Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2011 data_publication_text2 _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Cora E. MacBeth' _publ_contact_author_address ;Department of Chemistry Emory University 1515 Dickey Drive Atlanta, GA 30322 ; _publ_contact_author_email cora.macbeth@emory.edu _publ_contact_author_phone 404-727-7033 loop_ _publ_author_name _publ_author_address 'MacBeth, C. E.' ;Department of Chemistry Emory University 1515 Dickey Drive Atlanta, GA 30322 ; 'Sharma, S. K.' ;Department of Chemistry Emory University 1515 Dickey Drive Atlanta, GA 30322 ; 'May, P. S.' ;Department of Chemistry Emory University 1515 Dickey Drive Atlanta, GA 30322 ; 'Jones, M. B.' ;Department of Chemistry Emory University 1515 Dickey Drive Atlanta, GA 30322 ; 'Lense, S' ;Department of Chemistry Emory University 1515 Dickey Drive Atlanta, GA 30322 ; 'Hardcatle, K. I.' ;Department of Chemistry Emory University 1515 Dickey Drive Atlanta, GA 30322 ; data_new _database_code_depnum_ccdc_archive 'CCDC 782883' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H42 Co N4 O2' _chemical_formula_sum 'C28 H42 Co N4 O2' _chemical_formula_weight 525.59 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 Tetragonal _symmetry_space_group_name_H-M I4(1)22 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-y, x+1/2, z+1/4' 'y+1/2, -x, z+3/4' '-x+1/2, y, -z+3/4' 'x, -y+1/2, -z+1/4' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1, z+1' '-y+1/2, x+1, z+3/4' 'y+1, -x+1/2, z+5/4' '-x+1, y+1/2, -z+5/4' 'x+1/2, -y+1, -z+3/4' 'y+1, x+1, -z+1' '-y+1/2, -x+1/2, -z+1/2' _cell_length_a 18.7790(8) _cell_length_b 18.7790(8) _cell_length_c 35.798(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12624.1(13) _cell_formula_units_Z 16 _cell_measurement_temperature 172(2) _cell_measurement_reflns_used 9697 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 30.20 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.37 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4496 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7874 _exptl_absorpt_correction_T_max 0.8166 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 172(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_reflns_number 120959 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 30.71 _reflns_number_total 9495 _reflns_number_gt 6914 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+30.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.504(18) _refine_ls_number_reflns 9495 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1505 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 C1 C 0.53549(12) 0.55298(13) 0.93502(7) 0.0175(5) Uani 1 1 d . . . C2 C 0.57523(16) 0.53465(15) 0.90412(8) 0.0242(5) Uani 1 1 d . . . H2A H 0.5788 0.4859 0.8972 0.029 Uiso 1 1 calc R . . C3 C 0.61007(17) 0.58556(17) 0.88282(8) 0.0307(7) Uani 1 1 d . . . H3A H 0.6391 0.5720 0.8623 0.037 Uiso 1 1 calc R . . C4 C 0.60148(19) 0.65713(17) 0.89232(9) 0.0352(7) Uani 1 1 d . . . H4A H 0.6220 0.6929 0.8769 0.042 Uiso 1 1 calc R . . C5 C 0.56402(17) 0.67655(16) 0.92333(8) 0.0291(6) Uani 1 1 d . . . H5A H 0.5606 0.7256 0.9295 0.035 Uiso 1 1 calc R . . C6 C 0.53029(14) 0.62633(13) 0.94637(7) 0.0182(5) Uani 1 1 d . . . C7 C 0.48977(15) 0.70350(13) 0.99599(9) 0.0236(5) Uani 1 1 d . . . C8 C 0.44006(17) 0.71149(15) 1.02929(9) 0.0295(6) Uani 1 1 d . . . H8A H 0.4227 0.6633 1.0370 0.035 Uiso 1 1 calc R . . C9 C 0.4806(2) 0.7449(2) 1.06165(10) 0.0451(9) Uani 1 1 d . . . H9A H 0.5218 0.7152 1.0679 0.068 Uiso 1 1 calc R . . H9B H 0.4492 0.7485 1.0834 0.068 Uiso 1 1 calc R . . H9C H 0.4969 0.7926 1.0545 0.068 Uiso 1 1 calc R . . C10 C 0.3768(2) 0.7569(2) 1.01821(13) 0.0472(9) Uani 1 1 d . . . H10A H 0.3507 0.7335 0.9980 0.071 Uiso 1 1 calc R . . H10B H 0.3936 0.8036 1.0097 0.071 Uiso 1 1 calc R . . H10C H 0.3453 0.7631 1.0398 0.071 Uiso 1 1 calc R . . C1B C 0.12382(15) 0.46687(15) 0.19733(8) 0.0220(5) Uani 1 1 d . . . C2B C 0.17579(16) 0.43105(18) 0.17539(8) 0.0311(7) Uani 1 1 d . . . H2BA H 0.2247 0.4342 0.1819 0.037 Uiso 1 1 calc R . . C3B C 0.15459(17) 0.3905(2) 0.14377(9) 0.0353(7) Uani 1 1 d . . . H3BA H 0.1892 0.3652 0.1297 0.042 Uiso 1 1 calc R . . C4B C 0.08424(17) 0.38789(17) 0.13351(8) 0.0288(6) Uani 1 1 d . . . H4BA H 0.0704 0.3615 0.1121 0.035 Uiso 1 1 calc R . . C5B C 0.03332(15) 0.42361(16) 0.15430(8) 0.0245(6) Uani 1 1 d . . . H5BA H -0.0153 0.4211 0.1471 0.029 Uiso 1 1 calc R . . C6B C 0.05286(14) 0.46345(13) 0.18584(7) 0.0186(5) Uani 1 1 d . . . C7B C 0.20360(14) 0.51055(15) 0.24593(9) 0.0246(6) Uani 1 1 d . . . C8B C 0.20820(15) 0.55770(18) 0.28050(9) 0.0305(6) Uani 1 1 d . . . H8BA H 0.1594 0.5736 0.2879 0.037 Uiso 1 1 calc R . . C9B C 0.2543(2) 0.62344(19) 0.27012(13) 0.0479(10) Uani 1 1 d . . . H9BA H 0.2591 0.6545 0.2920 0.072 Uiso 1 1 calc R . . H9BB H 0.2314 0.6497 0.2498 0.072 Uiso 1 1 calc R . . H9BC H 0.3016 0.6075 0.2621 0.072 Uiso 1 1 calc R . . C10B C 0.24361(19) 0.5186(2) 0.31315(10) 0.0406(8) Uani 1 1 d . . . H10BA H 0.2467 0.5506 0.3347 0.061 Uiso 1 1 calc R . . H10BB H 0.2916 0.5036 0.3058 0.061 Uiso 1 1 calc R . . H10BC H 0.2152 0.4767 0.3198 0.061 Uiso 1 1 calc R . . C1S C 0.68622(17) 0.73553(18) 0.02802(9) 0.0304(6) Uani 1 1 d . . . H1SA H 0.6871 0.6856 0.0368 0.036 Uiso 1 1 calc R . . H1SB H 0.6402 0.7432 0.0152 0.036 Uiso 1 1 calc R . . C2S C 0.6898(2) 0.7850(2) 0.06207(10) 0.0407(8) Uani 1 1 d . . . H2SA H 0.6468 0.7790 0.0772 0.061 Uiso 1 1 calc R . . H2SB H 0.6933 0.8345 0.0536 0.061 Uiso 1 1 calc R . . H2SC H 0.7318 0.7730 0.0771 0.061 Uiso 1 1 calc R . . C3S C 0.81909(16) 0.74233(17) 0.01826(9) 0.0311(6) Uani 1 1 d . . . H3SA H 0.8558 0.7434 -0.0016 0.037 Uiso 1 1 calc R . . H3SB H 0.8257 0.7853 0.0339 0.037 Uiso 1 1 calc R . . C4S C 0.83081(18) 0.67683(19) 0.04227(10) 0.0379(7) Uani 1 1 d . . . H4SA H 0.8765 0.6809 0.0553 0.057 Uiso 1 1 calc R . . H4SB H 0.8312 0.6343 0.0264 0.057 Uiso 1 1 calc R . . H4SC H 0.7923 0.6729 0.0606 0.057 Uiso 1 1 calc R . . C5S C -0.0507(2) 0.5752(2) 0.96051(11) 0.0462(9) Uani 1 1 d . . . H5SA H -0.0424 0.6190 0.9463 0.069 Uiso 1 1 calc R . . H5SB H -0.0972 0.5778 0.9729 0.069 Uiso 1 1 calc R . . H5SC H -0.0500 0.5343 0.9435 0.069 Uiso 1 1 calc R . . C6S C 0.0078(2) 0.56642(18) 0.98995(10) 0.0377(7) Uani 1 1 d . . . H6SA H 0.0546 0.5649 0.9772 0.045 Uiso 1 1 calc R . . H6SB H 0.0076 0.6087 1.0065 0.045 Uiso 1 1 calc R . . C7S C 0.06606(18) 0.49140(18) 1.03762(10) 0.0368(7) Uani 1 1 d . . . H7SA H 0.1079 0.4876 1.0209 0.044 Uiso 1 1 calc R . . H7SB H 0.0623 0.4461 1.0516 0.044 Uiso 1 1 calc R . . C8S C 0.0795(2) 0.5518(2) 1.06557(10) 0.0423(8) Uani 1 1 d . . . H8SA H 0.1231 0.5418 1.0797 0.063 Uiso 1 1 calc R . . H8SB H 0.0392 0.5552 1.0828 0.063 Uiso 1 1 calc R . . H8SC H 0.0849 0.5968 1.0521 0.063 Uiso 1 1 calc R . . Co1 Co 0.449530(17) 0.550470(17) 1.0000 0.01538(11) Uani 1 2 d S . . Co1B Co 0.050149(17) 0.550149(17) 0.2500 0.01539(11) Uani 1 2 d S . . N1 N 0.5000 0.5000 0.95705(8) 0.0185(5) Uani 1 2 d S . . N2 N 0.48948(12) 0.63930(11) 0.97919(6) 0.0201(4) Uani 1 1 d . . . N1B N 0.13865(12) 0.50803(12) 0.22925(6) 0.0203(4) Uani 1 1 d . . . N2B N 0.0000 0.5000 0.20681(7) 0.0142(5) Uani 1 2 d S . . N1S N 0.74582(11) 0.74582(11) 0.0000 0.0212(5) Uani 1 2 d S . . N2S N 0.0000 0.5000 1.01382(10) 0.0241(6) Uani 1 2 d S . . O1 O 0.52449(14) 0.75774(12) 0.98650(7) 0.0393(6) Uani 1 1 d . . . O1B O 0.25753(11) 0.47950(13) 0.23514(7) 0.0333(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0173(11) 0.0166(11) 0.0186(12) 0.0032(9) -0.0009(8) -0.0035(9) C2 0.0296(14) 0.0247(13) 0.0183(12) 0.0019(10) 0.0033(11) -0.0052(11) C3 0.0360(16) 0.0351(15) 0.0208(13) 0.0052(11) 0.0078(11) -0.0075(13) C4 0.0399(18) 0.0319(16) 0.0337(16) 0.0156(13) 0.0068(13) -0.0116(14) C5 0.0357(16) 0.0228(13) 0.0289(14) 0.0025(11) 0.0021(12) -0.0096(11) C6 0.0216(12) 0.0161(11) 0.0171(11) 0.0038(9) -0.0018(9) -0.0046(9) C7 0.0279(13) 0.0141(11) 0.0288(14) -0.0013(10) 0.0025(12) -0.0010(9) C8 0.0369(17) 0.0184(12) 0.0331(15) -0.0035(11) 0.0116(13) 0.0000(11) C9 0.062(2) 0.043(2) 0.0305(17) -0.0070(15) -0.0007(16) -0.0069(18) C10 0.0394(19) 0.0359(18) 0.066(3) -0.0026(18) 0.0099(18) 0.0058(15) C1B 0.0212(12) 0.0240(13) 0.0209(13) 0.0033(10) 0.0011(10) 0.0041(10) C2B 0.0200(13) 0.0463(18) 0.0271(14) -0.0069(13) 0.0049(11) 0.0114(12) C3B 0.0312(15) 0.052(2) 0.0224(14) -0.0105(13) 0.0047(12) 0.0164(14) C4B 0.0355(15) 0.0335(15) 0.0175(12) -0.0099(11) 0.0012(11) 0.0088(12) C5B 0.0229(13) 0.0297(14) 0.0207(13) -0.0051(11) -0.0015(10) 0.0027(11) C6B 0.0215(12) 0.0216(12) 0.0127(11) 0.0009(8) 0.0012(9) 0.0053(9) C7B 0.0195(12) 0.0232(12) 0.0310(15) 0.0030(12) 0.0014(11) 0.0027(10) C8B 0.0192(12) 0.0352(16) 0.0372(16) -0.0080(13) -0.0091(11) 0.0036(11) C9B 0.050(2) 0.0255(16) 0.068(3) 0.0004(16) -0.021(2) -0.0060(15) C10B 0.0315(17) 0.053(2) 0.0375(18) 0.0009(16) -0.0058(14) 0.0023(15) C1S 0.0280(14) 0.0345(16) 0.0287(14) 0.0001(12) 0.0024(12) 0.0016(12) C2S 0.0441(19) 0.0444(19) 0.0335(16) -0.0106(14) 0.0051(14) 0.0086(16) C3S 0.0213(13) 0.0313(15) 0.0406(16) 0.0032(13) -0.0076(12) 0.0003(11) C4S 0.0320(17) 0.0382(18) 0.0434(17) 0.0034(15) -0.0139(14) 0.0054(13) C5S 0.058(2) 0.0400(19) 0.0408(19) 0.0072(15) -0.0159(17) -0.0014(17) C6S 0.0434(18) 0.0297(16) 0.0399(18) 0.0049(13) -0.0072(14) -0.0038(14) C7S 0.0324(16) 0.0340(16) 0.0440(19) 0.0040(14) -0.0044(14) 0.0066(13) C8S 0.0438(19) 0.047(2) 0.0365(18) -0.0010(15) -0.0103(15) 0.0003(17) Co1 0.01461(14) 0.01461(14) 0.0169(2) 0.00060(13) 