# 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H38 Co5 N26 O14' _chemical_formula_weight 1353.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.275(5) _cell_length_b 12.922(7) _cell_length_c 14.564(8) _cell_angle_alpha 105.060(9) _cell_angle_beta 97.194(10) _cell_angle_gamma 96.254(10) _cell_volume 1653.8(16) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 170 _cell_measurement_theta_min 3.411 _cell_measurement_theta_max 16.997 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 683 _exptl_absorpt_coefficient_mu 1.297 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7128 _exptl_absorpt_correction_T_max 0.7375 _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 ? _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 8095 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5743 _reflns_number_gt 4029 _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^)+(0.1449P)^2^+1.1820P] 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 5743 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.2239 _refine_ls_wR_factor_gt 0.2110 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.1824(8) 0.4784(5) 0.2227(5) 0.0298(15) Uani 1 1 d . . . C2 C 1.2590(7) 0.5907(5) 0.2803(4) 0.0284(14) Uani 1 1 d . . . C3 C 1.3092(7) 0.6636(5) 0.2332(5) 0.0296(15) Uani 1 1 d . . . H3 H 1.2993 0.6438 0.1663 0.036 Uiso 1 1 calc R . . C4 C 1.3754(8) 0.7680(5) 0.2870(5) 0.0322(15) Uani 1 1 d . . . C5 C 1.3904(8) 0.7943(5) 0.3840(5) 0.0336(16) Uani 1 1 d . . . H5 H 1.4333 0.8639 0.4197 0.040 Uiso 1 1 calc R . . C6 C 1.3429(8) 0.7193(5) 0.4320(5) 0.0332(16) Uani 1 1 d . . . C7 C 1.2781(8) 0.6176(5) 0.3800(5) 0.0335(16) Uani 1 1 d . . . H7 H 1.2470 0.5668 0.4111 0.040 Uiso 1 1 calc R . . C8 C 0.6345(8) 0.2491(6) 0.4605(5) 0.0346(16) Uani 1 1 d . . . C9 C 0.4326(8) -0.1505(5) 0.2363(5) 0.0376(17) Uani 1 1 d . . . C10 C 1.0342(8) 0.2889(5) -0.0885(5) 0.0335(16) Uani 1 1 d . . . C11 C 0.9783(9) 0.1198(6) -0.1619(5) 0.0387(17) Uani 1 1 d . . . H11 H 0.9556 0.0550 -0.2107 0.046 Uiso 1 1 calc R . . C12 C 1.3279(7) 0.2144(5) 0.2182(5) 0.0334(16) Uani 1 1 d . . . C13 C 1.2929(8) 0.0530(5) 0.1323(5) 0.0361(17) Uani 1 1 d . . . H13 H 1.3062 -0.0187 0.1076 0.043 Uiso 1 1 calc R . . C14 C 0.7620(8) 0.0278(5) 0.1352(5) 0.0311(15) Uani 1 1 d . . . C15 C 0.8079(7) 0.1932(5) 0.2163(5) 0.0328(16) Uani 1 1 d . . . H15 H 0.8067 0.2587 0.2614 0.039 Uiso 1 1 calc R . . C16 C 0.7438(9) 0.3518(6) 0.0720(5) 0.0411(18) Uani 1 1 d . . . H16 H 0.7358 0.2897 0.0210 0.049 Uiso 1 1 calc R . . C17 C 0.6264(14) 0.4827(10) 0.1738(9) 0.099(4) Uani 1 1 d . . . H17A H 0.7090 0.4850 0.2215 0.148 Uiso 1 1 calc R . . H17B H 0.5374 0.4759 0.2004 0.148 Uiso 1 1 calc R . . H17C H 0.6361 0.5482 0.1542 0.148 Uiso 1 1 calc R . . C18 C 0.4787(11) 0.3429(12) 0.0335(10) 0.107(5) Uani 1 1 d . . . H18A H 0.4407 0.3940 0.0029 0.160 Uiso 1 1 calc R . . H18B H 0.4121 0.3243 0.0741 0.160 Uiso 1 1 calc R . . H18C H 0.4891 0.2788 -0.0148 0.160 Uiso 1 1 calc R . . Co1 Co 1.0000 0.0000 0.0000 0.0233(3) Uani 1 2 d S . . Co2 Co 0.55472(9) 0.08115(6) 0.28209(6) 0.0237(3) Uani 1 1 d . . . Co3 Co 1.04706(10) 0.29721(6) 0.12683(6) 0.0263(3) Uani 1 1 d . . . N1 N 0.8942(6) 0.1805(4) 0.1508(4) 0.0283(12) Uani 1 1 d . . . N2 N 0.8645(6) 0.0732(4) 0.0971(4) 0.0274(12) Uani 1 1 d . . . N3 N 0.7208(6) 0.1001(4) 0.2107(4) 0.0280(12) Uani 1 1 d . . . N4 N 0.6995(9) -0.0800(5) 0.1023(6) 0.072(3) Uani 1 1 d . . . H4A H 0.7271 -0.1222 0.0537 0.087 Uiso 1 1 calc R . . H4B H 0.6329 -0.1047 0.1304 0.087 Uiso 1 1 calc R . . N5 N 0.9876(6) 0.1270(4) -0.0711(4) 0.0310(13) Uani 1 1 d . . . N6 N 1.0227(6) 0.2357(4) -0.0218(4) 0.0305(13) Uani 1 1 d . . . N7 N 1.0059(7) 0.2181(5) -0.1766(4) 0.0403(15) Uani 1 1 d . . . N8 N 1.0691(9) 0.3950(5) -0.0699(5) 0.060(2) Uani 1 1 d . . . H8A H 1.0862 0.4350 -0.0113 0.072 Uiso 1 1 calc R . . H8B H 1.0746 0.4241 -0.1165 0.072 Uiso 1 1 calc R . . N9 N 1.1876(6) 0.0937(4) 0.0971(4) 0.0276(12) Uani 1 1 d . . . N10 N 1.2064(6) 0.2024(4) 0.1511(4) 0.0287(12) Uani 1 1 d . . . N11 N 0.3841(6) 0.1221(4) 0.2087(4) 0.0296(13) Uani 1 1 d . . . N12 N 1.3821(8) 0.3098(5) 0.2850(5) 0.063(2) Uani 1 1 d . . . H12A H 1.4594 0.3143 0.3260 0.075 Uiso 1 1 calc R . . H12B H 1.3392 0.3658 0.2863 0.075 Uiso 1 1 calc R . . N13 N 0.6217(8) 0.3911(6) 0.0916(5) 0.0582(19) Uani 1 1 d . . . O1 O 1.1803(5) 0.4472(4) 0.1333(3) 0.0375(12) Uani 1 1 d . . . O2 O 1.1213(5) 0.4174(3) 0.2657(3) 0.0352(11) Uani 1 1 d . . . O3 O 0.5024(6) -0.0626(4) 0.2936(4) 0.0458(14) Uani 1 1 d . . . O4 O 0.4107(7) -0.1722(4) 0.1487(4) 0.0535(16) Uani 1 1 d . . . O5 O 0.5955(6) 0.1480(4) 0.4193(3) 0.0444(13) Uani 1 1 d . . . O6 O 0.6532(7) 0.3184(4) 0.4171(4) 0.0576(16) Uani 1 1 d . . . O7 O 0.8668(6) 