# Electronic Supplementary Material (ESI) for CrystEngComm # 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 'C42 H32 Co2 N8 O15,3(O)' _chemical_formula_sum 'C42 H38 Co2 N8 O18' _chemical_formula_weight 1060.60 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' 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 P2/c _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 15.9990(15) _cell_length_b 10.6917(14) _cell_length_c 14.4959(19) _cell_angle_alpha 90.00 _cell_angle_beta 116.938(8) _cell_angle_gamma 90.00 _cell_volume 2210.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1833 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 23.07 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7865 _exptl_absorpt_correction_T_max 0.8633 _exptl_absorpt_process_details SADABS(Bruker,2000) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11566 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0893 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4200 _reflns_number_gt 2808 _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^)+(0.0345P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4200 _refine_ls_number_parameters 329 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.113 _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 Co1 Co 0.41832(4) 0.53916(5) 0.30551(4) 0.01940(17) Uani 1 1 d . . . O1 O 0.48326(19) 0.6378(3) 0.4426(2) 0.0313(8) Uani 1 1 d . . . H1A H 0.5110 0.7170 0.4509 0.038 Uiso 1 1 d R . . H1B H 0.4795 0.6272 0.5011 0.038 Uiso 1 1 d R . . O2 O 0.5000 0.6531(3) 0.2500 0.0214(9) Uani 1 2 d S . . H2A H 0.4588 0.6962 0.1978 0.026 Uiso 1 1 d R . . O3 O 0.36397(17) 0.4495(3) 0.1637(2) 0.0249(7) Uani 1 1 d . . . O4 O 0.48286(17) 0.3906(2) 0.1324(2) 0.0235(7) Uani 1 1 d . . . O5 O 0.0672(2) 0.2101(3) -0.0013(3) 0.0647(12) Uani 1 1 d . . . O6 O 0.08199(19) 0.0042(3) 0.0107(2) 0.0382(9) Uani 1 1 d . . . H6A H 0.0263 0.0071 -0.0034 0.023 Uiso 0.50 1 d PR . . O7 O 0.3944(2) -0.1858(3) 0.0966(3) 0.0560(11) Uani 1 1 d . . . O8 O 0.4871(2) -0.0821(3) 0.0515(3) 0.0498(10) Uani 1 1 d . . . H8A H 0.4645 -0.0693 -0.0215 0.030 Uiso 0.50 1 d PR . . N11 N 0.2460(2) 0.2675(3) 0.3442(3) 0.0235(8) Uani 1 1 d . . . N12 N 0.3352(2) 0.4263(3) 0.3497(3) 0.0224(8) Uani 1 1 d . . . N21 N 0.2180(2) -0.1682(3) 0.2298(3) 0.0242(8) Uani 1 1 d . . . N22 N 0.3122(2) -0.3258(3) 0.2455(3) 0.0233(8) Uani 1 1 d . . . C7 C 0.0492(3) 0.0418(4) 0.2590(3) 0.0232(10) Uani 1 1 d . . . C8 C 0.1021(3) 0.1496(4) 0.2944(3) 0.0253(10) Uani 1 1 d . . . H8 H 0.0757 0.2207 0.3075 0.030 Uiso 1 1 calc R . . C9 C 0.1942(3) 0.1522(4) 0.3103(3) 0.0232(10) Uani 1 1 d . . . C10 C 0.2349(3) 0.0475(4) 0.2903(3) 0.0241(10) Uani 1 1 d . . . H10 H 0.2967 0.0490 0.3007 0.029 Uiso 1 1 calc R . . C11 C 0.1805(3) -0.0589(4) 0.2543(3) 0.0235(10) Uani 1 1 d . . . C12 C 0.0889(3) -0.0630(4) 0.2401(3) 0.0257(10) Uani 1 1 d . . . H12 H 0.0543 -0.1364 0.2177 0.031 Uiso 1 1 calc R . . C13 C 0.3558(3) 0.2513(4) 0.0911(3) 0.0199(9) Uani 1 1 d . . . C14 C 0.2606(3) 0.2397(4) 0.0644(3) 0.0243(10) Uani 1 1 d . . . H14 H 0.2263 0.3105 0.0629 0.029 Uiso 1 1 calc R . . C15 C 0.2158(3) 0.1221(4) 0.0398(3) 0.0222(10) Uani 1 1 d . . . C16 C 0.2686(3) 0.0188(4) 0.0439(3) 0.0249(10) Uani 1 1 d . . . H16 H 0.2408 -0.0599 0.0318 0.030 Uiso 1 1 calc R . . C17 C 0.3627(3) 0.0289(4) 0.0656(3) 0.0222(10) Uani 1 1 d . . . C18 C 0.4055(3) 0.1461(4) 0.0883(3) 0.0217(10) Uani 1 1 d . . . H18 H 0.4679 0.1539 0.1017 0.026 Uiso 1 1 calc R . . C19 C 0.4046(3) 0.3728(4) 0.1314(3) 0.0191(9) Uani 1 1 d . . . C20 C 0.1131(3) 0.1154(5) 0.0144(4) 0.0323(11) Uani 1 1 d . . . C21 C 0.4169(3) -0.0876(4) 0.0717(4) 0.0338(12) Uani 1 1 d . . . C101 C 0.3116(3) 0.3112(4) 0.3188(3) 0.0251(10) Uani 1 1 d . . . H101 H 0.3370 0.2649 0.2833 0.030 Uiso 1 1 calc R . . C102 C 0.2829(3) 0.4590(4) 0.3990(4) 0.0361(12) Uani 1 1 d . . . H102 H 0.2855 0.5360 0.4301 0.043 Uiso 1 1 calc R . . C103 C 0.2267(3) 0.3625(4) 0.3959(4) 0.0416(14) Uani 1 1 d . . . H103 H 0.1840 0.3607 0.4230 0.050 Uiso 1 1 calc R . . C201 C 0.3038(3) -0.2192(4) 0.2857(3) 0.0255(10) Uani 1 1 d . . . H201 H 0.3509 -0.1833 0.3449 0.031 Uiso 1 1 calc R . . C202 C 0.1691(3) -0.2481(4) 0.1482(4) 0.0348(12) Uani 1 1 d . . . H202 H 0.1081 -0.2380 0.0962 0.042 Uiso 1 1 calc R . . C203 C 0.2276(3) -0.3435(4) 0.1593(3) 0.0334(12) Uani 1 1 d . . . H203 H 0.2130 -0.4119 0.1150 0.040 Uiso 1 1 calc R . . O2WA O 0.0000 0.479(2) 0.2500 0.072(11) Uani 0.248(15) 2 d SP A 2 O2WB O 0.0429(11) 0.5948(17) 0.3350(15) 0.176(8) Uani 0.376(7) 1 d PU A 3 O1W O 0.9978(8) 0.4010(9) 0.4170(8) 0.325(6) 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 Co1 0.0181(3) 0.0144(3) 0.0279(3) -0.0004(3) 0.0123(3) 0.0006(3) O1 0.0417(19) 0.0245(18) 0.0265(18) -0.0021(14) 0.0142(16) -0.0141(15) O2 0.017(2) 0.018(2) 0.026(2) 0.000 0.0072(19) 0.000 O3 0.0228(15) 0.0203(17) 0.0339(18) -0.0076(14) 0.0150(14) -0.0015(13) O4 0.0196(15) 0.0210(17) 0.0363(18) -0.0085(13) 0.0181(14) -0.0056(13) O5 0.0235(19) 0.032(2) 0.133(4) 0.000(2) 0.030(2) 0.0039(17) O6 0.0203(16) 0.031(2) 0.062(2) 0.0021(16) 0.0176(17) -0.0073(14) O7 0.044(2) 0.020(2) 0.096(3) 0.0191(19) 0.024(2) 0.0040(17) O8 0.048(2) 0.042(2) 0.072(3) 0.0068(19) 0.038(2) 0.0211(17) N11 0.025(2) 0.018(2) 0.034(2) -0.0059(16) 0.0186(18) -0.0040(16) N12 0.0190(19) 0.017(2) 0.034(2) -0.0007(16) 0.0150(17) -0.0018(15) N21 0.0176(19) 0.016(2) 0.039(2) -0.0037(16) 0.0128(18) 0.0010(15) N22 0.0221(19) 0.019(2) 0.031(2) -0.0031(16) 0.0132(18) 0.0021(16) C7 0.019(2) 0.017(2) 0.038(3) 0.002(2) 0.016(2) -0.0023(19) C8 0.023(2) 0.017(2) 0.045(3) -0.001(2) 0.023(2) 0.0048(19) C9 0.023(2) 0.019(2) 0.032(3) -0.0023(19) 0.016(2) -0.0073(19) C10 0.019(2) 0.022(2) 0.036(3) 0.002(2) 0.016(2) 0.0015(19) C11 0.024(2) 0.017(2) 0.031(3) 0.0007(19) 0.013(2) 0.0032(19) C12 0.022(2) 0.018(2) 0.039(3) -0.003(2) 0.015(2) -0.0009(19) C13 0.019(2) 0.018(2) 0.026(2) -0.0043(18) 0.012(2) -0.0031(18) C14 0.021(2) 0.019(2) 0.031(3) -0.002(2) 0.011(2) 0.0032(19) C15 0.019(2) 0.019(2) 0.030(3) -0.0023(19) 0.012(2) -0.0051(19) C16 0.029(2) 0.014(2) 0.032(3) -0.0020(19) 0.014(2) -0.0084(19) C17 0.024(2) 0.016(2) 0.028(2) 0.0016(19) 0.012(2) -0.0010(19) C18 0.018(2) 0.022(2) 0.027(3) -0.0019(19) 0.012(2) -0.0008(18) C19 0.017(2) 0.016(2) 0.023(2) 0.0013(18) 0.008(2) 0.0003(18) C20 0.023(2) 0.033(3) 0.039(3) -0.001(2) 0.013(2) -0.005(2) C21 0.029(3) 0.024(3) 0.044(3) -0.004(2) 0.013(2) 0.003(2) C101 0.024(2) 0.022(3) 0.036(3) -0.002(2) 0.020(2) -0.001(2) C102 0.040(3) 0.029(3) 0.054(3) -0.019(2) 0.034(3) -0.012(2) C103 0.047(3) 0.038(3) 0.063(4) -0.021(3) 0.045(3) -0.017(2) C201 0.017(2) 0.024(3) 0.033(3) -0.003(2) 0.010(2) 0.0013(19) C202 0.023(3) 0.031(3) 0.041(3) -0.006(2) 0.007(2) 0.005(2) C203 0.033(3) 0.026(3) 0.036(3) -0.008(2) 0.011(2) 0.003(2) O2WA 0.064(16) 0.07(2) 0.064(18) 0.000 0.013(14) 0.000 O2WB 0.150(10) 0.149(12) 0.236(12) -0.036(8) 0.093(9) 0.020(8) O1W 0.348(12) 0.278(12) 0.275(12) 0.088(8) 0.075(10) -0.094(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.066(3) . ? Co1 O3 2.070(3) . ? Co1 N22 2.094(3) 1_565 ? Co1 N12 2.098(3) . ? Co1 O4 2.132(3) 2_655 ? Co1 O2 2.189(2) . ? O1 H1A 0.9375 . ? O1 H1B 0.8848 . ? O2 Co1 2.189(2) 2_655 ? O2 H2A 0.8763 . ? O3 C19 1.261(4) . ? O4 C19 1.260(4) . ? O4 Co1 2.132(3) 2_655 ? O5 C20 1.211(5) . ? O6 C20 1.281(5) . ? O6 H6A 0.8200 . ? O7 C21 1.217(5) . ? O8 C21 1.284(5) . ? O8 H8A 0.9600 . ? N11 C101 1.344(5) . ? N11 C103 1.377(5) . ? N11 C9 1.442(5) . ? N12 C101 1.306(5) . ? N12 C102 1.371(5) . ? N21 C201 1.353(5) . ? N21 C202 1.379(5) . ? N21 C11 1.430(5) . ? N22 C201 1.314(5) . ? N22 C203 1.378(5) . ? N22 Co1 2.094(3) 1_545 ? C7 C12 1.376(5) . ? C7 C8 1.384(5) . ? C7 C7 1.473(7) 2 ? C8 C9 1.384(5) . ? C8 H8 0.9300 . ? C9 C10 1.390(5) . ? C10 C11 1.383(5) . ? C10 H10 0.9300 . ? C11 C12 1.385(5) . ? C12 H12 0.9300 . ? C13 C18 1.388(5) . ? C13 C14 1.396(5) . ? C13 C19 1.492(5) . ? C14 C15 1.411(5) . ? C14 H14 0.9300 . ? C15 C16 1.376(5) . ? C15 C20 1.513(5) . ? C16 C17 1.396(5) . ? C16 H16 0.9300 . ? C17 C18 1.394(5) . ? C17 C21 1.497(6) . ? C18 H18 0.9300 . ? C101 H101 0.9300 . ? C102 C103 1.356(6) . ? C102 H102 0.9300 . ? C103 H103 0.9300 . ? C201 H201 0.9300 . ? C202 C203 1.345(5) . ? C202 H202 0.9300 . ? C203 H203 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 Co1 O3 173.58(11) . . ? O1 Co1 N22 90.41(12) . 