0.00060(13) -0.00360(16) Co1B 0.01515(14) 0.01515(14) 0.0159(2) 0.00017(13) -0.00017(13) 0.00287(16) N1 0.0238(16) 0.0142(14) 0.0174(13) 0.000 0.000 -0.0089(11) N2 0.0223(11) 0.0141(10) 0.0239(11) -0.0001(8) 0.0039(9) -0.0039(8) N1B 0.0169(10) 0.0226(11) 0.0214(11) 0.0012(9) 0.0021(8) 0.0029(8) N2B 0.0149(13) 0.0158(14) 0.0120(12) 0.000 0.000 0.0010(10) N1S 0.0203(8) 0.0203(8) 0.0229(12) 0.0003(9) -0.0003(9) 0.0025(10) N2S 0.0241(17) 0.0199(16) 0.0284(14) 0.000 0.000 0.0004(12) O1 0.0464(13) 0.0189(10) 0.0525(15) -0.0055(10) 0.0137(11) -0.0125(9) O1B 0.0173(9) 0.0439(13) 0.0387(12) -0.0048(10) -0.0005(9) 0.0059(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.378(4) . ? C1 N1 1.434(3) . ? C1 C6 1.439(3) . ? C2 C3 1.387(4) . ? C2 H2A 0.9500 . ? C3 C4 1.396(5) . ? C3 H3A 0.9500 . ? C4 C5 1.364(5) . ? C4 H4A 0.9500 . ? C5 C6 1.404(4) . ? C5 H5A 0.9500 . ? C6 N2 1.424(3) . ? C7 O1 1.256(3) . ? C7 N2 1.347(3) . ? C7 C8 1.522(4) . ? C8 C10 1.515(5) . ? C8 C9 1.522(5) . ? C8 H8A 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C1B C6B 1.396(4) . ? C1B N1B 1.408(4) . ? C1B C2B 1.422(4) . ? C2B C3B 1.421(4) . ? C2B H2BA 0.9500 . ? C3B C4B 1.372(4) . ? C3B H3BA 0.9500 . ? C4B C5B 1.385(4) . ? C4B H4BA 0.9500 . ? C5B C6B 1.403(4) . ? C5B H5BA 0.9500 . ? C6B N2B 1.421(3) . ? C7B O1B 1.231(3) . ? C7B N1B 1.359(3) . ? C7B C8B 1.524(4) . ? C8B C10B 1.532(5) . ? C8B C9B 1.553(5) . ? C8B H8BA 1.0000 . ? C9B H9BA 0.9800 . ? C9B H9BB 0.9800 . ? C9B H9BC 0.9800 . ? C10B H10BA 0.9800 . ? C10B H10BB 0.9800 . ? C10B H10BC 0.9800 . ? C1S N1S 1.515(4) . ? C1S C2S 1.534(4) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? C3S C4S 1.516(4) . ? C3S N1S 1.525(3) . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? C5S C6S 1.532(5) . ? C5S H5SA 0.9800 . ? C5S H5SB 0.9800 . ? C5S H5SC 0.9800 . ? C6S N2S 1.519(4) . ? C6S H6SA 0.9900 . ? C6S H6SB 0.9900 . ? C7S N2S 1.514(4) . ? C7S C8S 1.533(5) . ? C7S H7SA 0.9900 . ? C7S H7SB 0.9900 . ? C8S H8SA 0.9800 . ? C8S H8SB 0.9800 . ? C8S H8SC 0.9800 . ? Co1 N2 1.975(2) 8_667 ? Co1 N2 1.975(2) . ? Co1 N1 2.040(2) . ? Co1 N1 2.040(2) 15_446 ? Co1 Co1 2.6807(9) 10_554 ? Co1B N1B 1.985(2) 7_455 ? Co1B N1B 1.985(2) . ? Co1B N2B 2.041(2) 7_455 ? Co1B N2B 2.041(2) . ? Co1B Co1B 2.6637(9) 10_454 ? N1 C1 1.434(3) 10_554 ? N1 Co1 2.040(2) 10_554 ? N2B C6B 1.421(3) 10_454 ? N2B Co1B 2.041(2) 10_454 ? N1S C1S 1.515(3) 15_444 ? N1S C3S 1.525(3) 15_444 ? N2S C7S 1.514(4) 10_454 ? N2S C6S 1.519(4) 10_454 ? 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 C2 C1 N1 121.3(2) . . ? C2 C1 C6 120.2(2) . . ? N1 C1 C6 118.5(2) . . ? C1 C2 C3 121.6(3) . . ? C1 C2 H2A 119.2 . . ? C3 C2 H2A 119.2 . . ? C2 C3 C4 118.4(3) . . ? C2 C3 H3A 120.8 . . ? C4 C3 H3A 120.8 . . ? C5 C4 C3 121.0(3) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 122.1(3) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 N2 127.8(2) . . ? C5 C6 C1 116.5(2) . . ? N2 C6 C1 115.7(2) . . ? O1 C7 N2 127.4(3) . . ? O1 C7 C8 116.8(2) . . ? N2 C7 C8 115.8(2) . . ? C10 C8 C7 109.3(3) . . ? C10 C8 C9 111.0(3) . . ? C7 C8 C9 109.3(3) . . ? C10 C8 H8A 109.1 . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6B C1B N1B 117.0(2) . . ? C6B C1B C2B 118.1(3) . . ? N1B C1B C2B 124.9(3) . . ? C3B C2B C1B 120.1(3) . . ? C3B C2B H2BA 120.0 . . ? C1B C2B H2BA 120.0 . . ? C4B C3B C2B 120.1(3) . . ? C4B C3B H3BA 119.9 . . ? C2B C3B H3BA 119.9 . . ? C3B C4B C5B 120.2(3) . . ? C3B C4B H4BA 119.9 . . ? C5B C4B H4BA 119.9 . . ? C4B C5B C6B 120.7(3) . . ? C4B C5B H5BA 119.7 . . ? C6B C5B H5BA 119.7 . . ? C1B C6B C5B 120.7(2) . . ? C1B C6B N2B 119.3(2) . . ? C5B C6B N2B 120.0(2) . . ? O1B C7B N1B 125.8(3) . . ? O1B C7B C8B 118.9(3) . . ? N1B C7B C8B 115.3(2) . . ? C7B C8B C10B 111.5(3) . . ? C7B C8B C9B 107.4(3) . . ? C10B C8B C9B 108.7(3) . . ? C7B C8B H8BA 109.7 . . ? C10B C8B H8BA 109.7 . . ? C9B C8B H8BA 109.7 . . ? C8B C9B H9BA 109.5 . . ? C8B C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? C8B C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? C8B C10B H10BA 109.5 . . ? C8B C10B H10BB 109.5 . . ? H10BA C10B H10BB 109.5 . . ? C8B C10B H10BC 109.5 . . ? H10BA C10B H10BC 109.5 . . ? H10BB C10B H10BC 109.5 . . ? N1S C1S C2S 114.6(3) . . ? N1S C1S H1SA 108.6 . . ? C2S C1S H1SA 108.6 . . ? N1S C1S H1SB 108.6 . . ? C2S C1S H1SB 108.6 . . ? H1SA C1S H1SB 107.6 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? C4S C3S N1S 114.1(3) . . ? C4S C3S H3SA 108.7 . . ? N1S C3S H3SA 108.7 . . ? C4S C3S H3SB 108.7 . . ? N1S C3S H3SB 108.7 . . ? H3SA C3S H3SB 107.6 . . ? C3S C4S H4SA 109.5 . . ? C3S C4S H4SB 109.5 . . ? H4SA C4S H4SB 109.5 . . ? C3S C4S H4SC 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? C6S C5S H5SA 109.5 . . ? C6S C5S H5SB 109.5 . . ? H5SA C5S H5SB 109.5 . . ? C6S C5S H5SC 109.5 . . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? N2S C6S C5S 113.9(3) . . ? N2S C6S H6SA 108.8 . . ? C5S C6S H6SA 108.8 . . ? N2S C6S H6SB 108.8 . . ? C5S C6S H6SB 108.8 . . ? H6SA C6S H6SB 107.7 . . ? N2S C7S C8S 115.1(3) . . ? N2S C7S H7SA 108.5 . . ? C8S C7S H7SA 108.5 . . ? N2S C7S H7SB 108.5 . . ? C8S C7S H7SB 108.5 . . ? H7SA C7S H7SB 107.5 . . ? C7S C8S H8SA 109.5 . . ? C7S C8S H8SB 109.5 . . ? H8SA C8S H8SB 109.5 . . ? C7S C8S H8SC 109.5 . . ? H8SA C8S H8SC 109.5 . . ? H8SB C8S H8SC 109.5 . . ? N2 Co1 N2 141.63(13) 8_667 . ? N2 Co1 N1 120.01(7) 8_667 . ? N2 Co1 N1 86.08(7) . . ? N2 Co1 N1 86.08(7) 8_667 15_446 ? N2 Co1 N1 120.02(7) . 15_446 ? N1 Co1 N1 97.84(11) . 15_446 ? N2 Co1 Co1 109.18(7) 8_667 10_554 ? N2 Co1 Co1 109.18(7) . 10_554 ? N1 Co1 Co1 48.92(5) . 10_554 ? N1 Co1 Co1 48.92(5) 15_446 10_554 ? N1B Co1B N1B 143.85(14) 7_455 . ? N1B Co1B N2B 85.36(7) 7_455 7_455 ? N1B Co1B N2B 119.08(7) . 7_455 ? N1B Co1B N2B 119.08(7) 7_455 . ? N1B Co1B N2B 85.35(7) . . ? N2B Co1B N2B 98.52(10) 7_455 . ? N1B Co1B Co1B 108.08(7) 7_455 10_454 ? N1B Co1B Co1B 108.07(7) . 10_454 ? N2B Co1B Co1B 49.26(5) 7_455 10_454 ? N2B Co1B Co1B 49.26(5) . 10_454 ? C1 N1 C1 113.3(3) 10_554 . ? C1 N1 Co1 107.94(11) 10_554 10_554 ? C1 N1 Co1 121.40(11) . 10_554 ? C1 N1 Co1 121.40(11) 10_554 . ? C1 N1 Co1 107.95(11) . . ? Co1 N1 Co1 82.16(11) 10_554 . ? C7 N2 C6 121.3(2) . . ? C7 N2 Co1 126.09(19) . . ? C6 N2 Co1 111.79(16) . . ? C7B N1B C1B 123.6(2) . . ? C7B N1B Co1B 124.99(19) . . ? C1B N1B Co1B 110.92(17) . . ? C6B N2B C6B 116.2(3) . 10_454 ? C6B N2B Co1B 119.98(11) . 10_454 ? C6B N2B Co1B 107.50(11) 10_454 10_454 ? C6B N2B Co1B 107.50(11) . . ? C6B N2B Co1B 119.97(11) 10_454 . ? Co1B N2B Co1B 81.48(10) 10_454 . ? C1S N1S C1S 104.5(3) 15_444 . ? C1S N1S C3S 111.53(18) 15_444 . ? C1S N1S C3S 112.17(18) . . ? C1S N1S C3S 112.17(18) 15_444 15_444 ? C1S N1S C3S 111.54(18) . 15_444 ? C3S N1S C3S 105.2(3) . 15_444 ? C7S N2S C7S 111.5(4) 10_454 . ? C7S N2S C6S 109.0(2) 10_454 10_454 ? C7S N2S C6S 108.0(2) . 10_454 ? C7S N2S C6S 108.0(2) 10_454 . ? C7S N2S C6S 109.0(2) . . ? C6S N2S C6S 111.5(4) 10_454 . ? 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 N1 C1 C2 C3 -179.6(3) . . . . ? C6 C1 C2 C3 -1.1(4) . . . . ? C1 C2 C3 C4 -2.9(5) . . . . ? C2 C3 C4 C5 4.7(5) . . . . ? C3 C4 C5 C6 -2.3(5) . . . . ? C4 C5 C6 N2 -179.6(3) . . . . ? C4 C5 C6 C1 -1.7(4) . . . . ? C2 C1 C6 C5 3.4(4) . . . . ? N1 C1 C6 C5 -178.1(2) . . . . ? C2 C1 C6 N2 -178.4(2) . . . . ? N1 C1 C6 N2 0.1(3) . . . . ? O1 C7 C8 C10 71.3(4) . . . . ? N2 C7 C8 C10 -106.4(3) . . . . ? O1 C7 C8 C9 -50.4(4) . . . . ? N2 C7 C8 C9 131.9(3) . . . . ? C6B C1B C2B C3B -2.8(5) . . . . ? N1B C1B C2B C3B 179.6(3) . . . . ? C1B C2B C3B C4B 2.3(5) . . . . ? C2B C3B C4B C5B -1.2(5) . . . . ? C3B C4B C5B C6B 0.6(5) . . . . ? N1B C1B C6B C5B -180.0(2) . . . . ? C2B C1B C6B C5B 2.3(4) . . . . ? N1B C1B C6B N2B -0.9(4) . . . . ? C2B C1B C6B N2B -178.7(2) . . . . ? C4B C5B C6B C1B -1.2(4) . . . . ? C4B C5B C6B N2B 179.8(3) . . . . ? O1B C7B C8B C10B -50.2(4) . . . . ? N1B C7B C8B C10B 131.0(3) . . . . ? O1B C7B C8B C9B 68.8(4) . . . . ? N1B C7B C8B C9B -110.0(3) . . . . ? C2 C1 N1 C1 -43.6(2) . . . 10_554 ? C6 C1 N1 C1 137.9(2) . . . 10_554 ? C2 C1 N1 Co1 87.4(3) . . . 10_554 ? C6 C1 N1 Co1 -91.1(2) . . . 10_554 ? C2 C1 N1 Co1 179.1(2) . . . . ? C6 C1 N1 Co1 0.6(2) . . . . ? N2 Co1 N1 C1 16.3(2) 8_667 . . 10_554 ? N2 Co1 N1 C1 -133.94(18) . . . 10_554 ? N1 Co1 N1 C1 106.28(16) 15_446 . . 10_554 ? Co1 Co1 N1 C1 106.28(16) 10_554 . . 10_554 ? N2 Co1 N1 C1 149.46(14) 8_667 . . . ? N2 Co1 N1 C1 -0.76(15) . . . . ? N1 Co1 N1 C1 -120.54(13) 15_446 . . . ? Co1 Co1 N1 C1 -120.54(13) 10_554 . . . ? N2 Co1 N1 Co1 -89.99(8) 8_667 . . 10_554 ? N2 Co1 N1 Co1 119.78(7) . . . 10_554 ? N1 Co1 N1 Co1 0.0 15_446 . . 10_554 ? O1 C7 N2 C6 -1.3(5) . . . . ? C8 C7 N2 C6 176.1(2) . . . . ? O1 C7 N2 Co1 167.3(3) . . . . ? C8 C7 N2 Co1 -15.3(4) . . . . ? C5 C6 N2 C7 -12.7(4) . . . . ? C1 C6 N2 C7 169.4(2) . . . . ? C5 C6 N2 Co1 177.2(2) . . . . ? C1 C6 N2 Co1 -0.7(3) . . . . ? N2 Co1 N2 C7 55.1(2) 8_667 . . . ? N1 Co1 N2 C7 -168.7(2) . . . . ? N1 Co1 N2 C7 -71.9(3) 15_446 . . . ? Co1 Co1 N2 C7 -124.9(2) 10_554 . . . ? N2 Co1 N2 C6 -135.32(18) 8_667 . . . ? N1 Co1 N2 C6 0.84(17) . . . . ? N1 Co1 N2 C6 97.63(18) 15_446 . . . ? Co1 Co1 N2 C6 44.68(18) 10_554 . . . ? O1B C7B N1B C1B 2.0(5) . . . . ? C8B C7B N1B C1B -179.3(3) . . . . ? O1B C7B N1B Co1B 173.2(2) . . . . ? C8B C7B N1B Co1B -8.1(4) . . . . ? C6B C1B N1B C7B 173.1(3) . . . . ? C2B C1B N1B C7B -9.3(4) . . . . ? C6B C1B N1B Co1B 0.8(3) . . . . ? C2B C1B N1B Co1B 178.4(2) . . . . ? N1B Co1B N1B C7B 51.8(2) 7_455 . . . ? N2B Co1B N1B C7B -75.3(2) 7_455 . . . ? N2B Co1B N1B C7B -172.5(2) . . . . ? Co1B Co1B N1B C7B -128.2(2) 10_454 . . . ? N1B Co1B N1B C1B -136.01(18) 7_455 . . . ? N2B Co1B N1B C1B 96.82(18) 7_455 . . . ? N2B Co1B N1B C1B -0.35(17) . . . . ? Co1B Co1B N1B C1B 43.99(18) 10_454 . . . ? C1B C6B N2B C6B 138.3(3) . . . 