# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 842832' #TrackingRef '- 842832.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H39 Co2 N7 O18' _chemical_formula_sum 'C62 H39 Co2 N7 O18' _chemical_formula_weight 1287.86 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2637(15) _cell_length_b 11.4301(14) _cell_length_c 12.4309(16) _cell_angle_alpha 102.078(4) _cell_angle_beta 109.688(4) _cell_angle_gamma 92.306(4) _cell_volume 1462.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7118 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.42 _exptl_crystal_description sheet _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 658 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8813 _exptl_absorpt_correction_T_max 0.9380 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 17846 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.01 _reflns_number_total 5655 _reflns_number_gt 4542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0463P)^2^+1.5965P] 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 5655 _refine_ls_number_parameters 511 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.14473(3) 0.51405(3) 0.41999(3) 0.03285(11) Uani 1 1 d . . . C1 C -0.1478(2) 0.4311(2) 0.3355(2) 0.0344(5) Uani 1 1 d . . . C2 C -0.1990(3) 0.3434(2) 0.2175(2) 0.0395(6) Uani 1 1 d . . . C3 C -0.3075(3) 0.2643(3) 0.1860(3) 0.0589(9) Uani 1 1 d . . . H3A H -0.3547 0.2704 0.2352 0.071 Uiso 1 1 calc R . . C4 C -0.3469(3) 0.1766(3) 0.0825(3) 0.0681(10) Uani 1 1 d . . . H4A H -0.4205 0.1244 0.0629 0.082 Uiso 1 1 calc R . . C5 C -0.2792(3) 0.1644(3) 0.0067(2) 0.0514(7) Uani 1 1 d . . . C6 C -0.1737(3) 0.2472(3) 0.0384(3) 0.0558(8) Uani 1 1 d . . . C7 C -0.1336(3) 0.3367(3) 0.1407(3) 0.0495(7) Uani 1 1 d . . . H7A H -0.0631 0.3921 0.1579 0.059 Uiso 1 1 calc R . . C8 C -0.3235(3) 0.0677(3) -0.1039(3) 0.0533(8) Uani 1 1 d . . . C9 C -0.3331(3) -0.0529(3) -0.1003(3) 0.0602(8) Uani 1 1 d . . . C10 C -0.3811(3) -0.1430(3) -0.2024(3) 0.0536(8) Uani 1 1 d . . . H10A H -0.3884 -0.2232 -0.1984 0.064 Uiso 1 1 calc R . . C11 C -0.4181(3) -0.1140(2) -0.3104(2) 0.0444(6) Uani 1 1 d . . . C12 C -0.4693(3) -0.2085(3) -0.4231(3) 0.0497(7) Uani 1 1 d . . . C13 C -0.4084(3) 0.0058(3) -0.3148(3) 0.0577(8) Uani 1 1 d . . . H13A H -0.4333 0.0261 -0.3872 0.069 Uiso 1 1 calc R . . C14 C -0.3618(4) 0.0955(3) -0.2123(3) 0.0628(9) Uani 1 1 d . . . H14A H -0.3563 0.1757 -0.2165 0.075 Uiso 1 1 calc R . . C15 C 0.2786(3) 0.5080(2) 0.2927(2) 0.0364(6) Uani 1 1 d . A . C16 C 0.3467(3) 0.5068(2) 0.2079(2) 0.0406(6) Uani 1 1 d . . . C17 C 0.2968(7) 0.4284(6) 0.0938(6) 0.0430(15) Uani 0.50 1 d P A 1 H17A H 0.2204 0.3797 0.0720 0.052 Uiso 0.50 1 calc PR A 1 C17' C 0.2771(7) 0.4912(7) 0.0946(6) 0.0484(16) Uani 0.50 1 d P A 2 H17B H 0.1889 0.4822 0.0702 0.058 Uiso 0.50 1 calc PR A 2 C18 C 0.3591(7) 0.4228(7) 0.0147(6) 0.0487(17) Uani 0.50 1 d P A 1 C18' C 0.3365(7) 0.4884(8) 0.0131(6) 0.0554(18) Uani 0.50 1 d P A 2 H18A H 0.2863 0.4774 -0.0657 0.066 Uiso 0.50 1 calc PR A 2 C19 C 0.4682(3) 0.5014(3) 0.0440(3) 0.0504(7) Uani 1 1 d . . . C20 C 0.5119(7) 0.5821(8) 0.1445(7) 0.0606(19) Uani 0.50 1 d P A 1 C20' C 0.5378(6) 0.5184(7) 0.1709(6) 0.0465(15) Uani 0.50 1 d P A 2 H20B H 0.6261 0.5277 0.1982 0.056 Uiso 0.50 1 calc PR A 2 C21 C 0.4569(7) 0.5826(7) 0.2291(6) 0.0535(18) Uani 0.50 1 d P A 1 H21A H 0.4947 0.6351 0.3026 0.064 Uiso 0.50 1 calc PR A 1 C21' C 0.4766(7) 0.5212(7) 0.2515(6) 0.0474(16) Uani 0.50 1 d P A 2 H21B H 0.5219 0.5324 0.3315 0.057 Uiso 0.50 1 calc PR A 2 C22 C 0.0657(3) 0.7385(2) 0.3246(3) 0.0505(7) Uani 1 1 d . . . H22A H 0.0153 0.6796 0.2592 0.061 Uiso 1 1 calc R . . C23 C 0.0612(3) 0.8576(2) 0.3189(3) 0.0512(7) Uani 1 1 d . . . H23A H 0.0086 0.8773 0.2511 0.061 Uiso 1 1 calc R . . C24 C 0.1352(3) 0.9474(2) 0.4142(3) 0.0407(6) Uani 1 1 d . . . C25 C 0.2107(3) 0.9106(2) 0.5102(3) 0.0578(8) Uani 1 1 d . . . H25A H 0.2626 0.9673 0.5767 0.069 Uiso 1 1 calc R . . C26 C 0.2100(3) 0.7904(2) 0.5082(3) 0.0557(8) Uani 1 1 d . . . H26A H 0.2632 0.7683 0.5743 0.067 Uiso 1 1 calc R . . C27 C 0.1357(3) 1.0775(2) 0.4140(3) 0.0404(6) Uani 1 1 d . . . C28 C 0.1158(3) 1.1175(2) 0.3131(3) 0.0515(7) Uani 1 1 d . . . H28A H 0.0976 1.0624 0.2413 0.062 Uiso 1 1 calc R . . C29 C 0.1230(3) 1.2400(2) 0.3188(3) 0.0482(7) Uani 1 1 d . . . H29A H 0.1100 1.2649 0.2495 0.058 Uiso 1 1 calc R . . C30 C 0.1658(4) 1.2848(2) 0.5147(3) 0.0613(9) Uani 1 1 d . . . H30A H 0.1829 1.3415 0.5852 0.074 Uiso 1 1 calc R . . C31 C 0.1609(4) 1.1646(2) 0.5167(3) 0.0613(9) Uani 1 1 d . . . H31A H 0.1746 1.1422 0.5873 0.074 Uiso 1 1 calc R . . N1 N -0.0853(4) 0.2299(5) -0.0235(3) 0.0648(13) Uani 0.640(4) 1 d P . . N1' N -0.2689(13) -0.0840(9) 0.0012(9) 0.098(4) Uani 0.360(4) 1 d PD . . N3 N 0.1377(2) 0.70348(17) 0.4176(2) 0.0389(5) Uani 1 1 d . . . N4 N 0.1475(2) 1.32404(17) 0.4178(2) 0.0391(5) Uani 1 1 d . . . O1 O -0.04670(18) 0.49669(15) 0.36146(16) 0.0421(4) Uani 1 1 d . . . O2 O -0.21198(18) 0.43240(15) 0.40158(15) 0.0400(4) Uani 1 1 d . . . O3 O -0.0458(5) 0.3173(5) -0.0452(4) 0.117(2) Uani 0.640(4) 1 d P . . O3' O -0.3228(14) -0.1567(13) 0.0292(10) 0.175(6) Uani 0.360(4) 1 d PD . . O4 O -0.0549(5) 0.1295(5) -0.0524(4) 0.1028(17) Uani 0.640(4) 1 d P . . O4' O -0.1652(12) -0.0380(12) 0.0693(12) 0.196(8) Uani 0.360(4) 1 d PD . . O5 O -0.4854(3) -0.1881(2) -0.5175(2) 0.0800(8) Uani 1 1 d . . . O6 O -0.4964(2) -0.31475(19) -0.4071(2) 0.0611(6) Uani 1 1 d . . . H6 H -0.537(3) -0.358(3) -0.476(3) 0.073(11) Uiso 1 1 d . . . O7 O 0.16068(19) 0.47800(16) 0.25167(16) 0.0441(4) Uani 1 1 d . . . O8 O 0.33636(19) 0.53735(16) 0.40161(16) 0.0461(5) Uani 1 1 d . . . N2 N 0.3105(9) 0.3203(9) -0.0887(7) 0.061(3) Uani 0.319(5) 1 d PD . . O9 O 0.3802(17) 0.2488(16) -0.1081(14) 0.104(7) Uani 0.319(5) 1 d PD . . O10 O 0.2048(9) 0.3202(12) -0.1550(9) 0.133(6) Uani 0.319(5) 1 d PD . . O10' O 0.693(2) 0.706(3) 0.2444(17) 0.168(14) Uani 0.181(5) 1 d P . 1 N2' N 0.6002(16) 0.6952(19) 0.1646(17) 0.070(6) Uani 0.181(5) 1 d P . 1 O9' O 0.589(3) 0.763(2) 0.100(3) 0.098(10) Uani 0.181(5) 1 d P . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0446(2) 0.02234(16) 0.03684(19) 0.00432(12) 0.02279(15) 0.00232(13) C1 0.0422(15) 0.0266(11) 0.0369(13) 0.0082(10) 0.0165(11) 0.0066(10) C2 0.0411(15) 0.0387(13) 0.0370(14) 0.0017(11) 0.0165(12) 0.0010(11) C3 0.0558(19) 0.071(2) 0.0446(17) -0.0066(15) 0.0262(15) -0.0178(16) C4 0.065(2) 0.078(2) 0.0487(18) -0.0118(16) 0.0248(16) -0.0321(18) C5 0.0560(19) 0.0514(16) 0.0382(15) -0.0039(12) 0.0158(14) -0.0055(14) C6 0.0568(19) 0.0602(18) 0.0478(17) -0.0062(14) 0.0277(15) -0.0048(15) C7 0.0492(17) 0.0481(16) 0.0480(17) -0.0028(13) 0.0234(14) -0.0093(13) C8 0.0578(19) 0.0535(17) 0.0392(16) -0.0058(13) 0.0170(14) -0.0072(14) C9 0.070(2) 0.0579(19) 0.0405(17) 0.0035(14) 0.0100(15) -0.0034(16) C10 0.061(2) 0.0465(16) 0.0452(17) 0.0058(13) 0.0131(14) -0.0011(14) C11 0.0448(16) 0.0449(15) 0.0409(15) 0.0010(12) 0.0179(13) -0.0007(12) C12 0.0573(19) 0.0455(16) 0.0420(17) 0.0020(12) 0.0173(14) 0.0034(13) C13 0.081(2) 0.0482(17) 0.0368(15) 0.0029(13) 0.0170(15) -0.0048(15) C14 0.089(3) 0.0447(16) 0.0479(18) 0.0013(13) 0.0232(17) -0.0051(16) C15 0.0483(17) 0.0243(11) 0.0430(15) 0.0054(10) 0.0257(13) 0.0045(11) C16 0.0440(16) 0.0398(14) 0.0447(16) 0.0085(11) 0.0248(13) 0.0056(12) C17 0.045(4) 0.042(3) 0.042(3) 0.001(3) 0.023(3) -0.003(3) C17' 0.042(4) 0.064(5) 0.050(4) 0.017(4) 0.026(3) 0.012(4) C18 0.053(4) 0.059(4) 0.037(3) 0.006(3) 0.023(3) 0.002(4) C18' 0.053(4) 0.084(6) 0.037(3) 0.021(4) 0.021(3) 0.014(4) C19 0.0487(18) 0.0584(18) 0.0507(17) 0.0099(14) 0.0279(14) 0.0050(14) C20 0.058(5) 0.077(5) 0.048(4) -0.004(4) 0.035(4) -0.016(4) C20' 0.036(3) 0.064(4) 0.044(4) 0.014(3) 0.020(3) 0.007(3) C21 0.058(4) 0.062(5) 0.038(4) -0.008(3) 0.029(3) -0.017(4) C21' 0.057(4) 0.057(4) 0.037(3) 0.017(3) 0.025(3) 0.007(3) C22 0.070(2) 0.0287(13) 0.0477(17) 0.0053(12) 0.0178(15) -0.0010(13) C23 0.069(2) 0.0334(14) 0.0517(17) 0.0150(12) 0.0182(15) 0.0060(13) C24 0.0465(16) 0.0240(12) 0.0589(17) 0.0090(11) 0.0284(14) 0.0040(11) C25 0.066(2) 0.0265(13) 0.064(2) 0.0043(13) 0.0065(16) 0.0005(13) C26 0.064(2) 0.0284(13) 0.0601(19) 0.0103(13) 0.0037(16) 0.0020(13) C27 0.0453(16) 0.0258(12) 0.0592(17) 0.0123(11) 0.0284(13) 0.0075(11) C28 0.072(2) 0.0267(13) 0.0540(18) 0.0044(12) 0.0237(16) 0.0041(13) C29 0.070(2) 0.0289(13) 0.0496(16) 0.0113(12) 0.0253(15) 0.0059(13) C30 0.113(3) 0.0273(13) 0.0566(19) 0.0068(12) 0.0474(19) 0.0168(15) C31 0.113(3) 0.0324(14) 0.0591(19) 0.0184(13) 0.050(2) 0.0205(16) N1 0.063(3) 0.082(3) 0.039(2) -0.015(2) 0.027(2) -0.019(2) N1' 0.140(11) 0.065(6) 0.062(6) 0.008(5) 0.005(7) -0.004(6) N3 0.0461(13) 0.0236(10) 0.0502(13) 0.0077(9) 0.0221(11) 0.0032(9) N4 0.0537(14) 0.0238(10) 0.0494(13) 0.0109(9) 0.0289(11) 0.0076(9) O1 0.0448(11) 0.0330(9) 0.0463(11) 0.0016(8) 0.0188(9) -0.0016(8) O2 0.0500(11) 0.0347(9) 0.0377(10) 0.0036(7) 0.0218(9) 0.0007(8) O3 0.142(5) 0.126(4) 0.092(4) -0.019(3) 0.087(4) -0.044(4) O3' 0.237(17) 0.178(14) 0.093(8) 0.061(9) 0.020(9) 0.030(12) O4 0.101(4) 0.123(4) 0.090(3) -0.004(3) 0.057(3) 0.032(3) O4' 0.172(13) 0.163(12) 0.156(12) 0.059(9) -0.074(10) -0.006(10) O5 0.132(2) 0.0597(14) 0.0412(13) 0.0000(11) 0.0303(14) -0.0066(14) O6 0.0847(17) 0.0409(11) 0.0445(13) -0.0008(10) 0.0138(12) -0.0019(11) O7 0.0490(12) 0.0449(10) 0.0443(11) 0.0075(8) 0.0267(9) -0.0027(9) O8 0.0541(12) 0.0438(10) 0.0419(11) -0.0006(8) 0.0258(9) 0.0037(9) N2 0.061(6) 0.082(7) 0.039(5) -0.004(4) 0.029(4) -0.014(5) O9 0.150(16) 0.090(10) 0.056(7) -0.013(6) 0.033(8) 0.042(9) O10 0.060(6) 0.206(13) 0.078(7) -0.051(7) 0.008(5) -0.006(7) O10' 0.16(2) 0.24(3) 0.062(12) 0.020(14) 0.010(13) -0.12(2) N2' 0.054(10) 0.115(17) 0.035(9) 0.009(10) 0.016(8) -0.011(9) O9' 0.107(16) 0.048(10) 0.18(3) 0.051(13) 0.090(17) 0.008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.0165(19) . ? Co1 O2 2.0323(18) 2_566 ? Co1 O7 2.1163(18) . ? Co1 N4 2.1680(19) 1_545 ? Co1 N3 2.176(2) . ? Co1 O8 2.2568(19) . ? C1 O1 1.244(3) . ? C1 O2 1.262(3) . ? C1 C2 1.502(3) . ? C2 C3 1.380(4) . ? C2 C7 1.382(4) . ? C3 C4 1.378(4) . ? C3 H3A 0.9300 . ? C4 C5 1.389(4) . ? C4 H4A 0.9300 . ? C5 C6 1.379(4) . ? C5 C8 1.489(4) . ? C6 C7 1.378(4) . ? C6 N1 1.446(5) . ? C7 H7A 0.9300 . ? C8 C14 1.379(4) . ? C8 C9 1.389(4) . ? C9 N1' 1.354(11) . ? C9 C10 1.383(4) . ? C10 C11 1.380(4) . ? C10 H10A 0.9300 . ? C11 C13 1.384(4) . ? C11 C12 1.495(4) . ? C12 O5 1.201(4) . ? C12 O6 1.311(4) . ? C13 C14 1.381(4) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 O8 1.252(3) . ? C15 O7 1.255(3) . ? C15 C16 1.497(4) . ? C16 C17' 1.330(8) . ? C16 C21' 1.367(8) . ? C16 C21 1.399(7) . ? C16 C17 1.422(7) . ? C17 C18 1.381(10) . ? C17 H17A 0.9300 . ? C17' C18' 1.386(10) . ? C17' H17B 0.9300 . ? C18 C19 1.386(8) . ? C18 N2 1.473(11) . ? C18' C19 1.394(8) . ? C18' H18A 0.9300 . ? C19 C20 1.312(8) . ? C19 C20' 1.472(7) . ? C19 C19 1.492(6) 2_665 ? C20 C21 1.388(9) . ? C20 N2' 1.52(2) . ? C20' C21' 1.391(9) . ? C20' H20B 0.9300 . ? C21 H21A 0.9300 . ? C21' H21B 0.9300 . ? C22 N3 1.321(4) . ? C22 C23 1.380(4) . ? C22 H22A 0.9300 . ? C23 C24 1.382(4) . ? C23 H23A 0.9300 . ? C24 C25 1.371(4) . ? C24 C27 1.488(3) . ? C25 C26 1.368(4) . ? C25 H25A 0.9300 . ? C26 N3 1.329(3) . ? C26 H26A 0.9300 . ? C27 C28 1.374(4) . ? C27 C31 1.380(4) . ? C28 C29 1.386(4) . ? C28 H28A 0.9300 . ? C29 N4 1.330(3) . ? C29 H29A 0.9300 . ? C30 N4 1.327(4) . ? C30 C31 1.378(4) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? N1 O3 1.195(6) . ? N1 O4 1.227(6) . ? N1' O3' 1.184(12) . ? N1' O4' 1.207(12) . ? N4 Co1 2.1680(19) 1_565 ? O2 Co1 2.0323(18) 2_566 ? O6 H6 0.85(4) . ? N2 O10 1.198(10) . ? N2 O9 1.199(14) . ? N2 O9' 1.53(3) 2_665 ? N2 N2' 1.586(18) 2_665 ? N2 O10' 1.88(2) 2_665 ? O9 O9' 0.37(4) 2_665 ? O9 N2' 1.11(2) 2_665 ? O9 O10' 1.81(3) 2_665 ? O10 O10' 1.84(3) 2_665 ? O10' N2' 1.16(3) . ? O10' O9 1.81(3) 2_665 ? O10' O10 1.84(3) 2_665 ? O10' N2 1.88(2) 2_665 ? N2' O9 1.11(3) 2_665 ? N2' O9' 1.21(4) . ? N2' N2 1.586(18) 2_665 ? O9' O9 0.37(4) 2_665 ? O9' N2 1.53(3) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O2 108.90(7) . 