Co2 O10 C25 4.4(4) . . . . ? O7 Co2 O10 C25 94.7(5) . . . . ? O8 Co2 O10 C25 -175.1(5) . . . . ? N5 Co3 O11 C26 0.2(5) . . . . ? O9 Co3 O11 C26 -26(4) . . . . ? N2 Co3 O11 C26 95.0(5) 2_655 . . . ? O2 Co3 O11 C26 178.6(5) 2_655 . . . ? O12 Co3 O11 C26 -93.2(5) . . . . ? N5 Co3 O12 C27 -8.8(8) . . . . ? O9 Co3 O12 C27 -102.0(8) . . . . ? N2 Co3 O12 C27 158.1(16) 2_655 . . . ? O2 Co3 O12 C27 167.8(8) 2_655 . . . ? O11 Co3 O12 C27 75.2(8) . . . . ? N4 Co1 N1 C7 78.6(7) . . . . ? O1 Co1 N1 C7 -12.8(7) . . . . ? O6 Co1 N1 C7 137(3) . . . . ? O3 Co1 N1 C7 168.3(7) . . . . ? O4 Co1 N1 C7 -103.5(7) . . . . ? N4 Co1 N1 N2 -87.2(5) . . . . ? O1 Co1 N1 N2 -178.6(4) . . . . ? O6 Co1 N1 N2 -29(3) . . . . ? O3 Co1 N1 N2 2.5(4) . . . . ? O4 Co1 N1 N2 90.7(5) . . . . ? C7 N1 N2 C8 -169.6(6) . . . . ? Co1 N1 N2 C8 -1.0(7) . . . . ? C7 N1 N2 Co3 3.0(7) . . . 2_655 ? Co1 N1 N2 Co3 171.6(3) . . . 2_655 ? O5 Co2 N3 C16 2.5(7) . . . . ? N6 Co2 N3 C16 -88.8(7) . . . . ? O10 Co2 N3 C16 -147(3) . . . . ? O7 Co2 N3 C16 -178.9(7) . . . . ? O8 Co2 N3 C16 91.1(7) . . . . ? O5 Co2 N3 N4 177.2(4) . . . . ? N6 Co2 N3 N4 86.0(4) . . . . ? O10 Co2 N3 N4 28(3) . . . . ? O7 Co2 N3 N4 -4.2(4) . . . . ? O8 Co2 N3 N4 -94.1(4) . . . . ? C16 N3 N4 C17 179.0(6) . . . . ? Co2 N3 N4 C17 3.2(7) . . . . ? C16 N3 N4 Co1 -0.3(7) . . . . ? Co2 N3 N4 Co1 -176.0(3) . . . . ? N1 Co1 N4 C17 -3.8(8) . . . . ? O1 Co1 N4 C17 89.7(8) . . . . ? O6 Co1 N4 C17 -179.9(8) . . . . ? O3 Co1 N4 C17 -87.3(8) . . . . ? O4 Co1 N4 C17 -162(2) . . . . ? N1 Co1 N4 N3 175.2(4) . . . . ? O1 Co1 N4 N3 -91.3(4) . . . . ? O6 Co1 N4 N3 -1.0(4) . . . . ? O3 Co1 N4 N3 91.7(4) . . . . ? O4 Co1 N4 N3 17(3) . . . . ? O9 Co3 N5 C25 -8.3(7) . . . . ? N2 Co3 N5 C25 83.8(7) 2_655 . . . ? O2 Co3 N5 C25 148(3) 2_655 . . . ? O11 Co3 N5 C25 173.0(7) . . . . ? O12 Co3 N5 C25 -98.0(7) . . . . ? O9 Co3 N5 N6 178.2(4) . . . . ? N2 Co3 N5 N6 -89.6(4) 2_655 . . . ? O2 Co3 N5 N6 -26(4) 2_655 . . . ? O11 Co3 N5 N6 -0.4(4) . . . . ? O12 Co3 N5 N6 88.5(4) . . . . ? C25 N5 N6 C26 -174.3(6) . . . . ? Co3 N5 N6 C26 0.5(7) . . . . ? C25 N5 N6 Co2 5.6(7) . . . . ? Co3 N5 N6 Co2 -179.6(3) . . . . ? N3 Co2 N6 C26 -2.0(8) . . . . ? O5 Co2 N6 C26 -96.1(8) . . . . ? O10 Co2 N6 C26 174.4(8) . . . . ? O7 Co2 N6 C26 81.7(8) . . . . ? O8 Co2 N6 C26 179(2) . . . . ? N3 Co2 N6 N5 178.2(4) . . . . ? O5 Co2 N6 N5 84.1(4) . . . . ? O10 Co2 N6 N5 -5.4(4) . . . . ? O7 Co2 N6 N5 -98.1(4) . . . . ? O8 Co2 N6 N5 -1(3) . . . . ? Co1 O1 C1 C6 171.0(6) . . . . ? Co1 O1 C1 C2 -9.0(11) . . . . ? O1 C1 C2 C3 -179.2(8) . . . . ? C6 C1 C2 C3 0.8(13) . . . . ? O1 C1 C2 C7 2.1(13) . . . . ? C6 C1 C2 C7 -177.9(8) . . . . ? C1 C2 C3 C4 0.5(15) . . . . ? C7 C2 C3 C4 179.3(9) . . . . ? C2 C3 C4 C5 -0.3(17) . . . . ? C3 C4 C5 C6 -1.2(18) . . . . ? C4 C5 C6 C1 2.5(18) . . . . ? O1 C1 C6 C5 177.7(9) . . . . ? C2 C1 C6 C5 -2.3(15) . . . . ? Co3 O2 C7 N1 3.4(8) 2_655 . . . ? Co3 O2 C7 C2 -176.3(6) 2_655 . . . ? N2 N1 C7 O2 -4.3(9) . . . . ? Co1 N1 C7 O2 -170.1(5) . . . . ? N2 N1 C7 C2 175.3(6) . . . . ? Co1 N1 C7 C2 9.6(10) . . . . ? C3 C2 C7 O2 -0.9(12) . . . . ? C1 C2 C7 O2 177.8(7) . . . . ? C3 C2 C7 N1 179.4(8) . . . . ? C1 C2 C7 N1 -1.8(12) . . . . ? Co1 O3 C8 N2 4.1(9) . . . . ? N1 N2 C8 O3 -2.2(10) . . . . ? Co3 N2 C8 O3 -172.0(5) 2_655 . . . ? C9C O4 C9A C9B 32(4) . . . . ? Co1 O4 C9A C9B -103(3) . . . . ? C9B O4 C9A C9C -32(4) . . . . ? Co1 O4 C9A C9C -135(3) . . . . ? O4 C9A C9B C9C -40(5) . . . . ? C9C C9A C9B O4 40(5) . . . . ? C9C O4 C9B C9A -139(6) . . . . ? Co1 O4 C9B C9A 105(3) . . . . ? C9A O4 C9B C9C 139(6) . . . . ? Co1 O4 C9B C9C -116(4) . . . . ? C9A C9B C9C O4 45(5) . . . . ? C9A C9B C9C O15B -139(10) . . . 2 ? O4 C9B C9C O15B 176(12) . . . 2 ? O4 C9B C9C C9A -45(5) . . . . ? C9A O4 C9C C9B -24(3) . . . . ? Co1 O4 C9C C9B 108(3) . . . . ? C9B O4 C9C O15B -175(16) . . . 2 ? C9A O4 C9C O15B 161(14) . . . 2 ? Co1 O4 C9C O15B -66(15) . . . 2 ? C9B O4 C9C C9A 24(3) . . . . ? Co1 O4 C9C C9A 132(3) . . . . ? O4 C9A C9C C9B 122(7) . . . . ? C9B C9A C9C O4 -122(7) . . . . ? C9B C9A C9C O15B 80(15) . . . 2 ? O4 C9A C9C O15B -158(16) . . . 