# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_year ? _journal_page_first ? loop_ _publ_author_name J.Qi 'Hong-Xia Ma' 'Xian-Jun Li' 'Zhong-Yuan Zhou' M.C.K.Chio 'Albert S. C. Chan' 'Qi-Yun Yang' _publ_contact_author_name 'Prof Albert S. C. Chan' _publ_contact_author_address ; Prof Albert S. C. Chan Department of Applied Biology & Chemical Technology The Hong Kong Polytechnic University Kowloon, Hong Kong, China Hong Kong China CHINA ; _publ_contact_author_email BCACHAN@POLYU.EDU.HK _publ_section_title ; Synthesis and Characterization of Cobalt (=A2=BB) Complexes Containing 2-Pyridinecarboxamide Ligands and Their Application in Catalytic Oxidation of Ethylbenzene with Dioxygen ; data_lxj2 _database_code_CSD 189734 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H28 Cl3 Co N6 O5' _chemical_formula_weight 789.92 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.0628(12) _cell_length_b 14.7653(12) _cell_length_c 16.8999(14) _cell_angle_alpha 90.00 _cell_angle_beta 100.672(2) _cell_angle_gamma 90.00 _cell_volume 3693.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4327 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type 'multi scans' _exptl_absorpt_correction_T_min 0.7787 _exptl_absorpt_correction_T_max 0.8326 _exptl_absorpt_process_details 'SADABS; Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8381 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.56 _reflns_number_total 8381 _reflns_number_gt 5246 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^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 8381 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0826 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1306 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.26977(2) -0.61740(2) 0.29150(2) 0.04241(12) Uani 1 1 d . . . Cl1 Cl -0.07348(8) -0.91597(8) 0.40705(7) 0.0961(3) Uani 1 1 d . . . Cl2 Cl 0.13275(12) -0.48467(8) 0.66658(8) 0.1293(6) Uani 1 1 d . . . Cl3 Cl 0.72260(7) -0.77606(8) 0.39394(9) 0.1077(4) Uani 1 1 d . . . O1 O 0.05364(15) -0.69813(17) 0.12891(15) 0.0758(6) Uani 1 1 d . . . O2 O 0.34010(15) -0.77325(15) 0.48661(14) 0.0689(6) Uani 1 1 d . . . O3 O 0.44911(15) -0.42061(14) 0.36999(14) 0.0659(6) Uani 1 1 d . . . N1 N 0.26169(16) -0.58130(15) 0.17872(14) 0.0493(5) Uani 1 1 d . . . N2 N 0.15131(15) -0.67071(15) 0.24837(14) 0.0498(5) Uani 1 1 d . . . N3 N 0.32359(14) -0.73409(14) 0.27810(15) 0.0481(5) Uani 1 1 d . . . N4 N 0.27562(15) -0.66069(14) 0.40068(14) 0.0473(5) Uani 1 1 d . . . N5 N 0.22437(15) -0.49852(14) 0.31319(12) 0.0461(5) Uani 1 1 d . . . N6 N 0.38660(15) -0.55800(14) 0.32494(13) 0.0455(5) Uani 1 1 d . . . C1 C 0.3199(2) -0.5317(2) 0.14668(18) 0.0593(7) Uani 1 1 d . . . H1A H 0.3699 -0.5075 0.1806 0.071 Uiso 1 1 calc R . . C2 C 0.3090(3) -0.5149(2) 0.0653(2) 0.0706(9) Uani 1 1 d . . . H2A H 0.3509 -0.4799 0.0449 0.085 Uiso 1 1 calc R . . C3 C 0.2363(3) -0.5502(2) 0.0151(2) 0.0713(9) Uani 1 1 d . . . H3A H 0.2288 -0.5414 -0.0403 0.086 Uiso 1 1 calc R . . C4 C 0.1743(2) -0.5986(2) 0.04706(19) 0.0654(9) Uani 1 1 d . . . H4A H 0.1233 -0.6219 0.0138 0.078 Uiso 1 1 calc R . . C5 C 0.1877(2) -0.61285(18) 0.12875(17) 0.0501(6) Uani 1 1 d . . . C6 C 0.1234(2) -0.66556(19) 0.16877(19) 0.0554(7) Uani 1 1 d . . . C7 C 0.09811(19) -0.72881(18) 0.28924(18) 0.0521(7) Uani 1 1 d . . . C8 C 0.1211(2) -0.81880(19) 0.30169(18) 0.0551(7) Uani 1 1 d . . . H8A H 0.1724 -0.8412 0.2851 0.066 Uiso 1 1 calc R . . C9 C 0.0687(2) -0.8757(2) 0.3384(2) 0.0613(8) Uani 1 1 d . . . H9A H 0.0843 -0.9364 0.3464 0.074 Uiso 1 1 calc R . . C10 C -0.0070(2) -0.8421(2) 0.3633(2) 0.0644(8) Uani 1 1 d . . . C11 C -0.0314(3) -0.7531(2) 0.3515(3) 0.0851(12) Uani 1 1 d . . . H11A H -0.0823 -0.7306 0.3686 0.102 Uiso 1 1 calc R . . C12 C 0.0214(2) -0.6975(2) 0.3135(3) 0.0803(11) Uani 1 1 d . . . H12A H 0.0047 -0.6372 0.3042 0.096 Uiso 1 1 calc R . . C13 C 0.3399(2) -0.7710(2) 0.2083(2) 0.0575(7) Uani 1 1 d . . . H13A H 0.3238 -0.7392 0.1603 0.069 Uiso 1 1 calc R . . C14 C 0.3800(2) -0.8545(2) 0.2082(3) 0.0712(9) Uani 1 1 d . . . H14A H 0.3897 -0.8799 0.1602 0.085 Uiso 1 1 calc R . . C15 C 0.4055(3) -0.9003(2) 0.2795(3) 0.0866(12) Uani 1 1 d . . . H15A H 0.4339 -0.9563 0.2802 0.104 Uiso 1 1 calc R . . C16 C 0.3888(2) -0.8632(2) 0.3494(3) 0.0742(10) Uani 1 1 d . . . H16A H 0.4054 -0.8938 0.3980 0.089 Uiso 1 1 calc R . . C17 C 0.34726(18) -0.78020(18) 0.34714(19) 0.0524(7) Uani 1 1 d . . . C18 C 0.32135(19) -0.73693(18) 0.41838(18) 0.0515(7) Uani 1 1 d . . . C19 C 0.2418(2) -0.61700(17) 0.46439(17) 0.0484(6) Uani 1 1 d . . . C20 C 0.1678(2) -0.6532(2) 0.4916(2) 0.0699(9) Uani 1 1 d . . . H20A H 0.1406 -0.7053 0.4675 0.084 Uiso 1 1 calc R . . C21 C 0.1341(3) -0.6137(3) 0.5532(3) 0.0846(12) Uani 1 1 d . . . H21A H 0.0852 -0.6392 0.5716 0.102 Uiso 1 1 calc R . . C22 C 0.1738(3) -0.5356(2) 0.5875(2) 0.0760(10) Uani 1 1 d . . . C23 C 0.2476(3) -0.4995(2) 0.5638(2) 0.0762(10) Uani 1 1 d . . . H23A H 0.2748 -0.4477 0.5886 0.091 Uiso 1 1 calc R . . C24 C 0.2821(2) -0.5409(2) 0.50211(18) 0.0608(8) Uani 1 1 d . . . H24A H 0.3331 -0.5169 0.4861 0.073 Uiso 1 1 calc R . . C25 C 0.1381(2) -0.4744(2) 0.30938(18) 0.0573(7) Uani 1 1 d . . . H25A H 0.0930 -0.5174 0.2947 0.069 Uiso 1 1 calc R . . C26 C 0.1142(2) -0.3874(2) 0.3267(2) 0.0693(9) Uani 1 1 d . . . H26A H 0.0539 -0.3726 0.3249 0.083 Uiso 1 1 calc R . . C27 C 0.1798(3) -0.3229(2) 0.3465(2) 0.0721(9) Uani 1 1 d . . . H27A H 0.1646 -0.2638 0.3576 0.087 Uiso 1 1 calc R . . C28 C 0.2686(2) -0.34694(19) 0.34982(19) 0.0628(8) Uani 1 1 d . . . H28A H 0.3142 -0.3040 0.3623 0.075 Uiso 1 1 calc R . . C29 C 0.2896(2) -0.43558(17) 0.33440(15) 0.0472(6) Uani 1 1 d . . . C30 C 0.3844(2) -0.47013(18) 0.34444(16) 0.0484(6) Uani 1 1 d . . . C31 C 0.47050(18) -0.60494(17) 0.34224(16) 0.0440(6) Uani 1 1 d . . . C32 C 0.5110(2) -0.6236(2) 0.42058(18) 0.0575(7) Uani 1 1 d . . . H32A H 0.4859 -0.6011 0.4629 0.069 Uiso 1 1 calc R . . C33 C 0.5888(2) -0.6758(2) 0.4369(2) 0.0685(9) Uani 1 1 d . . . H33A H 0.6162 -0.6876 0.4899 0.082 Uiso 1 1 calc R . . C34 C 0.6250(2) -0.7099(2) 0.3741(2) 0.0656(8) Uani 1 1 d . . . C35 C 0.5864(2) -0.6914(2) 0.2956(2) 0.0645(8) Uani 1 1 d . . . H35A H 0.6120 -0.7137 0.2535 0.077 Uiso 1 1 calc R . . C36 C 0.5090(2) -0.6392(2) 0.28023(19) 0.0560(7) Uani 1 1 d . . . H36A H 0.4822 -0.6268 0.2272 0.067 Uiso 1 1 calc R . . O1W O 0.4997(2) -0.76664(18) 0.59463(17) 0.0361(7) Uani 0.50 1 d P . . H1WA H 0.4424 -0.7644 0.5829 0.043 Uiso 0.50 1 d PR . . H1WB H 0.5195 -0.7135 0.6065 0.043 Uiso 0.50 1 d PR . . O2W O 0.5541(4) -0.9387(3) 0.5629(3) 0.0957(17) Uani 0.50 1 d P . . H2WC H 0.5318 -0.9900 0.5708 0.115 Uiso 0.50 1 d PR . . H2WD H 0.6050 -0.9338 0.5941 0.115 Uiso 0.50 1 d PR . . O3W O 0.7321(6) -0.9111(7) 0.6562(6) 0.174(4) Uani 0.50 1 d P . . H3WA H 0.7180 -0.9213 0.7018 0.208 Uiso 0.50 1 d PR . . H3WB H 0.7501 -0.9605 0.6387 0.208 Uiso 0.50 1 d PR . . O4W O -0.1114(3) -0.6113(3) 0.1037(3) 0.0733(13) Uani 0.50 1 d P . . H4WA H -0.1037 -0.5922 0.1520 0.088 Uiso 0.50 1 d PR . . H4WB H -0.0663 -0.6438 0.0985 0.088 Uiso 0.50 1 d PR . . 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 0.0373(2) 0.04102(19) 0.0501(2) -0.00241(15) 0.01101(15) -0.00179(15) Cl1 0.0797(7) 0.1035(7) 0.1103(8) 0.0111(6) 0.0311(6) -0.0354(6) Cl2 0.1899(15) 0.0934(7) 0.1372(10) 0.0015(7) 0.1158(11) 0.0276(8) Cl3 0.0648(6) 0.0965(7) 0.1603(11) 0.0141(7) 0.0171(7) 0.0259(5) O1 0.0518(13) 0.0839(15) 0.0841(16) -0.0203(13) -0.0068(11) -0.0066(12) O2 0.0654(14) 0.0645(12) 0.0761(15) 0.0217(11) 0.0113(11) 0.0029(11) O3 0.0592(13) 0.0550(11) 0.0847(15) -0.0108(11) 0.0166(11) -0.0184(10) N1 0.0499(14) 0.0462(11) 0.0528(13) -0.0040(10) 0.0119(11) 0.0055(11) N2 0.0394(12) 0.0494(12) 0.0609(15) -0.0040(10) 0.0101(11) -0.0001(10) N3 0.0341(12) 0.0472(11) 0.0637(15) -0.0079(11) 0.0113(10) -0.0041(9) N4 0.0415(12) 0.0449(11) 0.0574(13) 0.0003(10) 0.0145(10) -0.0030(10) N5 0.0476(13) 0.0466(11) 0.0458(12) 0.0015(9) 0.0129(10) -0.0008(10) N6 0.0417(12) 0.0482(11) 0.0489(12) -0.0026(9) 0.0140(10) -0.0051(10) C1 0.0622(19) 0.0637(17) 0.0560(18) 0.0052(14) 0.0212(15) -0.0016(15) C2 0.084(3) 0.069(2) 0.063(2) 0.0080(16) 0.0253(19) 0.0104(18) C3 0.089(3) 0.077(2) 0.0482(18) 0.0028(16) 0.0128(18) 0.023(2) C4 0.070(2) 0.0702(19) 0.0528(18) -0.0107(14) 0.0033(16) 0.0161(17) C5 0.0489(16) 0.0483(14) 0.0508(16) -0.0073(12) 0.0032(13) 0.0111(13) C6 0.0475(17) 0.0513(15) 0.065(2) -0.0140(14) 0.0054(14) 0.0060(13) C7 0.0366(14) 0.0518(15) 0.0681(18) -0.0066(13) 0.0103(13) -0.0048(12) C8 0.0396(15) 0.0537(15) 0.0702(19) -0.0088(14) 0.0053(13) -0.0039(13) C9 0.0491(18) 0.0559(16) 0.075(2) 0.0002(14) 0.0014(15) -0.0071(14) C10 0.0503(18) 0.068(2) 0.074(2) -0.0035(16) 0.0104(15) -0.0193(16) C11 0.063(2) 0.071(2) 0.133(3) -0.011(2) 0.047(2) -0.0110(18) C12 0.054(2) 0.0554(17) 0.140(3) -0.0044(19) 0.042(2) -0.0025(15) C13 0.0428(16) 0.0584(16) 0.072(2) -0.0171(14) 0.0135(14) -0.0009(13) C14 0.059(2) 0.0606(18) 0.097(3) -0.0260(19) 0.0226(19) 0.0025(16) C15 0.070(2) 0.0547(19) 0.138(4) -0.017(2) 0.026(2) 0.0160(17) C16 0.062(2) 0.0532(17) 0.105(3) 0.0011(18) 0.012(2) 0.0098(16) C17 0.0375(15) 0.0454(14) 0.074(2) 0.0020(13) 0.0107(13) -0.0036(12) C18 0.0423(15) 0.0468(14) 0.0646(19) 0.0067(13) 0.0080(13) -0.0057(12) C19 0.0501(16) 0.0481(14) 0.0502(15) 0.0061(12) 0.0181(12) -0.0020(12) C20 0.063(2) 0.0628(18) 0.091(2) -0.0017(17) 0.0338(18) -0.0108(16) C21 0.077(3) 0.077(2) 0.115(3) 0.009(2) 0.058(2) 0.001(2) C22 0.099(3) 0.0623(19) 0.080(2) 0.0092(17) 0.051(2) 0.0156(19) C23 0.111(3) 0.0600(18) 0.067(2) -0.0035(15) 0.042(2) -0.0135(19) C24 0.067(2) 0.0656(17) 0.0557(17) 0.0005(14) 0.0273(15) -0.0172(16) C25 0.0475(17) 0.0587(17) 0.0666(19) -0.0047(14) 0.0130(14) 0.0061(14) C26 0.061(2) 0.0635(19) 0.083(2) -0.0084(16) 0.0121(17) 0.0170(17) C27 0.084(3) 0.0507(16) 0.080(2) -0.0107(15) 0.0112(19) 0.0151(18) C28 0.078(2) 0.0445(14) 0.0655(19) -0.0034(14) 0.0121(17) -0.0033(15) C29 0.0564(17) 0.0435(13) 0.0434(15) -0.0002(11) 0.0134(13) -0.0036(12) C30 0.0518(16) 0.0466(14) 0.0495(15) -0.0018(12) 0.0166(13) -0.0104(13) C31 0.0357(13) 0.0476(13) 0.0499(15) -0.0024(11) 0.0113(11) -0.0091(11) C32 0.0500(17) 0.0703(19) 0.0531(17) 0.0010(14) 0.0121(14) -0.0045(15) C33 0.0532(19) 0.085(2) 0.065(2) 0.0106(17) 0.0060(16) -0.0039(17) C34 0.0433(17) 0.0589(17) 0.095(3) 0.0027(17) 0.0139(17) -0.0018(14) C35 0.0522(18) 0.0673(18) 0.077(2) -0.0146(16) 0.0207(16) 0.0012(15) C36 0.0454(16) 0.0678(18) 0.0564(17) -0.0043(13) 0.0137(13) -0.0040(14) O1W 0.048(2) 0.0258(14) 0.0306(16) 0.0020(12) -0.0028(14) 0.0017(13) O2W 0.115(5) 0.069(3) 0.105(4) 0.002(3) 0.024(3) 0.035(3) O3W 0.168(8) 0.213(9) 