2_566 ? O1 Co1 O7 95.96(8) . . ? O2 Co1 O7 154.75(8) 2_566 . ? O1 Co1 N4 91.95(8) . 1_545 ? O2 Co1 N4 93.97(8) 2_566 1_545 ? O7 Co1 N4 89.45(8) . 1_545 ? O1 Co1 N3 86.91(8) . . ? O2 Co1 N3 87.38(8) 2_566 . ? O7 Co1 N3 89.63(8) . . ? N4 Co1 N3 178.45(9) 1_545 . ? O1 Co1 O8 154.46(8) . . ? O2 Co1 O8 95.24(7) 2_566 . ? O7 Co1 O8 59.53(7) . . ? N4 Co1 O8 94.65(8) 1_545 . ? N3 Co1 O8 85.96(8) . . ? O1 C1 O2 124.6(2) . . ? O1 C1 C2 118.7(2) . . ? O2 C1 C2 116.7(2) . . ? C3 C2 C7 118.7(2) . . ? C3 C2 C1 121.3(2) . . ? C7 C2 C1 119.9(2) . . ? C4 C3 C2 120.8(3) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 121.4(3) . . ? C3 C4 H4A 119.3 . . ? C5 C4 H4A 119.3 . . ? C6 C5 C4 116.5(3) . . ? C6 C5 C8 123.4(3) . . ? C4 C5 C8 120.1(3) . . ? C7 C6 C5 123.0(3) . . ? C7 C6 N1 115.6(3) . . ? C5 C6 N1 120.3(3) . . ? C6 C7 C2 119.4(3) . . ? C6 C7 H7A 120.3 . . ? C2 C7 H7A 120.3 . . ? C14 C8 C9 118.3(3) . . ? C14 C8 C5 121.0(3) . . ? C9 C8 C5 120.6(3) . . ? N1' C9 C10 118.3(5) . . ? N1' C9 C8 118.9(5) . . ? C10 C9 C8 121.1(3) . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C11 C13 119.3(3) . . ? C10 C11 C12 121.8(3) . . ? C13 C11 C12 118.9(3) . . ? O5 C12 O6 124.2(3) . . ? O5 C12 C11 123.2(3) . . ? O6 C12 C11 112.6(3) . . ? C14 C13 C11 120.4(3) . . ? C14 C13 H13A 119.8 . . ? C11 C13 H13A 119.8 . . ? C8 C14 C13 121.0(3) . . ? C8 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? O8 C15 O7 120.3(2) . . ? O8 C15 C16 121.7(2) . . ? O7 C15 C16 118.0(2) . . ? C17' C16 C21' 124.0(5) . . ? C17' C16 C21 106.9(5) . . ? C21' C16 C21 34.4(3) . . ? C17' C16 C17 31.8(3) . . ? C21' C16 C17 112.1(4) . . ? C21 C16 C17 114.8(4) . . ? C17' C16 C15 117.9(4) . . ? C21' C16 C15 118.0(4) . . ? C21 C16 C15 125.0(3) . . ? C17 C16 C15 120.1(3) . . ? C18 C17 C16 121.5(6) . . ? C18 C17 H17A 119.2 . . ? C16 C17 H17A 119.2 . . ? C16 C17' C18' 119.7(6) . . ? C16 C17' H17B 120.1 . . ? C18' C17' H17B 120.1 . . ? C17 C18 C19 119.2(6) . . ? C17 C18 N2 114.7(6) . . ? C19 C18 N2 125.5(6) . . ? C17' C18' C19 122.9(6) . . ? C17' C18' H18A 118.5 . . ? C19 C18' H18A 118.5 . . ? C20 C19 C18 121.2(5) . . ? C20 C19 C18' 105.4(5) . . ? C18 C19 C18' 33.6(3) . . ? C20 C19 C20' 36.3(4) . . ? C18 C19 C20' 107.5(4) . . ? C18' C19 C20' 113.8(4) . . ? C20 C19 C19 119.7(4) . 2_665 ? C18 C19 C19 119.0(4) . 2_665 ? C18' C19 C19 122.8(4) . 2_665 ? C20' C19 C19 123.5(4) . 2_665 ? C19 C20 C21 120.3(6) . . ? C19 C20 N2' 122.9(9) . . ? C21 C20 N2' 115.2(9) . . ? C21' C20' C19 122.5(6) . . ? C21' C20' H20B 118.7 . . ? C19 C20' H20B 118.7 . . ? C20 C21 C16 122.4(6) . . ? C20 C21 H21A 118.8 . . ? C16 C21 H21A 118.8 . . ? C16 C21' C20' 117.0(6) . . ? C16 C21' H21B 121.5 . . ? C20' C21' H21B 121.5 . . ? N3 C22 C23 123.7(3) . . ? N3 C22 H22A 118.2 . . ? C23 C22 H22A 118.2 . . ? C22 C23 C24 119.7(3) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C25 C24 C23 116.4(2) . . ? C25 C24 C27 120.9(2) . . ? C23 C24 C27 122.6(3) . . ? C26 C25 C24 120.1(3) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? N3 C26 C25 123.9(3) . . ? N3 C26 H26A 118.0 . . ? C25 C26 H26A 118.0 . . ? C28 C27 C31 116.7(2) . . ? C28 C27 C24 122.1(2) . . ? C31 C27 C24 121.1(3) . . ? C27 C28 C29 119.7(3) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? N4 C29 C28 123.6(3) . . ? N4 C29 H29A 118.2 . . ? C28 C29 H29A 118.2 . . ? N4 C30 C31 123.7(3) . . ? N4 C30 H30A 118.1 . . ? C31 C30 H30A 118.1 . . ? C30 C31 C27 119.9(3) . . ? C30 C31 H31A 120.0 . . ? C27 C31 H31A 120.0 . . ? O3 N1 O4 122.8(5) . . ? O3 N1 C6 116.5(5) . . ? O4 N1 C6 120.6(5) . . ? O3' N1' O4' 117.2(12) . . ? O3' N1' C9 117.0(11) . . ? O4' N1' C9 125.5(11) . . ? C22 N3 C26 116.2(2) . . ? C22 N3 Co1 122.04(17) . . ? C26 N3 Co1 121.73(19) . . ? C30 N4 C29 116.3(2) . . ? C30 N4 Co1 121.46(17) . 1_565 ? C29 N4 Co1 122.12(18) . 1_565 ? C1 O1 Co1 147.93(17) . . ? C1 O2 Co1 126.34(17) . 2_566 ? C12 O6 H6 105(2) . . ? C15 O7 Co1 93.20(15) . . ? C15 O8 Co1 86.86(16) . . ? O10 N2 O9 123.6(10) . . ? O10 N2 C18 116.4(9) . . ? O9 N2 C18 119.6(10) . . ? O10 N2 O9' 130.2(16) . 2_665 ? O9 N2 O9' 6.7(19) . 2_665 ? C18 N2 O9' 113.0(15) . 2_665 ? O10 N2 N2' 107.1(10) . 2_665 ? O9 N2 N2' 44.3(12) . 2_665 ? C18 N2 N2' 112.6(9) . 2_665 ? O9' N2 N2' 45.7(15) 2_665 2_665 ? O10 N2 O10' 69.4(11) . 2_665 ? O9 N2 O10' 68.0(14) . 2_665 ? C18 N2 O10' 134.0(9) . 2_665 ? O9' N2 O10' 72.7(17) 2_665 2_665 ? N2' N2 O10' 37.8(10) 2_665 2_665 ? O9' O9 N2' 97(8) 2_665 2_665 ? O9' O9 N2 151(7) 2_665 . ? N2' O9 N2 86.6(17) 2_665 . ? O9' O9 O10' 124(8) 2_665 2_665 ? N2' O9 O10' 37.8(11) 2_665 2_665 ? N2 O9 O10' 74.1(14) . 2_665 ? N2 O10 O10' 73.0(9) . 2_665 ? N2' O10' O9 36.1(13) . 2_665 ? N2' O10' O10 94.6(15) . 2_665 ? O9 O10' O10 70.7(9) 2_665 2_665 ? N2' O10' N2 57.2(12) . 2_665 ? O9 O10' N2 37.9(6) 2_665 2_665 ? O10 O10' N2 37.6(6) 2_665 2_665 ? O9 N2' O10' 106(2) 2_665 . ? O9 N2' O9' 18(2) 2_665 . ? O10' N2' O9' 119(2) . . ? O9 N2' C20 135.6(18) 2_665 . ? O10' N2' C20 113(2) . . ? O9' N2' C20 127(2) . . ? O9 N2' N2 49.0(10) 2_665 2_665 ? O10' N2' N2 85.0(16) . 2_665 ? O9' N2' N2 64.9(17) . 2_665 ? C20 N2' N2 114.1(13) . 2_665 ? O9 O9' N2' 66(7) 2_665 . ? O9 O9' N2 22(6) 2_665 2_665 ? N2' O9' N2 69.5(19) . 2_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 176.9(3) . . . . ? O2 C1 C2 C3 -3.1(4) . . . . ? O1 C1 C2 C7 0.2(4) . . . . ? O2 C1 C2 C7 -179.8(3) . . . . ? C7 C2 C3 C4 3.0(5) . . . . ? C1 C2 C3 C4 -173.7(3) . . . . ? C2 C3 C4 C5 0.1(6) . . . . ? C3 C4 C5 C6 -2.3(6) . . . . ? C3 C4 C5 C8 179.3(3) . . . . ? C4 C5 C6 C7 1.5(5) . . . . ? C8 C5 C6 C7 179.8(3) . . . . ? C4 C5 C6 N1 169.4(4) . . . . ? C8 C5 C6 N1 -12.3(6) . . . . ? C5 C6 C7 C2 1.6(5) . . . . ? N1 C6 C7 C2 -166.8(4) . . . . ? C3 C2 C7 C6 -3.9(5) . . . . ? C1 C2 C7 C6 172.9(3) . . . . ? C6 C5 C8 C14 -62.3(5) . . . . ? C4 C5 C8 C14 116.0(4) . . . . ? C6 C5 C8 C9 121.0(4) . . . . ? C4 C5 C8 C9 -60.8(5) . . . . ? C14 C8 C9 N1' 164.1(8) . . . . ? C5 C8 C9 N1' -19.0(8) . . . . ? C14 C8 C9 C10 -0.6(5) . . . . ? C5 C8 C9 C10 176.2(3) . . . . ? N1' C9 C10 C11 -163.7(7) . . . . ? C8 C9 C10 C11 1.2(5) . . . . ? C9 C10 C11 C13 -0.9(5) . . . . ? C9 C10 C11 C12 179.5(3) . . . . ? C10 C11 C12 O5 -169.1(3) . . . . ? C13 C11 C12 O5 11.3(5) . . . . ? C10 C11 C12 O6 11.9(4) . . . . ? C13 C11 C12 O6 -167.7(3) . . . . ? C10 C11 C13 C14 0.2(5) . . . . ? C12 C11 C13 C14 179.8(3) . . . . ? C9 C8 C14 C13 -0.2(5) . . . . ? C5 C8 C14 C13 -177.0(3) . . . . ? C11 C13 C14 C8 0.4(6) . . . . ? O8 C15 C16 C17' -170.8(4) . . . . ? O7 C15 C16 C17' 9.6(5) . . . . ? O8 C15 C16 C21' 9.6(5) . . . . ? O7 C15 C16 C21' -170.1(4) . . . . ? O8 C15 C16 C21 -30.2(6) . . . . ? O7 C15 C16 C21 150.1(5) . . . . ? O8 C15 C16 C17 152.8(4) . . . . ? O7 C15 C16 C17 -26.8(5) . . . . ? C17' C16 C17 C18 86.5(11) . . . . ? C21' C16 C17 C18 -33.0(9) . . . . ? C21 C16 C17 C18 4.5(9) . . . . ? C15 C16 C17 C18 -178.2(6) . . . . ? C21' C16 C17' C18' 0.2(10) . . . . ? C21 C16 C17' C18' 33.6(9) . . . . ? C17 C16 C17' C18' -76.5(10) . . . . ? C15 C16 C17' C18' -179.4(6) . . . . ? C16 C17 C18 C19 -4.5(11) . . . . ? C16 C17 C18 N2 167.6(7) . . . . ? C16 C17' C18' C19 0.0(12) . . . . ? C17 C18 C19 C20 -1.2(11) . . . . ? N2 C18 C19 C20 -172.4(9) . . . . ? C17 C18 C19 C18' -70.7(9) . . . . ? N2 C18 C19 C18' 118.1(13) . . . . ? C17 C18 C19 C20' 36.0(9) . . . . ? N2 C18 C19 C20' -135.2(8) . . . . ? C17 C18 C19 C19 -177.3(6) . . . 2_665 ? N2 C18 C19 C19 11.5(11) . . . 2_665 ? C17' C18' C19 C20 -37.7(10) . . . . ? C17' C18' C19 C18 86.0(11) . . . . ? C17' C18' C19 C20' -0.1(10) . . . . ? C17' C18' C19 C19 -179.9(7) . . . 2_665 ? C18 C19 C20 C21 6.6(12) . . . . ? C18' C19 C20 C21 39.2(11) . . . . ? C20' C19 C20 C21 -70.1(10) . . . . ? C19 C19 C20 C21 -177.3(7) 2_665 . . . ? C18 C19 C20 N2' -158.4(11) . . . . ? C18' C19 C20 N2' -125.9(12) . . . . ? C20' C19 C20 N2' 124.8(15) . . . . ? C19 C19 C20 N2' 17.6(14) 2_665 . . . ? C20 C19 C20' C21' 83.8(9) . . . . ? C18 C19 C20' C21' -35.4(8) . . . . ? C18' C19 C20' C21' 0.0(9) . . . . ? C19 C19 C20' C21' 179.7(6) 2_665 . . . ? C19 C20 C21 C16 -6.5(14) . . . . ? N2' C20 C21 C16 159.6(11) . . . . ? C17' C16 C21 C20 -32.1(10) . . . . ? C21' C16 C21 C20 94.2(12) . . . . ? C17 C16 C21 C20 0.9(11) . . . . ? C15 C16 C21 C20 -176.2(7) . . . . ? C17' C16 C21' C20' -0.3(9) . . . . ? C21 C16 C21' C20' -68.8(8) . . . . ? C17 C16 C21' C20' 33.2(8) . . . . ? C15 C16 C21' C20' 179.3(5) . . . . ? C19 C20' C21' C16 0.2(10) . . . . ? N3 C22 C23 C24 0.2(5) . . . . ? C22 C23 C24 C25 0.5(4) . . . . ? C22 C23 C24 C27 179.6(3) . . . . ? C23 C24 C25 C26 -0.2(5) . . . . ? C27 C24 C25 C26 -179.2(3) . . . . ? C24 C25 C26 N3 -0.9(6) . . . . ? C25 C24 C27 C28 147.8(3) . . . . ? C23 C24 C27 C28 -31.3(4) . . . . ? C25 C24 C27 C31 -29.9(4) . . . . ? C23 C24 C27 C31 151.0(3) . . . . ? C31 C27 C28 C29 0.7(5) . . . . ? C24 C27 C28 C29 -177.1(3) . . . . ? C27 C28 C29 N4 -0.6(5) . . . . ? N4 C30 C31 C27 -0.1(6) . . . . ? C28 C27 C31 C30 -0.4(5) . . . . ? C24 C27 C31 C30 177.5(3) . . . . ? C7 C6 N1 O3 -52.7(6) . . . . ? C5 C6 N1 O3 138.5(5) . . . . ? C7 C6 N1 O4 127.9(5) . . . . ? C5 C6 N1 O4 -40.9(7) . . . . ? C10 C9 N1' O3' -56.6(16) . . . . ? C8 C9 N1' O3' 138.3(12) . . . . ? C10 C9 N1' O4' 129.0(14) . . . . ? C8 C9 N1' O4' -36.2(18) . . . . ? C23 C22 N3 C26 -1.1(5) . . . . ? C23 C22 N3 Co1 -178.4(2) . . . . ? C25 C26 N3 C22 1.5(5) . . . . ? C25 C26 N3 Co1 178.8(3) . . . . ? O1 Co1 N3 C22 -50.4(2) . . . . ? O2 Co1 N3 C22 -159.5(2) 2_566 . . . ? O7 Co1 N3 C22 45.6(2) . . . . ? N4 Co1 N3 C22 -8(3) 1_545 . . . ? O8 Co1 N3 C22 105.1(2) . . . . ? O1 Co1 N3 C26 132.5(2) . . . . ? O2 Co1 N3 C26 23.4(2) 2_566 . . . ? O7 Co1 N3 C26 -131.5(2) . . . . ? N4 Co1 N3 C26 175(3) 1_545 . . . ? O8 Co1 N3 C26 -72.0(2) . . . . ? C31 C30 N4 C29 0.2(5) . . . . ? C31 C30 N4 Co1 176.0(3) . . . 1_565 ? C28 C29 N4 C30 0.2(5) . . . . ? C28 C29 N4 Co1 -175.6(2) . . . 1_565 ? O2 C1 O1 Co1 99.5(3) . . . . ? C2 C1 O1 Co1 -80.5(4) . . . . ? O2 Co1 O1 C1 -88.7(3) 2_566 . . . ? O7 Co1 O1 C1 95.8(3) . . . . ? N4 Co1 O1 C1 6.2(3) 1_545 . . . ? N3 Co1 O1 C1 -174.9(3) . . . . ? O8 Co1 O1 C1 111.2(3) . . . . ? O1 C1 O2 Co1 -25.2(3) . . . 2_566 ? C2 C1 O2 Co1 154.73(17) . . . 