# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_16auga _database_code_depnum_ccdc_archive 'CCDC 794043' #TrackingRef '16auga.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 Cl4 Co4 N10 O19' _chemical_formula_weight 1450.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 18.199(5) _cell_length_b 15.471(5) _cell_length_c 24.134(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 111.657(5) _cell_angle_gamma 90.000(5) _cell_volume 6315(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3596 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 24.87 _exptl_crystal_description prism _exptl_crystal_colour brwon _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 1.276 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 17899 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.50 _reflns_number_total 6508 _reflns_number_gt 4691 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.1419P)^2^+31.2855P] 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 6508 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.2454 _refine_ls_wR_factor_gt 0.2136 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.004 _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 C1 C -0.1278(4) -0.2315(4) 0.5362(3) 0.0355(13) Uani 1 1 d . . . H1 H -0.1621 -0.1942 0.5085 0.043 Uiso 1 1 calc R . . C2 C -0.1552(4) -0.2797(4) 0.5728(3) 0.0444(15) Uani 1 1 d . . . H2 H -0.2072 -0.2735 0.5702 0.053 Uiso 1 1 calc R . . C3 C -0.1063(4) -0.3362(4) 0.6125(3) 0.0415(15) Uani 1 1 d . . . H3 H -0.1244 -0.3687 0.6373 0.050 Uiso 1 1 calc R . . C4 C -0.0304(4) -0.3447(4) 0.6156(3) 0.0381(14) Uani 1 1 d . . . H4 H 0.0037 -0.3837 0.6421 0.046 Uiso 1 1 calc R . . C5 C -0.0043(4) -0.2943(3) 0.5786(2) 0.0312(12) Uani 1 1 d . . . C6 C 0.0763(3) -0.2950(3) 0.5788(2) 0.0294(12) Uani 1 1 d . . . C7 C 0.1385(4) -0.3454(4) 0.6170(3) 0.0381(14) Uani 1 1 d . . . H7 H 0.1300 -0.3835 0.6439 0.046 Uiso 1 1 calc R . . C8 C 0.2123(4) -0.3377(4) 0.6139(3) 0.0418(15) Uani 1 1 d . . . H8 H 0.2545 -0.3698 0.6392 0.050 Uiso 1 1 calc R . . C9 C 0.2234(4) -0.2820(4) 0.5731(3) 0.0415(14) Uani 1 1 d . . . H9 H 0.2728 -0.2763 0.5704 0.050 Uiso 1 1 calc R . . C10 C 0.1596(4) -0.2350(4) 0.5363(3) 0.0372(13) Uani 1 1 d . . . H10 H 0.1669 -0.1978 0.5085 0.045 Uiso 1 1 calc R . . C11 C 0.2388(4) -0.0542(4) 0.5949(2) 0.0337(12) Uani 1 1 d . . . H11 H 0.2065 -0.0645 0.6163 0.040 Uiso 1 1 calc R . . C12 C 0.3193(4) -0.0702(4) 0.6222(3) 0.0337(12) Uani 1 1 d . . . H12 H 0.3405 -0.0910 0.6611 0.040 Uiso 1 1 calc R . . C13 C 0.3675(3) -0.0545(4) 0.5899(3) 0.0329(12) Uani 1 1 d . . . H13 H 0.4216 -0.0646 0.6067 0.040 Uiso 1 1 calc R . . C14 C 0.3332(4) -0.0236(4) 0.5327(3) 0.0339(12) Uani 1 1 d . . . H14 H 0.3641 -0.0132 0.5102 0.041 Uiso 1 1 calc R . . C15 C 0.2532(3) -0.0081(3) 0.5087(3) 0.0284(11) Uani 1 1 d . . . C16 C 0.2119(3) 0.0280(3) 0.4474(2) 0.0288(11) Uani 1 1 d . . . C17 C 0.2514(4) 0.0539(4) 0.4109(3) 0.0376(13) Uani 1 1 d . . . H17 H 0.3062 0.0507 0.4243 0.045 Uiso 1 1 calc R . . C18 C 0.2088(4) 0.0844(4) 0.3545(3) 0.0425(15) Uani 1 1 d . . . H18 H 0.2344 0.1017 0.3294 0.051 Uiso 1 1 calc R . . C19 C 0.1275(4) 0.0889(4) 0.3359(3) 0.0416(15) Uani 1 1 d . . . H19 H 0.0973 0.1081 0.2977 0.050 Uiso 1 1 calc R . . C20 C 0.0916(4) 0.0646(4) 0.3748(2) 0.0344(13) Uani 1 1 d . . . H20 H 0.0369 0.0686 0.3622 0.041 Uiso 1 1 calc R . . C21 C 0.0343(5) -0.1446(4) 0.3925(3) 0.0428(16) Uani 1 1 d . . . H21A H 0.0808 -0.1379 0.3822 0.051 Uiso 1 1 calc R . . H21B H -0.0089 -0.1122 0.3641 0.051 Uiso 1 1 calc R . . C22 C 0.0127(5) -0.2384(4) 0.3919(3) 0.0473(17) Uani 1 1 d . . . H22A H -0.0128 -0.2580 0.3511 0.057 Uiso 1 1 calc R . . H22B H 0.0601 -0.2726 0.4106 0.057 Uiso 1 1 calc R . . C23 C -0.1255(4) -0.2291(4) 0.3906(3) 0.0467(16) Uani 1 1 d . . . H23A H -0.1592 -0.2625 0.4057 0.056 Uiso 1 1 calc R . . H23B H -0.1388 -0.2439 0.3490 0.056 Uiso 1 1 calc R . . C24 C -0.1397(4) -0.1319(4) 0.3963(3) 0.0433(15) Uani 1 1 d . . . H24A H -0.1195 -0.0984 0.3710 0.052 Uiso 1 1 calc R . . H24B H -0.1957 -0.1201 0.3847 0.052 Uiso 1 1 calc R . . N1 N 0.0875(3) -0.2407(3) 0.53883(19) 0.0288(10) Uani 1 1 d . . . N2 N -0.0522(3) -0.2378(3) 0.54015(19) 0.0277(10) Uani 1 1 d . . . N3 N 0.2060(3) -0.0247(3) 0.5394(2) 0.0284(10) Uani 1 1 d . . . N4 N 0.1326(3) 0.0350(3) 0.4304(2) 0.0296(10) Uani 1 1 d . . . N5 N -0.0420(3) -0.2498(3) 0.4247(2) 0.0365(11) Uani 1 1 d . . . O1 O -0.0249(2) 0.0713(2) 0.45676(15) 0.0232(7) Uani 1 1 d . . . O2 O 0.0501(2) -0.1148(2) 0.45182(16) 0.0302(8) Uani 1 1 d . . . O3 O -0.0988(2) -0.1106(2) 0.45699(16) 0.0311(8) Uani 1 1 d . . . Co1 Co -0.00472(4) -0.17212(4) 0.49291(3) 0.0251(2) Uani 1 1 d . . . Co2 Co 0.08285(4) -0.00036(4) 0.49340(3) 0.0234(2) Uani 1 1 d . . . O2W O 0.0704(5) -0.2665(4) 0.7436(3) 0.094(2) Uani 1 1 d . . . O4W O 0.2915(5) -0.1754(5) 0.7482(3) 0.098(2) Uani 1 1 d . . . O3W O 0.3116(8) -0.4327(6) 0.7528(4) 0.161(5) Uani 1 1 d . . . O5W O 0.3206(5) 0.0979(6) 0.7250(3) 