1_565 ? O3 Co1 N22 90.58(12) . 1_565 ? O1 Co1 N12 96.46(12) . . ? O3 Co1 N12 89.87(12) . . ? N22 Co1 N12 90.94(13) 1_565 . ? O1 Co1 O4 91.20(11) . 2_655 ? O3 Co1 O4 88.38(11) . 2_655 ? N22 Co1 O4 174.76(11) 1_565 2_655 ? N12 Co1 O4 83.92(11) . 2_655 ? O1 Co1 O2 86.87(9) . . ? O3 Co1 O2 86.82(9) . . ? N22 Co1 O2 88.31(11) 1_565 . ? N12 Co1 O2 176.60(10) . . ? O4 Co1 O2 96.76(9) 2_655 . ? Co1 O1 H1A 126.0 . . ? Co1 O1 H1B 129.3 . . ? H1A O1 H1B 103.1 . . ? Co1 O2 Co1 112.38(16) 2_655 . ? Co1 O2 H2A 108.4 2_655 . ? Co1 O2 H2A 105.6 . . ? C19 O3 Co1 127.9(2) . . ? C19 O4 Co1 131.3(3) . 2_655 ? C20 O6 H6A 109.5 . . ? C21 O8 H8A 109.0 . . ? C101 N11 C103 106.8(3) . . ? C101 N11 C9 127.0(3) . . ? C103 N11 C9 125.5(3) . . ? C101 N12 C102 105.6(3) . . ? C101 N12 Co1 124.2(3) . . ? C102 N12 Co1 129.3(3) . . ? C201 N21 C202 107.0(4) . . ? C201 N21 C11 127.3(4) . . ? C202 N21 C11 125.5(3) . . ? C201 N22 C203 105.4(3) . . ? C201 N22 Co1 129.8(3) . 1_545 ? C203 N22 Co1 124.1(3) . 1_545 ? C12 C7 C8 119.4(3) . . ? C12 C7 C7 121.1(3) . 2 ? C8 C7 C7 119.4(3) . 2 ? C7 C8 C9 120.3(4) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C8 C9 C10 120.9(4) . . ? C8 C9 N11 118.5(4) . . ? C10 C9 N11 120.6(3) . . ? C11 C10 C9 117.8(4) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? C10 C11 C12 121.7(4) . . ? C10 C11 N21 120.2(4) . . ? C12 C11 N21 118.1(4) . . ? C7 C12 C11 119.8(4) . . ? C7 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C18 C13 C14 119.1(4) . . ? C18 C13 C19 120.8(3) . . ? C14 C13 C19 119.8(4) . . ? C13 C14 C15 121.0(4) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 118.2(4) . . ? C16 C15 C20 123.3(4) . . ? C14 C15 C20 118.4(4) . . ? C15 C16 C17 121.7(4) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C18 C17 C16 119.2(4) . . ? C18 C17 C21 121.6(4) . . ? C16 C17 C21 119.1(4) . . ? C13 C18 C17 120.5(4) . . ? C13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? O4 C19 O3 125.1(4) . . ? O4 C19 C13 118.5(4) . . ? O3 C19 C13 116.4(3) . . ? O5 C20 O6 125.2(4) . . ? O5 C20 C15 120.4(4) . . ? O6 C20 C15 114.4(4) . . ? O7 C21 O8 120.9(4) . . ? O7 C21 C17 119.6(4) . . ? O8 C21 C17 119.5(4) . . ? N12 C101 N11 112.0(4) . . ? N12 C101 H101 124.0 . . ? N11 C101 H101 124.0 . . ? C103 C102 N12 109.9(4) . . ? C103 C102 H102 125.1 . . ? N12 C102 H102 125.1 . . ? C102 C103 N11 105.8(4) . . ? C102 C103 H103 127.1 . . ? N11 C103 H103 127.1 . . ? N22 C201 N21 111.3(4) . . ? N22 C201 H201 124.3 . . ? N21 C201 H201 124.3 . . ? C203 C202 N21 105.9(4) . . ? C203 C202 H202 127.1 . . ? N21 C202 H202 127.1 . . ? C202 C203 N22 110.4(4) . . ? C202 C203 H203 124.8 . . ? N22 C203 H203 124.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 O2 Co1 125.37(8) . . . 2_655 ? O3 Co1 O2 Co1 -53.45(7) . . . 2_655 ? N22 Co1 O2 Co1 -144.13(9) 1_565 . . 2_655 ? N12 Co1 O2 Co1 -66.7(19) . . . 2_655 ? O4 Co1 O2 Co1 34.53(8) 2_655 . . 2_655 ? O1 Co1 O3 C19 62.1(11) . . . . ? N22 Co1 O3 C19 161.0(3) 1_565 . . . ? N12 Co1 O3 C19 -108.1(3) . . . . ? O4 Co1 O3 C19 -24.2(3) 2_655 . . . ? O2 Co1 O3 C19 72.7(3) . . . . ? O1 Co1 N12 C101 -147.0(3) . . . . ? O3 Co1 N12 C101 31.9(3) . . . . ? N22 Co1 N12 C101 122.4(3) 1_565 . . . ? O4 Co1 N12 C101 -56.5(3) 2_655 . . . ? O2 Co1 N12 C101 45(2) . . . . ? O1 Co1 N12 C102 45.0(4) . . . . ? O3 Co1 N12 C102 -136.1(4) . . . . ? N22 Co1 N12 C102 -45.5(4) 1_565 . . . ? O4 Co1 N12 C102 135.5(4) 2_655 . . . ? O2 Co1 N12 C102 -122.9(19) . . . . ? C12 C7 C8 C9 0.2(7) . . . . ? C7 C7 C8 C9 -179.0(5) 2 . . . ? C7 C8 C9 C10 0.6(7) . . . . ? C7 C8 C9 N11 178.2(4) . . . . ? C101 N11 C9 C8 -145.5(4) . . . . ? C103 N11 C9 C8 23.6(6) . . . . ? C101 N11 C9 C10 32.1(6) . . . . ? C103 N11 C9 C10 -158.8(4) . . . . ? C8 C9 C10 C11 -0.1(6) . . . . ? N11 C9 C10 C11 -177.7(4) . . . . ? C9 C10 C11 C12 -1.1(6) . . . . ? C9 C10 C11 N21 178.3(4) . . . . ? C201 N21 C11 C10 44.0(6) . . . . ? C202 N21 C11 C10 -142.3(4) . . . . ? C201 N21 C11 C12 -136.6(4) . . . . ? C202 N21 C11 C12 37.2(6) . . . . ? C8 C7 C12 C11 -1.4(6) . . . . ? C7 C7 C12 C11 177.7(5) 2 . . . ? C10 C11 C12 C7 1.9(7) . . . . ? N21 C11 C12 C7 -177.5(4) . . . . ? C18 C13 C14 C15 3.2(6) . . . . ? C19 C13 C14 C15 -171.2(4) . . . . ? C13 C14 C15 C16 0.7(6) . . . . ? C13 C14 C15 C20 178.3(4) . . . . ? C14 C15 C16 C17 -3.7(6) . . . . ? C20 C15 C16 C17 178.8(4) . . . . ? C15 C16 C17 C18 2.9(6) . . . . ? C15 C16 C17 C21 178.4(4) . . . . ? C14 C13 C18 C17 -4.1(6) . . . . ? C19 C13 C18 C17 170.2(4) . . . . ? C16 C17 C18 C13 1.1(6) . . . . ? C21 C17 C18 C13 -174.2(4) . . . . ? Co1 O4 C19 O3 5.1(6) 2_655 . . . ? Co1 O4 C19 C13 -173.6(2) 2_655 . . . ? Co1 O3 C19 O4 -51.4(5) . . . . ? Co1 O3 C19 C13 127.3(3) . . . . ? C18 C13 C19 O4 21.8(6) . . . . ? C14 C13 C19 O4 -163.9(4) . . . . ? C18 C13 C19 O3 -157.0(4) . . . . ? C14 C13 C19 O3 17.3(6) . . . . ? C16 C15 C20 O5 -170.3(5) . . . . ? C14 C15 C20 O5 12.2(7) . . . . ? C16 C15 C20 O6 9.0(6) . . . . ? C14 C15 C20 O6 -168.5(4) . . . . ? C18 C17 C21 O7 147.8(4) . . . . ? C16 C17 C21 O7 -27.5(7) . . . . ? C18 C17 C21 O8 -31.6(6) . . . . ? C16 C17 C21 O8 153.0(4) . . . . ? C102 N12 C101 N11 0.7(5) . . . . ? Co1 N12 C101 N11 -169.7(3) . . . . ? C103 N11 C101 N12 -0.2(5) . . . . ? C9 N11 C101 N12 170.5(4) . . . . ? C101 N12 C102 C103 -0.9(5) . . . . ? Co1 N12 C102 C103 168.8(3) . . . . ? N12 C102 C103 N11 0.7(5) . . . . ? C101 N11 C103 C102 -0.3(5) . . . . ? C9 N11 C103 C102 -171.2(4) . . . . ? C203 N22 C201 N21 0.4(5) . . . . ? Co1 N22 C201 N21 -170.3(3) 1_545 . . . ? C202 N21 C201 N22 -0.5(5) . . . . ? C11 N21 C201 N22 174.2(4) . . . . ? C201 N21 C202 C203 0.4(5) . . . . ? C11 N21 C202 C203 -174.4(4) . . . . ? N21 C202 C203 N22 -0.1(5) . . . . ? C201 N22 C203 C202 -0.1(5) . . . . ? Co1 N22 C203 C202 171.3(3) 1_545 . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.845 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.082 _database_code_depnum_ccdc_archive 'CCDC 942556' ####################################################################### # # 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 'C66 H42 Co3 N16 O12, 4(H2O) ' _chemical_formula_sum 'C66 H50 Co3 N16 O16' _chemical_formula_weight 1500.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M '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 27.882(3) _cell_length_b 13.2793(16) _cell_length_c 18.463(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.198(2) _cell_angle_gamma 90.00 _cell_volume 6530.