2_566 ? O8 C15 O7 Co1 3.5(2) . . . . ? C16 C15 O7 Co1 -176.81(19) . . . . ? O1 Co1 O7 C15 170.42(14) . . . . ? O2 Co1 O7 C15 0.5(3) 2_566 . . . ? N4 Co1 O7 C15 -97.68(15) 1_545 . . . ? N3 Co1 O7 C15 83.57(15) . . . . ? O8 Co1 O7 C15 -1.96(13) . . . . ? O7 C15 O8 Co1 -3.3(2) . . . . ? C16 C15 O8 Co1 177.0(2) . . . . ? O1 Co1 O8 C15 -15.9(2) . . . . ? O2 Co1 O8 C15 -176.99(14) 2_566 . . . ? O7 Co1 O8 C15 1.96(13) . . . . ? N4 Co1 O8 C15 88.58(15) 1_545 . . . ? N3 Co1 O8 C15 -89.99(15) . . . . ? C17 C18 N2 O10 66.0(12) . . . . ? C19 C18 N2 O10 -122.5(11) . . . . ? C17 C18 N2 O9 -120.7(15) . . . . ? C19 C18 N2 O9 50.9(18) . . . . ? C17 C18 N2 O9' -120.0(13) . . . 2_665 ? C19 C18 N2 O9' 51.5(15) . . . 2_665 ? C17 C18 N2 N2' -169.8(11) . . . 2_665 ? C19 C18 N2 N2' 1.8(15) . . . 2_665 ? C17 C18 N2 O10' 152.2(16) . . . 2_665 ? C19 C18 N2 O10' -36(2) . . . 2_665 ? O10 N2 O9 O9' 178(16) . . . 2_665 ? C18 N2 O9 O9' 5(17) . . . 2_665 ? N2' N2 O9 O9' 98(17) 2_665 . . 2_665 ? O10' N2 O9 O9' 134(17) 2_665 . . 2_665 ? O10 N2 O9 N2' 80(2) . . . 2_665 ? C18 N2 O9 N2' -92.8(14) . . . 2_665 ? O9' N2 O9 N2' -98(17) 2_665 . . 2_665 ? O10' N2 O9 N2' 36.3(12) 2_665 . . 2_665 ? O10 N2 O9 O10' 43.7(17) . . . 2_665 ? C18 N2 O9 O10' -129.2(10) . . . 2_665 ? O9' N2 O9 O10' -134(17) 2_665 . . 2_665 ? N2' N2 O9 O10' -36.3(12) 2_665 . . 2_665 ? O9 N2 O10 O10' -43.2(19) . . . 2_665 ? C18 N2 O10 O10' 129.9(11) . . . 2_665 ? O9' N2 O10 O10' -42.9(18) 2_665 . . 2_665 ? N2' N2 O10 O10' 2.9(14) 2_665 . . 2_665 ? O10 O10' N2' O9 -48(2) 2_665 . . 2_665 ? N2 O10' N2' O9 -44.8(13) 2_665 . . 2_665 ? O9 O10' N2' O9' -13(2) 2_665 . . . ? O10 O10' N2' O9' -60(3) 2_665 . . . ? N2 O10' N2' O9' -57(2) 2_665 . . . ? O9 O10' N2' C20 159(3) 2_665 . . . ? O10 O10' N2' C20 111.4(14) 2_665 . . . ? N2 O10' N2' C20 114.1(18) 2_665 . . . ? O9 O10' N2' N2 44.8(13) 2_665 . . 2_665 ? O10 O10' N2' N2 -2.8(13) 2_665 . . 2_665 ? C19 C20 N2' O9 25(3) . . . 2_665 ? C21 C20 N2' O9 -140(2) . . . 2_665 ? C19 C20 N2' O10' -125(2) . . . . ? C21 C20 N2' O10' 69(2) . . . . ? C19 C20 N2' O9' 46(3) . . . . ? C21 C20 N2' O9' -120(3) . . . . ? C19 C20 N2' N2 -30(2) . . . 2_665 ? C21 C20 N2' N2 164.3(11) . . . 2_665 ? O10' N2' O9' O9 44(7) . . . 2_665 ? C20 N2' O9' O9 -126(6) . . . 2_665 ? N2 N2' O9' O9 -24(6) 2_665 . . 2_665 ? O9 N2' O9' N2 24(6) 2_665 . . 2_665 ? O10' N2' O9' N2 68(3) . . . 2_665 ? C20 N2' O9' N2 -102(2) . . . 2_665 ? 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 O6 H6 O8 0.85(4) 1.85(4) 2.665(3) 160(4) 1_444 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.310 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.051 data_2 _database_code_depnum_ccdc_archive 'CCDC 842833' #TrackingRef '- 842833.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H53 Co3 N9 O22' _chemical_formula_weight 1573.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.5771(11) _cell_length_b 18.2763(9) _cell_length_c 22.6883(11) _cell_angle_alpha 90.00 _cell_angle_beta 117.481(2) _cell_angle_gamma 90.00 _cell_volume 7937.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3220 _exptl_absorpt_coefficient_mu 0.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8455 _exptl_absorpt_correction_T_max 0.9338 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 48903 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.01 _reflns_number_total 7808 _reflns_number_gt 5062 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1161P)^2^+28.7920P] 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 7808 _refine_ls_number_parameters 501 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1207 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.2365 _refine_ls_wR_factor_gt 0.1961 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.89305(3) 1.01235(4) 0.43491(3) 0.0346(2) Uani 1 1 d . . . Co2 Co 0.7500 0.2500 0.5000 0.0371(3) Uani 1 2 d S . . N1 N 0.8867(4) 1.0178(4) 0.3373(3) 0.0484(13) Uani 0.675(6) 1 d PG . 1 C1 C 0.8591(5) 0.9575(3) 0.2960(3) 0.077(3) Uani 0.675(6) 1 d PG . 1 H1A H 0.8416 0.9182 0.3097 0.092 Uiso 0.675(6) 1 calc PR . 1 C2 C 0.8576(5) 0.9560(4) 0.2341(3) 0.080(3) Uani 0.675(6) 1 d PG . 1 H2A H 0.8392 0.9157 0.2065 0.095 Uiso 0.675(6) 1 calc PR . 1 C3 C 0.8838(4) 1.0148(4) 0.2135(3) 0.0550(17) Uani 0.675(6) 1 d PG . 1 C4 C 0.9113(5) 1.0751(4) 0.2548(4) 0.094(5) Uani 0.675(6) 1 d PG . 1 H4A H 0.9288 1.1144 0.2411 0.113 Uiso 0.675(6) 1 calc PR . 1 C5 C 0.9128(5) 1.0766(4) 0.3167(4) 0.090(5) Uani 0.675(6) 1 d PG . 1 H5A H 0.9312 1.1170 0.3443 0.108 Uiso 0.675(6) 1 calc PR . 1 N1' N 0.8960(9) 1.0186(9) 0.3411(6) 0.0484(13) Uani 0.325(6) 1 d PG . 2 C1' C 0.9246(10) 0.9597(8) 0.3233(7) 0.077(3) Uani 0.325(6) 1 d PG . 2 H1'A H 0.9452 0.9214 0.3530 0.092 Uiso 0.325(6) 1 calc PR . 2 C2' C 0.9222(10) 0.9580(8) 0.2611(7) 0.080(3) Uani 0.325(6) 1 d PG . 2 H2'A H 0.9413 0.9185 0.2491 0.095 Uiso 0.325(6) 1 calc PR . 2 C3' C 0.8914(9) 1.0151(10) 0.2167(6) 0.0550(17) Uani 0.325(6) 1 d PG . 2 C4' C 0.8628(9) 1.0741(9) 0.2345(8) 0.094(5) Uani 0.325(6) 1 d PG . 2 H4'A H 0.8422 1.1123 0.2048 0.113 Uiso 0.325(6) 1 calc PR . 2 C5' C 0.8652(9) 1.0758(8) 0.2967(9) 0.090(5) Uani 0.325(6) 1 d PG . 2 H5'A H 0.8461 1.1152 0.3087 0.108 Uiso 0.325(6) 1 calc PR . 2 N2 N 0.8913(6) 1.0011(9) 0.0270(5) 0.0452(14) Uani 0.675(6) 1 d PG . 1 C8 C 0.8867(6) 0.9375(8) 0.0584(5) 0.060(3) Uani 0.675(6) 1 d PG . 1 H8A H 0.8848 0.8922 0.0390 0.072 Uiso 0.675(6) 1 calc PR . 1 C7 C 0.8847(7) 0.9418(8) 0.1187(5) 0.064(3) Uani 0.675(6) 1 d PG . 1 H7A H 0.8816 0.8992 0.1397 0.076 Uiso 0.675(6) 1 calc PR . 1 C6 C 0.8874(8) 1.0095(10) 0.1476(6) 0.0550(17) Uani 0.675(6) 1 d PG . 1 C10 C 0.8921(7) 1.0731(8) 0.1162(8) 0.081(5) Uani 0.675(6) 1 d PG . 1 H10A H 0.8939 1.1184 0.1355 0.097 Uiso 0.675(6) 1 calc PR . 1 C9 C 0.8940(6) 1.0689(8) 0.0559(7) 0.072(4) Uani 0.675(6) 1 d PG . 1 H9A H 0.8972 1.1114 0.0349 0.087 Uiso 0.675(6) 1 calc PR . 1 N2' N 0.8896(13) 0.996(2) 0.0291(11) 0.0452(14) Uani 0.325(6) 1 d PG . 2 C8' C 0.9115(13) 0.9390(17) 0.0751(13) 0.060(3) Uani 0.325(6) 1 d PG . 2 H8'A H 0.9280 0.8957 0.0659 0.072 Uiso 0.325(6) 1 calc PR . 2 C7' C 0.9086(15) 0.9469(19) 0.1347(11) 0.064(3) Uani 0.325(6) 1 d PG . 2 H7'A H 0.9232 0.9089 0.1654 0.076 Uiso 0.325(6) 1 calc PR . 2 C6' C 0.8839(17) 1.012(2) 0.1484(13) 0.0550(17) Uani 0.325(6) 1 d PG . 2 C10' C 0.8620(15) 1.0684(18) 0.1024(18) 0.081(5) Uani 0.325(6) 1 d PG . 2 H10B H 0.8454 1.1117 0.1116 0.097 Uiso 0.325(6) 1 calc PR . 2 C9' C 0.8648(13) 1.0605(18) 0.0428(16) 0.072(4) Uani 0.325(6) 1 d PG . 2 H9'A H 0.8502 1.0985 0.0121 0.087 Uiso 0.325(6) 1 calc PR . 2 C11 C 0.9957(3) 0.8797(3) 0.4932(3) 0.0379(12) Uani 1 1 d . . . C12 C 0.9686(3) 0.8027(3) 0.4812(3) 0.0448(13) Uani 1 1 d . . . C13 C 1.0059(4) 0.7466(4) 0.5214(4) 0.074(2) Uani 1 1 d . . . H13C H 1.0501 0.7556 0.5562 0.089 Uiso 1 1 calc R . . C14 C 0.9786(5) 0.6755(4) 0.5111(5) 0.096(3) Uani 1 1 d . . . H14A H 1.0052 0.6378 0.5388 0.115 Uiso 1 1 calc R . . C15 C 0.9134(4) 0.6606(4) 0.4607(4) 0.074(2) Uani 1 1 d . . . C16 C 0.8775(5) 0.7180(4) 0.4195(4) 0.097(3) Uani 1 1 d D . . C17 C 0.9043(4) 0.7868(4) 0.4293(4) 0.084(2) Uani 1 1 d . . . H17A H 0.8786 0.8239 0.4002 0.101 Uiso 1 1 calc R . . C18 C 0.8787(5) 0.5859(5) 0.4506(6) 0.073(3) Uani 0.654(10) 1 d PG . 1 C19 C 0.8373(6) 0.5676(4) 0.4806(6) 0.088(4) Uani 0.654(10) 1 d PG . 1 H19A H 0.8252 0.6031 0.5027 0.105 Uiso 0.654(10) 1 calc PR . 1 C20 C 0.8140(5) 0.4961(4) 0.4774(5) 0.077(3) Uani 0.654(10) 1 d PG . 1 H20A H 0.7863 0.4838 0.4974 0.093 Uiso 0.654(10) 1 calc PR . 1 C21 C 0.8320(5) 0.4429(4) 0.4442(6) 0.0569(17) Uani 0.654(10) 1 d PG . 1 C22 C 0.8735(5) 0.4613(7) 0.4143(5) 0.061(3) Uani 0.654(10) 1 d PG . 1 H22A H 0.8856 0.4257 0.3921 0.073 Uiso 0.654(10) 1 calc PR . 1 C23 C 0.8968(6) 0.5328(7) 0.4175(6) 0.069(4) Uani 0.654(10) 1 d PGD . 1 C18' C 0.8971(12) 0.5798(11) 0.4561(12) 0.073(3) Uani 0.346(10) 1 d PG . 2 C19' C 0.8897(11) 0.5513(9) 0.5092(10) 0.088(4) Uani 0.346(10) 1 d PG . 2 H19B H 0.9037 0.5785 0.5479 0.105 Uiso 0.346(10) 1 calc PR . 2 C20' C 0.8613(10) 0.4819(8) 0.5046(9) 0.077(3) Uani 0.346(10) 1 d PG . 2 H20B H 0.8563 0.4628 0.5401 0.093 Uiso 0.346(10) 1 calc PR . 2 C21' C 0.8403(10) 0.4412(9) 0.4468(11) 0.0569(17) Uani 0.346(10) 1 d PG . 2 C22' C 0.8477(12) 0.4698(15) 0.3936(8) 0.061(3) Uani 0.346(10) 1 d PG . 2 H22B H 0.8337 0.4425 0.3549 0.073 Uiso 0.346(10) 1 calc PR . 2 C23' C 0.8762(13) 0.5391(16) 0.3983(10) 0.069(4) Uani 0.346(10) 1 d PG . 2 H23A H 0.8811 0.5582 0.3627 0.083 Uiso 0.346(10) 1 calc PR . 2 C24 C 0.8113(3) 0.3642(3) 0.4435(3) 0.0498(14) Uani 1 1 d . . . C25 C 0.6558(3) 0.2585(4) 0.3471(3) 0.0557(16) Uani 1 1 d . . . H25A H 0.6991 0.2640 0.3479 0.067 Uiso 1 1 calc R . . C26 C 0.5975(3) 0.2598(4) 0.2864(3) 0.0540(15) Uani 1 1 d . . . H26A H 0.6021 0.2662 0.2479 0.065 Uiso 1 1 calc R . . C27 C 0.5326(3) 0.2516(3) 0.2825(3) 0.0453(13) Uani 1 1 d . . . C28 C 0.5309(3) 0.2410(4) 0.3422(3) 0.0583(16) Uani 1 1 d . . . H28A H 0.4883 0.2338 0.3424 0.070 Uiso 1 1 calc R . . C29 C 0.5913(3) 0.2411(4) 0.4009(3) 0.0563(16) Uani 1 1 d . . . H29A H 0.5884 0.2348 0.4402 0.068 Uiso 1 1 calc R . . C30 C 0.7623(3) 1.0033(3) 0.3777(3) 0.0495(14) Uani 1 1 d . . . C31 C 0.6844(3) 0.9989(4) 0.3402(4) 0.0625(18) Uani 1 1 d . . . C32 C 0.6444(4) 1.0523(4) 0.3462(5) 0.099(3) Uani 1 1 d . . . H32A H 0.6650 1.0919 0.3743 0.119 Uiso 1 1 calc R . . C33 C 0.5715(4) 1.0476(5) 0.3095(6) 0.109(3) Uani 1 1 d . . . H33A H 0.5447 1.0852 0.3134 0.131 Uiso 1 1 calc R . . C34 C 0.5388(4) 0.9917(5) 0.2692(4) 0.081(2) Uani 1 1 d . . . C35 C 0.5798(4) 0.9372(6) 0.2655(5) 0.116(4) Uani 1 1 d D . . C36 C 0.6525(4) 0.9396(5) 0.3021(6) 0.118(4) Uani 1 1 d . . . H36A H 0.6792 0.9005 0.3004 0.141 Uiso 1 1 calc R . . O1 O 0.79138(19) 1.0640(2) 0.3961(2) 0.0530(10) Uani 1 1 d . . . O2 O 0.7971(2) 0.9455(2) 0.3883(2) 0.0564(10) Uani 1 1 d . . . O3 O 0.9575(2) 0.9274(2) 0.4535(2) 0.0503(9) Uani 1 1 d . . . O4 O 1.05472(19) 0.8905(2) 0.54104(18) 0.0452(9) Uani 1 1 d . . . O9 O 0.8226(3) 0.3199(2) 0.4078(3) 0.0730(14) Uani 1 1 d . . . O10 O 0.7827(2) 0.3491(2) 0.4792(2) 0.0543(10) Uani 1 1 d . . . O11 O 0.8048(2) 0.1960(2) 0.4575(2) 0.0484(10) Uani 1 1 d . . . H11A H 0.809(4) 0.229(4) 0.442(4) 0.073 Uiso 1 1 d . . . H11B H 0.799(4) 0.162(4) 0.440(4) 0.073 Uiso 1 1 d . . . N3 N 0.6549(2) 0.2499(2) 0.4044(2) 0.0445(11) Uani 1 1 d . . . N4 N 0.5603(16) 0.8655(16) 0.231(2) 0.116(7) Uani 0.50 1 d PD . . O5 O 0.563(3) 0.804(2) 0.251(2) 0.132(5) Uani 0.50 1 d PD . . O6 O 0.515(2) 0.8859(16) 0.1781(17) 0.136(17) Uani 0.50 1 d PD . . O7 O 0.9357(11) 0.5973(7) 0.3534(8) 0.120(5) Uani 0.626(7) 1 d PD . 1 N5 N 0.9332(16) 0.5426(9) 0.3771(15) 0.106(7) Uani 0.626(7) 1 d PD . 1 O8 O 0.9799(13) 0.4977(15) 0.3880(15) 0.165(9) Uani 0.626(7) 1 d PD . 