# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global_1 _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 loop_ _publ_author_name 'Yun Gong' 'Yu-Chao Zhou' 'Tian-Fu Liu' 'Jian Lu' ; D.M.Proserpio ; 'Rong Cao' data_complex2 _database_code_depnum_ccdc_archive 'CCDC 764788' #TrackingRef '- complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H22 Co N4 O6' _chemical_formula_weight 617.47 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 24.36(4) _cell_length_b 23.37(7) _cell_length_c 16.13(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.104(15) _cell_angle_gamma 90.00 _cell_volume 8865(35) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'red purple' _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 0.421 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 173(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 32736 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9939 _reflns_number_gt 6888 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^. Part of a benzen ring in the asymmetric unit is disordered on two position c9a c9b c12a c12b c13a c13b c14a c14b with occupancy 50%:50% The structure contains disordered solvents. Because it was difficult to refine a consistent disordered model, their contribution was subtracted from the observed structure factors according to the BYPASS procedure, as implemented in PLATON. van der Sluis, P., Spek, A. L. (1990). Acta Cryst. A46, 194-201. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. (see more at the bottom of this .cif file) ; _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^)+(0.1981P)^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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.050(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9939 _refine_ls_number_parameters 419 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.2848 _refine_ls_wR_factor_gt 0.2682 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.046 _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 0.227658(15) 0.00980(2) 0.76334(2) 0.0681(3) Uani 1 1 d . C . O1 O 0.23939(10) -0.02557(11) 0.64602(14) 0.0766(6) Uani 1 1 d . . . N1 N 0.21079(11) 0.09266(14) 0.71182(18) 0.0832(8) Uani 1 1 d . . . C1 C 0.23915(12) -0.07520(14) 0.67856(17) 0.0681(7) Uani 1 1 d . . . O2 O 0.23425(11) -0.08150(11) 0.75293(14) 0.0860(7) Uani 1 1 d . . . N2 N 0.18675(14) 0.25753(15) 0.6043(2) 0.0994(10) Uani 1 1 d . . . H2 H 0.2153 0.2702 0.5854 0.119 Uiso 1 1 calc R . . C2 C 0.24332(13) -0.12628(14) 0.62500(18) 0.0704(7) Uani 1 1 d . . . O3 O 0.20202(9) 0.01785(11) 0.87721(15) 0.0779(7) Uani 1 1 d . C . N3 N 0.31517(10) 0.02438(11) 0.81702(17) 0.0667(6) Uani 1 1 d . . . C3 C 0.23955(17) -0.12136(15) 0.5382(2) 0.0813(9) Uani 1 1 d . . . H3 H 0.2358 -0.0847 0.5119 0.098 Uiso 1 1 calc R . . O4 O 0.13683(10) -0.00200(15) 0.75887(17) 0.1057(11) Uani 1 1 d . C . N4 N 0.48557(11) 0.06752(14) 0.9307(2) 0.0886(8) Uani 1 1 d . . . H4 H 0.4898 0.0932 0.9719 0.106 Uiso 1 1 calc R . . C4 C 0.24126(18) -0.16970(15) 0.48987(19) 0.0883(10) Uani 1 1 d . . . H1 H 0.2368 -0.1659 0.4298 0.106 Uiso 1 1 calc R . . O5 O 0.09942(15) 0.27949(18) 0.6178(4) 0.170(2) Uani 1 1 d . . . C5 C 0.24928(19) -0.22381(15) 0.52657(19) 0.0891(11) Uani 1 1 d . . . O6 O 0.53417(15) 0.01313(19) 0.8602(5) 0.195(3) Uani 1 1 d . . . C6 C 0.2538(3) -0.22738(18) 0.6133(2) 0.131(2) Uani 1 1 d . . . H6 H 0.2592 -0.2639 0.6402 0.157 Uiso 1 1 calc R . . C7 C 0.2508(3) -0.17980(18) 0.6624(2) 0.1200(18) Uani 1 1 d . . . H7 H 0.2539 -0.1839 0.7221 0.144 Uiso 1 1 calc R . . C8 C 0.15150(13) 0.00672(18) 0.8387(2) 0.0887(11) Uani 1 1 d D . . C10 C 0.12169(13) 0.00125(16) 0.9762(2) 0.0776(9) Uani 1 1 d D . . H10 H 0.1605 0.0044 1.0072 0.093 Uiso 1 1 calc R A 1 C11 C 0.07958(14) -0.00084(17) 1.0201(2) 0.0801(9) Uani 1 1 d D C . H11 H 0.0904 0.0092 1.0792 0.096 Uiso 1 1 calc R B 1 C15 C 0.2404(2) 0.1140(2) 0.6611(4) 0.1204(17) Uani 1 1 d . . . H15 H 0.2700 0.0909 0.6506 0.144 Uiso 1 1 calc R . . C16 C 0.17165(16) 0.12768(19) 0.7274(2) 0.0949(11) Uani 1 1 d . . . H16 H 0.1493 0.1141 0.7635 0.114 Uiso 1 1 calc R . . C17 C 0.16116(17) 0.1825(2) 0.6949(3) 0.1009(12) Uani 1 1 d . . . H17 H 0.1327 0.2054 0.7089 0.121 Uiso 1 1 calc R . . C18 C 0.19257(16) 0.20332(19) 0.6419(3) 0.0942(11) Uani 1 1 d . . . C19 C 0.2321(2) 0.1656(2) 0.6233(4) 0.138(2) Uani 1 1 d . . . H19 H 0.2532 0.1764 0.5838 0.165 Uiso 1 1 calc R . . C20 C 0.14076(17) 0.29248(19) 0.5943(3) 0.1058(13) Uani 1 1 d . . . C21 C 0.14287(14) 0.34801(17) 0.5499(3) 0.0913(10) Uani 1 1 d . . . C22 C 0.19272(14) 0.3767(2) 0.5498(3) 0.1047(14) Uani 1 1 d . . . H22 H 0.2284 0.3614 0.5803 0.126 Uiso 1 1 calc R . . C23 C 0.19057(16) 0.42604(19) 0.5068(4) 0.1100(15) Uani 1 1 d . . . H23 H 0.2251 0.4453 0.5079 0.132 Uiso 1 1 calc R . . C24 C 0.13946(15) 0.45017(18) 0.4603(4) 0.1084(14) Uani 1 1 d . . . H24 H 0.1392 0.4842 0.4279 0.130 Uiso 1 1 calc R . . C25 C 0.08848(14) 0.42325(15) 0.4625(3) 0.0957(12) Uani 1 1 d . . . C26 C 0.09100(14) 0.37188(16) 0.5093(3) 0.0968(12) Uani 1 1 d . . . H26 H 0.0568 0.3536 0.5129 0.116 Uiso 1 1 calc R . . C27 C 0.33153(14) 0.0571(2) 0.8863(2) 0.0929(11) Uani 1 1 d . . . H27 H 0.3029 0.0724 0.9102 0.111 Uiso 1 1 calc R . . C28 C 0.38682(16) 0.0702(2) 0.9255(2) 0.1040(14) Uani 1 1 d . . . H28 H 0.3956 0.0929 0.9762 0.125 Uiso 1 1 calc R . . C29 C 0.42996(12) 0.05078(14) 0.8920(2) 0.0764(8) Uani 1 1 d . . . C30 C 0.41327(16) 0.01694(19) 0.8215(4) 0.1099(16) Uani 1 1 d . . . H30 H 0.4409 0.0013 0.7959 0.132 Uiso 1 1 calc R . . C31 C 0.35695(16) 0.00518(19) 0.7873(4) 0.1075(16) Uani 1 1 d . . . H31 H 0.3473 -0.0188 0.7381 0.129 Uiso 1 1 calc R . . C32 C 0.53441(14) 0.04906(17) 0.9127(4) 0.1079(15) Uani 1 1 d . . . C9A C 0.1078(3) -0.0012(3) 0.8922(6) 0.082(3) Uani 0.50 1 d PD C 1 C12A C 0.0250(4) -0.0158(4) 0.9866(6) 0.077(2) Uani 0.50 1 d PD . 1 C13A C 0.0093(2) -0.0204(3) 0.8950(3) 0.0715(17) Uani 0.50 1 d PD C 1 H13A H -0.0293 -0.0255 0.8646 0.086 Uiso 0.50 1 calc PR C 1 C14A C 0.0510(2) -0.0173(3) 0.8514(3) 0.0628(14) Uani 0.50 1 d PD C 1 H14A H 0.0414 -0.0262 0.7919 0.075 Uiso 0.50 1 calc PR C 1 C13B C 0.00802(18) 0.0280(2) 0.8789(3) 0.0726(15) Uani 0.50 1 d PD C 2 H13B H -0.0298 0.0378 0.8490 0.087 Uiso 0.50 1 calc PR C 2 C12B C 0.02123(18) 0.0111(2) 0.9704(3) 0.065(2) Uani 0.50 1 d PRD . 