0.105(3) Uani 1 1 d . . . Cl2 Cl 0.11835(10) -0.10671(12) 0.68008(7) 0.0489(4) Uani 1 1 d . . . Cl1 Cl -0.04108(16) -0.44513(17) 0.44798(13) 0.0849(7) Uani 1 1 d . . . O7W O 0.4112(2) -0.0439(2) 0.81386(17) 0.0317(8) Uani 1 1 d . . . O1W O 0.4062(4) -0.2836(4) 0.7207(2) 0.0651(15) Uani 1 1 d . . . O6W O 0.5000 -0.1191(9) 0.7500 0.105(4) Uani 1 2 d S . . H01 H -0.033(4) -0.312(5) 0.434(3) 0.049(19) Uiso 1 1 d . . . H02 H -0.050(6) 0.091(6) 0.413(4) 0.09(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(3) 0.033(3) 0.045(3) -0.001(2) 0.021(3) 0.000(2) C2 0.049(4) 0.035(3) 0.060(4) -0.010(3) 0.034(3) -0.015(3) C3 0.064(4) 0.031(3) 0.043(3) 0.000(2) 0.035(3) -0.011(3) C4 0.059(4) 0.027(3) 0.032(3) 0.004(2) 0.020(3) -0.006(3) C5 0.040(3) 0.025(3) 0.030(3) -0.004(2) 0.016(2) -0.001(2) C6 0.040(3) 0.020(2) 0.025(3) 0.0001(19) 0.010(2) 0.001(2) C7 0.053(4) 0.024(3) 0.037(3) 0.003(2) 0.015(3) 0.004(3) C8 0.040(3) 0.032(3) 0.042(3) 0.003(3) 0.003(3) 0.015(3) C9 0.041(3) 0.032(3) 0.055(4) -0.002(3) 0.022(3) 0.005(3) C10 0.050(4) 0.029(3) 0.040(3) 0.002(2) 0.024(3) 0.007(3) C11 0.033(3) 0.036(3) 0.032(3) 0.002(2) 0.012(2) 0.003(2) C12 0.035(3) 0.030(3) 0.033(3) 0.002(2) 0.010(2) -0.001(2) C13 0.020(3) 0.032(3) 0.046(3) -0.002(2) 0.012(2) 0.001(2) C14 0.032(3) 0.032(3) 0.045(3) -0.003(2) 0.022(3) -0.002(2) C15 0.032(3) 0.020(2) 0.038(3) -0.001(2) 0.018(2) 0.001(2) C16 0.034(3) 0.024(3) 0.035(3) 0.000(2) 0.021(2) 0.004(2) C17 0.043(3) 0.034(3) 0.049(3) 0.001(3) 0.032(3) 0.003(3) C18 0.059(4) 0.042(3) 0.041(3) 0.006(3) 0.035(3) 0.004(3) C19 0.055(4) 0.040(3) 0.035(3) 0.008(3) 0.024(3) 0.008(3) C20 0.041(3) 0.035(3) 0.032(3) 0.008(2) 0.018(3) 0.009(3) C21 0.071(5) 0.037(3) 0.032(3) -0.005(2) 0.033(3) -0.005(3) C22 0.075(5) 0.036(3) 0.039(3) -0.013(3) 0.032(3) -0.005(3) C23 0.049(4) 0.042(4) 0.037(3) -0.016(3) 0.002(3) -0.003(3) C24 0.049(4) 0.037(3) 0.028(3) -0.002(2) -0.004(3) 0.006(3) N1 0.040(3) 0.022(2) 0.028(2) -0.0002(17) 0.017(2) 0.0034(19) N2 0.036(3) 0.020(2) 0.030(2) -0.0016(17) 0.014(2) -0.0032(18) N3 0.031(2) 0.025(2) 0.032(2) 0.0042(18) 0.015(2) 0.0030(19) N4 0.036(3) 0.027(2) 0.029(2) 0.0019(18) 0.016(2) 0.001(2) N5 0.053(3) 0.025(2) 0.033(3) -0.0013(19) 0.018(2) 0.001(2) O1 0.0286(18) 0.0194(17) 0.0224(17) 0.0014(13) 0.0104(15) 0.0006(14) O2 0.047(2) 0.0229(18) 0.0269(18) -0.0008(14) 0.0204(17) -0.0002(17) O3 0.035(2) 0.0277(19) 0.0271(19) -0.0011(15) 0.0074(17) 0.0015(16) Co1 0.0333(4) 0.0193(4) 0.0242(4) 0.0006(2) 0.0125(3) 0.0007(3) Co2 0.0272(4) 0.0216(4) 0.0245(4) 0.0025(2) 0.0130(3) 0.0018(3) O2W 0.142(7) 0.067(4) 0.091(5) -0.010(3) 0.066(5) -0.016(4) O4W 0.120(6) 0.103(5) 0.072(4) 0.021(4) 0.037(4) 0.030(5) O3W 0.280(14) 0.109(7) 0.073(5) 0.006(5) 0.040(7) 0.071(8) O5W 0.117(7) 0.128(7) 0.070(4) -0.009(4) 0.034(4) -0.003(5) Cl2 0.0466(9) 0.0676(11) 0.0343(8) 0.0053(7) 0.0171(7) -0.0050(8) Cl1 0.0795(16) 0.0814(16) 0.1064(19) 0.0035(14) 0.0492(15) -0.0101(13) O7W 0.029(2) 0.030(2) 0.035(2) -0.0020(16) 0.0105(17) 0.0028(16) O1W 0.101(4) 0.069(3) 0.050(3) -0.009(3) 0.056(3) 0.009(3) O6W 0.042(5) 0.186(12) 0.076(6) 0.000 0.009(5) 0.000 _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 C1 N2 1.347(7) . ? C1 C2 1.381(9) . ? C1 H1 0.9300 . ? C2 C3 1.358(10) . ? C2 H2 0.9300 . ? C3 C4 1.361(9) . ? C3 H3 0.9300 . ? C4 C5 1.393(8) . ? C4 H4 0.9300 . ? C5 N2 1.338(7) . ? C5 C6 1.465(8) . ? C6 N1 1.350(7) . ? C6 C7 1.403(8) . ? C7 C8 1.378(10) . ? C7 H7 0.9300 . ? C8 C9 1.377(9) . ? C8 H8 0.9300 . ? C9 C10 1.381(9) . ? C9 H9 0.9300 . ? C10 N1 1.338(8) . ? C10 H10 0.9300 . ? C11 N3 1.330(7) . ? C11 C12 1.389(8) . ? C11 H11 0.9300 . ? C12 C13 1.392(8) . ? C12 H12 0.9300 . ? C13 C14 1.374(8) . ? C13 H13 0.9300 . ? C14 C15 1.375(8) . ? C14 H14 0.9300 . ? C15 N3 1.348(7) . ? C15 C16 1.498(8) . ? C16 N4 1.351(7) . ? C16 C17 1.386(8) . ? C17 C18 1.377(9) . ? C17 H17 0.9300 . ? C18 C19 1.381(10) . ? C18 H18 0.9300 . ? C19 C20 1.379(8) . ? C19 H19 0.9300 . ? C20 N4 1.351(7) . ? C20 H20 0.9300 . ? C21 O2 1.429(6) . ? C21 C22 1.502(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N5 1.494(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 N5 1.473(9) . ? C23 C24 1.540(9) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 O3 1.415(7) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? N1 Co1 1.949(5) . ? N2 Co1 1.951(4) . ? N3 Co2 2.136(5) . ? N4 Co2 2.110(5) . ? N5 Co1 1.946(5) . ? N5 H01 1.00(7) . ? O1 Co1 1.928(3) 5_556 ? O1 Co2 2.139(4) . ? O1 Co2 2.168(3) 5_556 ? O1 H02 1.04(10) . ? O2 Co1 1.870(4) . ? O2 Co2 2.014(4) . ? O3 Co1 1.870(4) . ? O3 Co2 2.051(4) 5_556 ? Co1 O1 1.928(3) 5_556 ? Co2 O3 2.051(4) 5_556 ? Co2 O1 2.168(3) 5_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C2 121.1(6) . . ? N2 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 120.1(6) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 119.3(6) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.2(6) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N2 