0.167(8) -0.044(7) 0.099(7) -0.067(7) O4W 0.047(2) 0.062(2) 0.116(4) 0.028(2) 0.027(2) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 1.935(2) . ? Co1 N4 1.939(2) . ? Co1 N5 1.943(2) . ? Co1 N6 1.954(2) . ? Co1 N1 1.961(2) . ? Co1 N2 1.963(2) . ? Cl1 C10 1.736(3) . ? Cl2 C22 1.743(3) . ? Cl3 C34 1.745(3) . ? O1 C6 1.236(3) . ? O2 C18 1.255(3) . ? O3 C30 1.231(3) . ? N1 C1 1.332(4) . ? N1 C5 1.351(4) . ? N2 C6 1.335(4) . ? N2 C7 1.435(3) . ? N3 C17 1.341(4) . ? N3 C13 1.362(4) . ? N4 C18 1.325(3) . ? N4 C19 1.428(3) . ? N5 C25 1.337(4) . ? N5 C29 1.352(3) . ? N6 C30 1.341(3) . ? N6 C31 1.423(3) . ? C1 C2 1.378(4) . ? C1 H1A 0.9300 . ? C2 C3 1.359(5) . ? C2 H2A 0.9300 . ? C3 C4 1.365(5) . ? C3 H3A 0.9300 . ? C4 C5 1.374(4) . ? C4 H4A 0.9300 . ? C5 C6 1.497(4) . ? C7 C12 1.376(4) . ? C7 C8 1.379(4) . ? C8 C9 1.376(4) . ? C8 H8A 0.9300 . ? C9 C10 1.379(5) . ? C9 H9A 0.9300 . ? C10 C11 1.370(5) . ? C11 C12 1.380(5) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C14 1.373(4) . ? C13 H13A 0.9300 . ? C14 C15 1.373(6) . ? C14 H14A 0.9300 . ? C15 C16 1.367(6) . ? C15 H15A 0.9300 . ? C16 C17 1.373(4) . ? C16 H16A 0.9300 . ? C17 C18 1.478(4) . ? C19 C24 1.376(4) . ? C19 C20 1.389(4) . ? C20 C21 1.372(5) . ? C20 H20A 0.9300 . ? C21 C22 1.376(5) . ? C21 H21A 0.9300 . ? C22 C23 1.359(5) . ? C23 C24 1.390(4) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.381(4) . ? C25 H25A 0.9300 . ? C26 C27 1.369(5) . ? C26 H26A 0.9300 . ? C27 C28 1.375(5) . ? C27 H27A 0.9300 . ? C28 C29 1.382(4) . ? C28 H28A 0.9300 . ? C29 C30 1.496(4) . ? C31 C32 1.379(4) . ? C31 C36 1.383(4) . ? C32 C33 1.386(4) . ? C32 H32A 0.9300 . ? C33 C34 1.376(5) . ? C33 H33A 0.9300 . ? C34 C35 1.373(5) . ? C35 C36 1.383(4) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WC 0.8500 . ? O2W H2WD 0.8499 . ? O3W H3WA 0.8501 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8501 . ? 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 N3 Co1 N4 82.63(9) . . ? N3 Co1 N5 174.87(10) . . ? N4 Co1 N5 94.24(9) . . ? N3 Co1 N6 93.39(9) . . ? N4 Co1 N6 89.60(9) . . ? N5 Co1 N6 82.50(9) . . ? N3 Co1 N1 94.60(9) . . ? N4 Co1 N1 176.42(9) . . ? N5 Co1 N1 88.69(9) . . ? N6 Co1 N1 92.84(10) . . ? N3 Co1 N2 88.35(9) . . ? N4 Co1 N2 95.69(9) . . ? N5 Co1 N2 96.02(9) . . ? N6 Co1 N2 174.61(9) . . ? N1 Co1 N2 81.93(10) . . ? C1 N1 C5 117.7(3) . . ? C1 N1 Co1 128.1(2) . . ? C5 N1 Co1 114.17(19) . . ? C6 N2 C7 114.8(2) . . ? C6 N2 Co1 116.49(19) . . ? C7 N2 Co1 127.67(19) . . ? C17 N3 C13 119.3(2) . . ? C17 N3 Co1 113.57(19) . . ? C13 N3 Co1 127.2(2) . . ? C18 N4 C19 117.2(2) . . ? C18 N4 Co1 115.16(19) . . ? C19 N4 Co1 127.51(17) . . ? C25 N5 C29 118.8(2) . . ? C25 N5 Co1 127.2(2) . . ? C29 N5 Co1 114.03(18) . . ? C30 N6 C31 118.8(2) . . ? C30 N6 Co1 116.33(19) . . ? C31 N6 Co1 123.97(16) . . ? N1 C1 C2 122.6(3) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 119.2(3) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? C2 C3 C4 119.0(3) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 115.1(2) . . ? C4 C5 C6 123.1(3) . . ? O1 C6 N2 127.2(3) . . ? O1 C6 C5 120.8(3) . . ? N2 C6 C5 112.1(2) . . ? C12 C7 C8 118.6(3) . . ? C12 C7 N2 121.1(3) . . ? C8 C7 N2 120.2(2) . . ? C9 C8 C7 120.6(3) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C8 C9 C10 119.5(3) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C11 C10 C9 121.0(3) . . ? C11 C10 Cl1 120.3(3) . . ? C9 C10 Cl1 118.6(3) . . ? C10 C11 C12 118.5(3) . . ? C10 C11 H11A 120.8 . . ? C12 C11 H11A 120.8 . . ? C7 C12 C11 121.7(3) . . ? C7 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? N3 C13 C14 120.7(3) . . ? N3 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C13 C14 C15 119.5(3) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? C16 C15 C14 119.6(3) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? C15 C16 C17 119.3(4) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? N3 C17 C16 121.6(3) . . ? N3 C17 C18 114.9(2) . . ? C16 C17 C18 123.4(3) . . ? O2 C18 N4 126.1(3) . . ? O2 C18 C17 121.0(3) . . ? N4 C18 C17 112.8(3) . . ? C24 C19 C20 118.3(3) . . ? C24 C19 N4 122.0(2) . . ? C20 C19 N4 119.7(3) . . ? C21 C20 C19 121.4(3) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C20 C21 C22 118.8(3) . . ? C20 C21 H21A 120.6 . . ? C22 C21 H21A 120.6 . . ? C23 C22 C21 121.4(3) . . ? C23 C22 Cl2 118.8(3) . . ? C21 C22 Cl2 119.7(3) . . ? C22 C23 C24 119.3(3) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? C19 C24 C23 120.8(3) . . ? C19 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? N5 C25 C26 121.8(3) . . ? N5 C25 H25A 119.1 . . ? C26 C25 H25A 119.1 . . ? C27 C26 C25 119.7(3) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 118.9(3) . . ? C26 C27 H27A 120.6 . . ? C28 C27 H27A 120.6 . . ? C27 C28 C29 119.4(3) . . ? C27 C28 H28A 120.3 . . ? C29 C28 H28A 120.3 . . ? N5 C29 C28 121.4(3) . . ? N5 C29 C30 115.3(2) . . ? C28 C29 C30 123.2(3) . . ? O3 C30 N6 127.4(3) . . ? O3 C30 C29 121.0(2) . . ? N6 C30 C29 111.6(2) . . ? C32 C31 C36 118.8(3) . . ? C32 C31 N6 120.8(2) . . ? C36 C31 N6 120.2(2) . . ? C31 C32 C33 120.6(3) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C34 C33 C32 119.4(3) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C35 C34 C33 121.0(3) . . ? C35 C34 Cl3 119.2(3) . . ? C33 C34 Cl3 119.8(3) . . ? C34 C35 C36 118.9(3) . . ? C34 C35 H35A 120.5 . . ? C36 C35 H35A 120.5 . . ? C35 C36 C31 121.2(3) . . ? C35 C36 H36A 119.4 . . ? C31 C36 H36A 119.4 . . ? H1WA O1W H1WB 108.5 . . ? H2WC O2W H2WD 108.4 . . ? H3WA O3W H3WB 108.3 . . ? H4WA O4W H4WB 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 N3 Co1 N1 C1 -95.2(2) . . . . ? N4 Co1 N1 C1 -134.3(14) . . . . ? N5 Co1 N1 C1 80.9(2) . . . . ? N6 Co1 N1 C1 -1.5(2) . . . . ? N2 Co1 N1 C1 177.2(2) . . . . ? N3 Co1 N1 C5 83.81(18) . . . . ? N4 Co1 N1 C5 44.7(16) . . . . ? N5 Co1 N1 C5 -100.13(18) . . . . ? N6 Co1 N1 C5 177.45(18) . . . . ? N2 Co1 N1 C5 -3.86(18) . . . . ? N3 Co1 N2 C6 -90.4(2) . . . . ? N4 Co1 N2 C6 -172.81(19) . . . . ? N5 Co1 N2 C6 92.3(2) . . . . ? N6 Co1 N2 C6 18.5(11) . . . . ? N1 Co1 N2 C6 4.49(19) . . . . ? N3 Co1 N2 C7 77.2(2) . . . . ? N4 Co1 N2 C7 -5.2(2) . . . . ? N5 Co1 N2 C7 -100.1(2) . . . . ? N6 Co1 N2 C7 -173.8(9) . . . . ? N1 Co1 N2 C7 172.1(2) . . . . ? N4 Co1 N3 C17 -7.16(18) . . . . ? N5 Co1 N3 C17 45.4(11) . . . . ? N6 Co1 N3 C17 81.99(19) . . . . ? N1 Co1 N3 C17 175.11(19) . . . . ? N2 Co1 N3 C17 -103.12(19) . . . . ? N4 Co1 N3 C13 173.9(2) . . . . ? N5 Co1 N3 C13 -133.6(10) . . . . ? N6 Co1 N3 C13 -97.0(2) . . . . ? N1 Co1 N3 C13 -3.8(2) . . . . ? N2 Co1 N3 C13 77.9(2) . . . . ? N3 Co1 N4 C18 8.78(19) . . . . ? N5 Co1 N4 C18 -167.14(19) . . . . ? N6 Co1 N4 C18 -84.69(19) . . . . ? N1 Co1 N4 C18 48.2(16) . . . . ? N2 Co1 N4 C18 96.37(19) . . . . ? N3 Co1 N4 C19 -175.7(2) . . . . ? N5 Co1 N4 C19 8.4(2) . . . . ? N6 Co1 N4 C19 90.8(2) . . . . ? N1 Co1 N4 C19 -136.3(14) . . . . ? N2 Co1 N4 C19 -88.1(2) . . . . ? N3 Co1 N5 C25 -139.3(10) . . . . ? N4 Co1 N5 C25 -87.2(2) . . . . ? N6 Co1 N5 C25 -176.3(2) . . . . ? N1 Co1 N5 C25 90.7(2) . . . . ? N2 Co1 N5 C25 9.0(2) . . . . ? N3 Co1 N5 C29 40.5(11) . . . . ? N4 Co1 N5 C29 92.60(18) . . . . ? N6 Co1 N5 C29 3.57(17) . . . . ? N1 Co1 N5 C29 -89.47(18) . . . . ? N2 Co1 N5 C29 -171.20(18) . . . . ? N3 Co1 N6 C30 -178.17(19) . . . . ? N4 Co1 N6 C30 -95.58(19) . . . . ? N5 Co1 N6 C30 -1.25(19) . . . . ? N1 Co1 N6 C30 87.05(19) . . . . ? N2 Co1 N6 C30 73.1(10) . . . . ? N3 Co1 N6 C31 -9.0(2) . . . . ? N4 Co1 N6 C31 73.6(2) . . . . ? N5 Co1 N6 C31 167.9(2) . . . . ? N1 Co1 N6 C31 -103.8(2) . . . . ? N2 Co1 N6 C31 -117.7(9) . . . . ? C5 N1 C1 C2 -2.6(4) . . . . ? Co1 N1 C1 C2 176.4(2) . . . . ? N1 C1 C2 C3 -0.1(5) . . . . ? C1 C2 C3 C4 2.3(5) . . . . ? C2 C3 C4 C5 -1.7(5) . . . . ? C1 N1 C5 C4 3.2(4) . . . . ? Co1 N1 C5 C4 -175.9(2) . . . . ? C1 N1 C5 C6 -178.1(2) . . . . ? Co1 N1 C5 C6 2.8(3) . . . . ? C3 C4 C5 N1 -1.1(4) . . . . ? C3 C4 C5 C6 -179.7(3) . . . . ? C7 N2 C6 O1 7.1(4) . . . . ? Co1 N2 C6 O1 176.3(2) . . . . ? C7 N2 C6 C5 -173.3(2) . . . . ? Co1 N2 C6 C5 -4.1(3) . . . . ? N1 C5 C6 O1 -179.6(2) . . . . ? C4 C5 C6 O1 -0.9(4) . . . . ? N1 C5 C6 N2 0.8(3) . . . . ? C4 C5 C6 N2 179.5(3) . . . . ? C6 N2 C7 C12 -85.6(4) . . . . ? Co1 N2 C7 C12 106.6(3) . . . . ? C6 N2 C7 C8 91.5(3) . . . . ? Co1 N2 C7 C8 -76.3(3) . . . . ? C12 C7 C8 C9 -0.7(5) . . . . ? N2 C7 C8 C9 -177.8(3) . . . . ? C7 C8 C9 C10 -0.3(5) . . . . ? C8 C9 C10 C11 0.5(5) . . . . ? C8 C9 C10 Cl1 178.3(2) . . . . ? C9 C10 C11 C12 0.4(6) . . . . ? Cl1 C10 C11 C12 -177.4(3) . . . . ? C8 C7 C12 C11 1.5(6) . . . . ? N2 C7 C12 C11 178.7(4) . . . . ? C10 C11 C12 C7 -1.4(7) . . . . ? C17 N3 C13 C14 0.2(4) . . . . ? Co1 N3 C13 C14 179.1(2) . . . . ? N3 C13 C14 C15 -1.4(5) . . . . ? C13 C14 C15 C16 1.5(6) . . . . ? C14 C15 C16 C17 -0.4(6) . . . . ? C13 N3 C17 C16 1.0(4) . . . . ? Co1 N3 C17 C16 -178.1(2) . . . . ? C13 N3 C17 C18 -176.3(2) . . . . ? Co1 N3 C17 C18 4.7(3) . . . . ? C15 C16 C17 N3 -0.8(5) . . . . ? C15 C16 C17 C18 176.2(3) . . . . ? C19 N4 C18 O2 -2.2(4) . . . . ? Co1 N4 C18 O2 173.8(2) . . . . ? C19 N4 C18 C17 175.6(2) . . . . ? Co1 N4 C18 C17 -8.4(3) . . . . ? N3 C17 C18 O2 -179.7(2) . . . . ? C16 C17 C18 O2 3.2(4) . . . . ? N3 C17 C18 N4 2.4(3) . . . . ? C16 C17 C18 N4 -174.8(3) . . . . ? C18 N4 C19 C24 103.8(3) . . . . ? Co1 N4 C19 C24 -71.6(4) . . . . ? C18 N4 C19 C20 -74.0(4) . . . . ? Co1 N4 C19 C20 110.6(3) . . . . ? C24 C19 C20 C21 1.3(5) . . . . ? N4 C19 C20 C21 179.3(3) . . . . ? C19 C20 C21 C22 1.2(6) . . . . ? C20 C21 C22 C23 -2.9(6) . . . . ? C20 C21 C22 Cl2 -179.4(3) . . . . ? C21 C22 C23 C24 1.9(6) . . . . ? Cl2 C22 C23 C24 178.4(3) . . . . ? C20 C19 C24 C23 -2.3(5) . . . . ? N4 C19 C24 C23 179.8(3) . . . . ? C22 C23 C24 C19 0.7(5) . . . . ? C29 N5 C25 C26 -0.2(4) . . . . ? Co1 N5 C25 C26 179.6(2) . . . . ? N5 C25 C26 C27 1.6(5) . . . . ? C25 C26 C27 C28 -0.9(5) . . . . ? C26 C27 C28 C29 -1.0(5) . . . . ? C25 N5 C29 C28 -1.9(4) . . . . ? Co1 N5 C29 C28 178.3(2) . . . . ? C25 N5 C29 C30 174.7(2) . . . . ? Co1 N5 C29 C30 -5.2(3) . . . . ? C27 C28 C29 N5 2.5(4) . . . . ? C27 C28 C29 C30 -173.8(3) . . . . ? C31 N6 C30 O3 7.1(4) . . . . ? Co1 N6 C30 O3 176.9(2) . . . . ? C31 N6 C30 C29 -170.8(2) . . . . ? Co1 N6 C30 C29 -1.1(3) . . . . ? N5 C29 C30 O3 -174.0(2) . . . . ? C28 C29 C30 O3 2.5(4) . . . . ? N5 C29 C30 N6 4.1(3) . . . . ? C28 C29 C30 N6 -179.4(2) . . . . ? C30 N6 C31 C32 69.6(3) . . . . ? Co1 N6 C31 C32 -99.4(3) . . . . ? C30 N6 C31 C36 -115.8(3) . . . . ? Co1 N6 C31 C36 75.2(3) . . . . ? C36 C31 C32 C33 0.0(4) . . . . ? N6 C31 C32 C33 174.6(3) . . . . ? C31 C32 C33 C34 -0.8(5) . . . . ? C32 C33 C34 C35 1.5(5) . . . . ? C32 C33 C34 Cl3 -179.7(2) . . . . ? C33 C34 C35 C36 -1.4(5) . . . . ? Cl3 C34 C35 C36 179.9(2) . . . . ? C34 C35 C36 C31 0.5(5) . . . . ? C32 C31 C36 C35 0.2(4) . . . . ? N6 C31 C36 C35 -174.6(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O2 0.85 2.03 2.738(4) 140.6 . O1W H1WB O3 0.85 2.06 2.903(3) 172.7 3_646 O2W H2WD O3W 0.85 2.03 2.877(11) 171.8 . O3W H3WB O4W 0.85 2.51 2.688(9) 93.0 4_646 O3W H3WA Cl2 0.85 3.00 3.469(11) 116.6 2_646 O4W H4WA O3W 0.85 2.49 2.688(9) 94.2 4_445 O4W H4WB O1 0.85 1.96 2.759(5) 157.2 . _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.689 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.069 data_l3 _database_code_CSD 189735 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H39 Co N6 O5' _chemical_formula_weight 742.70 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.0000 '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 13.756(2) _cell_length_b 15.878(3) _cell_length_c 19.388(3) _cell_angle_alpha 107.558(3) _cell_angle_beta 97.914(3) _cell_angle_gamma 106.467(3) _cell_volume 3754.