2 C9B C 0.10513(18) 0.0115(2) 0.8824(3) 0.120(6) Uani 0.50 1 d PRD C 2 C14B C 0.0504(2) 0.0295(3) 0.8372(3) 0.0647(13) Uani 0.50 1 d PD C 2 H14B H 0.0429 0.0423 0.7795 0.078 Uiso 0.50 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0443(3) 0.0951(4) 0.0660(3) -0.02423(18) 0.0161(2) 0.00242(15) O1 0.0821(15) 0.0852(14) 0.0618(11) -0.0163(10) 0.0176(10) 0.0102(11) N1 0.0607(14) 0.111(2) 0.0782(16) -0.0115(14) 0.0195(12) 0.0247(14) C1 0.0599(15) 0.0860(19) 0.0582(14) -0.0156(13) 0.0148(11) 0.0020(13) O2 0.0993(17) 0.0964(16) 0.0694(13) -0.0245(11) 0.0348(12) -0.0152(12) N2 0.0753(18) 0.108(2) 0.112(2) 0.0010(18) 0.0178(16) 0.0387(16) C2 0.0738(18) 0.0785(17) 0.0595(14) -0.0088(13) 0.0182(12) 0.0119(13) O3 0.0437(10) 0.1222(18) 0.0697(12) -0.0310(11) 0.0179(9) -0.0042(10) N3 0.0475(11) 0.0768(14) 0.0756(14) -0.0107(11) 0.0157(10) 0.0010(10) C3 0.111(3) 0.0748(17) 0.0607(15) -0.0027(13) 0.0278(16) 0.0198(17) O4 0.0493(12) 0.197(3) 0.0738(15) -0.0562(16) 0.0221(11) -0.0196(14) N4 0.0540(14) 0.0989(19) 0.111(2) -0.0016(17) 0.0184(13) -0.0223(13) C4 0.131(3) 0.088(2) 0.0505(14) -0.0006(13) 0.0314(16) 0.026(2) O5 0.086(2) 0.135(3) 0.304(6) 0.065(3) 0.078(3) 0.050(2) C5 0.132(3) 0.0771(18) 0.0564(15) -0.0007(13) 0.0206(17) 0.0329(19) O6 0.0556(18) 0.137(3) 0.375(8) -0.120(4) 0.028(3) -0.0111(17) C6 0.250(7) 0.082(2) 0.0575(18) -0.0016(16) 0.034(3) 0.037(3) C7 0.216(6) 0.088(2) 0.0528(16) -0.0036(16) 0.030(2) 0.017(3) C8 0.0418(14) 0.150(3) 0.075(2) -0.046(2) 0.0159(13) -0.0022(15) C10 0.0390(14) 0.120(3) 0.0738(19) -0.0148(16) 0.0143(13) -0.0085(13) C11 0.0479(16) 0.126(3) 0.0671(18) -0.0128(16) 0.0152(13) -0.0069(14) C15 0.101(3) 0.133(4) 0.148(4) 0.041(3) 0.070(3) 0.063(3) C16 0.080(2) 0.120(3) 0.089(2) -0.013(2) 0.0286(17) 0.033(2) C17 0.083(2) 0.124(3) 0.097(2) -0.017(2) 0.0266(19) 0.042(2) C18 0.070(2) 0.113(3) 0.096(2) -0.009(2) 0.0163(17) 0.0360(19) C19 0.123(4) 0.137(4) 0.181(5) 0.048(4) 0.088(4) 0.075(3) C20 0.065(2) 0.107(3) 0.137(3) -0.012(2) 0.012(2) 0.0309(19) C21 0.0628(18) 0.094(2) 0.110(3) -0.022(2) 0.0107(17) 0.0228(16) C22 0.0484(16) 0.116(3) 0.134(3) -0.031(3) -0.0032(18) 0.0195(17) C23 0.0537(18) 0.096(3) 0.172(4) -0.033(3) 0.014(2) 0.0030(16) C24 0.0574(18) 0.083(2) 0.175(4) -0.024(2) 0.013(2) 0.0046(15) C25 0.0505(16) 0.080(2) 0.148(3) -0.028(2) 0.0105(18) 0.0100(13) C26 0.0539(16) 0.079(2) 0.146(3) -0.025(2) 0.0055(18) 0.0172(14) C27 0.0583(16) 0.141(3) 0.082(2) -0.027(2) 0.0239(15) -0.0147(18) C28 0.071(2) 0.166(4) 0.079(2) -0.032(2) 0.0269(16) -0.041(2) C29 0.0507(14) 0.0764(17) 0.097(2) 0.0041(16) 0.0110(14) -0.0124(12) C30 0.0507(18) 0.112(3) 0.165(4) -0.059(3) 0.025(2) -0.0057(16) C31 0.0492(18) 0.118(3) 0.154(4) -0.065(3) 0.024(2) -0.0021(16) C32 0.0517(17) 0.074(2) 0.185(4) 0.003(3) 0.007(2) -0.0107(14) C9A 0.024(4) 0.160(8) 0.063(5) -0.041(5) 0.009(3) -0.002(4) C12A 0.067(4) 0.107(6) 0.061(4) 0.003(4) 0.021(3) 0.008(4) C13A 0.038(2) 0.132(6) 0.044(2) -0.010(3) 0.0085(19) -0.002(3) C14A 0.038(2) 0.108(5) 0.040(2) -0.006(2) 0.0078(18) -0.002(2) C13B 0.049(3) 0.113(5) 0.057(3) 0.011(3) 0.015(2) 0.001(3) C12B 0.027(2) 0.120(6) 0.047(3) -0.016(3) 0.007(2) 0.001(3) C9B 0.067(8) 0.222(15) 0.076(8) -0.063(8) 0.027(6) -0.028(8) C14B 0.050(3) 0.100(4) 0.045(2) 0.000(2) 0.014(2) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.096(4) . ? Co1 N1 2.105(6) . ? Co1 N3 2.109(4) . ? Co1 O2 2.150(7) . ? Co1 O1 2.151(4) . ? Co1 O4 2.212(5) . ? Co1 C1 2.469(6) . ? Co1 C8 2.470(5) . ? O1 C1 1.274(5) . ? N1 C15 1.321(6) . ? N1 C16 1.329(4) . ? C1 O2 1.245(4) . ? C1 C2 1.492(5) . ? N2 C20 1.362(5) . ? N2 C18 1.396(6) . ? C2 C7 1.380(6) . ? C2 C3 1.384(5) . ? O3 C8 1.253(4) . ? N3 C31 1.312(5) . ? N3 C27 1.327(5) . ? C3 C4 1.379(5) . ? O4 C8 1.260(5) . ? N4 C32 1.366(6) . ? N4 C29 1.392(4) . ? C4 C5 1.388(6) . ? O5 C20 1.204(6) . ? C5 C6 1.376(5) . ? C5 C5 1.500(7) 7_546 ? O6 C32 1.192(7) . ? C6 C7 1.378(6) . ? C8 C9B 1.483(6) . ? C8 C9A 1.547(8) . ? C10 C9A 1.309(10) . ? C10 C11 1.390(5) . ? C10 C9B 1.481(6) . ? C11 C12A 1.344(11) . ? C11 C12B 1.465(6) . ? C15 C19 1.343(8) . ? C16 C17 1.382(7) . ? C17 C18 1.376(6) . ? C18 C19 1.396(5) . ? C20 C21 1.490(7) . ? C21 C26 1.380(5) . ? C21 C22 1.388(6) . ? C22 C23 1.340(8) . ? C23 C24 1.394(6) . ? C24 C25 1.401(6) . ? C25 C26 1.411(7) . ? C25 C32 1.499(5) 8_455 ? C27 C28 1.365(5) . ? C28 C29 1.378(5) . ? C29 C30 1.357(6) . ? C30 C31 1.367(6) . ? C32 C25 1.499(5) 8_556 ? C9A C14A 1.418(9) . ? C12A C13A 1.429(11) . ? C12A C12A 1.578(18) 5_557 ? C13A C14A 1.380(7) . ? C13B C14B 1.370(7) . ? C13B C12B 1.4793 . ? C12B C12B 1.664(9) 5_557 ? C9B C14B 1.408(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 N1 101.01(13) . . ? O3 Co1 N3 97.24(14) . . ? N1 Co1 N3 94.93(13) . . ? O3 Co1 O2 101.71(10) . . ? N1 Co1 O2 153.27(13) . . ? N3 Co1 O2 95.99(11) . . ? O3 Co1 O1 160.58(11) . . ? N1 Co1 O1 93.64(17) . . ? N3 Co1 O1 94.09(12) . . ? O2 Co1 O1 61.31(10) . . ? O3 Co1 O4 61.05(10) . . ? N1 Co1 O4 90.64(13) . . ? N3 Co1 O4 158.27(12) . . ? O2 Co1 O4 88.17(12) . . ? O1 Co1 O4 106.52(10) . . ? O3 Co1 C1 131.31(13) . . ? N1 Co1 C1 124.08(19) . . ? N3 Co1 C1 96.25(12) . . ? O2 Co1 C1 30.28(12) . . ? O1 Co1 C1 31.04(10) . . ? O4 Co1 C1 97.96(11) . . ? O3 Co1 C8 30.46(10) . . ? N1 Co1 C8 97.28(14) . . ? N3 Co1 C8 127.68(16) . . ? O2 Co1 C8 95.20(12) . . ? O1 Co1 C8 135.30(11) . . ? O4 Co1 C8 30.60(12) . . ? C1 Co1 C8 117.22(14) . . ? C1 O1 Co1 88.4(2) . . ? C15 N1 C16 114.8(4) . . ? C15 N1 Co1 120.6(2) . . ? C16 N1 Co1 124.6(3) . . ? O2 C1 O1 121.1(3) . . ? O2 C1 C2 120.1(3) . . ? O1 C1 C2 118.8(3) . . ? O2 C1 Co1 60.5(2) . . ? O1 C1 Co1 60.6(2) . . ? C2 C1 Co1 177.4(2) . . ? C1 O2 Co1 89.2(2) . . ? C20 N2 C18 125.7(4) . . ? C7 C2 C3 118.9(3) . . ? C7 C2 C1 119.6(3) . . ? C3 C2 C1 121.5(3) . . ? C8 O3 Co1 91.5(2) . . ? C31 N3 C27 114.4(3) . . ? C31 N3 Co1 126.3(3) . . ? C27 N3 Co1 119.2(2) . . ? C4 C3 C2 120.0(3) . . ? C8 O4 Co1 86.07(19) . . ? C32 N4 C29 128.0(4) . . ? C3 C4 C5 121.8(3) . . ? C6 C5 C4 117.0(3) . . ? C6 C5 C5 121.6(4) . 7_546 ? C4 C5 C5 121.4(4) . 