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5045 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 26.10 _exptl_crystal_description prismatic _exptl_crystal_colour violet _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.518 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3036 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7875 _exptl_absorpt_correction_T_max 0.9211 _exptl_absorpt_process_details sadabs _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_decay_% ? _diffrn_reflns_number 16435 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5955 _reflns_number_gt 4724 _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^)+(0.0848P)^2^+5.4975P] 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 5955 _refine_ls_number_parameters 496 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1494 _refine_ls_wR_factor_gt 0.1424 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.216952(16) 0.46000(4) 1.03570(3) 0.02934(17) Uani 1 1 d . . . Co2 Co 0.5000 0.11416(5) 1.2500 0.0356(2) Uani 1 2 d SU . . O1 O 0.27051(9) 0.3838(2) 1.10704(15) 0.0430(7) Uani 1 1 d . . . O2 O 0.21600(11) 0.3885(2) 1.17211(17) 0.0590(8) Uani 1 1 d . . . O3 O 0.43852(10) 0.2275(2) 1.21786(18) 0.0536(8) Uani 1 1 d . . . O4 O 0.44517(12) 0.1167(2) 1.30594(17) 0.0623(9) Uani 1 1 d U . . O5 O 0.31843(11) 0.0727(2) 1.43481(16) 0.0514(8) Uani 1 1 d . . . O6 O 0.24091(13) 0.1212(3) 1.3792(2) 0.0712(10) Uani 1 1 d . . . N1 N 0.16122(10) 0.3570(2) 0.99600(17) 0.0351(7) Uani 1 1 d . . . N2 N 0.08926(10) 0.2830(2) 0.98606(18) 0.0369(7) Uani 1 1 d . . . N3 N -0.04312(11) 0.3900(3) 1.08671(19) 0.0446(8) Uani 1 1 d . . . N4 N -0.03912(12) 0.5093(3) 1.17035(19) 0.0434(8) Uani 1 1 d . . . N5 N -0.20040(10) 0.0029(2) 0.88416(16) 0.0327(7) Uani 1 1 d . . . N6 N -0.25389(10) -0.0203(2) 0.94911(17) 0.0332(7) Uani 1 1 d . . . N7 N -0.09302(12) -0.0249(2) 0.72022(19) 0.0426(8) Uani 1 1 d . . . N8 N -0.0900(14) -0.1139(11) 0.6222(13) 0.113(8) Uani 0.494(9) 1 d P A 1 N8' N -0.1038(7) -0.0584(19) 0.6019(6) 0.073(4) Uani 0.506(9) 1 d P A 2 C1 C 0.42043(15) 0.1841(3) 1.2636(2) 0.0427(9) Uani 1 1 d . . . C2 C 0.36936(14) 0.2079(3) 1.2688(2) 0.0370(9) Uani 1 1 d . . . C3 C 0.35234(14) 0.1621(3) 1.3244(2) 0.0401(9) Uani 1 1 d . . . H3 H 0.3734 0.1186 1.3589 0.048 Uiso 1 1 calc R . . C4 C 0.30476(14) 0.1804(3) 1.3290(2) 0.0386(9) Uani 1 1 d . . . C5 C 0.28603(17) 0.1233(3) 1.3851(2) 0.0462(10) Uani 1 1 d . . . C6 C 0.27366(14) 0.2465(3) 1.2773(2) 0.0397(9) Uani 1 1 d . . . H6 H 0.2417 0.2602 1.2805 0.048 Uiso 1 1 calc R . . C7 C 0.28969(14) 0.2916(3) 1.2215(2) 0.0368(9) Uani 1 1 d . . . C8 C 0.33761(13) 0.2719(3) 1.2176(2) 0.0359(8) Uani 1 1 d . . . H8 H 0.3486 0.3022 1.1799 0.043 Uiso 1 1 calc R . . C9 C 0.25564(15) 0.3588(3) 1.1641(2) 0.0410(9) Uani 1 1 d . . . C10 C 0.16474(14) 0.2570(3) 0.9806(3) 0.0482(11) Uani 1 1 d . . . H10 H 0.1933 0.2257 0.9750 0.058 Uiso 1 1 calc R . . C11 C 0.12092(14) 0.2106(3) 0.9748(3) 0.0508(11) Uani 1 1 d . . . H11 H 0.1137 0.1427 0.9650 0.061 Uiso 1 1 calc R . . C12 C 0.11531(13) 0.3697(3) 0.9982(2) 0.0385(9) Uani 1 1 d . . . H12 H 0.1022 0.4313 1.0072 0.046 Uiso 1 1 calc R . . C13 C 0.03844(13) 0.2720(3) 0.9872(2) 0.0368(9) Uani 1 1 d . . . C14 C 0.00704(13) 0.2012(3) 0.9428(2) 0.0370(9) Uani 1 1 d . . . H14 H 0.0188 0.1591 0.9115 0.044 Uiso 1 1 calc R . . C15 C -0.04228(13) 0.1928(3) 0.9448(2) 0.0338(8) Uani 1 1 d . . . C16 C -0.05937(13) 0.2583(3) 0.9905(2) 0.0368(9) Uani 1 1 d . . . H16 H -0.0928 0.2561 0.9902 0.044 Uiso 1 1 calc R . . C17 C -0.02685(14) 0.3267(3) 1.0364(2) 0.0395(9) Uani 1 1 d . . . C18 C 0.02255(14) 0.3327(3) 1.0365(2) 0.0427(10) Uani 1 1 d . . . H18 H 0.0447 0.3767 1.0690 0.051 Uiso 1 1 calc R . . C19 C -0.01862(15) 0.4711(3) 1.1217(2) 0.0453(10) Uani 1 1 d . . . H19 H 0.0099 0.4974 1.1123 0.054 Uiso 1 1 calc R . . C20 C -0.07952(17) 0.4495(4) 1.1656(3) 0.0674(15) Uani 1 1 d . . . H20 H -0.1018 0.4584 1.1939 0.081 Uiso 1 1 calc R . . C21 C -0.08276(18) 0.3765(4) 1.1150(3) 0.0738(17) Uani 1 1 d . . . H21 H -0.1071 0.3264 1.1015 0.089 Uiso 1 1 calc R . . C22 C -0.07702(13) 0.1171(3) 0.8973(2) 0.0321(8) Uani 1 1 d . A . C23 C -0.06818(13) 0.0762(3) 0.8331(2) 0.0351(8) Uani 1 1 d . . . H23 H -0.0392 0.0934 0.8209 0.042 Uiso 1 1 calc R A . C24 C -0.10196(14) 0.0106(3) 0.7878(2) 0.0363(9) Uani 1 1 d . A . C25 C -0.14606(14) -0.0158(3) 0.8035(2) 0.0368(9) Uani 1 1 d . . . H25 H -0.1690 -0.0597 0.7722 0.044 Uiso 1 1 calc R A . C26 C -0.15468(13) 0.0254(3) 0.8672(2) 0.0319(8) Uani 1 1 d . A . C27 C -0.12121(13) 0.0911(3) 0.9131(2) 0.0331(8) Uani 1 1 d . . . H27 H -0.1282 0.1186 0.9553 0.040 Uiso 1 1 calc R A . C28 C -0.24554(15) -0.0201(4) 0.8330(2) 0.0537(12) Uani 1 1 d . . . H28 H -0.2526 -0.0250 0.7807 0.064 Uiso 1 1 calc R . . C29 C -0.27775(15) -0.0344(3) 0.8739(2) 0.0510(11) Uani 1 1 d . . . H29 H -0.3114 -0.0513 0.8537 0.061 Uiso 1 1 calc R . . C30 C -0.20726(13) 0.0029(3) 0.9525(2) 0.0350(8) Uani 1 1 d . . . H30 H -0.1822 0.0175 0.9972 0.042 Uiso 1 1 calc R . . C31 C -0.0757(3) 0.0340(7) 0.6712(5) 0.046(3) Uani 0.494(9) 1 d P A 1 H31 H -0.0673 0.1018 0.6785 0.056 Uiso 0.494(9) 1 calc PR A 1 C32 C -0.0731(9) -0.0191(12) 0.6140(9) 0.054(3) Uani 0.494(9) 1 d P A 1 H32 H -0.0617 0.0030 0.5742 0.065 Uiso 0.494(9) 1 calc PR A 1 C33 C -0.1036(6) -0.1123(10) 0.6862(8) 0.102(6) Uani 0.494(9) 1 d P A 1 H33 H -0.1185 -0.1658 0.7040 0.122 Uiso 0.494(9) 1 calc PR A 1 C31' C -0.0452(3) -0.0520(8) 0.7143(5) 0.062(3) Uani 0.506(9) 1 d P A 2 H31' H -0.0148 -0.0566 0.7525 0.074 Uiso 0.506(9) 1 calc PR A 2 C32' C -0.0552(5) -0.070(2) 0.6368(9) 0.059(3) Uani 0.506(9) 1 d P A 2 H32' H -0.0313 -0.0872 0.6131 0.071 Uiso 0.506(9) 1 calc PR A 2 C33' C -0.1239(3) -0.0331(9) 0.6543(5) 0.058(3) Uani 0.506(9) 1 d P A 2 H33' H -0.1582 -0.0220 0.6444 0.070 Uiso 0.506(9) 1 calc PR A 2 O1W O 0.1876(3) 0.2438(7) 0.4565(7) 0.305(7) Uani 1 1 d . . . O2W O 0.1176(2) 0.4018(7) 0.1769(4) 0.207(4) 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 Co1 0.0227(3) 0.0359(3) 0.0323(3) -0.0006(2) 0.0125(2) -0.00117(19) Co2 0.0414(4) 0.0353(4) 0.0344(4) 0.000 0.0180(3) 0.000 O1 0.0405(15) 0.0493(16) 0.0394(16) 0.0118(13) 0.0121(13) 0.0081(12) O2 0.0421(16) 0.084(2) 0.0537(19) 0.0126(17) 0.0182(15) 0.0210(16) O3 0.0463(16) 0.0541(18) 0.069(2) 0.0079(16) 0.0297(16) 0.0080(14) O4 0.070(2) 0.080(2) 0.0457(17) 0.0210(16) 0.0306(15) 0.0466(18) O5 0.0643(19) 0.0473(16) 0.0400(16) 0.0112(14) 0.0115(15) -0.0174(15) O6 0.063(2) 0.076(2) 0.086(3) 0.0230(19) 0.0397(19) -0.0052(18) N1 0.0248(15) 0.0454(19) 0.0394(18) -0.0080(14) 0.0159(14) -0.0058(13) N2 0.0259(15) 0.0424(18) 0.0458(19) -0.0094(15) 0.0158(14) -0.0062(13) N3 0.0321(17) 0.056(2) 0.051(2) -0.0233(17) 0.0208(16) -0.0126(15) N4 0.0350(18) 0.054(2) 0.044(2) -0.0164(16) 0.0153(15) -0.0037(15) N5 0.0297(15) 0.0421(17) 0.0286(16) -0.0040(13) 0.0123(13) -0.0112(13) N6 0.0282(15) 0.0433(18) 0.0307(17) -0.0020(14) 0.0126(13) -0.0094(13) N7 0.0432(19) 0.052(2) 0.041(2) -0.0141(16) 0.0241(17) -0.0103(15) N8 0.22(3) 0.072(9) 0.092(12) -0.023(8) 0.112(15) -0.019(13) N8' 0.066(8) 0.126(14) 0.030(5) -0.013(7) 0.020(5) 0.007(9) C1 0.046(2) 0.046(2) 0.034(2) -0.0071(19) 0.0080(19) 0.0100(19) C2 0.041(2) 0.037(2) 0.033(2) -0.0002(17) 0.0112(17) 0.0047(17) C3 0.046(2) 0.035(2) 0.037(2) 0.0040(17) 