# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Gade, Lutz' _publ_contact_author_name 'Gade, Lutz' _publ_contact_author_email lutz.gade@uni-hd.de _publ_section_title ; Bis(2-pyridylimino)isoindolato Iron(II) and Cobalt(II) Complexes: Structural Chemistry and Paramagnetic NMR Spectroscopy ; # Attachment '- ga_mkr12-ga_mkr20-ga_ds12-ga_mkr14-ga_ds17.cif' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 821499' #TrackingRef '- ga_mkr12-ga_mkr20-ga_ds12-ga_mkr14-ga_ds17.cif' _audit_creation_method SHELXL-97 _audit_block_code ga_mkr12 _audit_block_refno 901 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H25 N5' _chemical_melting_point ? _exptl_crystal_description irregular _exptl_crystal_colour yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 407.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration . loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.864(5) _cell_length_b 15.282(6) _cell_length_c 12.121(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.420(10) _cell_angle_gamma 90.00 _cell_volume 2045.9(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8005 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 32.05 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8196 _exptl_absorpt_correction_T_max 0.8623 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) SADABS (Sheldrick & Bruker AXS, 2004-2008) ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Smart 1000' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean 8.19 _diffrn_reflns_number 51391 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 31.50 _reflns_number_total 6741 _reflns_number_gt 5732 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-5.631 (Bruker AXS, 2003)' _computing_cell_refinement ; SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors of the unit cell constants from Monte Carlo simulations. ; _computing_data_reduction 'SAINT (Bruker AXS, 1997-2008); SADABS (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0741P)^2^+0.4956P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6741 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1130 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 N1 N 0.42292(7) 0.13322(5) 0.05598(6) 0.01552(14) Uani 1 1 d . . . H1 H 0.4869(14) 0.1265(10) 0.1204(14) 0.034(4) Uiso 1 1 d . . . N2 N 0.50852(7) 0.09275(5) -0.09101(7) 0.01716(15) Uani 1 1 d . . . N3 N 0.66748(7) 0.12008(5) 0.09664(7) 0.01675(15) Uani 1 1 d . . . N4 N 0.27184(7) 0.17079(5) 0.13999(6) 0.01646(14) Uani 1 1 d . . . N5 N 0.45215(6) 0.11733(5) 0.28776(6) 0.01530(14) Uani 1 1 d . . . C1 C 0.42223(8) 0.11416(5) -0.05621(7) 0.01536(15) Uani 1 1 d . . . C2 C 0.29541(8) 0.12343(6) -0.13735(7) 0.01670(16) Uani 1 1 d . . . C3 C 0.24376(9) 0.11232(6) -0.25929(8) 0.02153(18) Uani 1 1 d . . . H3 H 0.2938(13) 0.0935(9) -0.3052(12) 0.026 Uiso 1 1 d . . . C4 C 0.12014(9) 0.12857(7) -0.31346(8) 0.0246(2) Uani 1 1 d . . . H4 H 0.0798(13) 0.1203(10) -0.4007(13) 0.030 Uiso 1 1 d . . . C5 C 0.05133(9) 0.15512(7) -0.24731(9) 0.02400(19) Uani 1 1 d . . . H5 H -0.0361(13) 0.1665(10) -0.2869(13) 0.029 Uiso 1 1 d . . . C6 C 0.10363(8) 0.16533(6) -0.12472(8) 0.02024(17) Uani 1 1 d . . . H6 H 0.0563(12) 0.1825(9) -0.0793(12) 0.024 Uiso 1 1 d . . . C7 C 0.22689(8) 0.14899(6) -0.07110(8) 0.01639(16) Uani 1 1 d . . . C8 C 0.30811(7) 0.15249(5) 0.05436(7) 0.01517(15) Uani 1 1 d . . . C9 C 0.63013(8) 0.08970(6) -0.01508(7) 0.01554(15) Uani 1 1 d . . . C10 C 0.71095(8) 0.05565(6) -0.06405(8) 0.01880(17) Uani 1 1 d . . . H10 H 0.6790(12) 0.0318(9) -0.1452(12) 0.023 Uiso 1 1 d . . . C11 C 0.83244(9) 0.05321(7) 0.00475(8) 0.02101(18) Uani 1 1 d . . . H11 H 0.8903(12) 0.0289(9) -0.0281(12) 0.025 Uiso 1 1 d . . . C12 C 0.87389(8) 0.08478(6) 0.12092(8) 0.01800(16) Uani 1 1 d . . . C13 C 1.00718(9) 0.08257(7) 0.19716(9) 0.02367(19) Uani 1 1 d . . . H13A H 1.0498(13) 0.1237(10) 0.1636(13) 0.028 Uiso 1 1 d . . . H13B H 1.0386(12) 0.0233(10) 0.1895(12) 0.028 Uiso 1 1 d . . . C14 C 1.03275(8) 0.10353(7) 0.32712(9) 0.02294(18) Uani 1 1 d . . . H14A H 1.1199(13) 0.1143(9) 0.3697(13) 0.028 Uiso 1 1 d . . . H14B H 1.0128(12) 0.0519(10) 0.3674(13) 0.028 Uiso 1 1 d . . . C15 C 0.95650(9) 0.18145(6) 0.33663(9) 0.02190(18) Uani 1 1 d . . . H15A H 0.9714(12) 0.2322(10) 0.2927(12) 0.026 Uiso 1 1 d . . . H15B H 0.9782(12) 0.2025(10) 0.4222(12) 0.026 Uiso 1 1 d . . . C16 C 0.82353(8) 0.15503(7) 0.28590(8) 0.02134(18) Uani 1 1 d . . . H16A H 0.8118(13) 0.1074(9) 0.3375(12) 0.026 Uiso 1 1 d . . . H16B H 0.7710(13) 0.2021(9) 0.2843(12) 0.026 Uiso 1 1 d . . . C17 C 0.78689(8) 0.11849(6) 0.16225(8) 0.01624(16) Uani 1 1 d . . . C18 C 0.35008(7) 0.16450(6) 0.25874(7) 0.01524(15) Uani 1 1 d . . . C19 C 0.31565(8) 0.20543(6) 0.34509(8) 0.01760(16) Uani 1 1 d . . . H19 H 0.2422(12) 0.2392(9) 0.3223(11) 0.021 Uiso 1 1 d . . . C20 C 0.39100(8) 0.19799(6) 0.46294(8) 0.01786(16) Uani 1 1 d . . . H20 H 0.3697(12) 0.2289(9) 0.5248(12) 0.021 Uiso 1 1 d . . . C21 C 0.49780(8) 0.14921(6) 0.49454(7) 0.01550(15) Uani 1 1 d . . . C22 C 0.58555(8) 0.14591(7) 0.62149(8) 0.01907(17) Uani 1 1 d . . . H22A H 0.5415(12) 0.1300(9) 0.6757(12) 0.023 Uiso 1 1 d . . . H22B H 0.6144(12) 0.2063(9) 0.6429(12) 0.023 Uiso 1 1 d . . . C23 C 0.69428(8) 0.08536(7) 0.64222(8) 0.02006(17) Uani 1 1 d . . . H23A H 0.7607(12) 0.1044(9) 0.7172(12) 0.024 Uiso 1 1 d . . . H23B H 0.6733(12) 0.0236(9) 0.6547(12) 0.024 Uiso 1 1 d . . . C24 C 0.73714(8) 0.08721(6) 0.53790(8) 0.01895(17) Uani 1 1 d . . . H24A H 0.8109(12) 0.0502(9) 0.5538(12) 0.023 Uiso 1 1 d . . . H24B H 0.7606(12) 0.1480(9) 0.5247(12) 0.023 Uiso 1 1 d . . . C25 C 0.63493(8) 0.05431(6) 0.42749(8) 0.01697(16) Uani 1 1 d . . . H25A H 0.6559(11) 0.0540(9) 0.3551(12) 0.020 Uiso 1 1 d . . . H25B H 0.6165(11) -0.0076(9) 0.4392(11) 0.020 Uiso 1 1 d . . . C26 C 0.52301(7) 0.10915(6) 0.40251(7) 0.01447(15) 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 N1 0.0141(3) 0.0206(3) 0.0110(3) -0.0003(2) 0.0036(2) 0.0015(2) N2 0.0191(3) 0.0182(3) 0.0140(3) 0.0009(3) 0.0058(3) 0.0027(3) N3 0.0169(3) 0.0186(3) 0.0149(3) -0.0011(3) 0.0059(3) 0.0015(3) N4 0.0152(3) 0.0200(3) 0.0127(3) -0.0009(3) 0.0033(2) 0.0015(3) N5 0.0146(3) 0.0177(3) 0.0126(3) -0.0003(2) 0.0038(2) -0.0001(2) C1 0.0183(4) 0.0151(3) 