7_546 ? C5 C6 C7 122.2(4) . . ? C6 C7 C2 120.1(4) . . ? O3 C8 O4 121.4(3) . . ? O3 C8 C9B 121.4(3) . . ? O4 C8 C9B 116.7(3) . . ? O3 C8 C9A 118.6(4) . . ? O4 C8 C9A 119.8(4) . . ? C9B C8 C9A 12.5(4) . . ? O3 C8 Co1 58.0(2) . . ? O4 C8 Co1 63.3(2) . . ? C9B C8 Co1 173.9(3) . . ? C9A C8 Co1 173.2(4) . . ? C9A C10 C11 119.9(4) . . ? C9A C10 C9B 11.8(4) . . ? C11 C10 C9B 119.0(3) . . ? C12A C11 C10 126.1(5) . . ? C12A C11 C12B 27.5(4) . . ? C10 C11 C12B 117.0(4) . . ? N1 C15 C19 125.3(3) . . ? N1 C16 C17 124.7(4) . . ? C18 C17 C16 119.1(3) . . ? C17 C18 N2 125.5(3) . . ? C17 C18 C19 115.9(4) . . ? N2 C18 C19 118.5(4) . . ? C15 C19 C18 120.0(5) . . ? O5 C20 N2 122.8(5) . . ? O5 C20 C21 120.5(3) . . ? N2 C20 C21 116.7(4) . . ? C26 C21 C22 119.8(4) . . ? C26 C21 C20 116.0(4) . . ? C22 C21 C20 124.2(4) . . ? C23 C22 C21 120.0(4) . . ? C22 C23 C24 122.4(4) . . ? C23 C24 C25 118.6(5) . . ? C24 C25 C26 118.7(3) . . ? C24 C25 C32 117.0(4) . 8_455 ? C26 C25 C32 124.3(4) . 8_455 ? C21 C26 C25 120.3(4) . . ? N3 C27 C28 124.2(3) . . ? C27 C28 C29 120.4(4) . . ? C30 C29 C28 115.3(3) . . ? C30 C29 N4 125.7(3) . . ? C28 C29 N4 119.0(4) . . ? C29 C30 C31 120.4(4) . . ? N3 C31 C30 125.2(4) . . ? O6 C32 N4 122.0(4) . . ? O6 C32 C25 121.7(4) . 8_556 ? N4 C32 C25 116.3(5) . 8_556 ? C10 C9A C14A 116.7(6) . . ? C10 C9A C8 122.8(5) . . ? C14A C9A C8 120.2(6) . . ? C11 C12A C13A 113.8(7) . . ? C11 C12A C12A 121.4(10) . 5_557 ? C13A C12A C12A 107.5(9) . 5_557 ? C14A C13A C12A 119.3(6) . . ? C13A C14A C9A 122.4(6) . . ? C14B C13B C12B 120.0(3) . . ? C11 C12B C13B 121.6(2) . . ? C11 C12B C12B 106.6(5) . 5_557 ? C13B C12B C12B 130.5(3) . 5_557 ? C14B C9B C10 123.1(4) . . ? C14B C9B C8 120.9(4) . . ? C10 C9B C8 115.8(4) . . ? C13B C14B C9B 118.1(5) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.709 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.064 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.000 0.239 0.025 1014 79 ' ' 2 0.500 0.261 -0.032 1015 78 ' ' 3 0.500 0.739 0.069 1014 79 ' ' 4 1.000 0.761 -0.032 1015 78 ' ' _platon_squeeze_details ; R1 = 0.1332 for 7136 Fo > 4sig(Fo) and 0.1505 for all 9939 data wR2 = 0.4149, GooF = S = 1.591, Restrained GooF = 1.591 for all data 508 parameters refined using 2 restraints ; data_complex1 _database_code_depnum_ccdc_archive 'CCDC 764789' #TrackingRef '- complex1_764789.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H34 N6 O8 Co' _chemical_formula_sum 'C36 H34 Co N6 O8' _chemical_formula_weight 737.63 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 22.162(2) _cell_length_b 20.532(2) _cell_length_c 16.1364(15) _cell_angle_alpha 90.00 _cell_angle_beta 95.937(2) _cell_angle_gamma 90.00 _cell_volume 7303.3(12) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.881 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 298(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 'Siemens SMART CCD' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean none _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 18983 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6439 _reflns_number_gt 3366 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _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^)+(0.1720P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6439 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1412 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2795 _refine_ls_wR_factor_gt 0.2389 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 0.21323(4) 1.01443(4) 0.75473(5) 0.0504(3) Uani 1 1 d . . . N1 N 0.1893(2) 0.9232(3) 0.7039(3) 0.0579(14) Uani 1 1 d . . . N2 N 0.1677(3) 0.7381(3) 0.5990(4) 0.0777(18) Uani 1 1 d . . . H2 H 0.1988 0.7257 0.5755 0.093 Uiso 1 1 calc R . . N3 N 0.3052(2) 0.9912(3) 0.7867(3) 0.0542(13) Uani 1 1 d . . . N4 N 0.4800(3) 0.9419(3) 0.8901(4) 0.0753(17) Uani 1 1 d . . . H4 H 0.4838 0.9016 0.9046 0.090 Uiso 1 1 calc R . . N5 N 0.1234(4) 0.7728(6) 0.3141(7) 0.132(3) Uani 1 1 d . . . N6 N 0.4629(10) 0.7191(13) 0.0149(17) 0.156(10) Uani 0.50 1 d P . . O1 O 0.1186(2) 1.0321(3) 0.7820(3) 0.0720(13) Uani 1 1 d . . . O2 O 0.1885(2) 0.9951(3) 0.8738(3) 0.0737(14) Uani 1 1 d . . . O3 O 0.2314(2) 1.1181(2) 0.7474(3) 0.0658(12) Uani 1 1 d . . . O4 O 0.2239(2) 1.0569(2) 0.6377(3) 0.0685(13) Uani 1 1 d . . . O5 O 0.0758(3) 0.7034(4) 0.6326(5) 0.136(3) Uani 1 1 d . . . O6 O 0.0315(2) 0.4648(3) 0.3826(4) 0.0956(19) Uani 1 1 d . . . O7 O 0.1971(3) 0.7748(4) 0.4257(4) 0.117(2) Uani 1 1 d . . . O8 O 0.4627(6) 0.8023(5) -0.0678(9) 0.090(4) Uani 0.50 1 d P . . C1 C 0.1342(3) 1.0125(4) 0.8538(4) 0.0634(18) Uani 1 1 d . . . C2 C 0.0743(3) 0.9889(4) 1.0625(5) 0.078(2) Uani 1 1 d . . . H2A H 0.0893 0.9820 1.1178 0.094 Uiso 1 1 calc R . . C3 C 0.1131(3) 0.9940(4) 1.0029(5) 0.075(2) Uani 1 1 d . . . H3 H 0.1546 0.9892 1.0172 0.090 Uiso 1 1 calc R . . C4 C 0.0904(3) 1.0068(4) 0.9187(4) 0.0660(19) Uani 1 1 d . . . C5 C 0.0307(3) 1.0132(4) 0.8965(5) 0.074(2) Uani 1 1 d . . . H5 H 0.0166 1.0221 0.8414 0.089 Uiso 1 1 calc R . . C6 C -0.0123(3) 1.0060(4) 0.9593(4) 0.0656(19) Uani 1 1 d . . . C7 C 0.2312(3) 1.1119(3) 0.6694(4) 0.0575(16) Uani 1 1 d . . . C8 C 0.2665(3) 1.2822(3) 0.6072(4) 0.0684(19) Uani 1 1 d . . . H8 H 0.2783 1.3212 0.6333 0.082 Uiso 1 1 calc R . . C9 C 0.2577(3) 1.2294(3) 0.6546(4) 0.0652(18) Uani 1 1 d . . . H9 H 0.2629 1.2326 0.7124 0.078 Uiso 1 1 calc R . . C10 C 0.2408(3) 1.1698(3) 0.6163(4) 0.0556(16) Uani 1 1 d . . . C11 C 0.2336(3) 1.1652(3) 0.5322(4) 0.0583(16) Uani 1 1 d . . . H11 H 0.2231 1.1253 0.5073 0.070 Uiso 1 1 calc R . . C12 C 0.2419(3) 1.2202(3) 0.4814(4) 0.0561(16) Uani 1 1 d . . . C13 C 0.1219(4) 0.6945(4) 0.5966(5) 0.083(2) Uani 1 1 d . . . C14 C 0.0298(3) 0.5211(4) 0.4067(5) 0.0673(19) Uani 1 1 d . . . C15 C 0.1311(3) 0.6330(4) 0.5479(5) 0.0702(19) Uani 1 1 d . . . C16 C 0.0795(3) 0.6066(4) 0.5029(5) 0.076(2) Uani 1 1 d . . . H16 H 0.0421 0.6267 0.5051 0.091 Uiso 1 1 calc R . . C17 C 0.0832(3) 0.5519(4) 0.4562(4) 0.0624(18) Uani 1 1 d . . . C18 C 0.1375(3) 0.5203(4) 0.4572(4) 0.0652(18) Uani 1 1 d . . . H18 H 0.1403 0.4821 0.4268 0.078 Uiso 1 1 calc R . . C19 C 0.1890(3) 0.5458(4) 0.5044(5) 0.073(2) Uani 1 1 d . . . H19 H 0.2258 0.5238 0.5067 0.088 Uiso 1 1 calc R . . C20 C 0.1850(3) 0.6035(4) 0.5472(5) 0.071(2) Uani 1 1 d . . . H20 H 0.2195 0.6218 0.5755 0.085 Uiso 1 1 calc R . . C21 C 0.1440(3) 0.8859(4) 0.7198(5) 0.0696(19) Uani 1 1 d . . . H21 H 0.1171 0.9019 0.7554 0.083 Uiso 1 1 calc R . . C22 C 0.1339(3) 0.8245(4) 0.6871(5) 0.076(2) Uani 1 1 d . . . H22 H 0.1013 0.7999 