0.0077(18) 0.0025(17) C4 0.045(2) 0.037(2) 0.032(2) 0.0010(17) 0.0109(18) -0.0065(17) C5 0.059(3) 0.039(2) 0.043(2) -0.0019(19) 0.018(2) -0.011(2) C6 0.035(2) 0.044(2) 0.041(2) -0.0011(18) 0.0134(18) -0.0039(17) C7 0.039(2) 0.033(2) 0.038(2) 0.0019(16) 0.0109(17) 0.0008(16) C8 0.040(2) 0.038(2) 0.032(2) 0.0025(16) 0.0139(17) -0.0007(17) C9 0.038(2) 0.043(2) 0.040(2) 0.0002(18) 0.0093(18) -0.0017(17) C10 0.0282(19) 0.045(2) 0.076(3) -0.017(2) 0.024(2) -0.0002(17) C11 0.039(2) 0.040(2) 0.077(3) -0.019(2) 0.023(2) -0.0066(18) C12 0.0300(19) 0.040(2) 0.050(2) -0.0084(18) 0.0186(18) -0.0044(16) C13 0.0274(18) 0.045(2) 0.042(2) -0.0049(18) 0.0154(16) -0.0075(16) C14 0.0321(19) 0.043(2) 0.040(2) -0.0095(17) 0.0171(17) -0.0057(16) C15 0.0305(18) 0.040(2) 0.0323(19) -0.0033(16) 0.0121(16) -0.0098(16) C16 0.0229(17) 0.048(2) 0.042(2) -0.0075(18) 0.0138(16) -0.0108(16) C17 0.036(2) 0.048(2) 0.041(2) -0.0107(18) 0.0210(18) -0.0078(17) C18 0.035(2) 0.046(2) 0.052(2) -0.0151(19) 0.0190(19) -0.0132(17) C19 0.038(2) 0.053(3) 0.050(2) -0.016(2) 0.0200(19) -0.0094(19) C20 0.052(3) 0.080(3) 0.087(4) -0.035(3) 0.047(3) -0.015(2) C21 0.059(3) 0.087(4) 0.096(4) -0.047(3) 0.056(3) -0.035(3) C22 0.0286(18) 0.038(2) 0.0314(19) -0.0008(16) 0.0119(15) -0.0051(15) C23 0.0304(19) 0.044(2) 0.035(2) -0.0024(17) 0.0172(17) -0.0073(16) C24 0.040(2) 0.041(2) 0.034(2) -0.0063(17) 0.0204(17) -0.0027(17) C25 0.037(2) 0.039(2) 0.036(2) -0.0093(17) 0.0136(17) -0.0113(16) C26 0.0284(18) 0.040(2) 0.0284(19) -0.0009(16) 0.0107(15) -0.0082(15) C27 0.0337(19) 0.042(2) 0.0265(19) -0.0032(16) 0.0139(16) -0.0060(16) C28 0.044(2) 0.086(3) 0.030(2) -0.011(2) 0.0096(19) -0.029(2) C29 0.033(2) 0.080(3) 0.041(2) -0.009(2) 0.0112(19) -0.025(2) C30 0.0298(19) 0.049(2) 0.0280(19) -0.0010(17) 0.0109(16) -0.0075(16) C31 0.054(5) 0.049(5) 0.038(5) 0.003(4) 0.015(4) -0.006(4) C32 0.062(10) 0.073(10) 0.041(7) 0.003(7) 0.034(7) 0.014(9) C33 0.189(15) 0.056(7) 0.105(11) -0.037(8) 0.114(11) -0.049(9) C31' 0.033(5) 0.105(8) 0.051(6) -0.031(5) 0.018(4) -0.006(5) C32' 0.050(8) 0.088(11) 0.053(8) -0.032(7) 0.034(7) -0.010(8) C33' 0.043(5) 0.094(9) 0.040(5) -0.018(5) 0.016(4) 0.004(5) O1W 0.140(6) 0.244(9) 0.497(17) -0.216(11) 0.040(8) 0.016(6) O2W 0.108(4) 0.363(10) 0.175(6) -0.126(7) 0.080(4) -0.094(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.956(2) . ? Co1 O5 1.956(3) 4_557 ? Co1 N6 2.013(3) 3 ? Co1 N1 2.037(3) . ? Co2 O4 2.083(3) . ? Co2 O4 2.083(3) 2_657 ? Co2 N4 2.084(3) 3_545 ? Co2 N4 2.084(3) 4_547 ? Co2 O3 2.226(3) . ? Co2 O3 2.226(3) 2_657 ? Co2 C1 2.485(4) 2_657 ? O1 C9 1.284(5) . ? O2 C9 1.223(5) . ? O3 C1 1.246(5) . ? O4 C1 1.252(5) . ? O5 C5 1.273(5) . ? O5 Co1 1.956(3) 4_547 ? O6 C5 1.230(5) . ? N1 C12 1.304(4) . ? N1 C10 1.367(5) . ? N2 C12 1.344(5) . ? N2 C11 1.363(5) . ? N2 C13 1.431(4) . ? N3 C19 1.336(5) . ? N3 C21 1.366(5) . ? N3 C17 1.422(5) . ? N4 C19 1.301(5) . ? N4 C20 1.360(5) . ? N4 Co2 2.084(3) 3_455 ? N5 C30 1.331(4) . ? N5 C28 1.366(5) . ? N5 C26 1.431(4) . ? N6 C30 1.319(4) . ? N6 C29 1.364(5) . ? N6 Co1 2.013(3) 3_445 ? N7 C33' 1.271(9) . ? N7 C33 1.310(11) . ? N7 C31 1.387(9) . ? N7 C31' 1.416(9) . ? N7 C24 1.424(5) . ? N8 C33 1.345(17) . ? N8 C32 1.37(3) . ? N8' C33' 1.299(15) . ? N8' C32' 1.33(2) . ? C1 C2 1.490(5) . ? C2 C8 1.380(5) . ? C2 C3 1.391(5) . ? C3 C4 1.376(5) . ? C3 H3 0.9300 . ? C4 C6 1.395(5) . ? C4 C5 1.496(5) . ? C6 C7 1.376(5) . ? C6 H6 0.9300 . ? C7 C8 1.384(5) . ? C7 C9 1.492(5) . ? C8 H8 0.9300 . ? C10 C11 1.344(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.378(5) . ? C13 C18 1.382(5) . ? C14 C15 1.391(5) . ? C14 H14 0.9300 . ? C15 C16 1.391(5) . ? C15 C22 1.489(5) . ? C16 C17 1.382(5) . ? C16 H16 0.9300 . ? C17 C18 1.379(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.332(6) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.390(5) . ? C22 C27 1.391(5) . ? C23 C24 1.370(5) . ? C23 H23 0.9300 . ? C24 C25 1.389(5) . ? C25 C26 1.380(5) . ? C25 H25 0.9300 . ? C26 C27 1.373(5) . ? C27 H27 0.9300 . ? C28 C29 1.346(6) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.291(14) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C31' C32' 1.395(15) . ? C31' H31' 0.9300 . ? C32' H32' 0.9300 . ? C33' H33' 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 Co1 O5 123.76(12) . 4_557 ? O1 Co1 N6 101.23(12) . 3 ? O5 Co1 N6 118.48(13) 4_557 3 ? O1 Co1 N1 104.13(12) . . ? O5 Co1 N1 102.72(13) 4_557 . ? N6 Co1 N1 104.21(12) 3 . ? O4 Co2 O4 178.13(18) . 2_657 ? O4 Co2 N4 93.04(13) . 3_545 ? O4 Co2 N4 88.21(12) 2_657 3_545 ? O4 Co2 N4 88.21(12) . 4_547 ? O4 Co2 N4 93.04(13) 2_657 4_547 ? N4 Co2 N4 96.1(2) 3_545 4_547 ? O4 Co2 O3 60.06(11) . . ? O4 Co2 O3 118.49(13) 2_657 . ? N4 Co2 O3 93.60(12) 3_545 . ? N4 Co2 O3 147.26(12) 4_547 . ? O4 Co2 O3 118.49(13) . 2_657 ? O4 Co2 O3 60.06(11) 2_657 2_657 ? N4 Co2 O3 147.26(12) 3_545 2_657 ? N4 Co2 O3 93.60(12) 4_547 2_657 ? O3 Co2 O3 94.88(16) . 2_657 ? O4 Co2 C1 148.42(14) . 2_657 ? O4 Co2 C1 30.22(12) 2_657 2_657 ? N4 Co2 C1 118.36(13) 3_545 2_657 ? N4 Co2 C1 91.38(13) 4_547 2_657 ? O3 Co2 C1 111.13(13) . 2_657 ? O3 Co2 C1 30.03(11) 2_657 2_657 ? C9 O1 Co1 108.6(2) . . ? C1 O3 Co2 86.6(2) . . ? C1 O4 Co2 92.9(3) . . ? C5 O5 Co1 107.2(3) . 4_547 ? C12 N1 C10 105.3(3) . . ? C12 N1 Co1 123.5(3) . . ? C10 N1 Co1 129.3(2) . . ? C12 N2 C11 106.7(3) . . ? C12 N2 C13 125.0(3) . . ? C11 N2 C13 128.3(3) . . ? C19 N3 C21 106.1(3) . . ? C19 N3 C17 125.2(3) . . ? C21 N3 C17 128.5(3) . . ? C19 N4 C20 104.7(3) . . ? C19 N4 Co2 120.1(3) . 3_455 ? C20 N4 Co2 133.3(3) . 3_455 ? C30 N5 C28 107.1(3) . . ? C30 N5 C26 126.5(3) . . ? C28 N5 C26 126.4(3) . . ? C30 N6 C29 104.9(3) . . ? C30 N6 Co1 128.0(2) . 3_445 ? C29 N6 Co1 127.0(2) . 3_445 ? C33' N7 C33 58.1(8) . . ? C33' N7 C31 72.0(6) . . ? C33 N7 C31 105.1(7) . . ? C33' N7 C31' 107.0(6) . . ? C33 N7 C31' 79.8(8) . . ? C31 N7 C31' 64.9(6) . . ? C33' N7 C24 128.6(5) . . ? C33 N7 C24 129.8(6) . . ? C31 N7 C24 124.7(5) . . ? C31' N7 C24 124.4(5) . . ? C33 N8 C32 106.2(12) . . ? C33' N8' C32' 105.7(10) . . ? O3 C1 O4 119.7(4) . . ? O3 C1 C2 122.2(4) . . ? O4 C1 C2 118.1(4) . . ? C8 C2 C3 119.0(3) . . ? C8 C2 C1 121.2(3) . . ? C3 C2 C1 119.8(3) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C6 118.9(3) . . ? C3 C4 C5 119.6(4) . . ? C6 C4 C5 121.3(4) . . ? O6 C5 O5 122.8(4) . . ? O6 C5 C4 120.4(4) . . ? O5 C5 C4 116.6(4) . . ? C7 C6 C4 120.9(3) . . ? C7 C6 H6 119.6 . . ? C4 C6 H6 119.6 . . ? C6 C7 C8 119.3(3) . . ? C6 C7 C9 120.9(3) . . ? C8 C7 C9 119.8(3) . . ? C2 C8 C7 121.0(3) . . ? C2 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? O2 C9 O1 122.5(4) . . ? O2 C9 C7 121.0(4) . . ? O1 C9 C7 116.5(3) . . ? C11 C10 N1 110.0(3) . . ? C11 C10 H10 125.0 . . ? N1 C10 H10 125.0 . . ? C10 C11 N2 106.2(3) . . ? C10 C11 H11 126.9 . . ? N2 C11 H11 126.9 . . ? N1 C12 N2 111.7(3) . . ? N1 C12 H12 124.1 . . ? N2 C12 H12 124.1 . . ? C14 C13 C18 121.3(3) . . ? C14 C13 N2 121.2(3) . . ? C18 C13 N2 117.5(3) . . ? C13 C14 C15 119.8(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 119.0(3) . . ? C16 C15 C22 120.0(3) . . ? C14 C15 C22 121.0(3) . . ? C17 C16 C15 120.2(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 120.9(3) . . ? C18 C17 N3 118.4(3) . . ? C16 C17 N3 120.7(3) . . ? C17 C18 C13 118.7(3) . . ? C17 C18 H18 120.7 . . ? C13 C18 H18 120.7 . . ? N4 C19 N3 112.4(4) . . ? N4 C19 H19 123.8 . . ? N3 C19 H19 123.8 . . ? C21 C20 N4 110.7(4) . . ? C21 C20 H20 124.7 . . ? N4 C20 H20 124.7 . . ? C20 C21 N3 106.2(4) . . ? C20 C21 H21 126.9 . . ? N3 C21 H21 126.9 . . ? C23 C22 C27 118.2(3) . . ? C23 C22 C15 121.2(3) . . ? C27 C22 C15 120.4(3) . . ? C24 C23 C22 120.3(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 121.6(3) . . ? C23 C24 N7 118.6(3) . . ? C25 C24 N7 119.6(3) . . ? C26 C25 C24 117.7(3) . . ? C26 C25 H25 121.1 . . ? C24 C25 H25 121.1 . . ? C27 C26 C25 121.4(3) . . ? C27 C26 N5 119.0(3) . . ? C25 C26 N5 119.6(3) . . ? C26 C27 C22 120.7(3) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? C29 C28 N5 106.0(4) . . ? C29 C28 H28 127.0 . . ? N5 C28 H28 127.0 . . ? C28 C29 N6 110.3(3) . . ? C28 C29 H29 124.9 . . ? N6 C29 H29 124.9 . . ? N6 C30 N5 111.8(3) . . ? N6 C30 H30 124.1 . . ? N5 C30 H30 124.1 . . ? C32 C31 N7 109.9(9) . . ? C32 C31 H31 125.0 . . ? N7 C31 H31 125.0 . . ? C31 C32 N8 107.9(11) . . ? C31 C32 H32 126.1 . . ? N8 C32 H32 126.1 . . ? N7 C33 N8 110.7(11) . . ? N7 C33 H33 124.7 . . ? N8 C33 H33 124.7 . . ? C32' C31' N7 102.4(8) . . ? C32' C31' H31' 128.8 . . ? N7 C31' H31' 128.8 . . ? N8' C32' C31' 110.3(10) . . ? N8' C32' H32' 124.9 . . ? C31' C32' H32' 124.9 . . ? N7 C33' N8' 114.6(10) . . ? N7 C33' H33' 122.7 . . ? N8' C33' H33' 122.7 . . ? 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 O5 Co1 O1 C9 48.8(3) 4_557 . . . ? N6 Co1 O1 C9 -175.3(3) 3 . . . ? N1 Co1 O1 C9 -67.4(3) . . . . ? O4 Co2 O3 C1 -4.9(2) . . . . ? O4 Co2 O3 C1 176.4(2) 2_657 . . . ? N4 Co2 O3 C1 86.5(3) 3_545 . . . ? N4 Co2 O3 C1 -20.7(4) 4_547 . . . ? O3 Co2 O3 C1 -125.1(3) 2_657 . . . ? C1 Co2 O3 C1 -151.2(2) 2_657 . . . ? O4 Co2 O4 C1 44.4(3) 2_657 . . . ? N4 Co2 O4 C1 -87.5(3) 3_545 . . . ? N4 Co2 O4 C1 176.4(3) 4_547 . . . ? O3 Co2 O4 C1 4.9(2) . . . . ? O3 Co2 O4 C1 83.3(3) 2_657 . . . ? C1 Co2 O4 C1 86.7(4) 2_657 . . . ? O1 Co1 N1 C12 125.8(3) . . . . ? O5 Co1 N1 C12 -4.4(3) 4_557 . . . ? N6 Co1 N1 C12 -128.5(3) 3 . . . ? O1 Co1 N1 C10 -36.4(4) . . . . ? O5 Co1 N1 C10 -166.5(4) 4_557 . . . ? N6 Co1 N1 C10 69.3(4) 3 . . . ? Co2 O3 C1 O4 8.2(4) . . . . ? Co2 O3 C1 C2 -170.6(3) . . . . ? Co2 O4 C1 O3 -8.7(4) . . . . ? Co2 O4 C1 C2 170.1(3) . . . . ? O3 C1 C2 C8 7.0(6) . . . . ? O4 C1 C2 C8 -171.8(4) . . . . ? O3 C1 C2 C3 -175.6(4) . . . . ? O4 C1 C2 C3 5.7(6) . . . . ? C8 C2 C3 C4 -0.4(6) . . . . ? C1 C2 C3 C4 -177.9(3) . . . . ? C2 C3 C4 C6 -0.5(6) . . . . ? C2 C3 C4 C5 174.8(3) . . . . ? Co1 O5 C5 O6 23.0(5) 4_547 . . . ? Co1 O5 C5 C4 -152.2(3) 4_547 . . . ? C3 C4 C5 O6 -163.7(4) . . . . ? C6 C4 C5 O6 11.5(6) . . . . ? C3 C4 C5 O5 11.6(5) . . . . ? C6 C4 C5 O5 -173.2(4) . . . . ? C3 C4 C6 C7 1.2(6) . . . . ? C5 C4 C6 C7 -174.0(4) . . . . ? C4 C6 C7 C8 -0.9(6) . . . . ? C4 C6 C7 C9 177.3(3) . . . . ? C3 C2 C8 C7 0.7(6) . . . . ? C1 C2 C8 C7 178.2(3) . . . . ? C6 C7 C8 C2 -0.1(6) . . . . ? C9 C7 C8 C2 -178.3(3) . . . . ? Co1 O1 C9 O2 -6.3(5) . . . . ? Co1 O1 C9 C7 174.4(3) . . . . ? C6 C7 C9 O2 12.1(6) . . . . ? C8 C7 C9 O2 -169.8(4) . . . . ? C6 C7 C9 O1 -168.6(4) . . . . ? C8 C7 C9 O1 9.5(5) . . . . ? C12 N1 C10 C11 -0.8(5) . . . . ? Co1 N1 C10 C11 163.8(3) . . . . ? N1 C10 C11 N2 0.5(5) . . . . ? C12 N2 C11 C10 -0.1(5) . . . . ? C13 N2 C11 C10 -178.5(4) . . . . ? C10 N1 C12 N2 0.8(5) . . . . ? Co1 N1 C12 N2 -165.0(3) . . . . ? C11 N2 C12 N1 -0.5(5) . . . . ? C13 N2 C12 N1 178.1(3) . . . . ? C12 N2 C13 C14 149.5(4) . . . . ? C11 N2 C13 C14 -32.3(6) . . . . ? C12 N2 C13 C18 -32.7(6) . . . . ? C11 N2 C13 C18 145.5(4) . . . . ? C18 C13 C14 C15 2.7(6) . . . . ? N2 C13 C14 C15 -179.6(3) . . . . ? C13 C14 C15 C16 1.6(6) . . . . ? C13 C14 C15 C22 179.9(3) . . . . ? C14 C15 C16 C17 -3.6(6) . . . . ? C22 C15 C16 C17 178.1(4) . . . . ? C15 C16 C17 C18 1.4(6) . . . . ? C15 C16 C17 N3 -176.2(4) . . . . ? C19 N3 C17 C18 16.5(6) . . . . ? C21 N3 C17 C18 -156.5(5) . . . . ? C19 N3 C17 C16 -165.8(4) . . . . ? C21 N3 C17 C16 21.2(7) . . . . ? C16 C17 C18 C13 2.9(6) . . . . ? N3 C17 C18 C13 -179.5(4) . . . . ? C14 C13 C18 C17 -4.9(6) . . . . ? N2 C13 C18 C17 177.2(4) . . . . ? C20 N4 C19 N3 -0.7(5) . . . . ? Co2 N4 C19 N3 165.8(3) 3_455 . . . ? C21 N3 C19 N4 0.8(5) . . . . ? C17 N3 C19 N4 -173.5(4) . . . . ? C19 N4 C20 C21 0.3(6) . . . . ? Co2 N4 C20 C21 -163.5(4) 3_455 . . . ? N4 C20 C21 N3 0.2(7) . . . . ? C19 N3 C21 C20 -0.6(6) . . . . ? C17 N3 C21 C20 173.4(5) . . . . ? C16 C15 C22 C23 157.0(4) . . . . ? C14 C15 C22 C23 -21.3(6) . . . . ? C16 C15 C22 C27 -18.3(5) . . . . ? C14 C15 C22 C27 163.5(4) . . . . ? C27 C22 C23 C24 -1.2(6) . . . . ? C15 C22 C23 C24 -176.5(3) . . . . ? C22 C23 C24 C25 1.0(6) . . . . ? C22 C23 C24 N7 176.3(3) . . . . ? C33' N7 C24 C23 -135.5(8) . . . . ? C33 N7 C24 C23 146.9(12) . . . . ? C31 N7 C24 C23 -41.3(7) . . . . ? C31' N7 C24 C23 40.0(7) . . . . ? C33' N7 C24 C25 40.0(9) . . . . ? C33 N7 C24 C25 -37.7(13) . . . . ? C31 N7 C24 C25 134.1(6) . . . . ? C31' N7 C24 C25 -144.6(6) . . . . ? C23 C24 C25 C26 -0.7(6) . . . . ? N7 C24 C25 C26 -176.0(3) . . . . ? C24 C25 C26 C27 0.7(6) . . . . ? C24 C25 C26 N5 177.9(3) . . . . ? C30 N5 C26 C27 -29.6(6) . . . . ? C28 N5 C26 C27 148.6(4) . . . . ? C30 N5 C26 C25 153.1(4) . . . . ? C28 N5 C26 C25 -28.7(6) . . . . ? C25 C26 C27 C22 -1.0(6) . . . . ? N5 C26 C27 C22 -178.2(3) . . . . ? C23 C22 C27 C26 1.2(5) . . . . ? C15 C22 C27 C26 176.5(3) . . . . ? C30 N5 C28 C29 -0.8(5) . . . . ? C26 N5 C28 C29 -179.3(4) . . . . ? N5 C28 C29 N6 0.3(5) . . . . ? C30 N6 C29 C28 0.3(5) . . . . ? Co1 N6 C29 C28 -176.1(3) 3_445 . . . ? C29 N6 C30 N5 -0.9(5) . . . . ? Co1 N6 C30 N5 175.5(2) 3_445 . . . ? C28 N5 C30 N6 1.1(5) . . . . ? C26 N5 C30 N6 179.5(3) . . . . ? C33' N7 C31 C32 -52.9(13) . . . . ? C33 N7 C31 C32 -4.4(16) . . . . ? C31' N7 C31 C32 66.5(13) . . . . ? C24 N7 C31 C32 -177.9(12) . . . . ? N7 C31 C32 N8 2(3) . . . . ? C33 N8 C32 C31 1(4) . . . . ? C33' N7 C33 N8 62(2) . . . . ? C31 N7 C33 N8 5(2) . . . . ? C31' N7 C33 N8 -55(2) . . . . ? C24 N7 C33 N8 178.2(18) . . . . ? C32 N8 C33 N7 -4(4) . . . . ? C33' N7 C31' C32' 2.9(15) . . . . ? C33 N7 C31' C32' 54.9(14) . . . . ? C31 N7 C31' C32' -57.1(13) . . . . ? C24 N7 C31' C32' -173.4(12) . . . . ? C33' N8' C32' C31' 1(4) . . . . ? N7 C31' C32' N8' -2(3) . . . . ? C33 N7 C33' N8' -68.7(16) . . . . ? C31 N7 C33' N8' 52.8(15) . . . . ? C31' N7 C33' N8' -2.8(17) . . . . ? C24 N7 C33' N8' 173.3(14) . . . . ? C32' N8' C33' N7 1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.882 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.084 _database_code_depnum_ccdc_archive 'CCDC 942557' ####################################################################### # # 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_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H26 Co2 N8 O9, 2H2O' _chemical_formula_sum 'C33 H30 Co2 N8 O11' _chemical_formula_weight 832.51 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pccn ' _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 20.0960(10) _cell_length_b 23.0880(10) _cell_length_c 14.6160(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6781.