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 5822 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.509 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8624 _exptl_absorpt_correction_T_max 0.8877 _exptl_absorpt_process_details 'SADABS; Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13115 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0959 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13115 _reflns_number_gt 6830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^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 13115 _refine_ls_number_parameters 935 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1270 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1724 _refine_ls_wR_factor_gt 0.1433 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.005 _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 0.87037(3) 0.31796(3) -0.29121(2) 0.03723(11) Uani 1 1 d . . . O1 O 0.85556(16) 0.19078(14) -0.13902(12) 0.0585(6) Uani 1 1 d . . . O2 O 1.11026(17) 0.30966(17) -0.38654(13) 0.0770(9) Uani 1 1 d . . . O3 O 0.71889(18) 0.41799(15) -0.42302(13) 0.0739(8) Uani 1 1 d . . . N1 N 0.80336(17) 0.35850(15) -0.21053(13) 0.0381(7) Uani 1 1 d . . . N2 N 0.88858(17) 0.23126(15) -0.24089(13) 0.0402(7) Uani 1 1 d . . . N3 N 1.00891(17) 0.40449(15) -0.23564(13) 0.0403(7) Uani 1 1 d . . . N4 N 0.94332(17) 0.27482(15) -0.36611(13) 0.0409(7) Uani 1 1 d . . . N5 N 0.73051(17) 0.23979(15) -0.35174(13) 0.0412(7) Uani 1 1 d . . . N6 N 0.84423(18) 0.40573(15) -0.33725(13) 0.0437(7) Uani 1 1 d . . . C1 C 0.7564(2) 0.4234(2) -0.19964(18) 0.0482(9) Uani 1 1 d . . . H1 H 0.7569 0.4565 -0.2319 0.058 Uiso 1 1 calc R . . C2 C 0.7071(2) 0.4426(2) -0.1419(2) 0.0618(11) Uani 1 1 d . . . H2 H 0.6752 0.4878 -0.1361 0.074 Uiso 1 1 calc R . . C3 C 0.7054(3) 0.3952(2) -0.0937(2) 0.0647(11) Uani 1 1 d . . . H3 H 0.6733 0.4080 -0.0545 0.078 Uiso 1 1 calc R . . C4 C 0.7529(2) 0.3270(2) -0.10476(18) 0.0540(10) Uani 1 1 d . . . H4 H 0.7522 0.2929 -0.0733 0.065 Uiso 1 1 calc R . . C5 C 0.8008(2) 0.31094(19) -0.16253(17) 0.0401(8) Uani 1 1 d . . . C6 C 0.8520(2) 0.23756(19) -0.18009(17) 0.0401(8) Uani 1 1 d . . . C7 C 0.9427(2) 0.16460(18) -0.25700(16) 0.0402(8) Uani 1 1 d . . . C8 C 1.0491(2) 0.1938(2) -0.23031(18) 0.0527(10) Uani 1 1 d . . . H8 H 1.0871 0.2571 -0.2039 0.063 Uiso 1 1 calc R . . C9 C 1.1001(2) 0.1284(2) -0.2429(2) 0.0648(12) Uani 1 1 d . . . H9 H 1.1724 0.1490 -0.2258 0.078 Uiso 1 1 calc R . . C10 C 1.0455(2) 0.0330(2) -0.28033(19) 0.0552(10) Uani 1 1 d . . . C11 C 0.9409(2) 0.0068(2) -0.3073(2) 0.0586(11) Uani 1 1 d . . . H11 H 0.9029 -0.0564 -0.3344 0.070 Uiso 1 1 calc R . . C12 C 0.8884(2) 0.0711(2) -0.29600(19) 0.0517(10) Uani 1 1 d . . . H12 H 0.8165 0.0505 -0.3149 0.062 Uiso 1 1 calc R . . C13 C 1.0979(3) -0.0409(2) -0.2901(2) 0.0794(13) Uani 1 1 d . . . H13A H 1.0729 -0.0801 -0.2626 0.119 Uiso 1 1 calc R . . H13B H 1.1722 -0.0104 -0.2719 0.119 Uiso 1 1 calc R . . H13C H 1.0816 -0.0788 -0.3420 0.119 Uiso 1 1 calc R . . C14 C 1.0359(2) 0.4712(2) -0.16727(18) 0.0525(10) Uani 1 1 d . . . H14 H 0.9847 0.4762 -0.1411 0.063 Uiso 1 1 calc R . . C15 C 1.1372(3) 0.5323(2) -0.1349(2) 0.0671(12) Uani 1 1 d . . . H15 H 1.1542 0.5766 -0.0870 0.081 Uiso 1 1 calc R . . C16 C 1.2119(3) 0.5274(2) -0.1734(2) 0.0693(13) Uani 1 1 d . . . H16 H 1.2799 0.5699 -0.1531 0.083 Uiso 1 1 calc R . . C17 C 1.1856(3) 0.4582(2) -0.2436(2) 0.0627(11) Uani 1 1 d . . . H17 H 1.2363 0.4520 -0.2700 0.075 Uiso 1 1 calc R . . C18 C 1.0829(2) 0.3984(2) -0.27352(17) 0.0473(9) Uani 1 1 d . . . C19 C 1.0469(2) 0.3220(2) -0.34846(18) 0.0488(9) Uani 1 1 d . . . C20 C 0.8991(2) 0.1923(2) -0.43184(17) 0.0459(9) Uani 1 1 d . . . C21 C 0.8196(3) 0.1839(2) -0.48676(17) 0.0569(10) Uani 1 1 d . . . H21 H 0.8019 0.2366 -0.4855 0.068 Uiso 1 1 calc R . . C22 C 0.7644(3) 0.0988(2) -0.54469(19) 0.0655(12) Uani 1 1 d . . . H22 H 0.7083 0.0941 -0.5802 0.079 Uiso 1 1 calc R . . C23 C 0.7936(3) 0.0206(2) -0.5493(2) 0.0653(12) Uani 1 1 d . . . C24 C 0.8798(3) 0.0317(2) -0.49633(19) 0.0657(12) Uani 1 1 d . . . H24 H 0.9022 -0.0192 -0.4999 0.079 Uiso 1 1 calc R . . C25 C 0.9328(2) 0.1160(2) -0.43877(18) 0.0544(10) Uani 1 1 d . . . H25 H 0.9912 0.1221 -0.4045 0.065 Uiso 1 1 calc R . . C26 C 0.7318(3) -0.0758(3) -0.6093(3) 0.1031(18) Uani 1 1 d . . . H26A H 0.6985 -0.1182 -0.5863 0.155 Uiso 1 1 calc R . . H26B H 0.7785 -0.0999 -0.6351 0.155 Uiso 1 1 calc R . . H26C H 0.6797 -0.0698 -0.6440 0.155 Uiso 1 1 calc R . . C27 C 0.6758(2) 0.1513(2) -0.35737(18) 0.0498(10) Uani 1 1 d . . . H27 H 0.7065 0.1229 -0.3295 0.060 Uiso 1 1 calc R . . C28 C 0.5768(3) 0.1017(2) -0.4026(2) 0.0619(12) Uani 1 1 d . . . H28 H 0.5414 0.0412 -0.4049 0.074 Uiso 1 1 calc R . . C29 C 0.5304(3) 0.1428(2) -0.4447(2) 0.0659(12) Uani 1 1 d . . . H29 H 0.4637 0.1101 -0.4759 0.079 Uiso 1 1 calc R . . C30 C 0.5846(2) 0.2335(2) -0.43967(19) 0.0599(11) Uani 1 1 d . . . H30 H 0.5550 0.2622 -0.4678 0.072 Uiso 1 1 calc R . . C31 C 0.6837(2) 0.2808(2) -0.39208(17) 0.0458(9) Uani 1 1 d . . . C32 C 0.7517(2) 0.3765(2) -0.38539(18) 0.0503(9) Uani 1 1 d . . . C33 C 0.9214(2) 0.48880(19) -0.33608(17) 0.0445(9) Uani 1 1 d . . . C34 C 0.9507(3) 0.5718(2) -0.2764(2) 0.0590(11) Uani 1 1 d . . . H34 H 0.9186 0.5749 -0.2370 0.071 Uiso 1 1 calc R . . C35 C 1.0285(3) 0.6516(2) -0.2748(2) 0.0745(13) Uani 1 1 d . . . H35 H 1.0486 0.7070 -0.2337 0.089 Uiso 1 1 calc R . . C36 C 1.0763(3) 0.6498(2) -0.3332(2) 0.0660(11) Uani 1 1 d . . . C37 C 1.0459(3) 0.5663(2) -0.3925(2) 0.0661(11) Uani 1 1 d . . . H37 H 1.0771 0.5634 -0.4323 0.079 Uiso 1 1 calc R . . C38 C 0.9696(2) 0.4864(2) -0.39418(19) 0.0581(10) Uani 1 1 d . . . H38 H 0.9507 0.4307 -0.4349 0.070 Uiso 1 1 calc R . . C39 C 1.1608(3) 0.7392(2) -0.3299(3) 0.1116(18) Uani 1 1 d . . . H39A H 1.1915 0.7246 -0.3715 0.167 Uiso 1 1 calc R . . H39B H 1.2139 0.7632 -0.2843 0.167 Uiso 1 1 calc R . . H39C H 1.1298 0.7858 -0.3318 0.167 Uiso 1 1 calc R . . Co2 Co 0.35455(3) 0.23331(3) 0.26311(2) 0.03982(12) Uani 1 1 d . . . O4 O 0.19887(17) 0.35332(15) 0.15395(14) 0.0674(8) Uani 1 1 d . . . O5 O 0.35750(18) 0.08986(15) 0.40337(12) 0.0640(7) Uani 1 1 d . . . O6 O 0.60009(16) 0.26027(15) 0.17159(13) 0.0635(8) Uani 1 1 d . . . N7 N 0.21870(18) 0.15574(16) 0.19603(13) 0.0429(7) Uani 1 1 d . . . N8 N 0.32465(17) 0.32872(16) 0.22885(13) 0.0432(7) Uani 1 1 d . . . N9 N 0.28338(18) 0.25769(17) 0.34425(14) 0.0466(7) Uani 1 1 d . . . N10 N 0.37551(18) 0.13709(16) 0.30248(14) 0.0467(8) Uani 1 1 d . . . N11 N 0.48978(18) 0.31916(15) 0.32493(13) 0.0415(7) Uani 1 1 d . . . N12 N 0.43215(17) 0.20889(15) 0.18801(13) 0.0395(7) Uani 1 1 d . . . C40 C 0.1701(2) 0.0623(2) 0.17766(19) 0.0573(11) Uani 1 1 d . . . H40 H 0.2042 0.0285 0.1972 0.069 Uiso 1 1 calc R . . C41 C 0.0724(3) 0.0160(3) 0.1312(2) 0.0707(13) Uani 1 1 d . . . H41 H 0.0404 -0.0482 0.1197 0.085 Uiso 1 1 calc R . . C42 C 0.0213(3) 0.0647(3) 0.1015(2) 0.0739(14) Uani 1 1 d . . . H42 H -0.0454 0.0338 0.0701 0.089 Uiso 1 1 calc R . . C43 C 0.0703(2) 0.1609(2) 0.1190(2) 0.0636(12) Uani 1 1 d . . . H43 H 0.0372 0.1953 0.0996 0.076 Uiso 1 1 calc R . . C44 C 0.1691(2) 0.2034(2) 0.16565(17) 0.0458(9) Uani 1 1 d . . . C45 C 0.2328(2) 0.3043(2) 0.18263(18) 0.0486(9) Uani 1 1 d . . . C46 C 0.4015(2) 0.41850(19) 0.24030(18) 0.0452(9) Uani 1 1 d . . . C47 C 0.4212(3) 0.4957(2) 0.3041(2) 0.0643(12) Uani 1 1 d . . . H47 H 0.3828 0.4916 0.3396 0.077 Uiso 1 1 calc R . . C48 C 0.4988(3) 0.5791(2) 0.3144(2) 0.0833(15) Uani 1 1 d . . . H48 H 0.5136 0.6301 0.3584 0.100 Uiso 1 1 calc R . . C49 C 0.5553(3) 0.5894(2) 0.2617(3) 0.0828(15) Uani 1 1 d . . . C50 C 0.5348(3) 0.5127(2) 0.1991(2) 0.0678(12) Uani 1 1 d . . . H50 H 0.5726 0.5173 0.1633 0.081 Uiso 1 1 calc R . . C51 C 0.4588(2) 0.4281(2) 0.18797(19) 0.0525(10) Uani 1 1 d . . . H51 H 0.4459 0.3767 0.1447 0.063 Uiso 1 1 calc R . . C52 C 0.6396(4) 0.6840(3) 0.2747(3) 0.137(2) Uani 1 1 d . . . H52A H 0.6907 0.7024 0.3204 0.206 Uiso 1 1 calc R . . H52B H 0.6078 0.7311 0.2778 0.206 Uiso 1 1 calc R . . H52C H 0.6730 0.6775 0.2340 0.206 Uiso 1 1 calc R . . C53 C 0.2318(2) 0.3191(2) 0.36115(18) 0.0555(10) Uani 1 1 d . . . H53 H 0.2268 0.3545 0.3312 0.067 Uiso 1 1 calc R . . C54 C 0.1864(3) 0.3317(3) 0.4206(2) 0.0712(13) Uani 1 1 d . . . H54 H 0.1507 0.3740 0.4301 0.085 Uiso 1 1 calc R . . C55 C 0.1947(3) 0.2806(3) 0.4662(2) 0.0741(13) Uani 1 1 d . . . H55 H 0.1653 0.2882 0.5070 0.089 Uiso 1 1 calc R . . C56 C 0.2481(3) 0.2174(3) 0.44956(19) 0.0652(12) Uani 1 1 d . . . H56 H 0.2551 0.1823 0.4794 0.078 Uiso 1 1 calc R . . C57 C 0.2906(2) 0.2073(2) 0.38829(17) 0.0474(10) Uani 1 1 d . . . C58 C 0.3449(2) 0.1377(2) 0.36488(18) 0.0472(10) Uani 1 1 d . . . C59 C 0.4301(2) 0.07338(19) 0.27589(17) 0.0457(9) Uani 1 1 d . . . C60 C 0.3759(3) -0.0203(2) 0.2327(2) 0.0615(11) Uani 1 1 d . . . H60 H 0.3033 -0.0431 0.2218 0.074 Uiso 1 1 calc R . . C61 C 0.4292(3) -0.0801(2) 0.2056(2) 0.0673(12) Uani 1 1 d . . . H61 H 0.3913 -0.1429 0.1771 0.081 Uiso 1 1 calc R . . C62 C 0.5363(3) -0.0494(2) 0.21960(19) 0.0560(10) Uani 1 1 d . . . C63 C 0.5914(3) 0.0437(2) 0.26441(19) 0.0583(11) Uani 1 1 d . . . H63 H 0.6641 0.0657 0.2761 0.070 Uiso 1 1 calc R . . C64 C 0.5385(2) 0.1044(2) 0.29205(18) 0.0517(10) Uani 1 1 d . . . H64 H 0.5765 0.1667 0.3218 0.062 Uiso 1 1 calc R . . C65 C 0.5907(3) -0.1163(2) 0.1841(3) 0.0871(15) Uani 1 1 d . . . H65A H 0.6026 -0.1508 0.2154 0.131 Uiso 1 1 calc R . . H65B H 0.6564 -0.0809 0.1784 0.131 Uiso 1 1 calc R . . H65C H 0.5474 -0.1594 0.1361 0.131 Uiso 1 1 calc R . . C66 C 0.5145(2) 0.3744(2) 0.39712(18) 0.0524(10) Uani 1 1 d . . . H66 H 0.4626 0.3698 0.4233 0.063 Uiso 1 1 calc R . . C67 C 0.6127(3) 0.4371(2) 0.4338(2) 0.0662(12) Uani 1 1 d . . . H67 H 0.6270 0.4739 0.4840 0.079 Uiso 1 1 calc R . . C68 C 0.6903(3) 0.4454(2) 0.3958(2) 0.0698(13) Uani 1 1 d . . . H68 H 0.7572 0.4887 0.4193 0.084 Uiso 1 1 calc R . . C69 C 0.6664(2) 0.3883(2) 0.3225(2) 0.0586(11) Uani 1 1 d . . . H69 H 0.7176 0.3915 0.2957 0.070 Uiso 1 1 calc R . . C70 C 0.5657(2) 0.32590(19) 0.28860(18) 0.0451(9) Uani 1 1 d . . . C71 C 0.5341(2) 0.26026(19) 0.20950(18) 0.0435(9) Uani 1 1 d . . . C72 C 0.3925(2) 0.14071(19) 0.11418(17) 0.0420(9) Uani 1 1 d . . . C73 C 0.4197(2) 0.0607(2) 0.09323(18) 0.0523(10) Uani 1 1 d . . . H73 H 0.4665 0.0521 0.1277 0.063 Uiso 1 1 calc R . . C74 C 0.3796(3) -0.0053(2) 0.02368(19) 0.0613(11) Uani 1 1 d . . . H74 H 0.3997 -0.0581 0.0120 0.074 Uiso 1 1 calc R . . C75 C 0.3107(3) 0.0026(2) -0.03018(19) 0.0576(11) Uani 1 1 d . . . C76 C 0.2851(3) 0.0851(2) -0.01041(19) 0.0583(11) Uani 1 1 d . . . H76 H 0.2403 0.0944 -0.0456 0.070 Uiso 1 1 calc R . . C77 C 0.3255(2) 0.1522(2) 0.06042(17) 0.0496(10) Uani 1 1 d . . . H77 H 0.3074 0.2061 0.0723 0.060 Uiso 1 1 calc R . . C78 C 0.2647(3) -0.0724(3) -0.1070(2) 0.0861(15) Uani 1 1 d . . . H78A H 0.2392 -0.0459 -0.1410 0.129 Uiso 1 1 calc R . . H78B H 0.2081 -0.1229 -0.1051 0.129 Uiso 1 1 calc R . . H78C H 0.3176 -0.0960 -0.1237 0.129 Uiso 1 1 calc R . . O7 O 1.0404(3) 0.3646(3) 0.0575(2) 0.1622(8) Uani 1 1 d D . . H7A H 1.0854 0.3842 0.0965 0.195 Uiso 1 1 calc R . . C79 C 1.0962(6) 0.3449(5) -0.0160(3) 0.233(2) Uani 1 1 d D . . H79A H 1.0530 0.3472 -0.0582 0.350 Uiso 1 1 calc R . . H79B H 1.1033 0.2840 -0.0284 0.350 Uiso 1 1 calc R . . H79C H 1.1640 0.3923 -0.0030 0.350 Uiso 1 1 calc R . . O8 O 1.5320(4) 0.3748(4) 0.0132(3) 0.255(3) Uani 1 1 d D . . H8A H 1.5439 0.3262 0.0103 0.306 Uiso 1 1 calc R . . C80 C 1.4102(6) 0.3479(7) -0.0373(6) 0.329(6) Uani 1 1 d D . . H80A H 1.3975 0.4048 -0.0358 0.494 Uiso 1 1 calc R . . H80B H 1.3604 0.3134 -0.0168 0.494 Uiso 1 1 calc R . . H80C H 1.4032 0.3102 -0.0880 0.494 Uiso 1 1 calc R . . O1W O 0.8430(3) 0.2176(3) 0.0129(2) 0.1656(18) Uani 1 1 d . . . H1WA H 0.8468 0.2092 -0.0320 0.199 Uiso 1 1 d R . . H1WB H 0.9017 0.2608 0.0358 0.199 Uiso 1 1 d R . . O2W O 0.6425(3) 0.2522(2) 0.0340(2) 0.1527(12) Uani 1 1 d . . . H2WA H 0.6295 0.2546 0.0760 0.183 Uiso 1 1 d R . . H2WB H 0.6100 0.2884 0.0275 0.183 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 0.0388(2) 0.03362(19) 0.0415(2) 0.01250(16) 0.01149(17) 0.01606(16) O1 0.0826(13) 0.0600(11) 0.0632(12) 0.0386(9) 0.0342(11) 0.0438(10) O2 0.0607(13) 0.0878(17) 0.0732(16) 0.0122(13) 0.0437(12) 0.0172(12) O3 0.0783(15) 0.0759(13) 0.0843(15) 0.0494(11) 0.0077(13) 0.0347(12) N1 0.0409(12) 0.0324(11) 0.0431(14) 0.0102(10) 0.0094(11) 0.0198(10) N2 0.0414(12) 0.0371(12) 0.0481(14) 0.0158(10) 0.0127(11) 0.0209(10) N3 0.0416(13) 0.0367(12) 0.0450(14) 0.0142(10) 0.0123(11) 0.0165(10) N4 0.0405(12) 0.0413(12) 0.0410(14) 0.0118(10) 0.0112(11) 0.0165(10) N5 0.0407(12) 0.0431(12) 0.0449(14) 0.0169(10) 0.0129(11) 0.0198(10) N6 0.0474(13) 0.0389(12) 0.0473(14) 0.0162(10) 0.0099(12) 0.0188(11) C1 0.0497(17) 0.0432(16) 0.0565(19) 0.0176(14) 0.0167(15) 0.0215(13) C2 0.0644(18) 0.0596(18) 0.077(2) 0.0216(16) 0.0341(17) 0.0394(15) C3 0.0689(19) 0.064(2) 0.079(2) 0.0258(17) 0.0427(17) 0.0368(16) C4 0.0671(19) 0.0464(16) 0.0588(19) 0.0209(14) 0.0296(16) 0.0257(15) C5 0.0387(15) 0.0347(14) 0.0458(17) 0.0125(12) 0.0117(13) 0.0123(12) C6 0.0395(15) 0.0385(15) 0.0443(17) 0.0139(13) 0.0103(13) 0.0173(12) C7 0.0451(15) 0.0367(14) 0.0513(17) 0.0197(12) 0.0183(13) 0.0252(12) C8 0.0440(17) 0.0421(16) 0.071(2) 0.0163(15) 0.0108(16) 0.0193(14) C9 0.0392(17) 0.0570(19) 0.094(3) 0.0184(18) 0.0076(18) 0.0242(15) C10 0.0578(18) 0.0459(16) 0.078(2) 0.0282(14) 0.0248(16) 0.0318(14) C11 0.0576(19) 0.0332(15) 0.088(2) 0.0180(15) 0.0252(18) 0.0215(14) C12 0.0373(16) 0.0392(16) 0.072(2) 0.0106(15) 0.0124(15) 0.0148(13) C13 0.071(2) 0.067(2) 0.122(3) 0.040(2) 0.036(2) 0.0443(17) C14 0.0498(18) 0.0464(17) 0.053(2) 0.0054(15) 0.0125(15) 0.0172(14) C15 0.057(2) 0.055(2) 0.067(2) 0.0011(18) 0.0076(19) 0.0129(17) C16 0.046(2) 0.056(2) 0.082(3) 0.0082(19) 0.0058(19) 0.0045(17) C17 0.0481(18) 0.0561(19) 0.084(2) 0.0245(17) 0.0256(17) 0.0142(15) C18 0.0504(17) 0.0459(16) 0.0522(18) 0.0225(13) 0.0160(15) 0.0191(14) C19 0.0516(17) 0.0483(17) 0.0484(18) 0.0143(14) 0.0178(15) 0.0205(14) C20 0.0499(17) 0.0464(16) 0.0423(17) 0.0105(13) 0.0168(14) 0.0212(13) C21 0.073(2) 0.0571(18) 0.0413(18) 0.0121(14) 0.0140(16) 0.0295(16) C22 0.066(2) 0.071(2) 0.049(2) 0.0092(17) 0.0115(18) 0.0229(18) C23 0.065(2) 0.058(2) 0.052(2) 0.0019(17) 0.0174(18) 0.0078(18) C24 0.088(2) 0.0512(19) 0.063(2) 0.0120(16) 0.0326(19) 0.0338(17) C25 0.0552(18) 0.0535(18) 0.054(2) 0.0123(15) 0.0176(16) 0.0234(15) C26 0.104(3) 0.065(3) 0.089(3) -0.012(2) 0.019(3) -0.002(2) C27 0.0444(17) 0.0400(15) 0.065(2) 0.0188(14) 0.0106(15) 0.0150(13) C28 0.052(2) 0.0449(18) 0.076(2) 0.0140(17) 0.0022(18) 0.0114(16) C29 0.0433(19) 0.065(2) 0.071(2) 0.0105(19) 0.0004(18) 0.0123(17) C30 0.0535(18) 0.0680(19) 0.063(2) 0.0231(16) 0.0050(16) 0.0329(16) C31 0.0464(16) 0.0500(16) 0.0446(18) 0.0146(13) 0.0089(14) 0.0254(13) C32 0.0587(18) 0.0492(16) 0.0558(19) 0.0260(14) 0.0173(15) 0.0281(14) C33 0.0496(17) 0.0373(14) 0.0570(18) 0.0247(13) 0.0150(14) 0.0209(13) C34 0.067(2) 0.0483(17) 0.070(2) 0.0222(15) 0.0288(17) 0.0249(15) C35 0.078(2) 0.0365(17) 0.106(3) 0.0175(18) 0.026(2) 0.0213(17) C36 0.061(2) 0.0483(17) 0.106(3) 0.0406(17) 0.0326(19) 0.0262(15) C37 0.073(2) 0.0621(19) 0.088(2) 0.0443(16) 0.0406(18) 0.0318(16) C38 0.070(2) 0.0484(17) 0.067(2) 0.0267(15) 0.0297(17) 0.0248(15) C39 0.090(3) 0.054(2) 0.209(5) 0.064(2) 0.060(3) 0.021(2) Co2 0.0402(2) 0.0361(2) 0.0443(2) 0.01231(17) 0.01252(18) 0.01594(16) O4 0.0569(13) 0.0555(12) 0.0931(17) 0.0296(11) 0.0020(12) 0.0287(10) O5 0.0787(15) 0.0621(12) 0.0574(13) 0.0326(10) 0.0144(12) 0.0222(11) O6 0.0470(12) 0.0654(14) 0.0738(15) 0.0152(11) 0.0298(11) 0.0165(10) N7 0.0398(13) 0.0439(13) 0.0454(14) 0.0159(11) 0.0133(11) 0.0139(11) N8 0.0432(13) 0.0398(12) 0.0483(15) 0.0113(10) 0.0097(11) 0.0221(10) N9 0.0458(13) 0.0513(14) 0.0446(14) 0.0140(11) 0.0146(11) 0.0214(11) N10 0.0482(14) 0.0447(13) 0.0505(15) 0.0176(11) 0.0140(12) 0.0193(11) N11 0.0474(13) 0.0332(12) 0.0419(14) 0.0099(10) 0.0079(11) 0.0160(10) N12 0.0444(13) 0.0382(12) 0.0401(13) 0.0130(10) 0.0139(11) 0.0196(10) C40 0.053(2) 0.0451(17) 0.066(2) 0.0195(15) 0.0127(17) 0.0068(15) C41 0.061(2) 0.057(2) 0.071(2) 0.0171(18) 0.0027(19) -0.0014(18) C42 0.044(2) 0.080(3) 0.071(3) 0.014(2) 0.0045(19) 0.0014(19) C43 0.0450(19) 0.067(2) 0.068(2) 0.0172(18) 0.0049(17) 0.0152(17) C44 0.0369(16) 0.0488(17) 0.0506(18) 0.0160(14) 0.0119(14) 0.0148(13) C45 0.0482(17) 0.0475(16) 0.0557(19) 0.0178(14) 0.0140(15) 0.0249(14) C46 0.0456(16) 0.0338(14) 0.0556(19) 0.0122(13) 0.0045(15) 0.0206(13) C47 0.072(2) 0.0413(17) 0.076(2) 0.0102(16) 0.0091(19) 0.0295(16) C48 0.096(3) 0.0315(17) 0.100(3) -0.0002(19) -0.008(2) 0.0300(18) C49 0.063(2) 0.0390(18) 0.132(4) 0.022(2) 0.003(2) 0.0162(17) C50 0.058(2) 0.0448(17) 0.111(3) 0.0364(17) 0.0272(19) 0.0216(15) C51 0.0505(18) 0.0362(15) 0.072(2) 0.0185(14) 0.0122(16) 0.0194(14) C52 0.101(4) 0.045(2) 0.232(6) 0.044(3) 0.003(4) -0.001(2) C53 0.0570(18) 0.0647(19) 0.050(2) 0.0153(15) 0.0203(15) 0.0311(15) C54 0.073(2) 0.080(2) 0.059(2) 0.0083(18) 0.0312(18) 0.0352(18) C55 0.078(2) 0.089(3) 0.056(2) 0.0169(19) 0.0344(19) 0.032(2) C56 0.070(2) 0.074(2) 0.050(2) 0.0203(17) 0.0243(17) 0.0198(18) C57 0.0413(17) 0.0506(17) 0.0417(18) 0.0118(14) 0.0093(14) 0.0089(14) C58 0.0441(18) 0.0397(16) 0.0487(19) 0.0144(14) 0.0041(15) 0.0063(14) C59 0.0530(17) 0.0335(14) 0.0580(19) 0.0209(13) 0.0165(15) 0.0194(13) C60 0.0499(19) 0.0382(17) 0.089(3) 0.0167(16) 0.0224(18) 0.0081(15) C61 0.071(2) 0.0347(17) 0.090(3) 0.0128(17) 0.025(2) 0.0170(16) C62 0.063(2) 0.0395(16) 0.071(2) 0.0196(15) 0.0183(17) 0.0251(15) C63 0.0513(18) 0.0455(17) 0.077(2) 0.0203(16) 0.0075(17) 0.0202(15) C64 0.0473(18) 0.0373(16) 0.063(2) 0.0144(14) 0.0016(16) 0.0128(14) C65 0.088(2) 0.056(2) 0.116(3) 0.015(2) 0.024(2) 0.0403(19) C66 0.0569(19) 0.0466(17) 0.0523(19) 0.0156(14) 0.0077(16) 0.0206(15) C67 0.068(2) 0.056(2) 0.055(2) 0.0082(17) -0.0081(19) 0.0172(18) C68 0.055(2) 0.054(2) 0.074(3) 0.0057(19) -0.003(2) 0.0071(17) C69 0.0414(18) 0.0561(19) 0.068(2) 0.0177(17) 0.0033(17) 0.0119(15) C70 0.0445(17) 0.0351(14) 0.0569(19) 0.0169(13) 0.0064(15) 0.0178(13) C71 0.0371(16) 0.0380(15) 0.0553(19) 0.0157(13) 0.0103(14) 0.0142(13) C72 0.0427(15) 0.0357(14) 0.0519(18) 0.0147(13) 0.0214(14) 0.0166(12) C73 0.0557(18) 0.0432(16) 0.060(2) 0.0155(14) 0.0166(16) 0.0222(14) C74 0.075(2) 0.0463(18) 0.059(2) 0.0074(16) 0.0139(18) 0.0283(16) C75 0.066(2) 0.0496(19) 0.0434(19) 0.0040(15) 0.0130(17) 0.0130(16) C76 0.0540(19) 0.063(2) 0.055(2) 0.0203(16) 0.0093(16) 0.0189(16) C77 0.0543(18) 0.0457(16) 0.0512(19) 0.0139(14) 0.0167(15) 0.0226(14) C78 0.099(3) 0.073(3) 0.063(3) 0.000(2) 0.014(2) 0.023(2) O7 0.124(3) 0.141(3) 0.157(2) -0.020(3) -0.033(3) 0.0615(19) C79 0.250(4) 0.183(4) 0.106(4) 0.037(4) -0.073(5) -0.092(5) O8 0.252(4) 0.203(4) 0.323(6) 0.069(4) 0.152(4) 0.085(4) C80 0.228(5) 0.230(6) 0.328(9) 0.005(9) 0.004(10) -0.087(8) O1W 0.196(4) 0.187(3) 0.119(3) 0.078(2) 0.055(3) 0.041(3) O2W 0.247(2) 0.108(2) 0.119(2) 0.0469(19) 0.079(2) 0.062(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 1.933(2) . ? Co1 N5 1.940(2) . ? Co1 N4 1.943(2) . ? Co1 N6 1.953(3) . ? Co1 N1 1.959(2) . ? Co1 N2 1.962(3) . ? O1 C6 1.247(4) . ? O2 C19 1.237(4) . ? O3 C32 1.241(4) . ? N1 C1 1.345(4) . ? N1 C5 1.362(4) . ? N2 C6 1.332(4) . ? N2 C7 1.443(4) . ? N3 C18 1.343(4) . ? N3 C14 1.346(4) . ? N4 C19 1.346(4) . ? N4 C20 1.428(3) . ? N5 C27 1.356(4) . ? N5 C31 1.363(4) . ? N6 C32 1.336(4) . ? N6 C33 1.431(4) . ? C1 C2 1.388(5) . ? C1 H1 0.9300 . ? C2 C3 1.364(5) . ? C2 H2 0.9300 . ? C3 C4 1.395(5) . ? C3 H3 0.9300 . ? C4 C5 1.371(4) . ? C4 H4 0.9300 . ? C5 C6 1.503(4) . ? C7 C12 1.368(4) . ? C7 C8 1.374(4) . ? C8 C9 1.391(5) . ? C8 H8 0.9300 . ? C9 C10 1.388(4) . ? C9 H9 0.9300 . ? C10 C11 1.356(4) . ? C10 C13 1.521(5) . ? C11 C12 1.392(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.380(4) . ? C14 H14 0.9300 . ? C15 C16 1.357(5) . ? C15 H15 0.9300 . ? C16 C17 1.388(5) . ? C16 H16 0.9300 . ? C17 C18 1.384(4) . ? C17 H17 0.9300 . ? C18 C19 1.492(4) . ? C20 C21 1.363(4) . ? C20 C25 1.393(5) . ? C21 C22 1.390(4) . ? C21 H21 0.9300 . ? C22 C23 1.392(5) . ? C22 H22 0.9300 . ? C23 C24 1.388(5) . ? C23 C26 1.527(5) . ? C24 C25 