0.0117(3) 0.0004(3) 0.0043(3) 0.0014(3) C2 0.0187(4) 0.0163(4) 0.0125(3) -0.0001(3) 0.0027(3) 0.0020(3) C3 0.0254(4) 0.0227(4) 0.0130(4) -0.0014(3) 0.0029(3) 0.0037(3) C4 0.0267(5) 0.0263(5) 0.0137(4) -0.0020(3) -0.0010(3) 0.0038(4) C5 0.0209(4) 0.0245(4) 0.0187(4) -0.0020(3) -0.0021(3) 0.0037(3) C6 0.0170(4) 0.0219(4) 0.0178(4) -0.0015(3) 0.0016(3) 0.0029(3) C7 0.0167(4) 0.0167(4) 0.0128(3) -0.0002(3) 0.0020(3) 0.0016(3) C8 0.0146(3) 0.0160(4) 0.0132(3) -0.0003(3) 0.0031(3) 0.0013(3) C9 0.0183(4) 0.0153(3) 0.0139(3) 0.0012(3) 0.0069(3) 0.0014(3) C10 0.0217(4) 0.0211(4) 0.0166(4) -0.0002(3) 0.0106(3) 0.0014(3) C11 0.0211(4) 0.0246(4) 0.0217(4) -0.0011(3) 0.0130(3) 0.0019(3) C12 0.0171(4) 0.0184(4) 0.0207(4) 0.0002(3) 0.0095(3) 0.0000(3) C13 0.0162(4) 0.0290(5) 0.0274(5) -0.0027(4) 0.0098(3) -0.0006(3) C14 0.0162(4) 0.0252(4) 0.0260(4) 0.0000(4) 0.0060(3) 0.0002(3) C15 0.0203(4) 0.0209(4) 0.0219(4) -0.0013(3) 0.0048(3) -0.0014(3) C16 0.0178(4) 0.0270(5) 0.0186(4) -0.0053(3) 0.0061(3) 0.0014(3) C17 0.0169(4) 0.0159(4) 0.0170(4) -0.0003(3) 0.0075(3) 0.0002(3) C18 0.0145(3) 0.0178(4) 0.0129(3) -0.0003(3) 0.0044(3) -0.0003(3) C19 0.0158(3) 0.0215(4) 0.0156(4) -0.0011(3) 0.0058(3) 0.0017(3) C20 0.0178(4) 0.0218(4) 0.0148(4) -0.0027(3) 0.0069(3) -0.0009(3) C21 0.0156(3) 0.0182(4) 0.0123(3) -0.0007(3) 0.0047(3) -0.0031(3) C22 0.0181(4) 0.0259(4) 0.0116(3) -0.0014(3) 0.0035(3) -0.0020(3) C23 0.0188(4) 0.0262(4) 0.0133(3) 0.0027(3) 0.0036(3) -0.0012(3) C24 0.0152(4) 0.0247(4) 0.0150(4) 0.0023(3) 0.0032(3) 0.0002(3) C25 0.0161(3) 0.0190(4) 0.0146(4) 0.0008(3) 0.0041(3) 0.0016(3) C26 0.0145(3) 0.0157(3) 0.0127(3) 0.0002(3) 0.0043(3) -0.0013(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 N1 C8 1.3867(12) . ? N1 C1 1.3877(12) . ? N1 H1 0.874(16) . ? N2 C1 1.2840(12) . ? N2 C9 1.4004(12) . ? N3 C9 1.3444(12) . ? N3 C17 1.3481(12) . ? N4 C8 1.2912(12) . ? N4 C18 1.4024(12) . ? N5 C18 1.3412(12) . ? N5 C26 1.3427(11) . ? C1 C2 1.4732(13) . ? C2 C3 1.3883(13) . ? C2 C7 1.3910(13) . ? C3 C4 1.3930(15) . ? C3 H3 0.993(14) . ? C4 C5 1.3973(15) . ? C4 H4 0.997(15) . ? C5 C6 1.3943(14) . ? C5 H5 0.986(14) . ? C6 C7 1.3889(13) . ? C6 H6 0.956(14) . ? C7 C8 1.4744(12) . ? C9 C10 1.3994(12) . ? C10 C11 1.3771(14) . ? C10 H10 0.986(13) . ? C11 C12 1.3971(14) . ? C11 H11 0.983(14) . ? C12 C17 1.3998(12) . ? C12 C13 1.5127(14) . ? C13 C14 1.5255(16) . ? C13 H13A 0.984(15) . ? C13 H13B 0.997(15) . ? C14 C15 1.5250(15) . ? C14 H14A 0.986(14) . ? C14 H14B 1.001(15) . ? C15 C16 1.5236(15) . ? C15 H15A 0.993(14) . ? C15 H15B 1.025(14) . ? C16 C17 1.5070(14) . ? C16 H16A 1.002(15) . ? C16 H16B 0.947(14) . ? C18 C19 1.4021(12) . ? C19 C20 1.3856(13) . ? C19 H19 0.962(13) . ? C20 C21 1.3978(13) . ? C20 H20 0.994(13) . ? C21 C26 1.3972(12) . ? C21 C22 1.5113(13) . ? C22 C23 1.5319(14) . ? C22 H22A 1.008(14) . ? C22 H22B 0.985(14) . ? C23 C24 1.5258(14) . ? C23 H23A 1.005(14) . ? C23 H23B 1.001(14) . ? C24 C25 1.5261(13) . ? C24 H24A 1.000(13) . ? C24 H24B 0.999(14) . ? C25 C26 1.5045(13) . ? C25 H25A 0.995(13) . ? C25 H25B 0.993(14) . ? 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 C8 N1 C1 112.11(7) . . ? C8 N1 H1 124.5(10) . . ? C1 N1 H1 122.9(10) . . ? C1 N2 C9 123.12(8) . . ? C9 N3 C17 118.47(8) . . ? C8 N4 C18 121.34(8) . . ? C18 N5 C26 119.05(7) . . ? N2 C1 N1 130.94(8) . . ? N2 C1 C2 123.20(8) . . ? N1 C1 C2 105.85(7) . . ? C3 C2 C7 121.68(9) . . ? C3 C2 C1 130.18(8) . . ? C7 C2 C1 108.13(8) . . ? C2 C3 C4 117.35(9) . . ? C2 C3 H3 120.7(8) . . ? C4 C3 H3 122.0(8) . . ? C3 C4 C5 121.10(9) . . ? C3 C4 H4 119.5(8) . . ? C5 C4 H4 119.4(8) . . ? C6 C5 C4 121.21(9) . . ? C6 C5 H5 118.6(9) . . ? C4 C5 H5 120.2(9) . . ? C7 C6 C5 117.47(9) . . ? C7 C6 H6 121.3(8) . . ? C5 C6 H6 121.2(8) . . ? C6 C7 C2 121.18(9) . . ? C6 C7 C8 130.99(8) . . ? C2 C7 C8 107.82(8) . . ? N4 C8 N1 130.45(8) . . ? N4 C8 C7 123.57(8) . . ? N1 C8 C7 105.99(7) . . ? N3 C9 C10 122.07(8) . . ? N3 C9 N2 122.14(8) . . ? C10 C9 N2 115.77(8) . . ? C11 C10 C9 118.75(9) . . ? C11 C10 H10 122.0(8) . . ? C9 C10 H10 119.1(8) . . ? C10 C11 C12 120.42(8) . . ? C10 C11 H11 119.7(8) . . ? C12 C11 H11 119.8(8) . . ? C11 C12 C17 116.98(8) . . ? C11 C12 C13 120.84(8) . . ? C17 C12 C13 122.18(9) . . ? C12 C13 C14 113.30(8) . . ? C12 C13 H13A 108.3(8) . . ? C14 C13 H13A 110.7(9) . . ? C12 C13 H13B 107.8(8) . . ? C14 C13 H13B 110.3(8) . . ? H13A C13 H13B 106.1(12) . . ? C15 C14 C13 110.02(8) . . ? C15 C14 H14A 111.6(8) . . ? C13 C14 H14A 110.5(8) . . ? C15 C14 H14B 109.0(8) . . ? C13 C14 H14B 110.2(8) . . ? H14A C14 H14B 105.4(11) . . ? C16 C15 C14 108.54(8) . . ? C16 C15 H15A 110.6(8) . . ? C14 C15 H15A 110.0(8) . . ? C16 C15 H15B 109.4(8) . . ? C14 C15 H15B 112.6(8) . . ? H15A C15 H15B 105.7(11) . . ? C17 C16 C15 112.32(8) . . ? C17 C16 H16A 107.2(8) . . ? C15 C16 H16A 107.5(8) . . ? C17 C16 H16B 108.2(8) . . ? C15 C16 H16B 112.6(9) . . ? H16A C16 H16B 108.9(12) . . ? N3 C17 C12 123.29(9) . . ? N3 C17 C16 116.06(8) . . ? C12 C17 C16 120.64(8) . . ? N5 C18 C19 121.69(8) . . ? N5 C18 N4 120.13(8) . . ? C19 C18 N4 118.13(8) . . ? C20 C19 C18 118.61(8) . . ? C20 C19 H19 121.0(8) . . ? C18 C19 H19 120.3(8) . . ? C19 C20 C21 120.35(8) . . ? C19 C20 H20 119.5(8) . . ? C21 C20 H20 120.1(8) . . ? C26 C21 C20 116.86(8) . . ? C26 C21 C22 121.98(8) . . ? C20 C21 C22 121.01(8) . . ? C21 C22 C23 114.39(8) . . ? C21 C22 H22A 110.1(8) . . ? C23 C22 H22A 110.7(8) . . ? C21 C22 H22B 106.3(8) . . ? C23 C22 H22B 109.4(8) . . ? H22A C22 H22B 105.5(11) . . ? C24 C23 C22 111.62(7) . . ? C24 C23 H23A 110.8(8) . . ? C22 C23 H23A 108.0(8) . . ? C24 C23 H23B 108.6(8) . . ? C22 C23 H23B 110.7(8) . . ? H23A C23 H23B 107.0(11) . . ? C23 C24 C25 108.79(8) . . ? C23 C24 H24A 111.3(8) . . ? C25 C24 H24A 110.0(8) . . ? C23 C24 H24B 110.3(8) . . ? C25 C24 H24B 110.1(8) . . ? H24A C24 H24B 106.3(11) . . ? C26 C25 C24 110.69(8) . . ? C26 C25 H25A 108.2(8) . . ? C24 C25 H25A 113.6(7) . . ? C26 C25 H25B 109.6(7) . . ? C24 C25 H25B 109.5(7) . . ? H25A C25 H25B 105.1(11) . . ? N5 C26 C21 123.41(8) . . ? N5 C26 C25 115.66(7) . . ? C21 C26 C25 120.92(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 N2 C1 N1 -4.14(15) . . . . ? C9 N2 C1 C2 175.55(8) . . . . ? C8 N1 C1 N2 -179.33(9) . . . . ? C8 