0.3920(4) 0.1168(4) 0.0420(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.038(4) 0.013(3) 0.035(4) 0.002(3) 0.008(3) 0.000(3) C2 0.037(4) 0.019(3) 0.026(3) 0.001(3) 0.009(3) 0.000(3) C3 0.040(4) 0.018(3) 0.026(3) 0.002(3) 0.005(3) -0.006(3) C4 0.042(4) 0.021(3) 0.031(4) 0.005(3) 0.010(3) 0.001(3) C5 0.049(4) 0.015(3) 0.033(4) 0.004(3) 0.008(3) -0.003(3) C6 0.046(4) 0.025(3) 0.024(3) 0.002(3) 0.008(3) -0.004(3) C7 0.041(4) 0.030(4) 0.031(4) 0.011(3) 0.011(3) 0.000(3) C8 0.038(4) 0.035(4) 0.025(3) 0.000(3) 0.005(3) -0.002(3) C9 0.047(4) 0.025(4) 0.046(5) 0.014(3) 0.016(4) 0.007(3) C10 0.043(4) 0.030(4) 0.030(4) 0.012(3) 0.008(3) 0.007(3) C11 0.060(5) 0.035(4) 0.019(3) 0.005(3) 0.005(3) 0.006(3) C12 0.034(4) 0.024(3) 0.038(4) 0.005(3) 0.008(3) -0.003(3) C13 0.039(4) 0.024(3) 0.038(4) -0.005(3) 0.008(3) 0.002(3) C14 0.040(4) 0.019(3) 0.034(4) 0.005(3) 0.015(3) 0.001(3) C15 0.039(4) 0.026(3) 0.030(4) 0.003(3) 0.012(3) -0.003(3) C16 0.047(5) 0.039(4) 0.038(4) 0.010(3) 0.012(4) 0.009(4) C17 0.095(9) 0.090(9) 0.112(10) 0.002(8) 0.046(8) 0.040(7) C18 0.039(6) 0.150(12) 0.128(11) 0.033(10) 0.016(7) 0.012(7) Co1 0.0306(7) 0.0166(6) 0.0216(6) 0.0027(5) 0.0089(5) 0.0005(5) Co2 0.0317(5) 0.0186(4) 0.0204(4) 0.0043(3) 0.0094(3) -0.0017(3) Co3 0.0358(5) 0.0164(4) 0.0251(5) 0.0029(3) 0.0097(4) -0.0013(4) N1 0.039(3) 0.020(3) 0.023(3) 0.000(2) 0.016(2) -0.002(2) N2 0.037(3) 0.015(2) 0.028(3) -0.003(2) 0.018(2) 0.000(2) N3 0.038(3) 0.024(3) 0.023(3) 0.005(2) 0.015(2) 0.001(2) N4 0.086(6) 0.041(4) 0.085(6) -0.001(4) 0.048(5) -0.008(4) N5 0.044(3) 0.023(3) 0.025(3) 0.003(2) 0.014(3) 0.003(2) N6 0.046(3) 0.016(3) 0.029(3) 0.005(2) 0.008(3) -0.001(2) N7 0.062(4) 0.033(3) 0.028(3) 0.009(3) 0.010(3) 0.007(3) N8 0.116(7) 0.028(3) 0.036(4) 0.015(3) 0.008(4) 0.001(4) N9 0.029(3) 0.019(3) 0.029(3) -0.004(2) 0.005(2) 0.002(2) N10 0.039(3) 0.023(3) 0.019(3) -0.002(2) 0.009(2) 0.001(2) N11 0.032(3) 0.028(3) 0.025(3) 0.002(2) 0.005(2) 0.004(2) N12 0.067(5) 0.034(4) 0.065(5) -0.010(3) -0.026(4) 0.009(3) N13 0.047(4) 0.067(5) 0.062(5) 0.016(4) 0.022(4) 0.006(4) O1 0.049(3) 0.032(3) 0.025(3) 0.002(2) 0.007(2) -0.008(2) O2 0.051(3) 0.020(2) 0.031(2) 0.0036(19) 0.009(2) -0.005(2) O3 0.070(4) 0.021(2) 0.040(3) 0.008(2) 0.004(3) -0.011(2) O4 0.088(4) 0.037(3) 0.031(3) 0.009(2) 0.011(3) -0.010(3) O5 0.071(4) 0.035(3) 0.019(2) -0.002(2) 0.006(2) -0.007(3) O6 0.086(4) 0.047(3) 0.036(3) 0.017(3) 0.000(3) -0.012(3) O7 0.042(3) 0.032(3) 0.050(3) 0.008(2) 0.011(3) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.255(8) . ? C1 O2 1.258(8) . ? C1 C2 1.519(8) . ? C1 Co3 2.496(6) . ? C2 C3 1.377(8) . ? C2 C7 1.385(9) . ? C3 C4 1.400(8) . ? C3 H3 0.9300 . ? C4 C5 1.349(9) . ? C4 C9 1.522(9) 1_665 ? C5 C6 1.400(9) . ? C5 H5 0.9300 . ? C6 C7 1.363(9) . ? C6 C8 1.493(9) 2_766 ? C7 H7 0.9300 . ? C8 O6 1.232(8) . ? C8 O5 1.277(8) . ? C8 C6 1.493(9) 2_766 ? C9 O4 1.218(8) . ? C9 O3 1.272(8) . ? C9 C4 1.522(9) 1_445 ? C10 N8 1.322(9) . ? C10 N6 1.335(8) . ? C10 N7 1.344(9) . ? C11 N5 1.292(8) . ? C11 N7 1.346(9) . ? C11 H11 0.9300 . ? C12 N11 1.334(9) 1_655 ? C12 N12 1.356(9) . ? C12 N10 1.362(8) . ? C13 N9 1.273(9) . ? C13 N11 1.354(8) 1_655 ? C13 H13 0.9300 . ? C14 N2 1.318(8) . ? C14 N3 1.370(8) . ? C14 N4 1.383(9) . ? C15 N1 1.310(8) . ? C15 N3 1.352(8) . ? C15 H15 0.9300 . ? C16 O7 1.227(9) . ? C16 N13 1.323(10) . ? C16 H16 0.9300 . ? C17 N13 1.440(13) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N13 1.459(12) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? Co1 N2 2.117(5) 2_755 ? Co1 N2 2.117(5) . ? Co1 N9 2.128(5) 2_755 ? Co1 N9 2.128(5) . ? Co1 N5 2.162(5) 2_755 ? Co1 N5 2.162(5) . ? Co2 O3 1.924(5) . ? Co2 O5 1.930(5) . ? Co2 N3 1.991(5) . ? Co2 N11 1.995(5) . ? Co3 N10 2.074(6) . ? Co3 N6 2.077(5) . ? Co3 N1 2.083(5) . ? Co3 O1 2.156(5) . ? Co3 O2 2.182(4) . ? Co3 O7 2.190(5) . ? N1 N2 1.381(7) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N5 N6 1.382(7) . ? N8 H8A 0.8600 . ? N8 H8B 0.8600 . ? N9 N10 1.399(7) . ? N11 C12 1.334(9) 1_455 ? N11 C13 1.354(8) 1_455 ? N12 H12A 0.8600 . ? N12 H12B 0.8600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 120.6(5) . . ? O1 C1 C2 120.2(6) . . ? O2 C1 C2 119.1(6) . . ? O1 C1 Co3 59.8(3) . . ? O2 C1 Co3 60.9(3) . . ? C2 C1 Co3 177.7(5) . . ? C3 C2 C7 121.1(6) . . ? C3 C2 C1 119.8(6) . . ? C7 C2 C1 119.1(6) . . ? C2 C3 C4 119.3(6) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 119.2(6) . . ? C5 C4 C9 120.7(6) . 1_665 ? C3 C4 C9 120.1(6) . 1_665 ? C4 C5 C6 121.5(6) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 119.5(6) . . ? C7 C6 C8 120.7(6) . 2_766 ? C5 C6 C8 119.8(6) . 2_766 ? C6 C7 C2 119.4(6) . . ? C6 C7 H7 120.3 . . ? C2 C7 H7 120.3 . . ? O6 C8 O5 124.2(6) . . ? O6 C8 C6 120.4(6) . 