C5 C4 121.4(6) . . ? N2 C5 C6 113.7(5) . . ? C4 C5 C6 124.8(5) . . ? N1 C6 C7 121.1(6) . . ? N1 C6 C5 114.1(5) . . ? C7 C6 C5 124.8(5) . . ? C8 C7 C6 118.9(6) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C9 119.7(6) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 118.6(6) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N1 C10 C9 122.7(6) . . ? N1 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N3 C11 C12 122.8(5) . . ? N3 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C11 C12 C13 118.4(5) . . ? C11 C12 H12 120.8 . . ? C13 C12 H12 120.8 . . ? C14 C13 C12 118.5(5) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 120.1(5) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? N3 C15 C14 121.7(5) . . ? N3 C15 C16 115.1(5) . . ? C14 C15 C16 123.2(5) . . ? N4 C16 C17 121.9(5) . . ? N4 C16 C15 114.9(5) . . ? C17 C16 C15 123.2(5) . . ? C18 C17 C16 119.5(6) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 118.9(6) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? C20 C19 C18 118.9(6) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? N4 C20 C19 122.8(6) . . ? N4 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? O2 C21 C22 106.0(5) . . ? O2 C21 H21A 110.5 . . ? C22 C21 H21A 110.5 . . ? O2 C21 H21B 110.5 . . ? C22 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? N5 C22 C21 109.5(5) . . ? N5 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? N5 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? N5 C23 C24 109.6(5) . . ? N5 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? N5 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? O3 C24 C23 106.2(5) . . ? O3 C24 H24A 110.5 . . ? C23 C24 H24A 110.5 . . ? O3 C24 H24B 110.5 . . ? C23 C24 H24B 110.5 . . ? H24A C24 H24B 108.7 . . ? C10 N1 C6 118.9(5) . . ? C10 N1 Co1 126.2(4) . . ? C6 N1 Co1 114.8(4) . . ? C5 N2 C1 118.9(5) . . ? C5 N2 Co1 115.5(4) . . ? C1 N2 Co1 125.6(4) . . ? C11 N3 C15 118.5(5) . . ? C11 N3 Co2 125.4(4) . . ? C15 N3 Co2 116.1(4) . . ? C20 N4 C16 117.8(5) . . ? C20 N4 Co2 125.2(4) . . ? C16 N4 Co2 117.0(4) . . ? C23 N5 C22 115.4(5) . . ? C23 N5 Co1 107.7(4) . . ? C22 N5 Co1 106.4(4) . . ? C23 N5 H01 113(4) . . ? C22 N5 H01 99(4) . . ? Co1 N5 H01 115(4) . . ? Co1 O1 Co2 99.12(16) 5_556 . ? Co1 O1 Co2 98.05(15) 5_556 5_556 ? Co2 O1 Co2 93.89(13) . 5_556 ? Co1 O1 H02 109(5) 5_556 . ? Co2 O1 H02 125(5) . . ? Co2 O1 H02 126(5) 5_556 . ? C21 O2 Co1 115.5(4) . . ? C21 O2 Co2 134.1(3) . . ? Co1 O2 Co2 105.67(17) . . ? C24 O3 Co1 113.7(4) . . ? C24 O3 Co2 134.9(3) . 5_556 ? Co1 O3 Co2 104.32(17) . 5_556 ? O2 Co1 O3 95.14(17) . . ? O2 Co1 O1 82.58(15) . 5_556 ? O3 Co1 O1 82.82(16) . 5_556 ? O2 Co1 N5 86.10(19) . . ? O3 Co1 N5 87.1(2) . . ? O1 Co1 N5 164.07(18) 5_556 . ? O2 Co1 N1 92.50(18) . . ? O3 Co1 N1 171.98(18) . . ? O1 Co1 N1 95.78(17) 5_556 . ? N5 Co1 N1 95.9(2) . . ? O2 Co1 N2 174.35(18) . . ? O3 Co1 N2 90.49(19) . . ? O1 Co1 N2 97.72(16) 5_556 . ? N5 Co1 N2 94.6(2) . . ? N1 Co1 N2 81.86(19) . . ? O2 Co2 O3 168.17(16) . 5_556 ? O2 Co2 N4 89.75(16) . . ? O3 Co2 N4 101.39(17) 5_556 . ? O2 Co2 N3 99.45(17) . . ? O3 Co2 N3 87.07(16) 5_556 . ? N4 Co2 N3 76.87(18) . . ? O2 Co2 O1 101.08(15) . . ? O3 Co2 O1 73.66(14) 5_556 . ? N4 Co2 O1 98.01(16) . . ? N3 Co2 O1 158.81(16) . . ? O2 Co2 O1 73.53(14) . 5_556 ? O3 Co2 O1 95.33(14) 5_556 5_556 ? N4 Co2 O1 163.28(16) . 5_556 ? N3 Co2 O1 104.76(15) . 5_556 ? O1 Co2 O1 86.11(14) . 5_556 ? 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 N2 C1 C2 C3 -1.7(9) . . . . ? C1 C2 C3 C4 -0.2(9) . . . . ? C2 C3 C4 C5 1.0(9) . . . . ? C3 C4 C5 N2 0.0(8) . . . . ? C3 C4 C5 C6 177.9(5) . . . . ? N2 C5 C6 N1 -2.1(7) . . . . ? C4 C5 C6 N1 179.8(5) . . . . ? N2 C5 C6 C7 177.0(5) . . . . ? C4 C5 C6 C7 -1.0(9) . . . . ? N1 C6 C7 C8 1.3(8) . . . . ? C5 C6 C7 C8 -177.8(5) . . . . ? C6 C7 C8 C9 -1.1(9) . . . . ? C7 C8 C9 C10 0.2(9) . . . . ? C8 C9 C10 N1 0.5(9) . . . . ? N3 C11 C12 C13 0.2(9) . . . . ? C11 C12 C13 C14 0.2(8) . . . . ? C12 C13 C14 C15 0.7(8) . . . . ? C13 C14 C15 N3 -1.9(8) . . . . ? C13 C14 C15 C16 178.1(5) . . . . ? N3 C15 C16 N4 -3.0(7) . . . . ? C14 C15 C16 N4 177.0(5) . . . . ? N3 C15 C16 C17 176.0(5) . . . . ? C14 C15 C16 C17 -4.0(8) . . . . ? N4 C16 C17 C18 -2.7(9) . . . . ? C15 C16 C17 C18 178.4(5) . . . . ? C16 C17 C18 C19 0.4(9) . . . . ? C17 C18 C19 C20 1.4(9) . . . . ? C18 C19 C20 N4 -1.0(9) . . . . ? O2 C21 C22 N5 43.4(7) . . . . ? N5 C23 C24 O3 -43.1(7) . . . . ? C9 C10 N1 C6 -0.3(8) . . . . ? C9 C10 N1 Co1 175.7(4) . . . . ? C7 C6 N1 C10 -0.6(8) . . . . ? C5 C6 N1 C10 178.6(5) . . . . ? C7 C6 N1 Co1 -177.0(4) . . . . ? C5 C6 N1 Co1 2.2(6) . . . . ? C4 C5 N2 C1 -1.8(8) . . . . ? C6 C5 N2 C1 -179.9(5) . . . . ? C4 C5 N2 Co1 179.2(4) . . . . ? C6 C5 N2 Co1 1.1(6) . . . . ? C2 C1 N2 C5 2.6(8) . . . . ? C2 C1 N2 Co1 -178.5(4) . . . . ? C12 C11 N3 C15 -1.4(8) . . . . ? C12 C11 N3 Co2 178.9(4) . . . . ? C14 C15 N3 C11 2.3(8) . . . . ? C16 C15 N3 C11 -177.8(5) . . . . ? C14 C15 N3 Co2 -178.0(4) . . . . ? C16 C15 N3 Co2 2.0(6) . . . . ? C19 C20 N4 C16 -1.2(9) . . . . ? C19 C20 N4 Co2 178.3(4) . . . . ? C17 C16 N4 C20 3.1(8) . . . . ? C15 C16 N4 C20 -177.9(5) . . . . ? C17 C16 N4 Co2 -176.4(4) . . . . ? C15 C16 N4 Co2 2.6(6) . . . . ? C24 C23 N5 C22 -86.9(6) . . . . ? C24 C23 N5 Co1 31.8(6) . . . . ? C21 C22 N5 C23 80.8(7) . . . . ? C21 C22 N5 Co1 -38.5(6) . . . . ? C22 C21 O2 Co1 -28.8(7) . . . . ? C22 C21 O2 Co2 179.9(4) . . . . ? C23 C24 O3 Co1 34.7(6) . . . . ? C23 C24 O3 Co2 179.8(4) . . . 