10_454 ? C5B C6B N2B C6B -42.7(2) . . . 10_454 ? C1B C6B N2B Co1B -89.6(2) . . . 10_454 ? C5B C6B N2B Co1B 89.5(3) . . . 10_454 ? C1B C6B N2B Co1B 0.6(3) . . . . ? C5B C6B N2B Co1B 179.6(2) . . . . ? N1B Co1B N2B C6B 151.75(14) 7_455 . . . ? N1B Co1B N2B C6B -0.11(14) . . . . ? N2B Co1B N2B C6B -118.85(13) 7_455 . . . ? Co1B Co1B N2B C6B -118.85(13) 10_454 . . . ? N1B Co1B N2B C6B 15.94(19) 7_455 . . 10_454 ? N1B Co1B N2B C6B -135.91(17) . . . 10_454 ? N2B Co1B N2B C6B 105.34(16) 7_455 . . 10_454 ? Co1B Co1B N2B C6B 105.34(16) 10_454 . . 10_454 ? N1B Co1B N2B Co1B -89.40(8) 7_455 . . 10_454 ? N1B Co1B N2B Co1B 118.74(7) . . . 10_454 ? N2B Co1B N2B Co1B 0.0 7_455 . . 10_454 ? C2S C1S N1S C1S 173.5(3) . . . 15_444 ? C2S C1S N1S C3S 52.6(3) . . . . ? C2S C1S N1S C3S -65.1(3) . . . 15_444 ? C4S C3S N1S C1S -65.2(3) . . . 15_444 ? C4S C3S N1S C1S 51.6(3) . . . . ? C4S C3S N1S C3S 173.0(3) . . . 15_444 ? C8S C7S N2S C7S -56.4(3) . . . 10_454 ? C8S C7S N2S C6S -176.1(3) . . . 10_454 ? C8S C7S N2S C6S 62.6(4) . . . . ? C5S C6S N2S C7S -67.2(4) . . . 10_454 ? C5S C6S N2S C7S 171.6(3) . . . . ? C5S C6S N2S C6S 52.5(3) . . . 10_454 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 30.71 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.811 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.078 data_twin5 _database_code_depnum_ccdc_archive 'CCDC 782884' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49.47 H68.94 Cl2.94 Co N7 O4' _chemical_formula_weight 988.85 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.264(10) _cell_length_b 14.280(12) _cell_length_c 15.642(13) _cell_angle_alpha 101.969(10) _cell_angle_beta 91.656(10) _cell_angle_gamma 103.820(10) _cell_volume 2593(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 346 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 12.49 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1047 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8613 _exptl_absorpt_correction_T_max 0.9638 _exptl_absorpt_process_details twinabs _exptl_special_details ; ? ; _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 '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 9132 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.4061 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9133 _reflns_number_gt 3096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+9.5000P] 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 9133 _refine_ls_number_parameters 560 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3335 _refine_ls_R_factor_gt 0.1377 _refine_ls_wR_factor_ref 0.3228 _refine_ls_wR_factor_gt 0.2424 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 C1 C 0.3132(13) 0.5748(12) 0.3324(11) 0.034(4) Uiso 1 1 d . . . C2 C 0.2524(16) 0.4958(14) 0.3670(12) 0.056(5) Uiso 1 1 d . . . H2A H 0.1873 0.4508 0.3347 0.067 Uiso 1 1 calc R . . C3 C 0.2882(15) 0.4845(14) 0.4479(12) 0.056(6) Uiso 1 1 d . . . H3A H 0.2490 0.4314 0.4719 0.067 Uiso 1 1 calc R . . C4 C 0.3827(14) 0.5529(12) 0.4930(11) 0.032(4) Uiso 1 1 d . . . H4A H 0.4034 0.5471 0.5504 0.039 Uiso 1 1 calc R . . C5 C 0.4488(16) 0.6280(15) 0.4615(11) 0.052(6) Uani 1 1 d . . . H5A H 0.5166 0.6692 0.4930 0.063 Uiso 1 1 calc R . . C6 C 0.4097(14) 0.6411(12) 0.3784(10) 0.032(4) Uani 1 1 d . . . C7 C 0.5778(14) 0.7603(14) 0.3659(11) 0.041(5) Uani 1 1 d . . . C8 C 0.6556(16) 0.7046(13) 0.3786(11) 0.045(5) Uani 1 1 d . . . H8A H 0.6298 0.6354 0.3741 0.054 Uiso 1 1 calc R . . C9 C 0.7669(17) 0.7497(15) 0.3971(11) 0.051(6) Uani 1 1 d . . . H9A H 0.8170 0.7125 0.4111 0.061 Uiso 1 1 calc R . . C10 C 0.8089(19) 0.8471(16) 0.3961(13) 0.070(6) Uani 1 1 d . . . H10A H 0.8878 0.8757 0.4039 0.085 Uiso 1 1 calc R . . C11 C 0.7383(18) 0.9007(12) 0.3842(13) 0.062(6) Uani 1 1 d . . . H11A H 0.7672 0.9697 0.3889 0.074 Uiso 1 1 calc R . . C12 C 0.6259(16) 0.8611(15) 0.3656(10) 0.039(5) Uani 1 1 d . . . C13 C 0.5737(19) 1.0094(18) 0.3373(14) 0.057(6) Uani 1 1 d . . . C14 C 0.4659(16) 1.0509(14) 0.3258(12) 0.053(6) Uani 1 1 d . . . H14A H 0.3962 0.9959 0.3195 0.064 Uiso 1 1 calc R . . C15 C 0.4681(14) 1.1247(12) 0.4086(12) 0.049(5) Uani 1 1 d . . . H15A H 0.4042 1.1543 0.4057 0.074 Uiso 1 1 calc R . . H15B H 0.5386 1.1765 0.4167 0.074 Uiso 1 1 calc R . . H15C H 0.4630 1.0919 0.4581 0.074 Uiso 1 1 calc R . . C16 C 0.4728(17) 1.0921(16) 0.2449(12) 0.075(7) Uani 1 1 d . . . H16A H 0.4659 1.0383 0.1931 0.113 Uiso 1 1 calc R . . H16B H 0.5455 1.1403 0.2479 0.113 Uiso 1 1 calc R . . H16C H 0.4116 1.1247 0.2408 0.113 Uiso 1 1 calc R . . C17 C 0.2103(18) 0.5345(15) 0.1904(12) 0.052(6) Uani 1 1 d . . . C18 C 0.2002(15) 0.5672(13) 0.1034(11) 0.048(5) Uani 1 1 d . . . H18A H 0.2636 0.6260 0.1032 0.058 Uiso 1 1 calc R . . C19 C 0.2063(16) 0.4835(13) 0.0269(11) 0.057(6) Uani 1 1 d . . . H19A H 0.1987 0.5044 -0.0284 0.086 Uiso 1 1 calc R . . H19B H 0.1451 0.4253 0.0275 0.086 Uiso 1 1 calc R . . H19C H 0.2789 0.4670 0.0324 0.086 Uiso 1 1 calc R . . C20 C 0.0865(15) 0.5956(13) 0.0944(12) 0.061(5) Uani 1 1 d . . . H20A H 0.0790 0.6145 0.0382 0.091 Uiso 1 1 calc R . . H20B H 0.0847 0.6514 0.1424 0.091 Uiso 1 1 calc R . . H20C H 0.0242 0.5390 0.0969 0.091 Uiso 1 1 calc R . . C21 C 0.3201(15) 0.8396(13) 0.1381(10) 0.040(5) Uani 1 1 d . . . C22 C 0.2575(15) 0.8845(11) 0.0887(11) 0.041(5) Uani 1 1 d . . . H22A H 0.1880 0.8962 0.1073 0.049 Uiso 1 1 calc R . . C23 C 0.2980(16) 0.9116(12) 0.0127(12) 0.048(5) Uani 1 1 d . . . H23A H 0.2557 0.9418 -0.0201 0.057 Uiso 1 1 calc R . . C24 C 0.3969(19) 0.8954(17) -0.0149(13) 0.069(7) Uani 1 1 d . . . H24A H 0.4241 0.9145 -0.0666 0.082 Uiso 1 1 calc R . . C25 C 0.4590(17) 0.8502(13) 0.0336(11) 0.049(5) Uani 1 1 d . . . H25A H 0.5284 0.8389 0.0143 0.059 Uiso 1 1 calc R . . C26 C 0.4209(14) 0.8220(14) 0.1086(11) 0.039(5) Uani 1 1 d . . . C27 C 0.5884(17) 0.7782(15) 0.1552(11) 0.043(5) Uani 1 1 d . . . C28 C 0.6631(17) 0.8672(17) 0.1543(11) 0.056(6) Uani 1 1 d . . . H28A H 0.6335 0.9216 0.1488 0.067 Uiso 1 1 calc R . . C29 C 0.7746(19) 0.8805(15) 0.1607(12) 0.057(6) Uani 1 1 d . . . H29A H 0.8224 0.9438 0.1615 0.068 Uiso 1 1 calc R . . C30 C 0.8211(17) 0.8022(16) 0.1663(13) 0.061(6) Uani 1 1 d . . . H30A H 0.9005 0.8107 0.1706 0.074 Uiso 1 1 calc R . . C31 C 0.7481(18) 0.7108(16) 0.1653(10) 0.054(6) Uani 1 1 d . . . H31A H 0.7783 0.6561 0.1681 0.065 Uiso 1 1 calc R . . C32 C 0.6322(16) 0.6979(13) 0.1602(11) 0.039(5) Uani 1 1 d . . . C33 C 0.5727(17) 0.5186(12) 0.1734(12) 0.039(5) Uani 1 1 d . . . C34 C 0.4715(16) 0.4375(14) 0.1653(12) 0.053(6) Uani 1 1 d . . . H34A H 0.4034 0.4638 0.1611 0.063 Uiso 1 1 calc R . . C35 C 0.4670(17) 0.3892(15) 0.2447(14) 0.079(7) Uani 1 1 d . . . H35A H 0.4707 0.4394 0.2987 0.119 Uiso 1 1 calc R . . H35B H 0.5311 0.3595 0.2469 0.119 Uiso 1 1 calc R . . H35C H 0.3965 0.3377 0.2392 0.119 Uiso 1 1 calc R . . C36 C 0.4760(19) 0.3648(16) 0.0792(16) 0.105(10) Uani 1 1 d . . . H36A H 0.4757 0.3979 0.0303 0.158 Uiso 1 1 calc R . . H36B H 0.4102 0.3082 0.0707 0.158 Uiso 1 1 calc R . . H36C H 0.5449 0.3418 0.0816 0.158 Uiso 1 1 calc R . . C37 C 0.2147(15) 0.8474(16) 0.2676(10) 0.050(6) Uani 1 1 d . . . C38 C 0.1936(16) 0.8068(13) 0.3511(12) 0.044(5) Uani 1 1 d . . . H38A H 0.2486 0.7666 0.3575 0.053 Uiso 1 1 calc R . . C39 C 0.214(2) 0.8891(16) 0.4251(12) 0.084(7) Uani 1 1 d . . . H39A H 0.2003 0.8647 0.4790 0.125 Uiso 1 1 calc R . . H39B H 0.1630 0.9310 0.4183 0.125 Uiso 1 1 calc R . . H39C H 0.2922 0.9277 0.4286 0.125 Uiso 1 1 calc R . . C40 C 0.0790(19) 0.7416(17) 0.3401(13) 0.097(8) Uani 1 1 d . . . H40A H 0.0641 0.7145 0.3924 0.145 Uiso 1 1 calc R . . H40B H 0.0724 0.6873 0.2887 0.145 Uiso 1 1 calc R . . H40C H 0.0242 0.7795 0.3317 0.145 Uiso 1 1 calc R . . C1C C 0.7797(17) 0.2983(15) 0.3508(13) 0.064(6) Uani 1 1 d . . . H1CA H 0.7413 0.2273 0.3307 0.077 Uiso 1 1 calc R . . H1CB H 0.7211 0.3358 0.3585 0.077 Uiso 1 1 calc R . . C2C C 0.848(2) 0.3149(15) 0.4413(13) 0.087(8) Uani 1 1 d . . . H2CA H 0.7971 0.2921 0.4840 0.131 Uiso 1 1 calc R . . H2CB H 0.8846 0.3854 0.4624 0.131 Uiso 1 1 calc R . . H2CC H 0.9060 0.2774 0.4341 0.131 Uiso 1 1 calc R . . C3C C 0.9241(14) 0.4346(14) 0.3102(12) 0.054(5) Uani 1 1 d . . . H3CA H 0.9822 0.4370 0.3565 0.065 Uiso 1 1 calc R . . H3CB H 0.9637 0.4520 0.2592 0.065 Uiso 1 1 calc R . . C4C C 0.8629(17) 0.5103(12) 0.3433(13) 0.072(6) Uani 1 1 d . . . H4CA H 0.9164 0.5755 0.3595 0.107 Uiso 1 1 calc R . . H4CB H 0.8249 0.4952 0.3948 0.107 Uiso 1 1 calc R . . H4CC H 0.8069 0.5106 0.2974 0.107 Uiso 1 1 calc R . . C5C C 0.7718(17) 0.3221(14) 0.2030(13) 0.061(6) Uani 1 1 d . . . H5CA H 0.7223 0.2542 0.1876 0.073 Uiso 1 1 calc R . . H5CB H 0.7232 0.3680 0.2200 0.073 Uiso 1 1 calc R . . C6C C 0.8270(16) 0.3439(16) 0.1240(13) 0.076(7) Uani 1 1 d . . . H6CA H 0.7693 0.3362 0.0766 0.114 Uiso 1 1 calc R . . H6CB H 0.8743 0.2981 0.1056 0.114 Uiso 1 1 calc R . . H6CC H 0.8738 0.4120 0.1375 0.114 Uiso 1 1 calc R . . C7C C 0.9323(17) 0.2649(15) 0.2577(12) 0.066(6) Uani 1 1 d . . . H7CA H 0.9813 0.2915 0.2147 0.079 Uiso 1 1 calc R . . H7CB H 0.9813 0.2693 0.3106 0.079 Uiso 1 1 calc R . . C8C C 0.8773(16) 0.1572(14) 0.2192(13) 0.072(7) Uani 1 1 d . . . H8CA H 0.9355 0.1205 0.2086 0.109 Uiso 