2_766 ? O5 C8 C6 115.5(6) . 2_766 ? O4 C9 O3 125.9(6) . . ? O4 C9 C4 120.5(6) . 1_445 ? O3 C9 C4 113.7(6) . 1_445 ? N8 C10 N6 124.8(6) . . ? N8 C10 N7 125.5(6) . . ? N6 C10 N7 109.7(6) . . ? N5 C11 N7 111.2(6) . . ? N5 C11 H11 124.4 . . ? N7 C11 H11 124.4 . . ? N11 C12 N12 125.7(7) 1_655 . ? N11 C12 N10 111.6(6) 1_655 . ? N12 C12 N10 122.7(7) . . ? N9 C13 N11 114.8(6) . 1_655 ? N9 C13 H13 122.6 . . ? N11 C13 H13 122.6 1_655 . ? N2 C14 N3 112.4(5) . . ? N2 C14 N4 124.5(6) . . ? N3 C14 N4 123.1(6) . . ? N1 C15 N3 112.3(6) . . ? N1 C15 H15 123.9 . . ? N3 C15 H15 123.9 . . ? O7 C16 N13 124.3(8) . . ? O7 C16 H16 117.9 . . ? N13 C16 H16 117.9 . . ? N13 C17 H17A 109.5 . . ? N13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N13 C18 H18A 109.5 . . ? N13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 Co1 N2 180.0(4) 2_755 . ? N2 Co1 N9 89.2(2) 2_755 2_755 ? N2 Co1 N9 90.8(2) . 2_755 ? N2 Co1 N9 90.8(2) 2_755 . ? N2 Co1 N9 89.2(2) . . ? N9 Co1 N9 180.0(5) 2_755 . ? N2 Co1 N5 90.3(2) 2_755 2_755 ? N2 Co1 N5 89.7(2) . 2_755 ? N9 Co1 N5 90.0(2) 2_755 2_755 ? N9 Co1 N5 90.0(2) . 2_755 ? N2 Co1 N5 89.7(2) 2_755 . ? N2 Co1 N5 90.3(2) . . ? N9 Co1 N5 90.0(2) 2_755 . ? N9 Co1 N5 90.0(2) . . ? N5 Co1 N5 180.0(2) 2_755 . ? O3 Co2 O5 94.5(2) . . ? O3 Co2 N3 115.7(2) . . ? O5 Co2 N3 115.7(2) . . ? O3 Co2 N11 109.1(2) . . ? O5 Co2 N11 116.8(2) . . ? N3 Co2 N11 105.0(2) . . ? N10 Co3 N6 93.1(2) . . ? N10 Co3 N1 87.6(2) . . ? N6 Co3 N1 97.2(2) . . ? N10 Co3 O1 101.4(2) . . ? N6 Co3 O1 95.40(18) . . ? N1 Co3 O1 164.0(2) . . ? N10 Co3 O2 92.95(19) . . ? N6 Co3 O2 155.82(18) . . ? N1 Co3 O2 106.37(18) . . ? O1 Co3 O2 60.45(17) . . ? N10 Co3 O7 172.5(2) . . ? N6 Co3 O7 92.4(2) . . ? N1 Co3 O7 86.7(2) . . ? O1 Co3 O7 83.1(2) . . ? O2 Co3 O7 84.02(19) . . ? N10 Co3 C1 99.1(2) . . ? N6 Co3 C1 125.6(2) . . ? N1 Co3 C1 135.8(2) . . ? O1 Co3 C1 30.20(19) . . ? O2 Co3 C1 30.26(19) . . ? O7 Co3 C1 81.7(2) . . ? C15 N1 N2 107.3(5) . . ? C15 N1 Co3 127.9(4) . . ? N2 N1 Co3 124.8(4) . . ? C14 N2 N1 105.5(5) . . ? C14 N2 Co1 129.6(4) . . ? N1 N2 Co1 123.3(4) . . ? C15 N3 C14 102.5(5) . . ? C15 N3 Co2 127.5(4) . . ? C14 N3 Co2 129.3(4) . . ? C14 N4 H4A 120.0 . . ? C14 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C11 N5 N6 107.3(5) . . ? C11 N5 Co1 128.7(5) . . ? N6 N5 Co1 122.6(4) . . ? C10 N6 N5 106.3(5) . . ? C10 N6 Co3 129.0(4) . . ? N5 N6 Co3 124.7(4) . . ? C10 N7 C11 105.5(5) . . ? C10 N8 H8A 120.0 . . ? C10 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? C13 N9 N10 106.0(5) . . ? C13 N9 Co1 123.8(4) . . ? N10 N9 Co1 128.7(4) . . ? C12 N10 N9 104.8(5) . . ? C12 N10 Co3 135.4(4) . . ? N9 N10 Co3 119.3(4) . . ? C12 N11 C13 102.8(6) 1_455 1_455 ? C12 N11 Co2 132.9(5) 1_455 . ? C13 N11 Co2 124.2(5) 1_455 . ? C12 N12 H12A 120.0 . . ? C12 N12 H12B 120.0 . . ? H12A N12 H12B 120.0 . . ? C16 N13 C17 120.2(8) . . ? C16 N13 C18 122.1(8) . . ? C17 N13 C18 117.7(9) . . ? C1 O1 Co3 90.0(4) . . ? C1 O2 Co3 88.8(4) . . ? C9 O3 Co2 134.1(5) . . ? C8 O5 Co2 125.8(4) . . ? C16 O7 Co3 122.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 8.7(10) . . . . ? O2 C1 C2 C3 -171.4(6) . . . . ? Co3 C1 C2 C3 -80(12) . . . . ? O1 C1 C2 C7 -170.9(7) . . . . ? O2 C1 C2 C7 9.1(10) . . . . ? Co3 C1 C2 C7 100(12) . . . . ? C7 C2 C3 C4 -2.5(11) . . . . ? C1 C2 C3 C4 177.9(6) . . . . ? C2 C3 C4 C5 0.9(11) . . . . ? C2 C3 C4 C9 179.5(6) . . . 1_665 ? C3 C4 C5 C6 0.7(11) . . . . ? C9 C4 C5 C6 -177.9(7) 1_665 . . . ? C4 C5 C6 C7 -0.8(11) . . . . ? C4 C5 C6 C8 178.3(7) . . . 2_766 ? C5 C6 C7 C2 -0.7(11) . . . . ? C8 C6 C7 C2 -179.8(7) 2_766 . . . ? C3 C2 C7 C6 2.4(11) . . . . ? C1 C2 C7 C6 -178.0(7) . . . . ? O1 C1 Co3 N10 97.1(4) . . . . ? O2 C1 Co3 N10 -80.2(4) . . . . ? C2 C1 Co3 N10 -172(12) . . . . ? O1 C1 Co3 N6 -3.4(5) . . . . ? O2 C1 Co3 N6 179.3(4) . . . . ? C2 C1 Co3 N6 87(12) . . . . ? O1 C1 Co3 N1 -166.9(4) . . . . ? O2 C1 Co3 N1 15.8(6) . . . . ? C2 C1 Co3 N1 -76(12) . . . . ? O2 C1 Co3 O1 -177.3(7) . . . . ? C2 C1 Co3 O1 90(12) . . . . ? O1 C1 Co3 O2 177.3(7) . . . . ? C2 C1 Co3 O2 -92(12) . . . . ? O1 C1 Co3 O7 -90.4(4) . . . . ? O2 C1 Co3 O7 92.3(4) . . . . ? C2 C1 Co3 O7 0(12) . . . . ? N3 C15 N1 N2 0.2(8) . . . . ? N3 C15 N1 Co3 179.3(4) . . . . ? N10 Co3 N1 C15 121.0(6) . . . . ? N6 Co3 N1 C15 -146.2(6) . . . . ? O1 Co3 N1 C15 -4.1(12) . . . . ? O2 Co3 N1 C15 28.6(6) . . . . ? O7 Co3 N1 C15 -54.2(6) . . . . ? C1 Co3 N1 C15 20.4(7) . . . . ? N10 Co3 N1 N2 -60.1(5) . . . . ? N6 Co3 N1 N2 32.7(5) . . . . ? O1 Co3 N1 N2 174.8(6) . . . . ? O2 Co3 N1 N2 -152.5(5) . . . . ? O7 Co3 N1 N2 124.7(5) . . . . ? C1 Co3 N1 N2 -160.7(4) . . . . ? N3 C14 N2 N1 0.9(8) . . . . ? N4 C14 N2 N1 179.4(7) . . . . ? N3 C14 N2 Co1 