2 ? Co2 O5 C10 C15 -176.4(6) . . . . ? Co2 O5 C10 C11 3.7(10) . . . . ? O5 C10 C11 C12 177.7(7) . . . . ? C15 C10 C11 C12 -2.1(11) . . . . ? O5 C10 C11 C16 -2.2(11) . . . . ? C15 C10 C11 C16 177.9(7) . . . . ? C10 C11 C12 C13 1.5(12) . . . . ? C16 C11 C12 C13 -178.6(8) . . . . ? C11 C12 C13 C14 -0.8(14) . . . . ? C12 C13 C14 C15 0.7(17) . . . . ? C13 C14 C15 C10 -1.4(17) . . . . ? O5 C10 C15 C14 -177.8(9) . . . . ? C11 C10 C15 C14 2.1(13) . . . . ? Co1 O6 C16 N3 -3.0(8) . . . . ? Co1 O6 C16 C11 175.7(5) . . . . ? N4 N3 C16 O6 2.2(9) . . . . ? Co2 N3 C16 O6 176.9(5) . . . . ? N4 N3 C16 C11 -176.5(5) . . . . ? Co2 N3 C16 C11 -1.8(10) . . . . ? C12 C11 C16 O6 2.5(10) . . . . ? C10 C11 C16 O6 -177.6(6) . . . . ? C12 C11 C16 N3 -178.8(7) . . . . ? C10 C11 C16 N3 1.1(10) . . . . ? N3 N4 C17 O7 0.6(9) . . . . ? Co1 N4 C17 O7 179.6(5) . . . . ? Co2 O7 C17 N4 -3.9(8) . . . . ? Co3 O9 C19 C24 176.3(5) . . . . ? Co3 O9 C19 C20 -4.9(10) . . . . ? O9 C19 C20 C21 -179.6(7) . . . . ? C24 C19 C20 C21 -0.8(11) . . . . ? O9 C19 C20 C25 -0.7(11) . . . . ? C24 C19 C20 C25 178.1(7) . . . . ? C19 C20 C21 C22 0.5(12) . . . . ? C25 C20 C21 C22 -178.4(8) . . . . ? C20 C21 C22 C23 -1.5(14) . . . . ? C21 C22 C23 C24 2.7(16) . . . . ? C22 C23 C24 C19 -3.2(16) . . . . ? O9 C19 C24 C23 -178.9(8) . . . . ? C20 C19 C24 C23 2.2(13) . . . . ? Co2 O10 C25 N5 -2.5(8) . . . . ? Co2 O10 C25 C20 176.7(5) . . . . ? N6 N5 C25 O10 -2.1(9) . . . . ? Co3 N5 C25 O10 -175.5(5) . . . . ? N6 N5 C25 C20 178.7(5) . . . . ? Co3 N5 C25 C20 5.3(10) . . . . ? C21 C20 C25 O10 0.5(10) . . . . ? C19 C20 C25 O10 -178.4(7) . . . . ? C21 C20 C25 N5 179.7(7) . . . . ? C19 C20 C25 N5 0.8(10) . . . . ? Co3 O11 C26 N6 0.0(8) . . . . ? N5 N6 C26 O11 -0.4(10) . . . . ? Co2 N6 C26 O11 179.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.734 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.109 data_4 #C64 H104 N18 O36 Co6 _database_code_CSD 141232 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C64 H104 Co6 N18 O36 _chemical_formula_sum 'C64 H104 Co6 N18 O36' _chemical_formula_weight 2055.23 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 11.510(3) _cell_length_b 13.970(3) _cell_length_c 15.748(6) _cell_angle_alpha 111.40(2) _cell_angle_beta 90.63(3) _cell_angle_gamma 105.62(2) _cell_volume 2254(1) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour brown-black _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART 1000 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11802 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0881 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7868 _reflns_number_gt 4838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens (1995) ASTRO and SAINT' _computing_cell_refinement 'Siemens (1995) ASTRO and SAINT' _computing_data_reduction 'Siemens (1995) ASTRO and SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL/PC (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1030P)^2^+1.1842P] 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 7868 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1238 _refine_ls_goodness_of_fit_ref 0.848 _refine_ls_restrained_S_all 0.848 _refine_ls_shift/su_max 1.056 _refine_ls_shift/su_mean 0.004 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 0.68483(6) 0.20680(5) 0.27473(5) 0.0323(2) Uani 1 1 d . . . Co2 Co 0.78451(6) 0.29895(5) 0.03672(5) 0.0298(2) Uani 1 1 d . . . Co3 Co 0.50482(6) 0.14003(5) -0.20958(5) 0.0327(2) Uani 1 1 d . . . O1 O 0.8480(3) 0.2375(3) 0.3173(2) 0.0406(9) Uani 1 1 d . . . O2 O 0.6507(3) -0.0847(3) 0.2808(2) 0.0376(9) Uani 1 1 d . . . O3 O 0.5165(3) 0.1692(3) 0.2309(2) 0.0359(8) Uani 1 1 d . . . O4 O 0.6437(4) 0.2378(3) 0.3986(2) 0.0592(12) Uani 1 1 d . . . H44A H 0.5820 0.1657 0.4103 0.08(2) Uiso 1 1 d R . . O5 O 0.7683(3) 0.4357(3) 0.0599(3) 0.0428(9) Uani 1 1 d . . . O6 O 0.7057(3) 0.3531(3) 0.2951(2) 0.0377(9) Uani 1 1 d . . . O7 O 0.8000(3) 0.1602(3) 0.0184(2) 0.0337(8) Uani 1 1 d . . . O8 O 0.9529(3) 0.3604(3) 0.0972(3) 0.0417(9) Uani 1 1 d . . . H48A H 0.9508 0.3818 0.1754 0.22(5) Uiso 1 1 d R . . O9 O 0.5835(3) 0.1058(3) -0.3145(2) 0.0419(9) Uani 1 1 d . . . O10 O 0.8444(3) 