N1 C1 C2 0.93(10) . . . . ? N2 C1 C2 C3 -0.02(15) . . . . ? N1 C1 C2 C3 179.74(9) . . . . ? N2 C1 C2 C7 -178.67(8) . . . . ? N1 C1 C2 C7 1.09(10) . . . . ? C7 C2 C3 C4 0.56(14) . . . . ? C1 C2 C3 C4 -177.93(9) . . . . ? C2 C3 C4 C5 0.10(15) . . . . ? C3 C4 C5 C6 -0.72(16) . . . . ? C4 C5 C6 C7 0.65(15) . . . . ? C5 C6 C7 C2 0.01(14) . . . . ? C5 C6 C7 C8 -179.09(9) . . . . ? C3 C2 C7 C6 -0.63(14) . . . . ? C1 C2 C7 C6 178.15(8) . . . . ? C3 C2 C7 C8 178.65(8) . . . . ? C1 C2 C7 C8 -2.56(10) . . . . ? C18 N4 C8 N1 -7.01(14) . . . . ? C18 N4 C8 C7 173.33(8) . . . . ? C1 N1 C8 N4 177.83(9) . . . . ? C1 N1 C8 C7 -2.47(10) . . . . ? C6 C7 C8 N4 2.00(15) . . . . ? C2 C7 C8 N4 -177.19(8) . . . . ? C6 C7 C8 N1 -177.72(9) . . . . ? C2 C7 C8 N1 3.08(10) . . . . ? C17 N3 C9 C10 0.91(13) . . . . ? C17 N3 C9 N2 -176.95(8) . . . . ? C1 N2 C9 N3 -8.99(13) . . . . ? C1 N2 C9 C10 173.03(8) . . . . ? N3 C9 C10 C11 0.10(13) . . . . ? N2 C9 C10 C11 178.09(8) . . . . ? C9 C10 C11 C12 -0.45(14) . . . . ? C10 C11 C12 C17 -0.18(14) . . . . ? C10 C11 C12 C13 -179.88(9) . . . . ? C11 C12 C13 C14 -169.23(9) . . . . ? C17 C12 C13 C14 11.10(13) . . . . ? C12 C13 C14 C15 -43.76(11) . . . . ? C13 C14 C15 C16 65.64(10) . . . . ? C14 C15 C16 C17 -53.51(11) . . . . ? C9 N3 C17 C12 -1.62(13) . . . . ? C9 N3 C17 C16 178.83(8) . . . . ? C11 C12 C17 N3 1.26(13) . . . . ? C13 C12 C17 N3 -179.05(8) . . . . ? C11 C12 C17 C16 -179.21(9) . . . . ? C13 C12 C17 C16 0.48(13) . . . . ? C15 C16 C17 N3 -159.17(8) . . . . ? C15 C16 C17 C12 21.27(13) . . . . ? C26 N5 C18 C19 0.03(13) . . . . ? C26 N5 C18 N4 -177.15(8) . . . . ? C8 N4 C18 N5 -18.44(13) . . . . ? C8 N4 C18 C19 164.28(8) . . . . ? N5 C18 C19 C20 1.36(13) . . . . ? N4 C18 C19 C20 178.59(8) . . . . ? C18 C19 C20 C21 -1.19(13) . . . . ? C19 C20 C21 C26 -0.26(13) . . . . ? C19 C20 C21 C22 175.43(8) . . . . ? C26 C21 C22 C23 -7.90(12) . . . . ? C20 C21 C22 C23 176.63(8) . . . . ? C21 C22 C23 C24 36.31(11) . . . . ? C22 C23 C24 C25 -61.84(10) . . . . ? C23 C24 C25 C26 57.68(10) . . . . ? C18 N5 C26 C21 -1.63(13) . . . . ? C18 N5 C26 C25 179.29(8) . . . . ? C20 C21 C26 N5 1.74(13) . . . . ? C22 C21 C26 N5 -173.91(8) . . . . ? C20 C21 C26 C25 -179.24(8) . . . . ? C22 C21 C26 C25 5.12(12) . . . . ? C24 C25 C26 N5 148.78(8) . . . . ? C24 C25 C26 C21 -30.31(11) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.511 _refine_diff_density_min -0.262 _refine_diff_density_rms 0.056 _diffrn_ambient_environment 'perfluoro polyether oil' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_specimen_support 'polyimid foil' _diffrn_detector 'CCD plate' _diffrn_detector_type CCD-PXL-KAF2 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 821500' #TrackingRef '- ga_mkr12-ga_mkr20-ga_ds12-ga_mkr14-ga_ds17.cif' _audit_creation_method SHELXL-97 _audit_block_code ga_mkr20 _audit_block_refno 992 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Li N5 O' _chemical_properties_physical 'air-sensitive, moisture-sensitive' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 485.55 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' Li Li -0.0003 0.0001 '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 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration . loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.194(5) _cell_length_b 18.995(9) _cell_length_c 11.738(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.689(11) _cell_angle_gamma 90.00 _cell_volume 2496(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8077 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 31.72 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7964 _exptl_absorpt_correction_T_max 0.8623 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) SADABS (Sheldrick & Bruker AXS, 2004-2008) ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Smart 1000' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean 8.19 _diffrn_reflns_number 63099 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 32.26 _reflns_number_total 8437 _reflns_number_gt 6541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-5.631 (Bruker AXS, 2003)' _computing_cell_refinement ; SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors of the unit cell constants from Monte Carlo simulations. ; _computing_data_reduction 'SAINT (Bruker AXS, 1997-2008); SADABS (Bruker AXS, 2008)' _computing_structure_solution 'SUPERFLIP (Palatinus, 2007-2009)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0767P)^2^+0.7653P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8437 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1445 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 O1 O 0.63094(8) 0.94536(4) 0.18288(7) 0.02113(17) Uani 1 1 d . . . N1 N 0.37275(8) 0.94594(4) 0.31270(8) 0.01515(17) Uani 1 1 d . . . N2 N 0.32552(8) 0.82133(5) 0.30444(8) 0.01709(18) Uani 1 1 d . . . N3 N 0.53389(8) 0.83369(5) 0.36160(8) 0.01575(17) Uani 1 1 d . . . N4 N 0.33290(8) 1.07148(5) 0.30384(8) 0.01560(17) Uani 1 1 d . . . N5 N 0.54052(8) 1.05543(5) 0.36130(7) 0.01453(17) Uani 1 1 d . . . C1 C 0.30245(9) 0.88805(5) 0.29176(9) 0.01496(19) Uani 1 1 d . . . C2 C 0.18226(9) 0.91142(5) 0.25241(9) 0.01529(19) Uani 1 1 d . . . C3 C 0.08105(10) 0.87460(6) 0.21856(10) 0.0205(2) Uani 1 1 d . . . H3 H 0.0818(14) 0.8246(9) 0.2170(13) 0.025 Uiso 1 1 d . . . C4 C -0.01957(10) 0.91376(7) 0.18696(11) 0.0235(2) Uani 1 1 d . . . H4 H -0.0924(15) 0.8885(9) 0.1607(14) 0.028 Uiso 1 1 d . . . C5 C -0.01785(10) 0.98717(6) 0.19024(11) 0.0227(2) Uani 1 1 d . . . H5 H -0.0891(14) 1.0148(9) 0.1666(14) 0.027 Uiso 1 1 d . . . C6 C 0.08383(10) 1.02385(6) 0.22554(10) 0.0193(2) Uani 1 1 d . . . H6 H 0.0867(13) 1.0745(9) 0.2282(13) 0.023 Uiso 1 1 d . . . C7 C 0.18350(9) 0.98460(5) 0.25614(9) 0.01504(19) Uani 1 1 d . . . C8 C 0.30523(9) 1.00508(5) 0.29411(9) 0.01424(18) Uani 1 1 d . . . C9 C 0.43346(10) 0.79506(5) 0.34628(9) 0.01592(19) Uani 1 1 d . . . C10 C 0.43210(10) 0.72236(6) 0.37106(10) 0.0189(2) Uani 1 1 d . . . H10 H 0.3580(13) 0.6967(8) 0.3578(13) 0.023 Uiso 1 1 d . . . C11 C 0.53425(11) 0.69050(6) 0.41237(10) 0.0193(2) Uani 1 1 d . . . H11 H 0.5333(14) 0.6404(8) 0.4326(13) 0.023 Uiso 1 1 d . . . C12 C 0.63929(10) 0.72929(5) 0.42668(9) 0.0173(2) Uani 1 1 d . . . C13 