166.4(4) . . . . ? N4 C14 N2 Co1 -15.1(11) . . . . ? C15 N1 N2 C14 -0.7(7) . . . . ? Co3 N1 N2 C14 -179.8(5) . . . . ? C15 N1 N2 Co1 -167.3(5) . . . . ? Co3 N1 N2 Co1 13.6(7) . . . . ? N2 Co1 N2 C14 115(100) 2_755 . . . ? N9 Co1 N2 C14 53.7(6) 2_755 . . . ? N9 Co1 N2 C14 -126.3(6) . . . . ? N5 Co1 N2 C14 -36.4(6) 2_755 . . . ? N5 Co1 N2 C14 143.6(6) . . . . ? N2 Co1 N2 N1 -81(100) 2_755 . . . ? N9 Co1 N2 N1 -143.1(5) 2_755 . . . ? N9 Co1 N2 N1 36.9(5) . . . . ? N5 Co1 N2 N1 126.8(5) 2_755 . . . ? N5 Co1 N2 N1 -53.2(5) . . . . ? N1 C15 N3 C14 0.3(8) . . . . ? N1 C15 N3 Co2 -171.5(4) . . . . ? N2 C14 N3 C15 -0.8(8) . . . . ? N4 C14 N3 C15 -179.3(7) . . . . ? N2 C14 N3 Co2 170.8(5) . . . . ? N4 C14 N3 Co2 -7.7(10) . . . . ? O3 Co2 N3 C15 -158.1(5) . . . . ? O5 Co2 N3 C15 -48.9(6) . . . . ? N11 Co2 N3 C15 81.5(6) . . . . ? O3 Co2 N3 C14 32.3(6) . . . . ? O5 Co2 N3 C14 141.4(5) . . . . ? N11 Co2 N3 C14 -88.1(6) . . . . ? N7 C11 N5 N6 0.2(9) . . . . ? N7 C11 N5 Co1 -166.2(5) . . . . ? N2 Co1 N5 C11 38.1(7) 2_755 . . . ? N2 Co1 N5 C11 -141.9(7) . . . . ? N9 Co1 N5 C11 -51.0(7) 2_755 . . . ? N9 Co1 N5 C11 129.0(7) . . . . ? N5 Co1 N5 C11 167(44) 2_755 . . . ? N2 Co1 N5 N6 -126.4(5) 2_755 . . . ? N2 Co1 N5 N6 53.6(5) . . . . ? N9 Co1 N5 N6 144.4(5) 2_755 . . . ? N9 Co1 N5 N6 -35.6(5) . . . . ? N5 Co1 N5 N6 3(44) 2_755 . . . ? N8 C10 N6 N5 -178.8(7) . . . . ? N7 C10 N6 N5 0.9(8) . . . . ? N8 C10 N6 Co3 2.1(11) . . . . ? N7 C10 N6 Co3 -178.2(5) . . . . ? C11 N5 N6 C10 -0.7(8) . . . . ? Co1 N5 N6 C10 166.7(5) . . . . ? C11 N5 N6 Co3 178.4(5) . . . . ? Co1 N5 N6 Co3 -14.2(7) . . . . ? N10 Co3 N6 C10 -124.8(6) . . . . ? N1 Co3 N6 C10 147.2(6) . . . . ? O1 Co3 N6 C10 -23.0(6) . . . . ? O2 Co3 N6 C10 -20.5(10) . . . . ? O7 Co3 N6 C10 60.2(6) . . . . ? C1 Co3 N6 C10 -21.3(7) . . . . ? N10 Co3 N6 N5 56.3(5) . . . . ? N1 Co3 N6 N5 -31.7(5) . . . . ? O1 Co3 N6 N5 158.1(5) . . . . ? O2 Co3 N6 N5 160.6(5) . . . . ? O7 Co3 N6 N5 -118.7(5) . . . . ? C1 Co3 N6 N5 159.8(5) . . . . ? N8 C10 N7 C11 178.9(8) . . . . ? N6 C10 N7 C11 -0.7(8) . . . . ? N5 C11 N7 C10 0.3(9) . . . . ? N11 C13 N9 N10 1.6(8) 1_655 . . . ? N11 C13 N9 Co1 -165.3(4) 1_655 . . . ? N2 Co1 N9 C13 -57.0(6) 2_755 . . . ? N2 Co1 N9 C13 123.0(6) . . . . ? N9 Co1 N9 C13 163(100) 2_755 . . . ? N5 Co1 N9 C13 33.2(6) 2_755 . . . ? N5 Co1 N9 C13 -146.8(6) . . . . ? N2 Co1 N9 N10 139.2(5) 2_755 . . . ? N2 Co1 N9 N10 -40.8(5) . . . . ? N9 Co1 N9 N10 -1(100) 2_755 . . . ? N5 Co1 N9 N10 -130.5(5) 2_755 . . . ? N5 Co1 N9 N10 49.5(5) . . . . ? N11 C12 N10 N9 0.3(7) 1_655 . . . ? N12 C12 N10 N9 -180.0(7) . . . . ? N11 C12 N10 Co3 171.8(4) 1_655 . . . ? N12 C12 N10 Co3 -8.5(11) . . . . ? C13 N9 N10 C12 -1.1(7) . . . . ? Co1 N9 N10 C12 164.9(4) . . . . ? C13 N9 N10 Co3 -174.2(4) . . . . ? Co1 N9 N10 Co3 -8.2(7) . . . . ? N6 Co3 N10 C12 146.9(6) . . . . ? N1 Co3 N10 C12 -116.0(6) . . . . ? O1 Co3 N10 C12 50.7(6) . . . . ? O2 Co3 N10 C12 -9.7(6) . . . . ? O7 Co3 N10 C12 -75.5(17) . . . . ? C1 Co3 N10 C12 20.1(6) . . . . ? N6 Co3 N10 N9 -42.6(4) . . . . ? N1 Co3 N10 N9 54.5(4) . . . . ? O1 Co3 N10 N9 -138.8(4) . . . . ? O2 Co3 N10 N9 160.8(4) . . . . ? O7 Co3 N10 N9 95.0(15) . . . . ? C1 Co3 N10 N9 -169.4(4) . . . . ? O3 Co2 N11 C12 140.7(6) . . . 1_455 ? O5 Co2 N11 C12 35.1(7) . . . 1_455 ? N3 Co2 N11 C12 -94.7(6) . . . 1_455 ? O3 Co2 N11 C13 -38.2(6) . . . 1_455 ? O5 Co2 N11 C13 -143.8(5) . . . 1_455 ? N3 Co2 N11 C13 86.4(6) . . . 1_455 ? O7 C16 N13 C17 -4.3(13) . . . . ? O7 C16 N13 C18 177.2(9) . . . . ? O2 C1 O1 Co3 2.8(7) . . . . ? C2 C1 O1 Co3 -177.3(6) . . . . ? N10 Co3 O1 C1 -88.5(4) . . . . ? N6 Co3 O1 C1 177.2(4) . . . . ? N1 Co3 O1 C1 35.0(9) . . . . ? O2 Co3 O1 C1 -1.6(4) . . . . ? O7 Co3 O1 C1 85.5(4) . . . . ? O1 C1 O2 Co3 -2.7(7) . . . . ? C2 C1 O2 Co3 177.3(6) . . . . ? N10 Co3 O2 C1 103.0(4) . . . . ? N6 Co3 O2 C1 -1.3(8) . . . . ? N1 Co3 O2 C1 -168.6(4) . . . . ? O1 Co3 O2 C1 1.6(4) . . . . ? O7 Co3 O2 C1 -83.8(4) . . . . ? O4 C9 O3 Co2 19.8(13) . . . . ? C4 C9 O3 Co2 -160.5(5) 1_445 . . . ? O5 Co2 O3 C9 162.3(7) . . . . ? N3 Co2 O3 C9 -76.3(8) . . . . ? N11 Co2 O3 C9 41.8(8) . . . . ? O6 C8 O5 Co2 -0.9(11) . . . . ? C6 C8 O5 Co2 179.1(5) 2_766 . . . ? O3 Co2 O5 C8 -178.2(6) . . . . ? N3 Co2 O5 C8 60.4(7) . . . . ? N11 Co2 O5 C8 -64.1(7) . . . . ? N13 C16 O7 Co3 153.4(6) . . . . ? N10 Co3 O7 C16 -84.2(16) . . . . ? N6 Co3 O7 C16 53.5(6) . . . . ? N1 Co3 O7 C16 -43.6(6) . . . . ? O1 Co3 O7 C16 148.6(6) . . . . ? O2 Co3 O7 C16 -150.5(6) . . . . ? C1 Co3 O7 C16 179.1(6) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.004 0.011 0.500 495.9 175.5 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.006 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.180 _database_code_depnum_ccdc_archive 'CCDC 936925' ####################################################################### # # 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_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H21 Co5 N10 O20' _chemical_formula_weight 1196.27 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 16.245(7) _cell_length_b 18.294(7) _cell_length_c 16.222(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.622(8) _cell_angle_gamma 90.00 _cell_volume 4619(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 400 _cell_measurement_theta_min 2.617 _cell_measurement_theta_max 15.126 _exptl_crystal_description block _exptl_crystal_colour reddish _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 1.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6261 _exptl_absorpt_correction_T_max 0.7567 _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 ? _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 11474 _diffrn_reflns_av_R_equivalents 0.1399 _diffrn_reflns_av_sigmaI/netI 0.1699 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4108 _reflns_number_gt 2231 _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^)+(0.1460P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4108 _refine_ls_number_parameters 329 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1665 _refine_ls_R_factor_gt 0.1019 _refine_ls_wR_factor_ref 0.2998 _refine_ls_wR_factor_gt 0.2619 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.002 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 0.29413(11) 0.91269(8) 0.90907(11) 0.0323(6) Uani 1 1 d . . . Co2 Co 0.18489(13) 0.98885(9) 0.72419(12) 0.0366(6) Uani 1 1 d . . . Co3 Co 0.2500 0.7500 1.0000 0.0263(7) Uani 1 2 d S . . O8 O 0.1611(6) 0.9137(4) 0.8238(5) 0.038(2) Uani 1 1 d . . . O6 O 0.6769(6) 0.9814(4) 1.0736(6) 0.045(3) Uani 1 1 d . . . O4 O 0.4077(6) 0.8620(4) 0.9416(6) 0.043(2) Uani 1 1 d . . . O7 O 0.2220(6) 0.8097(4) 0.8760(5) 0.038(2) Uani 1 1 d . . . O5 O 0.7775(6) 0.9288(4) 1.1815(6) 0.040(2) Uani 1 1 d . . . N2 N 0.2606(7) 0.6521(5) 0.9418(6) 0.031(3) Uani 1 1 d . . . C9 C 0.4300(8) 0.8079(6) 0.9924(9) 0.032(3) Uani 1 1 d . . . O1 O 0.6492(6) 0.6006(4) 1.1396(6) 0.042(2) Uani 1 1 d . . . N3 N 0.2345(8) 0.5883(5) 0.9771(7) 0.040(3) Uani 1 1 d . . . C12 C 0.1565(8) 0.8447(7) 0.8306(7) 0.031(3) Uani 1 1 d . . . O11 O 0.3126(6) 0.9408(5) 0.7758(6) 0.046(3) Uani 1 1 d . . . C10 C 0.2491(9) 0.5335(7) 0.9282(9) 0.038(3) Uani 1 1 d U . . H10 H 0.2371 0.4848 0.9363 0.046 Uiso 1 1 calc R . . C5 C 0.5750(8) 0.8606(6) 1.0490(8) 0.031(3) Uani 1 1 d . . . H5 H 0.5504 0.9057 1.0303 0.038 Uiso 1 1 calc R . . C7 C 0.5637(8) 0.7312(6) 1.0620(7) 0.028(3) Uani 1 1 d . . . H7 H 0.5306 0.6890 1.0552 0.034 Uiso 1 1 calc R . . O3 O 0.3798(5) 0.7632(4) 1.0110(6) 0.037(2) Uani 1 1 d . . . C2 C 0.6508(8) 0.7266(6) 1.1011(8) 0.031(3) Uani 1 1 d . . . C13 C 0.0760(8) 0.8041(6) 0.7884(7) 0.029(3) Uani 1 1 d . . . C6 C 0.5238(8) 0.7975(6) 1.0324(8) 0.034(3) Uani 1 1 d U . . N4 N 0.2836(8) 0.5568(5) 0.8650(6) 0.037(3) Uani 1 1 d . . . C1 C 0.6941(10) 0.6551(7) 1.1380(9) 0.044(4) Uani 1 1 d . . . C18 C 0.0000 0.8424(9) 0.7500 0.031(4) Uani 1 2 d SU . . H18 H 0.0000 0.8932 0.7500 0.037 Uiso 1 2 calc SR . . C15 C 0.0000 0.6878(11) 0.7500 0.052(6) Uani 1 2 d SU . . C4 C 0.6626(9) 0.8565(6) 1.0933(8) 0.031(3) Uani 1 1 d U . . N1 N 0.0592(8) 1.0266(6) 0.6905(8) 0.050(3) Uani 1 1 d . . . O2 O 0.7758(7) 0.6565(5) 1.1656(8) 0.071(4) Uani 1 1 d . . . C8 C 0.7119(10) 0.9264(6) 1.1187(9) 0.039(4) Uani 1 1 d . . . C14 C 0.0758(9) 0.7288(7) 0.7885(9) 0.047(4) Uani 1 1 d . . . H14 H 0.1266 0.7041 0.8146 0.057 Uiso 1 1 calc R . . C3 C 0.6998(8) 0.7898(6) 1.1178(8) 0.036(3) Uani 1 1 d . . . H3 H 0.7583 0.7869 1.1457 0.044 Uiso 1 1 calc R . . N5 N 0.3222(8) 0.6755(6) 0.8286(7) 0.047(3) Uani 1 1 d . . . H5A H 0.3258 0.7215 0.8401 0.056 Uiso 1 1 calc R . . H5B H 0.3397 0.6588 0.7870 0.056 Uiso 1 1 calc R . . C11 C 0.2892(9) 0.6298(7) 0.8757(9) 0.039(3) Uani 1 1 d . . . O9 O 0.0841(13) 0.5766(10) 0.7592(13) 0.051(5) Uani 0.50 1 d PU . . C19 C 0.0201(16) 0.6086(14) 0.7257(15) 0.029(6) Uani 0.50 1 d PU . . O10 O -0.0474(14) 0.5779(10) 0.6715(14) 0.054(5) Uani 0.50 1 d PU . . C16 C 0.0016(19) 1.0329(17) 0.620(3) 0.175(17) Uani 1 1 d . . . C17 C -0.065(3) 1.088(2) 0.604(3) 0.23(2) Uiso 1 1 d . . . H17A H -0.0891 1.0894 0.6511 0.343 Uiso 1 1 calc R . . H17B H -0.1088 1.0754 0.5520 0.343 Uiso 1 1 calc R . . H17C H -0.0408 1.1343 0.5970 0.343 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0349(11) 0.0128(9) 0.0345(11) 0.0038(7) -0.0134(8) -0.0018(7) Co2 0.0455(13) 0.0148(9) 0.0368(11) 0.0041(7) -0.0088(8) -0.0026(7) Co3 0.0292(14) 0.0068(11) 0.0323(14) -0.0003(9) -0.0083(10) -0.0014(9) O8 