0.2907(3) -0.0764(2) 0.0342(8) Uani 1 1 d . . . O11 O 0.4331(3) 0.1776(3) -0.0980(2) 0.0358(8) Uani 1 1 d . . . O12 O 0.5119(3) 0.2802(3) -0.2117(3) 0.0470(10) Uani 1 1 d . . . H52A H 0.5751 0.3389 -0.1580 0.10(3) Uiso 1 1 d R . . N1 N 0.6474(3) 0.0629(3) 0.2557(3) 0.0297(9) Uani 1 1 d . . . N2 N 0.5263(4) 0.0025(3) 0.2144(3) 0.0322(10) Uani 1 1 d . . . N3 N 0.3494(4) 0.0276(4) 0.1654(3) 0.0511(13) Uani 1 1 d . . . H03A H 0.3187 -0.0414 0.1325 0.051(18) Uiso 1 1 d R . . H03B H 0.3345 0.0815 0.1433 0.066(19) Uiso 1 1 d R . . N4 N 0.7331(4) 0.2943(3) 0.1462(3) 0.0293(9) Uani 1 1 d . . . N5 N 0.7244(4) 0.1961(3) 0.1555(3) 0.0306(10) Uani 1 1 d . . . N6 N 0.7605(5) 0.0319(3) 0.0787(3) 0.0487(13) Uani 1 1 d . . . H06A H 0.7053 -0.0014 0.1168 0.053(17) Uiso 1 1 d R . . H06B H 0.7652 -0.0142 0.0155 0.09(2) Uiso 1 1 d R . . N7 N 0.6482(4) 0.2009(3) -0.1304(3) 0.0290(9) Uani 1 1 d . . . N8 N 0.6311(4) 0.2304(3) -0.0369(3) 0.0313(10) Uani 1 1 d . . . N9 N 0.4756(4) 0.2355(4) 0.0562(3) 0.0428(11) Uani 1 1 d . . . H09A H 0.3891 0.2151 0.0595 0.044(15) Uiso 1 1 d R . . H09B H 0.5169 0.2241 0.1194 0.12(3) Uiso 1 1 d R . . C1 C 0.8941(5) 0.1713(4) 0.3407(4) 0.0368(13) Uani 1 1 d . . . C2 C 0.8310(4) 0.0662(4) 0.3311(3) 0.0337(12) Uani 1 1 d . . . C3 C 0.8923(5) 0.0057(5) 0.3590(4) 0.0450(14) Uani 1 1 d . . . H3A H 0.8509 -0.0641 0.3526 0.054 Uiso 1 1 calc R . . C4 C 1.0133(6) 0.0490(5) 0.3958(4) 0.0577(17) Uani 1 1 d . . . H4A H 1.0529 0.0084 0.4138 0.069 Uiso 1 1 calc R . . C5 C 1.0741(5) 0.1514(5) 0.4056(5) 0.0581(17) Uani 1 1 d . . . H5A H 1.1553 0.1806 0.4304 0.070 Uiso 1 1 calc R . . C6 C 1.0162(5) 0.2116(5) 0.3789(4) 0.0498(15) Uani 1 1 d . . . H6A H 1.0594 0.2814 0.3865 0.060 Uiso 1 1 calc R . . C7 C 0.7046(5) 0.0129(4) 0.2886(3) 0.0318(12) Uani 1 1 d . . . C8 C 0.4667(5) 0.0670(4) 0.2042(3) 0.0356(12) Uani 1 1 d . . . C9 C 0.7077(7) 0.3282(5) 0.4768(4) 0.074(2) Uani 1 1 d . . . H9A H 0.7525 0.3086 0.5235 0.32(9) Uiso 1 1 d R . . H9B H 0.6519 0.3655 0.5077 0.382 Uiso 1 1 d R . . H9C H 0.7664 0.3763 0.4569 0.382 Uiso 1 1 d R . . C10 C 0.7561(5) 0.5036(4) 0.1431(4) 0.0388(13) Uani 1 1 d . . . C11 C 0.7369(5) 0.4782(4) 0.2212(4) 0.0370(13) Uani 1 1 d . . . C12 C 0.7248(5) 0.5585(4) 0.3033(4) 0.0452(14) Uani 1 1 d . . . H12A H 0.7120 0.5422 0.3553 0.054 Uiso 1 1 calc R . . C13 C 0.7314(5) 0.6594(4) 0.3087(5) 0.0553(17) Uani 1 1 d . . . H13A H 0.7234 0.7111 0.3639 0.066 Uiso 1 1 calc R . . C14 C 0.7498(6) 0.6843(5) 0.2325(5) 0.0561(17) Uani 1 1 d . . . H14A H 0.7529 0.7527 0.2356 0.067 Uiso 1 1 calc R . . C15 C 0.7638(5) 0.6082(4) 0.1514(4) 0.0463(15) Uani 1 1 d . . . H15A H 0.7788 0.6269 0.1008 0.056 Uiso 1 1 calc R . . C16 C 0.7257(5) 0.3718(4) 0.2211(4) 0.0337(12) Uani 1 1 d . . . C17 C 0.7609(4) 0.1308(4) 0.0840(3) 0.0300(11) Uani 1 1 d . . . C18 C 1.0398(6) 0.4451(5) 0.0836(5) 0.067(2) Uani 1 1 d . . . H18A H 1.1162 0.4804 0.1325 0.08(2) Uiso 1 1 d R . . H18B H 1.0022 0.4992 0.0852 0.096 Uiso 1 1 d R . . H18C H 1.0650 0.4179 0.0237 0.096 Uiso 1 1 d R . . C19 C 0.7011(5) 0.1541(4) -0.3165(4) 0.0388(13) Uani 1 1 d . . . C20 C 0.7885(5) 0.2149(4) -0.2391(3) 0.0349(12) Uani 1 1 d . . . C21 C 0.9085(5) 0.2586(4) -0.2524(4) 0.0422(14) Uani 1 1 d . . . H21A H 0.9667 0.2990 -0.2014 0.051 Uiso 1 1 calc R . . C22 C 0.9423(5) 0.2435(5) -0.3380(4) 0.0503(15) Uani 1 1 d . . . H22A H 1.0225 0.2729 -0.3452 0.060 Uiso 1 1 calc R . . C23 C 0.8564(6) 0.1845(5) -0.4134(4) 0.0523(16) Uani 1 1 d . . . H23A H 0.8789 0.1740 -0.4720 0.063 Uiso 1 1 calc R . . C24 C 0.7379(5) 0.1409(5) -0.4036(4) 0.0493(15) Uani 1 1 d . . . H24A H 0.6811 0.1019 -0.4556 0.059 Uiso 1 1 calc R . . C25 C 0.7599(4) 0.2364(4) -0.1451(3) 0.0304(11) Uani 1 1 d . . . C26 C 0.5129(4) 0.2134(4) -0.0276(4) 0.0316(12) Uani 1 1 d . . . C27 C 0.5445(8) 0.3091(8) -0.2894(7) 0.091(3) Uani 1 1 d . . . H27A H 0.5040 0.2563 -0.3426 0.26(8) Uiso 1 1 d R . . H27B H 0.6303 0.3222 -0.2922 0.315 Uiso 1 1 d R . . H27C H 0.5252 0.3742 -0.2822 0.315 Uiso 1 1 d R . . C28 C 0.0326(9) 0.4837(6) 0.3429(6) 0.096(3) Uani 1 1 d . . . H28A H 0.1202 0.5194 0.3374 0.11(3) Uiso 1 1 d R . . H28B H 0.0270 0.4731 