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9963 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 28.29 _exptl_crystal_description needle-like _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 1.054 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7428 _exptl_absorpt_correction_T_max 0.8169 _exptl_absorpt_process_details sadabs(Bruker,2000) _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 36643 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6018 _reflns_number_gt 5037 _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^)+(0.0663P)^2^+8.0178P] 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 6018 _refine_ls_number_parameters 515 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1555 _refine_ls_wR_factor_gt 0.1499 _refine_ls_goodness_of_fit_ref 1.337 _refine_ls_restrained_S_all 1.349 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.41631(2) 0.09138(2) 0.32661(3) 0.02737(17) Uani 1 1 d U . . Co2 Co 0.41196(2) 0.09195(2) 0.08505(3) 0.02782(17) Uani 1 1 d . . . O1 O 0.47085(16) 0.0705(2) -0.1226(2) 0.0767(12) Uani 1 1 d . . . O2 O 0.38163(14) 0.10222(12) -0.04891(18) 0.0391(6) Uani 1 1 d . . . O3 O 0.47555(14) 0.07649(18) -0.4547(2) 0.0629(10) Uani 1 1 d . . . O4 O 0.38797(13) 0.10428(12) -0.53594(17) 0.0368(6) Uani 1 1 d . . . O5 O 0.17282(12) 0.12829(11) -0.21803(17) 0.0322(6) Uani 1 1 d . . . O6 O 0.17454(12) 0.13106(12) -0.37155(18) 0.0356(6) Uani 1 1 d . . . O7 O 0.45632(14) 0.07003(12) 0.20365(17) 0.0385(6) Uani 1 1 d U . . O8 O 0.51145(15) 0.04859(14) 0.3828(2) 0.0498(7) Uani 1 1 d U . . H8B H 0.5420 0.0739 0.3874 0.060 Uiso 1 1 d R C . H8C H 0.5035 0.0342 0.4353 0.060 Uiso 1 1 d R . . O9 O 0.5088(3) 0.0466(2) 0.0386(4) 0.1154(17) Uani 1 1 d U . . H9A H 0.5370 0.0359 0.0788 0.138 Uiso 1 1 d R C . H9B H 0.5168 0.0426 -0.0175 0.138 Uiso 1 1 d R . . O12 O 0.6464(3) 0.0825(4) 0.3364(8) 0.095(3) Uani 0.50 1 d P . . O13 O 0.7219(15) 0.7667(14) 0.5701(15) 0.29(2) Uani 0.50 1 d P . . O14A O 0.6130(10) 0.0699(8) 0.1431(13) 0.101(6) Uani 0.35 1 d P A 1 O14B O 0.5951(8) 0.0786(7) 0.1934(13) 0.084(5) Uani 0.35 1 d P B 2 O14C O 0.5223(9) 0.0504(8) 0.1790(12) 0.105(5) Uani 0.30 1 d PU C 3 N11 N 0.33817(14) -0.08351(13) 0.3482(2) 0.0307(7) Uani 1 1 d . C . N12 N 0.36568(15) 0.00771(13) 0.3335(2) 0.0329(7) Uani 1 1 d . . . N21 N 0.46357(14) -0.25806(12) 0.4231(2) 0.0249(6) Uani 1 1 d . . . N22 N 0.53789(14) -0.32794(12) 0.4260(2) 0.0297(7) Uani 1 1 d . . . N31 N 0.53770(14) 0.24471(12) 0.3281(2) 0.0275(6) Uani 1 1 d . C . N32 N 0.46284(15) 0.17472(13) 0.3223(2) 0.0306(7) Uani 1 1 d . . . N41 N 0.66457(15) 0.41709(12) 0.4119(2) 0.0308(7) Uani 1 1 d . . . N42 N 0.63745(16) 0.50892(13) 0.4225(2) 0.0336(7) Uani 1 1 d . . . C1 C 0.28180(16) -0.23345(14) 0.3954(2) 0.0247(7) Uani 1 1 d . . . C2 C 0.28157(16) -0.17464(14) 0.3753(2) 0.0274(7) Uani 1 1 d . . . H2 H 0.2415 -0.1559 0.3640 0.033 Uiso 1 1 calc R . . C3 C 0.34057(16) -0.14382(14) 0.3719(2) 0.0261(7) Uani 1 1 d . . . C4 C 0.40132(17) -0.17042(14) 0.3877(3) 0.0271(7) Uani 1 1 d . . . H4 H 0.4409 -0.1496 0.3847 0.033 Uiso 1 1 calc R . . C5 C 0.40134(16) -0.22929(14) 0.4081(2) 0.0234(7) Uani 1 1 d . . . C6 C 0.34257(16) -0.26054(14) 0.4128(2) 0.0250(7) Uani 1 1 d . . . H6 H 0.3436 -0.2997 0.4277 0.030 Uiso 1 1 calc R . . C7 C 0.71885(16) 0.26740(14) 0.3590(2) 0.0252(7) Uani 1 1 d . . . C8 C 0.65795(17) 0.24126(15) 0.3388(2) 0.0271(7) Uani 1 1 d . . . H8 H 0.6565 0.2026 0.3209 0.033 Uiso 1 1 calc R . . C9 C 0.59996(16) 0.27291(15) 0.3457(2) 0.0257(7) Uani 1 1 d . . . C10 C 0.60041(17) 0.33117(14) 0.3707(2) 0.0274(7) Uani 1 1 d . . . H10 H 0.5610 0.3519 0.3767 0.033 Uiso 1 1 calc R . . C11 C 0.66174(17) 0.35721(14) 0.3863(2) 0.0265(7) Uani 1 1 d . . . C12 C 0.72043(16) 0.32582(14) 0.3811(2) 0.0271(7) Uani 1 1 d . . . H12 H 0.7609 0.3440 0.3924 0.033 Uiso 1 1 calc R . . C13 C 0.37737(18) 0.10107(16) -0.2095(2) 0.0306(8) Uani 1 1 d . . . C14 C 0.41048(18) 0.09363(16) -0.2909(3) 0.0315(9) Uani 1 1 d . . . H14 H 0.4549 0.0825 -0.2903 0.038 Uiso 1 1 calc R . . C15 C 0.37865(17) 0.10251(15) -0.3744(2) 0.0285(8) Uani 1 1 d . . . C16 C 0.31146(17) 0.11779(15) -0.3754(2) 0.0285(8) Uani 1 1 d . . . H16 H 0.2898 0.1241 -0.4308 0.034 Uiso 1 1 calc R . . C17 C 0.27679(17) 0.12359(15) -0.2933(2) 0.0273(8) Uani 1 1 d . . . C18 C 0.31015(18) 0.11693(16) -0.2105(2) 0.0296(8) Uani 1 1 d . . . H18 H 0.2877 0.1230 -0.1557 0.036 Uiso 1 1 calc R . . C19 C 0.41264(18) 0.09046(17) -0.1190(3) 0.0357(9) Uani 1 1 d . . . C20 C 0.41601(17) 0.09357(15) -0.4627(3) 0.0288(8) Uani 1 1 d . . . C21 C 0.20171(17) 0.12916(14) -0.2943(2) 0.0262(7) Uani 1 1 d . . . C101 C 0.38439(19) -0.04296(15) 0.3627(3) 0.0339(8) Uani 1 1 d . C . H101 H 0.4252 -0.0501 0.3904 0.041 Uiso 1 1 calc R . . C102 C 0.30287(19) -0.00114(17) 0.2973(3) 0.0418(10) Uani 1 1 d . C . H102 H 0.2766 0.0275 0.2710 0.050 Uiso 1 1 calc R . . C103 C 0.28544(19) -0.05651(17) 0.3054(3) 0.0428(10) Uani 1 1 d . . . H103 H 0.2459 -0.0735 0.2862 0.051 Uiso 1 1 calc R C . C201 C 0.47638(17) -0.31462(15) 0.4055(2) 0.0282(8) Uani 1 1 d . . . H201 H 0.4455 -0.3406 0.3818 0.034 Uiso 1 1 calc R . . C202 C 0.56610(18) -0.27748(16) 0.4584(3) 0.0361(9) Uani 1 1 d . . . H202 H 0.6097 -0.2739 0.4788 0.043 Uiso 1 1 calc R . . C203 C 0.52120(17) -0.23398(16) 0.4563(3) 0.0320(8) Uani 1 1 d . . . H203 H 0.5279 -0.1957 0.4737 0.038 Uiso 1 1 calc R . . C301 C 0.52491(17) 0.18735(15) 0.3417(3) 0.0306(8) Uani 1 1 d . C . H301 H 0.5562 0.1606 0.3621 0.037 Uiso 1 1 calc R . . C302 C 0.43435(19) 0.22590(17) 0.2947(3) 0.0372(9) Uani 1 1 d . C . H302 H 0.3904 0.2301 0.2760 0.045 Uiso 1 1 calc R . . C303 C 0.47961(18) 0.26938(17) 0.2988(3) 0.0356(9) Uani 1 1 d . . . H303 H 0.4726 0.3082 0.2845 0.043 Uiso 1 1 calc R C . C401 C 0.62008(18) 0.45856(15) 0.3909(3) 0.0320(8) Uani 1 1 d . . . H401 H 0.5814 0.4519 0.3576 0.038 Uiso 1 1 calc R . . C402 C 0.6974(2) 0.50013(16) 0.4657(3) 0.0489(12) Uani 1 1 d . . . H402 H 0.7221 0.5287 0.4951 0.059 Uiso 1 1 calc R . . C403 C 0.7151(2) 0.44423(17) 0.4593(3) 0.0505(12) Uani 1 1 d . . . H403 H 0.7536 0.4272 0.4821 0.061 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 0.0262(3) 0.0284(3) 0.0276(3) 0.00230(19) -0.00344(19) -0.00669(19) Co2 0.0292(3) 0.0274(3) 0.0269(3) 0.00036(19) -0.00101(19) -0.00948(19) O1 0.0357(18) 0.141(4) 0.054(2) 0.009(2) -0.0096(15) 0.027(2) O2 0.0403(15) 0.0501(16) 0.0269(14) 0.0024(12) -0.0036(12) -0.0044(13) O3 0.0287(15) 0.122(3) 0.0379(17) -0.0118(18) -0.0016(13) 0.0207(17) O4 0.0337(14) 0.0497(16) 0.0270(14) 0.0005(12) 0.0022(11) 0.0056(12) O5 0.0265(13) 0.0354(14) 0.0347(14) 0.0021(11) 0.0050(11) 0.0036(11) O6 0.0247(12) 0.0462(16) 0.0358(15) 0.0063(12) -0.0029(11) -0.0002(11) O7 0.0394(16) 0.0414(16) 0.0346(12) -0.0012(11) -0.0040(10) 0.0016(13) O8 0.0433(15) 0.0582(19) 0.0477(17) 0.0054(15) -0.0009(13) 0.0028(13) O9 0.099(3) 0.129(3) 0.118(3) -0.004(3) 0.013(3) 0.010(3) O12 0.027(3) 0.084(6) 0.173(9) -0.042(6) 0.024(5) -0.011(3) O13 0.34(5) 0.28(4) 0.240(19) -0.11(2) 0.01(2) -0.16(3) O14A 0.107(15) 0.079(9) 0.117(15) 0.006(11) -0.045(11) 0.042(10) O14B 0.065(8) 0.064(9) 0.122(15) 0.033(9) 0.026(9) 0.012(7) O14C 0.114(9) 0.096(8) 0.106(8) -0.006(7) -0.014(7) 0.018(7) N11 0.0221(14) 0.0281(16) 0.0417(18) 0.0054(13) -0.0009(13) 0.0019(12) N12 0.0313(16) 0.0228(16) 0.0446(19) 0.0032(13) -0.0023(14) -0.0039(13) N21 0.0205(14) 0.0207(14) 0.0335(15) 0.0004(12) 0.0009(12) 0.0023(11) N22 0.0251(15) 0.0273(15) 0.0367(16) -0.0015(13) -0.0011(13) 0.0054(12) N31 0.0236(14) 0.0226(15) 0.0362(16) 0.0001(12) -0.0012(12) -0.0037(12) N32 0.0253(15) 0.0305(16) 0.0362(17) -0.0034(13) -0.0012(13) -0.0058(13) N41 