0.038(6) 0.016(5) 0.039(5) -0.002(4) -0.020(4) -0.003(4) O6 0.048(6) 0.014(5) 0.056(6) 0.011(4) -0.015(5) -0.012(4) O4 0.041(6) 0.022(5) 0.051(6) 0.025(4) -0.012(4) 0.004(4) O7 0.036(6) 0.023(5) 0.035(5) 0.001(4) -0.024(4) -0.006(4) O5 0.049(6) 0.009(4) 0.046(6) -0.002(4) -0.014(5) 0.001(4) N2 0.048(7) 0.010(5) 0.027(6) 0.004(4) -0.003(5) -0.013(5) C9 0.018(7) 0.016(6) 0.051(8) -0.006(6) -0.007(6) 0.005(5) O1 0.044(6) 0.018(5) 0.048(6) 0.009(4) -0.012(4) -0.001(4) N3 0.058(8) 0.016(6) 0.031(6) -0.006(5) -0.009(5) 0.000(5) C12 0.033(8) 0.031(8) 0.021(6) -0.015(5) -0.007(5) -0.005(6) O11 0.041(6) 0.031(5) 0.048(6) 0.013(4) -0.018(4) 0.002(4) C10 0.058(7) 0.014(5) 0.040(7) -0.001(5) 0.008(6) 0.001(5) C5 0.027(7) 0.012(6) 0.042(7) 0.010(5) -0.010(6) -0.001(5) C7 0.023(7) 0.019(6) 0.035(7) 0.003(5) -0.005(5) 0.009(5) O3 0.021(5) 0.014(4) 0.061(6) 0.005(4) -0.015(4) -0.007(4) C2 0.038(8) 0.011(6) 0.033(7) 0.009(5) -0.008(6) 0.001(5) C13 0.033(8) 0.016(6) 0.024(6) -0.002(5) -0.014(5) 0.008(5) C6 0.038(7) 0.014(5) 0.037(6) 0.009(5) -0.008(5) -0.008(5) N4 0.060(8) 0.018(6) 0.024(6) -0.005(5) -0.004(5) 0.000(5) C1 0.061(11) 0.014(7) 0.051(9) 0.003(6) 0.005(8) 0.005(7) C18 0.040(8) 0.016(7) 0.032(7) 0.000 0.001(6) 0.000 C15 0.051(9) 0.032(8) 0.054(9) 0.000 -0.014(7) 0.000 C4 0.046(7) 0.017(5) 0.028(6) 0.004(5) 0.007(5) -0.013(5) N1 0.050(8) 0.019(6) 0.059(8) 0.014(6) -0.017(6) 0.006(5) O2 0.041(7) 0.030(6) 0.115(10) 0.023(6) -0.022(6) 0.016(5) C8 0.053(10) 0.009(6) 0.047(9) -0.002(6) 0.002(7) -0.008(6) C14 0.042(9) 0.022(7) 0.057(9) -0.007(6) -0.020(7) 0.015(6) C3 0.025(7) 0.016(6) 0.053(8) -0.005(6) -0.013(6) 0.004(5) N5 0.075(10) 0.020(6) 0.043(7) -0.008(5) 0.012(7) -0.006(6) C11 0.034(8) 0.024(7) 0.052(9) -0.001(7) 0.002(7) 0.003(6) O9 0.048(9) 0.028(8) 0.062(9) -0.006(7) -0.009(7) 0.012(7) C19 0.026(10) 0.029(9) 0.031(9) -0.004(7) 0.006(7) -0.009(7) O10 0.051(9) 0.037(8) 0.057(9) -0.008(7) -0.014(7) -0.002(7) C16 0.09(2) 0.14(3) 0.30(4) 0.16(3) 0.06(3) 0.042(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O6 1.995(8) 5_677 ? Co1 O4 1.996(9) . ? Co1 N3 2.029(12) 7_567 ? Co1 O7 2.203(8) . ? Co1 O8 2.208(8) . ? Co1 O11 2.324(10) . ? Co2 N1 2.075(13) . ? Co2 N4 2.080(11) 4_556 ? Co2 O1 2.108(8) 8_465 ? Co2 O5 2.110(8) 5_677 ? Co2 O11 2.188(9) . ? Co2 O8 2.238(9) . ? Co3 N2 2.055(10) 7_567 ? Co3 N2 2.055(10) . ? Co3 O3 2.079(9) . ? Co3 O3 2.079(9) 7_567 ? Co3 O7 2.218(8) 7_567 ? Co3 O7 2.218(8) . ? O8 C12 1.272(14) . ? O6 C8 1.278(15) . ? O6 Co1 1.995(8) 5_677 ? O4 C9 1.272(14) . ? O7 C12 1.279(15) . ? O5 C8 1.247(16) . ? O5 Co2 2.110(8) 5_677 ? N2 C11 1.348(17) . ? N2 N3 1.418(14) . ? C9 O3 1.251(15) . ? C9 C6 1.489(17) . ? O1 C1 1.240(16) . ? O1 Co2 2.108(8) 8_566 ? N3 C10 1.341(16) . ? N3 Co1 2.029(12) 7_567 ? C12 C13 1.490(16) . ? C10 N4 1.369(17) . ? C10 H10 0.9300 . ? C5 C6 1.402(16) . ? C5 C4 1.401(17) . ? C5 H5 0.9300 . ? C7 C2 1.378(17) . ? C7 C6 1.394(16) . ? C7 H7 0.9300 . ? C2 C3 1.386(16) . ? C2 C1 1.524(16) . ? C13 C14 1.377(17) . ? C13 C18 1.402(14) . ? N4 C11 1.347(16) . ? N4 Co2 2.080(11) 4_546 ? C1 O2 1.274(18) . ? C18 C13 1.402(14) 2_556 ? C18 H18 0.9300 . ? C15 C14 1.425(17) . ? C15 C14 1.425(17) 2_556 ? C15 C19 1.56(3) 2_556 ? C15 C19 1.56(3) . ? C4 C3 1.368(17) . ? C4 C8 1.502(16) . ? N1 C16 1.25(4) . ? C14 H14 0.9300 . ? C3 H3 0.9300 . ? N5 C11 1.343(17) . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? O9 C19 1.18(3) . ? O9 O10 1.42(3) 2_556 ? O9 C19 1.87(3) 2_556 ? C19 C19 1.16(5) 2_556 ? C19 O10 1.32(3) . ? C19 O10 1.69(3) 2_556 ? C19 O9 1.87(3) 2_556 ? O10 O9 1.42(3) 2_556 ? O10 C19 1.69(3) 2_556 ? C16 C17 1.44(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Co1 O4 104.5(4) 5_677 . ? O6 Co1 N3 89.2(4) 5_677 7_567 ? O4 Co1 N3 101.0(4) . 7_567 ? O6 Co1 O7 162.4(4) 5_677 . ? O4 Co1 O7 93.1(3) . . ? N3 Co1 O7 88.3(4) 7_567 . ? O6 Co1 O8 103.3(3) 5_677 . ? O4 Co1 O8 146.6(3) . . ? N3 Co1 O8 97.6(4) 7_567 . ? O7 Co1 O8 59.8(3) . . ? O6 Co1 O11 80.1(4) 5_677 . ? O4 Co1 O11 89.6(4) . . ? N3 Co1 O11 166.6(4) 7_567 . ? O7 Co1 O11 99.4(3) . . ? O8 Co1 O11 77.2(3) . . ? N1 Co2 N4 92.2(5) . 4_556 ? N1 Co2 O1 91.1(4) . 8_465 ? N4 Co2 O1 95.0(4) 4_556 8_465 ? N1 Co2 O5 90.7(4) . 5_677 ? N4 Co2 O5 90.0(4) 4_556 5_677 ? O1 Co2 O5 174.6(4) 8_465 5_677 ? N1 Co2 O11 171.4(4) . . ? N4 Co2 O11 96.4(4) 4_556 . ? O1 Co2 O11 89.5(4) 8_465 . ? O5 Co2 O11 87.9(4) 5_677 . ? N1 Co2 O8 92.0(4) . . ? N4 Co2 O8 175.8(4) 4_556 . ? O1 Co2 O8 85.5(3) 8_465 . ? O5 Co2 O8 89.3(3) 5_677 . ? O11 Co2 O8 79.5(3) . . ? N2 Co3 N2 180.000(2) 7_567 . ? N2 Co3 O3 94.3(4) 7_567 . ? N2 Co3 O3 85.7(4) . . ? N2 Co3 O3 85.7(4) 7_567 7_567 ? N2 Co3 O3 94.3(4) . 7_567 ? O3 Co3 O3 180.000(1) . 