0.3998 0.127 Uiso 1 1 d R . . H28C H -0.0184 0.5270 0.3402 0.127 Uiso 1 1 d R . . O13 O -0.0021(4) 0.3854(3) 0.2687(3) 0.0586(12) Uani 1 1 d . . . H53A H -0.0521 0.3203 0.2748 0.09(2) Uiso 1 1 d R . . C29 C 0.3855(8) 0.4535(6) 0.0714(7) 0.101(3) Uani 1 1 d . . . H29A H 0.4022 0.4374 0.1217 0.16(4) Uiso 1 1 d R . . H29B H 0.4545 0.4517 0.0378 0.189 Uiso 1 1 d R . . H29C H 0.3185 0.3949 0.0328 0.189 Uiso 1 1 d R . . O14 O 0.3589(6) 0.5503(4) 0.0797(4) 0.0974(19) Uani 1 1 d . . . H54A H 0.2951 0.5405 0.0259 0.14(4) Uiso 1 1 d R . . C30 C 0.3795(9) 0.1271(8) 0.4566(9) 0.153(6) Uani 1 1 d . . . H30A H 0.3054 0.0800 0.4577 0.22(6) Uiso 1 1 d R . . H30B H 0.3658 0.1556 0.4117 0.265 Uiso 1 1 d R . . H30C H 0.3978 0.1861 0.5152 0.265 Uiso 1 1 d R . . O15 O 0.4861(4) 0.0973(4) 0.4372(3) 0.0642(13) Uani 1 1 d . . . H55A H 0.4356 0.0365 0.3889 0.21(6) Uiso 1 1 d R . . C31 C 0.1531(13) 0.1891(11) 0.1607(9) 0.186(7) Uani 1 1 d . . . H31A H 0.1467 0.1601 0.1981 0.13(4) Uiso 1 1 d R . . H31B H 0.0720 0.1850 0.1410 0.156 Uiso 1 1 d R . . H31C H 0.1943 0.2639 0.1944 0.156 Uiso 1 1 d R . . O16 O 0.2052(4) 0.1572(4) 0.0837(4) 0.0785(15) Uani 1 1 d . . . H56A H 0.1609 0.1610 0.0312 0.41(13) Uiso 1 1 d R . . C32 C 0.0411(11) 0.1198(10) -0.1258(8) 0.137(4) Uani 1 1 d . . . H32A H -0.0092 0.1324 -0.1774 0.21(6) Uiso 1 1 d R . . H32B H 0.0058 0.0461 -0.1336 0.257 Uiso 1 1 d R . . H32C H 0.1218 0.1258 -0.1427 0.257 Uiso 1 1 d R . . O17 O 0.0541(7) 0.1744(9) -0.0376(6) 0.191(5) Uani 1 1 d . . . H57A H -0.0224 0.1829 -0.0091 0.33(10) Uiso 1 1 d R . . O18 O 0.4190(13) 0.3948(10) 0.3711(10) 0.384(12) Uani 1 1 d . . . H58A H 0.4952 0.4062 0.3880 0.000(9) Uiso 1 1 d R . . H58B H 0.3976 0.3223 0.3713 0.031(14) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0357(4) 0.0285(4) 0.0295(4) 0.0099(3) 0.0017(3) 0.0062(3) Co2 0.0288(4) 0.0274(4) 0.0323(4) 0.0118(3) 0.0017(3) 0.0065(3) Co3 0.0292(4) 0.0318(4) 0.0368(4) 0.0160(3) -0.0020(3) 0.0047(3) O1 0.033(2) 0.040(2) 0.046(2) 0.0210(18) -0.0075(17) 0.0003(16) O2 0.032(2) 0.035(2) 0.047(2) 0.0222(17) -0.0080(16) 0.0031(16) O3 0.034(2) 0.030(2) 0.042(2) 0.0112(16) -0.0003(16) 0.0110(16) O4 0.071(3) 0.048(3) 0.031(2) 0.0028(19) 0.010(2) -0.009(2) O5 0.056(2) 0.033(2) 0.042(2) 0.0170(18) 0.0007(19) 0.0135(18) O6 0.049(2) 0.0280(19) 0.031(2) 0.0056(16) 0.0078(17) 0.0114(16) O7 0.039(2) 0.033(2) 0.030(2) 0.0119(16) 0.0073(16) 0.0124(16) O8 0.031(2) 0.043(2) 0.045(2) 0.0190(18) -0.0029(17) -0.0028(16) O9 0.038(2) 0.049(2) 0.030(2) 0.0135(17) -0.0021(16) 0.0009(17) O10 0.0258(18) 0.039(2) 0.035(2) 0.0170(16) 0.0008(16) 0.0000(15) O11 0.0264(19) 0.038(2) 0.041(2) 0.0140(17) 0.0007(16) 0.0080(15) O12 0.046(2) 0.039(2) 0.060(3) 0.028(2) -0.005(2) 0.0052(18) N1 0.029(2) 0.031(2) 0.027(2) 0.0124(18) -0.0044(18) 0.0044(18) N2 0.030(2) 0.028(2) 0.034(2) 0.0100(19) -0.0050(18) 0.0039(18) N3 0.034(3) 0.037(3) 0.076(4) 0.020(3) -0.016(2) 0.004(2) N4 0.033(2) 0.023(2) 0.030(2) 0.0084(18) 0.0008(18) 0.0077(18) N5 0.039(2) 0.024(2) 0.027(2) 0.0074(18) 0.0015(19) 0.0104(19) N6 0.078(4) 0.029(3) 0.046(3) 0.016(2) 0.022(3) 0.024(2) N7 0.030(2) 0.029(2) 0.026(2) 0.0118(18) 0.0016(17) 0.0051(18) N8 0.027(2) 0.030(2) 0.035(3) 0.0123(19) 0.0040(18) 0.0054(18) N9 0.028(3) 0.058(3) 0.044(3) 0.021(2) 0.011(2) 0.012(2) C1 0.036(3) 0.037(3) 0.034(3) 0.013(2) 0.004(2) 0.006(2) C2 0.029(3) 0.042(3) 0.028(3) 0.012(2) 0.003(2) 0.009(2) C3 0.043(3) 0.047(4) 0.043(3) 0.016(3) -0.003(3) 0.013(3) C4 0.044(4) 0.061(4) 0.074(5) 0.033(4) -0.008(3) 0.018(3) C5 0.028(3) 0.073(5) 0.077(5) 0.038(4) -0.007(3) 0.007(3) C6 0.032(3) 0.056(4) 0.060(4) 0.031(3) -0.003(3) -0.001(3) C7 0.035(3) 0.033(3) 0.027(3) 0.011(2) 0.001(2) 0.008(2) C8 0.037(3) 0.035(3) 0.033(3) 0.009(2) 0.002(2) 0.013(3) C9 0.111(6) 0.050(4) 0.033(4) 0.001(3) -0.002(4) 0.003(4) C10 0.028(3) 0.031(3) 0.052(4) 0.013(3) -0.001(2) 0.006(2) C11 0.032(3) 0.026(3) 0.049(4) 0.011(3) 0.006(2) 0.008(2) C12 0.042(3) 0.036(3) 0.050(4) 0.009(3) 0.010(3) 0.010(3) C13 0.049(4) 0.026(3) 0.075(5) 0.002(3) 0.008(3) 0.010(3) C14 0.055(4) 0.029(3) 0.080(5) 0.016(3) 0.005(3) 0.012(3) C15 0.045(3) 0.030(3) 0.062(4) 