5_556 ? C21 O2 Co1 O3 -80.4(4) . . . . ? Co2 O2 Co1 O3 78.61(19) . . . . ? C21 O2 Co1 O1 -162.5(4) . . . 5_556 ? Co2 O2 Co1 O1 -3.44(17) . . . 5_556 ? C21 O2 Co1 N5 6.3(4) . . . . ? Co2 O2 Co1 N5 165.3(2) . . . . ? C21 O2 Co1 N1 102.0(4) . . . . ? Co2 O2 Co1 N1 -98.9(2) . . . . ? C21 O2 Co1 N2 104.1(17) . . . . ? Co2 O2 Co1 N2 -96.9(17) . . . . ? C24 O3 Co1 O2 71.1(4) . . . . ? Co2 O3 Co1 O2 -84.19(18) 5_556 . . . ? C24 O3 Co1 O1 152.9(4) . . . 5_556 ? Co2 O3 Co1 O1 -2.36(16) 5_556 . . 5_556 ? C24 O3 Co1 N5 -14.7(4) . . . . ? Co2 O3 Co1 N5 -170.0(2) 5_556 . . . ? C24 O3 Co1 N1 -126.6(12) . . . . ? Co2 O3 Co1 N1 78.1(13) 5_556 . . . ? C24 O3 Co1 N2 -109.3(4) . . . . ? Co2 O3 Co1 N2 95.37(19) 5_556 . . . ? C23 N5 Co1 O2 -106.1(4) . . . . ? C22 N5 Co1 O2 18.2(4) . . . . ? C23 N5 Co1 O3 -10.8(4) . . . . ? C22 N5 Co1 O3 113.6(4) . . . . ? C23 N5 Co1 O1 -61.4(9) . . . 5_556 ? C22 N5 Co1 O1 62.9(9) . . . 5_556 ? C23 N5 Co1 N1 161.8(4) . . . . ? C22 N5 Co1 N1 -73.9(4) . . . . ? C23 N5 Co1 N2 79.5(4) . . . . ? C22 N5 Co1 N2 -156.2(4) . . . . ? C10 N1 Co1 O2 2.4(5) . . . . ? C6 N1 Co1 O2 178.5(4) . . . . ? C10 N1 Co1 O3 -159.9(11) . . . . ? C6 N1 Co1 O3 16.2(15) . . . . ? C10 N1 Co1 O1 -80.4(5) . . . 5_556 ? C6 N1 Co1 O1 95.8(4) . . . 5_556 ? C10 N1 Co1 N5 88.8(5) . . . . ? C6 N1 Co1 N5 -95.1(4) . . . . ? C10 N1 Co1 N2 -177.4(5) . . . . ? C6 N1 Co1 N2 -1.2(4) . . . . ? C5 N2 Co1 O2 -2.1(19) . . . . ? C1 N2 Co1 O2 179(100) . . . . ? C5 N2 Co1 O3 -177.6(4) . . . . ? C1 N2 Co1 O3 3.5(5) . . . . ? C5 N2 Co1 O1 -94.8(4) . . . 5_556 ? C1 N2 Co1 O1 86.3(5) . . . 5_556 ? C5 N2 Co1 N5 95.3(4) . . . . ? C1 N2 Co1 N5 -83.6(5) . . . . ? C5 N2 Co1 N1 0.0(4) . . . . ? C1 N2 Co1 N1 -178.9(5) . . . . ? C21 O2 Co2 O3 136.3(8) . . . 5_556 ? Co1 O2 Co2 O3 -16.9(8) . . . 5_556 ? C21 O2 Co2 N4 -24.2(6) . . . . ? Co1 O2 Co2 N4 -177.5(2) . . . . ? C21 O2 Co2 N3 -100.9(6) . . . . ? Co1 O2 Co2 N3 105.9(2) . . . . ? C21 O2 Co2 O1 73.9(6) . . . . ? Co1 O2 Co2 O1 -79.37(19) . . . . ? C21 O2 Co2 O1 156.4(6) . . . 5_556 ? Co1 O2 Co2 O1 3.16(16) . . . 5_556 ? C20 N4 Co2 O2 79.5(5) . . . . ? C16 N4 Co2 O2 -101.0(4) . . . . ? C20 N4 Co2 O3 -96.5(5) . . . 5_556 ? C16 N4 Co2 O3 83.0(4) . . . 5_556 ? C20 N4 Co2 N3 179.3(5) . . . . ? C16 N4 Co2 N3 -1.2(4) . . . . ? C20 N4 Co2 O1 -21.6(5) . . . . ? C16 N4 Co2 O1 157.9(4) . . . . ? C20 N4 Co2 O1 81.7(7) . . . 5_556 ? C16 N4 Co2 O1 -98.8(6) . . . 5_556 ? C11 N3 Co2 O2 -93.3(5) . . . . ? C15 N3 Co2 O2 87.0(4) . . . . ? C11 N3 Co2 O3 76.8(5) . . . 5_556 ? C15 N3 Co2 O3 -102.9(4) . . . 5_556 ? C11 N3 Co2 N4 179.2(5) . . . . ? C15 N3 Co2 N4 -0.5(4) . . . . ? C11 N3 Co2 O1 101.1(6) . . . . ? C15 N3 Co2 O1 -78.6(6) . . . . ? C11 N3 Co2 O1 -18.0(5) . . . 5_556 ? C15 N3 Co2 O1 162.3(4) . . . 5_556 ? Co1 O1 Co2 O2 171.17(14) 5_556 . . . ? Co2 O1 Co2 O2 72.37(15) 5_556 . . . ? Co1 O1 Co2 O3 2.09(14) 5_556 . . 5_556 ? Co2 O1 Co2 O3 -96.71(15) 5_556 . . 5_556 ? Co1 O1 Co2 N4 -97.50(17) 5_556 . . . ? Co2 O1 Co2 N4 163.70(16) 5_556 . . . ? Co1 O1 Co2 N3 -23.3(5) 5_556 . . . ? Co2 O1 Co2 N3 -122.1(4) 5_556 . . . ? Co1 O1 Co2 O1 98.80(16) 5_556 . . 5_556 ? Co2 O1 Co2 O1 0.0 5_556 . . 5_556 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.068 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.156 data_18juld _database_code_depnum_ccdc_archive 'CCDC 794044' #TrackingRef '18juld.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H52 Cl4 Co4 N10 O20' _chemical_formula_weight 1562.60 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' Co Co 0.3494 0.9721 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.483(2) _cell_length_b 13.791(2) _cell_length_c 15.873(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.667(2) _cell_angle_gamma 90.00 _cell_volume 3341.