7_567 ? N2 Co3 O7 92.0(3) 7_567 7_567 ? N2 Co3 O7 88.0(3) . 7_567 ? O3 Co3 O7 92.3(3) . 7_567 ? O3 Co3 O7 87.7(3) 7_567 7_567 ? N2 Co3 O7 88.0(3) 7_567 . ? N2 Co3 O7 92.0(3) . . ? O3 Co3 O7 87.7(3) . . ? O3 Co3 O7 92.3(3) 7_567 . ? O7 Co3 O7 180.000(2) 7_567 . ? C12 O8 Co1 90.5(7) . . ? C12 O8 Co2 134.3(9) . . ? Co1 O8 Co2 96.7(4) . . ? C8 O6 Co1 129.4(8) . 5_677 ? C9 O4 Co1 127.0(9) . . ? C12 O7 Co1 90.5(7) . . ? C12 O7 Co3 133.6(9) . . ? Co1 O7 Co3 104.1(3) . . ? C8 O5 Co2 128.3(8) . 5_677 ? C11 N2 N3 106.5(10) . . ? C11 N2 Co3 136.3(8) . . ? N3 N2 Co3 117.2(8) . . ? O3 C9 O4 125.5(11) . . ? O3 C9 C6 117.9(11) . . ? O4 C9 C6 116.6(11) . . ? C1 O1 Co2 125.7(9) . 8_566 ? C10 N3 N2 104.5(11) . . ? C10 N3 Co1 131.2(9) . 7_567 ? N2 N3 Co1 123.2(7) . 7_567 ? O8 C12 O7 119.2(11) . . ? O8 C12 C13 121.4(11) . . ? O7 C12 C13 119.4(11) . . ? Co2 O11 Co1 94.8(4) . . ? N3 C10 N4 113.0(11) . . ? N3 C10 H10 123.5 . . ? N4 C10 H10 123.5 . . ? C6 C5 C4 120.9(11) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C2 C7 C6 121.8(11) . . ? C2 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C9 O3 Co3 140.4(8) . . ? C7 C2 C3 119.7(11) . . ? C7 C2 C1 122.1(11) . . ? C3 C2 C1 117.7(12) . . ? C14 C13 C18 119.9(12) . . ? C14 C13 C12 120.0(11) . . ? C18 C13 C12 120.1(11) . . ? C7 C6 C5 117.3(12) . . ? C7 C6 C9 125.3(11) . . ? C5 C6 C9 117.1(10) . . ? C11 N4 C10 103.9(11) . . ? C11 N4 Co2 131.4(10) . 4_546 ? C10 N4 Co2 124.8(8) . 4_546 ? O1 C1 O2 124.7(12) . . ? O1 C1 C2 119.3(13) . . ? O2 C1 C2 116.0(12) . . ? C13 C18 C13 120.0(16) 2_556 . ? C13 C18 H18 120.0 2_556 . ? C13 C18 H18 120.0 . . ? C14 C15 C14 116.4(17) . 2_556 ? C14 C15 C19 126.6(13) . 2_556 ? C14 C15 C19 112.5(12) 2_556 2_556 ? C14 C15 C19 112.5(12) . . ? C14 C15 C19 126.6(13) 2_556 . ? C19 C15 C19 43.6(18) 2_556 . ? C3 C4 C5 119.7(11) . . ? C3 C4 C8 121.5(12) . . ? C5 C4 C8 118.6(11) . . ? C16 N1 Co2 134(2) . . ? O5 C8 O6 125.2(11) . . ? O5 C8 C4 121.2(11) . . ? O6 C8 C4 113.5(12) . . ? C13 C14 C15 121.9(13) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C4 C3 C2 120.4(12) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C11 N5 H5A 120.0 . . ? C11 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? N5 C11 N2 123.2(12) . . ? N5 C11 N4 124.6(13) . . ? N2 C11 N4 112.1(13) . . ? C19 O9 O10 80.9(19) . 2_556 ? C19 O9 C19 36.5(18) . 2_556 ? O10 O9 C19 44.7(12) 2_556 2_556 ? C19 C19 O9 106(3) 2_556 . ? C19 C19 O10 86(3) 2_556 . ? O9 C19 O10 123(2) . . ? C19 C19 C15 68.2(9) 2_556 . ? O9 C19 C15 124(2) . . ? O10 C19 C15 112(2) . . ? C19 C19 O10 51(2) 2_556 2_556 ? O9 C19 O10 55.5(17) . 2_556 ? O10 C19 O10 117(2) . 2_556 ? C15 C19 O10 94.2(14) . 2_556 ? C19 C19 O9 37.3(18) 2_556 2_556 ? O9 C19 O9 120(2) . 2_556 ? O10 C19 O9 48.9(14) . 2_556 ? C15 C19 O9 89.7(13) . 2_556 ? O10 C19 O9 76.1(13) 2_556 2_556 ? C19 O10 O9 86.4(18) . 2_556 ? C19 O10 C19 43.1(18) . 2_556 ? O9 O10 C19 43.5(12) 2_556 2_556 ? N1 C16 C17 124(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Co1 O8 C12 -173.9(8) 5_677 . . . ? O4 Co1 O8 C12 40.5(11) . . . . ? N3 Co1 O8 C12 -82.9(8) 7_567 . . . ? O7 Co1 O8 C12 0.6(7) . . . . ? O11 Co1 O8 C12 109.6(8) . . . . ? O6 Co1 O8 Co2 51.3(4) 5_677 . . . ? O4 Co1 O8 Co2 -94.3(6) . . . . ? N3 Co1 O8 Co2 142.3(4) 7_567 . . . ? O7 Co1 O8 Co2 -134.2(5) . . . . ? O11 Co1 O8 Co2 -25.2(3) . . . . ? N1 Co2 O8 C12 110.6(12) . . . . ? N4 Co2 O8 C12 -78(5) 4_556 . . . ? O1 Co2 O8 C12 19.7(11) 8_465 . . . ? O5 Co2 O8 C12 -158.7(11) 5_677 . . . ? O11 Co2 O8 C12 -70.7(11) . . . . ? N1 Co2 O8 Co1 -152.1(4) . . . . ? N4 Co2 O8 Co1 20(5) 4_556 . . . ? O1 Co2 O8 Co1 116.9(4) 8_465 . . . ? O5 Co2 O8 Co1 -61.4(4) 5_677 . . . ? O11 Co2 O8 Co1 26.6(3) . . . . ? O6 Co1 O4 C9 130.5(10) 5_677 . . . ? N3 Co1 O4 C9 38.4(11) 7_567 . . . ? O7 Co1 O4 C9 -50.4(10) . . . . ? O8 Co1 O4 C9 -84.2(12) . . . . ? O11 Co1 O4 C9 -149.8(10) . . . . ? O6 Co1 O7 C12 17.2(16) 5_677 . . . ? O4 Co1 O7 C12 -159.9(8) . . . . ? N3 Co1 O7 C12 99.2(8) 7_567 . . . ? O8 Co1 O7 C12 -0.6(7) . . . . ? O11 Co1 O7 C12 -69.8(8) . . . . ? O6 Co1 O7 Co3 -118.3(11) 5_677 . . . ? O4 Co1 O7 Co3 64.6(4) . . . . ? N3 Co1 O7 Co3 -36.3(4) 7_567 . . . ? O8 Co1 O7 Co3 -136.1(5) . . . . ? O11 Co1 O7 Co3 154.7(4) . . . . ? N2 Co3 O7 C12 -64.4(11) 7_567 . . . ? N2 Co3 O7 C12 115.6(11) . . . . ? O3 Co3 O7 C12 -158.8(11) . . . . ? O3 Co3 O7 C12 21.2(11) 7_567 . . . ? O7 Co3 O7 C12 0(100) 7_567 . . . ? N2 Co3 O7 Co1 40.2(4) 7_567 . . . ? N2 Co3 O7 Co1 -139.8(4) . . . . ? O3 Co3 O7 Co1 -54.2(4) . . . . ? O3 Co3 O7 Co1 125.8(4) 7_567 . . . ? O7 Co3 O7 Co1 0(100) 7_567 . . . ? N2 Co3 N2 C11 -110(100) 7_567 . . . ? O3 Co3 N2 C11 -53.0(13) . . . . ? O3 Co3 N2 C11 127.0(13) 7_567 . . . ? O7 Co3 N2 C11 -145.5(13) 7_567 . . . ? O7 Co3 N2 C11 34.5(13) . . . . ? N2 Co3 N2 N3 68(100) 7_567 . . . ? O3 Co3 N2 N3 125.0(8) . . . . ? O3 Co3 N2 N3 -55.0(8) 7_567 . . . ? O7 Co3 N2 N3 32.5(8) 7_567 . . . ? O7 Co3 N2 N3 -147.5(8) . . . . ? Co1 O4 C9 O3 22.8(19) . . . . ? Co1 O4 C9 C6 -157.5(9) . . . . ? C11 N2 N3 C10 -0.7(13) . . . . ? Co3 N2 N3 C10 -179.2(8) . . . . ? C11 N2 N3 Co1 168.7(9) . . . 