0.019(3) -0.001(3) 0.006(3) C16 0.033(3) 0.027(3) 0.035(3) 0.007(2) 0.004(2) 0.006(2) C17 0.028(3) 0.027(3) 0.034(3) 0.010(2) 0.000(2) 0.009(2) C18 0.048(4) 0.071(5) 0.068(5) 0.034(4) -0.005(3) -0.015(3) C19 0.037(3) 0.040(3) 0.042(3) 0.021(3) 0.004(3) 0.008(3) C20 0.033(3) 0.038(3) 0.033(3) 0.015(2) 0.004(2) 0.007(2) C21 0.036(3) 0.047(3) 0.041(3) 0.017(3) 0.007(3) 0.007(3) C22 0.038(3) 0.064(4) 0.051(4) 0.029(3) 0.012(3) 0.007(3) C23 0.053(4) 0.068(4) 0.039(4) 0.025(3) 0.014(3) 0.016(3) C24 0.049(4) 0.058(4) 0.037(3) 0.019(3) 0.000(3) 0.008(3) C25 0.030(3) 0.029(3) 0.031(3) 0.013(2) 0.000(2) 0.004(2) C26 0.030(3) 0.026(3) 0.037(3) 0.010(2) 0.001(2) 0.009(2) C27 0.104(7) 0.096(6) 0.116(7) 0.078(6) 0.020(6) 0.045(5) C28 0.112(8) 0.059(5) 0.089(6) 0.026(5) -0.027(5) -0.014(5) O13 0.054(3) 0.054(3) 0.054(3) 0.024(2) -0.014(2) -0.009(2) C29 0.119(8) 0.063(5) 0.131(8) 0.045(5) -0.020(6) 0.033(5) O14 0.143(5) 0.044(3) 0.093(4) 0.017(3) -0.050(4) 0.023(3) C30 0.085(7) 0.073(6) 0.260(16) 0.017(7) 0.073(9) 0.023(6) O15 0.054(3) 0.062(3) 0.059(3) 0.017(2) 0.015(2) -0.001(2) C31 0.271(19) 0.259(17) 0.120(10) 0.082(12) 0.089(12) 0.203(16) O16 0.065(3) 0.079(4) 0.086(4) 0.013(3) 0.027(3) 0.038(3) C32 0.198(13) 0.182(12) 0.092(8) 0.068(8) 0.033(8) 0.128(10) O17 0.127(7) 0.326(13) 0.118(7) 0.023(7) 0.019(5) 0.153(8) O18 0.270(18) 0.208(14) 0.59(3) 0.060(16) 0.023(18) 0.071(12) _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 N1 1.846(4) . ? Co1 O1 1.867(4) . ? Co1 O6 1.895(3) . ? Co1 N5 1.899(4) . ? Co1 O3 1.914(3) . ? Co1 O4 1.932(4) . ? Co2 N4 1.847(4) . ? Co2 O5 1.871(4) . ? Co2 O10 1.893(3) . ? Co2 N8 1.901(4) . ? Co2 O7 1.911(3) . ? Co2 O8 1.967(3) . ? Co3 N7 1.851(4) . ? Co3 O9 1.862(4) . ? Co3 N2 1.898(4) 2_655 ? Co3 O11 1.907(4) . ? Co3 O2 1.907(3) 2_655 ? Co3 O12 1.950(4) . ? O1 C1 1.335(6) . ? O2 C7 1.296(6) . ? O2 Co3 1.907(3) 2_655 ? O3 C8 1.288(6) . ? O4 C9 1.414(7) . ? O4 H44A 1.1427 . ? O5 C10 1.343(6) . ? O6 C16 1.294(6) . ? O7 C17 1.288(6) . ? O8 C18 1.414(6) . ? O8 H48A 1.1592 . ? O9 C19 1.347(6) . ? O10 C25 1.293(6) . ? O11 C26 1.284(6) . ? O12 C27 1.447(8) . ? O12 H52A 1.0374 . ? N1 C7 1.301(6) . ? N1 N2 1.422(5) . ? N2 C8 1.320(6) . ? N2 Co3 1.898(4) 2_655 ? N3 C8 1.355(6) . ? N3 H03A 0.8775 . ? N3 H03B 0.9878 . ? N4 C16 1.301(6) . ? N4 N5 1.409(5) . ? N5 C17 1.321(6) . ? N6 C17 1.352(6) . ? N6 H06A 1.0165 . ? N6 H06B 0.9793 . ? N7 C25 1.303(6) . ? N7 N8 1.408(5) . ? N8 C26 1.335(6) . ? N9 C26 1.345(6) . ? N9 H09A 0.9671 . ? N9 H09B 1.1777 . ? C1 C6 1.401(7) . ? C1 C2 1.403(7) . ? C2 C3 1.410(7) . ? C2 C7 1.466(7) . ? C3 C4 1.383(8) . ? C3 H3A 0.9300 . ? C4 C5 1.363(8) . ? C4 H4A 0.9300 . ? C5 C6 1.371(8) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C9 H9A 1.0465 . ? C9 H9B 0.9599 . ? C9 H9C 0.9598 . ? C10 C15 1.396(7) . ? C10 C11 1.404(8) . ? C11 C12 1.407(7) . ? C11 C16 1.456(7) . ? C12 C13 1.362(8) . ? C12 H12A 0.9300 . ? C13 C14 1.370(9) . ? C13 H13A 0.9300 . ? C14 C15 1.376(8) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C18 H18A 1.0405 . ? C18 H18B 0.9600 . ? C18 H18C 0.9601 . ? C19 C24 1.402(7) . ? C19 C20 1.406(7) . ? C20 C21 1.403(7) . ? C20 C25 1.460(7) . ? C21 C22 1.364(7) . ? C21 H21A 0.9300 . ? C22 C23 1.374(8) . ? C22 H22A 0.9300 . ? C23 C24 1.371(8) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C27 H27A 0.9041 . ? C27 H27B 0.9598 . ? C27 H27C 0.9600 . ? C28 O13 1.391(8) . ? C28 H28A 1.0175 . ? C28 H28B 0.9599 . ? C28 H28C 0.9600 . ? O13 H53A 0.9745 . ? C29 O14 1.427(8) . ? C29 H29A 0.9296 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? O14 H54A 1.0594 . ? C30 O15 1.401(9) . ? C30 H30A 0.9304 . ? C30 H30B 0.9601 . ? C30 H30C 0.9601 . ? O15 H44A 1.4313 . ? O15 H55A 0.9437 . ? C31 O16 1.339(11) . ? C31 H31A 0.8230 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? O16 H56A 0.9922 . ? C32 O17 1.302(11) . ? C32 H32A 1.0847 . ? C32 H32B 0.9601 . ? C32 H32C 0.9599 . ? O17 H57A 1.0088 . ? O18 H58A 0.8681 . ? O18 H58B 0.9775 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 O1 94.28(17) . . ? N1 Co1 O6 174.00(17) . . ? O1 Co1 O6 91.23(16) . . ? N1 Co1 N5 98.31(17) . . ? O1 Co1 