1.375(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.374(4) . ? C27 H27 0.9300 . ? C28 C29 1.384(5) . ? C28 H28 0.9300 . ? C29 C30 1.388(5) . ? C29 H29 0.9300 . ? C30 C31 1.389(4) . ? C30 H30 0.9300 . ? C31 C32 1.496(4) . ? C33 C34 1.374(4) . ? C33 C38 1.380(5) . ? C34 C35 1.396(4) . ? C34 H34 0.9300 . ? C35 C36 1.381(5) . ? C35 H35 0.9300 . ? C36 C37 1.374(4) . ? C36 C39 1.537(5) . ? C37 C38 1.386(4) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? Co2 N11 1.928(2) . ? Co2 N12 1.932(2) . ? Co2 N7 1.939(2) . ? Co2 N8 1.947(3) . ? Co2 N9 1.963(3) . ? Co2 N10 1.973(3) . ? O4 C45 1.237(4) . ? O5 C58 1.243(4) . ? O6 C71 1.244(4) . ? N7 C40 1.353(4) . ? N7 C44 1.355(4) . ? N8 C45 1.323(4) . ? N8 C46 1.445(3) . ? N9 C53 1.351(4) . ? N9 C57 1.346(4) . ? N10 C58 1.333(4) . ? N10 C59 1.440(4) . ? N11 C70 1.335(4) . ? N11 C66 1.343(4) . ? N12 C71 1.338(3) . ? N12 C72 1.426(3) . ? C40 C41 1.366(4) . ? C40 H40 0.9300 . ? C41 C42 1.374(6) . ? C41 H41 0.9300 . ? C42 C43 1.394(5) . ? C42 H42 0.9300 . ? C43 C44 1.377(4) . ? C43 H43 0.9300 . ? C44 C45 1.499(4) . ? C46 C47 1.382(4) . ? C46 C51 1.385(5) . ? C47 C48 1.383(5) . ? C47 H47 0.9300 . ? C48 C49 1.387(6) . ? C48 H48 0.9300 . ? C49 C50 1.362(5) . ? C49 C52 1.539(5) . ? C50 C51 1.383(4) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C54 1.375(5) . ? C53 H53 0.9300 . ? C54 C55 1.381(6) . ? C54 H54 0.9300 . ? C55 C56 1.392(5) . ? C55 H55 0.9300 . ? C56 C57 1.381(5) . ? C56 H56 0.9300 . ? C57 C58 1.499(5) . ? C59 C60 1.385(4) . ? C59 C64 1.389(4) . ? C60 C61 1.384(5) . ? C60 H60 0.9300 . ? C61 C62 1.374(5) . ? C61 H61 0.9300 . ? C62 C63 1.386(4) . ? C62 C65 1.521(5) . ? C63 C64 1.392(5) . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 C67 1.366(4) . ? C66 H66 0.9300 . ? C67 C68 1.376(5) . ? C67 H67 0.9300 . ? C68 C69 1.369(5) . ? C68 H68 0.9300 . ? C69 C70 1.382(4) . ? C69 H69 0.9300 . ? C70 C71 1.491(4) . ? C72 C77 1.383(4) . ? C72 C73 1.386(4) . ? C73 C74 1.355(4) . ? C73 H73 0.9300 . ? C74 C75 1.371(5) . ? C74 H74 0.9300 . ? C75 C76 1.408(5) . ? C75 C78 1.510(4) . ? C76 C77 1.379(4) . ? C76 H76 0.9300 . ? C77 H77 0.9300 . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? O7 C79 1.699(8) . ? O7 H7A 0.8200 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? O8 C80 1.685(9) . ? O8 H8A 0.8200 . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? O1W H1WA 0.8501 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8506 . ? O2W H2WB 0.8490 . ? 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 N3 Co1 N5 174.41(11) . . ? N3 Co1 N4 83.23(10) . . ? N5 Co1 N4 96.17(10) . . ? N3 Co1 N6 92.13(10) . . ? N5 Co1 N6 82.30(10) . . ? N4 Co1 N6 90.12(11) . . ? N3 Co1 N1 94.65(9) . . ? N5 Co1 N1 86.32(9) . . ? N4 Co1 N1 175.55(11) . . ? N6 Co1 N1 93.87(11) . . ? N3 Co1 N2 89.50(10) . . ? N5 Co1 N2 96.09(10) . . ? N4 Co1 N2 94.04(11) . . ? N6 Co1 N2 175.69(11) . . ? N1 Co1 N2 82.01(10) . . ? C1 N1 C5 117.4(3) . . ? C1 N1 Co1 127.8(2) . . ? C5 N1 Co1 114.6(2) . . ? C6 N2 C7 113.9(3) . . ? C6 N2 Co1 116.6(2) . . ? C7 N2 Co1 129.4(2) . . ? C18 N3 C14 118.7(2) . . ? C18 N3 Co1 113.86(18) . . ? C14 N3 Co1 127.3(2) . . ? C19 N4 C20 118.7(3) . . ? C19 N4 Co1 115.32(19) . . ? C20 N4 Co1 125.45(19) . . ? C27 N5 C31 117.9(2) . . ? C27 N5 Co1 127.5(2) . . ? C31 N5 Co1 114.66(18) . . ? C32 N6 C33 116.6(3) . . ? C32 N6 Co1 116.5(2) . . ? C33 N6 Co1 125.63(19) . . ? N1 C1 C2 122.2(3) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C3 C2 C1 120.1(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 118.3(3) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 119.3(3) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? N1 C5 C4 122.7(3) . . ? N1 C5 C6 114.1(3) . . ? C4 C5 C6 123.3(3) . . ? O1 C6 N2 127.9(3) . . ? O1 C6 C5 119.5(3) . . ? N2 C6 C5 112.7(3) . . ? C12 C7 C8 119.1(3) . . ? C12 C7 N2 120.6(2) . . ? C8 C7 N2 120.2(2) . . ? C7 C8 C9 119.9(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 121.5(3) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C9 117.1(3) . . ? C11 C10 C13 120.2(3) . . ? C9 C10 C13 122.7(3) . . ? C10 C11 C12 122.4(3) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C7 C12 C11 120.0(3) . . ? C7 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C15 121.9(3) . . ? N3 C14 H14 119.1 . . ? C15 C14 H14 119.0 . . ? C16 C15 C14 119.6(3) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 119.2(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 119.0(3) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? N3 C18 C17 121.6(3) . . ? N3 C18 C19 115.3(2) . . ? C17 C18 C19 123.1(3) . . ? O2 C19 N4 128.1(3) . . ? O2 C19 C18 119.8(3) . . ? N4 C19 C18 112.1(3) . . ? C21 C20 C25 118.6(3) . . ? C21 C20 N4 121.4(3) . . ? C25 C20 N4 119.9(3) . . ? C20 C21 C22 121.8(3) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C23 C22 C21 119.6(3) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 118.1(3) . . ? C24 C23 C26 120.3(4) . . ? C22 C23 C26 121.6(4) . . ? C25 C24 C23 121.6(4) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 C20 119.9(3) . . ? C24 C25 H25 120.1 . . ? C20 C25 H25 120.1 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 C28 122.7(3) . . ? N5 C27 H27 118.6 . . ? C28 C27 H27 118.6 . . ? C27 C28 C29 119.3(3) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C30 119.1(3) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C29 C30 C31 119.1(3) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? N5 C31 C30 121.9(3) . . ? N5 C31 C32 114.2(2) . . ? C30 C31 C32 123.8(3) . . ? O3 C32 N6 128.2(3) . . ? O3 C32 C31 119.5(3) . . ? N6 C32 C31 112.3(3) . . ? C34 C33 C38 118.7(3) . . ? C34 C33 N6 120.8(3) . . ? C38 C33 N6 120.5(3) . . ? C33 C34 C35 120.2(3) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 121.3(3) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C37 C36 C35 117.8(3) . . ? C37 C36 C39 122.4(4) . . ? C35 C36 C39 119.9(3) . . ? C36 C37 C38 121.4(4) . . ? C36 C37 H37 119.3 . . ? C38 C37 H37 119.3 . . ? C33 C38 C37 120.6(3) . . ? C33 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N11 Co2 N12 83.22(10) . . ? N11 Co2 N7 174.37(11) . . ? N12 Co2 N7 95.10(10) . . ? N11 Co2 N8 92.64(10) . . ? N12 Co2 N8 89.39(11) . . ? N7 Co2 N8 81.96(10) . . ? N11 Co2 N9 93.97(10) . . ? N12 Co2 N9 176.08(11) . . ? N7 Co2 N9 87.96(10) . . ? N8 Co2 N9 93.48(11) . . ? N11 Co2 N10 89.12(10) . . ? N12 Co2 N10 95.32(11) . . ? N7 Co2 N10 96.40(10) . . ? N8 Co2 N10 175.14(11) . . ? N9 Co2 N10 81.87(11) . . ? C40 N7 C44 118.4(3) . . ? C40 N7 Co2 127.4(2) . . ? C44 N7 Co2 114.14(17) . . ? C45 N8 C46 117.4(3) . . ? C45 N8 Co2 117.5(2) . . ? C46 N8 Co2 124.24(19) . . ? C53 N9 C57 117.9(3) . . ? C53 N9 Co2 128.0(2) . . ? C57 N9 Co2 114.1(2) . . ? C58 N10 C59 116.5(3) . . ? C58 N10 Co2 116.1(2) . . ? C59 N10 Co2 127.1(2) . . ? C70 N11 C66 117.7(2) . . ? C70 N11 Co2 113.90(18) . . ? C66 N11 Co2 128.3(2) . . ? C71 N12 C72 117.9(3) . . ? C71 N12 Co2 115.38(19) . . ? C72 N12 Co2 126.72(18) . . ? N7 C40 C41 121.8(3) . . ? N7 C40 H40 119.1 . . ? C41 C40 H40 119.1 . . ? C40 C41 C42 119.8(3) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C41 C42 C43 119.5(3) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C44 C43 C42 118.0(4) . . ? C44 C43 H43 121.0 . . ? C42 C43 H43 121.0 . . ? N7 C44 C43 122.5(3) . . ? N7 C44 C45 114.9(2) . . ? C43 C44 C45 122.6(3) . . ? O4 C45 N8 127.9(3) . . ? O4 C45 C44 120.9(3) . . ? N8 C45 C44 111.2(3) . . ? C47 C46 C51 118.6(3) . . ? C47 C46 N8 121.1(3) . . ? C51 C46 N8 120.3(3) . . ? C46 C47 C48 119.2(4) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? C47 C48 C49 122.3(3) . . ? C47 C48 H48 118.8 . . ? C49 C48 H48 118.8 . . ? C50 C49 C48 117.8(3) . . ? C50 C49 C52 121.5(5) . . ? C48 C49 C52 120.7(4) . . ? C49 C50 C51 121.0(4) . . ? C49 C50 H50 119.5 . . ? C51 C50 H50 119.5 . . ? C50 C51 C46 121.1(3) . . ? C50 C51 H51 119.5 . . ? C46 C51 H51 119.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N9 C53 C54 123.0(4) . . ? N9 C53 H53 118.5 . . ? C54 C53 H53 118.5 . . ? C53 C54 C55 119.0(4) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? C54 C55 C56 118.6(4) . . ? C54 C55 H55 120.7 . . ? C56 C55 H55 120.7 . . ? C57 C56 C55 119.3(4) . . ? C57 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? N9 C57 C56 122.2(3) . . ? N9 C57 C58 115.4(3) . . ? C56 C57 C58 122.4(3) . . ? O5 C58 N10 128.1(3) . . ? O5 C58 C57 119.8(3) . . ? N10 C58 C57 112.2(3) . . ? C60 C59 C64 118.0(3) . . ? C60 C59 N10 121.0(3) . . ? C64 C59 N10 121.0(2) . . ? C59 C60 C61 120.4(3) . . ? C59 C60 H60 119.8 . . ? C61 C60 H60 119.8 . . ? C62 C61 C60 121.9(3) . . ? C62 C61 H61 119.1 . . ? C60 C61 H61 119.1 . . ? C61 C62 C63 118.1(3) . . ? C61 C62 C65 119.8(3) . . ? C63 C62 C65 122.1(3) . . ? C62 C63 C64 120.4(3) . . ? C62 C63 H63 119.8 . . ? C64 C63 H63 119.8 . . ? C59 C64 C63 121.1(3) . . ? C59 C64 H64 119.5 . . ? C63 C64 H64 119.5 . . ? C62 C65 H65A 109.5 . . ? C62 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C62 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N11 C66 C67 122.8(3) . . ? N11 C66 H66 118.6 . . ? C67 C66 H66 118.6 . . ? C66 C67 C68 119.3(3) . . ? C66 C67 H67 120.3 . . ? C68 C67 H67 120.3 . . ? C69 C68 C67 118.3(3) . . ? C69 C68 H68 120.8 . . ? C67 C68 H68 120.8 . . ? C68 C69 C70 119.6(3) . . ? C68 C69 H69 120.2 . . ? C70 C69 H69 120.2 . . ? N11 C70 C69 122.2(3) . . ? N11 C70 C71 115.1(2) . . ? C69 C70 C71 122.7(3) . . ? O6 C71 N12 128.1(3) . . ? O6 C71 C70 119.7(3) . . ? N12 C71 C70 112.2(3) . . ? C77 C72 C73 117.3(3) . . ? C77 C72 N12 121.2(3) . . ? C73 C72 N12 121.5(3) . . ? C74 C73 C72 121.4(3) . . ? C74 C73 H73 119.3 . . ? C72 C73 H73 119.3 . . ? C73 C74 C75 122.7(3) . . ? C73 C74 H74 118.6 . . ? C75 C74 H74 118.6 . . ? C74 C75 C76 116.4(3) . . ? C74 C75 C78 122.3(3) . . ? C76 C75 C78 121.3(3) . . ? C77 C76 C75 120.9(3) . . ? C77 C76 H76 119.5 . . ? C75 C76 H76 119.5 . . ? C76 C77 C72 121.1(3) . . ? C76 C77 H77 119.4 . . ? C72 C77 H77 119.4 . . ? C75 C78 H78A 109.5 . . ? C75 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C75 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C79 O7 H7A 109.5 . . ? O7 C79 H79A 109.5 . . ? O7 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? O7 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C80 O8 H8A 109.5 . . ? O8 C80 H80A 109.5 . . ? O8 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? O8 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? H1WA O1W H1WB 99.9 . . ? H2WA O2W H2WB 94.6 . . ? 