0.7014 0.091 Uiso 1 1 calc R . . C23 C 0.1721(3) 0.7998(4) 0.6334(4) 0.0628(18) Uani 1 1 d . . . C24 C 0.2169(4) 0.8401(4) 0.6142(5) 0.078(2) Uani 1 1 d . . . H24 H 0.2430 0.8265 0.5760 0.093 Uiso 1 1 calc R . . C25 C 0.2244(3) 0.8996(4) 0.6493(4) 0.074(2) Uani 1 1 d . . . H25 H 0.2559 0.9256 0.6343 0.089 Uiso 1 1 calc R . . C26 C 0.3183(3) 0.9373(4) 0.8300(5) 0.075(2) Uani 1 1 d . . . H26 H 0.2865 0.9096 0.8391 0.089 Uiso 1 1 calc R . . C27 C 0.3752(3) 0.9197(4) 0.8622(5) 0.078(2) Uani 1 1 d . . . H27 H 0.3815 0.8804 0.8905 0.093 Uiso 1 1 calc R . . C28 C 0.4230(3) 0.9604(3) 0.8524(4) 0.0584(17) Uani 1 1 d . . . C29 C 0.4111(3) 1.0149(4) 0.8063(5) 0.0655(18) Uani 1 1 d . . . H29 H 0.4424 1.0427 0.7955 0.079 Uiso 1 1 calc R . . C30 C 0.3517(3) 1.0289(3) 0.7754(4) 0.0615(18) Uani 1 1 d . . . H30 H 0.3443 1.0670 0.7450 0.074 Uiso 1 1 calc R . . C31 C 0.1654(5) 0.7981(6) 0.3689(8) 0.119(4) Uani 1 1 d . . . H31 H 0.1714 0.8425 0.3619 0.143 Uiso 1 1 calc R . . C32 C 0.1137(7) 0.7002(8) 0.3135(10) 0.190(6) Uani 1 1 d . . . H32A H 0.1343 0.6816 0.3632 0.284 Uiso 1 1 calc R . . H32B H 0.1294 0.6816 0.2656 0.284 Uiso 1 1 calc R . . H32C H 0.0711 0.6910 0.3115 0.284 Uiso 1 1 calc R . . C33 C 0.0933(6) 0.8051(8) 0.2411(9) 0.177(6) Uani 1 1 d . . . H33A H 0.0564 0.7825 0.2228 0.265 Uiso 1 1 calc R . . H33B H 0.1195 0.8050 0.1973 0.265 Uiso 1 1 calc R . . H33C H 0.0841 0.8492 0.2549 0.265 Uiso 1 1 calc R . . C34 C 0.4450(10) 0.7758(15) -0.014(2) 0.146(11) Uani 0.50 1 d P . . H34 H 0.4151 0.7966 0.0129 0.175 Uiso 0.50 1 calc PR . . C35 C 0.4425(9) 0.6836(11) 0.0866(16) 0.129(8) Uani 0.50 1 d P . . H35A H 0.4369 0.7138 0.1305 0.194 Uiso 0.50 1 calc PR . . H35B H 0.4725 0.6519 0.1061 0.194 Uiso 0.50 1 calc PR . . H35C H 0.4048 0.6620 0.0697 0.194 Uiso 0.50 1 calc PR . . C36 C 0.5139(14) 0.6846(12) -0.0216(18) 0.154(10) Uani 0.50 1 d P . . H36A H 0.4977 0.6497 -0.0567 0.231 Uiso 0.50 1 calc PR . . H36B H 0.5417 0.6674 0.0225 0.231 Uiso 0.50 1 calc PR . . H36C H 0.5348 0.7148 -0.0540 0.231 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0460(5) 0.0592(6) 0.0455(5) 0.0041(4) 0.0024(3) -0.0031(4) N1 0.055(3) 0.066(4) 0.052(3) 0.004(3) 0.004(3) -0.011(3) N2 0.082(4) 0.076(4) 0.076(4) -0.011(3) 0.011(3) -0.026(4) N3 0.052(3) 0.056(3) 0.054(3) 0.004(3) 0.001(2) -0.005(3) N4 0.066(4) 0.065(4) 0.091(4) -0.001(3) -0.015(3) 0.012(3) N5 0.117(7) 0.131(9) 0.144(8) 0.016(7) -0.006(6) -0.029(6) N6 0.099(14) 0.139(19) 0.21(2) 0.062(18) -0.068(15) -0.073(14) O1 0.065(3) 0.087(4) 0.066(3) 0.000(3) 0.013(2) 0.001(3) O2 0.055(3) 0.109(4) 0.057(3) -0.001(3) 0.006(2) -0.004(3) O3 0.078(3) 0.062(3) 0.060(3) 0.002(2) 0.016(2) 0.009(2) O4 0.090(3) 0.058(3) 0.054(3) 0.007(2) -0.008(2) -0.012(3) O5 0.099(5) 0.120(6) 0.193(7) -0.068(6) 0.038(5) -0.033(4) O6 0.063(3) 0.085(4) 0.134(5) -0.033(4) -0.010(3) 0.002(3) O7 0.132(6) 0.136(6) 0.083(4) 0.004(4) 0.005(4) 0.003(5) O8 0.097(9) 0.034(5) 0.127(10) 0.038(6) -0.049(7) -0.022(5) C1 0.057(4) 0.083(5) 0.051(4) -0.008(4) 0.011(3) -0.011(4) C2 0.059(4) 0.119(7) 0.054(4) 0.007(4) -0.005(3) -0.002(4) C3 0.058(4) 0.105(6) 0.062(4) -0.002(4) 0.007(3) -0.003(4) C4 0.046(4) 0.089(5) 0.063(4) -0.011(4) 0.009(3) -0.005(3) C5 0.065(5) 0.098(6) 0.060(4) -0.006(4) 0.005(3) -0.004(4) C6 0.049(4) 0.092(6) 0.053(4) -0.004(4) -0.006(3) -0.004(3) C7 0.058(4) 0.054(4) 0.059(4) 0.005(3) -0.002(3) 0.006(3) C8 0.091(5) 0.051(4) 0.061(4) -0.007(4) -0.003(4) -0.001(4) C9 0.089(5) 0.057(4) 0.047(4) 0.004(3) -0.003(3) 0.004(4) C10 0.061(4) 0.049(4) 0.055(4) 0.004(3) 0.000(3) 0.004(3) C11 0.066(4) 0.049(4) 0.058(4) 0.000(3) -0.002(3) -0.001(3) C12 0.069(4) 0.048(4) 0.049(4) 0.000(3) -0.006(3) 0.005(3) C13 0.075(5) 0.088(6) 0.085(5) -0.010(5) 0.004(4) -0.017(5) C14 0.064(5) 0.064(5) 0.073(5) -0.005(4) 0.006(4) -0.006(4) C15 0.070(5) 0.065(5) 0.074(5) -0.003(4) -0.002(4) -0.015(4) C16 0.061(4) 0.077(5) 0.088(5) -0.002(5) -0.003(4) -0.007(4) C17 0.051(4) 0.071(5) 0.064(4) -0.002(4) -0.001(3) -0.016(4) C18 0.066(5) 0.063(4) 0.066(4) 0.000(4) 0.008(3) -0.013(4) C19 0.059(4) 0.088(6) 0.072(5) 0.016(5) 0.004(4) -0.001(4) C20 0.055(4) 0.085(6) 0.071(5) 0.000(4) -0.003(4) -0.029(4) C21 0.061(4) 0.072(5) 0.077(5) -0.003(4) 0.014(4) -0.015(4) C22 0.066(5) 0.078(6) 0.084(5) 0.000(4) 0.006(4) -0.019(4) C23 0.067(4) 0.065(5) 0.056(4) -0.007(4) 0.006(3) -0.022(4) C24 0.083(5) 0.079(6) 0.074(5) -0.020(4) 0.023(4) -0.024(4) C25 0.078(5) 0.079(6) 0.069(5) -0.008(4) 0.020(4) -0.025(4) C26 0.063(4) 0.069(5) 0.087(5) 0.021(4) -0.011(4) -0.015(4) C27 0.071(5) 0.063(5) 0.093(6) 0.018(4) -0.013(4) -0.001(4) C28 0.053(4) 0.057(4) 0.064(4) 0.006(3) 0.000(3) 0.009(3) C29 0.048(4) 0.068(5) 0.079(5) 0.013(4) 0.001(3) -0.005(3) C30 0.056(4) 0.058(4) 0.070(4) 0.013(3) 0.004(3) -0.001(3) C31 0.112(8) 0.133(10) 0.111(8) -0.008(8) 0.010(7) -0.042(7) C32 0.212(16) 0.174(16) 0.179(14) -0.015(12) 0.001(12) -0.021(13) C33 0.138(11) 0.211(16) 0.169(13) 0.027(12) -0.040(9) -0.041(10) C34 0.075(14) 0.12(2) 0.22(3) 0.01(2) -0.071(18) -0.019(15) C35 0.093(14) 0.122(18) 0.17(2) 0.039(17) 0.024(14) -0.022(12) C36 0.15(2) 0.108(19) 0.20(3) 0.017(19) 0.01(2) -0.038(18) _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 O2 2.090(5) . ? Co1 N1 2.091(6) . ? Co1 N3 2.106(5) . ? Co1 O4 2.115(4) . ? Co1 O3 2.171(5) . ? Co1 O1 2.216(5) . ? Co1 C7 2.485(7) . ? Co1 C1 2.491(7) . ? N1 C21 1.309(8) . ? N1 C25 1.325(9) . ? N2 C13 1.352(9) . ? N2 C23 1.382(9) . ? N3 C30 1.315(8) . ? N3 C26 1.325(8) . ? N4 C14 1.343(9) 8_566 ? N4 C28 1.398(8) . ? N5 C31 1.323(13) . ? N5 C33 1.454(15) . ? N5 C32 1.506(17) . ? N6 C34 1.30(3) . ? N6 C35 1.48(3) . ? N6 C36 1.50(3) . ? O1 C1 1.241(8) . ? O2 C1 1.266(8) . ? O3 C7 1.265(8) . ? O4 C7 1.244(8) . ? O5 C13 1.240(10) . ? O6 C14 1.221(9) . ? O7 C31 1.197(13) . ? O8 C34 1.13(3) . ? C1 C4 1.503(9) . ? C2 C3 1.358(10) . ? C2 C6 1.386(9) 5_577 ? C3 C4 1.424(10) . ? C4 C5 1.340(10) . ? C5 C6 1.470(10) . ? C6 C2 1.386(9) 5_577 ? C6 C6 1.392(13) 5_577 ? C7 C10 1.492(9) . ? C8 C9 1.352(9) . ? C8 C12 1.424(9) 7_576 ? C9 C10 1.404(9) . ? C10 C11 1.355(9) . ? C11 C12 1.417(9) . ? C12 C12 1.395(12) 7_576 ? C12 C8 1.424(9) 7_576 ? C13 C15 1.510(11) . ? C14 N4 1.343(9) 8_465 ? C14 C17 1.498(9) . ? C15 C20 1.340(10) . ? C15 C16 1.400(10) . ? C16 C17 1.360(10) . ? C17 C18 1.366(9) . ? C18 C19 