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4001 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 25.89 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 1.214 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD 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 17660 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6212 _reflns_number_gt 4910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _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^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6212 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1248 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Co2 Co 0.04363(3) 0.06354(3) 0.85538(3) 0.01368(14) Uani 1 1 d . . . Co1 Co -0.02286(3) 0.10669(3) 1.02406(3) 0.01399(14) Uani 1 1 d . . . O2 O 0.10635(14) -0.04180(16) 0.90908(14) 0.0161(5) Uani 1 1 d . . . O1 O 0.06565(14) 0.14678(17) 0.94951(14) 0.0162(5) Uani 1 1 d . . . O01 O -0.04697(15) 0.01513(17) 0.91376(14) 0.0146(5) Uani 1 1 d . . . C12 C -0.0366(2) 0.0389(3) 0.6862(2) 0.0162(7) Uani 1 1 d . . . N1 N 0.1540(2) 0.1090(2) 0.8282(2) 0.0185(7) Uani 1 1 d . . . N4 N -0.02685(18) 0.1632(2) 0.78829(17) 0.0155(6) Uani 1 1 d . . . N5 N 0.01193(17) -0.0122(2) 0.75074(17) 0.0146(6) Uani 1 1 d . . . C4 C -0.0642(2) 0.0014(3) 0.6042(2) 0.0183(7) Uani 1 1 d . . . N2 N 0.02802(18) 0.2239(2) 1.10495(17) 0.0167(6) Uani 1 1 d . . . N3 N -0.11830(18) 0.2185(2) 0.98711(18) 0.0185(6) Uani 1 1 d . . . C6 C -0.1377(2) 0.1538(3) 0.5618(2) 0.0215(8) Uani 1 1 d . . . H6 H -0.1712 0.1917 0.5201 0.026 Uiso 1 1 calc R . . C22 C 0.1037(2) 0.2265(3) 1.1587(2) 0.0200(8) Uani 1 1 d . . . H22 H 0.1346 0.1690 1.1715 0.024 Uiso 1 1 calc R . . C21 C 0.1389(2) 0.3137(3) 1.1971(2) 0.0227(8) Uani 1 1 d . . . H21 H 0.1931 0.3138 1.2328 0.027 Uiso 1 1 calc R . . C20 C 0.0922(2) 0.3982(3) 1.1810(2) 0.0248(9) Uani 1 1 d . . . H20 H 0.1138 0.4557 1.2071 0.030 Uiso 1 1 calc R . . C19 C 0.0120(2) 0.3977(2) 1.1253(2) 0.0198(8) Uani 1 1 d . . . C28 C 0.1973(2) -0.0269(3) 0.9261(2) 0.0231(8) Uani 1 1 d . . . H28A H 0.2281 -0.0885 0.9314 0.028 Uiso 1 1 calc R . . H28B H 0.2138 0.0091 0.9789 0.028 Uiso 1 1 calc R . . C17 C -0.1169(2) 0.4788(3) 1.0482(2) 0.0270(9) Uani 1 1 d . . . H17 H -0.1506 0.5346 1.0368 0.032 Uiso 1 1 calc R . . C25 C 0.1478(2) 0.1936(3) 0.9617(2) 0.0231(8) Uani 1 1 d . . . H25A H 0.1905 0.1563 1.0002 0.028 Uiso 1 1 calc R . . H25B H 0.1432 0.2575 0.9861 0.028 Uiso 1 1 calc R . . C1 C 0.0342(2) -0.1030(2) 0.7346(2) 0.0183(8) Uani 1 1 d . . . H1 H 0.0681 -0.1386 0.7777 0.022 Uiso 1 1 calc R . . C7 C -0.1110(2) 0.1931(3) 0.6463(2) 0.0188(8) Uani 1 1 d . . . C13 C -0.1913(2) 0.2137(3) 0.9299(2) 0.0226(8) Uani 1 1 d . . . H13 H -0.2073 0.1545 0.9038 0.027 Uiso 1 1 calc R . . C8 C -0.1339(2) 0.2851(3) 0.6740(2) 0.0218(8) Uani 1 1 d . . . H8 H -0.1704 0.3259 0.6372 0.026 Uiso 1 1 calc R . . C18 C -0.0418(3) 0.4820(3) 1.1048(2) 0.0282(9) Uani 1 1 d . . . H18 H -0.0242 0.5405 1.1314 0.034 Uiso 1 1 calc R . . C16 C -0.1454(2) 0.3898(3) 1.0053(2) 0.0211(8) Uani 1 1 d . . . C11 C -0.0591(2) 0.1350(3) 0.7071(2) 0.0162(7) Uani 1 1 d . . . C24 C -0.0960(2) 0.3052(3) 1.0248(2) 0.0177(7) Uani 1 1 d . . . C26 C 0.1754(3) 0.2018(3) 0.8748(2) 0.0263(9) Uani 1 1 d . . . H26A H 0.1446 0.2550 0.8429 0.032 Uiso 1 1 calc R . . H26B H 0.2378 0.2143 0.8814 0.032 Uiso 1 1 calc R . . C3 C -0.0401(2) -0.0939(3) 0.5900(2) 0.0211(8) Uani 1 1 d . . . H3 H -0.0567 -0.1220 0.5364 0.025 Uiso 1 1 calc R . . C23 C -0.0169(2) 0.3082(3) 1.0864(2) 0.0177(7) Uani 1 1 d . . . C10 C -0.0475(2) 0.2525(3) 0.8117(2) 0.0208(8) Uani 1 1 d . . . H10 H -0.0252 0.2744 0.8664 0.025 Uiso 1 1 calc R . . C27 C 0.2197(2) 0.0308(3) 0.8506(2) 0.0244(8) Uani 1 1 d . . . H27A H 0.2777 0.0587 0.8654 0.029 Uiso 1 1 calc R . . H27B H 0.2195 -0.0118 0.8019 0.029 Uiso 1 1 calc R . . C2 C 0.0080(2) -0.1461(3) 0.6546(2) 0.0206(8) Uani 1 1 d . . . H2 H 0.0232 -0.2100 0.6455 0.025 Uiso 1 1 calc R . . C5 C -0.1152(2) 0.0633(3) 0.5420(2) 0.0206(8) Uani 1 1 d . . . H5 H -0.1330 0.0404 0.4867 0.025 Uiso 1 1 calc R . . C9 C -0.1021(2) 0.3135(3) 0.7554(2) 0.0227(8) Uani 1 1 d . . . H9 H -0.1167 0.3743 0.7741 0.027 Uiso 1 1 calc R . . C14 C -0.2451(2) 0.2945(3) 0.9073(2) 0.0268(9) Uani 1 1 d . . . H14 H -0.2963 0.2883 0.8675 0.032 Uiso 1 1 calc R . . C15 C -0.2220(2) 0.3817(3) 0.9438(2) 0.0257(9) Uani 1 1 d . . . H15 H -0.2567 0.4360 0.9282 0.031 Uiso 1 1 calc R . . O4W O 0.38063(17) -0.06241(19) 1.08646(17) 0.0291(6) Uani 1 1 d . . . O7W O -0.05389(17) 0.40449(19) 1.32873(16) 0.0277(6) Uani 1 1 d . . . O1W O -0.10233(18) 0.59410(19) 1.27403(17) 0.0322(7) Uani 1 1 d . . . O6W O -0.08689(17) -0.3220(2) 0.44364(17) 0.0319(7) Uani 1 1 d . . . O2W O 0.26531(18) 0.39462(19) 0.83189(17) 0.0315(7) Uani 1 1 d . . . O5W O 0.17155(17) -0.2701(2) 0.76229(17) 0.0308(6) Uani 1 1 d . . . O3W O 0.41381(18) 0.1092(2) 0.99448(17) 0.0304(6) Uani 1 1 d . . . Cl1 Cl 0.33498(6) 0.62097(6) 0.87107(5) 0.0220(2) Uani 1 1 d . . . Cl2 Cl -0.23459(5) -0.00699(6) 0.80982(6) 0.0244(2) Uani 1 1 d . . . H001 H 0.148(3) 0.119(3) 0.779(3) 0.021(11) Uiso 1 1 d . . . H01 H -0.095(3) 0.003(3) 0.888(2) 0.017(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co2 0.0138(3) 0.0134(3) 0.0133(3) 0.00015(18) 0.00104(18) -0.00077(18) Co1 0.0154(3) 0.0114(3) 0.0151(3) -0.00005(18) 0.00226(18) 0.00019(18) O2 0.0131(12) 0.0151(13) 0.0192(12) 0.0025(10) 0.0001(9) 0.0015(9) O1 0.0163(12) 0.0181(13) 0.0143(12) -0.0017(10) 0.0028(9) -0.0060(10) O01 0.0127(12) 0.0149(13) 0.0152(12) 0.0012(9) -0.0005(10) -0.0018(10) C12 0.0123(16) 0.0202(19) 0.0158(17) 0.0011(14) 0.0018(13) -0.0006(14) N1 0.0194(16) 0.0213(18) 