1 1 calc R . . H8CB H 0.8342 0.1510 0.1637 0.109 Uiso 1 1 calc R . . H8CC H 0.8266 0.1302 0.2603 0.109 Uiso 1 1 calc R . . C1S C 0.8529(16) 0.8914(15) 0.6350(13) 0.042(6) Uiso 0.80 1 d P . . H1SA H 0.8033 0.9009 0.5881 0.051 Uiso 0.80 1 calc PR . . H1SB H 0.8512 0.9417 0.6887 0.051 Uiso 0.80 1 calc PR . . C2S C 0.8406(19) 0.7696(17) 0.9281(16) 0.038(6) Uiso 0.67 1 d P . . H2SA H 0.8376 0.7168 0.8753 0.045 Uiso 0.67 1 calc PR . . H2SB H 0.7892 0.7416 0.9692 0.045 Uiso 0.67 1 calc PR . . Cl1S Cl 0.9881(5) 0.9086(5) 0.6040(4) 0.0624(19) Uani 0.80 1 d P . . Cl2S Cl 0.8008(5) 0.7718(5) 0.6553(5) 0.0610(19) Uani 0.80 1 d P . . Cl3S Cl 0.7980(8) 0.8685(6) 0.8988(6) 0.082(3) Uani 0.67 1 d P . . Cl4S Cl 0.9808(6) 0.8130(6) 0.9789(4) 0.061(2) Uani 0.67 1 d P . . Co1 Co 0.37779(16) 0.7224(2) 0.24127(19) 0.0437(6) Uani 1 1 d . . . N1 N 0.2876(11) 0.5936(10) 0.2484(9) 0.040(4) Uani 1 1 d . . . N2 N 0.4658(12) 0.7205(11) 0.3459(9) 0.038(4) Uiso 1 1 d . . . N3 N 0.5469(13) 0.9156(11) 0.3526(9) 0.044(4) Uani 1 1 d . . . H3B H 0.4752 0.8872 0.3544 0.052 Uiso 1 1 calc R . . N4 N 0.2923(11) 0.8127(10) 0.2171(9) 0.039(4) Uani 1 1 d . . . N5 N 0.4724(13) 0.7675(10) 0.1545(9) 0.042(4) Uani 1 1 d . . . N6 N 0.5604(13) 0.6077(11) 0.1590(8) 0.041(4) Uani 1 1 d . . . H6A H 0.4897 0.6063 0.1459 0.049 Uiso 1 1 calc R . . N1C N 0.8525(10) 0.3302(13) 0.2829(10) 0.043(3) Uani 1 1 d . . . O1 O 0.1482(11) 0.4518(10) 0.1961(8) 0.067(4) Uani 1 1 d . . . O2 O 0.6664(12) 1.0632(10) 0.3362(10) 0.074(5) Uani 1 1 d . . . O3 O 0.1621(11) 0.9040(10) 0.2504(8) 0.064(4) Uani 1 1 d . . . O4 O 0.6688(10) 0.5115(9) 0.1947(9) 0.065(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 C5 0.057(13) 0.082(17) 0.028(11) 0.010(11) 0.023(10) 0.038(12) C6 0.048(12) 0.036(11) 0.023(10) 0.010(9) 0.006(8) 0.028(9) C7 0.038(12) 0.050(14) 0.042(11) 0.017(10) 0.007(9) 0.016(10) C8 0.048(14) 0.041(12) 0.054(12) 0.007(10) 0.003(10) 0.028(10) C9 0.052(15) 0.055(14) 0.059(14) 0.026(11) -0.008(10) 0.030(11) C10 0.066(15) 0.057(15) 0.078(16) 0.002(13) -0.017(12) 0.008(13) C11 0.062(15) 0.010(10) 0.117(19) 0.017(11) 0.019(13) 0.012(11) C12 0.044(13) 0.056(14) 0.024(10) 0.013(9) 0.009(9) 0.021(11) C13 0.064(16) 0.055(18) 0.044(14) -0.014(13) 0.012(12) 0.018(14) C14 0.058(14) 0.053(14) 0.049(13) -0.004(11) 0.016(10) 0.025(11) C15 0.044(12) 0.038(12) 0.074(15) 0.014(11) 0.021(10) 0.024(10) C16 0.097(17) 0.094(19) 0.053(14) 0.039(13) 0.008(12) 0.039(14) C17 0.079(16) 0.034(13) 0.035(12) 0.018(10) -0.014(11) -0.006(12) C18 0.044(12) 0.044(12) 0.049(13) -0.002(11) -0.012(9) 0.007(10) C19 0.100(16) 0.061(14) 0.032(11) 0.014(10) -0.004(10) 0.057(12) C20 0.075(15) 0.053(13) 0.056(13) 0.003(10) -0.003(11) 0.026(11) C21 0.071(13) 0.044(11) 0.014(9) 0.014(8) 0.004(8) 0.023(9) C22 0.056(11) 0.029(10) 0.050(11) 0.029(9) 0.011(9) 0.014(8) C23 0.064(13) 0.032(11) 0.056(12) 0.018(9) 0.010(10) 0.023(9) C24 0.086(17) 0.090(17) 0.048(13) 0.039(12) 0.012(12) 0.037(14) C25 0.083(15) 0.041(13) 0.026(11) -0.001(10) 0.013(11) 0.028(11) C26 0.036(12) 0.048(13) 0.036(12) 0.004(10) 0.009(9) 0.019(10) C27 0.048(13) 0.051(14) 0.033(10) 0.009(10) 0.009(9) 0.018(11) C28 0.039(14) 0.085(19) 0.047(12) 0.010(12) 0.011(10) 0.025(13) C29 0.068(17) 0.037(13) 0.058(14) -0.011(11) 0.017(11) 0.017(12) C30 0.036(12) 0.062(16) 0.069(15) 0.003(12) -0.003(10) -0.010(12) C31 0.068(15) 0.072(16) 0.024(10) 0.009(10) 0.006(9) 0.024(13) C32 0.049(13) 0.021(11) 0.062(13) 0.011(9) 0.017(10) 0.030(10) C33 0.064(14) 0.028(13) 0.040(12) 0.024(10) 0.005(10) 0.022(11) C34 0.055(14) 0.045(14) 0.071(15) 0.038(12) -0.004(11) 0.017(11) C35 0.073(15) 0.083(18) 0.114(19) 0.058(15) 0.014(13) 0.048(14) C36 0.09(2) 0.08(2) 0.09(2) -0.046(17) 0.019(15) -0.003(16) C37 0.046(13) 0.080(16) 0.009(10) -0.016(10) -0.006(9) 0.009(12) C38 0.052(13) 0.031(11) 0.053(13) 0.007(11) 0.011(10) 0.020(10) C39 0.16(2) 0.081(17) 0.032(13) 0.038(13) 0.019(13) 0.049(16) C40 0.097(19) 0.12(2) 0.047(14) 0.025(14) 0.006(12) -0.029(16) C1C 0.068(16) 0.060(15) 0.070(16) 0.016(12) 0.025(12) 0.023(12) C2C 0.16(2) 0.078(16) 0.056(14) 0.025(13) 0.018(15) 0.074(16) C3C 0.039(11) 0.063(15) 0.067(13) 0.019(11) -0.012(9) 0.025(11) C4C 0.119(18) 0.019(11) 0.086(15) 0.014(11) -0.002(14) 0.034(11) C5C 0.072(15) 0.045(13) 0.079(16) 0.035(12) -0.026(12) 0.022(11) C6C 0.077(15) 0.107(19) 0.062(15) 0.046(14) -0.004(12) 0.034(14) C7C 0.091(16) 0.066(15) 0.057(13) 0.013(12) 0.002(11) 0.052(13) C8C 0.073(15) 0.076(18) 0.066(14) 0.007(14) -0.010(12) 0.023(12) Cl1S 0.041(4) 0.058(4) 0.100(5) 0.048(4) -0.001(3) 0.009(3) Cl2S 0.053(4) 0.052(4) 0.088(5) 0.033(4) 0.015(4) 0.018(4) Cl3S 0.114(7) 0.054(5) 0.087(6) 0.013(5) -0.022(5) 0.044(5) Cl4S 0.045(4) 0.096(6) 0.046(4) 0.015(4) 0.010(3) 0.025(4) Co1 0.0557(13) 0.0423(15) 0.0408(13) 0.0143(10) 0.0031(16) 0.0226(18) N1 0.046(10) 0.031(10) 0.047(10) 0.011(8) -0.015(8) 0.017(8) N3 0.051(10) 0.026(10) 0.057(11) 0.005(8) 0.010(8) 0.019(8) N4 0.035(9) 0.050(11) 0.037(9) 0.012(8) -0.008(7) 0.019(8) N5 0.073(11) 0.039(9) 0.026(8) 0.010(7) 0.006(7) 0.032(8) N6 0.058(11) 0.039(11) 0.036(9) 0.015(8) 0.002(7) 0.027(9) N1C 0.057(8) 0.038(9) 0.042(8) 0.019(7) 0.004(9) 0.019(10) O1 0.088(11) 0.048(9) 0.058(9) 0.008(8) -0.006(7) 0.009(8) O2 0.064(11) 0.059(11) 0.107(12) 0.044(10) 0.009(9) 0.011(8) O3 0.070(9) 0.082(11) 0.071(10) 0.050(8) -0.003(7) 0.048(8) O4 0.040(9) 0.058(10) 0.103(11) 0.009(9) -0.010(7) 0.032(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.40(2) . ? C1 C2 1.41(2) . ? C1 N1 1.435(19) . ? C2 C3 1.38(2) . ? C2 H2A 0.9500 . ? C3 C4 1.39(2) . ? C3 H3A 0.9500 . ? C4 C5 1.37(2) . ? C4 H4A 0.9500 . ? C5 C6 1.44(2) . ? C5 H5A 0.9500 . ? C6 N2 1.379(19) . ? C7 N2 1.355(19) . ? C7 C8 1.41(2) . ? C7 C12 1.42(2) . ? C8 C9 1.36(2) . ? C8 H8A 0.9500 . ? C9 C10 1.37(2) . ? C9 H9A 0.9500 . ? C10 C11 1.32(2) . ? C10 H10A 0.9500 . ? C11 C12 1.36(2) . ? C11 H11A 0.9500 . ? C12 N3 1.41(2) . ? C13 O2 1.21(2) . ? C13 N3 1.37(3) . ? C13 C14 1.59(3) . ? C14 C15 1.49(2) . ? C14 C16 1.50(2) . ? C14 H14A 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O1 1.265(19) . ? C17 N1 1.30(2) . ? C17 C18 1.54(2) . ? C18 C19 1.52(2) . ? C18 C20 1.55(2) . ? C18 H18A 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.39(2) . ? C21 N4 1.397(19) . ? C21 C22 1.42(2) . ? C22 C23 1.39(2) . ? C22 H22A 0.9500 . ? C23 C24 1.35(2) . ? C23 H23A 0.9500 . ? C24 C25 1.41(2) . ? C24 H24A 0.9500 . ? C25 C26 1.38(2) . ? C25 H25A 0.9500 . ? C26 N5 1.40(2) . ? C27 C28 1.38(2) . ? C27 C32 1.39(2) . ? C27 N5 1.39(2) . ? C28 C29 1.33(2) . ? C28 H28A 0.9500 . ? C29 C30 1.39(3) . ? C29 H29A 0.9500 . ? C30 C31 1.39(2) . ? C30 H30A 0.9500 . ? C31 C32 1.39(2) . ? C31 H31A 0.9500 . ? C32 N6 1.37(2) . ? C33 O4 1.249(19) . ? C33 N6 1.38(2) . ? C33 C34 1.46(2) . ? C34 C36 1.53(2) . ? C34 C35 1.54(2) . ? C34 H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 O3 1.21(2) . ? C37 N4 1.37(2) . ? C37 C38 1.54(2) . ? C38 C39 1.44(2) . ? C38 C40 1.47(2) . ? C38 H38A 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C1C N1C 1.48(2) . ? C1C C2C 1.57(2) . ? C1C H1CA 0.9900 . ? C1C H1CB 0.9900 . ? C2C H2CA 0.9800 . ? C2C H2CB 0.9800 . ? C2C H2CC 0.9800 . ? C3C C4C 1.48(2) . ? C3C N1C 1.50(2) . ? C3C H3CA 0.9900 . ? C3C H3CB 0.9900 . ? C4C H4CA 0.9800 . ? C4C H4CB 0.9800 . ? C4C H4CC 0.9800 . ? C5C C6C 1.48(3) . ? C5C N1C 1.54(2) . ? C5C H5CA 0.9900 . ? C5C H5CB 0.9900 . ? C6C H6CA 0.9800 . ? C6C H6CB 0.9800 . ? C6C H6CC 0.9800 . ? C7C C8C 1.51(2) . ? C7C N1C 1.51(2) . ? C7C H7CA 0.9900 . ? C7C H7CB 0.9900 . ? C8C H8CA 0.9800 . ? C8C H8CB 0.9800 . ? C8C H8CC 0.9800 . ? C1S Cl1S 1.716(19) . ? C1S Cl2S 1.77(2) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2S Cl3S 1.76(2) . ? C2S Cl4S 1.78(2) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? Co1 N5 1.923(15) . ? Co1 N1 1.933(14) . ? Co1 N4 1.933(13) . ? Co1 N2 1.943(14) . ? N3 H3B 0.8800 . ? N6 H6A 0.8800 . ? 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 C6 C1 C2 121.0(16) . . ? C6 C1 N1 113.4(14) . . ? C2 C1 N1 125.5(16) . . ? C3 C2 C1 119.6(18) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C4 118.1(19) . . ? C2 C3 H3A 120.9 . . ? C4 C3 H3A 120.9 . . ? C5 C4 C3 125.2(18) . . ? C5 C4 H4A 117.4 . . ? C3 C4 H4A 117.4 . . ? C4 C5 C6 116.3(18) . . ? C4 C5 H5A 121.9 . . ? C6 C5 H5A 121.9 . . ? N2 C6 C1 120.7(14) . . ? N2 C6 C5 119.8(16) . . ? C1 C6 C5 119.5(17) . . ? N2 C7 C8 123.7(17) . . ? N2 C7 C12 120.5(16) . . ? C8 C7 C12 115.4(17) . . ? C9 C8 C7 120.3(17) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C8 C9 C10 121.7(18) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C11 C10 C9 119(2) . . ? C11 C10 H10A 120.5 . . ? C9 C10 H10A 120.5 . . ? C10 C11 C12 122.4(18) . . ? C10 C11 H11A 118.8 . . ? C12 C11 H11A 118.8 . . ? C11 C12 N3 124.5(18) . . ? C11 C12 C7 120.6(17) . . ? N3 C12 C7 114.6(17) . . ? O2 C13 N3 128(2) . . ? O2 C13 C14 119(2) . . ? N3 C13 C14 112.9(19) . . ? C15 C14 C16 114.6(18) . . ? C15 C14 C13 105.0(16) . . ? C16 C14 C13 108.8(16) . . ? C15 C14 H14A 109.4 . . ? C16 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 N1 127.2(16) . . ? O1 C17 C18 117.5(17) . . ? N1 C17 C18 115.1(16) . . ? C19 C18 C17 109.8(15) . . ? C19 C18 C20 110.0(14) . . ? C17 C18 C20 109.4(16) . . ? C19 C18 H18A 109.2 . . ? C17 C18 H18A 109.2 . . ? C20 C18 H18A 109.2 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 N4 115.1(15) . . ? C26 C21 C22 118.8(16) . . ? N4 C21 C22 126.1(16) . . ? C23 C22 C21 120.0(17) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C24 