C 0.75367(11) 0.69445(6) 0.46721(11) 0.0231(2) Uani 1 1 d . . . H13A H 0.7878(14) 0.6676(9) 0.3999(14) 0.028 Uiso 1 1 d . . . H13B H 0.7330(14) 0.6599(9) 0.5283(14) 0.028 Uiso 1 1 d . . . C14 C 0.84716(11) 0.74702(7) 0.50960(11) 0.0255(2) Uani 1 1 d . . . H14A H 0.9252(15) 0.7230(9) 0.5208(14) 0.031 Uiso 1 1 d . . . H14B H 0.8228(15) 0.7671(9) 0.5861(15) 0.031 Uiso 1 1 d . . . C15 C 0.85940(10) 0.80643(6) 0.42351(11) 0.0221(2) Uani 1 1 d . . . H15A H 0.8770(14) 0.7862(8) 0.3490(14) 0.027 Uiso 1 1 d . . . H15B H 0.9253(14) 0.8387(9) 0.4429(14) 0.027 Uiso 1 1 d . . . C16 C 0.74239(10) 0.84747(6) 0.41395(10) 0.0182(2) Uani 1 1 d . . . H16A H 0.7460(13) 0.8802(8) 0.3483(13) 0.022 Uiso 1 1 d . . . H16B H 0.7305(13) 0.8768(8) 0.4854(13) 0.022 Uiso 1 1 d . . . C17 C 0.63421(9) 0.80091(5) 0.39970(9) 0.01552(19) Uani 1 1 d . . . C18 C 0.44584(9) 1.09643(5) 0.33400(9) 0.01474(18) Uani 1 1 d . . . C19 C 0.45553(10) 1.17051(5) 0.33199(9) 0.0174(2) Uani 1 1 d . . . H19 H 0.3845(13) 1.1988(8) 0.3133(13) 0.021 Uiso 1 1 d . . . C20 C 0.56415(10) 1.20133(6) 0.35487(9) 0.0184(2) Uani 1 1 d . . . H20 H 0.5765(13) 1.2529(8) 0.3524(13) 0.022 Uiso 1 1 d . . . C21 C 0.66385(10) 1.15963(6) 0.38026(9) 0.01676(19) Uani 1 1 d . . . C22 C 0.78547(10) 1.19244(6) 0.39710(11) 0.0215(2) Uani 1 1 d . . . H22A H 0.7934(14) 1.2099(8) 0.4771(14) 0.026 Uiso 1 1 d . . . H22B H 0.7938(14) 1.2341(9) 0.3442(14) 0.026 Uiso 1 1 d . . . C23 C 0.88420(10) 1.13950(6) 0.37192(10) 0.0208(2) Uani 1 1 d . . . H23A H 0.8796(14) 1.1267(8) 0.2891(14) 0.025 Uiso 1 1 d . . . H23B H 0.9623(14) 1.1607(8) 0.3829(13) 0.025 Uiso 1 1 d . . . C24 C 0.86580(10) 1.07399(6) 0.44458(10) 0.0200(2) Uani 1 1 d . . . H24A H 0.9328(14) 1.0400(8) 0.4358(14) 0.024 Uiso 1 1 d . . . H24B H 0.8654(14) 1.0887(8) 0.5246(14) 0.024 Uiso 1 1 d . . . C25 C 0.74865(10) 1.03738(6) 0.41209(9) 0.01677(19) Uani 1 1 d . . . H25A H 0.7629(13) 1.0081(8) 0.3434(13) 0.020 Uiso 1 1 d . . . H25B H 0.7233(13) 1.0048(8) 0.4738(13) 0.020 Uiso 1 1 d . . . C26 C 0.64676(9) 1.08698(5) 0.38478(8) 0.01455(18) Uani 1 1 d . . . C27 C 0.64042(12) 1.00815(6) 0.11576(10) 0.0225(2) Uani 1 1 d . . . H27A H 0.5613(15) 1.0293(9) 0.1059(14) 0.027 Uiso 1 1 d . . . H27B H 0.6915(15) 1.0420(9) 0.1580(14) 0.027 Uiso 1 1 d . . . C28 C 0.69272(13) 0.98522(8) 0.00180(11) 0.0297(3) Uani 1 1 d . . . H28A H 0.6558(15) 1.0095(9) -0.0630(16) 0.036 Uiso 1 1 d . . . H28B H 0.7776(16) 0.9963(9) -0.0009(15) 0.036 Uiso 1 1 d . . . C29 C 0.67195(16) 0.90522(9) -0.00153(12) 0.0379(4) Uani 1 1 d . . . H29A H 0.6343(17) 0.8895(10) -0.0728(17) 0.045 Uiso 1 1 d . . . H29B H 0.7473(18) 0.8807(10) 0.0031(17) 0.045 Uiso 1 1 d . . . C30 C 0.59676(14) 0.89102(7) 0.10315(11) 0.0303(3) Uani 1 1 d . . . H30A H 0.6161(16) 0.8467(10) 0.1400(15) 0.036 Uiso 1 1 d . . . H30B H 0.5080(16) 0.8981(10) 0.0816(15) 0.036 Uiso 1 1 d . . . Li1 Li 0.54096(18) 0.94483(10) 0.33389(18) 0.0202(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 O1 0.0272(4) 0.0188(4) 0.0174(4) -0.0004(3) 0.0015(3) 0.0022(3) N1 0.0165(4) 0.0116(4) 0.0173(4) -0.0003(3) -0.0006(3) -0.0005(3) N2 0.0178(4) 0.0139(4) 0.0196(4) -0.0002(3) -0.0003(3) -0.0005(3) N3 0.0177(4) 0.0131(4) 0.0164(4) 0.0006(3) -0.0001(3) 0.0003(3) N4 0.0161(4) 0.0131(4) 0.0176(4) -0.0007(3) 0.0001(3) -0.0004(3) N5 0.0166(4) 0.0128(4) 0.0142(4) -0.0003(3) 0.0008(3) -0.0005(3) C1 0.0158(4) 0.0143(4) 0.0148(4) -0.0009(3) 0.0003(3) -0.0009(3) C2 0.0146(4) 0.0160(4) 0.0153(4) -0.0012(3) 0.0007(3) -0.0009(3) C3 0.0178(5) 0.0181(5) 0.0255(5) -0.0035(4) -0.0009(4) -0.0020(4) C4 0.0163(5) 0.0253(6) 0.0290(6) -0.0038(5) -0.0020(4) -0.0017(4) C5 0.0161(5) 0.0242(5) 0.0276(6) -0.0010(4) -0.0022(4) 0.0029(4) C6 0.0171(5) 0.0182(5) 0.0227(5) 0.0004(4) 0.0004(4) 0.0015(4) C7 0.0152(4) 0.0155(4) 0.0144(4) -0.0002(3) 0.0005(3) -0.0007(3) C8 0.0148(4) 0.0148(4) 0.0131(4) -0.0004(3) 0.0006(3) 0.0002(3) C9 0.0191(5) 0.0130(4) 0.0157(4) -0.0009(3) 0.0008(4) 0.0005(3) C10 0.0231(5) 0.0126(4) 0.0209(5) -0.0004(4) 0.0007(4) -0.0020(4) C11 0.0267(5) 0.0114(4) 0.0199(5) 0.0009(4) 0.0019(4) 0.0006(4) C12 0.0227(5) 0.0129(4) 0.0164(5) 0.0010(4) 0.0010(4) 0.0027(4) C13 0.0243(5) 0.0161(5) 0.0290(6) 0.0054(4) -0.0005(4) 0.0052(4) C14 0.0238(5) 0.0235(6) 0.0289(6) 0.0069(5) -0.0045(4) 0.0043(4) C15 0.0194(5) 0.0213(5) 0.0255(6) 0.0045(4) -0.0007(4) 0.0018(4) C16 0.0186(5) 0.0149(4) 0.0210(5) 0.0024(4) -0.0017(4) 0.0000(4) C17 0.0190(5) 0.0130(4) 0.0145(4) 0.0007(3) 0.0009(3) 0.0016(3) C18 0.0175(4) 0.0123(4) 0.0144(4) -0.0008(3) 0.0015(3) -0.0002(3) C19 0.0201(5) 0.0123(4) 0.0199(5) -0.0004(4) 0.0004(4) 0.0008(4) C20 0.0235(5) 0.0119(4) 0.0197(5) -0.0009(4) 0.0011(4) -0.0017(4) C21 0.0199(5) 0.0142(4) 0.0162(4) -0.0014(3) 0.0005(4) -0.0026(4) C22 0.0214(5) 0.0170(5) 0.0263(6) -0.0012(4) -0.0005(4) -0.0052(4) C23 0.0189(5) 0.0233(5) 0.0202(5) 0.0013(4) -0.0007(4) -0.0046(4) C24 0.0194(5) 0.0228(5) 0.0176(5) 0.0011(4) -0.0024(4) -0.0013(4) C25 0.0178(5) 0.0155(4) 0.0169(5) 0.0008(4) -0.0014(4) 0.0002(4) C26 0.0176(4) 0.0130(4) 0.0130(4) -0.0004(3) 0.0009(3) 0.0000(3) C27 0.0277(6) 0.0225(5) 0.0173(5) 0.0037(4) 0.0006(4) -0.0001(4) C28 0.0277(6) 0.0450(8) 0.0165(5) 0.0022(5) 0.0028(4) 0.0022(5) C29 0.0534(9) 0.0414(8) 0.0188(6) -0.0055(5) 0.0009(6) 0.0210(7) C30 0.0471(8) 0.0198(6) 0.0240(6) -0.0058(4) -0.0014(5) 0.0051(5) Li1 0.0208(9) 0.0159(9) 0.0240(10) 0.0004(7) 0.0000(7) -0.0008(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 O1 C27 1.4340(15) . ? O1 C30 1.4419(16) . ? O1 Li1 2.049(2) . ? N1 C8 1.3699(14) . ? N1 C1 1.3725(14) . ? N1 Li1 1.896(2) . ? N2 C1 1.3016(15) . ? N2 C9 1.3914(15) . ? N3 C9 1.3527(14) . ? N3 C17 1.3553(14) . ? N3 Li1 2.137(2) . ? N4 C8 1.3034(14) . ? N4 C18 1.3920(14) . ? N5 C18 1.3507(14) . ? N5 C26 1.3570(14) . ? N5 Li1 2.125(2) . ? C1 C2 1.4851(15) . ? C2 C3 1.3855(15) . ? C2 C7 1.3908(16) . ? C3 C4 1.3962(17) . ? C3 H3 0.950(16) . ? C4 C5 1.3952(19) . ? C4 H4 0.991(16) . ? C5 C6 1.3932(17) . ? C5 H5 0.992(16) . ? C6 C7 1.3855(15) . ? C6 H6 0.964(16) . ? C7 C8 1.4806(15) . ? C9 C10 1.4113(16) . ? C10 C11 1.3768(17) . ? C10 H10 0.973(15) . ? C11 C12 1.3960(16) . ? C11 H11 0.981(15) . ? C12 C17 1.3978(16) . ? C12 C13 1.5129(16) . ? C13 C14 1.5257(19) . ? C13 H13A 1.018(16) . ? C13 H13B 1.001(17) . ? C14 C15 1.5221(18) . ? C14 H14A 0.992(17) . ? C14 H14B 1.016(17) . ? C15 C16 1.5272(17) . ? C15 H15A 0.977(16) . ? C15 H15B 0.984(16) . ? C16 C17 1.5072(16) . ? C16 H16A 0.991(15) . ? C16 H16B 1.017(15) . ? C18 C19 1.4115(16) . ? C19 C20 1.3731(16) . ? C19 H19 0.983(15) . ? C20 C21 1.3978(16) . ? C20 H20 0.990(15) . ? C21 C26 1.3942(16) . ? C21 C22 1.5081(16) . ? C22 C23 1.5258(18) . ? C22 H22A 0.999(16) . ? C22 H22B 1.011(16) . ? C23 C24 1.5239(17) . ? C23 H23A 1.003(16) . ? C23 H23B 0.969(16) . ? C24 C25 1.5285(16) . ? C24 H24A 0.996(16) . ? C24 H24B 0.979(16) . ? C25 C26 1.5107(15) . ? C25 H25A 0.995(15) . ? C25 H25B 0.997(15) . ? C27 C28 1.5299(18) . ? C27 H27A 0.978(16) . ? C27 H27B 0.989(17) . ? C28 C29 1.538(2) . ? C28 H28A 0.978(18) . ? C28 H28B 0.973(18) . ? C29 C30 1.522(2) . ? C29 H29A 0.98(2) . ? C29 H29B 0.96(2) . ? C30 H30A 0.969(18) . ? C30 H30B 1.031(18) . ? 