1 N5' N 0.8167(14) 0.7099(17) 0.3529(10) 0.106(7) Uani 0.374(7) 1 d PD . . O7' O 0.7712(14) 0.6760(12) 0.3558(13) 0.120(5) Uani 0.374(7) 1 d PD . . O8' O 0.805(2) 0.736(4) 0.2997(16) 0.165(9) Uani 0.374(7) 1 d PD . . O12 O 0.7548(19) 0.8153(19) 0.2427(18) 0.151(11) Uiso 0.25 1 d P . . O12' O 0.6533(19) 0.776(2) 0.1999(19) 0.155(12) Uiso 0.25 1 d P . . O13C O 0.741(4) 0.690(4) 0.531(4) 0.29(3) Uiso 0.25 1 d P . . O13B O 0.773(4) 0.697(4) 0.579(4) 0.26(3) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0419(4) 0.0339(4) 0.0298(4) -0.0026(3) 0.0180(3) -0.0040(3) Co2 0.0365(5) 0.0285(5) 0.0393(5) 0.0012(4) 0.0116(4) -0.0021(4) N1 0.073(4) 0.042(3) 0.036(3) -0.006(2) 0.030(3) -0.006(3) C1 0.136(10) 0.058(5) 0.060(6) -0.011(5) 0.064(7) -0.016(7) C2 0.138(10) 0.060(6) 0.062(6) -0.021(5) 0.065(7) -0.025(7) C3 0.085(5) 0.050(4) 0.043(3) 0.000(3) 0.041(3) 0.001(3) C4 0.169(15) 0.076(6) 0.058(7) -0.023(5) 0.069(9) -0.055(9) C5 0.154(14) 0.075(6) 0.066(7) -0.025(5) 0.072(10) -0.050(9) N1' 0.073(4) 0.042(3) 0.036(3) -0.006(2) 0.030(3) -0.006(3) C1' 0.136(10) 0.058(5) 0.060(6) -0.011(5) 0.064(7) -0.016(7) C2' 0.138(10) 0.060(6) 0.062(6) -0.021(5) 0.065(7) -0.025(7) C3' 0.085(5) 0.050(4) 0.043(3) 0.000(3) 0.041(3) 0.001(3) C4' 0.169(15) 0.076(6) 0.058(7) -0.023(5) 0.069(9) -0.055(9) C5' 0.154(14) 0.075(6) 0.066(7) -0.025(5) 0.072(10) -0.050(9) N2 0.062(3) 0.045(4) 0.034(2) -0.001(2) 0.027(2) 0.004(2) C8 0.083(10) 0.062(5) 0.033(7) -0.010(5) 0.026(7) -0.010(7) C7 0.095(12) 0.054(5) 0.037(6) -0.007(5) 0.026(7) -0.013(7) C6 0.080(5) 0.054(4) 0.039(3) -0.006(3) 0.035(3) -0.003(3) C10 0.144(16) 0.057(5) 0.071(9) -0.013(5) 0.073(11) -0.008(9) C9 0.113(13) 0.058(6) 0.069(8) 0.003(6) 0.062(9) -0.002(8) N2' 0.062(3) 0.045(4) 0.034(2) -0.001(2) 0.027(2) 0.004(2) C8' 0.083(10) 0.062(5) 0.033(7) -0.010(5) 0.026(7) -0.010(7) C7' 0.095(12) 0.054(5) 0.037(6) -0.007(5) 0.026(7) -0.013(7) C6' 0.080(5) 0.054(4) 0.039(3) -0.006(3) 0.035(3) -0.003(3) C10' 0.144(16) 0.057(5) 0.071(9) -0.013(5) 0.073(11) -0.008(9) C9' 0.113(13) 0.058(6) 0.069(8) 0.003(6) 0.062(9) -0.002(8) C11 0.050(3) 0.029(3) 0.044(3) -0.003(2) 0.030(3) -0.005(2) C12 0.057(3) 0.029(3) 0.051(3) -0.001(2) 0.027(3) -0.008(2) C13 0.065(4) 0.037(4) 0.101(6) 0.005(4) 0.022(4) -0.010(3) C14 0.098(6) 0.036(4) 0.132(8) 0.028(4) 0.036(6) 0.000(4) C15 0.102(6) 0.042(4) 0.075(5) -0.005(3) 0.037(4) -0.030(4) C16 0.116(7) 0.048(5) 0.077(5) -0.009(4) 0.003(5) -0.037(5) C17 0.091(5) 0.045(4) 0.076(5) 0.013(4) 0.003(4) -0.022(4) C18 0.090(9) 0.036(4) 0.091(6) 0.000(4) 0.041(6) -0.018(5) C19 0.109(10) 0.049(6) 0.134(12) -0.017(6) 0.081(10) -0.023(7) C20 0.085(8) 0.055(6) 0.111(10) -0.007(6) 0.062(9) -0.025(6) C21 0.069(5) 0.034(3) 0.062(4) -0.001(3) 0.025(4) -0.015(3) C22 0.068(10) 0.038(5) 0.078(8) -0.004(6) 0.035(8) -0.011(6) C23 0.093(10) 0.046(5) 0.068(9) -0.005(6) 0.038(8) -0.026(6) C18' 0.090(9) 0.036(4) 0.091(6) 0.000(4) 0.041(6) -0.018(5) C19' 0.109(10) 0.049(6) 0.134(12) -0.017(6) 0.081(10) -0.023(7) C20' 0.085(8) 0.055(6) 0.111(10) -0.007(6) 0.062(9) -0.025(6) C21' 0.069(5) 0.034(3) 0.062(4) -0.001(3) 0.025(4) -0.015(3) C22' 0.068(10) 0.038(5) 0.078(8) -0.004(6) 0.035(8) -0.011(6) C23' 0.093(10) 0.046(5) 0.068(9) -0.005(6) 0.038(8) -0.026(6) C24 0.052(3) 0.033(3) 0.058(3) 0.004(3) 0.020(3) -0.005(3) C25 0.035(3) 0.078(5) 0.047(3) 0.003(3) 0.013(2) -0.002(3) C26 0.044(3) 0.075(4) 0.039(3) 0.002(3) 0.015(2) -0.003(3) C27 0.040(3) 0.045(3) 0.044(3) -0.004(2) 0.013(2) -0.003(2) C28 0.040(3) 0.084(5) 0.047(3) 0.002(3) 0.017(3) -0.002(3) C29 0.043(3) 0.078(5) 0.039(3) 0.004(3) 0.012(3) -0.005(3) C30 0.038(3) 0.052(4) 0.053(3) -0.007(3) 0.017(3) -0.003(3) C31 0.038(3) 0.058(4) 0.079(5) -0.015(3) 0.016(3) -0.003(3) C32 0.051(4) 0.060(5) 0.162(9) -0.030(5) 0.029(5) -0.007(4) C33 0.063(5) 0.071(6) 0.175(10) -0.026(6) 0.040(6) 0.006(4) C34 0.044(4) 0.084(6) 0.096(6) -0.006(5) 0.017(4) -0.007(4) C35 0.048(4) 0.108(7) 0.146(9) -0.057(7) 0.005(5) -0.010(5) C36 0.049(4) 0.095(7) 0.170(10) -0.057(7) 0.018(5) -0.010(4) O1 0.045(2) 0.047(2) 0.059(2) -0.0141(19) 0.0170(19) -0.0046(19) O2 0.045(2) 0.047(3) 0.071(3) -0.009(2) 0.021(2) -0.0056(19) O3 0.054(2) 0.034(2) 0.059(2) 0.0020(18) 0.023(2) 0.0007(18) O4 0.050(2) 0.038(2) 0.043(2) -0.0034(16) 0.0178(19) -0.0097(17) O9 0.096(4) 0.039(3) 0.104(4) -0.008(2) 0.063(3) -0.020(2) O10 0.070(3) 0.035(2) 0.059(2) 0.0022(18) 0.031(2) -0.0083(19) O11 0.059(2) 0.029(2) 0.056(3) -0.0024(18) 0.026(2) 0.000(2) N3 0.041(2) 0.045(3) 0.040(2) 0.000(2) 0.011(2) -0.003(2) N4 0.19(2) 0.055(10) 0.167(18) -0.032(11) 0.135(18) -0.069(12) O5 0.225(17) 0.070(8) 0.146(12) 0.000(8) 0.123(13) -0.017(9) O6 0.10(3) 0.17(4) 0.10(2) -0.11(3) 0.01(2) 0.00(2) O7 0.208(17) 0.062(8) 0.135(12) -0.001(8) 0.117(13) -0.019(9) N5 0.165(19) 0.051(10) 0.152(17) -0.026(11) 0.116(17) -0.061(11) O8 0.16(2) 0.18(2) 0.19(2) 0.004(18) 0.102(19) -0.050(17) N5' 0.165(19) 0.051(10) 0.152(17) -0.026(11) 0.116(17) -0.061(11) O7' 0.208(17) 0.062(8) 0.135(12) -0.001(8) 0.117(13) -0.019(9) O8' 0.16(2) 0.18(2) 0.19(2) 0.004(18) 0.102(19) -0.050(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 1.995(4) . ? Co1 O4 2.037(4) 5_776 ? Co1 N2 2.121(11) 6_576 ? Co1 N1 2.157(5) . ? Co1 N1' 2.161(11) . ? Co1 O1 2.167(4) . ? Co1 N2' 2.18(2) 6_576 ? Co1 O2 2.207(4) . ? Co1 C30 2.508(6) . ? Co2 O10 2.077(4) 7_656 ? Co2 O10 2.077(4) . ? Co2 O11 2.087(4) 7_656 ? Co2 O11 2.087(4) . ? Co2 N3 2.193(4) 7_656 ? Co2 N3 2.193(4) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C1 H1A 0.9300 . ? C2 C3 1.3900 . ? C2 H2A 0.9300 . ? C3 C4 1.3900 . ? C3 C6 1.537(12) . ? C4 C5 1.3900 . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? N1' C1' 1.3900 . ? N1' C5' 1.3900 . ? C1' C2' 1.3900 . ? C1' H1'A 0.9300 . ? C2' C3' 1.3900 . ? C2' H2'A 0.9300 . ? C3' C4' 1.3900 . ? C3' C6' 1.48(3) . ? C4' C5' 1.3900 . ? C4' H4'A 0.9300 . ? C5' H5'A 0.9300 . ? N2 C8 1.3900 . ? N2 C9 1.3900 . ? N2 Co1 2.121(11) 6_575 ? C8 C7 1.3900 . ? C8 H8A 0.9300 . ? C7 C6 1.3900 . ? C7 H7A 0.9300 . ? C6 C10 1.3900 . ? C10 C9 1.3900 . ? C10 H10A 0.9300 . ? C9 H9A 0.9300 . ? N2' C8' 1.3900 . ? N2' C9' 1.3900 . ? N2' Co1 2.18(2) 6_575 ? C8' C7' 1.3900 . ? C8' H8'A 0.9300 . ? C7' C6' 1.3900 . ? C7' H7'A 0.9300 . ? C6' C10' 1.3900 . ? C10' C9' 1.3900 . ? C10' H10B 0.9300 . ? C9' H9'A 0.9300 . ? C11 O4 1.251(6) . ? C11 O3 1.252(6) . ? C11 C12 1.499(7) . ? C12 C13 1.363(9) . ? C12 C17 1.374(9) . ? C13 C14 1.400(10) . ? C13 H13C 0.9300 . ? C14 C15 1.370(11) . ? C14 H14A 0.9300 . ? C15 C16 1.380(11) . ? C15 C18' 1.510(19) . ? C15 C18 1.523(10) . ? C16 C17 1.358(10) . ? C16 N5' 1.482(18) . ? C17 H17A 0.9300 . ? C18 C19 1.3900 . ? C18 C23 1.3900 . ? C19 C20 1.3900 . ? C19 H19A 0.9300 . ? C20 C21 1.3900 . ? C20 H20A 0.9300 . ? C21 C22 1.3900 . ? C21 C24 1.504(10) . ? C22 C23 1.3900 . ? C22 H22A 0.9300 . ? C23 N5 1.469(14) . ? C18' C19' 1.3900 . ? C18' C23' 1.3900 . ? C19' C20' 1.3900 . ? C19' H19B 0.9300 . ? C20' C21' 1.3900 . ? C20' H20B 0.9300 . ? C21' C22' 1.3900 . ? C21' C24 1.527(18) . ? C22' C23' 1.3900 . ? C22' H22B 0.9300 . ? C23' H23A 0.9300 . ? C24 O9 1.246(7) . ? C24 O10 1.256(7) . ? C25 N3 1.318(7) . ? C25 C26 1.372(8) . ? C25 H25A 0.9300 . ? C26 C27 1.371(8) . ? C26 H26A 0.9300 . ? C27 C28 1.387(8) . ? C27 C27 1.495(10) 2_655 ? C28 C29 1.368(8) . ? C28 H28A 0.9300 . ? C29 N3 1.347(7) . ? C29 H29A 0.9300 . ? C30 O1 1.248(7) . ? C30 O2 1.252(7) . ? C30 C31 1.496(8) . ? C31 C32 1.350(10) . ? C31 C36 1.358(10) . ? C32 C33 1.402(11) . ? C32 H32A 0.9300 . ? C33 C34 1.335(11) . ? C33 H33A 0.9300 . ? C34 C35 1.359(11) . ? C34 C34 1.488(14) 2_655 ? C35 C36 1.396(10) . ? C35 N4 1.488(19) . ? C36 H36A 0.9300 . ? O4 Co1 2.037(4) 5_776 ? O11 H11A 0.73(8) . ? O11 H11B 0.73(7) . ? N4 O5 1.199(19) . ? N4 O6 1.203(18) . ? O7 N5 1.147(15) . ? N5 O8 1.233(19) . ? N5' O7' 1.187(17) . ? N5' O8' 1.214(18) . ? O13C O13B 0.99(9) . ? 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 O3 Co1 O4 112.11(16) . 5_776 ? O3 Co1 N2 91.7(4) . 6_576 ? O4 Co1 N2 95.5(5) 5_776 6_576 ? O3 Co1 N1 87.8(3) . . ? O4 Co1 N1 90.0(2) 5_776 . ? N2 Co1 N1 174.3(4) 6_576 . ? O3 Co1 N1' 85.1(5) . . ? O4 Co1 N1' 87.4(4) 5_776 . ? N2 Co1 N1' 176.3(6) 6_576 . ? N1 Co1 N1' 4.8(6) . . ? O3 Co1 O1 154.25(15) . . ? O4 Co1 O1 93.48(15) 5_776 . ? N2 Co1 O1 88.6(3) 6_576 . ? N1 Co1 O1 89.4(3) . . ? N1' Co1 O1 93.5(5) . . ? O3 Co1 N2' 94.3(9) . 6_576 ? O4 Co1 N2' 93.6(10) 5_776 6_576 ? N2 Co1 N2' 2.9(14) 6_576 6_576 ? N1 Co1 N2' 174.9(7) . 6_576 ? N1' Co1 N2' 179.1(11) . 6_576 ? O1 Co1 N2' 86.7(7) . 6_576 ? O3 Co1 O2 94.49(16) . . ? O4 Co1 O2 152.97(16) 5_776 . ? N2 Co1 O2 88.2(4) 6_576 . ? N1 Co1 O2 86.1(2) . . ? N1' Co1 O2 90.3(4) . . ? O1 Co1 O2 59.78(15) . . ? N2' Co1 O2 89.0(8) 6_576 . ? O3 Co1 C30 124.41(18) . . ? O4 Co1 C30 123.19(18) 5_776 . ? N2 Co1 C30 88.6(3) 6_576 . ? N1 Co1 C30 87.0(2) . . ? N1' Co1 C30 91.8(5) . . ? O1 Co1 C30 29.84(17) . . ? N2' Co1 C30 87.9(7) 6_576 . ? O2 Co1 C30 29.94(17) . . ? O10 Co2 O10 180.00(10) 7_656 . ? O10 Co2 O11 89.02(16) 7_656 7_656 ? O10 Co2 O11 90.98(16) . 7_656 ? O10 Co2 O11 90.98(16) 7_656 . ? O10 Co2 O11 89.02(16) . . ? O11 Co2 O11 180.00(19) 7_656 . ? O10 Co2 N3 92.09(16) 7_656 7_656 ? O10 Co2 N3 87.91(16) . 7_656 ? O11 Co2 N3 90.77(17) 7_656 7_656 ? O11 Co2 N3 89.23(17) . 7_656 ? O10 Co2 N3 87.91(16) 7_656 . ? O10 Co2 N3 92.09(16) . . ? O11 Co2 N3 89.23(17) 7_656 . ? O11 Co2 N3 90.77(17) . . ? N3 Co2 N3 180.000(1) 7_656 . ? C1 N1 C5 120.0 . . ? C1 N1 Co1 117.4(4) . . ? C5 N1 Co1 122.5(4) . . ? N1 C1 C2 120.0 . . ? N1 C1 H1A 120.0 . . ? C2 C1 H1A 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 C6 120.5(7) . . ? C2 C3 C6 119.3(7) . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 H5A 120.0 . . ? N1 C5 H5A 120.0 . . ? C1' N1' C5' 120.0 . . ? C1' N1' Co1 117.7(9) . . ? C5' N1' Co1 122.1(9) . . ? N1' C1' C2' 120.0 . . ? N1' C1' H1'A 120.0 . . ? C2' C1' H1'A 120.0 . . ? C3' C2' C1' 120.0 . . ? C3' C2' H2'A 120.0 . . ? C1' C2' H2'A 120.0 . . ? C2' C3' C4' 120.0 . . ? C2' C3' C6' 121(2) . . ? C4' C3' C6' 119(2) . . ? C5' C4' C3' 120.0 . . ? C5' C4' H4'A 120.0 . . ? C3' C4' H4'A 120.0 . . ? C4' C5' N1' 120.0 . . ? C4' C5' H5'A 120.0 . . ? N1' C5' H5'A 120.0 . . ? C8 N2 C9 120.0 . . ? C8 N2 Co1 116.5(8) . 6_575 ? C9 N2 Co1 123.5(8) . 6_575 ? N2 C8 C7 120.0 . . ? N2 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C10 C6 C7 120.0 . . ? C10 C6 C3 119.6(10) . . ? C7 C6 C3 120.4(10) . . ? C6 C10 C9 120.0 . . ? C6 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C10 C9 N2 120.0 . . ? C10 C9 H9A 120.0 . . ? N2 C9 H9A 120.0 . . ? C8' N2' C9' 120.0 . . ? C8' N2' Co1 122.1(18) . 6_575 ? C9' N2' Co1 117.9(18) . 6_575 ? C7' C8' N2' 120.0 . . ? C7' C8' H8'A 120.0 . . ? N2' C8' H8'A 120.0 . . ? C8' C7' C6' 120.0 . . ? C8' C7' H7'A 120.0 . . ? C6' C7' H7'A 120.0 . . ? C10' C6' C7' 120.0 . . ? C10' C6' C3' 126(3) . . ? C7' C6' C3' 114(3) . . ? C9' C10' C6' 120.0 . . ? C9' C10' H10B 120.0 . . ? C6' C10' H10B 120.0 . . ? C10' C9' N2' 120.0 . . ? C10' C9' H9'A 120.0 . . ? N2' C9' H9'A 120.0 . . ? O4 C11 O3 125.7(5) . . ? O4 C11 C12 117.6(5) . . ? O3 C11 C12 116.8(5) . . ? C13 C12 C17 117.7(6) . . ? C13 C12 C11 121.6(6) . . ? C17 C12 C11 120.6(5) . . ? C12 C13 C14 120.9(7) . . ? C12 C13 H13C 119.5 . . ? C14 C13 H13C 119.5 . . ? C15 C14 C13 120.9(7) . . ? C15 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? C14 C15 C16 116.9(6) . . ? C14 C15 C18' 111.6(11) . . ? C16 C15 C18' 131.0(12) . . ? C14 C15 C18 123.2(8) . . ? C16 C15 C18 119.8(8) . . ? C18' C15 C18 14.2(12) . . ? C17 C16 C15 122.0(7) . . ? C17 C16 N5' 111.7(12) . . ? C15 C16 N5' 124.7(13) . . ? C16 C17 C12 121.4(7) . . ? C16 C17 H17A 119.3 . . ? C12 C17 H17A 119.3 . . ? C19 C18 C23 120.0 . . ? C19 C18 C15 121.7(8) . . ? C23 C18 C15 117.8(8) . . ? C18 C19 C20 120.0 . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C22 C21 C20 120.0 . . ? C22 C21 C24 118.7(7) . . ? C20 C21 C24 121.2(7) . . ? C21 C22 C23 120.0 . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C18 120.0 . . ? C22 C23 N5 111.6(11) . . ? C18 C23 N5 128.1(11) . . ? C19' C18' C23' 120.0 . . ? C19' C18' C15 115.1(15) . . ? C23' C18' C15 123.6(15) . . ? C18' C19' C20' 120.0 . . ? C18' C19' H19B 120.0 . . ? C20' C19' H19B 120.0 . . ? C21' C20' C19' 120.0 . . ? C21' C20' H20B 120.0 . . ? C19' C20' H20B 120.0 . . ? C22' C21' C20' 120.0 . . ? C22' C21' C24 120.8(15) . . ? C20' C21' C24 119.2(14) . . ? C23' C22' C21' 120.0 . . ? C23' C22' H22B 120.0 . . ? C21' C22' H22B 120.0 . . ? C22' C23' C18' 120.0 . . ? C22' C23' H23A 120.0 . . ? C18' C23' H23A 120.0 . . ? O9 C24 O10 125.3(5) . . ? O9 C24 C21 118.9(6) . . ? O10 C24 C21 115.8(7) . . ? O9 C24 C21' 115.6(10) . . ? O10 C24 C21' 118.9(10) . . ? C21 C24 C21' 6.1(10) . . ? N3 C25 C26 124.6(5) . . ? N3 C25 H25A 117.7 . . ? C26 C25 H25A 117.7 . . ? C27 C26 C25 119.9(5) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C28 116.1(5) . . ? C26 C27 C27 122.1(6) . 2_655 ? C28 C27 C27 121.7(6) . 2_655 ? C29 C28 C27 120.5(5) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? N3 C29 C28 123.0(5) . . ? N3 C29 H29A 118.5 . . ? C28 C29 H29A 118.5 . . ? O1 C30 O2 121.4(5) . . ? O1 C30 C31 119.8(5) . . ? O2 C30 C31 118.8(5) . . ? O1 C30 Co1 59.8(3) . . ? O2 C30 Co1 61.6(3) . . ? C31 C30 Co1 177.0(5) . . ? C32 C31 C36 118.8(7) . . ? C32 C31 C30 120.4(6) . . ? C36 C31 C30 120.7(6) . . ? C31 C32 C33 119.2(7) . . ? C31 C32 H32A 120.4 . . ? C33 C32 H32A 120.4 . . ? C34 C33 C32 123.3(8) . . ? C34 C33 H33A 118.3 . . ? C32 C33 H33A 118.3 . . ? C33 C34 C35 116.6(7) . . ? C33 C34 C34 119.9(6) . 2_655 ? C35 C34 C34 123.6(6) . 2_655 ? C34 C35 C36 121.7(8) . . ? C34 C35 N4 130.2(15) . . ? C36 C35 N4 107.9(14) . . ? C31 C36 C35 120.2(8) . . ? C31 C36 H36A 119.9 . . ? C35 C36 H36A 119.9 . . ? C30 O1 Co1 90.4(3) . . ? C30 O2 Co1 88.4(3) . . ? C11 O3 Co1 149.1(4) . . ? C11 O4 Co1 125.9(3) . 5_776 ? C24 O10 Co2 131.2(4) . . ? Co2 O11 H11A 93(6) . . ? Co2 O11 H11B 132(6) . . ? H11A O11 H11B 119(9) . . ? C25 N3 C29 115.9(5) . . ? C25 N3 Co2 122.8(4) . . ? C29 N3 Co2 121.4(4) . . ? O5 N4 O6 123(2) . . ? O5 N4 C35 132(4) . . ? O6 N4 C35 99(2) . . ? O7 N5 O8 117.7(18) . . ? O7 N5 C23 123.6(19) . . ? O8 N5 C23 115(2) . . ? O7' N5' O8' 118(2) . . ? O7' N5' C16 111(2) . . ? O8' N5' C16 131(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.846 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.125 data_3 _database_code_depnum_ccdc_archive 'CCDC 842834' #TrackingRef '- 842834.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H29.50 Co2 N5 O12.25' _chemical_formula_weight 966.11 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.568(7) _cell_length_b 14.343(3) _cell_length_c 19.344(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.71(3) _cell_angle_gamma 90.00 _cell_volume 8641(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3940 _exptl_absorpt_coefficient_mu 0.839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8845 _exptl_absorpt_correction_T_max 0.9134 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18638 _diffrn_reflns_av_R_equivalents 0.0945 _diffrn_reflns_av_sigmaI/netI 0.1231 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.51 _reflns_number_total 8745 _reflns_number_gt 5682 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+12.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8745 _refine_ls_number_parameters 618 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1132 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1221 _refine_ls_goodness_of_fit_ref 0.821 _refine_ls_restrained_S_all 0.821 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.60527(2) 0.83727(5) 0.63396(4) 0.0296(2) Uani 1 1 d . . . Co2 Co 0.70850(2) 0.85879(5) 0.59319(4) 0.0347(2) Uani 1 1 d . . . C1 C 0.6761(2) 0.7025(4) 0.6293(3) 0.0350(14) Uani 1 1 d . . . C2 C 0.67408(18) 0.6011(3) 0.6431(3) 0.0319(14) Uani 1 1 d . . . C3 C 0.63477(19) 0.5565(4) 0.6185(3) 0.0379(15) Uani 1 1 d . A . H3A H 0.6095 0.5909 0.5980 0.045 Uiso 1 1 calc R . . C4 C 0.63344(19) 0.4610(4) 0.6245(3) 0.0389(15) Uani 1 1 d . . . C5 C 0.6696(2) 0.4060(4) 0.6566(3) 0.0361(15) Uani 1 1 d . A . C6 C 0.7087(2) 0.4521(4) 0.6854(3) 0.0495(17) Uani 1 1 d . . . H6A H 0.7339 0.4181 0.7103 0.059 Uiso 1 1 calc R A . C7 C 0.7110(2) 0.5474(4) 0.6778(3) 0.0454(16) Uani 1 1 d . A . H7A H 0.7378 0.5762 0.6962 0.054 Uiso 1 1 calc R . . C8 C 0.6681(2) 0.3026(4) 0.6578(3) 0.0419(16) Uani 1 1 d . . . C9 C 0.6398(3) 0.2537(4) 0.6773(5) 0.073(2) Uani 1 1 d D A . C10 C 0.6374(2) 0.1586(4) 0.6717(5) 0.074(2) Uani 1 1 d . . . H10A H 0.6174 0.1275 0.6834 0.089 Uiso 1 1 calc R A . C11 C 0.66341(19) 0.1084(4) 0.6497(3) 0.0380(15) Uani 1 1 d . A . C12 C 0.6938(2) 0.1557(4) 0.6353(4) 0.0567(19) Uani 1 1 d . . . H12A H 0.7132 0.1227 0.6231 0.068 Uiso 1 1 calc R A . C13 C 0.6957(2) 0.2514(4) 0.6388(4) 0.0575(19) Uani 1 1 d . A . H13A H 0.7162 0.2823 0.6281 0.069 Uiso 1 1 calc R . . C14 C 0.6596(2) 0.0051(4) 0.6410(3) 0.0393(15) Uani 1 1 d . . . C15 C 0.5427(2) 0.7713(4) 0.6515(3) 0.0406(15) Uani 1 1 d . . . C16 C 0.50398(18) 0.7200(4) 0.6484(3) 0.0369(15) Uani 1 1 d . . . C17 C 0.5027(2) 0.6253(4) 0.6439(4) 0.0504(17) Uani 1 1 d . . . H17A H 0.5263 0.5927 0.6456 0.061 Uiso 1 1 calc R . . C18 C 0.4666(2) 0.5773(4) 0.6368(4) 0.0470(17) Uani 1 1 d . . . C19 C 0.43053(19) 0.6221(4) 0.6329(3) 0.0413(15) Uani 1 1 d . . . C20 C 0.4325(2) 0.7166(4) 0.6395(4) 0.062(2) Uani 1 1 d . . . H20A H 0.4091 0.7488 0.6393 0.074 Uiso 1 1 calc R . . C21 C 0.4684(2) 0.7658(4) 0.6465(4) 0.0589(19) Uani 1 1 d . . . H21A H 0.4686 0.8305 0.6500 0.071 Uiso 1 1 calc R . . C22 C 0.39007(19) 0.5709(4) 0.6204(3) 0.0391(15) Uani 1 1 d . . . C23 C 0.38678(19) 0.5220(4) 0.6791(4) 0.0479(17) Uani 1 1 d . . . H23A H 0.4099 0.5185 0.7273 0.057 Uiso 1 1 calc R . . C24 C 0.3481(2) 0.4779(4) 0.6648(4) 0.0481(17) Uani 1 1 d . . . H24A H 0.3457 0.4443 0.7039 0.058 Uiso 1 1 calc R . . C25 C 0.31359(18) 0.4831(4) 0.5942(3) 0.0371(14) Uani 1 1 d . . . C26 C 0.31722(19) 0.5326(4) 0.5365(3) 0.0472(16) Uani 1 1 d . . . H26A H 0.2940 0.5369 0.4884 0.057 Uiso 1 1 calc R . . C27 C 0.35538(19) 0.5758(4) 0.5501(3) 0.0465(16) Uani 1 1 d . . . H27A H 0.3577 0.6090 0.5108 0.056 Uiso 1 1 calc R . . C28 C 0.2706(2) 0.4438(4) 0.5825(4) 0.0441(16) Uani 1 1 d . . . C29 C 0.54415(19) 0.9362(4) 0.4874(3) 0.0446(16) Uani 1 1 d . . . H29A H 0.5546 0.9890 0.5177 0.054 Uiso 1 1 calc R . . C30 C 0.5114(2) 0.9477(4) 0.4143(3) 0.0481(17) Uani 1 1 d . . . H30A H 0.5002 1.0067 0.3970 0.058 Uiso 1 1 calc R . . C31 C 0.49549(19) 0.8720(4) 0.3677(3) 0.0435(16) Uani 1 1 d . . . C32 C 0.5137(2) 0.7873(5) 0.3969(4) 0.059(2) Uani 1 1 d . . . H32A H 0.5043 0.7338 0.3670 0.071 Uiso 1 1 calc R . . C33 C 0.5460(2) 0.7815(4) 0.4708(3) 0.0514(18) Uani 1 1 d . . . H33A H 0.5576 0.7232 0.4896 0.062 Uiso 1 1 calc R . . C34 C 0.4603(2) 0.8848(5) 0.2902(4) 0.0531(18) Uani 1 1 d . . . H34A H 0.4515 0.9456 0.2745 0.064 Uiso 1 1 calc R . . C35 C 0.4407(2) 0.8190(5) 0.2423(4) 0.0572(18) Uani 1 1 d . . . H35A H 0.4501 0.7585 0.2581 0.069 Uiso 1 1 calc R . . C36 C 0.4047(2) 0.8295(5) 0.1644(3) 0.0466(16) Uani 1 1 d . . . C37 C 0.3928(2) 0.9158(5) 0.1289(4) 0.0540(18) Uani 1 1 d . . . H37A H 0.4072 0.9696 0.1536 0.065 Uiso 1 1 calc R . . C38 C 0.3591(2) 0.9201(4) 0.0557(4) 0.0523(17) Uani 1 1 d . . . H38A H 0.3514 0.9779 0.0317 0.063 Uiso 1 1 calc R . . C39 C 0.3490(2) 0.7629(4) 0.0538(3) 0.0539(18) Uani 1 1 d . . . H39A H 0.3339 0.7100 0.0285 0.065 Uiso 1 1 calc R . . C40 C 0.3820(2) 0.7527(5) 0.1252(4) 0.061(2) Uani 1 1 d . . . H40A H 0.3892 0.6938 0.1472 0.073 Uiso 1 1 calc R . . C41 C 0.6626(2) 0.8965(4) 0.8007(3) 0.0458(16) Uani 1 1 d . . . H41A H 0.6534 0.9563 0.7824 0.055 Uiso 1 1 calc R . . C42 C 0.6920(2) 0.8864(4) 0.8763(3) 0.0488(17) Uani 1 1 d . . . H42A H 0.7015 0.9387 0.9076 0.059 Uiso 1 1 calc R . . C43 C 0.70712(18) 0.8002(4) 0.9055(3) 0.0360(14) Uani 1 1 d . . . C44 C 0.6904(2) 0.7253(4) 0.8560(3) 0.0427(16) Uani 1 1 d . . . H44A H 0.6994 0.6650 0.8728 0.051 Uiso 1 1 calc R . . C45 C 0.66033(19) 0.7410(4) 0.7815(3) 0.0399(15) Uani 1 1 d . . . H45A H 0.6488 0.6897 0.7497 0.048 Uiso 1 1 calc R . . C46 C 0.73909(19) 0.7878(4) 0.9848(3) 0.0426(16) Uani 1 1 d . . . H46A H 0.7445 0.8392 1.0170 0.051 Uiso 1 1 calc R . . N3 N 0.64698(14) 0.8258(3) 0.7528(2) 0.0358(11) Uani 1 1 d . . . N4 N 0.56139(15) 0.8553(3) 0.5165(2) 0.0373(12) Uani 1 1 d . . . N5 N 0.33724(15) 0.8451(3) 0.0185(3) 0.0437(13) Uani 1 1 d . . . O1 O 0.64291(13) 0.7500(2) 0.6052(2) 0.0376(10) Uani 1 1 d . . . O2 O 0.71222(13) 0.7345(2) 0.6400(2) 0.0489(11) Uani 1 1 d . . . O3 O 0.62558(13) -0.0312(2) 0.6360(2) 0.0425(10) Uani 1 1 d . . . O4 O 0.69100(14) -0.0379(2) 0.6391(2) 0.0528(12) Uani 1 1 d . . . O5 O 0.57039(13) 0.7231(3) 0.6429(2) 0.0444(10) Uani 1 1 d . . . O6 O 0.54540(13) 0.8577(3) 0.6596(2) 0.0488(11) Uani 1 1 d . . . O11 O 0.27050(13) 0.3764(3) 0.6230(3) 0.0551(12) Uani 1 1 d . . . O12 O 0.23757(15) 0.4806(3) 0.5366(3) 0.0713(14) Uani 1 1 d . . . O13 O 0.7923(10) 0.6371(17) 0.6362(17) 0.140(10) Uani 0.25 1 d P . . N2 N 0.4664(2) 0.4775(5) 0.6283(6) 0.103(3) Uani 1 1 d . . . O8 O 0.5002(3) 0.4380(5) 0.6769(5) 0.158(3) Uani 1 1 d . . . O7 O 0.4397(2) 0.4326(4) 0.5917(5) 0.143(3) Uani 1 1 d . . . N1 N 0.5907(3) 0.4200(5) 0.5947(5) 0.064(2) Uani 0.799(6) 1 d P A 1 O9 O 0.5817(2) 0.3615(4) 0.5450(4) 0.080(2) Uani 0.799(6) 1 d P A 1 O10 O 0.5669(3) 0.4436(6) 0.6217(6) 0.140(5) Uani 0.799(6) 1 d P A 1 N1' N 0.5962(8) 0.297(3) 0.644(2) 0.110(15) Uiso 0.201(6) 1 d PD A 2 O10' O 0.5997(15) 0.339(3) 0.6997(18) 0.18(2) Uani 0.201(6) 1 d PD A 2 O9' O 0.5590(9) 0.295(2) 0.594(2) 0.18(2) Uani 0.201(6) 1 d PD A 2 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 0.0241(4) 0.0253(4) 0.0353(5) 0.0035(3) 0.0092(4) -0.0030(3) Co2 0.0263(5) 0.0292(4) 0.0429(5) 0.0033(4) 0.0097(4) -0.0026(3) C1 0.035(4) 0.037(3) 0.028(3) 0.001(3) 0.009(3) -0.006(3) C2 0.032(4) 0.025(3) 0.038(3) -0.003(3) 0.015(3) 0.000(3) C3 0.032(4) 0.033(3) 0.048(4) -0.002(3) 0.017(3) -0.001(3) C4 0.037(4) 0.032(3) 0.051(4) -0.006(3) 0.022(3) -0.009(3) C5 0.047(4) 0.028(3) 0.036(3) -0.002(3) 0.021(3) -0.007(3) C6 0.045(4) 0.028(3) 0.066(5) 0.010(3) 0.016(4) 0.004(3) C7 0.039(4) 0.033(3) 0.057(4) 0.000(3) 0.013(3) -0.008(3) C8 0.056(5) 0.027(3) 0.046(4) -0.004(3) 0.025(3) -0.009(3) C9 0.094(7) 0.033(4) 0.133(7) -0.006(4) 0.087(6) -0.004(4) C10 0.087(6) 0.031(4) 0.146(7) -0.003(4) 0.089(6) -0.008(4) C11 0.043(4) 0.028(3) 0.046(4) -0.004(3) 0.022(3) -0.005(3) C12 0.056(5) 0.032(4) 0.099(6) -0.001(4) 0.050(4) 0.000(3) C13 0.054(5) 0.032(4) 0.103(6) 0.003(4) 0.049(5) -0.006(3) C14 0.037(4) 0.040(4) 0.032(4) 0.006(3) 0.006(3) 0.000(3) C15 0.037(4) 0.039(4) 0.039(4) 0.007(3) 0.009(3) -0.005(3) C16 0.020(4) 0.044(4) 0.038(4) 0.003(3) 0.004(3) -0.007(3) C17 0.034(4) 0.045(4) 