C23 C22 120.9(18) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C25 119.4(19) . . ? C23 C24 H24A 120.3 . . ? C25 C24 H24A 120.3 . . ? C26 C25 C24 121.2(19) . . ? C26 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C25 C26 C21 119.8(17) . . ? C25 C26 N5 123.8(16) . . ? C21 C26 N5 116.1(16) . . ? C28 C27 C32 118.1(19) . . ? C28 C27 N5 122.3(17) . . ? C32 C27 N5 119.6(18) . . ? C29 C28 C27 123(2) . . ? C29 C28 H28A 118.4 . . ? C27 C28 H28A 118.4 . . ? C28 C29 C30 120(2) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C29 C30 C31 118(2) . . ? C29 C30 H30A 121.0 . . ? C31 C30 H30A 121.0 . . ? C32 C31 C30 121(2) . . ? C32 C31 H31A 119.3 . . ? C30 C31 H31A 119.3 . . ? N6 C32 C31 121.4(16) . . ? N6 C32 C27 119.7(17) . . ? C31 C32 C27 119.0(18) . . ? O4 C33 N6 118.7(17) . . ? O4 C33 C34 123.1(15) . . ? N6 C33 C34 118.2(16) . . ? C33 C34 C36 105.9(17) . . ? C33 C34 C35 111.2(16) . . ? C36 C34 C35 112.3(18) . . ? C33 C34 H34A 109.1 . . ? C36 C34 H34A 109.1 . . ? C35 C34 H34A 109.1 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O3 C37 N4 125.4(18) . . ? O3 C37 C38 119.5(17) . . ? N4 C37 C38 115.0(18) . . ? C39 C38 C40 114.6(18) . . ? C39 C38 C37 108.3(15) . . ? C40 C38 C37 108.2(15) . . ? C39 C38 H38A 108.5 . . ? C40 C38 H38A 108.5 . . ? C37 C38 H38A 108.5 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N1C C1C C2C 112.2(16) . . ? N1C C1C H1CA 109.2 . . ? C2C C1C H1CA 109.2 . . ? N1C C1C H1CB 109.2 . . ? C2C C1C H1CB 109.2 . . ? H1CA C1C H1CB 107.9 . . ? C1C C2C H2CA 109.5 . . ? C1C C2C H2CB 109.5 . . ? H2CA C2C H2CB 109.5 . . ? C1C C2C H2CC 109.5 . . ? H2CA C2C H2CC 109.5 . . ? H2CB C2C H2CC 109.5 . . ? C4C C3C N1C 115.4(15) . . ? C4C C3C H3CA 108.4 . . ? N1C C3C H3CA 108.4 . . ? C4C C3C H3CB 108.4 . . ? N1C C3C H3CB 108.4 . . ? H3CA C3C H3CB 107.5 . . ? C3C C4C H4CA 109.5 . . ? C3C C4C H4CB 109.5 . . ? H4CA C4C H4CB 109.5 . . ? C3C C4C H4CC 109.5 . . ? H4CA C4C H4CC 109.5 . . ? H4CB C4C H4CC 109.5 . . ? C6C C5C N1C 115.3(17) . . ? C6C C5C H5CA 108.5 . . ? N1C C5C H5CA 108.5 . . ? C6C C5C H5CB 108.5 . . ? N1C C5C H5CB 108.5 . . ? H5CA C5C H5CB 107.5 . . ? C5C C6C H6CA 109.5 . . ? C5C C6C H6CB 109.5 . . ? H6CA C6C H6CB 109.5 . . ? C5C C6C H6CC 109.5 . . ? H6CA C6C H6CC 109.5 . . ? H6CB C6C H6CC 109.5 . . ? C8C C7C N1C 115.6(17) . . ? C8C C7C H7CA 108.4 . . ? N1C C7C H7CA 108.4 . . ? C8C C7C H7CB 108.4 . . ? N1C C7C H7CB 108.4 . . ? H7CA C7C H7CB 107.4 . . ? C7C C8C H8CA 109.5 . . ? C7C C8C H8CB 109.5 . . ? H8CA C8C H8CB 109.5 . . ? C7C C8C H8CC 109.5 . . ? H8CA C8C H8CC 109.5 . . ? H8CB C8C H8CC 109.5 . . ? Cl1S C1S Cl2S 111.8(11) . . ? Cl1S C1S H1SA 109.3 . . ? Cl2S C1S H1SA 109.3 . . ? Cl1S C1S H1SB 109.3 . . ? Cl2S C1S H1SB 109.3 . . ? H1SA C1S H1SB 107.9 . . ? Cl3S C2S Cl4S 109.2(13) . . ? Cl3S C2S H2SA 109.8 . . ? Cl4S C2S H2SA 109.8 . . ? Cl3S C2S H2SB 109.8 . . ? Cl4S C2S H2SB 109.8 . . ? H2SA C2S H2SB 108.3 . . ? N5 Co1 N1 132.7(6) . . ? N5 Co1 N4 85.1(6) . . ? N1 Co1 N4 114.6(4) . . ? N5 Co1 N2 111.7(5) . . ? N1 Co1 N2 87.3(6) . . ? N4 Co1 N2 131.8(6) . . ? C17 N1 C1 123.8(15) . . ? C17 N1 Co1 126.9(12) . . ? C1 N1 Co1 109.1(11) . . ? C7 N2 C6 121.2(15) . . ? C7 N2 Co1 126.8(12) . . ? C6 N2 Co1 107.6(11) . . ? C13 N3 C12 124.9(17) . . ? C13 N3 H3B 117.5 . . ? C12 N3 H3B 117.5 . . ? C37 N4 C21 122.9(15) . . ? C37 N4 Co1 127.1(13) . . ? C21 N4 Co1 110.0(11) . . ? C27 N5 C26 120.1(15) . . ? C27 N5 Co1 125.9(11) . . ? C26 N5 Co1 110.4(12) . . ? C32 N6 C33 135.2(16) . . ? C32 N6 H6A 112.4 . . ? C33 N6 H6A 112.4 . . ? C1C N1C C3C 113.9(15) . . ? C1C N1C C7C 111.8(15) . . ? C3C N1C C7C 106.5(12) . . ? C1C N1C C5C 105.8(12) . . ? C3C N1C C5C 109.1(14) . . ? C7C N1C C5C 109.7(15) . . ? 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 C6 C1 C2 C3 1(3) . . . . ? N1 C1 C2 C3 178.1(16) . . . . ? C1 C2 C3 C4 1(3) . . . . ? C2 C3 C4 C5 -4(3) . . . . ? C3 C4 C5 C6 6(3) . . . . ? C2 C1 C6 N2 -177.2(15) . . . . ? N1 C1 C6 N2 5(2) . . . . ? C2 C1 C6 C5 1(2) . . . . ? N1 C1 C6 C5 -176.8(14) . . . . ? C4 C5 C6 N2 174.2(15) . . . . ? C4 C5 C6 C1 -4(2) . . . . ? N2 C7 C8 C9 178.9(16) . . . . ? C12 C7 C8 C9 6(2) . . . . ? C7 C8 C9 C10 -6(3) . . . . ? C8 C9 C10 C11 6(3) . . . . ? C9 C10 C11 C12 -6(3) . . . . ? C10 C11 C12 N3 179.8(18) . . . . ? C10 C11 C12 C7 6(3) . . . . ? N2 C7 C12 C11 -179.0(16) . . . . ? C8 C7 C12 C11 -6(2) . . . . ? N2 C7 C12 N3 6(2) . . . . ? C8 C7 C12 N3 179.9(14) . . . . ? O2 C13 C14 C15 -71(2) . . . . ? N3 C13 C14 C15 105.8(18) . . . . ? O2 C13 C14 C16 52(2) . . . . ? N3 C13 C14 C16 -131.1(18) . . . . ? O1 C17 C18 C19 -49(2) . . . . ? N1 C17 C18 C19 127.2(18) . . . . ? O1 C17 C18 C20 72(2) . . . . ? N1 C17 C18 C20 -112.0(19) . . . . ? C26 C21 C22 C23 -1(3) . . . . ? N4 C21 C22 C23 177.1(16) . . . . ? C21 C22 C23 C24 0(3) . . . . ? C22 C23 C24 C25 0(3) . . . . ? C23 C24 C25 C26 0(3) . . . . ? C24 C25 C26 C21 -1(3) . . . . ? C24 C25 C26 N5 173.0(18) . . . . ? N4 C21 C26 C25 -176.8(16) . . . . ? C22 C21 C26 C25 1(3) . . . . ? N4 C21 C26 N5 9(2) . . . . ? C22 C21 C26 N5 -173.1(15) . . . . ? C32 C27 C28 C29 -2(3) . . . . ? N5 C27 C28 C29 175.4(16) . . . . ? C27 C28 C29 C30 2(3) . . . . ? C28 C29 C30 C31 0(3) . . . . ? C29 C30 C31 C32 -1(3) . . . . ? C30 C31 C32 N6 179.8(17) . . . . ? C30 C31 C32 C27 1(3) . . . . ? C28 C27 C32 N6 -178.3(15) . . . . ? N5 C27 C32 N6 4(3) . . . . ? C28 C27 C32 C31 1(3) . . . . ? N5 C27 C32 C31 -176.8(14) . . . . ? O4 C33 C34 C36 -75(2) . . . . ? N6 C33 C34 C36 106.4(19) . . . . ? O4 C33 C34 C35 47(3) . . . . ? N6 C33 C34 C35 -131.4(17) . . . . ? O3 C37 C38 C39 -57(2) . . . . ? N4 C37 C38 C39 124.1(18) . . . . ? O3 C37 C38 C40 67(2) . . . . ? N4 C37 C38 C40 -111.1(18) . . . . ? O1 C17 N1 C1 -2(3) . . . . ? C18 C17 N1 C1 -177.7(15) . . . . ? O1 C17 N1 Co1 -177.2(15) . . . . ? C18 C17 N1 Co1 7(3) . . . . ? C6 C1 N1 C17 171.3(17) . . . . ? C2 C1 N1 C17 -6(3) . . . . ? C6 C1 N1 Co1 -12.8(16) . . . . ? C2 C1 N1 Co1 169.6(14) . . . . ? N5 Co1 N1 C17 -54.1(19) . . . . ? N4 Co1 N1 C17 53.1(18) . . . . ? N2 Co1 N1 C17 -171.5(17) . . . . ? N5 Co1 N1 C1 130.1(11) . . . . ? N4 Co1 N1 C1 -122.7(10) . . . . ? N2 Co1 N1 C1 12.7(11) . . . . ? C8 C7 N2 C6 34(2) . . . . ? C12 C7 N2 C6 -153.3(15) . . . . ? C8 C7 N2 Co1 -119.3(16) . . . . ? C12 C7 N2 Co1 54(2) . . . . ? C1 C6 N2 C7 -152.4(16) . . . . ? C5 C6 N2 C7 29(2) . . . . ? C1 C6 N2 Co1 5.3(18) . . . . ? C5 C6 N2 Co1 -172.8(12) . . . . ? N5 Co1 N2 C7 10.7(18) . . . . ? N1 Co1 N2 C7 146.1(15) . . . . ? N4 Co1 N2 C7 -92.8(16) . . . . ? N5 Co1 N2 C6 -145.4(9) . . . . ? N1 Co1 N2 C6 -10.0(11) . . . . ? N4 Co1 N2 C6 111.1(11) . . . . ? O2 C13 N3 C12 -4(3) . . . . ? C14 C13 N3 C12 -179.7(14) . . . . ? C11 C12 N3 C13 16(3) . . . . ? C7 C12 N3 C13 -170.2(17) . . . . ? O3 C37 N4 C21 0(3) . . . . ? C38 C37 N4 C21 178.4(15) . . . . ? O3 C37 N4 Co1 -179.8(14) . . . . ? C38 C37 N4 Co1 -1(2) . . . . ? C26 C21 N4 C37 162.2(16) . . . . ? C22 C21 N4 C37 -16(3) . . . . ? C26 C21 N4 Co1 -18.0(19) . . . . ? C22 C21 N4 Co1 163.9(14) . . . . ? N5 Co1 N4 C37 -163.7(15) . . . . ? N1 Co1 N4 C37 61.1(16) . . . . ? N2 Co1 N4 C37 -48.7(17) . . . . ? N5 Co1 N4 C21 16.5(11) . . . . ? N1 Co1 N4 C21 -118.7(11) . . . . ? N2 Co1 N4 C21 131.5(11) . . . . ? C28 C27 N5 C26 34(2) . . . . ? C32 C27 N5 C26 -148.3(17) . . . . ? C28 C27 N5 Co1 -122.3(16) . . . . ? C32 C27 N5 Co1 55(2) . . . . ? C25 C26 N5 C27 31(3) . . . . ? C21 C26 N5 C27 -154.6(15) . . . . ? C25 C26 N5 Co1 -169.1(15) . . . . ? C21 C26 N5 Co1 5.2(19) . . . . ? N1 Co1 N5 C27 -94.3(15) . . . . ? N4 Co1 N5 C27 146.3(15) . . . . ? N2 Co1 N5 C27 13.0(17) . . . . ? N1 Co1 N5 C26 107.3(12) . . . . ? N4 Co1 N5 C26 -12.0(12) . . . . ? N2 Co1 N5 C26 -145.3(10) . . . . ? C31 C32 N6 C33 11(3) . . . . ? C27 C32 N6 C33 -170.2(18) . . . . ? O4 C33 N6 C32 2(3) . . . . ? C34 C33 N6 C32 -179.9(17) . . . . ? C2C C1C N1C C3C -53(2) . . . . ? C2C C1C N1C C7C 68(2) . . . . ? C2C C1C N1C C5C -172.9(14) . . . . ? C4C C3C N1C C1C -52(2) . . . . ? C4C C3C N1C C7C -176.1(14) . . . . ? C4C C3C N1C C5C 65(2) . . . . ? C8C C7C N1C C1C 61(2) . . . . ? C8C C7C N1C C3C -174.0(14) . . . . ? C8C C7C N1C C5C -56(2) . . . . ? C6C C5C N1C C1C -175.9(15) . . . . ? C6C C5C N1C C3C 61(2) . . . . ? C6C C5C N1C C7C -55(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.976 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.132 data_PSM16B _database_code_depnum_ccdc_archive 'CCDC 782885' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H86 Co N8 O4' _chemical_formula_sum 'C56 H86 Co N8 O4' _chemical_formula_weight 994.26 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 Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 17.364(4) _cell_length_b 16.539(4) _cell_length_c 19.385(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5567(2) _cell_formula_units_Z 4 _cell_measurement_temperature 172(2) _cell_measurement_reflns_used 5350 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 21.56 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2148 _exptl_absorpt_coefficient_mu 0.359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9415 _exptl_absorpt_correction_T_max 0.9753 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 172(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_reflns_number 97086 _diffrn_reflns_av_R_equivalents 0.1821 _diffrn_reflns_av_sigmaI/netI 0.1735 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 30.63 _reflns_number_total 16016 _reflns_number_gt 7221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(15) _refine_ls_number_reflns 