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 C27 O1 C30 105.04(10) . . ? C27 O1 Li1 121.31(9) . . ? C30 O1 Li1 115.38(10) . . ? C8 N1 C1 108.32(9) . . ? C8 N1 Li1 125.10(9) . . ? C1 N1 Li1 125.50(9) . . ? C1 N2 C9 124.05(9) . . ? C9 N3 C17 118.59(10) . . ? C9 N3 Li1 123.22(9) . . ? C17 N3 Li1 118.16(9) . . ? C8 N4 C18 124.47(9) . . ? C18 N5 C26 118.47(9) . . ? C18 N5 Li1 122.50(9) . . ? C26 N5 Li1 117.62(9) . . ? N2 C1 N1 130.32(10) . . ? N2 C1 C2 120.29(9) . . ? N1 C1 C2 109.37(9) . . ? C3 C2 C7 121.42(10) . . ? C3 C2 C1 132.29(10) . . ? C7 C2 C1 106.27(9) . . ? C2 C3 C4 117.49(11) . . ? C2 C3 H3 120.1(9) . . ? C4 C3 H3 122.4(9) . . ? C5 C4 C3 120.95(11) . . ? C5 C4 H4 120.2(10) . . ? C3 C4 H4 118.9(10) . . ? C6 C5 C4 121.26(11) . . ? C6 C5 H5 118.0(10) . . ? C4 C5 H5 120.7(10) . . ? C7 C6 C5 117.42(11) . . ? C7 C6 H6 120.2(9) . . ? C5 C6 H6 122.4(9) . . ? C6 C7 C2 121.46(10) . . ? C6 C7 C8 132.22(10) . . ? C2 C7 C8 106.31(9) . . ? N4 C8 N1 130.50(10) . . ? N4 C8 C7 119.83(9) . . ? N1 C8 C7 109.67(9) . . ? N3 C9 N2 124.69(10) . . ? N3 C9 C10 120.96(10) . . ? N2 C9 C10 114.34(9) . . ? C11 C10 C9 119.45(10) . . ? C11 C10 H10 122.6(9) . . ? C9 C10 H10 118.0(9) . . ? C10 C11 C12 120.34(10) . . ? C10 C11 H11 120.1(9) . . ? C12 C11 H11 119.6(9) . . ? C11 C12 C17 117.03(10) . . ? C11 C12 C13 121.02(10) . . ? C17 C12 C13 121.93(10) . . ? C12 C13 C14 113.01(10) . . ? C12 C13 H13A 107.4(9) . . ? C14 C13 H13A 108.5(9) . . ? C12 C13 H13B 108.1(9) . . ? C14 C13 H13B 111.0(9) . . ? H13A C13 H13B 108.7(13) . . ? C15 C14 C13 109.61(10) . . ? C15 C14 H14A 110.0(10) . . ? C13 C14 H14A 110.0(10) . . ? C15 C14 H14B 109.6(10) . . ? C13 C14 H14B 110.1(9) . . ? H14A C14 H14B 107.5(13) . . ? C14 C15 C16 110.08(10) . . ? C14 C15 H15A 108.9(9) . . ? C16 C15 H15A 108.5(9) . . ? C14 C15 H15B 112.5(10) . . ? C16 C15 H15B 109.8(9) . . ? H15A C15 H15B 107.0(13) . . ? C17 C16 C15 113.32(10) . . ? C17 C16 H16A 108.8(9) . . ? C15 C16 H16A 109.5(9) . . ? C17 C16 H16B 107.5(9) . . ? C15 C16 H16B 109.9(9) . . ? H16A C16 H16B 107.7(12) . . ? N3 C17 C12 123.59(10) . . ? N3 C17 C16 115.36(10) . . ? C12 C17 C16 121.03(10) . . ? N5 C18 N4 124.87(10) . . ? N5 C18 C19 121.24(10) . . ? N4 C18 C19 113.88(9) . . ? C20 C19 C18 119.32(10) . . ? C20 C19 H19 121.5(9) . . ? C18 C19 H19 119.2(9) . . ? C19 C20 C21 120.20(10) . . ? C19 C20 H20 122.7(9) . . ? C21 C20 H20 117.1(9) . . ? C26 C21 C20 117.35(10) . . ? C26 C21 C22 121.88(10) . . ? C20 C21 C22 120.72(10) . . ? C21 C22 C23 110.92(10) . . ? C21 C22 H22A 109.3(9) . . ? C23 C22 H22A 110.2(9) . . ? C21 C22 H22B 109.4(9) . . ? C23 C22 H22B 108.9(9) . . ? H22A C22 H22B 108.0(13) . . ? C24 C23 C22 109.07(10) . . ? C24 C23 H23A 109.8(9) . . ? C22 C23 H23A 108.6(9) . . ? C24 C23 H23B 113.1(10) . . ? C22 C23 H23B 110.7(9) . . ? H23A C23 H23B 105.4(13) . . ? C23 C24 C25 110.68(9) . . ? C23 C24 H24A 111.4(9) . . ? C25 C24 H24A 108.9(9) . . ? C23 C24 H24B 107.8(9) . . ? C25 C24 H24B 110.8(9) . . ? H24A C24 H24B 107.2(13) . . ? C26 C25 C24 114.36(10) . . ? C26 C25 H25A 107.8(9) . . ? C24 C25 H25A 108.2(9) . . ? C26 C25 H25B 108.7(9) . . ? C24 C25 H25B 110.6(9) . . ? H25A C25 H25B 107.0(12) . . ? N5 C26 C21 123.34(10) . . ? N5 C26 C25 115.17(9) . . ? C21 C26 C25 121.45(10) . . ? O1 C27 C28 105.97(11) . . ? O1 C27 H27A 109.5(10) . . ? C28 C27 H27A 111.6(9) . . ? O1 C27 H27B 108.1(10) . . ? C28 C27 H27B 113.5(10) . . ? H27A C27 H27B 108.1(14) . . ? C27 C28 C29 104.13(11) . . ? C27 C28 H28A 112.5(10) . . ? C29 C28 H28A 112.6(11) . . ? C27 C28 H28B 110.5(11) . . ? C29 C28 H28B 111.1(11) . . ? H28A C28 H28B 106.1(15) . . ? C30 C29 C28 103.86(10) . . ? C30 C29 H29A 113.6(12) . . ? C28 C29 H29A 112.7(12) . . ? C30 C29 H29B 111.2(12) . . ? C28 C29 H29B 110.1(12) . . ? H29A C29 H29B 105.5(16) . . ? O1 C30 C29 104.61(12) . . ? O1 C30 H30A 106.0(11) . . ? C29 C30 H30A 113.1(11) . . ? O1 C30 H30B 108.3(10) . . ? C29 C30 H30B 108.6(10) . . ? H30A C30 H30B 115.6(14) . . ? N1 Li1 O1 112.58(11) . . ? N1 Li1 N5 90.27(9) . . ? O1 Li1 N5 97.36(9) . . ? N1 Li1 N3 89.57(9) . . ? O1 Li1 N3 98.97(9) . . ? N5 Li1 N3 162.37(12) . . ? 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 C9 N2 C1 N1 1.03(18) . . . . ? C9 N2 C1 C2 -176.63(9) . . . . ? C8 N1 C1 N2 -175.47(11) . . . . ? Li1 N1 C1 N2 15.93(18) . . . . ? C8 N1 C1 C2 2.38(11) . . . . ? Li1 N1 C1 C2 -166.21(10) . . . . ? N2 C1 C2 C3 -3.36(18) . . . . ? N1 C1 C2 C3 178.53(11) . . . . ? N2 C1 C2 C7 175.50(10) . . . . ? N1 C1 C2 C7 -2.61(11) . . . . ? C7 C2 C3 C4 0.72(16) . . . . ? C1 C2 C3 C4 179.43(11) . . . . ? C2 C3 C4 C5 -0.39(18) . . . . ? C3 C4 C5 C6 -0.29(19) . . . . ? C4 C5 C6 C7 0.64(17) . . . . ? C5 C6 C7 C2 -0.31(16) . . . . ? C5 C6 C7 C8 178.23(11) . . . . ? C3 C2 C7 C6 -0.38(16) . . . . ? C1 C2 C7 C6 -179.39(10) . . . . ? C3 C2 C7 C8 -179.25(10) . . . . ? C1 C2 C7 C8 1.74(11) . . . . ? C18 N4 C8 N1 2.14(18) . . . . ? C18 N4 C8 C7 -177.11(9) . . . . ? C1 N1 C8 N4 179.41(11) . . . . ? Li1 N1 C8 N4 -11.94(18) . . . . ? C1 N1 C8 C7 -1.28(11) . . . . ? Li1 N1 C8 C7 167.37(10) . . . . ? C6 C7 C8 N4 0.32(17) . . . . ? C2 C7 C8 N4 179.02(9) . . . . ? C6 C7 C8 N1 -179.08(11) . . . . ? C2 C7 C8 N1 -0.38(11) . . . . ? C17 N3 C9 N2 -177.93(9) . . . . ? Li1 N3 C9 N2 4.15(16) . . . . ? C17 N3 C9 C10 1.02(15) . . . . ? Li1 N3 C9 C10 -176.90(10) . . . . ? C1 N2 C9 N3 -11.23(17) . . . . ? C1 N2 C9 C10 169.76(10) . . . . ? N3 C9 C10 C11 0.58(16) . . . . ? N2 C9 C10 C11 179.63(10) . . . . ? C9 C10 C11 C12 -1.77(16) . . . . ? C10 C11 C12 C17 1.33(16) . . . . ? C10 C11 C12 C13 -177.37(10) . . . . ? C11 C12 C13 C14 -163.62(11) . . . . ? C17 C12 C13 C14 17.74(16) . . . . ? C12 C13 C14 C15 -47.87(14) . . . . ? C13 C14 C15 C16 63.88(13) . . . . ? C14 C15 C16 C17 -48.11(13) . . . . ? C9 N3 C17 C12 -1.48(15) . . . . ? Li1 N3 C17 C12 176.54(10) . . . . ? C9 N3 C17 C16 179.68(9) . . . . ? Li1 N3 C17 C16 -2.29(13) . . . . ? C11 C12 C17 N3 0.31(16) . . . . ? C13 C12 C17 N3 179.01(10) . . . . ? C11 C12 C17 C16 179.08(10) . . . . ? C13 C12 C17 C16 -2.23(16) . . . . ? C15 C16 C17 N3 -163.53(9) . . . . ? C15 C16 C17 C12 17.61(14) . . . . ? C26 N5 C18 N4 177.48(9) . . . . ? Li1 N5 C18 N4 11.33(15) . . . . ? C26 N5 C18 C19 -1.30(15) . . . . ? Li1 N5 C18 C19 -167.46(10) . . . . ? C8 N4 C18 N5 -2.59(16) . . . . ? C8 N4 C18 C19 176.27(10) . . . . ? N5 C18 C19 C20 1.99(16) . . . . ? N4 C18 C19 C20 -176.92(10) . . . . ? C18 C19 C20 C21 -0.23(16) . . . . ? C19 C20 C21 C26 -2.04(16) . . . . ? C19 C20 C21 C22 175.50(10) . . . . ? C26 C21 C22 C23 22.37(15) . . . . ? C20 C21 C22 C23 -155.07(10) . . . . ? C21 C22 C23 C24 -54.82(13) . . . . ? C22 C23 C24 C25 63.94(13) . . . . ? C23 C24 C25 C26 -38.52(13) . . . . ? C18 N5 C26 C21 -1.16(15) . . . . ? Li1 N5 C26 C21 165.67(10) . . . . ? C18 N5 C26 C25 -178.77(9) . . . . ? Li1 N5 C26 C25 -11.94(13) . . . . ? C20 C21 C26 N5 2.82(16) . . . . ? C22 C21 C26 N5 -174.69(10) . . . . ? C20 C21 C26 C25 -179.70(9) . . . . ? C22 C21 C26 C25 2.78(16) . . . . ? C24 C25 C26 N5 -176.85(9) . . . . ? C24 C25 C26 C21 5.49(14) . . . . ? C30 O1 C27 C28 -37.02(13) . . . . ? Li1 O1 C27 C28 -170.08(10) . . . . ? O1 C27 C28 C29 17.87(14) . . . . ? C27 C28 C29 C30 6.62(15) . . . . ? C27 O1 C30 C29 41.33(13) . . . . ? Li1 O1 C30 C29 177.64(10) . . . . ? C28 C29 C30 O1 -28.81(14) . . . . ? C8 N1 Li1 O1 -83.41(13) . . . . ? C1 N1 Li1 O1 83.33(13) . . . . ? C8 N1 Li1 N5 14.68(13) . . . . ? C1 N1 Li1 N5 -178.58(9) . . . . ? C8 N1 Li1 N3 177.05(9) . . . . ? C1 N1 Li1 N3 -16.21(13) . . . . ? C27 O1 Li1 N1 75.24(13) . . . . ? C30 O1 Li1 N1 -53.43(14) . . . . ? C27 O1 Li1 N5 -18.14(13) . . . . ? C30 O1 Li1 N5 -146.81(9) . . . . ? C27 O1 Li1 N3 168.53(9) . . . . ? C30 O1 Li1 N3 39.86(12) . . . . ? C18 N5 Li1 N1 -14.88(13) . . . . ? C26 N5 Li1 N1 178.85(8) . . . . ? C18 N5 Li1 O1 97.94(11) . . . . ? C26 N5 Li1 O1 -68.32(11) . . . . ? C18 N5 Li1 N3 -104.3(4) . . . . ? C26 N5 Li1 N3 89.4(4) . . . . ? C9 N3 Li1 N1 7.47(13) . . . . ? C17 N3 Li1 N1 -170.46(8) . . . . ? C9 N3 Li1 O1 -105.34(11) . . . . ? C17 N3 Li1 O1 76.73(12) . . . . ? C9 N3 Li1 N5 97.0(4) . . . . ? C17 N3 Li1 N5 -80.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.540 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.061 _diffrn_ambient_environment 'perfluoro polyether oil' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_specimen_support 'polyimid foil' _diffrn_detector 'CCD plate' _diffrn_detector_type CCD-PXL-KAF2 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_3a _database_code_depnum_ccdc_archive 'CCDC 821501' #TrackingRef '- ga_mkr12-ga_mkr20-ga_ds12-ga_mkr14-ga_ds17.cif' _audit_creation_method SHELXL-97 _audit_block_code ga_ds12 _audit_block_refno 1005 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H30 Cl Co N5 O S' _chemical_melting_point ? _exptl_crystal_description irregular _exptl_crystal_colour red _diffrn_ambient_temperature 100(2) _chemical_formula_weight 579.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_int_tables_number 29 _chemical_absolute_configuration ad 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 16.954(9) _cell_length_b 8.904(5) _cell_length_c 17.198(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2596(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7635 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.53 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1204 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6923 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) SADABS (Sheldrick & Bruker AXS, 2004-2008) ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Smart 1000' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean 8.19 _diffrn_reflns_number 63380 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 30.51 _reflns_number_total 7944 _reflns_number_gt 6622 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-5.631 (Bruker AXS, 2003)' _computing_cell_refinement ; SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors of the unit cell constants from Monte Carlo simulations. ; _computing_data_reduction 'SAINT (Bruker AXS, 1997-2008); SADABS (Bruker AXS, 2008)' _computing_structure_solution 'SUPERFLIP (Palatinus, 2007-2009)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0236P)^2^+0.7692P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _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 0.009(11) _refine_ls_number_reflns 7944 _refine_ls_number_parameters 336 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0725 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.604001(16) 0.43175(3) 0.270307(17) 0.01297(6) Uani 1 1 d . . . Cl1 Cl 0.71734(3) 0.28463(6) 0.25974(3) 0.01779(11) Uani 1 1 d . . . S1 S 0.42741(3) 0.54107(6) 0.30616(3) 0.01478(11) Uani 1 1 d . . . O1 O 0.49878(9) 0.45257(19) 0.33400(9) 0.0166(3) Uani 1 1 d . . . N1 N 0.60659(11) 0.6006(2) 0.19896(11) 0.0139(4) Uani 1 1 d . . . N2 N 0.54393(11) 0.4967(2) 0.08423(11) 0.0153(4) Uani 1 1 d . . . N3 N 0.53715(11) 0.3038(2) 0.18524(11) 0.0143(4) Uani 1 1 d . . . N4 N 0.67656(10) 0.78679(19) 0.27561(12) 0.0149(4) Uani 1 1 d . . . N5 N 0.65645(11) 0.5690(2) 0.35910(11) 0.0138(4) Uani 1 1 d . . . C1 C 0.57961(14) 0.6006(3) 0.12282(13) 0.0142(5) Uani 1 1 d . . . C2 C 0.59729(13) 0.7483(3) 0.08733(14) 0.0152(5) Uani 1 1 d . . . C3 C 0.57960(14) 0.8085(3) 0.01486(14) 0.0193(5) Uani 1 1 d . . . H3 H 0.5523 0.7518 -0.0234 0.023 Uiso 1 1 calc R . . C4 C 0.60368(15) 0.9558(3) 0.00084(14) 0.0216(5) Uani 1 1 d . . . H4 H 0.5929 1.0001 -0.0483 0.026 Uiso 1 1 calc R . . C5 C 0.64282(14) 1.0388(3) 0.05678(14) 0.0194(5) Uani 1 1 d . . . H5 H 0.6582 1.1390 