7_567 ? Co3 N2 N3 Co1 -9.8(12) . . . 7_567 ? Co1 O8 C12 O7 -1.1(13) . . . . ? Co2 O8 C12 O7 98.8(13) . . . . ? Co1 O8 C12 C13 177.6(11) . . . . ? Co2 O8 C12 C13 -82.5(16) . . . . ? Co1 O7 C12 O8 1.1(13) . . . . ? Co3 O7 C12 O8 111.2(13) . . . . ? Co1 O7 C12 C13 -177.6(10) . . . . ? Co3 O7 C12 C13 -67.4(15) . . . . ? N1 Co2 O11 Co1 -16(3) . . . . ? N4 Co2 O11 Co1 154.4(4) 4_556 . . . ? O1 Co2 O11 Co1 -110.6(4) 8_465 . . . ? O5 Co2 O11 Co1 64.6(4) 5_677 . . . ? O8 Co2 O11 Co1 -25.1(3) . . . . ? O6 Co1 O11 Co2 -80.5(4) 5_677 . . . ? O4 Co1 O11 Co2 174.7(4) . . . . ? N3 Co1 O11 Co2 -42.8(18) 7_567 . . . ? O7 Co1 O11 Co2 81.6(4) . . . . ? O8 Co1 O11 Co2 25.7(3) . . . . ? N2 N3 C10 N4 0.9(15) . . . . ? Co1 N3 C10 N4 -167.4(9) 7_567 . . . ? O4 C9 O3 Co3 -13(2) . . . . ? C6 C9 O3 Co3 167.1(9) . . . . ? N2 Co3 O3 C9 -54.3(14) 7_567 . . . ? N2 Co3 O3 C9 125.7(14) . . . . ? O3 Co3 O3 C9 156(100) 7_567 . . . ? O7 Co3 O3 C9 -146.4(14) 7_567 . . . ? O7 Co3 O3 C9 33.6(14) . . . . ? C6 C7 C2 C3 5(2) . . . . ? C6 C7 C2 C1 176.7(12) . . . . ? O8 C12 C13 C14 172.6(13) . . . . ? O7 C12 C13 C14 -9(2) . . . . ? O8 C12 C13 C18 -8.8(18) . . . . ? O7 C12 C13 C18 169.9(10) . . . . ? C2 C7 C6 C5 -4.1(19) . . . . ? C2 C7 C6 C9 -177.6(12) . . . . ? C4 C5 C6 C7 0.2(19) . . . . ? C4 C5 C6 C9 174.3(12) . . . . ? O3 C9 C6 C7 25(2) . . . . ? O4 C9 C6 C7 -154.6(12) . . . . ? O3 C9 C6 C5 -148.4(12) . . . . ? O4 C9 C6 C5 31.8(18) . . . . ? N3 C10 N4 C11 -0.7(15) . . . . ? N3 C10 N4 Co2 -179.9(8) . . . 4_546 ? Co2 O1 C1 O2 24(2) 8_566 . . . ? Co2 O1 C1 C2 -155.9(9) 8_566 . . . ? C7 C2 C1 O1 -6(2) . . . . ? C3 C2 C1 O1 165.6(13) . . . . ? C7 C2 C1 O2 174.0(13) . . . . ? C3 C2 C1 O2 -14(2) . . . . ? C14 C13 C18 C13 -0.2(10) . . . 2_556 ? C12 C13 C18 C13 -178.9(13) . . . 2_556 ? C6 C5 C4 C3 3(2) . . . . ? C6 C5 C4 C8 -172.7(12) . . . . ? N4 Co2 N1 C16 52(2) 4_556 . . . ? O1 Co2 N1 C16 -43(2) 8_465 . . . ? O5 Co2 N1 C16 142(2) 5_677 . . . ? O11 Co2 N1 C16 -137(3) . . . . ? O8 Co2 N1 C16 -129(2) . . . . ? Co2 O5 C8 O6 37(2) 5_677 . . . ? Co2 O5 C8 C4 -139.0(10) 5_677 . . . ? Co1 O6 C8 O5 -6(2) 5_677 . . . ? Co1 O6 C8 C4 170.3(9) 5_677 . . . ? C3 C4 C8 O5 -21(2) . . . . ? C5 C4 C8 O5 154.0(14) . . . . ? C3 C4 C8 O6 162.7(13) . . . . ? C5 C4 C8 O6 -22.0(19) . . . . ? C18 C13 C14 C15 0(2) . . . . ? C12 C13 C14 C15 179.1(11) . . . . ? C14 C15 C14 C13 -0.2(10) 2_556 . . . ? C19 C15 C14 C13 -154.4(16) 2_556 . . . ? C19 C15 C14 C13 157.5(15) . . . . ? C5 C4 C3 C2 -2(2) . . . . ? C8 C4 C3 C2 173.4(13) . . . . ? C7 C2 C3 C4 -2(2) . . . . ? C1 C2 C3 C4 -173.9(13) . . . . ? N3 N2 C11 N5 -177.5(12) . . . . ? Co3 N2 C11 N5 1(2) . . . . ? N3 N2 C11 N4 0.3(14) . . . . ? Co3 N2 C11 N4 178.4(9) . . . . ? C10 N4 C11 N5 178.0(13) . . . . ? Co2 N4 C11 N5 -3(2) 4_546 . . . ? C10 N4 C11 N2 0.2(15) . . . . ? Co2 N4 C11 N2 179.3(9) 4_546 . . . ? O10 O9 C19 C19 -5.5(19) 2_556 . . 2_556 ? O10 O9 C19 O10 -101(3) 2_556 . . . ? C19 O9 C19 O10 -96(3) 2_556 . . . ? O10 O9 C19 C15 69(2) 2_556 . . . ? C19 O9 C19 C15 74(3) 2_556 . . . ? C19 O9 C19 O10 5(2) 2_556 . . 2_556 ? O10 O9 C19 O9 -43(2) 2_556 . . 2_556 ? C19 O9 C19 O9 -38.0(13) 2_556 . . 2_556 ? C14 C15 C19 C19 120(2) . . . 2_556 ? C14 C15 C19 C19 -85(3) 2_556 . . 2_556 ? C14 C15 C19 O9 25(3) . . . . ? C14 C15 C19 O9 180(2) 2_556 . . . ? C19 C15 C19 O9 -95(4) 2_556 . . . ? C14 C15 C19 O10 -163.9(17) . . . . ? C14 C15 C19 O10 -9(3) 2_556 . . . ? C19 C15 C19 O10 76(3) 2_556 . . . ? C14 C15 C19 O10 75.2(15) . . . 2_556 ? C14 C15 C19 O10 -129.8(14) 2_556 . . 2_556 ? C19 C15 C19 O10 -44.8(19) 2_556 . . 2_556 ? C14 C15 C19 O9 151.2(11) . . . 2_556 ? C14 C15 C19 O9 -53.8(17) 2_556 . . 2_556 ? C19 C15 C19 O9 31.3(18) 2_556 . . 2_556 ? C19 C19 O10 O9 -4.7(15) 2_556 . . 2_556 ? O9 C19 O10 O9 102(3) . . . 2_556 ? C15 C19 O10 O9 -69.3(18) . . . 2_556 ? O10 C19 O10 O9 37(2) 2_556 . . 2_556 ? O9 C19 O10 C19 107(3) . . . 2_556 ? C15 C19 O10 C19 -64.6(16) . . . 2_556 ? O10 C19 O10 C19 42.1(18) 2_556 . . 2_556 ? O9 C19 O10 C19 4.7(15) 2_556 . . 2_556 ? Co2 N1 C16 C17 -151(3) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.677 0.250 135.1 73.2 2 0.000 0.323 0.750 135.1 72.5 3 0.500 0.177 0.250 135.1 73.2 4 0.500 0.823 0.750 135.1 72.5 _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.212 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.224 _database_code_depnum_ccdc_archive 'CCDC 936926'