N5 91.24(17) . . ? O6 Co1 N5 83.91(16) . . ? N1 Co1 O3 83.25(16) . . ? O1 Co1 O3 177.53(15) . . ? O6 Co1 O3 91.22(15) . . ? N5 Co1 O3 89.33(17) . . ? N1 Co1 O4 89.52(17) . . ? O1 Co1 O4 90.13(18) . . ? O6 Co1 O4 88.10(16) . . ? N5 Co1 O4 171.92(18) . . ? O3 Co1 O4 89.63(17) . . ? N4 Co2 O5 94.49(17) . . ? N4 Co2 O10 173.48(16) . . ? O5 Co2 O10 91.76(16) . . ? N4 Co2 N8 97.77(17) . . ? O5 Co2 N8 91.98(17) . . ? O10 Co2 N8 83.87(16) . . ? N4 Co2 O7 83.08(16) . . ? O5 Co2 O7 177.52(15) . . ? O10 Co2 O7 90.66(15) . . ? N8 Co2 O7 88.81(16) . . ? N4 Co2 O8 89.03(17) . . ? O5 Co2 O8 91.73(16) . . ? O10 Co2 O8 88.91(15) . . ? N8 Co2 O8 171.97(16) . . ? O7 Co2 O8 87.78(15) . . ? N7 Co3 O9 93.65(16) . . ? N7 Co3 N2 97.80(17) . 2_655 ? O9 Co3 N2 90.44(17) . 2_655 ? N7 Co3 O11 83.09(16) . . ? O9 Co3 O11 176.72(15) . . ? N2 Co3 O11 89.63(16) 2_655 . ? N7 Co3 O2 174.12(16) . 2_655 ? O9 Co3 O2 91.98(16) . 2_655 ? N2 Co3 O2 83.81(16) 2_655 2_655 ? O11 Co3 O2 91.28(15) . 2_655 ? N7 Co3 O12 90.18(17) . . ? O9 Co3 O12 91.57(17) . . ? N2 Co3 O12 171.62(17) 2_655 . ? O11 Co3 O12 88.82(16) . . ? O2 Co3 O12 88.00(15) 2_655 . ? C1 O1 Co1 124.5(3) . . ? C7 O2 Co3 111.7(3) . 2_655 ? C8 O3 Co1 110.7(3) . . ? C9 O4 Co1 125.2(4) . . ? C9 O4 H44A 117.7 . . ? Co1 O4 H44A 114.6 . . ? C10 O5 Co2 123.9(3) . . ? C16 O6 Co1 111.8(3) . . ? C17 O7 Co2 111.1(3) . . ? C18 O8 Co2 123.9(4) . . ? C18 O8 H48A 108.8 . . ? Co2 O8 H48A 108.3 . . ? C19 O9 Co3 123.7(3) . . ? C25 O10 Co2 111.7(3) . . ? C26 O11 Co3 111.4(3) . . ? C27 O12 Co3 123.0(5) . . ? C27 O12 H52A 103.2 . . ? Co3 O12 H52A 108.5 . . ? C7 N1 N2 114.6(4) . . ? C7 N1 Co1 130.1(3) . . ? N2 N1 Co1 113.9(3) . . ? C8 N2 N1 109.9(4) . . ? C8 N2 Co3 139.6(4) . 2_655 ? N1 N2 Co3 109.5(3) . 2_655 ? C8 N3 H03A 119.8 . . ? C8 N3 H03B 106.0 . . ? H03A N3 H03B 120.6 . . ? C16 N4 N5 114.9(4) . . ? C16 N4 Co2 129.9(4) . . ? N5 N4 Co2 113.8(3) . . ? C17 N5 N4 110.7(4) . . ? C17 N5 Co1 139.2(4) . . ? N4 N5 Co1 109.4(3) . . ? C17 N6 H06A 118.0 . . ? C17 N6 H06B 110.9 . . ? H06A N6 H06B 118.2 . . ? C25 N7 N8 114.4(4) . . ? C25 N7 Co3 130.7(4) . . ? N8 N7 Co3 113.8(3) . . ? C26 N8 N7 110.3(4) . . ? C26 N8 Co2 139.6(4) . . ? N7 N8 Co2 109.5(3) . . ? C26 N9 H09A 117.7 . . ? C26 N9 H09B 127.5 . . ? H09A N9 H09B 103.5 . . ? O1 C1 C6 116.6(5) . . ? O1 C1 C2 125.8(5) . . ? C6 C1 C2 117.6(5) . . ? C1 C2 C3 119.3(5) . . ? C1 C2 C7 123.1(5) . . ? C3 C2 C7 117.6(5) . . ? C4 C3 C2 120.8(5) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C5 C4 C3 119.7(6) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 120.4(6) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 122.1(6) . . ? C5 C6 H6A 119.0 . . ? C1 C6 H6A 119.0 . . ? O2 C7 N1 119.7(5) . . ? O2 C7 C2 120.6(4) . . ? N1 C7 C2 119.6(5) . . ? O3 C8 N2 121.9(5) . . ? O3 C8 N3 117.2(5) . . ? N2 C8 N3 120.8(5) . . ? O4 C9 H9A 113.5 . . ? O4 C9 H9B 109.1 . . ? H9A C9 H9B 108.9 . . ? O4 C9 H9C 108.6 . . ? H9A C9 H9C 108.9 . . ? H9B C9 H9C 107.7 . . ? O5 C10 C15 116.4(5) . . ? O5 C10 C11 125.5(5) . . ? C15 C10 C11 118.0(5) . . ? C10 C11 C12 118.6(5) . . ? C10 C11 C16 123.3(5) . . ? C12 C11 C16 118.0(5) . . ? C13 C12 C11 121.8(6) . . ? C13 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? C12 C13 C14 119.7(6) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C13 C14 C15 120.0(6) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C14 C15 C10 121.8(6) . . ? C14 C15 H15A 119.1 . . ? C10 C15 H15A 119.1 . . ? O6 C16 N4 119.5(5) . . ? O6 C16 C11 120.2(4) . . ? N4 C16 C11 120.3(5) . . ? O7 C17 N5 121.0(4) . . ? O7 C17 N6 118.2(4) . . ? N5 C17 N6 120.8(5) . . ? O8 C18 H18A 113.5 . . ? O8 C18 H18B 108.8 . . ? H18A C18 H18B 108.9 . . ? O8 C18 H18C 108.9 . . ? H18A C18 H18C 108.9 . . ? H18B C18 H18C 107.7 . . ? O9 C19 C24 116.4(5) . . ? O9 C19 C20 125.4(5) . . ? C24 C19 C20 118.2(5) . . ? C21 C20 C19 118.8(5) . . ? C21 C20 C25 118.2(5) . . ? C19 C20 C25 123.0(5) . . ? C22 C21 C20 121.8(5) . . ? C22 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? C21 C22 C23 119.2(5) . . ? C21 C22 H22A 120.4 . . ? C23 C22 H22A 120.4 . . ? C24 C23 C22 120.9(6) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C19 