1.408(10) . ? C19 C20 1.379(11) . ? C21 C22 1.376(10) . ? C22 C23 1.369(10) . ? C23 C24 1.353(9) . ? C24 C25 1.351(10) . ? C26 C27 1.361(10) . ? C27 C28 1.371(10) . ? C28 C29 1.354(9) . ? C29 C30 1.389(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 N1 96.3(2) . . ? O2 Co1 N3 94.0(2) . . ? N1 Co1 N3 95.3(2) . . ? O2 Co1 O4 164.4(2) . . ? N1 Co1 O4 93.80(19) . . ? N3 Co1 O4 96.8(2) . . ? O2 Co1 O3 107.71(19) . . ? N1 Co1 O3 153.82(19) . . ? N3 Co1 O3 93.15(19) . . ? O4 Co1 O3 60.57(18) . . ? O2 Co1 O1 60.36(19) . . ? N1 Co1 O1 91.0(2) . . ? N3 Co1 O1 154.2(2) . . ? O4 Co1 O1 107.76(19) . . ? O3 Co1 O1 92.02(18) . . ? O2 Co1 C7 137.3(2) . . ? N1 Co1 C7 123.6(2) . . ? N3 Co1 C7 96.4(2) . . ? O4 Co1 C7 30.01(19) . . ? O3 Co1 C7 30.58(19) . . ? O1 Co1 C7 100.8(2) . . ? O2 Co1 C1 30.5(2) . . ? N1 Co1 C1 94.1(2) . . ? N3 Co1 C1 124.5(2) . . ? O4 Co1 C1 136.9(2) . . ? O3 Co1 C1 101.4(2) . . ? O1 Co1 C1 29.9(2) . . ? C7 Co1 C1 122.2(2) . . ? C21 N1 C25 115.6(6) . . ? C21 N1 Co1 128.0(5) . . ? C25 N1 Co1 116.5(5) . . ? C13 N2 C23 129.8(7) . . ? C30 N3 C26 115.7(6) . . ? C30 N3 Co1 125.8(5) . . ? C26 N3 Co1 118.2(4) . . ? C14 N4 C28 128.2(6) 8_566 . ? C31 N5 C33 126.5(12) . . ? C31 N5 C32 118.9(12) . . ? C33 N5 C32 113.2(11) . . ? C34 N6 C35 128(3) . . ? C34 N6 C36 120(3) . . ? C35 N6 C36 112(2) . . ? C1 O1 Co1 87.5(4) . . ? C1 O2 Co1 92.5(4) . . ? C7 O3 Co1 88.6(4) . . ? C7 O4 Co1 91.7(4) . . ? O1 C1 O2 119.6(6) . . ? O1 C1 C4 122.6(7) . . ? O2 C1 C4 117.8(6) . . ? O1 C1 Co1 62.7(3) . . ? O2 C1 Co1 57.0(3) . . ? C4 C1 Co1 174.5(6) . . ? C3 C2 C6 119.8(7) . 5_577 ? C2 C3 C4 120.2(7) . . ? C5 C4 C3 120.9(7) . . ? C5 C4 C1 119.8(7) . . ? C3 C4 C1 119.3(6) . . ? C4 C5 C6 120.0(7) . . ? C2 C6 C6 122.3(8) 5_577 5_577 ? C2 C6 C5 121.0(6) 5_577 . ? C6 C6 C5 116.7(8) 5_577 . ? O4 C7 O3 119.1(6) . . ? O4 C7 C10 120.5(6) . . ? O3 C7 C10 120.4(6) . . ? O4 C7 Co1 58.3(3) . . ? O3 C7 Co1 60.8(4) . . ? C10 C7 Co1 178.4(5) . . ? C9 C8 C12 121.9(6) . 7_576 ? C8 C9 C10 119.9(6) . . ? C11 C10 C9 120.0(6) . . ? C11 C10 C7 120.7(6) . . ? C9 C10 C7 119.3(6) . . ? C10 C11 C12 121.0(6) . . ? C12 C12 C11 119.6(7) 7_576 . ? C12 C12 C8 117.5(7) 7_576 7_576 ? C11 C12 C8 122.8(6) . 7_576 ? O5 C13 N2 122.7(8) . . ? O5 C13 C15 122.0(7) . . ? N2 C13 C15 115.3(8) . . ? O6 C14 N4 121.7(7) . 8_465 ? O6 C14 C17 121.4(7) . . ? N4 C14 C17 116.9(7) 8_465 . ? C20 C15 C16 120.1(7) . . ? C20 C15 C13 123.4(7) . . ? C16 C15 C13 116.5(7) . . ? C17 C16 C15 121.0(7) . . ? C16 C17 C18 119.3(6) . . ? C16 C17 C14 123.7(7) . . ? C18 C17 C14 116.8(7) . . ? C17 C18 C19 119.6(7) . . ? C20 C19 C18 119.9(7) . . ? C15 C20 C19 119.9(7) . . ? N1 C21 C22 123.9(7) . . ? C23 C22 C21 119.7(7) . . ? C24 C23 C22 115.7(7) . . ? C24 C23 N2 119.4(7) . . ? C22 C23 N2 124.9(6) . . ? C25 C24 C23 121.2(7) . . ? N1 C25 C24 123.7(7) . . ? N3 C26 C27 124.5(7) . . ? C26 C27 C28 119.4(7) . . ? C29 C28 C27 117.2(6) . . ? C29 C28 N4 125.4(6) . . ? C27 C28 N4 117.3(6) . . ? C28 C29 C30 119.5(6) . . ? N3 C30 C29 123.7(6) . . ? O7 C31 N5 132.3(13) . . ? O8 C34 N6 126(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.263 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.114 # * END # Attachment '- complex3_772375.CIF' data_complex3 _database_code_depnum_ccdc_archive 'CCDC 772375' #TrackingRef '- complex3_772375.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H32 Co N6 O8' _chemical_formula_weight 687.57 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' 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 7.601(2) _cell_length_b 29.239(8) _cell_length_c 14.315(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.331(5) _cell_angle_gamma 90.00 _cell_volume 3162.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'red purple' _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 298(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13707 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3626 _reflns_number_gt 2874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0878P)^2^+2.3923P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0040(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3626 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1820 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.07069(2) 0.2500 0.0416(2) Uani 1 2 d S . . O2 O 0.7609(3) 0.05232(8) 0.28872(15) 0.0474(5) Uani 1 1 d . . . O1 O 0.5617(3) 0.02068(8) 0.36892(17) 0.0505(6) Uani 1 1 d . . . O3 O 0.4784(4) 0.28102(9) -0.00283(18) 0.0692(8) Uani 1 1 d . . . N1 N 0.5189(3) 0.11971(9) 0.14311(18) 0.0449(6) Uani 1 1 d . . . N2 N 0.5636(4) 0.21557(10) -0.0711(2) 0.0516(7) Uani 1 1 d . . . C1 C 0.7204(4) 0.02887(10) 0.3581(2) 0.0425(7) Uani 1 1 d . . . C2 C 0.8654(4) 0.01302(10) 0.4305(2) 0.0395(6) Uani 1 1 d . . . C4 C 1.0422(4) 0.01781(11) 0.4156(2) 0.0434(7) Uani 1 1 d . . . H4 H 1.0718 0.0302 0.3580 0.052 Uiso 1 1 calc R . . C10 C 0.5174(5) 0.26099(11) -0.0725(2) 0.0504(8) Uani 1 1 d . . . C3 C 0.8240(4) -0.00456(11) 0.5157(2) 0.0435(7) Uani 1 1 d . . . H3 H 0.7037 -0.0075 0.5269 0.052 Uiso 1 1 calc R . . C7 C 0.5483(5) 0.18515(12) 0.0019(2) 0.0478(7) Uani 1 1 d . . . C12 C 0.5000 0.26089(16) -0.2500 0.0484(11) Uani 1 2 d S . . H12 H 0.5000 0.2284 -0.2500 0.058 Uiso 1 2 calc SR . . C5 C 0.6126(5) 0.11188(12) 0.0711(2) 0.0527(8) Uani 1 1 d . . . H5 H 0.6704 0.0832 0.0686 0.063 Uiso 1 1 calc R . . C6 C 0.6308(5) 0.14276(12) 0.0005(2) 0.0543(9) Uani 1 1 d . . . H6 H 0.6993 0.1352 -0.0490 0.065 Uiso 1 1 calc R . . C14 C 0.5000 0.35584(16) -0.2500 0.0520(11) Uani 1 2 d S . . H14 H 0.5000 0.3883 -0.2500 0.062 Uiso 1 2 calc SR . . C8 C 0.4485(5) 0.19350(13) 0.0757(3) 0.0569(9) Uani 1 1 d . . . H8 H 0.3895 0.2219 0.0800 0.068 Uiso 1 1 calc R . . C11 C 0.5119(5) 0.28440(11) -0.1651(2) 0.0463(7) Uani 1 1 d . . . C13 C 0.5100(5) 0.33211(11) -0.1662(3) 0.0520(8) Uani 1 1 d . . . H13 H 0.5156 0.3485 -0.1086 0.062 Uiso 1 1 calc R . . C9 C 0.4359(5) 0.16032(13) 0.1423(3) 0.0563(9) Uani 1 1 d . . . H9 H 0.3638 0.1664 0.1910 0.068 Uiso 1 1 calc R . . O4 O 0.2267(5) 0.33586(13) 0.2892(2) 0.0966(12) Uani 1 1 d . . . N3 N 0.2921(5) 0.38197(11) 0.1713(2) 0.0643(8) Uani 1 1 d . . . C16 C 0.2343(10) 0.42385(19) 0.2128(5) 0.106(2) Uani 1 1 d . . . H16A H 0.1972 0.4172 0.2748 0.159 Uiso 1 1 calc R . . H16B H 0.1345 0.4368 0.1722 0.159 Uiso 1 1 calc R . . H16C