0.0155(17) 0.0005(13) 0.0051(13) -0.0020(12) N4 0.0147(14) 0.0155(16) 0.0165(14) 0.0027(12) 0.0034(11) -0.0033(12) N5 0.0128(14) 0.0151(15) 0.0159(14) -0.0001(12) 0.0020(11) 0.0024(11) C4 0.0142(17) 0.022(2) 0.0189(18) -0.0001(15) 0.0039(14) -0.0040(14) N2 0.0188(15) 0.0148(16) 0.0162(15) -0.0009(12) 0.0022(12) 0.0002(12) N3 0.0182(15) 0.0179(16) 0.0190(15) -0.0013(12) 0.0018(12) -0.0010(12) C6 0.0180(18) 0.029(2) 0.0151(17) 0.0073(15) -0.0029(14) 0.0001(16) C22 0.0197(18) 0.0194(19) 0.0201(19) 0.0035(15) 0.0015(14) 0.0021(15) C21 0.0214(19) 0.024(2) 0.0205(19) -0.0028(16) -0.0026(15) -0.0032(16) C20 0.027(2) 0.019(2) 0.026(2) -0.0053(16) -0.0024(16) -0.0026(16) C19 0.0226(19) 0.0150(19) 0.0209(18) -0.0015(14) 0.0007(15) -0.0006(15) C28 0.0118(17) 0.028(2) 0.028(2) 0.0028(16) 0.0002(14) 0.0032(15) C17 0.030(2) 0.0146(19) 0.035(2) -0.0015(17) 0.0011(17) 0.0041(16) C25 0.0216(19) 0.028(2) 0.0199(19) -0.0073(16) 0.0032(15) -0.0108(16) C1 0.0195(18) 0.0176(19) 0.0186(18) 0.0048(14) 0.0051(14) 0.0035(14) C7 0.0145(17) 0.0181(19) 0.0238(19) 0.0054(15) 0.0034(14) -0.0018(14) C13 0.0209(19) 0.021(2) 0.025(2) -0.0039(15) 0.0020(15) -0.0029(15) C8 0.0182(18) 0.019(2) 0.027(2) 0.0063(15) 0.0011(15) 0.0023(15) C18 0.034(2) 0.017(2) 0.032(2) -0.0083(17) 0.0017(17) -0.0016(17) C16 0.0202(19) 0.020(2) 0.0231(19) -0.0004(15) 0.0040(15) 0.0037(15) C11 0.0151(17) 0.0182(18) 0.0157(17) 0.0006(14) 0.0038(13) -0.0032(14) C24 0.0190(18) 0.0193(19) 0.0162(17) -0.0008(14) 0.0064(14) -0.0006(14) C26 0.027(2) 0.027(2) 0.026(2) -0.0056(16) 0.0082(16) -0.0115(17) C3 0.0206(19) 0.025(2) 0.0178(18) -0.0022(15) 0.0024(15) -0.0031(15) C23 0.0200(18) 0.0194(19) 0.0150(17) -0.0020(14) 0.0068(14) 0.0015(15) C10 0.0245(19) 0.0187(19) 0.0198(18) -0.0029(15) 0.0051(15) -0.0006(15) C27 0.0178(18) 0.027(2) 0.028(2) 0.0037(16) 0.0038(15) 0.0010(16) C2 0.0225(19) 0.0168(19) 0.0225(19) -0.0025(15) 0.0042(15) -0.0001(15) C5 0.0193(18) 0.025(2) 0.0157(18) -0.0002(15) -0.0013(14) -0.0021(15) C9 0.024(2) 0.0138(18) 0.031(2) 0.0010(16) 0.0073(16) 0.0025(15) C14 0.0174(19) 0.030(2) 0.030(2) -0.0043(17) -0.0029(16) 0.0054(16) C15 0.023(2) 0.025(2) 0.027(2) -0.0021(16) 0.0005(16) 0.0073(16) O4W 0.0253(15) 0.0304(16) 0.0306(15) -0.0027(12) 0.0019(12) 0.0002(12) O7W 0.0229(14) 0.0319(16) 0.0275(15) -0.0002(12) 0.0023(11) 0.0035(11) O1W 0.0326(16) 0.0316(16) 0.0318(15) 0.0008(12) 0.0033(12) -0.0058(12) O6W 0.0305(15) 0.0307(16) 0.0321(15) 0.0007(12) -0.0015(12) 0.0042(12) O2W 0.0355(16) 0.0234(16) 0.0334(16) 0.0051(12) -0.0006(13) -0.0066(12) O5W 0.0267(15) 0.0326(16) 0.0322(15) -0.0030(12) 0.0024(12) 0.0078(12) O3W 0.0297(15) 0.0325(17) 0.0289(15) -0.0014(12) 0.0048(12) -0.0012(12) Cl1 0.0240(5) 0.0235(5) 0.0177(4) 0.0011(3) 0.0013(3) -0.0001(4) Cl2 0.0181(4) 0.0199(5) 0.0322(5) -0.0025(4) -0.0044(4) 0.0003(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 Co2 O1 1.870(2) . ? Co2 O2 1.871(2) . ? Co2 O01 1.926(2) . ? Co2 N1 1.936(3) . ? Co2 N5 1.953(3) . ? Co2 N4 1.955(3) . ? Co1 O2 2.015(2) 3_557 ? Co1 O1 2.032(2) . ? Co1 N2 2.131(3) . ? Co1 O01 2.140(2) . ? Co1 O01 2.146(2) 3_557 ? Co1 N3 2.148(3) . ? O2 C28 1.404(4) . ? O2 Co1 2.015(2) 3_557 ? O1 C25 1.410(4) . ? O01 Co1 2.146(2) 3_557 ? O01 H01 0.81(4) . ? C12 N5 1.361(4) . ? C12 C4 1.400(5) . ? C12 C11 1.423(5) . ? N1 C27 1.485(5) . ? N1 C26 1.487(5) . ? N1 H001 0.78(4) . ? N4 C10 1.340(4) . ? N4 C11 1.358(4) . ? N5 C1 1.336(4) . ? C4 C3 1.395(5) . ? C4 C5 1.437(5) . ? N2 C22 1.329(4) . ? N2 C23 1.362(4) . ? N3 C13 1.328(4) . ? N3 C24 1.356(4) . ? C6 C5 1.347(5) . ? C6 C7 1.442(5) . ? C6 H6 0.9300 . ? C22 C21 1.416(5) . ? C22 H22 0.9300 . ? C21 C20 1.373(5) . ? C21 H21 0.9300 . ? C20 C19 1.399(5) . ? C20 H20 0.9300 . ? C19 C23 1.418(5) . ? C19 C18 1.435(5) . ? C28 C27 1.527(5) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C17 C18 1.345(5) . ? C17 C16 1.437(5) . ? C17 H17 0.9300 . ? C25 C26 1.516(5) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C1 C2 1.398(5) . ? C1 H1 0.9300 . ? C7 C11 1.400(5) . ? C7 C8 1.408(5) . ? C13 C14 1.401(5) . ? C13 H13 0.9300 . ? C8 C9 1.361(5) . ? C8 H8 0.9300 . ? C18 H18 0.9300 . ? C16 C24 1.400(5) . ? C16 C15 1.409(5) . ? C24 C23 1.434(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C3 C2 1.366(5) . ? C3 H3 0.9300 . ? C10 C9 1.401(5) . ? C10 H10 0.9300 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C2 H2 0.9300 . ? C5 H5 0.9300 . ? C9 H9 0.9300 . ? C14 C15 1.358(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? 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 Co2 O2 95.83(10) . . ? O1 Co2 O01 83.00(10) . . ? O2 Co2 O01 82.88(10) . . ? O1 Co2 N1 85.96(11) . . ? O2 Co2 N1 86.74(12) . . ? O01 Co2 N1 163.98(12) . . ? O1 Co2 N5 173.58(11) . . ? O2 Co2 N5 90.55(11) . . ? O01 Co2 N5 97.16(11) . . ? N1 Co2 N5 95.10(12) . . ? O1 Co2 N4 90.80(11) . . ? O2 Co2 N4 173.29(11) . . ? O01 Co2 N4 96.93(11) . . ? N1 Co2 N4 94.80(12) . . ? N5 Co2 N4 82.81(11) . . ? O2 Co1 O1 169.36(9) 3_557 . ? O2 Co1 N2 102.97(10) 3_557 . ? O1 Co1 N2 85.83(10) . . ? O2 Co1 O01 97.45(9) 3_557 . ? O1 Co1 O01 74.11(9) . . ? N2 Co1 O01 159.47(10) . . ? O2 Co1 O01 74.24(9) 3_557 3_557 ? O1 Co1 O01 98.27(9) . 