0.078(5) 0.003(3) 0.030(4) 0.003(3) C18 0.033(4) 0.036(4) 0.074(5) -0.004(3) 0.025(4) -0.008(3) C19 0.025(4) 0.050(4) 0.046(4) -0.005(3) 0.012(3) -0.010(3) C20 0.044(5) 0.051(4) 0.103(6) -0.007(4) 0.044(4) -0.004(4) C21 0.047(5) 0.041(4) 0.092(6) -0.003(4) 0.033(4) -0.012(3) C22 0.030(4) 0.042(4) 0.046(4) -0.005(3) 0.017(3) -0.009(3) C23 0.031(4) 0.057(4) 0.045(4) 0.007(3) 0.007(3) -0.007(3) C24 0.039(4) 0.050(4) 0.054(4) 0.014(3) 0.020(3) -0.005(3) C25 0.026(4) 0.035(3) 0.050(4) -0.006(3) 0.017(3) -0.005(3) C26 0.028(4) 0.072(4) 0.039(4) -0.003(3) 0.012(3) -0.015(3) C27 0.040(4) 0.065(4) 0.039(4) -0.002(3) 0.021(3) -0.013(3) C28 0.026(4) 0.047(4) 0.059(4) 0.004(3) 0.018(3) 0.000(3) C29 0.046(4) 0.039(4) 0.037(4) 0.003(3) 0.007(3) 0.003(3) C30 0.049(4) 0.038(4) 0.045(4) 0.014(3) 0.009(3) 0.010(3) C31 0.034(4) 0.053(4) 0.042(4) 0.007(3) 0.016(3) 0.006(3) C32 0.052(5) 0.055(4) 0.045(4) -0.011(3) -0.003(4) 0.004(4) C33 0.058(5) 0.035(4) 0.042(4) 0.005(3) 0.004(4) 0.010(3) C34 0.044(4) 0.066(4) 0.045(4) -0.004(4) 0.015(4) 0.004(4) C35 0.050(5) 0.070(5) 0.046(4) 0.014(4) 0.016(4) 0.018(4) C36 0.044(4) 0.059(4) 0.035(4) 0.005(3) 0.015(3) 0.009(4) C37 0.040(4) 0.062(5) 0.046(4) -0.005(3) 0.006(3) 0.002(3) C38 0.048(5) 0.046(4) 0.052(4) -0.002(3) 0.012(4) 0.005(3) C39 0.061(5) 0.049(4) 0.039(4) 0.000(3) 0.010(4) 0.003(4) C40 0.062(5) 0.058(5) 0.049(4) 0.012(4) 0.012(4) 0.004(4) C41 0.051(4) 0.033(3) 0.040(4) 0.003(3) 0.007(3) 0.008(3) C42 0.057(5) 0.040(4) 0.035(4) -0.010(3) 0.006(3) 0.008(3) C43 0.038(4) 0.042(4) 0.025(3) 0.001(3) 0.010(3) 0.002(3) C44 0.053(4) 0.031(3) 0.035(4) 0.008(3) 0.010(3) 0.003(3) C45 0.049(4) 0.029(3) 0.033(4) 0.000(3) 0.009(3) -0.008(3) C46 0.044(4) 0.043(4) 0.034(4) -0.006(3) 0.010(3) 0.000(3) N3 0.034(3) 0.037(3) 0.030(3) -0.002(2) 0.008(2) -0.002(2) N4 0.037(3) 0.034(3) 0.036(3) 0.004(2) 0.011(2) 0.003(2) N5 0.042(3) 0.044(3) 0.039(3) -0.003(3) 0.011(3) 0.008(3) O1 0.036(3) 0.032(2) 0.044(2) 0.0050(18) 0.016(2) 0.0088(19) O2 0.031(3) 0.035(2) 0.069(3) 0.013(2) 0.011(2) -0.002(2) O3 0.035(3) 0.029(2) 0.056(3) 0.0057(19) 0.014(2) -0.0061(19) O4 0.047(3) 0.031(2) 0.081(3) -0.005(2) 0.028(3) 0.001(2) O5 0.030(3) 0.041(2) 0.060(3) 0.005(2) 0.018(2) -0.006(2) O6 0.038(3) 0.041(3) 0.064(3) 0.006(2) 0.019(2) -0.008(2) O11 0.031(3) 0.046(3) 0.087(3) 0.012(2) 0.025(2) -0.007(2) O12 0.036(3) 0.088(4) 0.080(4) 0.025(3) 0.015(3) -0.009(3) O13 0.16(3) 0.13(2) 0.19(3) 0.017(19) 0.13(2) 0.012(19) N2 0.041(5) 0.055(5) 0.219(10) -0.009(5) 0.062(6) -0.003(4) O8 0.149(8) 0.081(5) 0.228(9) 0.004(5) 0.069(7) 0.004(5) O7 0.070(5) 0.077(4) 0.266(9) -0.079(5) 0.060(5) -0.035(4) N1 0.062(6) 0.040(4) 0.096(6) -0.016(4) 0.038(5) -0.015(4) O9 0.069(5) 0.074(5) 0.088(5) -0.021(4) 0.027(4) -0.026(4) O10 0.082(6) 0.122(7) 0.263(12) -0.096(8) 0.119(8) -0.044(5) O10' 0.27(5) 0.17(4) 0.07(2) -0.03(2) 0.05(3) -0.16(4) O9' 0.12(3) 0.13(3) 0.35(6) 0.11(4) 0.15(4) 0.03(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.008(4) 1_565 ? Co1 O1 2.049(4) . ? Co1 O5 2.085(4) . ? Co1 N3 2.124(4) . ? Co1 N4 2.131(4) . ? Co1 O6 2.347(4) . ? Co1 C15 2.515(6) . ? Co2 O4 1.954(4) 1_565 ? Co2 O2 1.979(4) . ? Co2 O11 1.979(4) 3 ? Co2 N5 2.059(5) 2_655 ? C1 O1 1.239(6) . ? C1 O2 1.259(7) . ? C1 C2 1.486(7) . ? C2 C3 1.386(7) . ? C2 C7 1.389(7) . ? C3 C4 1.377(7) . ? C3 H3A 0.9300 . ? C4 C5 1.379(8) . ? C4 N1 1.457(9) . ? C5 C6 1.384(8) . ? C5 C8 1.484(7) . ? C6 C7 1.381(7) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C13 1.374(8) . ? C8 C9 1.385(8) . ? C9 C10 1.367(8) . ? C9 N1' 1.490(19) . ? C10 C11 1.358(8) . ? C10 H10A 0.9300 . ? C11 C12 1.378(8) . ? C11 C14 1.490(7) . ? C12 C13 1.374(7) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 O3 1.251(7) . ? C14 O4 1.262(7) . ? C15 O6 1.248(6) . ? C15 O5 1.249(7) . ? C15 C16 1.506(8) . ? C16 C17 1.361(7) . ? C16 C21 1.382(8) . ? C17 C18 1.377(8) . ? C17 H17A 0.9300 . ? C18 C19 1.376(8) . ? C18 N2 1.440(8) . ? C19 C20 1.360(8) . ? C19 C22 1.503(7) . ? C20 C21 1.382(8) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C27 1.369(8) . ? C22 C23 1.381(8) . ? C23 C24 1.394(8) . ? C23 H23A 0.9300 . ? C24 C25 1.372(8) . ? C24 H24A 0.9300 . ? C25 C26 1.374(8) . ? C25 C28 1.511(8) . ? C26 C27 1.375(8) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 O12 1.221(7) . ? C28 O11 1.247(7) . ? C29 N4 1.315(6) . ? C29 C30 1.386(7) . ? C29 H29A 0.9300 . ? C30 C31 1.364(8) . ? C30 H30A 0.9300 . ? C31 C32 1.373(8) . ? C31 C34 1.476(8) . ? C32 C33 1.384(8) . ? C32 H32A 0.9300 . ? C33 N4 1.333(7) . ? C33 H33A 0.9300 . ? C34 C35 1.289(8) . ? C34 H34A 0.9300 . ? C35 C36 1.489(8) . ? C35 H35A 0.9300 . ? C36 C40 1.373(8) . ? C36 C37 1.387(8) . ? C37 C38 1.392(8) . ? C37 H37A 0.9300 . ? C38 N5 1.332(7) . ? C38 H38A 0.9300 . ? C39 N5 1.333(7) . ? C39 C40 1.366(8) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 N3 1.321(6) . ? C41 C42 1.379(7) . ? C41 H41A 0.9300 . ? C42 C43 1.366(7) . ? C42 H42A 0.9300 . ? C43 C44 1.387(7) . ? C43 C46 1.460(7) . ? C44 C45 1.381(7) . ? C44 H44A 0.9300 . ? C45 N3 1.333(6) . ? C45 H45A 0.9300 . ? C46 C46 1.307(10) 7_667 ? C46 H46A 0.9300 . ? N5 Co2 2.059(5) 2_655 ? O3 Co1 2.008(3) 1_545 ? O4 Co2 1.954(4) 1_545 ? O11 Co2 1.979(4) 3_445 ? N2 O7 1.096(8) . ? N2 O8 1.272(9) . ? N1 O10 1.199(9) . ? N1 O9 1.210(8) . ? N1' O10' 1.202(19) . ? N1' O9' 1.227(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O1 108.78(16) 1_565 . ? O3 Co1 O5 161.17(17) 1_565 . ? O1 Co1 O5 90.04(16) . . ? O3 Co1 N3 89.12(16) 1_565 . ? O1 Co1 N3 91.90(16) . . ? O5 Co1 N3 89.68(16) . . ? O3 Co1 N4 89.30(16) 1_565 . ? O1 Co1 N4 91.54(16) . . ? O5 Co1 N4 90.81(16) . . ? N3 Co1 N4 176.52(18) . . ? O3 Co1 O6 102.20(15) 1_565 . ? O1 Co1 O6 148.87(14) . . ? O5 Co1 O6 59.05(14) . . ? N3 Co1 O6 91.59(16) . . ? N4 Co1 O6 85.71(16) . . ? O3 Co1 C15 131.67(19) 1_565 . ? O1 Co1 C15 119.42(18) . . ? O5 Co1 C15 29.66(16) . . ? N3 Co1 C15 92.54(18) . . ? N4 Co1 C15 86.19(18) . . ? O6 Co1 C15 29.49(15) . . ? O4 Co2 O2 116.55(18) 1_565 . ? O4 Co2 O11 106.29(18) 1_565 3 ? O2 Co2 O11 97.71(17) . 3 ? O4 Co2 N5 107.52(19) 1_565 2_655 ? O2 Co2 N5 105.18(18) . 2_655 ? O11 Co2 N5 124.04(19) 3 2_655 ? O1 C1 O2 123.5(5) . . ? O1 C1 C2 119.8(6) . . ? O2 C1 C2 116.6(6) . . ? C3 C2 C7 118.0(5) . . ? C3 C2 C1 120.4(5) . . ? C7 C2 C1 121.6(5) . . ? C4 C3 C2 119.6(6) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C3 C4 C5 123.4(6) . . ? C3 C4 N1 115.7(6) . . ? C5 C4 N1 120.9(5) . . ? C4 C5 C6 116.4(5) . . ? C4 C5 C8 123.2(6) . . ? C6 C5 C8 120.4(6) . . ? C7 C6 C5 121.5(6) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C2 121.0(6) . . ? C6 C7 H7A 119.5 . . ? C2 C7 H7A 119.5 . . ? C13 C8 C9 117.2(5) . . ? C13 C8 C5 119.8(6) . . ? C9 C8 C5 123.0(6) . . ? C10 C9 C8 120.6(6) . . ? C10 C9 N1' 111.3(18) . . ? C8 C9 N1' 111.9(18) . . ? C11 C10 C9 121.9(6) . . ? C11 C10 H10A 119.0 . . ? C9 C10 H10A 119.0 . . ? C10 C11 C12 118.0(5) . . ? C10 C11 C14 121.7(6) . . ? C12 C11 C14 120.3(6) . . ? C13 C12 C11 120.4(6) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C8 121.6(6) . . ? C12 C13 H13A 119.2 . . ? C8 C13 H13A 119.2 . . ? O3 C14 O4 125.8(6) . . ? O3 C14 C11 117.1(6) . . ? O4 C14 C11 117.0(6) . . ? O6 C15 O5 123.2(6) . . ? O6 C15 C16 120.4(6) . . ? O5 C15 C16 116.3(5) . . ? O6 C15 Co1 67.8(3) . . ? O5 C15 Co1 55.8(3) . . ? C16 C15 Co1 168.5(4) . . ? C17 C16 C21 117.9(6) . . ? C17 C16 C15 119.7(6) . . ? C21 C16 C15 122.3(5) . . ? C16 C17 C18 120.6(6) . . ? C16 C17 H17A 119.7 . . ? C18 C17 H17A 119.7 . . ? C19 C18 C17 122.1(6) . . ? C19 C18 N2 119.9(6) . . ? C17 C18 N2 117.9(6) . . ? C20 C19 C18 116.9(6) . . ? C20 C19 C22 120.5(6) . . ? C18 C19 C22 122.6(5) . . ? C19 C20 C21 121.7(7) . . ? C19 C20 H20A 119.2 . . ? C21 C20 H20A 119.2 . . ? C20 C21 C16 120.7(6) . . ? C20 C21 H21A 119.7 . . ? C16 C21 H21A 119.7 . . ? C27 C22 C23 119.5(6) . . ? C27 C22 C19 119.2(5) . . ? C23 C22 C19 121.2(5) . . ? C22 C23 C24 118.8(6) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? C25 C24 C23 121.2(6) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C24 C25 C26 119.4(6) . . ? C24 C25 C28 120.2(6) . . ? C26 C25 C28 120.1(6) . . ? C25 C26 C27 119.6(6) . . ? C25 C26 H26A 120.2 . . ? C27 C26 H26A 120.2 . . ? C22 C27 C26 121.5(6) . . ? C22 C27 H27A 119.3 . . ? C26 C27 H27A 119.3 . . ? O12 C28 O11 122.4(6) . . ? O12 C28 C25 119.8(6) . . ? O11 C28 C25 117.8(6) . . ? N4 C29 C30 124.0(6) . . ? N4 C29 H29A 118.0 . . ? C30 C29 H29A 118.0 . . ? C31 C30 C29 119.8(6) . . ? C31 C30 H30A 120.1 . . ? C29 C30 H30A 120.1 . . ? C30 C31 C32 116.8(6) . . ? C30 C31 C34 119.4(6) . . ? C32 C31 C34 123.8(6) . . ? C31 C32 C33 119.9(6) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? N4 C33 C32 123.3(5) . . ? N4 C33 H33A 118.4 . . ? C32 C33 H33A 118.4 . . ? C35 C34 C31 125.7(6) . . ? C35 C34 H34A 117.1 . . ? C31 C34 H34A 117.1 . . ? C34 C35 C36 126.9(6) . . ? C34 C35 H35A 116.5 . . ? C36 C35 H35A 116.5 . . ? C40 C36 C37 117.9(6) . . ? C40 C36 C35 120.2(6) . . ? C37 C36 C35 121.9(6) . . ? C36 C37 C38 118.7(6) . . ? C36 C37 H37A 120.6 . . ? C38 C37 H37A 120.6 . . ? N5 C38 C37 122.8(6) . . ? N5 C38 H38A 118.6 . . ? C37 C38 H38A 118.6 . . ? N5 C39 C40 123.2(6) . . ? N5 C39 H39A 118.4 . . ? C40 C39 H39A 118.4 . . ? C39 C40 C36 119.9(6) . . ? C39 C40 H40A 120.1 . . ? C36 C40 H40A 120.1 . . ? N3 C41 C42 123.6(5) . . ? N3 C41 H41A 118.2 . . ? C42 C41 H41A 118.2 . . ? C43 C42 C41 120.5(5) . . ? C43 C42 H42A 119.8 . . ? C41 C42 H42A 119.8 . . ? C42 C43 C44 116.4(5) . . ? C42 C43 C46 121.6(5) . . ? C44 C43 C46 122.0(5) . . ? C45 C44 C43 119.6(5) . . ? C45 C44 H44A 120.2 . . ? C43 C44 H44A 120.2 . . ? N3 C45 C44 123.4(5) . . ? N3 C45 H45A 118.3 . . ? C44 C45 H45A 118.3 . . ? C46 C46 C43 126.8(7) 7_667 . ? C46 C46 H46A 116.6 7_667 . ? C43 C46 H46A 116.6 . . ? C41 N3 C45 116.5(5) . . ? C41 N3 Co1 125.3(4) . . ? C45 N3 Co1 118.1(4) . . ? C29 N4 C33 116.2(5) . . ? C29 N4 Co1 123.0(4) . . ? C33 N4 Co1 120.4(4) . . ? C38 N5 C39 117.5(5) . . ? C38 N5 Co2 119.1(4) . 2_655 ? C39 N5 Co2 123.1(4) . 2_655 ? C1 O1 Co1 145.9(4) . . ? C1 O2 Co2 113.0(4) . . ? C14 O3 Co1 134.6(4) . 1_545 ? C14 O4 Co2 145.4(4) . 1_545 ? C15 O5 Co1 94.6(3) . . ? C15 O6 Co1 82.7(4) . . ? C28 O11 Co2 102.4(4) . 