H 0.3322 0.4458 0.2195 0.159 Uiso 1 1 calc R . . C15 C 0.2820(7) 0.34235(16) 0.2130(3) 0.0729(12) Uani 1 1 d . . . C17 C 0.3640(7) 0.38615(16) 0.0820(3) 0.0780(13) Uani 1 1 d . . . H17A H 0.3979 0.3558 0.0609 0.117 Uiso 1 1 calc R . . H17B H 0.4683 0.4061 0.0894 0.117 Uiso 1 1 calc R . . H17C H 0.2743 0.3994 0.0353 0.117 Uiso 1 1 calc R . . H1 H 0.620(6) 0.2061(14) -0.120(3) 0.071(13) Uiso 1 1 d . . . H2 H 0.328(6) 0.3173(16) 0.176(3) 0.078(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0415(4) 0.0426(4) 0.0384(4) 0.000 -0.0066(2) 0.000 O2 0.0458(13) 0.0551(13) 0.0398(12) 0.0125(10) -0.0020(9) 0.0030(10) O1 0.0398(12) 0.0538(13) 0.0554(14) 0.0105(10) -0.0066(9) -0.0057(10) O3 0.108(2) 0.0516(15) 0.0480(15) -0.0050(11) 0.0092(14) 0.0121(14) N1 0.0461(15) 0.0454(14) 0.0412(14) 0.0024(11) -0.0043(11) 0.0031(11) N2 0.068(2) 0.0488(16) 0.0382(15) 0.0043(12) 0.0048(13) 0.0101(14) C1 0.0443(17) 0.0410(15) 0.0400(16) 0.0016(12) -0.0044(12) 0.0008(12) C2 0.0378(15) 0.0382(15) 0.0410(15) 0.0034(11) -0.0029(11) -0.0005(11) C4 0.0459(17) 0.0436(16) 0.0400(16) 0.0073(12) 0.0014(12) -0.0002(13) C10 0.059(2) 0.0446(17) 0.0452(18) -0.0006(14) -0.0041(14) 0.0037(14) C3 0.0387(16) 0.0445(16) 0.0461(17) 0.0062(13) -0.0002(12) -0.0014(12) C7 0.0524(19) 0.0486(18) 0.0406(17) 0.0038(13) -0.0035(13) 0.0064(14) C12 0.057(3) 0.037(2) 0.048(3) 0.000 -0.006(2) 0.000 C5 0.069(2) 0.0441(17) 0.0451(18) 0.0043(13) 0.0071(15) 0.0118(16) C6 0.066(2) 0.0528(19) 0.0443(18) -0.0003(14) 0.0065(15) 0.0114(16) C14 0.062(3) 0.039(2) 0.055(3) 0.000 0.006(2) 0.000 C8 0.066(2) 0.056(2) 0.0494(19) 0.0092(15) 0.0109(16) 0.0211(17) C11 0.0530(19) 0.0425(16) 0.0421(17) -0.0014(12) -0.0007(13) 0.0014(13) C13 0.053(2) 0.0443(17) 0.058(2) -0.0075(14) 0.0037(15) -0.0017(14) C9 0.059(2) 0.061(2) 0.0494(19) 0.0119(16) 0.0090(15) 0.0160(17) O4 0.132(3) 0.099(3) 0.061(2) 0.0091(17) 0.0203(19) -0.041(2) N3 0.072(2) 0.061(2) 0.061(2) 0.0039(15) 0.0112(16) -0.0018(16) C16 0.138(6) 0.085(4) 0.106(5) 0.007(3) 0.057(4) 0.020(3) C15 0.091(3) 0.066(3) 0.060(3) 0.000(2) 0.004(2) -0.018(2) C17 0.104(4) 0.070(3) 0.063(3) 0.004(2) 0.023(2) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 2.070(2) 2_655 ? Co1 O2 2.070(2) . ? Co1 N1 2.113(3) 2_655 ? Co1 N1 2.113(3) . ? Co1 O1 2.254(2) 2_655 ? Co1 O1 2.254(2) . ? Co1 C1 2.475(3) 2_655 ? Co1 C1 2.475(3) . ? O2 C1 1.272(4) . ? O1 C1 1.257(4) . ? O3 C10 1.221(4) . ? N1 C5 1.336(4) . ? N1 C9 1.344(4) . ? N2 C10 1.373(4) . ? N2 C7 1.388(4) . ? N2 H1 0.90(4) . ? C1 C2 1.500(4) . ? C2 C4 1.391(4) . ? C2 C3 1.391(4) . ? C4 C3 1.390(4) 5_756 ? C4 H4 0.9500 . ? C10 C11 1.488(5) . ? C3 C4 1.390(4) 5_756 ? C3 H3 0.9500 . ? C7 C8 1.388(5) . ? C7 C6 1.390(5) . ? C12 C11 1.390(4) 2_654 ? C12 C11 1.390(4) . ? C12 H12 0.9500 . ? C5 C6 1.374(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C14 C13 1.381(4) 2_654 ? C14 C13 1.381(4) . ? C14 H14 0.9500 . ? C8 C9 1.371(5) . ? C8 H8 0.9500 . ? C11 C13 1.395(5) . ? C13 H13 0.9500 . ? C9 H9 0.9500 . ? O4 C15 1.225(5) . ? N3 C15 1.309(5) . ? N3 C16 1.450(6) . ? N3 C17 1.450(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15 H2 0.99(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 O2 Co1 O2 149.93(14) 2_655 . ? O2 Co1 N1 103.32(9) 2_655 2_655 ? O2 Co1 N1 96.99(10) . 2_655 ? O2 Co1 N1 96.99(10) 2_655 . ? O2 Co1 N1 103.32(9) . . ? N1 Co1 N1 94.58(15) 2_655 . ? O2 Co1 O1 61.07(8) 2_655 2_655 ? O2 Co1 O1 98.46(9) . 2_655 ? N1 Co1 O1 164.15(9) 2_655 2_655 ? N1 Co1 O1 85.30(10) . 2_655 ? O2 Co1 O1 98.46(9) 2_655 . ? O2 Co1 O1 61.07(8) . . ? N1 Co1 O1 85.30(10) 2_655 . ? N1 Co1 O1 164.15(9) . . ? O1 Co1 O1 99.10(13) 2_655 . ? O2 Co1 C1 30.91(9) 2_655 2_655 ? O2 Co1 C1 126.99(10) . 2_655 ? N1 Co1 C1 133.84(10) 2_655 2_655 ? N1 Co1 C1 88.72(10) . 2_655 ? O1 Co1 C1 30.36(9) 2_655 2_655 ? O1 Co1 C1 102.81(10) . 2_655 ? O2 Co1 C1 126.99(10) 2_655 . ? O2 Co1 C1 30.91(9) . . ? N1 Co1 C1 88.72(10) 2_655 . ? N1 Co1 C1 133.84(10) . . ? O1 Co1 C1 102.81(10) 2_655 . ? O1 Co1 C1 30.36(9) . . ? C1 Co1 C1 120.78(14) 2_655 . ? C1 O2 Co1 92.40(18) . . ? C1 O1 Co1 84.60(18) . . ? C5 N1 C9 115.7(3) . . ? C5 N1 Co1 121.8(2) . . ? C9 N1 Co1 122.4(2) . . ? C10 N2 C7 126.0(3) . . ? C10 N2 H1 115(3) . . ? C7 N2 H1 118(3) . . ? O1 C1 O2 121.1(3) . . ? O1 C1 C2 119.9(3) . . ? O2 C1 C2 118.9(3) . . ? O1 C1 Co1 65.04(16) . . ? O2 C1 Co1 56.69(15) . . ? C2 C1 Co1 168.4(2) . . ? C4 C2 C3 119.2(3) . . ? C4 C2 C1 120.8(3) . . ? C3 C2 C1 120.0(3) . . ? C3 C4 C2 120.5(3) 5_756 . ? C3 C4 H4 119.8 5_756 . ? C2 C4 H4 119.8 . . ? O3 C10 N2 122.5(3) . . ? O3 C10 C11 121.4(3) . . ? N2 C10 C11 116.1(3) . . ? C4 C3 C2 120.3(3) 5_756 . ? C4 C3 H3 119.8 5_756 . ? C2 C3 H3 119.8 . . ? N2 C7 C8 124.0(3) . . ? N2 C7 C6 119.0(3) . . ? C8 C7 C6 117.0(3) . . ? C11 C12 C11 120.8(4) 2_654 . ? C11 C12 H12 119.6 2_654 . ? C11 C12 H12 119.6 . . ? N1 C5 C6 124.1(3) . . ? N1 C5 H5 117.9 . . ? C6 C5 H5 117.9 . . ? C5 C6 C7 119.5(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C13 C14 C13 119.7(4) 2_654 . ? C13 C14 H14 120.2 2_654 . ? C13 C14 H14 120.2 . . ? C9 C8 C7 119.3(3) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C12 C11 C13 119.0(3) . . ? C12 C11 C10 122.9(3) . . ? C13 C11 C10 118.0(3) . . ? C14 C13 C11 120.8(3) . . ? C14 C13 H13 119.6 . . ? C11 C13 H13 119.6 . . ? N1 C9 C8 124.3(3) . . ? N1 C9 H9 117.9 . . ? C8 C9 H9 117.9 . . ? C15 N3 C16 121.6(4) . . ? C15 N3 C17 121.6(4) . . ? C16 N3 C17 116.8(4) . . ? N3 C16 H16A 109.5 . . ? N3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C15 N3 125.9(5) . . ? O4 C15 H2 122(3) . . ? N3 C15 H2 112(3) . . ? N3 C17 H17A 109.5 . . ? N3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.385 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.073 data_1010251 _database_code_depnum_ccdc_archive 'CCDC 846556' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 Co N6 O8' _chemical_formula_weight 737.62 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5853(5) _cell_length_b 12.8836(5) _cell_length_c 14.6733(6) _cell_angle_alpha 108.865(4) _cell_angle_beta 107.898(4) _cell_angle_gamma 99.825(4) _cell_volume 1719.05(13) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 766 _exptl_absorpt_coefficient_mu 0.561 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 12388 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 