0.0266(15) 0.0227(15) 0.0430(18) -0.0001(13) -0.0101(13) -0.0001(12) N42 0.0348(16) 0.0224(15) 0.0437(18) -0.0022(13) -0.0080(14) 0.0064(13) C1 0.0210(16) 0.0216(16) 0.0315(18) -0.0016(14) 0.0016(14) -0.0016(13) C2 0.0198(16) 0.0223(17) 0.040(2) 0.0017(15) -0.0013(14) 0.0034(13) C3 0.0269(17) 0.0178(16) 0.0335(19) 0.0016(14) 0.0017(14) -0.0004(13) C4 0.0200(16) 0.0215(17) 0.040(2) 0.0025(15) 0.0019(14) -0.0015(13) C5 0.0181(15) 0.0239(17) 0.0283(18) -0.0004(13) 0.0014(13) 0.0050(13) C6 0.0244(17) 0.0172(16) 0.0333(18) 0.0022(13) 0.0002(14) 0.0015(13) C7 0.0216(16) 0.0226(16) 0.0314(18) 0.0024(14) 0.0007(14) 0.0017(14) C8 0.0266(17) 0.0193(16) 0.0355(19) 0.0001(14) 0.0008(15) -0.0021(14) C9 0.0208(16) 0.0265(18) 0.0297(18) 0.0023(14) -0.0017(14) -0.0036(14) C10 0.0227(16) 0.0234(17) 0.036(2) 0.0015(14) -0.0019(14) 0.0018(13) C11 0.0281(17) 0.0175(16) 0.0340(18) 0.0003(14) -0.0032(14) 0.0003(13) C12 0.0213(16) 0.0219(16) 0.0381(19) 0.0016(15) -0.0039(14) -0.0024(13) C13 0.0230(18) 0.035(2) 0.033(2) 0.0009(15) -0.0039(15) -0.0040(15) C14 0.0219(18) 0.038(2) 0.035(2) -0.0014(16) -0.0014(14) -0.0010(15) C15 0.0226(17) 0.0317(18) 0.0312(19) -0.0011(15) 0.0014(15) -0.0044(14) C16 0.0260(17) 0.0315(19) 0.0279(18) 0.0020(15) -0.0018(14) -0.0020(14) C17 0.0236(17) 0.0272(18) 0.0309(19) 0.0015(14) -0.0003(14) -0.0008(14) C18 0.0262(18) 0.0322(19) 0.0305(19) -0.0009(15) 0.0009(14) -0.0043(15) C19 0.028(2) 0.042(2) 0.037(2) 0.0047(17) -0.0058(16) -0.0051(16) C20 0.0250(18) 0.035(2) 0.0265(19) -0.0024(15) -0.0009(14) -0.0032(14) C21 0.0236(17) 0.0225(17) 0.033(2) 0.0017(14) 0.0002(14) 0.0016(14) C101 0.034(2) 0.0234(18) 0.044(2) 0.0048(16) -0.0083(17) -0.0007(15) C102 0.029(2) 0.028(2) 0.068(3) 0.0126(19) -0.0040(19) 0.0010(16) C103 0.0243(19) 0.030(2) 0.074(3) 0.014(2) -0.0100(19) -0.0020(16) C201 0.0235(17) 0.0228(17) 0.038(2) -0.0023(15) -0.0010(14) 0.0027(14) C202 0.0241(18) 0.036(2) 0.048(2) -0.0077(17) -0.0092(16) 0.0036(16) C203 0.0250(18) 0.0279(18) 0.043(2) -0.0064(16) -0.0037(15) -0.0009(14) C301 0.0250(18) 0.0261(18) 0.041(2) 0.0007(15) -0.0031(15) -0.0036(14) C302 0.0255(18) 0.039(2) 0.047(2) 0.0019(17) -0.0088(16) -0.0009(17) C303 0.0267(19) 0.031(2) 0.049(2) 0.0028(17) -0.0064(16) 0.0013(16) C401 0.0297(19) 0.0254(18) 0.041(2) -0.0023(16) -0.0084(16) 0.0024(15) C402 0.044(2) 0.0247(19) 0.078(3) -0.010(2) -0.030(2) 0.0044(17) C403 0.042(2) 0.028(2) 0.083(3) -0.011(2) -0.034(2) 0.0070(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O7 2.030(3) . ? Co1 O5 2.088(3) 7_656 ? Co1 O4 2.109(3) 1_556 ? Co1 N32 2.140(3) . ? Co1 N12 2.186(3) . ? Co1 O8 2.304(3) . ? Co2 O7 2.014(3) . ? Co2 O6 2.059(3) 7_656 ? Co2 O2 2.064(3) . ? Co2 N22 2.113(3) 4_655 ? Co2 N42 2.162(3) 4_645 ? Co2 O9 2.312(5) . ? O1 C19 1.258(5) . ? O2 C19 1.229(5) . ? O3 C20 1.265(4) . ? O4 C20 1.235(5) . ? O4 Co1 2.109(3) 1_554 ? O5 C21 1.257(4) . ? O5 Co1 2.088(3) 7_655 ? O6 C21 1.255(4) . ? O6 Co2 2.059(3) 7_655 ? O7 O14C 1.447(19) . ? O8 H8B 0.8501 . ? O8 H8C 0.8500 . ? O9 H9A 0.8528 . ? O9 H9B 0.8409 . ? O13 O13 1.37(6) 2_665 ? N11 C101 1.336(5) . ? N11 C103 1.379(5) . ? N11 C3 1.436(4) . ? N12 C101 1.301(5) . ? N12 C102 1.384(5) . ? N21 C201 1.356(4) . ? N21 C203 1.373(4) . ? N21 C5 1.433(4) . ? N22 C201 1.309(4) . ? N22 C202 1.379(5) . ? N22 Co2 2.113(3) 4_645 ? N31 C301 1.364(5) . ? N31 C303 1.368(5) . ? N31 C9 1.434(4) . ? N32 C301 1.312(5) . ? N32 C302 1.374(5) . ? N41 C401 1.346(4) . ? N41 C403 1.380(5) . ? N41 C11 1.434(4) . ? N42 C401 1.299(5) . ? N42 C402 1.376(5) . ? N42 Co2 2.162(3) 4_655 ? C1 C2 1.389(5) . ? C1 C6 1.396(5) . ? C1 C1 1.489(6) 2_545 ? C2 C3 1.384(5) . ? C2 H2 0.9300 . ? C3 C4 1.386(5) . ? C4 C5 1.391(5) . ? C4 H4 0.9300 . ? C5 C6 1.386(5) . ? C6 H6 0.9300 . ? C7 C12 1.387(5) . ? C7 C8 1.396(5) . ? C7 C7 1.488(6) 2_655 ? C8 C9 1.379(5) . ? C8 H8 0.9300 . ? C9 C10 1.394(5) . ? C10 C11 1.390(5) . ? C10 H10 0.9300 . ? C11 C12 1.386(5) . ? C12 H12 0.9300 . ? C13 C14 1.375(5) . ? C13 C18 1.400(5) . ? C13 C19 1.521(5) . ? C14 C15 1.393(5) . ? C14 H14 0.9300 . ? C15 C16 1.396(5) . ? C15 C20 1.507(5) . ? C16 C17 1.394(5) . ? C16 H16 0.9300 . ? C17 C18 1.392(5) . ? C17 C21 1.514(5) . ? C18 H18 0.9300 . ? C101 H101 0.9300 . ? C102 C103 1.331(6) . ? C102 H102 0.9300 . ? C103 H103 0.9300 . ? C201 H201 0.9300 . ? C202 C203 1.351(5) . ? C202 H202 0.9300 . ? C203 H203 0.9300 . ? C301 H301 0.9300 . ? C302 C303 1.356(5) . ? C302 H302 0.9300 . ? C303 H303 0.9300 . ? C401 H401 0.9300 . ? C402 C403 1.342(5) . ? C402 H402 0.9300 . ? C403 H403 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 O7 Co1 O5 99.34(11) . 7_656 ? O7 Co1 O4 169.94(11) . 1_556 ? O5 Co1 O4 90.48(10) 7_656 1_556 ? O7 Co1 N32 91.11(12) . . ? O5 Co1 N32 89.93(11) 7_656 . ? O4 Co1 N32 91.09(11) 1_556 . ? O7 Co1 N12 90.60(12) . . ? O5 Co1 N12 88.61(11) 7_656 . ? O4 Co1 N12 87.44(12) 1_556 . ? N32 Co1 N12 177.92(12) . . ? O7 Co1 O8 83.28(11) . . ? O5 Co1 O8 176.77(11) 7_656 . ? O4 Co1 O8 86.83(11) 1_556 . ? N32 Co1 O8 91.91(12) . . ? N12 Co1 O8 89.48(12) . . ? O7 Co2 O6 102.63(11) . 7_656 ? O7 Co2 O2 167.43(12) . . ? O6 Co2 O2 89.57(11) 7_656 . ? O7 Co2 N22 94.29(12) . 4_655 ? O6 Co2 N22 92.43(11) 7_656 4_655 ? O2 Co2 N22 88.13(11) . 4_655 ? O7 Co2 N42 91.39(12) . 4_645 ? O6 Co2 N42 90.96(12) 7_656 4_645 ? O2 Co2 N42 85.30(12) . 4_645 ? N22 Co2 N42 172.59(12) 4_655 4_645 ? O7 Co2 O9 76.49(17) . . ? O6 Co2 O9 178.81(16) 7_656 . ? O2 Co2 O9 91.27(17) . . ? N22 Co2 O9 88.43(15) 4_655 . ? N42 Co2 O9 88.27(16) 4_645 . ? C19 O2 Co2 128.0(3) . . ? C20 O4 Co1 132.4(2) . 1_554 ? C21 O5 Co1 132.8(2) . 7_655 ? C21 O6 Co2 129.0(2) . 7_655 ? O14C O7 Co2 105.7(7) . . ? O14C O7 Co1 131.3(7) . . ? Co2 O7 Co1 121.73(14) . . ? Co1 O8 H8B 109.3 . . ? Co1 O8 H8C 109.5 . . ? H8B O8 H8C 109.5 . . ? Co2 O9 H9A 119.2 . . ? Co2 O9 H9B 119.8 . . ? H9A O9 H9B 120.8 . . ? C101 N11 C103 106.8(3) . . ? C101 N11 C3 128.2(3) . . ? C103 N11 C3 125.0(3) . . ? C101 N12 C102 104.8(3) . . ? C101 N12 Co1 132.5(3) . . ? C102 N12 Co1 122.5(2) . . ? C201 N21 C203 107.3(3) . . ? C201 N21 C5 125.7(3) . . ? C203 N21 C5 127.0(3) . . ? C201 N22 C202 105.6(3) . . ? C201 N22 Co2 129.7(2) . 4_645 ? C202 N22 Co2 124.7(2) . 4_645 ? C301 N31 C303 106.8(3) . . ? C301 N31 C9 125.4(3) . . ? C303 N31 C9 127.7(3) . . ? C301 N32 C302 105.6(3) . . ? C301 N32 Co1 127.5(3) . . ? C302 N32 Co1 126.9(2) . . ? C401 N41 C403 106.3(3) . . ? C401 N41 C11 126.9(3) . . ? C403 N41 C11 126.8(3) . . ? C401 N42 C402 105.5(3) . . ? C401 N42 Co2 130.7(3) . 4_655 ? C402 N42 Co2 123.8(2) . 4_655 ? C2 C1 C6 118.7(3) . . ? C2 C1 C1 119.9(4) . 2_545 ? C6 C1 C1 121.4(4) . 2_545 ? C3 C2 C1 120.5(3) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 121.4(3) . . ? C2 C3 N11 118.6(3) . . ? C4 C3 N11 120.0(3) . . ? C3 C4 C5 118.0(3) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? C6 C5 C4 121.3(3) . . ? C6 C5 N21 119.7(3) . . ? C4 C5 N21 119.1(3) . . ? C5 C6 C1 120.2(3) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C12 C7 C8 119.3(3) . . ? C12 C7 C7 120.4(4) . 2_655 ? C8 C7 C7 120.3(4) . 