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 N3 Co1 N1 C1 94.1(2) . . . . ? N5 Co1 N1 C1 -80.4(2) . . . . ? N4 Co1 N1 C1 155.5(11) . . . . ? N6 Co1 N1 C1 1.6(2) . . . . ? N2 Co1 N1 C1 -177.1(2) . . . . ? N3 Co1 N1 C5 -89.29(18) . . . . ? N5 Co1 N1 C5 96.23(18) . . . . ? N4 Co1 N1 C5 -27.9(12) . . . . ? N6 Co1 N1 C5 178.25(17) . . . . ? N2 Co1 N1 C5 -0.45(17) . . . . ? N3 Co1 N2 C6 94.39(19) . . . . ? N5 Co1 N2 C6 -85.77(19) . . . . ? N4 Co1 N2 C6 177.57(18) . . . . ? N6 Co1 N2 C6 -17.8(12) . . . . ? N1 Co1 N2 C6 -0.37(18) . . . . ? N3 Co1 N2 C7 -80.9(2) . . . . ? N5 Co1 N2 C7 98.9(2) . . . . ? N4 Co1 N2 C7 2.2(2) . . . . ? N6 Co1 N2 C7 166.8(11) . . . . ? N1 Co1 N2 C7 -175.7(2) . . . . ? N5 Co1 N3 C18 -80.6(11) . . . . ? N4 Co1 N3 C18 3.6(2) . . . . ? N6 Co1 N3 C18 -86.3(2) . . . . ? N1 Co1 N3 C18 179.6(2) . . . . ? N2 Co1 N3 C18 97.7(2) . . . . ? N5 Co1 N3 C14 95.2(11) . . . . ? N4 Co1 N3 C14 179.4(3) . . . . ? N6 Co1 N3 C14 89.5(3) . . . . ? N1 Co1 N3 C14 -4.6(3) . . . . ? N2 Co1 N3 C14 -86.5(3) . . . . ? N3 Co1 N4 C19 -2.0(2) . . . . ? N5 Co1 N4 C19 172.5(2) . . . . ? N6 Co1 N4 C19 90.2(2) . . . . ? N1 Co1 N4 C19 -63.7(12) . . . . ? N2 Co1 N4 C19 -91.0(2) . . . . ? N3 Co1 N4 C20 169.9(3) . . . . ? N5 Co1 N4 C20 -15.7(3) . . . . ? N6 Co1 N4 C20 -98.0(3) . . . . ? N1 Co1 N4 C20 108.1(11) . . . . ? N2 Co1 N4 C20 80.9(3) . . . . ? N3 Co1 N5 C27 173.1(10) . . . . ? N4 Co1 N5 C27 89.5(3) . . . . ? N6 Co1 N5 C27 178.8(3) . . . . ? N1 Co1 N5 C27 -86.8(3) . . . . ? N2 Co1 N5 C27 -5.2(3) . . . . ? N3 Co1 N5 C31 -7.5(12) . . . . ? N4 Co1 N5 C31 -91.1(2) . . . . ? N6 Co1 N5 C31 -1.8(2) . . . . ? N1 Co1 N5 C31 92.6(2) . . . . ? N2 Co1 N5 C31 174.2(2) . . . . ? N3 Co1 N6 C32 179.1(2) . . . . ? N5 Co1 N6 C32 -0.3(2) . . . . ? N4 Co1 N6 C32 95.9(2) . . . . ? N1 Co1 N6 C32 -86.1(2) . . . . ? N2 Co1 N6 C32 -68.7(12) . . . . ? N3 Co1 N6 C33 12.7(2) . . . . ? N5 Co1 N6 C33 -166.7(2) . . . . ? N4 Co1 N6 C33 -70.5(2) . . . . ? N1 Co1 N6 C33 107.5(2) . . . . ? N2 Co1 N6 C33 124.9(11) . . . . ? C5 N1 C1 C2 0.3(4) . . . . ? Co1 N1 C1 C2 176.8(2) . . . . ? N1 C1 C2 C3 0.2(4) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? C2 C3 C4 C5 0.9(4) . . . . ? C1 N1 C5 C4 -0.1(4) . . . . ? Co1 N1 C5 C4 -177.1(2) . . . . ? C1 N1 C5 C6 178.1(2) . . . . ? Co1 N1 C5 C6 1.1(3) . . . . ? C3 C4 C5 N1 -0.5(4) . . . . ? C3 C4 C5 C6 -178.5(2) . . . . ? C7 N2 C6 O1 -3.2(4) . . . . ? Co1 N2 C6 O1 -179.3(2) . . . . ? C7 N2 C6 C5 177.1(2) . . . . ? Co1 N2 C6 C5 1.0(3) . . . . ? N1 C5 C6 O1 178.9(2) . . . . ? C4 C5 C6 O1 -3.0(4) . . . . ? N1 C5 C6 N2 -1.4(3) . . . . ? C4 C5 C6 N2 176.8(2) . . . . ? C6 N2 C7 C12 84.4(4) . . . . ? Co1 N2 C7 C12 -100.2(3) . . . . ? C6 N2 C7 C8 -92.6(3) . . . . ? Co1 N2 C7 C8 82.8(3) . . . . ? C12 C7 C8 C9 -0.2(5) . . . . ? N2 C7 C8 C9 176.8(3) . . . . ? C7 C8 C9 C10 -1.8(6) . . . . ? C8 C9 C10 C11 3.1(6) . . . . ? C8 C9 C10 C13 -175.5(4) . . . . ? C9 C10 C11 C12 -2.6(6) . . . . ? C13 C10 C11 C12 176.1(4) . . . . ? C8 C7 C12 C11 0.8(5) . . . . ? N2 C7 C12 C11 -176.2(3) . . . . ? C10 C11 C12 C7 0.7(6) . . . . ? C18 N3 C14 C15 -0.8(5) . . . . ? Co1 N3 C14 C15 -176.5(3) . . . . ? N3 C14 C15 C16 1.9(6) . . . . ? C14 C15 C16 C17 -2.7(6) . . . . ? C15 C16 C17 C18 2.6(6) . . . . ? C14 N3 C18 C17 0.7(5) . . . . ? Co1 N3 C18 C17 176.9(3) . . . . ? C14 N3 C18 C19 179.3(3) . . . . ? Co1 N3 C18 C19 -4.5(4) . . . . ? C16 C17 C18 N3 -1.6(5) . . . . ? C16 C17 C18 C19 179.9(3) . . . . ? C20 N4 C19 O2 8.8(5) . . . . ? Co1 N4 C19 O2 -178.7(3) . . . . ? C20 N4 C19 C18 -172.3(3) . . . . ? Co1 N4 C19 C18 0.1(4) . . . . ? N3 C18 C19 O2 -178.2(3) . . . . ? C17 C18 C19 O2 0.4(5) . . . . ? N3 C18 C19 N4 2.9(4) . . . . ? C17 C18 C19 N4 -178.5(3) . . . . ? C19 N4 C20 C21 -123.6(4) . . . . ? Co1 N4 C20 C21 64.8(4) . . . . ? C19 N4 C20 C25 60.2(4) . . . . ? Co1 N4 C20 C25 -111.4(3) . . . . ? C25 C20 C21 C22 7.2(5) . . . . ? N4 C20 C21 C22 -169.0(3) . . . . ? C20 C21 C22 C23 -3.1(6) . . . . ? C21 C22 C23 C24 -1.9(6) . . . . ? C21 C22 C23 C26 176.6(4) . . . . ? C22 C23 C24 C25 2.8(6) . . . . ? C26 C23 C24 C25 -175.7(4) . . . . ? C23 C24 C25 C20 1.2(6) . . . . ? C21 C20 C25 C24 -6.2(5) . . . . ? N4 C20 C25 C24 170.1(3) . . . . ? C31 N5 C27 C28 1.1(5) . . . . ? Co1 N5 C27 C28 -179.6(3) . . . . ? N5 C27 C28 C29 0.3(5) . . . . ? C27 C28 C29 C30 -0.5(6) . . . . ? C28 C29 C30 C31 -0.6(5) . . . . ? C27 N5 C31 C30 -2.2(5) . . . . ? Co1 N5 C31 C30 178.3(3) . . . . ? C27 N5 C31 C32 -177.1(3) . . . . ? Co1 N5 C31 C32 3.4(3) . . . . ? C29 C30 C31 N5 2.0(5) . . . . ? C29 C30 C31 C32 176.4(3) . . . . ? C33 N6 C32 O3 -9.8(5) . . . . ? Co1 N6 C32 O3 -177.4(3) . . . . ? C33 N6 C32 C31 169.8(3) . . . . ? Co1 N6 C32 C31 2.2(4) . . . . ? N5 C31 C32 O3 176.0(3) . . . . ? C30 C31 C32 O3 1.2(5) . . . . ? N5 C31 C32 N6 -3.6(4) . . . . ? C30 C31 C32 N6 -178.4(3) . . . . ? C32 N6 C33 C34 109.4(4) . . . . ? Co1 N6 C33 C34 -84.2(4) . . . . ? C32 N6 C33 C38 -72.1(4) . . . . ? Co1 N6 C33 C38 94.3(3) . . . . ? C38 C33 C34 C35 -0.6(5) . . . . ? N6 C33 C34 C35 177.9(3) . . . . ? C33 C34 C35 C36 1.2(6) . . . . ? C34 C35 C36 C37 -1.0(6) . . . . ? C34 C35 C36 C39 179.3(4) . . . . ? C35 C36 C37 C38 0.2(6) . . . . ? C39 C36 C37 C38 179.9(4) . . . . ? C34 C33 C38 C37 -0.2(5) . . . . ? N6 C33 C38 C37 -178.7(3) . . . . ? C36 C37 C38 C33 0.4(6) . . . . ? N11 Co2 N7 C40 159.0(10) . . . . ? N12 Co2 N7 C40 86.6(3) . . . . ? N8 Co2 N7 C40 175.2(3) . . . . ? N9 Co2 N7 C40 -90.9(3) . . . . ? N10 Co2 N7 C40 -9.4(3) . . . . ? N11 Co2 N7 C44 -21.4(12) . . . . ? N12 Co2 N7 C44 -93.8(2) . . . . ? N8 Co2 N7 C44 -5.2(2) . . . . ? N9 Co2 N7 C44 88.6(2) . . . . ? N10 Co2 N7 C44 170.2(2) . . . . ? N11 Co2 N8 C45 -178.6(2) . . . . ? N12 Co2 N8 C45 98.2(2) . . . . ? N7 Co2 N8 C45 3.0(2) . . . . ? N9 Co2 N8 C45 -84.5(2) . . . . ? N10 Co2 N8 C45 -67.5(11) . . . . ? N11 Co2 N8 C46 12.2(2) . . . . ? N12 Co2 N8 C46 -71.0(2) . . . . ? N7 Co2 N8 C46 -166.2(2) . . . . ? N9 Co2 N8 C46 106.3(2) . . . . ? N10 Co2 N8 C46 123.3(10) . . . . ? N11 Co2 N9 C53 95.1(2) . . . . ? N12 Co2 N9 C53 139.1(13) . . . . ? N7 Co2 N9 C53 -79.6(2) . . . . ? N8 Co2 N9 C53 2.2(2) . . . . ? N10 Co2 N9 C53 -176.4(2) . . . . ? N11 Co2 N9 C57 -83.27(19) . . . . ? N12 Co2 N9 C57 -39.2(15) . . . . ? N7 Co2 N9 C57 102.03(19) . . . . ? N8 Co2 N9 C57 -176.16(18) . . . . ? N10 Co2 N9 C57 5.27(18) . . . . ? N11 Co2 N10 C58 88.0(2) . . . . ? N12 Co2 N10 C58 171.15(19) . . . . ? N7 Co2 N10 C58 -93.1(2) . . . . ? N8 Co2 N10 C58 -23.2(12) . . . . ? N9 Co2 N10 C58 -6.09(19) . . . . ? N11 Co2 N10 C59 -84.7(2) . . . . ? N12 Co2 N10 C59 -1.6(2) . . . . ? N7 Co2 N10 C59 94.1(2) . . . . ? N8 Co2 N10 C59 164.0(10) . . . . ? N9 Co2 N10 C59 -178.9(2) . . . . ? N12 Co2 N11 C70 4.2(2) . . . . ? N7 Co2 N11 C70 -68.8(11) . . . . ? N8 Co2 N11 C70 -84.9(2) . . . . ? N9 Co2 N11 C70 -178.5(2) . . . . ? N10 Co2 N11 C70 99.7(2) . . . . ? N12 Co2 N11 C66 -179.2(3) . . . . ? N7 Co2 N11 C66 107.9(11) . . . . ? N8 Co2 N11 C66 91.8(3) . . . . ? N9 Co2 N11 C66 -1.9(3) . . . . ? N10 Co2 N11 C66 -83.7(3) . . . . ? N11 Co2 N12 C71 -2.4(2) . . . . ? N7 Co2 N12 C71 172.2(2) . . . . ? N8 Co2 N12 C71 90.3(2) . . . . ? N9 Co2 N12 C71 -46.8(15) . . . . ? N10 Co2 N12 C71 -90.9(2) . . . . ? N11 Co2 N12 C72 175.5(3) . . . . ? N7 Co2 N12 C72 -9.9(3) . . . . ? N8 Co2 N12 C72 -91.7(3) . . . . ? N9 Co2 N12 C72 131.2(13) . . . . ? N10 Co2 N12 C72 87.1(3) . . . . ? C44 N7 C40 C41 -1.7(5) . . . . ? Co2 N7 C40 C41 177.9(3) . . . . ? N7 C40 C41 C42 0.5(6) . . . . ? C40 C41 C42 C43 0.3(6) . . . . ? C41 C42 C43 C44 0.2(6) . . . . ? C40 N7 C44 C43 2.2(5) . . . . ? Co2 N7 C44 C43 -177.4(3) . . . . ? C40 N7 C44 C45 -173.9(3) . . . . ? Co2 N7 C44 C45 6.5(3) . . . . ? C42 C43 C44 N7 -1.4(5) . . . . ? C42 C43 C44 C45 174.4(3) . . . . ? C46 N8 C45 O4 -9.3(5) . . . . ? Co2 N8 C45 O4 -179.3(3) . . . . ? C46 N8 C45 C44 169.6(3) . . . . ? Co2 N8 C45 C44 -0.3(4) . . . . ? N7 C44 C45 O4 175.0(3) . . . . ? C43 C44 C45 O4 -1.1(5) . . . . ? N7 C44 C45 N8 -4.0(4) . . . . ? C43 C44 C45 N8 179.9(3) . . . . ? C45 N8 C46 C47 102.4(4) . . . . ? Co2 N8 C46 C47 -88.4(3) . . . . ? C45 N8 C46 C51 -79.2(4) . . . . ? Co2 N8 C46 C51 90.1(3) . . . . ? C51 C46 C47 C48 -1.5(5) . . . . ? N8 C46 C47 C48 177.0(3) . . . . ? C46 C47 C48 C49 2.5(6) . . . . ? C47 C48 C49 C50 -2.4(6) . . . . ? C47 C48 C49 C52 178.8(4) . . . . ? C48 C49 C50 C51 1.3(6) . . . . ? C52 C49 C50 C51 -179.9(4) . . . . ? C49 C50 C51 C46 -0.4(6) . . . . ? C47 C46 C51 C50 0.5(5) . . . . ? N8 C46 C51 C50 -178.0(3) . . . . ? C57 N9 C53 C54 -0.4(4) . . . . ? Co2 N9 C53 C54 -178.6(2) . . . . ? N9 C53 C54 C55 1.0(5) . . . . ? C53 C54 C55 C56 -0.6(5) . . . . ? C54 C55 C56 C57 -0.3(5) . . . . ? C53 N9 C57 C56 -0.6(4) . . . . ? Co2 N9 C57 C56 177.9(2) . . . . ? C53 N9 C57 C58 177.6(2) . . . . ? Co2 N9 C57 C58 -3.8(3) . . . . ? C55 C56 C57 N9 0.9(4) . . . . ? C55 C56 C57 C58 -177.2(3) . . . . ? C59 N10 C58 O5 0.0(4) . . . . ? Co2 N10 C58 O5 -173.6(2) . . . . ? C59 N10 C58 C57 179.1(2) . . . . ? Co2 N10 C58 C57 5.5(3) . . . . ? N9 C57 C58 O5 178.1(2) . . . . ? C56 C57 C58 O5 -3.6(4) . . . . ? N9 C57 C58 N10 -1.1(3) . . . . ? C56 C57 C58 N10 177.2(3) . . . . ? C58 N10 C59 C60 83.7(4) . . . . ? Co2 N10 C59 C60 -103.5(3) . . . . ? C58 N10 C59 C64 -97.1(4) . . . . ? Co2 N10 C59 C64 75.6(4) . . . . ? C64 C59 C60 C61 -1.2(6) . . . . ? N10 C59 C60 C61 178.0(3) . . . . ? C59 C60 C61 C62 -0.6(6) . . . . ? C60 C61 C62 C63 2.3(6) . . . . ? C60 C61 C62 C65 -175.8(4) . . . . ? C61 C62 C63 C64 -2.1(6) . . . . ? C65 C62 C63 C64 175.9(4) . . . . ? C60 C59 C64 C63 1.3(5) . . . . ? N10 C59 C64 C63 -177.9(3) . . . . ? C62 C63 C64 C59 0.3(6) . . . . ? C70 N11 C66 C67 0.9(5) . . . . ? Co2 N11 C66 C67 -175.7(3) . . . . ? N11 C66 C67 C68 0.5(6) . . . . ? C66 C67 C68 C69 -1.5(6) . . . . ? C67 C68 C69 C70 1.2(6) . . . . ? C66 N11 C70 C69 -1.2(5) . . . . ? Co2 N11 C70 C69 175.8(3) . . . . ? C66 N11 C70 C71 177.9(3) . . . . ? Co2 N11 C70 C71 -5.1(3) . . . . ? C68 C69 C70 N11 0.1(5) . . . . ? C68 C69 C70 C71 -178.8(3) . . . . ? C72 N12 C71 O6 4.2(5) . . . . ? Co2 N12 C71 O6 -177.6(3) . . . . ? C72 N12 C71 C70 -177.8(3) . . . . ? Co2 N12 C71 C70 0.4(3) . . . . ? N11 C70 C71 O6 -178.7(3) . . . . ? C69 C70 C71 O6 0.3(5) . . . . ? N11 C70 C71 N12 3.1(4) . . . . ? C69 C70 C71 N12 -177.8(3) . . . . ? C71 N12 C72 C77 -111.0(3) . . . . ? Co2 N12 C72 C77 71.1(4) . . . . ? C71 N12 C72 C73 68.7(4) . . . . ? Co2 N12 C72 C73 -109.2(3) . . . . ? C77 C72 C73 C74 -2.2(5) . . . . ? N12 C72 C73 C74 178.1(3) . . . . ? C72 C73 C74 C75 0.4(6) . . . . ? C73 C74 C75 C76 1.8(5) . . . . ? C73 C74 C75 C78 -178.7(4) . . . . ? C74 C75 C76 C77 -2.0(5) . . . . ? C78 C75 C76 C77 178.4(3) . . . . ? C75 C76 C77 C72 0.1(5) . . . . ? C73 C72 C77 C76 2.0(5) . . . . ? N12 C72 C77 C76 -178.