26.74 _reflns_number_total 6055 _reflns_number_gt 3879 _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^)+(0.0602P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6055 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1257 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.90634(5) 0.01938(4) 0.72152(3) 0.02685(16) Uani 1 1 d . . . N1 N 0.9899(3) 0.1196(2) 1.6555(2) 0.0293(7) Uani 1 1 d . . . N2 N 1.1020(3) 0.3469(2) 1.5246(2) 0.0308(7) Uani 1 1 d . . . H2B H 1.0736 0.3182 1.4576 0.037 Uiso 1 1 calc R . . N3 N 1.0465(3) 0.3682(2) 1.1794(2) 0.0402(8) Uani 1 1 d . . . H3A H 1.0365 0.3338 1.2192 0.048 Uiso 1 1 calc R . . N4 N 0.9585(3) 0.1460(2) 0.8725(2) 0.0327(7) Uani 1 1 d . . . N5 N 0.5061(4) 0.0753(3) 0.6810(3) 0.0495(9) Uani 1 1 d . . . N6 N 1.3508(7) 0.5273(6) 1.0389(6) 0.143(2) Uiso 1 1 d . . . O1 O 1.2204(3) 0.5113(2) 1.6701(2) 0.0535(8) Uani 1 1 d . . . O2 O 1.0935(4) 0.5422(2) 1.1739(2) 0.0696(10) Uani 1 1 d . . . O3 O 1.0845(2) -0.0221(2) 0.77154(18) 0.0382(6) Uani 1 1 d . . . O4 O 1.0442(2) -0.21192(19) 0.71781(18) 0.0384(6) Uani 1 1 d . . . O5 O 0.7878(3) -0.1149(2) 0.7488(2) 0.0385(6) Uani 1 1 d . . . O6 O 0.7801(2) -0.1358(2) 0.59250(18) 0.0375(6) Uani 1 1 d . . . O7 O 0.7181(3) 0.0794(2) 0.67486(19) 0.0426(7) Uani 1 1 d . . . O8 O 1.3287(9) 0.3364(8) 0.9648(7) 0.262(4) Uiso 1 1 d . . . C1 C 1.0960(4) 0.2162(3) 1.7127(3) 0.0439(10) Uani 1 1 d . . . H1A H 1.1435 0.2317 1.7828 0.053 Uiso 1 1 calc R . . C2 C 1.1396(4) 0.2939(3) 1.6752(3) 0.0434(10) Uani 1 1 d . . . H2A H 1.2125 0.3610 1.7195 0.052 Uiso 1 1 calc R . . C3 C 1.0736(4) 0.2713(3) 1.5703(3) 0.0282(8) Uani 1 1 d . . . C4 C 0.9708(4) 0.1666(3) 1.5080(3) 0.0332(9) Uani 1 1 d . . . H4A H 0.9289 0.1447 1.4361 0.040 Uiso 1 1 calc R . . C5 C 0.9318(4) 0.0961(3) 1.5533(3) 0.0318(9) Uani 1 1 d . . . H5A H 0.8606 0.0276 1.5106 0.038 Uiso 1 1 calc R . . C6 C 1.1705(4) 0.4621(3) 1.5752(3) 0.0324(9) Uani 1 1 d . . . C7 C 1.1818(3) 0.5268(3) 1.5078(3) 0.0277(8) Uani 1 1 d . . . C8 C 1.1231(4) 0.4762(3) 1.3998(3) 0.0307(8) Uani 1 1 d . . . H8A H 1.0697 0.3994 1.3659 0.037 Uiso 1 1 calc R . . C9 C 1.1425(4) 0.5381(3) 1.3412(3) 0.0295(8) Uani 1 1 d . . . C10 C 1.2181(4) 0.6529(3) 1.3914(3) 0.0346(9) Uani 1 1 d . . . H10A H 1.2293 0.6960 1.3528 0.041 Uiso 1 1 calc R . . C11 C 1.2773(4) 0.7036(3) 1.4994(3) 0.0403(10) Uani 1 1 d . . . H11A H 1.3301 0.7806 1.5332 0.048 Uiso 1 1 calc R . . C12 C 1.2589(4) 0.6416(3) 1.5573(3) 0.0345(9) Uani 1 1 d . . . H12A H 1.2984 0.6769 1.6299 0.041 Uiso 1 1 calc R . . C13 C 1.0011(4) 0.1171(3) 0.9543(3) 0.0424(10) Uani 1 1 d . . . H13A H 1.0117 0.0443 0.9419 0.051 Uiso 1 1 calc R . . C14 C 1.0297(4) 0.1888(3) 1.0548(3) 0.0427(10) Uani 1 1 d . . . H14A H 1.0582 0.1642 1.1087 0.051 Uiso 1 1 calc R . . C15 C 1.0162(4) 0.2977(3) 1.0757(3) 0.0334(9) Uani 1 1 d . . . C16 C 0.9738(4) 0.3291(3) 0.9923(3) 0.0423(10) Uani 1 1 d . . . H16A H 0.9635 0.4018 1.0027 0.051 Uiso 1 1 calc R . . C17 C 0.9469(4) 0.2514(3) 0.8937(3) 0.0386(10) Uani 1 1 d . . . H17A H 0.9190 0.2741 0.8385 0.046 Uiso 1 1 calc R . . C18 C 1.0898(4) 0.4846(3) 1.2244(3) 0.0387(10) Uani 1 1 d . . . C19 C 0.7454(4) -0.1746(3) 0.6536(3) 0.0352(9) Uani 1 1 d . . . C20 C 0.6525(4) -0.2957(3) 0.6104(3) 0.0378(9) Uani 1 1 d . . . C21 C 0.5973(4) -0.3599(3) 0.5058(3) 0.0439(10) Uani 1 1 d . . . H21A H 0.6149 -0.3280 0.4608 0.053 Uiso 1 1 calc R . . C22 C 0.5109(4) -0.4783(3) 0.4636(3) 0.0374(9) Uani 1 1 d . . . C23 C 0.4559(4) -0.5454(3) 0.3578(3) 0.0490(11) Uani 1 1 d . . . H23A H 0.4731 -0.5151 0.3117 0.059 Uiso 1 1 calc R . . C24 C 0.3754(4) -0.6574(3) 0.3208(3) 0.0471(11) Uani 1 1 d . . . H24A H 0.3390 -0.7027 0.2495 0.057 Uiso 1 1 calc R . . C25 C 1.1172(4) -0.1113(3) 0.7751(3) 0.0269(8) Uani 1 1 d . . . C26 C 1.2590(3) -0.0885(3) 0.8554(3) 0.0279(8) Uani 1 1 d . . . C27 C 1.3335(4) 0.0203(3) 0.9283(3) 0.0328(9) Uani 1 1 d . . . H27A H 1.2938 0.0795 0.9295 0.039 Uiso 1 1 calc R . . C28 C 1.4702(4) 0.0456(3) 1.0024(3) 0.0329(9) Uani 1 1 d . . . C29 C 1.5498(4) 0.1575(3) 1.0780(3) 0.0421(10) Uani 1 1 d . . . H29A H 1.5113 0.2177 1.0811 0.050 Uiso 1 1 calc R . . C30 C 1.6813(4) 0.1791(3) 1.1462(3) 0.0380(9) Uani 1 1 d . . . H30A H 1.7323 0.2538 1.1942 0.046 Uiso 1 1 calc R . . C31 C 0.4055(5) 0.0452(5) 0.7231(4) 0.0871(18) Uani 1 1 d . . . H31A H 0.4432 0.0130 0.7720 0.131 Uiso 1 1 calc R . . H31B H 0.3221 -0.0102 0.6672 0.131 Uiso 1 1 calc R . . H31C H 0.3841 0.1129 0.7579 0.131 Uiso 1 1 calc R . . C32 C 0.4691(5) 0.1247(5) 0.6058(4) 0.0862(17) Uani 1 1 d . . . H32A H 0.5448 0.1403 0.5843 0.129 Uiso 1 1 calc R . . H32B H 0.4499 0.1951 0.6364 0.129 Uiso 1 1 calc R . . H32C H 0.3879 0.0718 0.5461 0.129 Uiso 1 1 calc R . . C33 C 0.6274(5) 0.0574(3) 0.7084(3) 0.0495(11) Uani 1 1 d . . . H33A H 0.6474 0.0253 0.7575 0.059 Uiso 1 1 calc R . . C34 C 1.2917(10) 0.5389(8) 0.9422(8) 0.210(4) Uiso 1 1 d . . . H34A H 1.2577 0.4648 0.8853 0.315 Uiso 1 1 calc R . . H34B H 1.3616 0.5890 0.9339 0.315 Uiso 1 1 calc R . . H34C H 1.2162 0.5709 0.9426 0.315 Uiso 1 1 calc R . . C35 C 1.4087(11) 0.6269(9) 1.1415(8) 0.225(5) Uiso 1 1 d . . . H35A H 1.4050 0.6961 1.1306 0.338 Uiso 1 1 calc R . . H35B H 1.5035 0.6328 1.1786 0.338 Uiso 1 1 calc R . . H35C H 1.3549 0.6162 1.1816 0.338 Uiso 1 1 calc R . . C36 C 1.3524(11) 0.4273(11) 1.0524(10) 0.217(5) Uiso 1 1 d . . . H36A H 1.3685 0.4225 1.1167 0.260 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 0.0307(3) 0.0209(3) 0.0219(3) 0.0089(2) 0.0040(2) 0.0019(2) N1 0.0298(17) 0.0294(16) 0.0264(17) 0.0137(14) 0.0070(14) 0.0052(14) N2 0.0402(19) 0.0294(17) 0.0223(16) 0.0114(14) 0.0129(14) 0.0057(15) N3 0.073(2) 0.0203(16) 0.0249(18) 0.0113(14) 0.0157(17) 0.0098(16) N4 0.0442(19) 0.0218(15) 0.0284(17) 0.0138(14) 0.0075(15) 0.0054(14) N5 0.036(2) 0.064(2) 0.053(2) 0.029(2) 0.0161(19) 0.0164(18) O1 0.079(2) 0.0401(16) 0.0231(15) 0.0079(13) 0.0134(15) -0.0038(15) O2 0.138(3) 0.0277(15) 0.0344(16) 0.0186(14) 0.0235(18) 0.0114(18) O3 0.0299(14) 0.0289(13) 0.0421(16) 0.0138(12) -0.0012(12) 0.0053(11) O4 0.0374(15) 0.0245(14) 0.0336(15) 0.0077(12) -0.0025(12) 0.0003(12) O5 0.0440(17) 0.0266(13) 0.0332(16) 0.0075(12) 0.0097(14) 0.0009(12) O6 0.0350(15) 0.0297(14) 0.0340(15) 0.0101(12) 0.0017(13) 0.0035(12) O7 0.0360(16) 0.0497(17) 0.0448(17) 0.0222(14) 0.0166(14) 0.0116(14) C1 