2_655 ? C9 C8 C7 119.8(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 121.7(3) . . ? C8 C9 N31 118.9(3) . . ? C10 C9 N31 119.4(3) . . ? C11 C10 C9 117.8(3) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? C12 C11 C10 121.3(3) . . ? C12 C11 N41 119.0(3) . . ? C10 C11 N41 119.7(3) . . ? C11 C12 C7 120.1(3) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 C18 119.4(3) . . ? C14 C13 C19 120.5(3) . . ? C18 C13 C19 120.1(3) . . ? C13 C14 C15 121.2(3) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 119.4(3) . . ? C14 C15 C20 120.1(3) . . ? C16 C15 C20 120.5(3) . . ? C17 C16 C15 119.9(3) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 119.8(3) . . ? C18 C17 C21 119.8(3) . . ? C16 C17 C21 119.8(3) . . ? C17 C18 C13 120.2(3) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? O2 C19 O1 126.0(4) . . ? O2 C19 C13 116.9(3) . . ? O1 C19 C13 117.1(4) . . ? O4 C20 O3 125.0(4) . . ? O4 C20 C15 119.2(3) . . ? O3 C20 C15 115.8(3) . . ? O6 C21 O5 126.7(3) . . ? O6 C21 C17 116.5(3) . . ? O5 C21 C17 116.7(3) . . ? N12 C101 N11 112.2(3) . . ? N12 C101 H101 123.9 . . ? N11 C101 H101 123.9 . . ? C103 C102 N12 110.4(3) . . ? C103 C102 H102 124.8 . . ? N12 C102 H102 124.8 . . ? C102 C103 N11 105.8(3) . . ? C102 C103 H103 127.1 . . ? N11 C103 H103 127.1 . . ? N22 C201 N21 111.2(3) . . ? N22 C201 H201 124.4 . . ? N21 C201 H201 124.4 . . ? C203 C202 N22 110.2(3) . . ? C203 C202 H202 124.9 . . ? N22 C202 H202 124.9 . . ? C202 C203 N21 105.7(3) . . ? C202 C203 H203 127.1 . . ? N21 C203 H203 127.1 . . ? N32 C301 N31 111.3(3) . . ? N32 C301 H301 124.3 . . ? N31 C301 H301 124.3 . . ? C303 C302 N32 110.1(3) . . ? C303 C302 H302 124.9 . . ? N32 C302 H302 124.9 . . ? C302 C303 N31 106.1(3) . . ? C302 C303 H303 126.9 . . ? N31 C303 H303 126.9 . . ? N42 C401 N41 112.2(3) . . ? N42 C401 H401 123.9 . . ? N41 C401 H401 123.9 . . ? C403 C402 N42 110.0(3) . . ? C403 C402 H402 125.0 . . ? N42 C402 H402 125.0 . . ? C402 C403 N41 106.1(3) . . ? C402 C403 H403 127.0 . . ? N41 C403 H403 127.0 . . ? 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 O7 Co2 O2 C19 -18.1(7) . . . . ? O6 Co2 O2 C19 175.7(3) 7_656 . . . ? N22 Co2 O2 C19 83.3(3) 4_655 . . . ? N42 Co2 O2 C19 -93.3(3) 4_645 . . . ? O9 Co2 O2 C19 -5.1(3) . . . . ? O6 Co2 O7 O14C -171.3(8) 7_656 . . . ? O2 Co2 O7 O14C 22.9(10) . . . . ? N22 Co2 O7 O14C -77.8(8) 4_655 . . . ? N42 Co2 O7 O14C 97.4(8) 4_645 . . . ? O9 Co2 O7 O14C 9.5(8) . . . . ? O6 Co2 O7 Co1 -3.13(18) 7_656 . . . ? O2 Co2 O7 Co1 -168.9(4) . . . . ? N22 Co2 O7 Co1 90.33(17) 4_655 . . . ? N42 Co2 O7 Co1 -94.43(17) 4_645 . . . ? O9 Co2 O7 Co1 177.7(2) . . . . ? O5 Co1 O7 O14C 169.5(10) 7_656 . . . ? O4 Co1 O7 O14C -23.2(13) 1_556 . . . ? N32 Co1 O7 O14C 79.4(10) . . . . ? N12 Co1 O7 O14C -101.8(10) . . . . ? O8 Co1 O7 O14C -12.4(10) . . . . ? O5 Co1 O7 Co2 4.69(18) 7_656 . . . ? O4 Co1 O7 Co2 172.0(5) 1_556 . . . ? N32 Co1 O7 Co2 -85.42(17) . . . . ? N12 Co1 O7 Co2 93.38(17) . . . . ? O8 Co1 O7 Co2 -177.21(17) . . . . ? O7 Co1 N12 C101 86.1(4) . . . . ? O5 Co1 N12 C101 -174.5(4) 7_656 . . . ? O4 Co1 N12 C101 -84.0(4) 1_556 . . . ? N32 Co1 N12 C101 -129(3) . . . . ? O8 Co1 N12 C101 2.9(4) . . . . ? O7 Co1 N12 C102 -88.7(3) . . . . ? O5 Co1 N12 C102 10.6(3) 7_656 . . . ? O4 Co1 N12 C102 101.2(3) 1_556 . . . ? N32 Co1 N12 C102 56(3) . . . . ? O8 Co1 N12 C102 -172.0(3) . . . . ? O7 Co1 N32 C301 -79.6(3) . . . . ? O5 Co1 N32 C301 -178.9(3) 7_656 . . . ? O4 Co1 N32 C301 90.6(3) 1_556 . . . ? N12 Co1 N32 C301 136(3) . . . . ? O8 Co1 N32 C301 3.7(3) . . . . ? O7 Co1 N32 C302 97.4(3) . . . . ? O5 Co1 N32 C302 -2.0(3) 7_656 . . . ? O4 Co1 N32 C302 -92.5(3) 1_556 . . . ? N12 Co1 N32 C302 -47(4) . . . . ? O8 Co1 N32 C302 -179.3(3) . . . . ? C6 C1 C2 C3 0.5(5) . . . . ? C1 C1 C2 C3 -177.7(3) 2_545 . . . ? C1 C2 C3 C4 0.5(5) . . . . ? C1 C2 C3 N11 178.1(3) . . . . ? C101 N11 C3 C2 161.6(4) . . . . ? C103 N11 C3 C2 -17.9(6) . . . . ? C101 N11 C3 C4 -20.7(6) . . . . ? C103 N11 C3 C4 159.8(4) . . . . ? C2 C3 C4 C5 -0.7(5) . . . . ? N11 C3 C4 C5 -178.3(3) . . . . ? C3 C4 C5 C6 -0.1(5) . . . . ? C3 C4 C5 N21 178.9(3) . . . . ? C201 N21 C5 C6 28.8(5) . . . . ? C203 N21 C5 C6 -152.3(3) . . . . ? C201 N21 C5 C4 -150.3(3) . . . . ? C203 N21 C5 C4 28.7(5) . . . . ? C4 C5 C6 C1 1.2(5) . . . . ? N21 C5 C6 C1 -177.9(3) . . . . ? C2 C1 C6 C5 -1.3(5) . . . . ? C1 C1 C6 C5 176.9(2) 2_545 . . . ? C12 C7 C8 C9 -3.3(5) . . . . ? C7 C7 C8 C9 175.2(2) 2_655 . . . ? C7 C8 C9 C10 1.3(5) . . . . ? C7 C8 C9 N31 -177.7(3) . . . . ? C301 N31 C9 C8 28.8(5) . . . . ? C303 N31 C9 C8 -154.2(4) . . . . ? C301 N31 C9 C10 -150.2(4) . . . . ? C303 N31 C9 C10 26.9(5) . . . . ? C8 C9 C10 C11 1.7(5) . . . . ? N31 C9 C10 C11 -179.3(3) . . . . ? C9 C10 C11 C12 -2.7(5) . . . . ? C9 C10 C11 N41 179.9(3) . . . . ? C401 N41 C11 C12 155.0(4) . . . . ? C403 N41 C11 C12 -21.6(6) . . . . ? C401 N41 C11 C10 -27.6(6) . . . . ? C403 N41 C11 C10 155.8(4) . . . . ? C10 C11 C12 C7 0.7(5) . . . . ? N41 C11 C12 C7 178.1(3) . . . . ? C8 C7 C12 C11 2.3(5) . . . . ? C7 C7 C12 C11 -176.2(3) 2_655 . . . ? C18 C13 C14 C15 1.1(6) . . . . ? C19 C13 C14 C15 179.2(3) . . . . ? C13 C14 C15 C16 -1.7(6) . . . . ? C13 C14 C15 C20 -179.5(3) . . . . ? C14 C15 C16 C17 -0.5(5) . . . . ? C20 C15 C16 C17 177.4(3) . . . . ? C15 C16 C17 C18 3.2(5) . . . . ? C15 C16 C17 C21 -168.7(3) . . . . ? C16 C17 C18 C13 -3.8(5) . . . . ? C21 C17 C18 C13 168.1(3) . . . . ? C14 C13 C18 C17 1.7(6) . . . . ? C19 C13 C18 C17 -176.5(3) . . . . ? Co2 O2 C19 O1 -1.7(6) . . . . ? Co2 O2 C19 C13 178.4(2) . . . . ? C14 C13 C19 O2 174.6(4) . . . . ? C18 C13 C19 O2 -7.3(5) . . . . ? C14 C13 C19 O1 -5.4(6) . . . . ? C18 C13 C19 O1 172.8(4) . . . . ? Co1 O4 C20 O3 8.2(6) 1_554 . . . ? Co1 O4 C20 C15 -173.5(2) 1_554 . . . ? C14 C15 C20 O4 -176.6(4) . . . . ? C16 C15 C20 O4 5.6(5) . . . . ? C14 C15 C20 O3 1.8(5) . . . . ? C16 C15 C20 O3 -176.0(4) . . . . ? Co2 O6 C21 O5 -36.7(5) 7_655 . . . ? Co2 O6 C21 C17 139.2(3) 7_655 . . . ? Co1 O5 C21 O6 34.6(5) 7_655 . . . ? Co1 O5 C21 C17 -141.3(3) 7_655 . . . ? C18 C17 C21 O6 -175.3(3) . . . . ? C16 C17 C21 O6 -3.4(5) . . . . ? C18 C17 C21 O5 1.0(5) . . . . ? C16 C17 C21 O5 173.0(3) . . . . ? C102 N12 C101 N11 -0.2(5) . . . . ? Co1 N12 C101 N11 -175.8(3) . . . . ? C103 N11 C101 N12 0.4(5) . . . . ? C3 N11 C101 N12 -179.1(3) . . . . ? C101 N12 C102 C103 0.0(5) . . . . ? Co1 N12 C102 C103 176.0(3) . . . . ? N12 C102 C103 N11 0.3(5) . . . . ? C101 N11 C103 C102 -0.4(5) . . . . ? C3 N11 C103 C102 179.2(4) . . . . ? C202 N22 C201 N21 0.0(4) . . . . ? Co2 N22 C201 N21 179.8(2) 4_645 . . . ? C203 N21 C201 N22 0.6(4) . . . . ? C5 N21 C201 N22 179.7(3) . . . . ? C201 N22 C202 C203 -0.5(5) . . . . ? Co2 N22 C202 C203 179.6(3) 4_645 . . . ? N22 C202 C203 N21 0.9(5) . . . . ? C201 N21 C203 C202 -0.9(4) . . . . ? C5 N21 C203 C202 -180.0(3) . . . . ? C302 N32 C301 N31 0.2(4) . . . . ? Co1 N32 C301 N31 177.7(2) . . . . ? C303 N31 C301 N32 0.3(4) . . . . ? C9 N31 C301 N32 177.9(3) . . . . ? C301 N32 C302 C303 -0.7(5) . . . . ? Co1 N32 C302 C303 -178.2(3) . . . . ? N32 C302 C303 N31 0.9(5) . . . . ? C301 N31 C303 C302 -0.8(4) . . . . ? C9 N31 C303 C302 -178.2(3) . . . . ? C402 N42 C401 N41 0.9(5) . . . . ? Co2 N42 C401 N41 -178.8(3) 4_655 . . . ? C403 N41 C401 N42 -1.4(5) . . . . ? C11 N41 C401 N42 -178.5(3) . . . . ? C401 N42 C402 C403 0.0(6) . . . . ? Co2 N42 C402 C403 179.7(3) 4_655 . . . ? N42 C402 C403 N41 -0.8(6) . . . . ? C401 N41 C403 C402 1.3(5) . . . . ? C11 N41 C403 C402 178.5(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.946 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.108 #====END _database_code_depnum_ccdc_archive 'CCDC 942558'