3_557 ? N2 Co1 O01 102.11(10) . 3_557 ? O01 Co1 O01 85.39(9) . 3_557 ? O2 Co1 N3 89.41(10) 3_557 . ? O1 Co1 N3 98.40(10) . . ? N2 Co1 N3 77.76(11) . . ? O01 Co1 N3 100.53(10) . . ? O01 Co1 N3 163.27(10) 3_557 . ? C28 O2 Co2 113.7(2) . . ? C28 O2 Co1 132.5(2) . 3_557 ? Co2 O2 Co1 104.77(10) . 3_557 ? C25 O1 Co2 115.5(2) . . ? C25 O1 Co1 136.5(2) . . ? Co2 O1 Co1 104.35(10) . . ? Co2 O01 Co1 98.51(10) . . ? Co2 O01 Co1 98.12(10) . 3_557 ? Co1 O01 Co1 94.61(9) . 3_557 ? Co2 O01 H01 121(3) . . ? Co1 O01 H01 125(3) . . ? Co1 O01 H01 115(3) 3_557 . ? N5 C12 C4 123.5(3) . . ? N5 C12 C11 115.6(3) . . ? C4 C12 C11 120.8(3) . . ? C27 N1 C26 114.8(3) . . ? C27 N1 Co2 107.8(2) . . ? C26 N1 Co2 107.4(2) . . ? C27 N1 H001 109(3) . . ? C26 N1 H001 109(3) . . ? Co2 N1 H001 109(3) . . ? C10 N4 C11 117.3(3) . . ? C10 N4 Co2 129.2(2) . . ? C11 N4 Co2 113.5(2) . . ? C1 N5 C12 118.0(3) . . ? C1 N5 Co2 128.9(2) . . ? C12 N5 Co2 113.0(2) . . ? C3 C4 C12 116.8(3) . . ? C3 C4 C5 125.5(3) . . ? C12 C4 C5 117.8(3) . . ? C22 N2 C23 118.6(3) . . ? C22 N2 Co1 127.2(2) . . ? C23 N2 Co1 113.2(2) . . ? C13 N3 C24 118.1(3) . . ? C13 N3 Co1 128.2(2) . . ? C24 N3 Co1 113.6(2) . . ? C5 C6 C7 121.3(3) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? N2 C22 C21 122.2(3) . . ? N2 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C20 C21 C22 119.3(3) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C19 C23 117.5(3) . . ? C20 C19 C18 124.0(3) . . ? C23 C19 C18 118.5(3) . . ? O2 C28 C27 106.1(3) . . ? O2 C28 H28A 110.5 . . ? C27 C28 H28A 110.5 . . ? O2 C28 H28B 110.5 . . ? C27 C28 H28B 110.5 . . ? H28A C28 H28B 108.7 . . ? C18 C17 C16 120.4(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? O1 C25 C26 107.1(3) . . ? O1 C25 H25A 110.3 . . ? C26 C25 H25A 110.3 . . ? O1 C25 H25B 110.3 . . ? C26 C25 H25B 110.3 . . ? H25A C25 H25B 108.5 . . ? N5 C1 C2 121.8(3) . . ? N5 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C11 C7 C8 116.5(3) . . ? C11 C7 C6 117.9(3) . . ? C8 C7 C6 125.6(3) . . ? N3 C13 C14 122.5(3) . . ? N3 C13 H13 118.8 . . ? C14 C13 H13 118.8 . . ? C9 C8 C7 119.0(3) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C17 C18 C19 121.9(3) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C24 C16 C15 116.9(3) . . ? C24 C16 C17 119.6(3) . . ? C15 C16 C17 123.5(3) . . ? N4 C11 C7 124.6(3) . . ? N4 C11 C12 115.0(3) . . ? C7 C11 C12 120.4(3) . . ? N3 C24 C16 123.2(3) . . ? N3 C24 C23 116.8(3) . . ? C16 C24 C23 120.0(3) . . ? N1 C26 C25 108.4(3) . . ? N1 C26 H26A 110.0 . . ? C25 C26 H26A 110.0 . . ? N1 C26 H26B 110.0 . . ? C25 C26 H26B 110.0 . . ? H26A C26 H26B 108.4 . . ? C2 C3 C4 120.1(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? N2 C23 C19 122.5(3) . . ? N2 C23 C24 118.0(3) . . ? C19 C23 C24 119.5(3) . . ? N4 C10 C9 121.4(3) . . ? N4 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? N1 C27 C28 109.3(3) . . ? N1 C27 H27A 109.8 . . ? C28 C27 H27A 109.8 . . ? N1 C27 H27B 109.8 . . ? C28 C27 H27B 109.8 . . ? H27A C27 H27B 108.3 . . ? C3 C2 C1 119.8(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C6 C5 C4 121.7(3) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C8 C9 C10 121.1(3) . . ? C8 C9 H9 119.5 . . ? C10 C9 H9 119.5 . . ? C15 C14 C13 119.6(3) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.8(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co2 O2 C28 -69.0(2) . . . . ? O01 Co2 O2 C28 -151.1(2) . . . . ? N1 Co2 O2 C28 16.6(2) . . . . ? N5 Co2 O2 C28 111.7(2) . . . . ? N4 Co2 O2 C28 120.1(9) . . . . ? O1 Co2 O2 Co1 82.41(11) . . . 3_557 ? O01 Co2 O2 Co1 0.24(10) . . . 3_557 ? N1 Co2 O2 Co1 168.02(13) . . . 3_557 ? N5 Co2 O2 Co1 -96.91(12) . . . 3_557 ? N4 Co2 O2 Co1 -88.5(9) . . . 3_557 ? O2 Co2 O1 C25 81.2(2) . . . . ? O01 Co2 O1 C25 163.3(2) . . . . ? N1 Co2 O1 C25 -5.1(2) . . . . ? N5 Co2 O1 C25 -104.9(10) . . . . ? N4 Co2 O1 C25 -99.9(2) . . . . ? O2 Co2 O1 Co1 -80.89(11) . . . . ? O01 Co2 O1 Co1 1.17(10) . . . . ? N1 Co2 O1 Co1 -167.19(13) . . . . ? N5 Co2 O1 Co1 93.0(10) . . . . ? N4 Co2 O1 Co1 98.05(12) . . . . ? O2 Co1 O1 C25 -119.0(5) 3_557 . . . ? N2 Co1 O1 C25 27.1(3) . . . . ? O01 Co1 O1 C25 -157.3(3) . . . . ? O01 Co1 O1 C25 -74.5(3) 3_557 . . . ? N3 Co1 O1 C25 104.1(3) . . . . ? O2 Co1 O1 Co2 37.2(5) 3_557 . . . ? N2 Co1 O1 Co2 -176.67(12) . . . . ? O01 Co1 O1 Co2 -1.08(10) . . . . ? O01 Co1 O1 Co2 81.69(11) 3_557 . . . ? N3 Co1 O1 Co2 -99.71(12) . . . . ? O1 Co2 O01 Co1 -1.08(10) . . . . ? O2 Co2 O01 Co1 95.72(10) . . . . ? N1 Co2 O01 Co1 45.7(4) . . . . ? N5 Co2 O01 Co1 -174.62(10) . . . . ? N4 Co2 O01 Co1 -91.04(11) . . . . ? O1 Co2 O01 Co1 -97.02(10) . . . 3_557 ? O2 Co2 O01 Co1 -0.22(9) . . . 3_557 ? N1 Co2 O01 Co1 -50.2(4) . . . 3_557 ? N5 Co2 O01 Co1 89.44(11) . . . 3_557 ? N4 Co2 O01 Co1 173.02(10) . . . 