16016 _refine_ls_number_parameters 622 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1796 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1544 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 C1 C -0.0355(2) 0.9001(2) 0.4401(2) 0.0342(10) Uani 1 1 d . . . C2 C -0.0469(3) 0.9789(3) 0.4613(3) 0.0450(12) Uani 1 1 d . . . H2A H -0.0174 0.9991 0.4988 0.054 Uiso 1 1 calc R . . C3 C -0.1003(3) 1.0298(3) 0.4295(3) 0.0518(14) Uani 1 1 d . . . H3A H -0.1075 1.0836 0.4455 0.062 Uiso 1 1 calc R . . C4 C -0.1432(3) 1.0002(3) 0.3737(3) 0.0559(14) Uani 1 1 d . . . H4A H -0.1800 1.0340 0.3516 0.067 Uiso 1 1 calc R . . C5 C -0.1323(2) 0.9228(3) 0.3509(2) 0.0419(11) Uani 1 1 d . . . H5A H -0.1611 0.9044 0.3123 0.050 Uiso 1 1 calc R . . C6 C -0.0793(2) 0.8686(3) 0.3829(2) 0.0343(10) Uani 1 1 d . . . C7 C -0.1090(2) 0.7582(2) 0.3064(2) 0.0324(10) Uani 1 1 d . . . C8 C -0.0745(3) 0.7349(3) 0.2437(2) 0.0385(11) Uani 1 1 d . . . H8A H -0.0203 0.7409 0.2389 0.046 Uiso 1 1 calc R . . C9 C -0.1158(3) 0.7037(3) 0.1889(2) 0.0501(13) Uani 1 1 d . . . H9A H -0.0903 0.6897 0.1472 0.060 Uiso 1 1 calc R . . C10 C -0.1948(3) 0.6932(3) 0.1952(3) 0.0588(15) Uani 1 1 d . . . H10A H -0.2237 0.6726 0.1575 0.071 Uiso 1 1 calc R . . C11 C -0.2315(3) 0.7129(3) 0.2569(3) 0.0484(13) Uani 1 1 d . . . H11A H -0.2853 0.7043 0.2618 0.058 Uiso 1 1 calc R . . C12 C -0.1893(2) 0.7450(3) 0.3114(2) 0.0397(11) Uani 1 1 d . . . C13 C -0.2968(3) 0.7976(3) 0.3851(3) 0.0460(13) Uani 1 1 d . . . C14 C -0.3196(3) 0.8139(3) 0.4593(3) 0.0566(14) Uani 1 1 d . . . H14A H -0.3032 0.7659 0.4870 0.068 Uiso 1 1 calc R . . C15 C -0.4068(3) 0.8216(4) 0.4673(3) 0.088(2) Uani 1 1 d . . . H15A H -0.4318 0.7737 0.4476 0.132 Uiso 1 1 calc R . . H15B H -0.4247 0.8701 0.4431 0.132 Uiso 1 1 calc R . . H15C H -0.4199 0.8258 0.5163 0.132 Uiso 1 1 calc R . . C16 C -0.2785(4) 0.8854(5) 0.4880(3) 0.120(3) Uani 1 1 d . . . H16A H -0.2229 0.8783 0.4821 0.179 Uiso 1 1 calc R . . H16B H -0.2904 0.8907 0.5373 0.179 Uiso 1 1 calc R . . H16C H -0.2952 0.9343 0.4637 0.179 Uiso 1 1 calc R . . C17 C 0.0639(2) 0.8621(3) 0.5221(2) 0.0401(11) Uani 1 1 d . . . C18 C 0.1383(2) 0.8123(3) 0.5317(2) 0.0400(11) Uani 1 1 d . . . H18A H 0.1501 0.7844 0.4871 0.048 Uiso 1 1 calc R . . C19 C 0.1262(3) 0.7470(3) 0.5878(3) 0.0581(15) Uani 1 1 d . . . H19A H 0.1734 0.7151 0.5930 0.087 Uiso 1 1 calc R . . H19B H 0.0837 0.7114 0.5743 0.087 Uiso 1 1 calc R . . H19C H 0.1138 0.7733 0.6318 0.087 Uiso 1 1 calc R . . C20 C 0.2048(3) 0.8681(3) 0.5489(3) 0.0575(14) Uani 1 1 d . . . H20A H 0.2111 0.9079 0.5119 0.086 Uiso 1 1 calc R . . H20B H 0.2522 0.8364 0.5535 0.086 Uiso 1 1 calc R . . H20C H 0.1941 0.8962 0.5924 0.086 Uiso 1 1 calc R . . C21 C 0.0618(2) 0.5763(2) 0.4594(2) 0.0281(9) Uani 1 1 d . . . C22 C 0.0615(2) 0.4977(3) 0.4852(2) 0.0384(11) Uani 1 1 d . . . H22A H 0.0236 0.4824 0.5181 0.046 Uiso 1 1 calc R . . C23 C 0.1156(2) 0.4415(3) 0.4637(3) 0.0451(12) Uani 1 1 d . . . H23A H 0.1137 0.3880 0.4815 0.054 Uiso 1 1 calc R . . C24 C 0.1720(2) 0.4623(2) 0.4169(3) 0.0412(10) Uani 1 1 d . . . H24A H 0.2096 0.4236 0.4035 0.049 Uiso 1 1 calc R . . C25 C 0.1738(2) 0.5405(3) 0.3893(2) 0.0363(11) Uani 1 1 d . . . H25A H 0.2122 0.5541 0.3563 0.044 Uiso 1 1 calc R . . C26 C 0.11965(18) 0.5992(2) 0.4096(2) 0.0252(8) Uani 1 1 d . . . C27 C 0.1735(2) 0.7066(2) 0.3385(2) 0.0313(10) Uani 1 1 d . . . C28 C 0.1548(3) 0.7251(3) 0.2694(2) 0.0392(11) Uani 1 1 d . . . H28A H 0.1051 0.7114 0.2526 0.047 Uiso 1 1 calc R . . C29 C 0.2060(3) 0.7622(3) 0.2256(2) 0.0403(11) Uani 1 1 d . . . H29A H 0.1920 0.7728 0.1791 0.048 Uiso 1 1 calc R . . C30 C 0.2788(3) 0.7843(3) 0.2500(2) 0.0477(12) Uani 1 1 d . . . H30A H 0.3136 0.8126 0.2208 0.057 Uiso 1 1 calc R . . C31 C 0.3004(2) 0.7648(3) 0.3171(2) 0.0413(11) Uani 1 1 d . . . H31A H 0.3504 0.7785 0.3333 0.050 Uiso 1 1 calc R . . C32 C 0.2488(2) 0.7253(2) 0.3609(2) 0.0325(10) Uani 1 1 d . . . C33 C 0.3405(2) 0.7004(3) 0.4603(2) 0.0407(11) Uani 1 1 d . . . C34 C 0.3415(2) 0.6684(3) 0.5344(2) 0.0442(12) Uani 1 1 d . . . H34A H 0.2979 0.6938 0.5601 0.053 Uiso 1 1 calc R . . C35 C 0.4168(3) 0.6925(4) 0.5700(3) 0.0632(15) Uani 1 1 d . . . H35A H 0.4223 0.7515 0.5689 0.095 Uiso 1 1 calc R . . H35B H 0.4603 0.6676 0.5458 0.095 Uiso 1 1 calc R . . H35C H 0.4159 0.6739 0.6180 0.095 Uiso 1 1 calc R . . C36 C 0.3308(3) 0.5765(3) 0.5361(3) 0.0656(15) Uani 1 1 d . . . H36A H 0.3314 0.5577 0.5840 0.098 Uiso 1 1 calc R . . H36B H 0.3727 0.5505 0.5105 0.098 Uiso 1 1 calc R . . H36C H 0.2813 0.5624 0.5148 0.098 Uiso 1 1 calc R . . C37 C -0.0375(2) 0.6357(2) 0.5320(2) 0.0304(9) Uani 1 1 d . . . C38 C -0.1050(2) 0.6950(2) 0.5352(2) 0.0340(10) Uani 1 1 d . . . H38A H -0.1030 0.7315 0.4941 0.041 Uiso 1 1 calc R . . C39 C -0.1021(3) 0.7467(3) 0.6015(3) 0.0533(14) Uani 1 1 d . . . H39A H -0.0541 0.7778 0.6025 0.080 Uiso 1 1 calc R . . H39B H -0.1044 0.7113 0.6420 0.080 Uiso 1 1 calc R . . H39C H -0.1461 0.7839 0.6022 0.080 Uiso 1 1 calc R . . C40 C -0.1799(2) 0.6461(3) 0.5332(2) 0.0429(11) Uani 1 1 d . . . H40A H -0.1818 0.6142 0.4906 0.064 Uiso 1 1 calc R . . H40B H -0.2240 0.6830 0.5346 0.064 Uiso 1 1 calc R . . H40C H -0.1818 0.6097 0.5731 0.064 Uiso 1 1 calc R . . Co1 Co 0.02088(3) 0.73774(3) 0.41407(3) 0.02813(13) Uani 1 1 d . . . N1 N 0.02367(18) 0.84575(19) 0.46363(17) 0.0326(8) Uani 1 1 d . . . N2 N -0.06397(18) 0.7902(2) 0.36093(17) 0.0316(8) Uani 1 1 d . . . N3 N -0.2264(2) 0.7627(2) 0.37608(19) 0.0429(9) Uani 1 1 d . . . H3B H -0.2010 0.7497 0.4137 0.051 Uiso 1 1 calc R . . N4 N 0.00575(17) 0.63724(19) 0.47307(16) 0.0265(7) Uani 1 1 d . . . N5 N 0.11517(17) 0.67824(19) 0.38415(15) 0.0290(8) Uani 1 1 d . . . N6 N 0.26893(18) 0.7030(2) 0.42983(17) 0.0386(9) Uani 1 1 d . . . H6A H 0.2302 0.6888 0.4565 0.046 Uiso 1 1 calc R . . O1 O 0.0485(2) 0.9124(2) 0.56631(18) 0.0638(10) Uani 1 1 d . . . O2 O -0.33900(18) 0.8154(2) 0.33644(19) 0.0589(10) Uani 1 1 d . . . O3 O -0.02854(16) 0.58843(19) 0.58185(15) 0.0443(8) Uani 1 1 d . . . O4 O 0.39937(17) 0.7192(2) 0.42983(17) 0.0628(10) Uani 1 1 d . . . N1C N 0.0794(2) 0.9996(2) 0.2332(2) 0.0446(10) Uani 1 1 d . . . C1C C 0.0988(4) 0.9995(4) 0.3080(3) 0.0847(19) Uani 1 1 d . . . H1C1 H 0.1309 1.0480 0.3165 0.102 Uiso 1 1 calc R . . H1C2 H 0.0499 1.0079 0.3334 0.102 Uiso 1 1 calc R . . C2C C 0.1383(3) 0.9308(3) 0.3413(3) 0.0652(16) Uani 1 1 d . . . H2CA H 0.1453 0.9423 0.3905 0.098 Uiso 1 1 calc R . . H2CB H 0.1886 0.9226 0.3196 0.098 Uiso 1 1 calc R . . H2CC H 0.1071 0.8818 0.3359 0.098 Uiso 1 1 calc R . . C3C C 0.0453(4) 1.0796(4) 0.2110(3) 0.086(2) Uani 1 1 d . . . H3CA H 0.0845 1.1221 0.2189 0.103 Uiso 1 1 calc R . . H3CB H 0.0358 1.0771 0.1607 0.103 Uiso 1 1 calc R . . C4C C -0.0279(3) 1.1060(4) 0.2453(3) 0.0833(19) Uani 1 1 d . . . H4CA H -0.0438 1.1585 0.2266 0.125 Uiso 1 1 calc R . . H4CB H -0.0195 1.1109 0.2951 0.125 Uiso 1 1 calc R . . H4CC H -0.0683 1.0660 0.2366 0.125 Uiso 1 1 calc R . . C5C C 0.1506(4) 0.9827(4) 0.1894(3) 0.0814(19) Uani 1 1 d . . . H5CA H 0.1675 0.9265 0.1986 0.098 Uiso 1 1 calc R . . H5CB H 0.1356 0.9857 0.1402 0.098 Uiso 1 1 calc R . . C6C C 0.2175(3) 1.0374(4) 0.2005(3) 0.092(2) Uani 1 1 d . . . H6CA H 0.2600 1.0210 0.1703 0.138 Uiso 1 1 calc R . . H6CB H 0.2340 1.0341 0.2488 0.138 Uiso 1 1 calc R . . H6CC H 0.2025 1.0931 0.1897 0.138 Uiso 1 1 calc R . . C7C C 0.0225(4) 0.9290(3) 0.2207(3) 0.0807(19) Uani 1 1 d . . . H7CA H 0.0492 0.8778 0.2320 0.097 Uiso 1 1 calc R . . H7CB H -0.0209 0.9348 0.2535 0.097 Uiso 1 1 calc R . . C8C C -0.0096(4) 0.9218(4) 0.1510(3) 0.107(3) Uani 1 1 d . . . H8CA H -0.0448 0.8754 0.1491 0.161 Uiso 1 1 calc R . . H8CB H 0.0323 0.9138 0.1178 0.161 Uiso 1 1 calc R . . H8CC H -0.0378 0.9712 0.1394 0.161 Uiso 1 1 calc R . . N2C N 0.95496(18) 0.4525(2) 0.26387(17) 0.0346(8) Uani 1 1 d . . . C9C C 0.9059(3) 0.4516(3) 0.3288(2) 0.0454(12) Uani 1 1 d . . . H9CA H 0.9369 0.4290 0.3671 0.054 Uiso 1 1 calc R . . H9CB H 0.8616 0.4150 0.3212 0.054 Uiso 1 1 calc R . . C10C C 0.8751(2) 0.5348(3) 0.3508(3) 0.0495(13) Uani 1 1 d . . . H10B H 0.8443 0.5289 0.3929 0.074 Uiso 1 1 calc R . . H10C H 0.8429 0.5571 0.3139 0.074 Uiso 1 1 calc R . . H10D H 0.9184 0.5713 0.3597 0.074 Uiso 1 1 calc R . . C11C C 0.9097(3) 0.4862(3) 0.2017(2) 0.0484(12) Uani 1 1 d . . . H11B H 0.9042 0.5454 0.2078 0.058 Uiso 1 1 calc R . . H11C H 0.9407 0.4773 0.1596 0.058 Uiso 1 1 calc R . . C12C C 0.8308(3) 0.4511(4) 0.1899(3) 0.0708(17) Uani 1 1 d . . . H12A H 0.8076 0.4763 0.1491 0.106 Uiso 1 1 calc R . . H12B H 0.7983 0.4616 0.2302 0.106 Uiso 1 1 calc R . . H12C H 0.8351 0.3927 0.1825 0.106 Uiso 1 1 calc R . . C13C C 0.9790(2) 0.3656(3) 0.2473(2) 0.0448(12) Uani 1 1 d . . . H13A H 0.9318 0.3326 0.2421 0.054 Uiso 1 1 calc R . . H13B H 1.0058 0.3656 0.2022 0.054 Uiso 1 1 calc R . . C14C C 1.0310(3) 0.3248(3) 0.3000(3) 0.0589(14) Uani 1 1 d . . . H14B H 1.0427 0.2697 0.2848 0.088 Uiso 1 1 calc R . . H14C H 1.0049 0.3230 0.3448 0.088 Uiso 1 1 calc R . . H14D H 1.0790 0.3556 0.3045 0.088 Uiso 1 1 calc R . . C15C C 1.0866(3) 0.5042(3) 0.2217(3) 0.0562(14) Uani 1 1 d . . . H15D H 1.1298 0.5390 0.2349 0.084 Uiso 1 1 calc R . . H15E H 1.0644 0.5235 0.1783 0.084 Uiso 1 1 calc R . . H15F H 1.1050 0.4486 0.2158 0.084 Uiso 1 1 calc R . . C16C C 1.0261(2) 0.5063(3) 0.2776(2) 0.0418(11) Uani 1 1 d . . . H16D H 1.0086 0.5628 0.2835 0.050 Uiso 1 1 calc R . . H16E H 1.0501 0.4890 0.3215 0.050 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 C1 0.030(2) 0.029(2) 0.043(3) 0.0029(18) 