0.039(2) 0.052(3) 0.025(2) 0.021(2) -0.0032(19) -0.006(2) C2 0.038(2) 0.042(2) 0.031(2) 0.0166(19) -0.0023(19) -0.0097(19) C3 0.030(2) 0.031(2) 0.029(2) 0.0159(17) 0.0145(18) 0.0113(17) C4 0.045(2) 0.029(2) 0.0214(19) 0.0090(17) 0.0099(18) 0.0064(18) C5 0.038(2) 0.0216(18) 0.027(2) 0.0070(16) 0.0086(18) 0.0006(17) C6 0.030(2) 0.031(2) 0.033(2) 0.0107(18) 0.0120(19) 0.0043(17) C7 0.030(2) 0.0226(18) 0.027(2) 0.0065(16) 0.0103(17) 0.0067(16) C8 0.036(2) 0.0184(18) 0.032(2) 0.0060(16) 0.0121(18) 0.0036(16) C9 0.036(2) 0.0218(19) 0.031(2) 0.0107(17) 0.0134(18) 0.0098(17) C10 0.047(2) 0.0213(19) 0.036(2) 0.0116(18) 0.018(2) 0.0087(18) C11 0.043(2) 0.0202(19) 0.047(3) 0.0083(19) 0.015(2) -0.0005(18) C12 0.039(2) 0.027(2) 0.027(2) 0.0048(17) 0.0081(19) 0.0058(18) C13 0.076(3) 0.025(2) 0.030(2) 0.0157(18) 0.018(2) 0.018(2) C14 0.071(3) 0.029(2) 0.029(2) 0.0187(18) 0.013(2) 0.013(2) C15 0.050(2) 0.0208(18) 0.026(2) 0.0108(17) 0.0113(19) 0.0064(18) C16 0.068(3) 0.025(2) 0.031(2) 0.0139(18) 0.011(2) 0.017(2) C17 0.058(3) 0.024(2) 0.026(2) 0.0122(17) 0.006(2) 0.0096(19) C18 0.055(3) 0.027(2) 0.034(2) 0.0154(19) 0.014(2) 0.0115(19) C19 0.023(2) 0.029(2) 0.053(3) 0.021(2) 0.008(2) 0.0075(17) C20 0.024(2) 0.028(2) 0.047(3) 0.007(2) 0.006(2) 0.0064(17) C21 0.033(2) 0.035(2) 0.061(3) 0.020(2) 0.014(2) 0.0108(19) C22 0.033(2) 0.041(2) 0.034(2) 0.0127(19) 0.009(2) 0.0132(19) C23 0.050(3) 0.048(3) 0.048(3) 0.022(2) 0.017(2) 0.010(2) C24 0.039(2) 0.034(2) 0.054(3) 0.017(2) 0.009(2) -0.0028(19) C25 0.028(2) 0.026(2) 0.0229(19) 0.0099(17) 0.0069(17) 0.0031(17) C26 0.030(2) 0.0259(19) 0.0234(19) 0.0086(16) 0.0077(17) 0.0055(16) C27 0.032(2) 0.029(2) 0.030(2) 0.0093(17) 0.0054(18) 0.0105(17) C28 0.031(2) 0.0268(19) 0.029(2) 0.0074(17) 0.0009(18) 0.0074(16) C29 0.037(2) 0.0241(19) 0.043(2) 0.0035(18) -0.003(2) 0.0105(17) C30 0.039(2) 0.0238(19) 0.035(2) 0.0033(17) 0.0029(19) 0.0063(17) C31 0.062(4) 0.120(5) 0.092(4) 0.044(4) 0.047(3) 0.023(3) C32 0.070(4) 0.124(5) 0.089(4) 0.065(4) 0.029(3) 0.047(4) C33 0.051(3) 0.051(3) 0.043(3) 0.020(2) 0.014(2) 0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O3 2.032(2) . ? Co1 N1 2.082(3) 1_554 ? Co1 O6 2.110(2) . ? Co1 N4 2.116(3) . ? Co1 O5 2.178(2) . ? Co1 O7 2.251(3) . ? Co1 C19 2.456(4) . ? N1 C1 1.336(4) . ? N1 C5 1.339(4) . ? N1 Co1 2.082(3) 1_556 ? N2 C6 1.367(4) . ? N2 C3 1.391(4) . ? N3 C18 1.354(4) . ? N3 C15 1.396(4) . ? N4 C17 1.328(4) . ? N4 C13 1.339(4) . ? N5 C33 1.306(5) . ? N5 C32 1.432(5) . ? N5 C31 1.443(5) . ? N6 C36 1.367(11) . ? N6 C34 1.433(10) . ? N6 C35 1.484(10) . ? O1 C6 1.218(4) . ? O2 C18 1.210(4) . ? O3 C25 1.267(4) . ? O4 C25 1.240(4) . ? O5 C19 1.243(4) . ? O6 C19 1.272(4) . ? O7 C33 1.237(4) . ? O8 C36 1.347(12) . ? C1 C2 1.369(5) . ? C2 C3 1.387(5) . ? C3 C4 1.390(5) . ? C4 C5 1.367(4) . ? C6 C7 1.502(5) . ? C7 C8 1.383(4) . ? C7 C12 1.383(5) . ? C8 C9 1.382(4) . ? C9 C10 1.378(5) . ? C9 C18 1.498(5) . ? C10 C11 1.382(5) . ? C11 C12 1.373(5) . ? C13 C14 1.367(5) . ? C14 C15 1.378(5) . ? C15 C16 1.382(5) . ? C16 C17 1.374(5) . ? C19 C20 1.502(5) . ? C20 C21 1.358(5) . ? C20 C24 1.410(5) 2_646 ? C21 C22 1.454(5) . ? C22 C23 1.380(5) . ? C22 C22 1.412(7) 2_646 ? C23 C24 1.375(5) . ? C24 C20 1.410(5) 2_646 ? C25 C26 1.506(5) . ? C26 C27 1.365(4) . ? C26 C30 1.417(5) 2_857 ? C27 C28 1.423(5) . ? C28 C29 1.413(5) . ? C28 C28 1.417(6) 2_857 ? C29 C30 1.360(5) . ? C30 C26 1.417(5) 2_857 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Co1 N1 92.45(11) . 1_554 ? O3 Co1 O6 100.39(9) . . ? N1 Co1 O6 103.85(10) 1_554 . ? O3 Co1 N4 91.24(11) . . ? N1 Co1 N4 100.09(11) 1_554 . ? O6 Co1 N4 152.80(11) . . ? O3 Co1 O5 92.25(10) . . ? N1 Co1 O5 165.26(10) 1_554 . ? O6 Co1 O5 61.54(9) . . ? N4 Co1 O5 93.77(10) . . ? O3 Co1 O7 175.61(10) . . ? N1 Co1 O7 85.81(10) 1_554 . ? O6 Co1 O7 83.95(9) . . ? N4 Co1 O7 85.10(11) . . ? O5 Co1 O7 90.43(10) . . ? O3 Co1 C19 96.64(10) . . ? N1 Co1 C19 135.02(13) 1_554 . ? O6 Co1 C19 31.18(11) . . ? N4 Co1 C19 123.53(13) . . ? O5 Co1 C19 30.37(10) . . ? O7 Co1 C19 87.42(11) . . ? C1 N1 C5 115.7(3) . . ? C1 N1 Co1 122.6(2) . 1_556 ? C5 N1 Co1 121.5(2) . 1_556 ? C6 N2 C3 126.8(3) . . ? C18 N3 C15 127.5(3) . . ? C17 N4 C13 116.3(3) . . ? C17 N4 Co1 125.6(2) . . ? C13 N4 Co1 118.0(2) . . ? C33 N5 C32 119.7(4) . . ? C33 N5 C31 122.2(4) . . ? C32 N5 C31 118.1(4) . . ? C36 N6 C34 127.0(9) . . ? C36 N6 C35 110.6(9) . . ? C34 N6 C35 122.2(8) . . ? C25 O3 Co1 136.9(2) . . ? C19 O5 Co1 87.3(2) . . ? C19 O6 Co1 89.6(2) . . ? C33 O7 Co1 117.9(3) . . ? N1 C1 C2 124.4(3) . . ? C1 C2 C3 119.0(3) . . ? C4 C3 C2 117.1(3) . . ? C4 C3 N2 118.5(3) . . ? C2 C3 N2 124.4(3) . . ? C5 C4 C3 119.3(3) . . ? N1 C5 C4 124.1(3) . . ? O1 C6 N2 122.4(3) . . ? O1 C6 C7 120.8(3) . . ? N2 C6 C7 116.8(3) . . ? C8 C7 C12 119.0(3) . . ? C8 C7 C6 123.3(3) . . ? C12 C7 C6 117.7(3) . . ? C9 C8 C7 121.1(3) . . ? C10 C9 C8 119.4(3) . . ? C10 C9 C18 117.7(3) . . ? C8 C9 C18 122.8(3) . . ? C9 C10 C11 119.7(3) . . ? C12 C11 C10 120.7(3) . . ? C11 C12 C7 120.1(3) . . ? N4 C13 C14 123.6(3) . . ? C13 C14 C15 119.6(3) . . ? C14 C15 C16 117.4(3) . . ? C14 C15 N3 117.8(3) . . ? C16 C15 N3 124.7(3) . . ? C17 C16 C15 119.1(3) . . ? N4 C17 C16 124.0(3) . . ? O2 C18 N3 122.1(3) . . ? O2 C18 C9 121.7(3) . . ? N3 C18 C9 116.1(3) . . ? O5 C19 O6 121.5(3) . . ? O5 C19 C20 119.0(4) . . ? O6 C19 C20 119.5(4) . . ? O5 C19 Co1 62.33(18) . . ? O6 C19 Co1 59.20(18) . . ? C20 C19 Co1 177.0(3) . . ? C21 C20 C24 120.3(4) . 2_646 ? C21 C20 C19 120.1(4) . . ? C24 C20 C19 119.7(4) 2_646 . ? C20 C21 C22 120.4(4) . . ? C23 C22 C22 122.0(5) . 2_646 ? C23 C22 C21 121.2(4) . . ? C22 C22 C21 116.8(4) 2_646 . ? C24 C23 C22 119.5(4) . . ? C23 C24 C20 120.9(4) . 2_646 ? O4 C25 O3 125.6(3) . . ? O4 C25 C26 119.5(3) . . ? O3 C25 C26 114.9(3) . . ? C27 C26 C30 119.2(3) . 2_857 ? C27 C26 C25 120.5(3) . . ? C30 C26 C25 120.2(3) 2_857 . ? C26 C27 C28 121.9(3) . . ? C29 C28 C27 122.9(3) . . ? C29 C28 C28 118.9(4) . 2_857 ? C27 C28 C28 118.1(4) . 2_857 ? C30 C29 C28 121.4(3) . . ? C29 C30 C26 120.4(3) . 2_857 ? O7 C33 N5 125.9(4) . . ? O8 C36 N6 114.4(11) . . ? _diffrn_measured_fraction_theta_max 0.826 _diffrn_reflns_theta_full 26.74 _diffrn_measured_fraction_theta_full 0.826 _refine_diff_density_max 0.588 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.070