3_445 ? O7 N2 O8 117.5(8) . . ? O7 N2 C18 128.2(8) . . ? O8 N2 C18 113.7(8) . . ? O10 N1 O9 123.7(8) . . ? O10 N1 C4 118.9(8) . . ? O9 N1 C4 117.4(7) . . ? O10' N1' O9' 112(3) . . ? O10' N1' C9 97(4) . . ? O9' N1' C9 148(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 9.8(8) . . . . ? O2 C1 C2 C3 -167.1(5) . . . . ? O1 C1 C2 C7 -172.9(5) . . . . ? O2 C1 C2 C7 10.2(8) . . . . ? C7 C2 C3 C4 -4.1(8) . . . . ? C1 C2 C3 C4 173.2(5) . . . . ? C2 C3 C4 C5 2.4(9) . . . . ? C2 C3 C4 N1 -177.9(6) . . . . ? C3 C4 C5 C6 1.6(9) . . . . ? N1 C4 C5 C6 -178.1(6) . . . . ? C3 C4 C5 C8 -175.3(5) . . . . ? N1 C4 C5 C8 4.9(9) . . . . ? C4 C5 C6 C7 -3.9(9) . . . . ? C8 C5 C6 C7 173.2(5) . . . . ? C5 C6 C7 C2 2.1(9) . . . . ? C3 C2 C7 C6 2.0(9) . . . . ? C1 C2 C7 C6 -175.4(5) . . . . ? C4 C5 C8 C13 134.9(7) . . . . ? C6 C5 C8 C13 -42.0(8) . . . . ? C4 C5 C8 C9 -44.9(9) . . . . ? C6 C5 C8 C9 138.2(7) . . . . ? C13 C8 C9 C10 -5.0(12) . . . . ? C5 C8 C9 C10 174.8(7) . . . . ? C13 C8 C9 N1' -138.8(17) . . . . ? C5 C8 C9 N1' 41.1(19) . . . . ? C8 C9 C10 C11 2.3(13) . . . . ? N1' C9 C10 C11 136.3(18) . . . . ? C9 C10 C11 C12 2.2(12) . . . . ? C9 C10 C11 C14 -177.8(7) . . . . ? C10 C11 C12 C13 -3.9(10) . . . . ? C14 C11 C12 C13 176.1(6) . . . . ? C11 C12 C13 C8 1.1(11) . . . . ? C9 C8 C13 C12 3.3(11) . . . . ? C5 C8 C13 C12 -176.5(6) . . . . ? C10 C11 C14 O3 17.3(9) . . . . ? C12 C11 C14 O3 -162.7(6) . . . . ? C10 C11 C14 O4 -162.9(6) . . . . ? C12 C11 C14 O4 17.1(9) . . . . ? O3 Co1 C15 O6 -2.3(4) 1_565 . . . ? O1 Co1 C15 O6 -177.6(3) . . . . ? O5 Co1 C15 O6 173.6(6) . . . . ? N3 Co1 C15 O6 88.7(3) . . . . ? N4 Co1 C15 O6 -88.0(3) . . . . ? O3 Co1 C15 O5 -176.0(3) 1_565 . . . ? O1 Co1 C15 O5 8.7(4) . . . . ? N3 Co1 C15 O5 -84.9(3) . . . . ? N4 Co1 C15 O5 98.4(3) . . . . ? O6 Co1 C15 O5 -173.6(6) . . . . ? O3 Co1 C15 C16 135(2) 1_565 . . . ? O1 Co1 C15 C16 -40(2) . . . . ? O5 Co1 C15 C16 -49(2) . . . . ? N3 Co1 C15 C16 -134(2) . . . . ? N4 Co1 C15 C16 50(2) . . . . ? O6 Co1 C15 C16 138(2) . . . . ? O6 C15 C16 C17 -176.3(6) . . . . ? O5 C15 C16 C17 6.1(8) . . . . ? Co1 C15 C16 C17 50(2) . . . . ? O6 C15 C16 C21 6.6(9) . . . . ? O5 C15 C16 C21 -171.0(6) . . . . ? Co1 C15 C16 C21 -127(2) . . . . ? C21 C16 C17 C18 0.7(10) . . . . ? C15 C16 C17 C18 -176.5(6) . . . . ? C16 C17 C18 C19 1.0(10) . . . . ? C16 C17 C18 N2 176.8(7) . . . . ? C17 C18 C19 C20 -2.7(10) . . . . ? N2 C18 C19 C20 -178.4(7) . . . . ? C17 C18 C19 C22 176.2(6) . . . . ? N2 C18 C19 C22 0.4(10) . . . . ? C18 C19 C20 C21 2.8(10) . . . . ? C22 C19 C20 C21 -176.1(6) . . . . ? C19 C20 C21 C16 -1.2(11) . . . . ? C17 C16 C21 C20 -0.6(10) . . . . ? C15 C16 C21 C20 176.5(6) . . . . ? C20 C19 C22 C27 73.1(8) . . . . ? C18 C19 C22 C27 -105.7(7) . . . . ? C20 C19 C22 C23 -104.5(8) . . . . ? C18 C19 C22 C23 76.7(8) . . . . ? C27 C22 C23 C24 0.6(9) . . . . ? C19 C22 C23 C24 178.3(6) . . . . ? C22 C23 C24 C25 -0.6(9) . . . . ? C23 C24 C25 C26 0.1(9) . . . . ? C23 C24 C25 C28 -173.3(6) . . . . ? C24 C25 C26 C27 0.3(9) . . . . ? C28 C25 C26 C27 173.7(6) . . . . ? C23 C22 C27 C26 -0.3(9) . . . . ? C19 C22 C27 C26 -177.9(6) . . . . ? C25 C26 C27 C22 -0.2(10) . . . . ? C24 C25 C28 O12 147.6(6) . . . . ? C26 C25 C28 O12 -25.8(9) . . . . ? C24 C25 C28 O11 -29.6(8) . . . . ? C26 C25 C28 O11 157.0(6) . . . . ? N4 C29 C30 C31 -0.8(10) . . . . ? C29 C30 C31 C32 -0.3(9) . . . . ? C29 C30 C31 C34 179.4(6) . . . . ? C30 C31 C32 C33 1.0(10) . . . . ? C34 C31 C32 C33 -178.7(6) . . . . ? C31 C32 C33 N4 -0.8(11) . . . . ? C30 C31 C34 C35 -175.6(7) . . . . ? C32 C31 C34 C35 4.2(11) . . . . ? C31 C34 C35 C36 178.9(6) . . . . ? C34 C35 C36 C40 -168.7(7) . . . . ? C34 C35 C36 C37 11.5(11) . . . . ? C40 C36 C37 C38 -0.4(10) . . . . ? C35 C36 C37 C38 179.4(6) . . . . ? C36 C37 C38 N5 0.8(10) . . . . ? N5 C39 C40 C36 0.6(11) . . . . ? C37 C36 C40 C39 -0.2(10) . . . . ? C35 C36 C40 C39 179.9(6) . . . . ? N3 C41 C42 C43 1.1(10) . . . . ? C41 C42 C43 C44 -1.9(9) . . . . ? C41 C42 C43 C46 178.2(6) . . . . ? C42 C43 C44 C45 0.4(9) . . . . ? C46 C43 C44 C45 -179.8(6) . . . . ? C43 C44 C45 N3 2.2(9) . . . . ? C42 C43 C46 C46 -168.0(8) . . . 7_667 ? C44 C43 C46 C46 12.2(12) . . . 7_667 ? C42 C41 N3 C45 1.4(9) . . . . ? C42 C41 N3 Co1 -175.4(5) . . . . ? C44 C45 N3 C41 -3.0(9) . . . . ? C44 C45 N3 Co1 174.0(5) . . . . ? O3 Co1 N3 C41 21.4(5) 1_565 . . . ? O1 Co1 N3 C41 130.1(5) . . . . ? O5 Co1 N3 C41 -139.9(5) . . . . ? N4 Co1 N3 C41 -42(3) . . . . ? O6 Co1 N3 C41 -80.8(5) . . . . ? C15 Co1 N3 C41 -110.3(5) . . . . ? O3 Co1 N3 C45 -155.3(4) 1_565 . . . ? O1 Co1 N3 C45 -46.6(4) . . . . ? O5 Co1 N3 C45 43.4(4) . . . . ? N4 Co1 N3 C45 142(3) . . . . ? O6 Co1 N3 C45 102.5(4) . . . . ? C15 Co1 N3 C45 73.0(4) . . . . ? C30 C29 N4 C33 1.1(9) . . . . ? C30 C29 N4 Co1 -171.0(5) . . . . ? C32 C33 N4 C29 -0.3(9) . . . . ? C32 C33 N4 Co1 172.0(5) . . . . ? O3 Co1 N4 C29 -30.1(5) 1_565 . . . ? O1 Co1 N4 C29 -138.9(5) . . . . ? O5 Co1 N4 C29 131.0(5) . . . . ? N3 Co1 N4 C29 33(3) . . . . ? O6 Co1 N4 C29 72.2(5) . . . . ? C15 Co1 N4 C29 101.7(5) . . . . ? O3 Co1 N4 C33 158.2(5) 1_565 . . . ? O1 Co1 N4 C33 49.4(5) . . . . ? O5 Co1 N4 C33 -40.7(5) . . . . ? N3 Co1 N4 C33 -139(3) . . . . ? O6 Co1 N4 C33 -99.6(5) . . . . ? C15 Co1 N4 C33 -70.0(5) . . . . ? C37 C38 N5 C39 -0.5(9) . . . . ? C37 C38 N5 Co2 -174.7(5) . . . 2_655 ? C40 C39 N5 C38 -0.3(10) . . . . ? C40 C39 N5 Co2 173.7(5) . . . 2_655 ? O2 C1 O1 Co1 -87.0(8) . . . . ? C2 C1 O1 Co1 96.2(7) . . . . ? O3 Co1 O1 C1 88.2(7) 1_565 . . . ? O5 Co1 O1 C1 -91.2(7) . . . . ? N3 Co1 O1 C1 -1.5(7) . . . . ? N4 Co1 O1 C1 178.0(7) . . . . ? O6 Co1 O1 C1 -97.7(7) . . . . ? C15 Co1 O1 C1 -95.5(7) . . . . ? O1 C1 O2 Co2 -13.0(7) . . . . ? C2 C1 O2 Co2 163.9(4) . . . . ? O4 Co2 O2 C1 68.4(4) 1_565 . . . ? O11 Co2 O2 C1 -179.0(4) 3 . . . ? N5 Co2 O2 C1 -50.6(4) 2_655 . . . ? O4 C14 O3 Co1 7.3(9) . . . 1_545 ? C11 C14 O3 Co1 -172.9(4) . . . 1_545 ? O3 C14 O4 Co2 37.2(11) . . . 1_545 ? C11 C14 O4 Co2 -142.6(6) . . . 1_545 ? O6 C15 O5 Co1 -7.1(6) . . . . ? C16 C15 O5 Co1 170.4(4) . . . . ? O3 Co1 O5 C15 9.4(7) 1_565 . . . ? O1 Co1 O5 C15 -172.4(3) . . . . ? N3 Co1 O5 C15 95.7(4) . . . . ? N4 Co1 O5 C15 -80.8(4) . . . . ? O6 Co1 O5 C15 3.7(3) . . . . ? O5 C15 O6 Co1 6.3(5) . . . . ? C16 C15 O6 Co1 -171.1(5) . . . . ? O3 Co1 O6 C15 178.2(3) 1_565 . . . ? O1 Co1 O6 C15 4.0(5) . . . . ? O5 Co1 O6 C15 -3.7(3) . . . . ? N3 Co1 O6 C15 -92.3(3) . . . . ? N4 Co1 O6 C15 89.9(3) . . . . ? O12 C28 O11 Co2 -1.8(8) . . . 3_445 ? C25 C28 O11 Co2 175.3(4) . . . 3_445 ? C19 C18 N2 O7 34.9(15) . . . . ? C17 C18 N2 O7 -141.1(11) . . . . ? C19 C18 N2 O8 -135.8(8) . . . . ? C17 C18 N2 O8 48.2(11) . . . . ? C3 C4 N1 O10 -59.6(11) . . . . ? C5 C4 N1 O10 120.1(9) . . . . ? C3 C4 N1 O9 122.4(7) . . . . ? C5 C4 N1 O9 -57.8(10) . . . . ? C10 C9 N1' O10' 123(3) . . . . ? C8 C9 N1' O10' -98(3) . . . . ? C10 C9 N1' O9' -36(8) . . . . ? C8 C9 N1' O9' 102(8) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.51 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.685 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.083 data_4 _database_code_depnum_ccdc_archive 'CCDC 891957' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H44 Co4 N6 O28' _chemical_formula_weight 1604.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.3413(6) _cell_length_b 7.9077(3) _cell_length_c 27.2146(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.5730(10) _cell_angle_gamma 90.00 _cell_volume 3264.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9868 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 28.18 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7716 _exptl_absorpt_correction_T_max 0.8985 _exptl_absorpt_process_details 'SADABS (Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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_% none _diffrn_reflns_number 42918 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8088 _reflns_number_gt 6506 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.1113P)^2^+8.8847P] 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 8088 _refine_ls_number_parameters 523 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1848 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.002 _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 0.39803(3) 0.72380(6) 0.489004(16) 0.02230(14) Uani 1 1 d . . . Co2 Co 0.27515(3) 1.06446(6) 0.467494(17) 0.02608(15) Uani 1 1 d . . . C1 C 0.2261(3) 0.6965(5) 0.44152(14) 0.0352(9) Uani 1 1 d . . . C2 C 0.1527(3) 0.6486(6) 0.40180(15) 0.0364(9) Uani 1 1 d . . . C3 C 0.0698(3) 0.7178(6) 0.40086(17) 0.0415(10) Uani 1 1 d . A . H3A H 0.0583 0.7880 0.4265 0.050 Uiso 1 1 calc R . . C4 C 0.0036(3) 0.6825(7) 0.36156(17) 0.0455(11) Uani 1 1 d D . . C5 C 0.0210(3) 0.5804(7) 0.32224(17) 0.0461(11) Uani 1 1 d . A . C6 C 0.1048(3) 0.5135(7) 0.32346(19) 0.0542(13) Uani 1 1 d . . . H6A H 0.1173 0.4458 0.2974 0.065 Uiso 1 1 calc R A . C7 C 0.1699(3) 0.5468(7) 0.36310(18) 0.0495(12) Uani 1 1 d . A . H7A H 0.2257 0.5003 0.3637 0.059 Uiso 1 1 calc R . . C8 C -0.0457(3) 0.5531(7) 0.27692(17) 0.0458(11) Uani 1 1 d . . . C9 C -0.1295(3) 0.4897(8) 0.27752(16) 0.0496(12) Uani 1 1 d . A . C10 C -0.1902(3) 0.4730(7) 0.23488(16) 0.0449(11) Uani 1 1 d . . . H10A H -0.2458 0.4285 0.2366 0.054 Uiso 1 1 calc R A . C11 C -0.1682(3) 0.5222(5) 0.19016(14) 0.0336(8) Uani 1 1 d . A . C12 C -0.0840(3) 0.5814(7) 0.18826(17) 0.0473(12) Uani 1 1 d . . . H12A H -0.0676 0.6114 0.1579 0.057 Uiso 1 1 calc R A . C13 C -0.0238(3) 0.5964(8) 0.23159(18) 0.0547(14) Uani 1 1 d . A . H13A H 0.0326 0.6366 0.2298 0.066 Uiso 1 1 calc R . . C14 C -0.2335(3) 0.5101(5) 0.14303(14) 0.0313(8) Uani 1 1 d . . . C15 C 0.3958(3) 0.9783(5) 0.56378(13) 0.0296(8) Uani 1 1 d . . . C16 C 0.4161(3) 0.9898(6) 0.61953(14) 0.0354(9) Uani 1 1 d . . . C17 C 0.3532(4) 1.0460(9) 0.64688(17) 0.0634(18) Uani 1 1 d . B . H17A H 0.2990 1.0836 0.6308 0.076 Uiso 1 1 calc R . . C18 C 0.3707(4) 1.0466(9) 0.69833(17) 0.0654(18) Uani 1 1 d D . . C19 C 0.4524(3) 0.9934(6) 0.72383(15) 0.0418(10) Uani 1 1 d . B . C20 C 0.5137(3) 0.9352(6) 0.69532(14) 0.0361(9) Uani 1 1 d . . . H20A H 0.5685 0.8988 0.7110 0.043 Uiso 1 1 calc R B . C21 C 0.4954(3) 0.9299(6) 0.64368(14) 0.0339(8) Uani 1 1 d . B . H21A H 0.5367 0.8857 0.6255 0.041 Uiso 1 1 calc R . . C22 C 0.4742(3) 0.9833(6) 0.77911(14) 0.0380(9) Uani 1 1 d . . . C23 C 0.4176(3) 0.9120(9) 0.80837(16) 0.0575(15) Uani 1 1 d D B . C24 C 0.4411(3) 0.9008(8) 0.85954(16) 0.0531(14) Uani 1 1 d . . . H24A H 0.4024 0.8525 0.8788 0.064 Uiso 1 1 calc R B . C25 C 0.5217(3) 0.9613(5) 0.88196(13) 0.0295(8) Uani 1 1 d . B . C26 C 0.5797(3) 1.0285(6) 0.85307(14) 0.0375(9) Uani 1 1 d . . . H26A H 0.6345 1.0678 0.8680 0.045 Uiso 1 1 calc R B . C27 C 0.5566(3) 1.0380(6) 0.80177(15) 0.0415(10) Uani 1 1 d . B . H27A H 0.5966 1.0812 0.7825 0.050 Uiso 1 1 calc R . . C28 C 0.5463(2) 0.9554(5) 0.93733(13) 0.0274(7) Uani 1 1 d . . . C29 C 0.1839(3) 1.3380(7) 0.51803(16) 0.0455(11) Uani 1 1 d . . . H29A H 0.2397 1.3510 0.5364 0.055 Uiso 1 1 calc R . . C30 C 0.1192(3) 1.4546(7) 0.52443(17) 0.0445(11) Uani 1 1 d . . . H30A H 0.1319 1.5440 0.5465 0.053 Uiso 1 1 calc R . . C31 C 0.0351(2) 1.4372(5) 0.49759(15) 0.0329(8) Uani 1 1 d . . . C32 C 0.0212(3) 1.2996(7) 0.4665(2) 0.0500(13) Uani 1 1 d . . . H32A H -0.0344 1.2808 0.4485 0.060 Uiso 1 1 calc R . . C33 C 0.0893(3) 1.1889(6) 0.4619(2) 0.0495(12) Uani 1 1 d . . . H33A H 0.0780 1.0972 0.4404 0.059 Uiso 1 1 calc R . . N3 N 0.1698(2) 1.2079(5) 0.48667(13) 0.0357(8) Uani 1 1 d . . . O3 O 0.2972(2) 0.6134(4) 0.44377(11) 0.0431(7) Uani 1 1 d . . . O4 O 0.2176(2) 0.8199(4) 0.46987(11) 0.0466(8) Uani 1 1 d . . . O5 O 0.45046(18) 0.8984(4) 0.54179(9) 0.0333(6) Uani 1 1 d . . . O6 O 0.32624(19) 1.0456(4) 0.54252(10) 0.0376(7) Uani 1 1 d . . . O7 O 0.60740(19) 1.0515(4) 0.95612(10) 0.0364(7) Uani 1 1 d . . . O8 O 0.5093(2) 0.8534(4) 0.96276(10) 0.0396(7) Uani 1 1 d . . . O13 O -0.30320(19) 0.4288(4) 0.14520(10) 0.0427(8) Uani 1 1 d . A . O14 O -0.21326(19) 0.5793(4) 0.10521(10) 0.0386(7) Uani 1 1 d . . . N1 N -0.1536(4) 0.4312(12) 0.3238(2) 0.082(3) Uani 0.785(5) 1 d P A 1 