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7A O4 0.82 2.05 2.754(5) 143.7 1_655 O1W H1WA O1 0.85 2.03 2.882(4) 179.2 . O1W H1WB O7 0.85 2.03 2.847(5) 161.8 . O2W H2WA O6 0.85 1.93 2.782(5) 179.9 . O2W H2WB O8 0.85 2.02 2.871(8) 179.4 1_455 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.788 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.073 data_q9 _database_code_CSD 189736 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H35 Co N6 O7' _chemical_formula_weight 758.66 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 10.0802(16) _cell_length_b 13.104(2) _cell_length_c 14.813(2) _cell_angle_alpha 97.860(3) _cell_angle_beta 108.441(4) _cell_angle_gamma 105.191(3) _cell_volume 1739.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 2781 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description PRISM _exptl_crystal_colour RED _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.8971 _exptl_absorpt_correction_T_max 0.9165 _exptl_absorpt_process_details 'SADABS; Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11760 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.1136 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.60 _reflns_number_total 7906 _reflns_number_gt 4363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^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 7906 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.25668(5) 0.35843(3) 0.19860(3) 0.02863(13) Uani 1 1 d . . . O1 O -0.1624(2) 0.3258(2) 0.04318(16) 0.0549(7) Uani 1 1 d . . . O2 O 0.0287(3) 0.2266(2) -0.30577(16) 0.0591(8) Uani 1 1 d . . . O3 O 0.6706(3) 0.52187(19) 0.39011(17) 0.0562(7) Uani 1 1 d . . . O4 O 0.6639(3) 0.1075(2) 0.51973(17) 0.0642(8) Uani 1 1 d . . . O5 O 0.2064(3) 0.04382(19) 0.11452(19) 0.0602(8) Uani 1 1 d . . . O6 O -0.2432(2) -0.01911(19) 0.31431(16) 0.0514(7) Uani 1 1 d . . . N1 N 0.1337(3) 0.38480(19) 0.26842(18) 0.0301(6) Uani 1 1 d . . . N2 N 0.0830(3) 0.3409(2) 0.08507(17) 0.0300(6) Uani 1 1 d . . . N3 N 0.3359(3) 0.51543(19) 0.21343(16) 0.0282(6) Uani 1 1 d . . . N4 N 0.4404(3) 0.3907(2) 0.31485(17) 0.0309(6) Uani 1 1 d . . . N5 N 0.3606(3) 0.3194(2) 0.11795(16) 0.0298(6) Uani 1 1 d . . . N6 N 0.1900(3) 0.20335(19) 0.18750(17) 0.0304(6) Uani 1 1 d . . . C1 C 0.1693(4) 0.4131(3) 0.3657(2) 0.0367(8) Uani 1 1 d . . . H1 H 0.2669 0.4277 0.4068 0.044 Uiso 1 1 calc R . . C2 C 0.0673(4) 0.4214(3) 0.4068(2) 0.0463(10) Uani 1 1 d . . . H2 H 0.0962 0.4413 0.4746 0.056 Uiso 1 1 calc R . . C3 C -0.0765(4) 0.4005(3) 0.3483(2) 0.0462(10) Uani 1 1 d . . . H3 H -0.1475 0.4041 0.3753 0.055 Uiso 1 1 calc R . . C4 C -0.1136(4) 0.3740(3) 0.2483(2) 0.0435(9) Uani 1 1 d . . . H4 H -0.2103 0.3609 0.2065 0.052 Uiso 1 1 calc R . . C5 C -0.0076(3) 0.3668(2) 0.2105(2) 0.0315(8) Uani 1 1 d . . . C6 C -0.0377(4) 0.3408(3) 0.1025(2) 0.0359(8) Uani 1 1 d . . . C7 C 0.0694(3) 0.3132(2) -0.0155(2) 0.0298(8) Uani 1 1 d . . . C8 C 0.1039(4) 0.3937(3) -0.0632(2) 0.0404(9) Uani 1 1 d . . . H8 H 0.1350 0.4664 -0.0302 0.048 Uiso 1 1 calc R . . C9 C 0.0929(4) 0.3674(3) -0.1601(2) 0.0445(10) Uani 1 1 d . . . H9 H 0.1182 0.4224 -0.1911 0.053 Uiso 1 1 calc R . . C10 C 0.0445(4) 0.2600(3) -0.2101(2) 0.0408(9) Uani 1 1 d . . . C11 C 0.0095(4) 0.1792(3) -0.1633(2) 0.0471(10) Uani 1 1 d . . . H11 H -0.0227 0.1065 -0.1969 0.057 Uiso 1 1 calc R . . C12 C 0.0217(4) 0.2049(3) -0.0668(2) 0.0407(9) Uani 1 1 d . . . H12 H -0.0021 0.1494 -0.0358 0.049 Uiso 1 1 calc R . . C13 C 0.0180(4) 0.3026(3) -0.3647(2) 0.0679(13) Uani 1 1 d . . . H13A H -0.0558 0.3339 -0.3587 0.102 Uiso 1 1 calc R . . H13B H -0.0093 0.2663 -0.4319 0.102 Uiso 1 1 calc R . . H13C H 0.1117 0.3591 -0.3435 0.102 Uiso 1 1 calc R . . C14 C 0.2694(4) 0.5797(3) 0.1673(2) 0.0350(8) Uani 1 1 d . . . H14 H 0.1699 0.5503 0.1271 0.042 Uiso 1 1 calc R . . C15 C 0.3417(4) 0.6872(3) 0.1767(2) 0.0430(9) Uani 1 1 d . . . H15 H 0.2914 0.7302 0.1451 0.052 Uiso 1 1 calc R . . C16 C 0.4903(4) 0.7306(3) 0.2339(2) 0.0493(10) Uani 1 1 d . . . H16 H 0.5436 0.8018 0.2378 0.059 Uiso 1 1 calc R . . C17 C 0.5576(4) 0.6669(3) 0.2845(2) 0.0448(10) Uani 1 1 d . . . H17 H 0.6568 0.6955 0.3253 0.054 Uiso 1 1 calc R . . C18 C 0.4788(3) 0.5605(3) 0.2751(2) 0.0343(8) Uani 1 1 d . . . C19 C 0.5405(4) 0.4883(3) 0.3318(2) 0.0356(8) Uani 1 1 d . . . C20 C 0.4940(3) 0.3169(3) 0.3674(2) 0.0321(8) Uani 1 1 d . . . C21 C 0.5512(4) 0.2448(3) 0.3294(2) 0.0459(9) Uani 1 1 d . . . H21 H 0.5526 0.2422 0.2666 0.055 Uiso 1 1 calc R . . C22 C 0.6061(4) 0.1768(3) 0.3811(3) 0.0543(10) Uani 1 1 d . . . H22 H 0.6441 0.1289 0.3534 0.065 Uiso 1 1 calc R . . C23 C 0.6055(4) 0.1787(3) 0.4739(3) 0.0432(9) Uani 1 1 d . . . C24 C 0.5510(4) 0.2503(3) 0.5141(2) 0.0451(9) Uani 1 1 d . . . H24 H 0.5517 0.2533 0.5774 0.054 Uiso 1 1 calc R . . C25 C 0.4944(4) 0.3187(3) 0.4607(2) 0.0421(9) Uani 1 1 d . . . H25 H 0.4561 0.3665 0.4883 0.050 Uiso 1 1 calc R . . C26 C 0.6600(4) 0.1027(3) 0.6147(3) 0.0673(13) Uani 1 1 d . . . H26A H 0.7212 0.1711 0.6603 0.101 Uiso 1 1 calc R . . H26B H 0.6960 0.0457 0.6357 0.101 Uiso 1 1 calc R . . H26C H 0.5601 0.0882 0.6118 0.101 Uiso 1 1 calc R . . C27 C 0.4500(3) 0.3839(3) 0.0839(2) 0.0393(9) Uani 1 1 d . . . H27 H 0.4649 0.4583 0.0985 0.047 Uiso 1 1 calc R . . C28 C 0.5206(4) 0.3459(3) 0.0285(2) 0.0497(10) Uani 1 1 d . . . H28 H 0.5819 0.3938 0.0063 0.060 Uiso 1 1 calc R . . C29 C 0.4999(4) 0.2357(3) 0.0060(3) 0.0578(11) Uani 1 1 d . . . H29 H 0.5474 0.2079 -0.0310 0.069 Uiso 1 1 calc R . . C30 C 0.4074(4) 0.1684(3) 0.0397(2) 0.0480(10) Uani 1 1 d . . . H30 H 0.3913 0.0938 0.0254 0.058 Uiso 1 1 calc R . . C31 C 0.3389(3) 0.2107(3) 0.0945(2) 0.0348(8) Uani 1 1 d . . . C32 C 0.2373(4) 0.1436(3) 0.1338(2) 0.0391(9) Uani 1 1 d . . . C33 C 0.0808(4) 0.1474(2) 0.2219(2) 0.0323(8) Uani 1 1 d . . . C34 C 0.1185(4) 0.1367(3) 0.3157(2) 0.0451(10) Uani 1 1 d . . . H34 H 0.2167 0.1667 0.3581 0.054 Uiso 1 1 calc R . . C35 C 0.0144(4) 0.0821(3) 0.3494(2) 0.0540(11) Uani 1 1 d . . . H35 H 0.0430 0.0757 0.4140 0.065 Uiso 1 1 calc R . . C36 C -0.1316(4) 0.0370(3) 0.2881(2) 0.0364(8) Uani 1 1 d . . . C37 C -0.1699(4) 0.0485(3) 0.1945(2) 0.0469(10) Uani 1 1 d . . . H37 H -0.2686 0.0202 0.1529 0.056 Uiso 1 1 calc R . . C38 C -0.0668(4) 0.1006(3) 0.1602(2) 0.0457(10) Uani 1 1 d . . . H38 H -0.0954 0.1049 0.0951 0.055 Uiso 1 1 calc R . . C39 C -0.1997(4) -0.0443(3) 0.4072(2) 0.0557(11) Uani 1 1 d . . . H39A H -0.1338 -0.0859 0.4098 0.084 Uiso 1 1 calc R . . H39B H -0.2856 -0.0859 0.4170 0.084 Uiso 1 1 calc R . . H39C H -0.1504 0.0220 0.4577 0.084 Uiso 1 1 calc R . . O1W O 0.6088(6) 0.0758(4) -0.1204(5) 0.248(3) Uani 1 1 d . . . H1WA H 0.5782 0.0134 -0.1097 0.297 Uiso 1 1 d R . . H1WB H 0.6830 0.0787 -0.1369 0.297 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 0.0258(3) 0.0276(2) 0.0267(2) 0.00510(18) 0.0045(2) 0.00657(19) O1 0.0298(15) 0.090(2) 0.0348(14) 0.0067(13) 0.0025(12) 0.0200(14) O2 0.088(2) 0.0604(17) 0.0344(14) 0.0107(13) 0.0298(14) 0.0247(15) O3 0.0292(14) 0.0502(16) 0.0594(16) 0.0153(13) -0.0116(12) -0.0021(12) O4 0.086(2) 0.0655(18) 0.0514(16) 0.0263(14) 0.0158(15) 0.0470(16) O5 0.0677(19) 0.0267(14) 0.091(2) 0.0073(13) 0.0416(16) 0.0114(13) O6 0.0399(15) 0.0605(17) 0.0489(15) 0.0174(13) 0.0184(13) 0.0036(13) N1 0.0282(16) 0.0286(15) 0.0296(15) 0.0089(12) 0.0051(13) 0.0086(12) N2 0.0233(15) 0.0356(16) 0.0236(14) 0.0033(12) 0.0036(12) 0.0055(12) N3 0.0277(16) 0.0267(15) 0.0246(14) 0.0026(11) 0.0055(12) 0.0067(12) N4 0.0233(15) 0.0322(15) 0.0293(14) 0.0065(12) 0.0015(12) 0.0070(13) N5 0.0257(15) 0.0336(16) 0.0261(14) 0.0104(12) 0.0049(12) 0.0075(13) N6 0.0302(16) 0.0262(15) 0.0309(15) 0.0057(12) 0.0084(13) 0.0070(13) C1 0.035(2) 0.046(2) 0.0238(18) 0.0044(15) 0.0046(16) 0.0142(17) C2 0.045(2) 0.058(2) 0.030(2) 0.0007(17) 0.0118(19) 0.015(2) C3 0.038(2) 0.061(3) 0.042(2) 0.0061(19) 0.0184(19) 0.0183(19) C4 0.026(2) 0.059(2) 0.037(2) 0.0054(18) 0.0066(17) 0.0099(18) C5 0.0280(19) 0.0321(19) 0.0305(18) 0.0082(15) 0.0064(16) 0.0085(15) C6 0.030(2) 0.037(2) 0.0314(19) 0.0082(15) 0.0021(17) 0.0076(16) C7 0.0215(18) 0.0338(19) 0.0250(17) 0.0057(15) -0.0001(14) 0.0060(15) C8 0.046(2) 0.0306(19) 0.0331(19) 0.0052(16) 0.0067(17) 0.0040(17) C9 0.055(2) 0.042(2) 0.034(2) 0.0158(17) 0.0173(18) 0.0084(19) C10 0.044(2) 0.049(2) 0.0274(19) 0.0090(17) 0.0125(17) 0.0129(18) C11 0.063(3) 0.035(2) 0.032(2) -0.0002(16) 0.0114(19) 0.0092(19) C12 0.048(2) 0.034(2) 0.0316(19) 0.0088(16) 0.0090(17) 0.0078(17) C13 0.082(3) 0.077(3) 0.039(2) 0.023(2) 0.018(2) 0.017(3) C14 0.033(2) 0.0322(19) 0.0317(18) 0.0055(15) 0.0027(16) 0.0096(16) C15 0.052(2) 0.0295(19) 0.039(2) 0.0066(16) 0.0058(18) 0.0131(18) C16 0.053(3) 0.033(2) 0.043(2) 0.0068(17) 0.007(2) -0.0029(19) C17 0.038(2) 0.034(2) 0.043(2) 0.0041(17) 0.0023(18) -0.0014(17) C18 0.0280(19) 0.0318(19) 0.0339(19) 0.0060(15) 0.0041(16) 0.0050(16) C19 0.029(2) 0.039(2) 0.0309(18) 0.0044(16) 0.0039(16) 0.0083(17) C20 0.0259(19) 0.0354(19) 0.0315(18) 0.0109(15) 0.0035(15) 0.0113(15) C21 0.050(2) 0.057(2) 0.037(2) 0.0131(18) 0.0146(19) 0.029(2) C22 0.069(3) 0.060(3) 0.045(2) 0.013(2) 0.020(2) 0.041(2) C23 0.042(2) 0.042(2) 0.040(2) 0.0139(18) 0.0038(18) 0.0174(18) C24 0.052(2) 0.052(2) 0.035(2) 0.0188(18) 0.0118(18) 0.024(2) C25 0.039(2) 0.049(2) 0.038(2) 0.0094(17) 0.0095(17) 0.0198(18) C26 0.070(3) 0.078(3) 0.060(3) 0.043(2) 0.012(2) 0.035(2) C27 0.037(2) 0.041(2) 0.0355(19) 0.0106(17) 0.0115(18) 0.0066(17) C28 0.048(2) 0.061(3) 0.047(2) 0.019(2) 0.027(2) 0.014(2) C29 0.058(3) 0.067(3) 0.053(2) 0.005(2) 0.033(2) 0.017(2) C30 0.044(2) 0.043(2) 0.051(2) -0.0011(18) 0.019(2) 0.0090(19) C31 0.031(2) 0.038(2) 0.0296(18) 0.0035(15) 0.0075(16) 0.0087(16) C32 0.034(2) 0.035(2) 0.040(2) 0.0056(17) 0.0072(17) 0.0063(17) C33 0.034(2) 0.0248(17) 0.0355(19) 0.0082(15) 0.0113(17) 0.0065(15) C34 0.034(2) 0.055(2) 0.032(2) 0.0131(17) 0.0045(17) -0.0006(18) C35 0.049(3) 0.069(3) 0.032(2) 0.0155(19) 0.0116(19) 0.003(2) C36 0.034(2) 0.0326(19) 0.041(2) 0.0091(16) 0.0154(18) 0.0056(16) C37 0.033(2) 0.045(2) 0.047(2) 0.0117(18) 0.0037(18) -0.0004(18) C38 0.041(2) 0.052(2) 0.034(2) 0.0181(17) 0.0072(18) 0.0025(19) C39 0.057(3) 0.056(3) 0.055(2) 0.017(2) 0.029(2) 0.007(2) O1W 0.288(6) 0.150(4) 0.545(10) 0.223(5) 0.326(7) 0.174(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 1.914(3) . ? Co1 N5 1.922(3) . ? Co1 N6 1.932(2) . ? Co1 N2 1.940(2) . ? Co1 N3 1.955(2) . ? Co1 N4 1.986(2) . ? O1 C6 1.231(3) . ? O2 C10 1.369(3) . ? O2 C13 1.413(4) . ? O3 C19 1.240(3) . ? O4 C23 1.374(4) . ? O4 C26 1.429(4) . ? O5 C32 1.232(4) . ? O6 C36 1.369(3) . ? O6 C39 1.419(4) . ? N1 C1 1.342(3) . ? N1 C5 1.347(4) . ? N2 C6 1.322(4) . ? N2 C7 1.438(4) . ? N3 C14 1.339(4) . ? N3 C18 1.353(3) . ? N4 C19 1.340(4) . ? N4 C20 1.430(4) . ? N5 C27 1.336(4) . ? N5 C31 1.361(4) . ? N6 C32 1.318(4) . ? N6 C33 1.430(4) . ? C1 C2 1.369(4) . ? C1 H1 0.9300 . ? C2 C3 1.364(4) . ? C2 H2 0.9300 . ? C3 C4 1.377(4) . ? C3 H3 0.9300 . ? C4 C5 1.372(4) . ? C4 H4 0.9300 . ? C5 C6 1.502(4) . ? C7 C8 1.378(4) . ? C7 C12 1.393(4) . ? C8 C9 1.391(4) . ? C8 H8 0.9300 . ? C9 C10 1.376(4) . ? C9 H9 0.9300 . ? C10 C11 1.374(4) . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.370(4) . ? C14 H14 0.9300 . ? C15 C16 1.380(4) . ? C15 H15 0.9300 . ? C16 C17 1.366(5) . ? C16 H16 0.9300 . ? C17 C18 1.375(4) . ? C17 H17 0.9300 . ? C18 C19 1.477(4) . ? C20 C21 1.374(4) . ? C20 C25 1.378(4) . ? C21 C22 1.365(4) . ? C21 H21 0.9300 . ? C22 C23 1.373(4) . ? C22 H22 0.9300 . ? C23 C24 1.365(5) . ? C24 C25 1.390(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.368(4) . ? C27 H27 0.9300 . ? C28 C29 1.381(5) . ? C28 H28 0.9300 . ? C29 C30 1.371(4) . ? C29 H29 0.9300 . ? C30 C31 1.370(4) . ? C30 H30 0.9300 . ? C31 C32 1.485(4) . ? C33 C34 1.356(4) . ? C33 C38 1.390(4) . ? C34 C35 1.378(4) . ? C34 H34 0.9300 . ? C35 C36 1.375(4) . ? C35 H35 0.9300 . ? C36 C37 1.358(4) . ? C37 C38 1.365(4) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? O1W H1WA 0.8499 . ? O1W H1WB 0.8501 . ? 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 N5 173.56(10) . . ? N1 Co1 N6 92.90(11) . . ? N5 Co1 N6 82.95(11) . . ? N1 Co1 N2 82.89(11) . . ? N5 Co1 N2 92.12(10) . . ? N6 Co1 N2 89.59(10) . . ? N1 Co1 N3 88.97(10) . . ? N5 Co1 N3 95.42(10) . . ? N6 Co1 N3 176.68(11) . . ? N2 Co1 N3 93.37(10) . . ? N1 Co1 N4 97.10(10) . . ? N5 Co1 N4 88.23(10) . . ? N6 Co1 N4 95.62(10) . . ? N2 Co1 N4 174.79(11) . . ? N3 Co1 N4 81.42(10) . . ? C10 O2 C13 117.6(3) . . ? C23 O4 C26 118.0(3) . . ? C36 O6 C39 116.3(3) . . ? C1 N1 C5 117.6(3) . . ? C1 N1 Co1 128.2(2) . . ? C5 N1 Co1 114.1(2) . . ? C6 N2 C7 117.7(3) . . ? C6 N2 Co1 116.0(2) . . ? C7 N2 Co1 125.7(2) . . ? C14 N3 C18 118.0(3) . . ? C14 N3 Co1 128.2(2) . . ? C18 N3 Co1 113.6(2) . . ? C19 N4 C20 115.2(3) . . ? C19 N4 Co1 114.3(2) . . ? C20 N4 Co1 128.6(2) . . ? C27 N5 C31 117.4(3) . . ? C27 N5 Co1 128.9(2) . . ? C31 N5 Co1 113.7(2) . . ? C32 N6 C33 117.5(3) . . ? C32 N6 Co1 116.4(2) . . ? C33 N6 Co1 125.6(2) . . ? N1 C1 C2 122.4(3) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C3 C2 C1 120.1(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 118.0(3) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? N1 C5 C4 122.0(3) . . ? N1 C5 C6 114.7(3) . . ? C4 C5 C6 123.3(3) . . ? O1 C6 N2 128.4(3) . . ? O1 C6 C5 119.9(3) . . ? N2 C6 C5 111.6(3) . . ? C8 C7 C12 118.6(3) . . ? C8 C7 N2 120.5(3) . . ? C12 C7 N2 120.9(3) . . ? C7 C8 C9 120.7(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? O2 C10 C11 116.3(3) . . ? O2 C10 C9 124.1(3) . . ? C11 C10 C9 119.6(3) . . ? C10 C11 C12 120.5(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C7 120.4(3) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? O2 C13 H13A 109.5 . . ? O2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C15 122.7(3) . . ? N3 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? C14 C15 C16 119.0(3) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C17 C16 C15 118.7(3) . . ? C17 C16 H16 120.7 . . ? C15 C16 H16 120.7 . . ? C16 C17 C18 120.0(3) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? N3 C18 C17 121.3(3) . . ? N3 C18 C19 115.2(3) . . ? C17 C18 C19 123.4(3) . . ? O3 C19 N4 127.0(3) . . ? O3 C19 C18 120.2(3) . . ? N4 C19 C18 112.7(3) . . ? C21 C20 C25 117.4(3) . . ? C21 C20 N4 122.2(3) . . ? C25 C20 N4 120.3(3) . . ? C22 C21 C20 121.9(3) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 120.4(4) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 119.1(3) . . ? C24 C23 O4 125.1(3) . . ? C22 C23 O4 115.7(3) . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C20 C25 C24 121.1(3) . . ? C20 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? O4 C26 H26A 109.5 . . ? O4 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O4 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 C28 123.3(3) . . ? N5 C27 H27 118.4 . . ? C28 C27 H27 118.4 . . ? C27 C28 C29 119.2(3) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C28 118.2(4) . . ? C30 C29 H29 120.9 . . ? C28 C29 H29 120.9 . . ? C31 C30 C29 120.2(4) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? N5 C31 C30 121.7(3) . . ? N5 C31 C32 114.6(3) . . ? C30 C31 C32 123.7(3) . . ? O5 C32 N6 127.7(3) . . ? O5 C32 C31 120.0(3) . . ? N6 C32 C31 112.3(3) . . ? C34 C33 C38 117.8(3) . . ? C34 C33 N6 120.9(3) . . ? C38 C33 N6 121.2(3) . . ? C33 C34 C35 121.4(3) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C36 C35 C34 120.4(3) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C37 C36 O6 116.8(3) . . ? C37 C36 C35 118.3(3) . . ? O6 C36 C35 124.9(3) . . ? C36 C37 C38 121.5(3) . . ? C36 C37 H37 119.2 . . ? C38 C37 H37 119.2 . . ? C37 C38 C33 120.5(3) . . ? C37 C38 H38 119.8 . . ? C33 C38 H38 119.8 . . ? O6 C39 H39A 109.5 . . ? O6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? O6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? H1WA O1W H1WB 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 N5 Co1 N1 C1 144.3(9) . . . . ? N6 Co1 N1 C1 94.5(3) . . . . ? N2 Co1 N1 C1 -176.2(3) . . . . ? N3 Co1 N1 C1 -82.7(3) . . . . ? N4 Co1 N1 C1 -1.5(3) . . . . ? N5 Co1 N1 C5 -32.3(11) . . . . ? N6 Co1 N1 C5 -82.0(2) . . . . ? N2 Co1 N1 C5 7.2(2) . . . . ? N3 Co1 N1 C5 100.8(2) . . . . ? N4 Co1 N1 C5 -178.0(2) . . . . ? N1 Co1 N2 C6 -7.6(2) . . . . ? N5 Co1 N2 C6 168.3(2) . . . . ? N6 Co1 N2 C6 85.4(2) . . . . ? N3 Co1 N2 C6 -96.1(2) . . . . ? N4 Co1 N2 C6 -97.9(12) . . . . ? N1 Co1 N2 C7 -178.4(2) . . . . ? N5 Co1 N2 C7 -2.5(2) . . . . ? N6 Co1 N2 C7 -85.4(2) . . . . ? N3 Co1 N2 C7 93.1(2) . . . . ? N4 Co1 N2 C7 91.3(12) . . . . ? N1 Co1 N3 C14 -73.1(3) . . . . ? N5 Co1 N3 C14 102.2(3) . . . . ? N6 Co1 N3 C14 162.5(17) . . . . ? N2 Co1 N3 C14 9.7(3) . . . . ? N4 Co1 N3 C14 -170.4(3) . . . . ? N1 Co1 N3 C18 110.6(2) . . . . ? N5 Co1 N3 C18 -74.1(2) . . . . ? N6 Co1 N3 C18 -13.8(19) . . . . ? N2 Co1 N3 C18 -166.6(2) . . . . ? N4 Co1 N3 C18 13.2(2) . . . . ? N1 Co1 N4 C19 -103.0(2) . . . . ? N5 Co1 N4 C19 80.7(2) . . . . ? N6 Co1 N4 C19 163.4(2) . . . . ? N2 Co1 N4 C19 -13.3(13) . . . . ? N3 Co1 N4 C19 -15.1(2) . . . . ? N1 Co1 N4 C20 93.3(3) . . . . ? N5 Co1 N4 C20 -83.0(3) . . . . ? N6 Co1 N4 C20 -0.3(3) . . . . ? N2 Co1 N4 C20 -177.1(11) . . . . ? N3 Co1 N4 C20 -178.8(3) . . . . ? N1 Co1 N5 C27 130.4(9) . . . . ? N6 Co1 N5 C27 -179.5(3) . . . . ? N2 Co1 N5 C27 91.2(3) . . . . ? N3 Co1 N5 C27 -2.4(3) . . . . ? N4 Co1 N5 C27 -83.6(3) . . . . ? N1 Co1 N5 C31 -50.3(11) . . . . ? N6 Co1 N5 C31 -0.2(2) . . . . ? N2 Co1 N5 C31 -89.5(2) . . . . ? N3 Co1 N5 C31 176.9(2) . . . . ? N4 Co1 N5 C31 95.7(2) . . . . ? N1 Co1 N6 C32 174.0(2) . . . . ? N5 Co1 N6 C32 -1.0(2) . . . . ? N2 Co1 N6 C32 91.2(2) . . . . ? N3 Co1 N6 C32 -61.7(19) . . . . ? N4 Co1 N6 C32 -88.5(2) . . . . ? N1 Co1 N6 C33 2.2(2) . . . . ? N5 Co1 N6 C33 -172.8(2) . . . . ? N2 Co1 N6 C33 -80.6(2) . . . . ? N3 Co1 N6 C33 126.5(18) . . . . ? N4 Co1 N6 C33 99.7(2) . . . . ? C5 N1 C1 C2 1.6(5) . . . . ? Co1 N1 C1 C2 -174.8(3) . . . . ? N1 C1 C2 C3 0.0(5) . . . . ? C1 C2 C3 C4 -1.6(5) . . . . ? C2 C3 C4 C5 1.5(5) . . . . ? C1 N1 C5 C4 -1.7(5) . . . . ? Co1 N1 C5 C4 175.2(3) . . . . ? C1 N1 C5 C6 177.1(3) . . . . ? Co1 N1 C5 C6 -5.9(3) . . . . ? C3 C4 C5 N1 0.2(5) . . . . ? C3 C4 C5 C6 -178.6(3) . . . . ? C7 N2 C6 O1 -4.5(5) . . . . ? Co1 N2 C6 O1 -176.1(3) . . . . ? C7 N2 C6 C5 177.7(3) . . . . ? Co1 N2 C6 C5 6.1(3) . . . . ? N1 C5 C6 O1 -178.1(3) . . . . ? C4 C5 C6 O1 0.7(5) . . . . ? N1 C5 C6 N2 -0.1(4) . . . . ? C4 C5 C6 N2 178.7(3) . . . . ? C6 N2 C7 C8 97.4(4) . . . . ? Co1 N2 C7 C8 -91.9(3) . . . . ? C6 N2 C7 C12 -82.8(4) . . . . ? Co1 N2 C7 C12 87.8(3) . . . . ? C12 C7 C8 C9 -0.7(5) . . . . ? N2 C7 C8 C9 179.1(3) . . . . ? C7 C8 C9 C10 1.1(5) . . . . ? C13 O2 C10 C11 160.6(3) . . . . ? C13 O2 C10 C9 -19.6(5) . . . . ? C8 C9 C10 O2 179.2(3) . . . . ? C8 C9 C10 C11 -1.0(6) . . . . ? O2 C10 C11 C12 -179.9(3) . . . . ? C9 C10 C11 C12 0.3(6) . . . . ? C10 C11 C12 C7 0.2(6) . . . . ? C8 C7 C12 C11 0.0(5) . . . . ? N2 C7 C12 C11 -179.8(3) . . . . ? C18 N3 C14 C15 2.9(5) . . . . ? Co1 N3 C14 C15 -173.3(2) . . . . ? N3 C14 C15 C16 1.9(5) . . . . ? C14 C15 C16 C17 -4.5(5) . . . . ? C15 C16 C17 C18 2.4(5) . . . . ? C14 N3 C18 C17 -5.1(4) . . . . ? Co1 N3 C18 C17 171.6(3) . . . . ? C14 N3 C18 C19 173.5(3) . . . . ? Co1 N3 C18 C19 -9.7(3) . . . . ? C16 C17 C18 N3 2.5(5) . . . . ? C16 C17 C18 C19 -176.0(3) . . . . ? C20 N4 C19 O3 -3.1(5) . . . . ? Co1 N4 C19 O3 -169.1(3) . . . . ? C20 N4 C19 C18 179.6(3) . . . . ? Co1 N4 C19 C18 13.6(3) . . . . ? N3 C18 C19 O3 179.8(3) . . . . ? C17 C18 C19 O3 -1.5(5) . . . . ? N3 C18 C19 N4 -2.7(4) . . . . ? C17 C18 C19 N4 176.0(3) . . . . ? C19 N4 C20 C21 -91.1(4) . . . . ? Co1 N4 C20 C21 72.4(4) . . . . ? C19 N4 C20 C25 86.6(4) . . . . ? Co1 N4 C20 C25 -109.8(3) . . . . ? C25 C20 C21 C22 0.3(5) . . . . ? N4 C20 C21 C22 178.1(3) . . . . ? C20 C21 C22 C23 0.0(6) . . . . ? C21 C22 C23 C24 -0.8(5) . . . . ? C21 C22 C23 O4 -179.7(3) . . . . ? C26 O4 C23 C24 3.9(5) . . . . ? C26 O4 C23 C22 -177.3(3) . . . . ? C22 C23 C24 C25 1.2(5) . . . . ? O4 C23 C24 C25 180.0(3) . . . . ? C21 C20 C25 C24 0.2(5) . . . . ? N4 C20 C25 C24 -177.7(3) . . . . ? C23 C24 C25 C20 -0.9(5) . . . . ? C31 N5 C27 C28 -0.9(4) . . . . ? Co1 N5 C27 C28 178.4(2) . . . . ? N5 C27 C28 C29 0.0(5) . . . . ? C27 C28 C29 C30 0.6(5) . . . . ? C28 C29 C30 C31 -0.3(5) . . . . ? C27 N5 C31 C30 1.2(4) . . . . ? Co1 N5 C31 C30 -178.2(2) . . . . ? C27 N5 C31 C32 -179.4(3) . . . . ? Co1 N5 C31 C32 1.2(3) . . . . ? C29 C30 C31 N5 -0.6(5) . . . . ? C29 C30 C31 C32 180.0(3) . . . . ? C33 N6 C32 O5 -5.5(5) . . . . ? Co1 N6 C32 O5 -178.0(3) . . . . ? C33 N6 C32 C31 174.4(3) . . . . ? Co1 N6 C32 C31 1.9(3) . . . . ? N5 C31 C32 O5 177.8(3) . . . . ? C30 C31 C32 O5 -2.7(5) . . . . ? N5 C31 C32 N6 -2.0(4) . . . . ? C30 C31 C32 N6 177.4(3) . . . . ? C32 N6 C33 C34 101.6(4) . . . . ? Co1 N6 C33 C34 -86.7(4) . . . . ? C32 N6 C33 C38 -77.2(4) . . . . ? Co1 N6 C33 C38 94.5(3) . . . . ? C38 C33 C34 C35 -0.6(5) . . . . ? N6 C33 C34 C35 -179.4(3) . . . . ? C33 C34 C35 C36 -0.1(6) . . . . ? C39 O6 C36 C37 171.3(3) . . . . ? C39 O6 C36 C35 -8.9(5) . . . . ? C34 C35 C36 C37 -0.5(5) . . . . ? C34 C35 C36 O6 179.7(3) . . . . ? O6 C36 C37 C38 -178.4(3) . . . . ? C35 C36 C37 C38 1.8(5) . . . . ? C36 C37 C38 C33 -2.5(6) . . . . ? C34 C33 C38 C37 1.9(5) . . . . ? N6 C33 C38 C37 -179.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WB O5 0.85 2.19 2.720(5) 120.6 2_655 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.667 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.068