3_557 ? O2 Co1 O01 Co2 -172.35(9) 3_557 . . . ? O1 Co1 O01 Co2 1.03(9) . . . . ? N2 Co1 O01 Co2 13.7(3) . . . . ? O01 Co1 O01 Co2 -98.94(11) 3_557 . . . ? N3 Co1 O01 Co2 96.86(11) . . . . ? O2 Co1 O01 Co1 -73.42(9) 3_557 . . 3_557 ? O1 Co1 O01 Co1 99.97(10) . . . 3_557 ? N2 Co1 O01 Co1 112.6(3) . . . 3_557 ? O01 Co1 O01 Co1 0.0 3_557 . . 3_557 ? N3 Co1 O01 Co1 -164.21(10) . . . 3_557 ? O1 Co2 N1 C27 105.3(2) . . . . ? O2 Co2 N1 C27 9.2(2) . . . . ? O01 Co2 N1 C27 58.8(5) . . . . ? N5 Co2 N1 C27 -81.0(2) . . . . ? N4 Co2 N1 C27 -164.2(2) . . . . ? O1 Co2 N1 C26 -19.0(2) . . . . ? O2 Co2 N1 C26 -115.1(2) . . . . ? O01 Co2 N1 C26 -65.5(5) . . . . ? N5 Co2 N1 C26 154.7(2) . . . . ? N4 Co2 N1 C26 71.5(2) . . . . ? O1 Co2 N4 C10 -1.9(3) . . . . ? O2 Co2 N4 C10 169.1(8) . . . . ? O01 Co2 N4 C10 81.2(3) . . . . ? N1 Co2 N4 C10 -87.9(3) . . . . ? N5 Co2 N4 C10 177.6(3) . . . . ? O1 Co2 N4 C11 178.8(2) . . . . ? O2 Co2 N4 C11 -10.2(10) . . . . ? O01 Co2 N4 C11 -98.1(2) . . . . ? N1 Co2 N4 C11 92.8(2) . . . . ? N5 Co2 N4 C11 -1.7(2) . . . . ? C4 C12 N5 C1 0.0(5) . . . . ? C11 C12 N5 C1 179.5(3) . . . . ? C4 C12 N5 Co2 177.5(3) . . . . ? C11 C12 N5 Co2 -3.0(4) . . . . ? O1 Co2 N5 C1 -175.2(8) . . . . ? O2 Co2 N5 C1 -1.3(3) . . . . ? O01 Co2 N5 C1 -84.2(3) . . . . ? N1 Co2 N5 C1 85.5(3) . . . . ? N4 Co2 N5 C1 179.7(3) . . . . ? O1 Co2 N5 C12 7.7(11) . . . . ? O2 Co2 N5 C12 -178.4(2) . . . . ? O01 Co2 N5 C12 98.7(2) . . . . ? N1 Co2 N5 C12 -91.6(2) . . . . ? N4 Co2 N5 C12 2.6(2) . . . . ? N5 C12 C4 C3 0.4(5) . . . . ? C11 C12 C4 C3 -179.2(3) . . . . ? N5 C12 C4 C5 -180.0(3) . . . . ? C11 C12 C4 C5 0.5(5) . . . . ? O2 Co1 N2 C22 98.4(3) 3_557 . . . ? O1 Co1 N2 C22 -75.6(3) . . . . ? O01 Co1 N2 C22 -87.8(4) . . . . ? O01 Co1 N2 C22 22.0(3) 3_557 . . . ? N3 Co1 N2 C22 -175.1(3) . . . . ? O2 Co1 N2 C23 -93.5(2) 3_557 . . . ? O1 Co1 N2 C23 92.5(2) . . . . ? O01 Co1 N2 C23 80.3(4) . . . . ? O01 Co1 N2 C23 -169.9(2) 3_557 . . . ? N3 Co1 N2 C23 -7.0(2) . . . . ? O2 Co1 N3 C13 -75.0(3) 3_557 . . . ? O1 Co1 N3 C13 97.7(3) . . . . ? N2 Co1 N3 C13 -178.4(3) . . . . ? O01 Co1 N3 C13 22.5(3) . . . . ? O01 Co1 N3 C13 -87.1(4) 3_557 . . . ? O2 Co1 N3 C24 109.2(2) 3_557 . . . ? O1 Co1 N3 C24 -78.0(2) . . . . ? N2 Co1 N3 C24 5.8(2) . . . . ? O01 Co1 N3 C24 -153.3(2) . . . . ? O01 Co1 N3 C24 97.2(4) 3_557 . . . ? C23 N2 C22 C21 0.0(5) . . . . ? Co1 N2 C22 C21 167.5(3) . . . . ? N2 C22 C21 C20 2.4(5) . . . . ? C22 C21 C20 C19 -1.8(6) . . . . ? C21 C20 C19 C23 -1.0(5) . . . . ? C21 C20 C19 C18 179.6(4) . . . . ? Co2 O2 C28 C27 -36.8(3) . . . . ? Co1 O2 C28 C27 -177.9(2) 3_557 . . . ? Co2 O1 C25 C26 27.2(4) . . . . ? Co1 O1 C25 C26 -178.5(2) . . . . ? C12 N5 C1 C2 -1.0(5) . . . . ? Co2 N5 C1 C2 -178.0(2) . . . . ? C5 C6 C7 C11 1.3(5) . . . . ? C5 C6 C7 C8 -177.4(4) . . . . ? C24 N3 C13 C14 0.3(5) . . . . ? Co1 N3 C13 C14 -175.3(3) . . . . ? C11 C7 C8 C9 2.7(5) . . . . ? C6 C7 C8 C9 -178.5(3) . . . . ? C16 C17 C18 C19 -0.7(6) . . . . ? C20 C19 C18 C17 177.4(4) . . . . ? C23 C19 C18 C17 -2.0(6) . . . . ? C18 C17 C16 C24 2.2(6) . . . . ? C18 C17 C16 C15 -178.3(4) . . . . ? C10 N4 C11 C7 0.9(5) . . . . ? Co2 N4 C11 C7 -179.7(3) . . . . ? C10 N4 C11 C12 -178.8(3) . . . . ? Co2 N4 C11 C12 0.6(4) . . . . ? C8 C7 C11 N4 -3.1(5) . . . . ? C6 C7 C11 N4 178.0(3) . . . . ? C8 C7 C11 C12 176.6(3) . . . . ? C6 C7 C11 C12 -2.3(5) . . . . ? N5 C12 C11 N4 1.6(4) . . . . ? C4 C12 C11 N4 -178.9(3) . . . . ? N5 C12 C11 C7 -178.1(3) . . . . ? C4 C12 C11 C7 1.4(5) . . . . ? C13 N3 C24 C16 -1.0(5) . . . . ? Co1 N3 C24 C16 175.2(3) . . . . ? C13 N3 C24 C23 180.0(3) . . . . ? Co1 N3 C24 C23 -3.8(4) . . . . ? C15 C16 C24 N3 0.6(5) . . . . ? C17 C16 C24 N3 -179.8(3) . . . . ? C15 C16 C24 C23 179.5(3) . . . . ? C17 C16 C24 C23 -0.9(5) . . . . ? C27 N1 C26 C25 -82.2(4) . . . . ? Co2 N1 C26 C25 37.8(3) . . . . ? O1 C25 C26 N1 -41.8(4) . . . . ? C12 C4 C3 C2 0.3(5) . . . . ? C5 C4 C3 C2 -179.4(3) . . . . ? C22 N2 C23 C19 -3.0(5) . . . . ? Co1 N2 C23 C19 -172.2(3) . . . . ? C22 N2 C23 C24 176.7(3) . . . . ? Co1 N2 C23 C24 7.5(4) . . . . ? C20 C19 C23 N2 3.5(5) . . . . ? C18 C19 C23 N2 -177.1(3) . . . . ? C20 C19 C23 C24 -176.2(3) . . . . ? C18 C19 C23 C24 3.2(5) . . . . ? N3 C24 C23 N2 -2.5(5) . . . . ? C16 C24 C23 N2 178.5(3) . . . . ? N3 C24 C23 C19 177.2(3) . . . . ? C16 C24 C23 C19 -1.8(5) . . . . ? C11 N4 C10 C9 1.7(5) . . . . ? Co2 N4 C10 C9 -177.6(2) . . . . ? C26 N1 C27 C28 88.7(4) . . . . ? Co2 N1 C27 C28 -31.0(3) . . . . ? O2 C28 C27 N1 43.7(4) . . . . ? C4 C3 C2 C1 -1.2(5) . . . . ? N5 C1 C2 C3 1.6(5) . . . . ? C7 C6 C5 C4 0.6(5) . . . . ? C3 C4 C5 C6 178.1(4) . . . . ? C12 C4 C5 C6 -1.5(5) . . . . ? C7 C8 C9 C10 -0.4(5) . . . . ? N4 C10 C9 C8 -2.0(6) . . . . ? N3 C13 C14 C15 1.0(6) . . . . ? C13 C14 C15 C16 -1.4(6) . . . . ? C24 C16 C15 C14 0.7(5) . . . . ? C17 C16 C15 C14 -178.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.226 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.116