0.0026(18) -0.0012(18) C2 0.049(3) 0.032(3) 0.053(3) -0.009(2) 0.005(2) 0.001(2) C3 0.053(3) 0.034(3) 0.068(4) -0.007(2) -0.006(3) 0.016(2) C4 0.042(3) 0.045(3) 0.081(4) 0.013(3) -0.002(3) 0.008(2) C5 0.035(3) 0.041(3) 0.050(3) 0.002(2) -0.008(2) 0.004(2) C6 0.029(2) 0.032(3) 0.042(3) 0.007(2) 0.001(2) 0.0026(19) C7 0.032(2) 0.029(2) 0.036(3) 0.0023(19) -0.0050(19) -0.0011(18) C8 0.036(3) 0.033(3) 0.047(3) 0.002(2) -0.003(2) 0.004(2) C9 0.054(3) 0.053(3) 0.043(3) -0.010(2) -0.006(3) 0.004(3) C10 0.056(4) 0.067(4) 0.053(4) -0.005(3) -0.031(3) 0.007(3) C11 0.033(3) 0.054(3) 0.058(4) 0.000(3) -0.008(3) 0.000(2) C12 0.032(2) 0.043(3) 0.044(3) 0.005(2) -0.011(2) 0.002(2) C13 0.034(3) 0.041(3) 0.063(3) 0.012(2) -0.001(2) -0.006(2) C14 0.048(3) 0.061(4) 0.060(4) 0.008(3) 0.006(3) 0.006(3) C15 0.058(4) 0.109(6) 0.096(5) -0.013(4) 0.023(4) 0.010(3) C16 0.125(6) 0.161(8) 0.073(5) -0.051(5) 0.028(4) -0.070(6) C17 0.043(3) 0.035(3) 0.042(3) -0.005(2) -0.003(2) -0.004(2) C18 0.039(3) 0.044(3) 0.037(3) -0.006(2) -0.008(2) -0.002(2) C19 0.051(3) 0.057(4) 0.066(4) 0.011(3) -0.017(3) -0.006(3) C20 0.050(3) 0.052(3) 0.070(4) 0.011(3) -0.009(3) -0.011(2) C21 0.026(2) 0.026(2) 0.032(2) -0.0034(18) -0.0039(19) -0.0007(17) C22 0.039(3) 0.038(3) 0.038(3) 0.005(2) 0.002(2) -0.004(2) C23 0.044(3) 0.031(3) 0.060(3) 0.013(2) 0.001(3) 0.004(2) C24 0.025(2) 0.034(2) 0.064(3) -0.008(3) -0.001(3) 0.0095(16) C25 0.022(2) 0.036(3) 0.051(3) 0.000(2) 0.0031(19) -0.0015(18) C26 0.0253(18) 0.0274(19) 0.023(2) 0.000(2) -0.006(2) -0.0022(14) C27 0.031(2) 0.031(2) 0.033(3) -0.0044(19) 0.0030(19) -0.0007(18) C28 0.041(3) 0.040(3) 0.037(3) -0.002(2) 0.003(2) 0.000(2) C29 0.046(3) 0.043(3) 0.032(3) 0.008(2) 0.009(2) 0.009(2) C30 0.049(3) 0.051(3) 0.043(3) 0.005(2) 0.020(2) -0.007(2) C31 0.028(2) 0.050(3) 0.046(3) 0.001(2) 0.004(2) -0.001(2) C32 0.026(2) 0.036(3) 0.036(3) -0.005(2) 0.0036(19) 0.0018(18) C33 0.027(2) 0.047(3) 0.048(3) -0.007(2) 0.001(2) -0.001(2) C34 0.033(3) 0.058(3) 0.041(3) -0.007(2) -0.004(2) 0.003(2) C35 0.045(3) 0.086(4) 0.058(4) -0.011(3) -0.015(3) -0.003(3) C36 0.071(4) 0.066(4) 0.060(4) 0.007(3) -0.019(3) -0.008(3) C37 0.029(2) 0.032(2) 0.030(2) 0.0025(19) 0.0022(19) -0.0080(17) C38 0.033(2) 0.035(3) 0.034(2) 0.007(2) 0.008(2) -0.0023(19) C39 0.043(3) 0.059(4) 0.058(4) -0.018(3) -0.003(3) -0.003(2) C40 0.034(2) 0.049(3) 0.045(3) -0.008(2) 0.005(2) -0.002(2) Co1 0.0250(2) 0.0298(3) 0.0296(3) 0.0020(3) -0.0009(3) -0.0001(2) N1 0.0296(19) 0.029(2) 0.039(2) -0.0003(16) -0.0045(18) 0.0004(15) N2 0.034(2) 0.0268(19) 0.034(2) 0.0024(15) -0.0040(16) 0.0009(15) N3 0.032(2) 0.051(3) 0.046(2) 0.0063(19) 0.0006(17) 0.0017(17) N4 0.0272(17) 0.0256(18) 0.0268(19) 0.0000(14) 0.0012(15) -0.0017(13) N5 0.0279(19) 0.0284(19) 0.0309(19) 0.0011(14) 0.0011(14) 0.0002(14) N6 0.0255(19) 0.049(2) 0.041(3) 0.0050(17) 0.0010(16) -0.0028(15) O1 0.076(3) 0.063(2) 0.052(2) -0.0242(19) -0.0133(19) 0.0161(19) O2 0.036(2) 0.065(2) 0.076(3) 0.001(2) -0.0125(18) 0.0070(17) O3 0.0449(19) 0.049(2) 0.0390(19) 0.0131(15) 0.0046(15) 0.0026(15) O4 0.0267(17) 0.101(3) 0.060(3) 0.009(2) 0.0007(16) -0.0052(16) N1C 0.047(2) 0.036(2) 0.051(3) 0.0067(19) -0.002(2) 0.0012(18) C1C 0.106(5) 0.077(5) 0.071(4) 0.010(3) -0.013(4) -0.014(4) C2C 0.058(3) 0.073(4) 0.064(4) 0.021(3) 0.000(3) 0.005(3) C3C 0.106(5) 0.053(4) 0.099(5) 0.014(4) -0.023(4) -0.007(4) C4C 0.069(4) 0.072(4) 0.109(5) 0.015(4) 0.017(4) 0.019(3) C5C 0.095(5) 0.068(4) 0.081(5) 0.012(3) 0.006(4) -0.002(4) C6C 0.080(4) 0.094(5) 0.101(6) 0.024(4) 0.014(4) -0.012(4) C7C 0.089(4) 0.055(4) 0.098(5) -0.004(4) -0.021(4) -0.025(3) C8C 0.160(7) 0.068(5) 0.094(5) 0.034(4) -0.075(5) -0.044(4) N2C 0.036(2) 0.033(2) 0.035(2) -0.0030(16) -0.0006(16) -0.0052(15) C9C 0.040(3) 0.055(3) 0.042(3) -0.003(2) 0.013(2) -0.009(2) C10C 0.045(3) 0.052(3) 0.051(3) -0.013(2) 0.007(2) 0.005(2) C11C 0.048(3) 0.050(3) 0.047(3) -0.006(2) -0.007(2) 0.003(2) C12C 0.048(3) 0.085(4) 0.080(4) -0.026(3) -0.026(3) 0.004(3) C13C 0.039(3) 0.036(3) 0.060(3) -0.015(2) 0.013(2) -0.006(2) C14C 0.060(3) 0.050(3) 0.066(4) 0.008(3) 0.009(3) 0.013(3) C15C 0.046(3) 0.069(4) 0.054(3) -0.011(3) 0.007(3) -0.023(3) C16C 0.043(3) 0.043(3) 0.039(3) -0.006(2) -0.001(2) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.380(6) . ? C1 N1 1.440(5) . ? C1 C6 1.441(5) . ? C2 C3 1.397(6) . ? C2 H2A 0.9500 . ? C3 C4 1.402(7) . ? C3 H3A 0.9500 . ? C4 C5 1.367(6) . ? C4 H4A 0.9500 . ? C5 C6 1.428(6) . ? C5 H5A 0.9500 . ? C6 N2 1.389(5) . ? C7 C8 1.408(6) . ? C7 C12 1.416(6) . ? C7 N2 1.418(5) . ? C8 C9 1.383(6) . ? C8 H8A 0.9500 . ? C9 C10 1.387(6) . ? C9 H9A 0.9500 . ? C10 C11 1.395(7) . ? C10 H10A 0.9500 . ? C11 C12 1.390(6) . ? C11 H11A 0.9500 . ? C12 N3 1.440(6) . ? C13 O2 1.229(5) . ? C13 N3 1.364(6) . ? C13 C14 1.517(7) . ? C14 C16 1.489(8) . ? C14 C15 1.527(7) . ? C14 H14A 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O1 1.224(5) . ? C17 N1 1.359(5) . ? C17 C18 1.543(6) . ? C18 C20 1.516(6) . ? C18 C19 1.547(7) . ? C18 H18A 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.393(6) . ? C21 N4 1.426(5) . ? C21 C26 1.443(5) . ? C22 C23 1.385(6) . ? C22 H22A 0.9500 . ? C23 C24 1.379(6) . ? C23 H23A 0.9500 . ? C24 C25 1.400(5) . ? C24 H24A 0.9500 . ? C25 C26 1.409(5) . ? C25 H25A 0.9500 . ? C26 N5 1.399(4) . ? C27 C32 1.411(5) . ? C27 C28 1.412(6) . ? C27 N5 1.424(5) . ? C28 C29 1.374(6) . ? C28 H28A 0.9500 . ? C29 C30 1.399(6) . ? C29 H29A 0.9500 . ? C30 C31 1.391(6) . ? C30 H30A 0.9500 . ? C31 C32 1.396(6) . ? C31 H31A 0.9500 . ? C32 N6 1.431(5) . ? C33 O4 1.220(5) . ? C33 N6 1.377(5) . ? C33 C34 1.530(6) . ? C34 C35 1.530(6) . ? C34 C36 1.533(7) . ? C34 H34A 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 O3 1.253(4) . ? C37 N4 1.367(5) . ? C37 C38 1.529(5) . ? C38 C40 1.532(5) . ? C38 C39 1.546(6) . ? C38 H38A 1.0000 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? Co1 N5 1.996(3) . ? Co1 N2 1.996(3) . ? Co1 N1 2.029(3) . ? Co1 N4 2.035(3) . ? N3 H3B 0.8800 . ? N6 H6A 0.8800 . ? N1C C1C 1.489(7) . ? N1C C3C 1.512(6) . ? N1C C5C 1.526(7) . ? N1C C7C 1.549(6) . ? C1C C2C 1.476(7) . ? C1C H1C1 0.9900 . ? C1C H1C2 0.9900 . ? C2C H2CA 0.9800 . ? C2C H2CB 0.9800 . ? C2C H2CC 0.9800 . ? C3C C4C 1.500(8) . ? C3C H3CA 0.9900 . ? C3C H3CB 0.9900 . ? C4C H4CA 0.9800 . ? C4C H4CB 0.9800 . ? C4C H4CC 0.9800 . ? C5C C6C 1.488(8) . ? C5C H5CA 0.9900 . ? C5C H5CB 0.9900 . ? C6C H6CA 0.9800 . ? C6C H6CB 0.9800 . ? C6C H6CC 0.9800 . ? C7C C8C 1.467(8) . ? C7C H7CA 0.9900 . ? C7C H7CB 0.9900 . ? C8C H8CA 0.9800 . ? C8C H8CB 0.9800 . ? C8C H8CC 0.9800 . ? N2C C9C 1.520(5) . ? N2C C13C 1.530(5) . ? N2C C11C 1.543(5) . ? N2C C16C 1.545(5) . ? C9C C10C 1.535(6) . ? C9C H9CA 0.9900 . ? C9C H9CB 0.9900 . ? C10C H10B 0.9800 . ? C10C H10C 0.9800 . ? C10C H10D 0.9800 . ? C11C C12C 1.505(6) . ? C11C H11B 0.9900 . ? C11C H11C 0.9900 . ? C12C H12A 0.9800 . ? C12C H12B 0.9800 . ? C12C H12C 0.9800 . ? C13C C14C 1.522(6) . ? C13C H13A 0.9900 . ? C13C H13B 0.9900 . ? C14C H14B 0.9800 . ? C14C H14C 0.9800 . ? C14C H14D 0.9800 . ? C15C C16C 1.509(6) . ? C15C H15D 0.9800 . ? C15C H15E 0.9800 . ? C15C H15F 0.9800 . ? C16C H16D 0.9900 . ? C16C H16E 0.9900 . ? 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 C2 C1 N1 126.7(4) . . ? C2 C1 C6 119.7(4) . . ? N1 C1 C6 113.2(4) . . ? C1 C2 C3 122.2(4) . . ? C1 C2 H2A 118.9 . . ? C3 C2 H2A 118.9 . . ? C2 C3 C4 118.9(4) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C5 C4 C3 120.1(4) . . ? C5 C4 H4A 119.9 . . ? C3 C4 H4A 119.9 . . ? C4 C5 C6 122.5(4) . . ? C4 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? N2 C6 C5 125.2(4) . . ? N2 C6 C1 118.2(4) . . ? C5 C6 C1 116.5(4) . . ? C8 C7 C12 115.8(4) . . ? C8 C7 N2 120.7(4) . . ? C12 C7 N2 123.4(4) . . ? C9 C8 C7 123.0(4) . . ? C9 C8 H8A 118.5 . . ? C7 C8 H8A 118.5 . . ? C8 C9 C10 119.5(5) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C9 C10 C11 119.9(4) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C12 C11 C10 120.0(4) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C11 C12 C7 121.8(4) . . ? C11 C12 N3 120.2(4) . . ? C7 C12 N3 117.9(4) . . ? O2 C13 N3 122.5(5) . . ? O2 C13 C14 122.0(5) . . ? N3 C13 C14 115.5(4) . . ? C16 C14 C13 111.8(5) . . ? C16 C14 C15 111.9(5) . . ? C13 C14 C15 111.7(5) . . ? C16 C14 H14A 107.1 . . ? C13 C14 H14A 107.1 . . ? C15 C14 H14A 107.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 N1 127.3(4) . . ? O1 C17 C18 117.5(4) . . ? N1 C17 C18 115.1(4) . . ? C20 C18 C17 109.8(4) . . ? C20 C18 C19 111.9(4) . . ? C17 C18 C19 110.0(4) . . ? C20 C18 H18A 108.3 . . ? C17 C18 H18A 108.3 . . ? C19 C18 H18A 108.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N4 126.2(4) . . ? C22 C21 C26 119.2(3) . . ? N4 C21 C26 114.4(3) . . ? C23 C22 C21 121.1(4) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C24 C23 C22 120.8(4) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C25 119.9(4) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 C26 120.9(4) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? N5 C26 C25 125.6(4) . . ? N5 C26 C21 116.3(3) . . ? C25 C26 C21 118.1(3) . . ? C32 C27 C28 117.2(4) . . ? C32 C27 N5 122.7(4) . . ? C28 C27 N5 119.8(4) . . ? C29 C28 C27 122.3(4) . . ? C29 C28 H28A 118.8 . . ? C27 C28 H28A 118.8 . . ? C28 C29 C30 119.5(4) . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 120.3 . . ? C31 C30 C29 119.9(4) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.2(4) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C31 C32 C27 120.7(4) . . ? C31 C32 N6 122.1(4) . . ? C27 C32 N6 117.2(4) . . ? O4 C33 N6 122.7(4) . . ? O4 C33 C34 122.2(4) . . ? N6 C33 C34 115.1(4) . . ? C35 C34 C33 110.1(4) . . ? C35 C34 C36 110.6(4) . . ? C33 C34 C36 111.2(4) . . ? C35 C34 H34A 108.3 . . ? C33 C34 H34A 108.3 . . ? C36 C34 H34A 108.3 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O3 C37 N4 126.0(4) . . ? O3 C37 C38 117.7(4) . . ? N4 C37 C38 116.3(3) . . ? C37 C38 C40 108.1(3) . . ? C37 C38 C39 111.4(4) . . ? C40 C38 C39 109.9(4) . . ? C37 C38 H38A 109.1 . . ? C40 C38 H38A 109.1 . . ? C39 C38 H38A 109.1 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N5 Co1 N2 132.03(13) . . ? N5 Co1 N1 123.50(13) . . ? N2 Co1 N1 83.05(13) . . ? N5 Co1 N4 82.33(13) . . ? N2 Co1 N4 123.38(13) . . ? N1 Co1 N4 117.14(13) . . ? C17 N1 C1 120.5(3) . . ? C17 N1 Co1 125.6(3) . . ? C1 N1 Co1 112.5(2) . . ? C6 N2 C7 118.2(3) . . ? C6 N2 Co1 112.8(3) . . ? C7 N2 Co1 129.0(3) . . ? C13 N3 C12 126.8(4) . . ? C13 N3 H3B 116.6 . . ? C12 N3 H3B 116.6 . . ? C37 N4 C21 121.2(3) . . ? C37 N4 Co1 123.8(3) . . ? C21 N4 Co1 112.6(2) . . ? C26 N5 C27 119.2(3) . . ? C26 N5 Co1 113.8(2) . . ? C27 N5 Co1 127.0(3) . . ? C33 N6 C32 129.0(4) . . ? C33 N6 H6A 115.5 . . ? C32 N6 H6A 115.5 . . ? C1C N1C C3C 111.5(4) . . ? C1C N1C C5C 110.9(4) . . ? C3C N1C C5C 108.6(4) . . ? C1C N1C C7C 107.2(4) . . ? C3C N1C C7C 111.5(4) . . ? C5C N1C C7C 107.0(4) . . ? C2C C1C N1C 122.1(5) . . ? C2C C1C H1C1 106.8 . . ? N1C C1C H1C1 106.8 . . ? C2C C1C H1C2 106.8 . . ? N1C C1C H1C2 106.8 . . ? H1C1 C1C H1C2 106.7 . . ? C1C C2C H2CA 109.5 . . ? C1C C2C H2CB 109.5 . . ? H2CA C2C H2CB 109.5 . . ? C1C C2C H2CC 109.5 . . ? H2CA C2C H2CC 109.5 . . ? H2CB C2C H2CC 109.5 . . ? C4C C3C N1C 117.4(5) . . ? C4C C3C H3CA 107.9 . . ? N1C C3C H3CA 107.9 . . ? C4C C3C H3CB 107.9 . . ? N1C C3C H3CB 107.9 . . ? H3CA C3C H3CB 107.2 . . ? C3C C4C H4CA 109.5 . . ? C3C C4C H4CB 109.5 . . ? H4CA C4C H4CB 109.5 . . ? C3C C4C H4CC 109.5 . . ? H4CA C4C H4CC 109.5 . . ? H4CB C4C H4CC 109.5 . . ? C6C C5C N1C 116.2(5) . . ? C6C C5C H5CA 108.2 . . ? N1C C5C H5CA 108.2 . . ? C6C C5C H5CB 108.2 . . ? N1C C5C H5CB 108.2 . . ? H5CA C5C H5CB 107.4 . . ? C5C C6C H6CA 109.5 . . ? C5C C6C H6CB 109.5 . . ? H6CA C6C H6CB 109.5 . . ? C5C C6C H6CC 109.5 . . ? H6CA C6C H6CC 109.5 . . ? H6CB C6C H6CC 109.5 . . ? C8C C7C N1C 116.6(5) . . ? C8C C7C H7CA 108.1 . . ? N1C C7C H7CA 108.1 . . ? C8C C7C H7CB 108.1 . . ? N1C C7C H7CB 108.1 . . ? H7CA C7C H7CB 107.3 . . ? C7C C8C H8CA 109.5 . . ? C7C C8C H8CB 109.5 . . ? H8CA C8C H8CB 109.5 . . ? C7C C8C H8CC 109.5 . . ? H8CA C8C H8CC 109.5 . . ? H8CB C8C H8CC 109.5 . . ? C9C N2C C13C 108.5(3) . . ? C9C N2C C11C 111.3(3) . . ? C13C N2C C11C 108.3(3) . . ? C9C N2C C16C 108.2(3) . . ? C13C N2C C16C 111.0(3) . . ? C11C N2C C16C 109.5(3) . . ? N2C C9C C10C 114.6(4) . . ? N2C C9C H9CA 108.6 . . ? C10C C9C H9CA 108.6 . . ? N2C C9C H9CB 108.6 . . ? C10C C9C H9CB 108.6 . . ? H9CA C9C H9CB 107.6 . . ? C9C C10C H10B 109.5 . . ? C9C C10C H10C 109.5 . . ? H10B C10C H10C 109.5 . . ? C9C C10C H10D 109.5 . . ? H10B C10C H10D 109.5 . . ? H10C C10C H10D 109.5 . . ? C12C C11C N2C 116.4(4) . . ? C12C C11C H11B 108.2 . . ? N2C C11C H11B 108.2 . . ? C12C C11C H11C 108.2 . . ? N2C C11C H11C 108.2 . . ? H11B C11C H11C 107.3 . . ? C11C C12C H12A 109.5 . . ? C11C C12C H12B 109.5 . . ? H12A C12C H12B 109.5 . . ? C11C C12C H12C 109.5 . . ? H12A C12C H12C 109.5 . . ? H12B C12C H12C 109.5 . . ? C14C C13C N2C 115.9(4) . . ? C14C C13C H13A 108.3 . . ? N2C C13C H13A 108.3 . . ? C14C C13C H13B 108.3 . . ? N2C C13C H13B 108.3 . . ? H13A C13C H13B 107.4 . . ? C13C C14C H14B 109.5 . . ? C13C C14C H14C 109.5 . . ? H14B C14C H14C 109.5 . . ? C13C C14C H14D 109.5 . . ? H14B C14C H14D 109.5 . . ? H14C C14C H14D 109.5 . . ? C16C C15C H15D 109.5 . . ? C16C C15C H15E 109.5 . . ? H15D C15C H15E 109.5 . . ? C16C C15C H15F 109.5 . . ? H15D C15C H15F 109.5 . . ? H15E C15C H15F 109.5 . . ? C15C C16C N2C 114.9(3) . . ? C15C C16C H16D 108.5 . . ? N2C C16C H16D 108.5 . . ? C15C C16C H16E 108.5 . . ? N2C C16C H16E 108.5 . . ? H16D C16C H16E 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 172.4(4) . . . . ? C6 C1 C2 C3 0.5(6) . . . . ? C1 C2 C3 C4 -0.7(7) . . . . ? C2 C3 C4 C5 -0.2(7) . . . . ? C3 C4 C5 C6 1.5(7) . . . . ? C4 C5 C6 N2 -177.9(4) . . . . ? C4 C5 C6 C1 -1.7(6) . . . . ? C2 C1 C6 N2 177.2(4) . . . . ? N1 C1 C6 N2 4.3(5) . . . . ? C2 C1 C6 C5 0.7(6) . . . . ? N1 C1 C6 C5 -172.3(4) . . . . ? C12 C7 C8 C9 2.3(6) . . . . ? N2 C7 C8 C9 -179.7(4) . . . . ? C7 C8 C9 C10 -1.1(7) . . . . ? C8 C9 C10 C11 -1.0(8) . . . . ? C9 C10 C11 C12 1.7(7) . . . . ? C10 C11 C12 C7 -0.4(7) . . . . ? C10 C11 C12 N3 -177.8(4) . . . . ? C8 C7 C12 C11 -1.5(6) . . . . ? N2 C7 C12 C11 -179.5(4) . . . . ? C8 C7 C12 N3 175.9(4) . . . . ? N2 C7 C12 N3 -2.1(6) . . . . ? O2 C13 C14 C16 -103.7(6) . . . . ? N3 C13 C14 C16 75.8(7) . . . . ? O2 C13 C14 C15 22.5(7) . . . . ? N3 C13 C14 C15 -158.1(4) . . . . ? O1 C17 C18 C20 -48.0(6) . . . . ? N1 C17 C18 C20 130.4(4) . . . . ? O1 C17 C18 C19 75.7(5) . . . . ? N1 C17 C18 C19 -106.0(5) . . . . ? N4 C21 C22 C23 174.4(4) . . . . ? C26 C21 C22 C23 -0.2(6) . . . . ? C21 C22 C23 C24 1.1(7) . . . . ? C22 C23 C24 C25 -1.7(7) . . . . ? C23 C24 C25 C26 1.4(6) . . . . ? C24 C25 C26 N5 -178.4(4) . . . . ? C24 C25 C26 C21 -0.5(6) . . . . ? C22 C21 C26 N5 178.0(3) . . . . ? N4 C21 C26 N5 2.8(5) . . . . ? C22 C21 C26 C25 -0.1(5) . . . . ? N4 C21 C26 C25 -175.3(3) . . . . ? C32 C27 C28 C29 -2.1(6) . . . . ? N5 C27 C28 C29 171.5(4) . . . . ? C27 C28 C29 C30 -1.3(7) . . . . ? C28 C29 C30 C31 3.3(7) . . . . ? C29 C30 C31 C32 -1.8(7) . . . . ? C30 C31 C32 C27 -1.8(6) . . . . ? C30 C31 C32 N6 178.9(4) . . . . ? C28 C27 C32 C31 3.7(6) . . . . ? N5 C27 C32 C31 -169.8(4) . . . . ? C28 C27 C32 N6 -177.0(4) . . . . ? N5 C27 C32 N6 9.6(6) . . . . ? O4 C33 C34 C35 20.4(6) . . . . ? N6 C33 C34 C35 -162.4(4) . . . . ? O4 C33 C34 C36 -102.6(5) . . . . ? N6 C33 C34 C36 74.6(5) . . . . ? O3 C37 C38 C40 -65.6(5) . . . . ? N4 C37 C38 C40 111.9(4) . . . . ? O3 C37 C38 C39 55.3(5) . . . . ? N4 C37 C38 C39 -127.3(4) . . . . ? O1 C17 N1 C1 13.3(7) . . . . ? C18 C17 N1 C1 -164.9(3) . . . . ? O1 C17 N1 Co1 -152.2(4) . . . . ? C18 C17 N1 Co1 29.6(5) . . . . ? C2 C1 N1 C17 15.6(6) . . . . ? C6 C1 N1 C17 -172.0(4) . . . . ? C2 C1 N1 Co1 -177.1(3) . . . . ? C6 C1 N1 Co1 -4.8(4) . . . . ? N5 Co1 N1 C17 -53.6(4) . . . . ? N2 Co1 N1 C17 169.7(3) . . . . ? N4 Co1 N1 C17 45.6(4) . . . . ? N5 Co1 N1 C1 139.9(2) . . . . ? N2 Co1 N1 C1 3.2(3) . . . . ? N4 Co1 N1 C1 -120.9(3) . . . . ? C5 C6 N2 C7 -6.0(6) . . . . ? C1 C6 N2 C7 177.7(3) . . . . ? C5 C6 N2 Co1 174.6(3) . . . . ? C1 C6 N2 Co1 -1.6(4) . . . . ? C8 C7 N2 C6 118.3(4) . . . . ? C12 C7 N2 C6 -63.8(5) . . . . ? C8 C7 N2 Co1 -62.4(5) . . . . ? C12 C7 N2 Co1 115.4(4) . . . . ? N5 Co1 N2 C6 -130.6(3) . . . . ? N1 Co1 N2 C6 -0.9(3) . . . . ? N4 Co1 N2 C6 117.1(3) . . . . ? N5 Co1 N2 C7 50.1(4) . . . . ? N1 Co1 N2 C7 179.8(3) . . . . ? N4 Co1 N2 C7 -62.1(4) . . . . ? O2 C13 N3 C12 3.1(7) . . . . ? C14 C13 N3 C12 -176.4(4) . . . . ? C11 C12 N3 C13 -41.9(6) . . . . ? C7 C12 N3 C13 140.6(4) . . . . ? O3 C37 N4 C21 7.6(6) . . . . ? C38 C37 N4 C21 -169.6(3) . . . . ? O3 C37 N4 Co1 -153.3(3) . . . . ? C38 C37 N4 Co1 29.6(4) . . . . ? C22 C21 N4 C37 25.3(6) . . . . ? C26 C21 N4 C37 -159.9(3) . . . . ? C22 C21 N4 Co1 -171.9(3) . . . . ? C26 C21 N4 Co1 2.9(4) . . . . ? N5 Co1 N4 C37 157.0(3) . . . . ? N2 Co1 N4 C37 -66.9(3) . . . . ? N1 Co1 N4 C37 33.2(3) . . . . ? N5 Co1 N4 C21 -5.3(2) . . . . ? N2 Co1 N4 C21 130.8(2) . . . . ? N1 Co1 N4 C21 -129.1(2) . . . . ? C25 C26 N5 C27 -6.4(6) . . . . ? C21 C26 N5 C27 175.7(3) . . . . ? C25 C26 N5 Co1 170.7(3) . . . . ? C21 C26 N5 Co1 -7.2(4) . . . . ? C32 C27 N5 C26 -72.7(5) . . . . ? C28 C27 N5 C26 114.0(4) . . . . ? C32 C27 N5 Co1 110.7(4) . . . . ? C28 C27 N5 Co1 -62.6(5) . . . . ? N2 Co1 N5 C26 -121.9(3) . . . . ? N1 Co1 N5 C26 124.4(3) . . . . ? N4 Co1 N5 C26 6.8(2) . . . . ? N2 Co1 N5 C27 54.8(4) . . . . ? N1 Co1 N5 C27 -58.8(3) . . . . ? N4 Co1 N5 C27 -176.4(3) . . . . ? O4 C33 N6 C32 0.8(7) . . . . ? C34 C33 N6 C32 -176.4(4) . . . . ? C31 C32 N6 C33 -13.6(7) . . . . ? C27 C32 N6 C33 167.0(4) . . . . ? C3C N1C C1C C2C -175.2(5) . . . . ? C5C N1C C1C C2C -54.0(7) . . . . ? C7C N1C C1C C2C 62.5(7) . . . . ? C1C N1C C3C C4C -60.4(7) . . . . ? C5C N1C C3C C4C 177.0(5) . . . . ? C7C N1C C3C C4C 59.4(7) . . . . ? C1C N1C C5C C6C -55.5(6) . . . . ? C3C N1C C5C C6C 67.4(6) . . . . ? C7C N1C C5C C6C -172.2(5) . . . . ? C1C N1C C7C C8C 175.1(6) . . . . ? C3C N1C C7C C8C 52.8(7) . . . . ? C5C N1C C7C C8C -65.8(7) . . . . ? C13C N2C C9C C10C -178.2(4) . . . . ? C11C N2C C9C C10C -59.1(5) . . . . ? C16C N2C C9C C10C 61.3(5) . . . . ? C9C N2C C11C C12C -48.8(5) . . . . ? C13C N2C C11C C12C 70.4(5) . . . . ? C16C N2C C11C C12C -168.4(4) . . . . ? C9C N2C C13C C14C -64.6(5) . . . . ? C11C N2C C13C C14C 174.4(4) . . . . ? C16C N2C C13C C14C 54.2(5) . . . . ? C9C N2C C16C C15C 171.7(4) . . . . ? C13C N2C C16C C15C 52.7(5) . . . . ? C11C N2C C16C C15C -66.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 30.63 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.826 _refine_diff_density_min -0.553 _refine_diff_density_rms 0.072 #**************************************************** #Cora MacBeth, Ph.D. #Assistant Professor of Chemistry #Emory University #Atlanta, GA 30322 #(404) 727-7033 #cora.macbeth@emory.edu #http://www.chemistry.emory.edu/faculty/macbeth/