121.1(5) . . ? C23 C24 H24A 119.5 . . ? C19 C24 H24A 119.5 . . ? O10 C25 N7 119.9(4) . . ? O10 C25 C20 120.4(4) . . ? N7 C25 C20 119.6(4) . . ? O11 C26 N8 120.9(5) . . ? O11 C26 N9 118.8(4) . . ? N8 C26 N9 120.3(5) . . ? O12 C27 H27A 110.9 . . ? O12 C27 H27B 109.9 . . ? H27A C27 H27B 109.3 . . ? O12 C27 H27C 109.5 . . ? H27A C27 H27C 109.3 . . ? H27B C27 H27C 107.9 . . ? O13 C28 H28A 105.5 . . ? O13 C28 H28B 110.5 . . ? H28A C28 H28B 110.7 . . ? O13 C28 H28C 110.7 . . ? H28A C28 H28C 110.7 . . ? H28B C28 H28C 108.8 . . ? C28 O13 H53A 121.5 . . ? O14 C29 H29A 123.2 . . ? O14 C29 H29B 106.0 . . ? H29A C29 H29B 106.6 . . ? O14 C29 H29C 106.9 . . ? H29A C29 H29C 106.6 . . ? H29B C29 H29C 106.6 . . ? C29 O14 H54A 113.8 . . ? O15 C30 H30A 124.1 . . ? O15 C30 H30B 104.9 . . ? H30A C30 H30B 106.6 . . ? O15 C30 H30C 107.1 . . ? H30A C30 H30C 106.6 . . ? H30B C30 H30C 106.6 . . ? C30 O15 H44A 118.2 . . ? C30 O15 H55A 85.0 . . ? H44A O15 H55A 115.9 . . ? O16 C31 H31A 123.6 . . ? O16 C31 H31B 105.6 . . ? H31A C31 H31B 106.3 . . ? O16 C31 H31C 107.5 . . ? H31A C31 H31C 106.3 . . ? H31B C31 H31C 106.4 . . ? C31 O16 H56A 111.7 . . ? O17 C32 H32A 125.6 . . ? O17 C32 H32B 105.3 . . ? H32A C32 H32B 106.2 . . ? O17 C32 H32C 105.9 . . ? H32A C32 H32C 106.2 . . ? H32B C32 H32C 106.4 . . ? C32 O17 H57A 116.5 . . ? H58A O18 H58B 91.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 O1 C1 -12.7(4) . . . . ? O6 Co1 O1 C1 165.0(4) . . . . ? N5 Co1 O1 C1 -111.1(4) . . . . ? O3 Co1 O1 C1 -8(4) . . . . ? O4 Co1 O1 C1 76.8(4) . . . . ? N1 Co1 O3 C8 -5.2(3) . . . . ? O1 Co1 O3 C8 -10(4) . . . . ? O6 Co1 O3 C8 177.1(3) . . . . ? N5 Co1 O3 C8 93.2(3) . . . . ? O4 Co1 O3 C8 -94.8(3) . . . . ? N1 Co1 O4 C9 140.3(6) . . . . ? O1 Co1 O4 C9 46.1(6) . . . . ? O6 Co1 O4 C9 -45.2(6) . . . . ? N5 Co1 O4 C9 -53.8(16) . . . . ? O3 Co1 O4 C9 -136.4(6) . . . . ? N4 Co2 O5 C10 15.2(4) . . . . ? O10 Co2 O5 C10 -162.9(4) . . . . ? N8 Co2 O5 C10 113.1(4) . . . . ? O7 Co2 O5 C10 5(4) . . . . ? O8 Co2 O5 C10 -74.0(4) . . . . ? N1 Co1 O6 C16 -107.1(15) . . . . ? O1 Co1 O6 C16 96.0(3) . . . . ? N5 Co1 O6 C16 4.9(3) . . . . ? O3 Co1 O6 C16 -84.3(3) . . . . ? O4 Co1 O6 C16 -173.9(4) . . . . ? N4 Co2 O7 C17 4.5(3) . . . . ? O5 Co2 O7 C17 15(4) . . . . ? O10 Co2 O7 C17 -177.4(3) . . . . ? N8 Co2 O7 C17 -93.5(3) . . . . ? O8 Co2 O7 C17 93.8(3) . . . . ? N4 Co2 O8 C18 -138.7(5) . . . . ? O5 Co2 O8 C18 -44.2(5) . . . . ? O10 Co2 O8 C18 47.5(5) . . . . ? N8 Co2 O8 C18 73.3(13) . . . . ? O7 Co2 O8 C18 138.2(5) . . . . ? N7 Co3 O9 C19 -21.1(4) . . . . ? N2 Co3 O9 C19 -119.0(4) 2_655 . . . ? O11 Co3 O9 C19 -28(3) . . . . ? O2 Co3 O9 C19 157.2(4) 2_655 . . . ? O12 Co3 O9 C19 69.2(4) . . . . ? N4 Co2 O10 C25 98.6(14) . . . . ? O5 Co2 O10 C25 -98.1(3) . . . . ? N8 Co2 O10 C25 -6.3(3) . . . . ? O7 Co2 O10 C25 82.4(3) . . . . ? O8 Co2 O10 C25 170.2(3) . . . . ? N7 Co3 O11 C26 -6.7(3) . . . . ? O9 Co3 O11 C26 0(3) . . . . ? N2 Co3 O11 C26 91.2(3) 2_655 . . . ? O2 Co3 O11 C26 175.0(3) 2_655 . . . ? O12 Co3 O11 C26 -97.0(3) . . . . ? N7 Co3 O12 C27 105.8(5) . . . . ? O9 Co3 O12 C27 12.1(5) . . . . ? N2 Co3 O12 C27 -91.7(13) 2_655 . . . ? O11 Co3 O12 C27 -171.1(5) . . . . ? O2 Co3 O12 C27 -79.8(5) 2_655 . . . ? O1 Co1 N1 C7 18.9(5) . . . . ? O6 Co1 N1 C7 -137.8(14) . . . . ? N5 Co1 N1 C7 110.8(5) . . . . ? O3 Co1 N1 C7 -160.8(5) . . . . ? O4 Co1 N1 C7 -71.2(5) . . . . ? O1 Co1 N1 N2 -175.3(3) . . . . ? O6 Co1 N1 N2 27.9(17) . . . . ? N5 Co1 N1 N2 -83.4(3) . . . . ? O3 Co1 N1 N2 4.9(3) . . . . ? O4 Co1 N1 N2 94.6(3) . . . . ? C7 N1 N2 C8 164.4(4) . . . . ? Co1 N1 N2 C8 -3.7(5) . . . . ? C7 N1 N2 Co3 -6.4(5) . . . 2_655 ? Co1 N1 N2 Co3 -174.46(19) . . . 