O9 O -0.1035(4) 0.3388(11) 0.3502(2) 0.094(2) Uani 0.785(5) 1 d P A 1 O10 O -0.2227(5) 0.483(2) 0.3337(3) 0.181(6) Uani 0.785(5) 1 d P A 1 N1' N -0.0788(10) 0.779(3) 0.3667(7) 0.082(3) Uani 0.215(5) 1 d PD A 2 O9' O -0.0809(16) 0.919(3) 0.3902(8) 0.094(2) Uani 0.215(5) 1 d PD A 2 O10' O -0.1546(14) 0.713(4) 0.3602(9) 0.181(6) Uani 0.215(5) 1 d PD A 2 N2 N 0.2958(4) 1.0918(10) 0.7249(2) 0.0559(18) Uani 0.720(6) 1 d PD B 1 O11 O 0.2233(4) 1.0322(16) 0.7119(3) 0.128(4) Uani 0.720(6) 1 d P B 1 O12 O 0.3102(4) 1.1887(8) 0.7585(2) 0.0647(17) Uani 0.720(6) 1 d P B 1 N2' N 0.3301(9) 0.945(2) 0.7819(5) 0.071(6) Uani 0.280(6) 1 d PD B 2 O11' O 0.2767(11) 1.055(3) 0.7895(7) 0.097(7) Uani 0.280(6) 1 d PD B 2 O12' O 0.3113(13) 0.828(3) 0.7525(6) 0.095(7) Uani 0.280(6) 1 d PD B 2 O1 O 0.3515(2) 1.2813(4) 0.45843(12) 0.0399(7) Uani 1 1 d D . . O2 O 0.38328(17) 0.9358(3) 0.44188(9) 0.0272(5) Uani 1 1 d D . . HW1A H 0.395(2) 1.307(5) 0.4807(13) 0.032(12) Uiso 1 1 d D . . HW1B H 0.324(3) 1.371(4) 0.449(2) 0.065(19) Uiso 1 1 d D . . HW2A H 0.4322(19) 0.990(6) 0.4442(16) 0.035(12) Uiso 1 1 d D . . HW2B H 0.358(3) 0.935(8) 0.4120(10) 0.067(19) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0228(2) 0.0256(3) 0.0157(2) -0.00410(17) -0.00661(16) 0.00449(18) Co2 0.0244(2) 0.0297(3) 0.0214(2) -0.00489(18) -0.00571(18) 0.00929(19) C1 0.037(2) 0.036(2) 0.0276(18) 0.0053(16) -0.0125(16) -0.0094(17) C2 0.037(2) 0.035(2) 0.0315(19) 0.0015(16) -0.0158(16) -0.0016(17) C3 0.039(2) 0.049(3) 0.034(2) -0.0007(19) -0.0051(17) -0.0033(19) C4 0.035(2) 0.056(3) 0.040(2) 0.001(2) -0.0114(18) 0.000(2) C5 0.044(2) 0.052(3) 0.035(2) 0.002(2) -0.0174(19) -0.008(2) C6 0.053(3) 0.055(3) 0.046(3) -0.017(2) -0.021(2) 0.006(2) C7 0.043(2) 0.052(3) 0.045(3) -0.011(2) -0.021(2) 0.010(2) C8 0.042(2) 0.055(3) 0.033(2) 0.0008(19) -0.0171(18) -0.006(2) C9 0.038(2) 0.081(4) 0.026(2) 0.000(2) -0.0082(17) -0.005(2) C10 0.031(2) 0.070(3) 0.030(2) 0.001(2) -0.0089(16) -0.009(2) C11 0.0322(19) 0.037(2) 0.0267(18) -0.0020(16) -0.0118(15) -0.0053(16) C12 0.041(2) 0.063(3) 0.033(2) 0.009(2) -0.0120(18) -0.016(2) C13 0.037(2) 0.079(4) 0.042(2) 0.009(2) -0.0153(19) -0.023(2) C14 0.0311(18) 0.034(2) 0.0239(17) -0.0015(15) -0.0105(14) -0.0040(15) C15 0.0349(19) 0.032(2) 0.0194(16) -0.0025(14) -0.0050(14) 0.0030(15) C16 0.042(2) 0.042(2) 0.0192(16) -0.0033(16) -0.0037(15) 0.0083(18) C17 0.057(3) 0.102(5) 0.026(2) -0.015(2) -0.010(2) 0.040(3) C18 0.060(3) 0.110(5) 0.024(2) -0.009(3) -0.001(2) 0.039(3) C19 0.050(2) 0.049(3) 0.0222(18) -0.0020(17) -0.0078(17) 0.008(2) C20 0.036(2) 0.047(2) 0.0218(17) 0.0037(16) -0.0046(15) 0.0027(17) C21 0.0344(19) 0.042(2) 0.0228(17) -0.0014(16) -0.0023(15) 0.0036(17) C22 0.044(2) 0.047(2) 0.0198(17) -0.0041(16) -0.0071(16) 0.0047(19) C23 0.038(2) 0.106(5) 0.025(2) -0.012(2) -0.0052(17) -0.010(3) C24 0.043(2) 0.090(4) 0.0249(19) -0.005(2) 0.0026(17) -0.026(3) C25 0.0340(18) 0.0297(19) 0.0231(17) 0.0009(14) -0.0014(14) -0.0038(15) C26 0.035(2) 0.052(3) 0.0226(17) 0.0008(17) -0.0036(15) -0.0137(18) C27 0.048(2) 0.052(3) 0.0228(18) 0.0051(17) 0.0007(17) -0.016(2) C28 0.0276(17) 0.0312(19) 0.0223(16) 0.0015(14) -0.0001(13) -0.0004(14) C29 0.033(2) 0.061(3) 0.038(2) -0.018(2) -0.0088(17) 0.018(2) C30 0.035(2) 0.053(3) 0.041(2) -0.022(2) -0.0089(18) 0.0155(19) C31 0.0287(18) 0.037(2) 0.0322(19) -0.0020(16) 0.0023(15) 0.0108(16) C32 0.0263(19) 0.052(3) 0.067(3) -0.024(2) -0.008(2) 0.0121(19) C33 0.037(2) 0.042(3) 0.065(3) -0.024(2) -0.005(2) 0.0094(19) N3 0.0292(16) 0.0394(19) 0.0363(17) -0.0060(15) -0.0020(13) 0.0147(14) O3 0.0405(16) 0.0410(17) 0.0399(16) 0.0072(13) -0.0203(13) -0.0032(13) O4 0.0544(19) 0.0504(19) 0.0323(15) -0.0103(14) -0.0022(13) -0.0184(16) O5 0.0326(13) 0.0429(16) 0.0218(12) -0.0091(11) -0.0047(10) 0.0063(12) O6 0.0354(14) 0.0512(18) 0.0227(13) -0.0051(12) -0.0063(11) 0.0149(13) O7 0.0346(14) 0.0486(18) 0.0246(13) -0.0026(12) -0.0006(11) -0.0127(13) O8 0.0413(15) 0.0485(18) 0.0288(13) 0.0083(13) 0.0048(12) -0.0115(14) O13 0.0338(14) 0.063(2) 0.0266(13) 0.0067(13) -0.0119(11) -0.0185(14) O14 0.0380(15) 0.0492(18) 0.0242(13) 0.0029(12) -0.0098(11) -0.0165(13) N1 0.044(3) 0.167(8) 0.031(3) 0.015(4) -0.009(2) -0.030(4) O9 0.088(4) 0.136(6) 0.052(3) 0.031(4) -0.015(3) -0.033(4) O10 0.056(4) 0.422(19) 0.069(4) 0.056(7) 0.022(3) 0.033(7) N1' 0.044(3) 0.167(8) 0.031(3) 0.015(4) -0.009(2) -0.030(4) O9' 0.088(4) 0.136(6) 0.052(3) 0.031(4) -0.015(3) -0.033(4) O10' 0.056(4) 0.422(19) 0.069(4) 0.056(7) 0.022(3) 0.033(7) N2 0.039(3) 0.099(5) 0.029(3) -0.009(3) 0.004(2) 0.009(3) O11 0.044(3) 0.253(12) 0.092(5) -0.083(7) 0.024(3) -0.031(5) O12 0.066(3) 0.078(4) 0.051(3) -0.021(3) 0.011(3) 0.016(3) N2' 0.044(9) 0.14(2) 0.030(7) -0.004(9) 0.009(6) -0.029(11) O11' 0.060(10) 0.17(2) 0.064(11) -0.002(12) 0.003(8) 0.020(12) O12' 0.098(13) 0.125(16) 0.053(9) 0.003(10) -0.012(8) -0.071(12) O1 0.0395(16) 0.0324(16) 0.0423(16) -0.0053(13) -0.0116(13) 0.0008(13) O2 0.0265(12) 0.0325(14) 0.0201(11) -0.0034(10) -0.0047(10) 0.0054(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.025(3) . ? Co1 O7 2.033(3) 2_646 ? Co1 O8 2.039(3) 4_575 ? Co1 O5 2.067(3) . ? Co1 O2 2.103(3) . ? Co2 O14 2.067(3) 2 ? Co2 O6 2.080(3) . ? Co2 N3 2.103(3) . ? Co2 O1 2.112(3) . ? Co2 O4 2.131(3) . ? Co2 O2 2.149(3) . ? C1 O4 1.262(6) . ? C1 O3 1.267(5) . ? C1 C2 1.489(5) . ? C2 C3 1.381(6) . ? C2 C7 1.382(7) . ? C3 C4 1.389(6) . ? C3 H3A 0.9300 . ? C4 C5 1.397(7) . ? C4 N1' 1.499(16) . ? C5 C6 1.387(7) . ? C5 C8 1.496(5) . ? C6 C7 1.381(6) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C13 1.370(7) . ? C8 C9 1.382(7) . ? C9 C10 1.382(6) . ? C9 N1 1.442(8) . ? C10 C11 1.367(6) . ? C10 H10A 0.9300 . ? C11 C12 1.382(6) . ? C11 C14 1.508(5) . ? C12 C13 1.391(6) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 O14 1.245(5) . ? C14 O13 1.257(5) . ? C15 O6 1.254(5) . ? C15 O5 1.269(5) . ? C15 C16 1.506(5) . ? C16 C17 1.377(7) . ? C16 C21 1.377(6) . ? C17 C18 1.386(6) . ? C17 H17A 0.9300 . ? C18 C19 1.404(7) . ? C18 N2 1.489(7) . ? C19 C20 1.384(6) . ? C19 C22 1.494(5) . ? C20 C21 1.392(5) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.383(7) . ? C22 C27 1.390(6) . ? C23 C24 1.388(6) . ? C23 N2' 1.449(13) . ? C24 C25 1.380(6) . ? C24 H24A 0.9300 . ? C25 C26 1.379(6) . ? C25 C28 1.499(5) . ? C26 C27 1.390(5) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 O8 1.254(5) . ? C28 O7 1.254(5) . ? C29 N3 1.333(6) . ? C29 C30 1.385(6) . ? C29 H29A 0.9300 . ? C30 C31 1.391(6) . ? C30 H30A 0.9300 . ? C31 C32 1.375(6) . ? C31 C31 1.486(7) 3_586 ? C32 C33 1.383(6) . ? C32 H32A 0.9300 . ? C33 N3 1.326(6) . ? C33 H33A 0.9300 . ? O7 Co1 2.033(3) 2_656 ? O8 Co1 2.039(3) 4_576 ? O14 Co2 2.067(3) 2_545 ? N1 O10 1.203(11) . ? N1 O9 1.215(10) . ? N1' O10' 1.262(16) . ? N1' O9' 1.284(17) . ? N2 O12 1.189(8) . ? N2 O11 1.211(9) . ? N2' O12' 1.231(16) . ? N2' O11' 1.233(16) . ? O1 HW1A 0.859(19) . ? O1 HW1B 0.846(19) . ? O2 HW2A 0.858(19) . ? O2 HW2B 0.846(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 O7 92.67(12) . 2_646 ? O3 Co1 O8 105.14(14) . 4_575 ? O7 Co1 O8 100.65(12) 2_646 4_575 ? O3 Co1 O5 153.26(13) . . ? O7 Co1 O5 89.51(12) 2_646 . ? O8 Co1 O5 100.61(12) 4_575 . ? O3 Co1 O2 88.28(11) . . ? O7 Co1 O2 166.01(11) 2_646 . ? O8 Co1 O2 92.56(12) 4_575 . ? O5 Co1 O2 83.48(11) . . ? O14 Co2 O6 174.80(12) 2 . ? O14 Co2 N3 86.94(12) 2 . ? O6 Co2 N3 89.21(12) . . ? O14 Co2 O1 91.47(13) 2 . ? O6 Co2 O1 92.22(13) . . ? N3 Co2 O1 92.90(14) . . ? O14 Co2 O4 86.98(13) 2 . ? O6 Co2 O4 90.12(13) . . ? N3 Co2 O4 98.35(15) . . ? O1 Co2 O4 168.54(13) . . ? O14 Co2 O2 89.02(10) 2 . ? O6 Co2 O2 95.06(10) . . ? N3 Co2 O2 174.18(13) . . ? O1 Co2 O2 83.01(12) . . ? O4 Co2 O2 85.61(13) . . ? O4 C1 O3 122.5(4) . . ? O4 C1 C2 120.3(4) . . ? O3 C1 C2 117.1(4) . . ? C3 C2 C7 119.7(4) . . ? C3 C2 C1 120.5(4) . . ? C7 C2 C1 119.5(4) . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 120.3(4) . . ? C3 C4 N1' 110.9(9) . . ? C5 C4 N1' 128.6(9) . . ? C6 C5 C4 119.0(4) . . ? C6 C5 C8 118.9(5) . . ? C4 C5 C8 121.9(4) . . ? C7 C6 C5 120.4(5) . . ? C7 C6 H6A 119.8 . . ? C5 C6 H6A 119.8 . . ? C6 C7 C2 120.6(5) . . ? C6 C7 H7A 119.7 . . ? C2 C7 H7A 119.7 . . ? C13 C8 C9 117.1(4) . . ? C13 C8 C5 118.5(4) . . ? C9 C8 C5 124.5(4) . . ? C10 C9 C8 122.5(4) . . ? C10 C9 N1 118.3(5) . . ? C8 C9 N1 119.2(4) . . ? C11 C10 C9 119.7(4) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C12 119.1(4) . . ? C10 C11 C14 121.2(4) . . ? C12 C11 C14 119.7(4) . . ? C11 C12 C13 120.3(4) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C8 C13 C12 121.4(4) . . ? C8 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? O14 C14 O13 125.6(3) . . ? O14 C14 C11 117.4(3) . . ? O13 C14 C11 117.0(3) . . ? O6 C15 O5 124.8(3) . . ? O6 C15 C16 118.3(3) . . ? O5 C15 C16 116.9(3) . . ? C17 C16 C21 119.5(4) . . ? C17 C16 C15 120.5(4) . . ? C21 C16 C15 119.7(4) . . ? C16 C17 C18 120.1(4) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C17 C18 C19 121.5(5) . . ? C17 C18 N2 116.4(5) . . ? C19 C18 N2 121.9(4) . . ? C20 C19 C18 117.0(4) . . ? C20 C19 C22 118.6(4) . . ? C18 C19 C22 124.3(4) . . ? C19 C20 C21 121.6(4) . . ? C19 C20 H20A 119.2 . . ? C21 C20 H20A 119.2 . . ? C16 C21 C20 120.2(4) . . ? C16 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C23 C22 C27 118.6(4) . . ? C23 C22 C19 122.4(4) . . ? C27 C22 C19 118.8(4) . . ? C22 C23 C24 120.8(4) . . ? C22 C23 N2' 104.8(7) . . ? C24 C23 N2' 126.3(7) . . ? C25 C24 C23 120.2(4) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C26 C25 C24 119.6(4) . . ? C26 C25 C28 119.8(3) . . ? C24 C25 C28 120.6(4) . . ? C25 C26 C27 120.3(4) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C22 C27 C26 120.5(4) . . ? C22 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? O8 C28 O7 122.5(3) . . ? O8 C28 C25 120.5(3) . . ? O7 C28 C25 116.9(3) . . ? N3 C29 C30 122.9(4) . . ? N3 C29 H29A 118.6 . . ? C30 C29 H29A 118.6 . . ? C29 C30 C31 119.6(4) . . ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? C32 C31 C30 116.6(4) . . ? C32 C31 C31 122.3(5) . 3_586 ? C30 C31 C31 121.1(5) . 3_586 ? C31 C32 C33 120.5(4) . . ? C31 C32 H32A 119.8 . . ? C33 C32 H32A 119.8 . . ? N3 C33 C32 122.7(4) . . ? N3 C33 H33A 118.6 . . ? C32 C33 H33A 118.6 . . ? C33 N3 C29 117.6(4) . . ? C33 N3 Co2 120.3(3) . . ? C29 N3 Co2 121.2(3) . . ? C1 O3 Co1 112.3(3) . . ? C1 O4 Co2 127.0(3) . . ? C15 O5 Co1 116.4(2) . . ? C15 O6 Co2 130.8(3) . . ? C28 O7 Co1 126.6(3) . 2_656 ? C28 O8 Co1 149.1(3) . 4_576 ? C14 O14 Co2 129.1(2) . 2_545 ? O10 N1 O9 125.0(8) . . ? O10 N1 C9 115.8(8) . . ? O9 N1 C9 119.2(7) . . ? O10' N1' O9' 109.5(17) . . ? O10' N1' C4 123(2) . . ? O9' N1' C4 124.7(18) . . ? O12 N2 O11 122.1(6) . . ? O12 N2 C18 117.4(6) . . ? O11 N2 C18 120.5(6) . . ? O12' N2' O11' 122.9(18) . . ? O12' N2' C23 107.3(15) . . ? O11' N2' C23 129.3(15) . . ? Co2 O1 HW1A 120(3) . . ? Co2 O1 HW1B 117(4) . . ? HW1A O1 HW1B 108(3) . . ? Co1 O2 Co2 101.40(11) . . ? Co1 O2 HW2A 110(3) . . ? Co2 O2 HW2A 117(3) . . ? Co1 O2 HW2B 125(4) . . ? Co2 O2 HW2B 93(4) . . ? HW2A O2 HW2B 110(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.086 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.090