2_655 ? O5 Co2 N4 C16 -17.8(5) . . . . ? O10 Co2 N4 C16 145.5(12) . . . . ? N8 Co2 N4 C16 -110.4(5) . . . . ? O7 Co2 N4 C16 161.7(5) . . . . ? O8 Co2 N4 C16 73.9(5) . . . . ? O5 Co2 N4 N5 176.5(3) . . . . ? O10 Co2 N4 N5 -20.3(15) . . . . ? N8 Co2 N4 N5 83.9(3) . . . . ? O7 Co2 N4 N5 -4.0(3) . . . . ? O8 Co2 N4 N5 -91.9(3) . . . . ? C16 N4 N5 C17 -165.2(4) . . . . ? Co2 N4 N5 C17 2.8(5) . . . . ? C16 N4 N5 Co1 6.9(5) . . . . ? Co2 N4 N5 Co1 174.91(19) . . . . ? N1 Co1 N5 C17 -23.2(5) . . . . ? O1 Co1 N5 C17 71.3(5) . . . . ? O6 Co1 N5 C17 162.4(5) . . . . ? O3 Co1 N5 C17 -106.3(5) . . . . ? O4 Co1 N5 C17 171.1(11) . . . . ? N1 Co1 N5 N4 168.1(3) . . . . ? O1 Co1 N5 N4 -97.4(3) . . . . ? O6 Co1 N5 N4 -6.3(3) . . . . ? O3 Co1 N5 N4 85.0(3) . . . . ? O4 Co1 N5 N4 2.4(14) . . . . ? O9 Co3 N7 C25 18.8(5) . . . . ? N2 Co3 N7 C25 109.8(4) 2_655 . . . ? O11 Co3 N7 C25 -161.6(5) . . . . ? O2 Co3 N7 C25 -144.7(14) 2_655 . . . ? O12 Co3 N7 C25 -72.8(4) . . . . ? O9 Co3 N7 N8 -173.7(3) . . . . ? N2 Co3 N7 N8 -82.7(3) 2_655 . . . ? O11 Co3 N7 N8 5.9(3) . . . . ? O2 Co3 N7 N8 22.8(17) 2_655 . . . ? O12 Co3 N7 N8 94.7(3) . . . . ? C25 N7 N8 C26 165.4(4) . . . . ? Co3 N7 N8 C26 -4.2(5) . . . . ? C25 N7 N8 Co2 -7.1(5) . . . . ? Co3 N7 N8 Co2 -176.72(18) . . . . ? N4 Co2 N8 C26 24.3(5) . . . . ? O5 Co2 N8 C26 -70.5(5) . . . . ? O10 Co2 N8 C26 -162.0(5) . . . . ? O7 Co2 N8 C26 107.2(5) . . . . ? O8 Co2 N8 C26 172.0(10) . . . . ? N4 Co2 N8 N7 -166.5(3) . . . . ? O5 Co2 N8 N7 98.7(3) . . . . ? O10 Co2 N8 N7 7.2(3) . . . . ? O7 Co2 N8 N7 -83.6(3) . . . . ? O8 Co2 N8 N7 -18.8(13) . . . . ? Co1 O1 C1 C6 -174.5(4) . . . . ? Co1 O1 C1 C2 5.1(7) . . . . ? O1 C1 C2 C3 179.9(5) . . . . ? C6 C1 C2 C3 -0.6(7) . . . . ? O1 C1 C2 C7 3.2(8) . . . . ? C6 C1 C2 C7 -177.3(5) . . . . ? C1 C2 C3 C4 0.2(8) . . . . ? C7 C2 C3 C4 177.1(5) . . . . ? C2 C3 C4 C5 0.2(9) . . . . ? C3 C4 C5 C6 -0.2(10) . . . . ? C4 C5 C6 C1 -0.3(10) . . . . ? O1 C1 C6 C5 -179.8(6) . . . . ? C2 C1 C6 C5 0.6(9) . . . . ? Co3 O2 C7 N1 5.1(6) 2_655 . . . ? Co3 O2 C7 C2 -172.6(3) 2_655 . . . ? N2 N1 C7 O2 0.9(7) . . . . ? Co1 N1 C7 O2 166.6(3) . . . . ? N2 N1 C7 C2 178.6(4) . . . . ? Co1 N1 C7 C2 -15.7(7) . . . . ? C1 C2 C7 O2 179.5(5) . . . . ? C3 C2 C7 O2 2.7(7) . . . . ? C1 C2 C7 N1 1.8(7) . . . . ? C3 C2 C7 N1 -175.0(5) . . . . ? Co1 O3 C8 N2 4.9(6) . . . . ? Co1 O3 C8 N3 -175.5(4) . . . . ? N1 N2 C8 O3 -1.0(7) . . . . ? Co3 N2 C8 O3 165.6(4) 2_655 . . . ? N1 N2 C8 N3 179.4(4) . . . . ? Co3 N2 C8 N3 -14.1(9) 2_655 . . . ? Co2 O5 C10 C15 170.5(4) . . . . ? Co2 O5 C10 C11 -9.3(7) . . . . ? O5 C10 C11 C12 -179.4(5) . . . . ? C15 C10 C11 C12 0.8(7) . . . . ? O5 C10 C11 C16 -1.0(8) . . . . ? C15 C10 C11 C16 179.2(5) . . . . ? C10 C11 C12 C13 -0.1(8) . . . . ? C16 C11 C12 C13 -178.5(5) . . . . ? C11 C12 C13 C14 0.3(9) . . . . ? C12 C13 C14 C15 -1.2(9) . . . . ? C13 C14 C15 C10 2.0(9) . . . . ? O5 C10 C15 C14 178.4(5) . . . . ? C11 C10 C15 C14 -1.8(8) . . . . ? Co1 O6 C16 N4 -2.2(6) . . . . ? Co1 O6 C16 C11 176.3(4) . . . . ? N5 N4 C16 O6 -3.3(6) . . . . ? Co2 N4 C16 O6 -168.9(3) . . . . ? N5 N4 C16 C11 178.2(4) . . . . ? Co2 N4 C16 C11 12.6(7) . . . . ? C10 C11 C16 O6 -178.7(5) . . . . ? C12 C11 C16 O6 -0.3(7) . . . . ? C10 C11 C16 N4 -0.2(8) . . . . ? C12 C11 C16 N4 178.2(5) . . . . ? Co2 O7 C17 N5 -4.3(6) . . . . ? Co2 O7 C17 N6 176.9(4) . . . . ? N4 N5 C17 O7 1.2(6) . . . . ? Co1 N5 C17 O7 -167.4(4) . . . . ? N4 N5 C17 N6 179.9(4) . . . . ? Co1 N5 C17 N6 11.3(8) . . . . ? Co3 O9 C19 C24 -163.4(4) . . . . ? Co3 O9 C19 C20 17.3(7) . . . . ? O9 C19 C20 C21 178.7(5) . . . . ? C24 C19 C20 C21 -0.6(8) . . . . ? O9 C19 C20 C25 -2.4(8) . . . . ? C24 C19 C20 C25 178.3(5) . . . . ? C19 C20 C21 C22 -0.1(8) . . . . ? C25 C20 C21 C22 -179.1(5) . . . . ? C20 C21 C22 C23 0.4(9) . . . . ? C21 C22 C23 C24 0.0(9) . . . . ? C22 C23 C24 C19 -0.7(9) . . . . ? O9 C19 C24 C23 -178.3(5) . . . . ? C20 C19 C24 C23 1.0(8) . . . . ? Co2 O10 C25 N7 4.1(6) . . . . ? Co2 O10 C25 C20 -176.3(4) . . . . ? N8 N7 C25 O10 2.1(6) . . . . ? Co3 N7 C25 O10 169.6(3) . . . . ? N8 N7 C25 C20 -177.5(4) . . . . ? Co3 N7 C25 C20 -10.1(7) . . . . ? C21 C20 C25 O10 -2.7(7) . . . . ? C19 C20 C25 O10 178.4(5) . . . . ? C21 C20 C25 N7 177.0(5) . . . . ? C19 C20 C25 N7 -2.0(8) . . . . ? Co3 O11 C26 N8 6.4(6) . . . . ? Co3 O11 C26 N9 -174.8(4) . . . . ? N7 N8 C26 O11 -1.7(6) . . . . ? Co2 N8 C26 O11 167.5(4) . . . . ? N7 N8 C26 N9 179.6(4) . . . . ? Co2 N8 C26 N9 -11.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.503 _refine_diff_density_min -0.396 _refine_diff_density_rms 0.080