0.0452 0.023 Uiso 1 1 calc R . . C6 C 0.66038(14) 0.9793(3) 0.12978(14) 0.0174(5) Uani 1 1 d . . . H6 H 0.6870 1.0365 0.1683 0.021 Uiso 1 1 calc R . . C7 C 0.63702(14) 0.8322(3) 0.14322(13) 0.0150(5) Uani 1 1 d . . . C8 C 0.64312(14) 0.7371(3) 0.21322(13) 0.0140(4) Uani 1 1 d . . . C9 C 0.51937(13) 0.3591(3) 0.11393(13) 0.0145(5) Uani 1 1 d . . . C10 C 0.47014(14) 0.2788(3) 0.06279(14) 0.0185(5) Uani 1 1 d . . . H10 H 0.4614 0.3146 0.0115 0.022 Uiso 1 1 calc R . . C11 C 0.43496(15) 0.1490(3) 0.08741(15) 0.0199(5) Uani 1 1 d . . . H11 H 0.3999 0.0969 0.0538 0.024 Uiso 1 1 calc R . . C12 C 0.45030(14) 0.0928(3) 0.16132(14) 0.0176(5) Uani 1 1 d . . . C13 C 0.40622(15) -0.0428(3) 0.19154(15) 0.0229(5) Uani 1 1 d . . . H13A H 0.4305 -0.1352 0.1703 0.028 Uiso 1 1 calc R . . H13B H 0.3509 -0.0387 0.1734 0.028 Uiso 1 1 calc R . . C14 C 0.40754(13) -0.0494(3) 0.28007(16) 0.0206(5) Uani 1 1 d . . . H14A H 0.3779 0.0364 0.3021 0.025 Uiso 1 1 calc R . . H14B H 0.3828 -0.1437 0.2985 0.025 Uiso 1 1 calc R . . C15 C 0.49354(13) -0.0429(3) 0.30548(15) 0.0186(5) Uani 1 1 d . . . H15A H 0.5238 -0.1229 0.2789 0.022 Uiso 1 1 calc R . . H15B H 0.4971 -0.0602 0.3622 0.022 Uiso 1 1 calc R . . C16 C 0.52905(14) 0.1107(3) 0.28554(12) 0.0173(5) Uani 1 1 d . . . H16A H 0.5130 0.1838 0.3259 0.021 Uiso 1 1 calc R . . H16B H 0.5873 0.1027 0.2871 0.021 Uiso 1 1 calc R . . C17 C 0.50494(13) 0.1701(3) 0.20741(14) 0.0148(5) Uani 1 1 d . . . C18 C 0.68174(14) 0.7110(3) 0.34619(13) 0.0147(5) Uani 1 1 d . . . C19 C 0.71699(14) 0.7956(3) 0.40560(13) 0.0175(5) Uani 1 1 d . . . H19 H 0.7332 0.8961 0.3962 0.021 Uiso 1 1 calc R . . C20 C 0.72786(14) 0.7315(3) 0.47756(14) 0.0195(5) Uani 1 1 d . . . H20 H 0.7518 0.7879 0.5181 0.023 Uiso 1 1 calc R . . C21 C 0.70389(13) 0.5845(3) 0.49112(13) 0.0166(5) Uani 1 1 d . . . C22 C 0.71814(16) 0.5123(3) 0.56977(14) 0.0227(5) Uani 1 1 d . . . H22A H 0.7107 0.5889 0.6109 0.027 Uiso 1 1 calc R . . H22B H 0.7735 0.4774 0.5724 0.027 Uiso 1 1 calc R . . C23 C 0.66362(15) 0.3801(3) 0.58603(15) 0.0227(5) Uani 1 1 d . . . H23A H 0.6821 0.3251 0.6326 0.027 Uiso 1 1 calc R . . H23B H 0.6095 0.4168 0.5962 0.027 Uiso 1 1 calc R . . C24 C 0.66335(16) 0.2756(3) 0.51597(14) 0.0227(5) Uani 1 1 d . . . H24A H 0.6304 0.1866 0.5275 0.027 Uiso 1 1 calc R . . H24B H 0.7178 0.2405 0.5056 0.027 Uiso 1 1 calc R . . C25 C 0.63131(15) 0.3549(3) 0.44402(14) 0.0172(5) Uani 1 1 d . . . H25A H 0.6417 0.2915 0.3979 0.021 Uiso 1 1 calc R . . H25B H 0.5734 0.3656 0.4493 0.021 Uiso 1 1 calc R . . C26 C 0.66692(14) 0.5080(3) 0.43077(13) 0.0156(5) Uani 1 1 d . . . C27 C 0.37958(16) 0.5975(3) 0.39352(14) 0.0249(6) Uani 1 1 d . . . H27A H 0.3724 0.5099 0.4273 0.037 Uiso 1 1 calc R . . H27B H 0.3280 0.6409 0.3811 0.037 Uiso 1 1 calc R . . H27C H 0.4120 0.6725 0.4203 0.037 Uiso 1 1 calc R . . C28 C 0.35677(13) 0.4071(3) 0.2743(2) 0.0262(5) Uani 1 1 d . . . H28A H 0.3764 0.3565 0.2275 0.039 Uiso 1 1 calc R . . H28B H 0.3070 0.4581 0.2623 0.039 Uiso 1 1 calc R . . H28C H 0.3480 0.3328 0.3154 0.039 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 0.01169(13) 0.01467(12) 0.01253(12) -0.00026(14) 0.00071(13) -0.00107(12) Cl1 0.0137(2) 0.0181(3) 0.0216(3) -0.0039(2) 0.0004(2) 0.0001(2) S1 0.0141(3) 0.0160(3) 0.0142(2) 0.0011(2) 0.0010(2) 0.0006(2) O1 0.0118(8) 0.0233(9) 0.0148(7) 0.0013(7) 0.0000(6) 0.0005(7) N1 0.0139(9) 0.0145(9) 0.0133(9) -0.0028(7) 0.0010(8) -0.0018(8) N2 0.0126(9) 0.0178(10) 0.0155(9) -0.0002(8) -0.0003(8) -0.0003(8) N3 0.0132(9) 0.0158(10) 0.0139(9) -0.0013(8) 0.0011(7) 0.0002(8) N4 0.0140(8) 0.0163(8) 0.0142(9) -0.0020(9) 0.0012(8) -0.0014(7) N5 0.0125(9) 0.0161(10) 0.0127(9) -0.0013(8) 0.0023(7) -0.0004(8) C1 0.0112(10) 0.0180(12) 0.0133(10) 0.0003(9) 0.0026(8) 0.0022(9) C2 0.0128(11) 0.0182(12) 0.0146(10) 0.0003(9) 0.0019(9) 0.0011(9) C3 0.0153(11) 0.0234(13) 0.0192(12) 0.0009(10) 0.0007(10) 0.0006(10) C4 0.0190(12) 0.0242(13) 0.0216(12) 0.0088(10) -0.0003(10) 0.0045(11) C5 0.0172(12) 0.0176(12) 0.0235(13) 0.0040(9) 0.0057(10) 0.0014(10) C6 0.0165(12) 0.0170(12) 0.0186(11) 0.0000(9) 0.0029(9) 0.0002(10) C7 0.0120(11) 0.0186(12) 0.0145(11) -0.0009(9) 0.0024(9) 0.0018(9) C8 0.0130(11) 0.0146(11) 0.0143(11) -0.0017(8) 0.0044(9) 0.0009(9) C9 0.0124(11) 0.0169(11) 0.0141(11) -0.0019(9) 0.0007(9) 0.0014(9) C10 0.0200(12) 0.0206(12) 0.0151(11) -0.0027(10) -0.0033(9) -0.0014(10) C11 0.0184(12) 0.0192(12) 0.0222(12) -0.0066(10) -0.0059(10) 0.0002(10) C12 0.0146(12) 0.0151(12) 0.0231(12) -0.0038(9) 0.0004(9) -0.0013(9) C13 0.0205(13) 0.0187(13) 0.0296(14) -0.0013(10) -0.0019(10) -0.0048(10) C14 0.0163(11) 0.0155(11) 0.0299(15) 0.0019(10) 0.0029(10) -0.0038(8) C15 0.0166(11) 0.0161(11) 0.0232(12) 0.0013(10) 0.0028(10) -0.0006(9) C16 0.0172(11) 0.0192(11) 0.0155(13) 0.0011(8) 0.0004(8) -0.0017(9) C17 0.0111(11) 0.0156(12) 0.0176(11) -0.0030(9) 0.0021(9) 0.0006(9) C18 0.0127(11) 0.0174(11) 0.0141(11) -0.0036(9) 0.0023(9) 0.0014(9) C19 0.0184(12) 0.0163(12) 0.0177(11) -0.0035(9) 0.0007(9) -0.0042(10) C20 0.0153(12) 0.0269(13) 0.0165(12) -0.0059(10) 0.0005(9) -0.0044(10) C21 0.0116(11) 0.0254(13) 0.0127(11) -0.0007(9) -0.0006(8) -0.0020(10) C22 0.0207(13) 0.0321(14) 0.0154(12) 0.0021(10) -0.0048(10) -0.0076(11) C23 0.0239(13) 0.0294(14) 0.0150(11) 0.0055(10) -0.0046(10) -0.0053(11) C24 0.0243(14) 0.0229(13) 0.0210(13) 0.0040(10) -0.0045(11) -0.0018(11) C25 0.0201(12) 0.0184(12) 0.0132(11) 0.0033(9) -0.0024(9) -0.0043(10) C26 0.0128(11) 0.0194(12) 0.0144(11) -0.0024(9) 0.0012(9) 0.0014(10) C27 0.0238(14) 0.0340(15) 0.0170(12) -0.0032(10) 0.0032(10) 0.0086(12) C28 0.0142(10) 0.0243(12) 0.0400(15) -0.0065(14) -0.0059(13) 0.0007(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 Co1 N1 1.941(2) . ? Co1 O1 2.1015(18) . ? Co1 N5 2.148(2) . ? Co1 N3 2.173(2) . ? Co1 Cl1 2.3327(11) . ? S1 O1 1.5213(18) . ? S1 C28 1.777(2) . ? S1 C27 1.780(3) . ? N1 C8 1.386(3) . ? N1 C1 1.387(3) . ? N2 C1 1.289(3) . ? N2 C9 1.391(3) . ? N3 C9 1.355(3) . ? N3 C17 1.364(3) . ? N4 C8 1.292(3) . ? N4 C18 1.392(3) . ? N5 C18 1.354(3) . ? N5 C26 1.359(3) . ? C1 C2 1.481(3) . ? C2 C3 1.389(3) . ? C2 C7 1.391(3) . ? C3 C4 1.395(4) . ? C3 H3 0.9500 . ? C4 C5 1.383(3) . ? C4 H4 0.9500 . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 C7 1.387(3) . ? C6 H6 0.9500 . ? C7 C8 1.476(3) . ? C9 C10 1.407(3) . ? C10 C11 1.368(3) . ? C10 H10 0.9500 . ? C11 C12 1.390(4) . ? C11 H11 0.9500 . ? C12 C17 1.400(3) . ? C12 C13 1.512(3) . ? C13 C14 1.524(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.523(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.533(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.501(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C18 C19 1.403(3) . ? C19 C20 1.375(3) . ? C19 H19 0.9500 . ? C20 C21 1.390(4) . ? C20 H20 0.9500 . ? C21 C26 1.391(3) . ? C21 C22 1.517(3) . ? C22 C23 1.523(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.522(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.525(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.508(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 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 N1 Co1 O1 106.28(8) . . ? N1 Co1 N5 89.97(8) . . ? O1 Co1 N5 86.02(7) . . ? N1 Co1 N3 89.55(8) . . ? O1 Co1 N3 87.39(7) . . ? N5 Co1 N3 172.98(7) . . ? N1 Co1 Cl1 111.54(6) . . ? O1 Co1 Cl1 142.13(5) . . ? N5 Co1 Cl1 91.94(6) . . ? N3 Co1 Cl1 94.75(6) . . ? O1 S1 C28 106.58(11) . . ? O1 S1 C27 104.05(11) . . ? C28 S1 C27 98.22(14) . . ? S1 O1 Co1 123.83(10) . . ? C8 N1 C1 108.33(19) . . ? C8 N1 Co1 125.27(16) . . ? C1 N1 Co1 126.10(15) . . ? C1 N2 C9 125.7(2) . . ? C9 N3 C17 118.7(2) . . ? C9 N3 Co1 122.35(16) . . ? C17 N3 Co1 118.56(16) . . ? C8 N4 C18 125.9(2) . . ? C18 N5 C26 118.7(2) . . ? C18 N5 Co1 123.08(15) . . ? C26 N5 Co1 118.14(16) . . ? N2 C1 N1 129.8(2) . . ? N2 C1 C2 121.3(2) . . ? N1 C1 C2 108.81(19) . . ? C3 C2 C7 121.1(2) . . ? C3 C2 C1 132.0(2) . . ? C7 C2 C1 106.9(2) . . ? C2 C3 C4 117.0(2) . . ? C2 C3 H3 121.5 . . ? C4 C3 H3 121.5 . . ? C5 C4 C3 121.5(2) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 121.7(2) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 116.6(2) . . ? C7 C6 H6 121.7 . . ? C5 C6 H6 121.7 . . ? C6 C7 C2 122.0(2) . . ? C6 C7 C8 131.1(2) . . ? C2 C7 C8 106.8(2) . . ? N4 C8 N1 130.1(2) . . ? N4 C8 C7 120.8(2) . . ? N1 C8 C7 109.1(2) . . ? N3 C9 N2 125.8(2) . . ? N3 C9 C10 120.9(2) . . ? N2 C9 C10 113.3(2) . . ? C11 C10 C9 119.6(2) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.3(2) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C17 117.7(2) . . ? C11 C12 C13 120.6(2) . . ? C17 C12 C13 121.7(2) . . ? C12 C13 C14 111.52(19) . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C15 C14 C13 107.4(2) . . ? C15 C14 H14A 110.2 . . ? C13 C14 H14A 110.2 . . ? C15 C14 H14B 110.2 . . ? C13 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? C14 C15 C16 110.23(19) . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? C17 C16 C15 114.06(19) . . ? C17 C16 H16A 108.7 . . ? C15 C16 H16A 108.7 . . ? C17 C16 H16B 108.7 . . ? C15 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N3 C17 C12 122.4(2) . . ? N3 C17 C16 116.7(2) . . ? C12 C17 C16 120.9(2) . . ? N5 C18 N4 125.2(2) . . ? N5 C18 C19 121.1(2) . . ? N4 C18 C19 113.7(2) . . ? C20 C19 C18 119.3(2) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 120.2(2) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C26 117.9(2) . . ? C20 C21 C22 120.1(2) . . ? C26 C21 C22 122.0(2) . . ? C21 C22 C23 113.3(2) . . ? C21 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? C21 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 109.2(2) . . ? C24 C23 H23A 109.8 . . ? C22 C23 H23A 109.8 . . ? C24 C23 H23B 109.8 . . ? C22 C23 H23B 109.8 . . ? H23A C23 H23B 108.3 . . ? C23 C24 C25 111.1(2) . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C26 C25 C24 113.5(2) . . ? C26 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? C26 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? N5 C26 C21 122.7(2) . . ? N5 C26 C25 116.5(2) . . ? C21 C26 C25 120.7(2) . . ? S1 C27 H27A 109.5 . . ? S1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C28 S1 O1 Co1 104.03(15) . . . . ? C27 S1 O1 Co1 -152.78(13) . . . . ? N1 Co1 O1 S1 22.19(13) . . . . ? N5 Co1 O1 S1 111.00(13) . . . . ? N3 Co1 O1 S1 -66.58(12) . . . . ? Cl1 Co1 O1 S1 -160.95(7) . . . . ? O1 Co1 N1 C8 93.51(19) . . . . ? N5 Co1 N1 C8 7.66(19) . . . . ? N3 Co1 N1 C8 -179.34(18) . . . . ? Cl1 Co1 N1 C8 -84.41(18) . . . . ? O1 Co1 N1 C1 -93.47(19) . . . . ? N5 Co1 N1 C1 -179.32(18) . . . . ? N3 Co1 N1 C1 -6.33(19) . . . . ? Cl1 Co1 N1 C1 88.60(18) . . . . ? N1 Co1 N3 C9 2.72(18) . . . . ? O1 Co1 N3 C9 109.04(18) . . . . ? N5 Co1 N3 C9 88.8(6) . . . . ? Cl1 Co1 N3 C9 -108.86(17) . . . . ? N1 Co1 N3 C17 -170.17(17) . . . . ? O1 Co1 N3 C17 -63.85(16) . . . . ? N5 Co1 N3 C17 -84.1(6) . . . . ? Cl1 Co1 N3 C17 78.25(16) . . . . ? N1 Co1 N5 C18 -5.43(19) . . . . ? O1 Co1 N5 C18 -111.76(18) . . . . ? N3 Co1 N5 C18 -91.5(6) . . . . ? Cl1 Co1 N5 C18 106.12(17) . . . . ? N1 Co1 N5 C26 176.80(17) . . . . ? O1 Co1 N5 C26 70.48(17) . . . . ? N3 Co1 N5 C26 90.7(6) . . . . ? Cl1 Co1 N5 C26 -71.65(16) . . . . ? C9 N2 C1 N1 4.5(4) . . . . ? C9 N2 C1 C2 -174.8(2) . . . . ? C8 N1 C1 N2 178.3(2) . . . . ? Co1 N1 C1 N2 4.3(4) . . . . ? C8 N1 C1 C2 -2.3(2) . . . . ? Co1 N1 C1 C2 -176.31(15) . . . . ? N2 C1 C2 C3 3.1(4) . . . . ? N1 C1 C2 C3 -176.4(2) . . . . ? N2 C1 C2 C7 -178.8(2) . . . . ? N1 C1 C2 C7 1.8(3) . . . . ? C7 C2 C3 C4 0.2(3) . . . . ? C1 C2 C3 C4 178.2(2) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? C4 C5 C6 C7 0.4(4) . . . . ? C5 C6 C7 C2 -0.7(3) . . . . ? C5 C6 C7 C8 -177.5(2) . . . . ? C3 C2 C7 C6 0.4(4) . . . . ? C1 C2 C7 C6 -178.0(2) . . . . ? C3 C2 C7 C8 177.9(2) . . . . ? C1 C2 C7 C8 -0.5(2) . . . . ? C18 N4 C8 N1 -1.6(4) . . . . ? C18 N4 C8 C7 176.1(2) . . . . ? C1 N1 C8 N4 179.9(2) . . . . ? Co1 N1 C8 N4 -6.0(3) . . . . ? C1 N1 C8 C7 2.0(2) . . . . ? Co1 N1 C8 C7 176.04(15) . . . . ? C6 C7 C8 N4 -1.9(4) . . . . ? C2 C7 C8 N4 -179.0(2) . . . . ? C6 C7 C8 N1 176.3(2) . . . . ? C2 C7 C8 N1 -0.8(3) . . . . ? C17 N3 C9 N2 176.5(2) . . . . ? Co1 N3 C9 N2 3.6(3) . . . . ? C17 N3 C9 C10 -1.5(3) . . . . ? Co1 N3 C9 C10 -174.34(17) . . . . ? C1 N2 C9 N3 -8.6(4) . . . . ? C1 N2 C9 C10 169.5(2) . . . . ? N3 C9 C10 C11 5.0(3) . . . . ? N2 C9 C10 C11 -173.3(2) . . . . ? C9 C10 C11 C12 -2.8(4) . . . . ? C10 C11 C12 C17 -2.6(3) . . . . ? C10 C11 C12 C13 174.6(2) . . . . ? C11 C12 C13 C14 -158.2(2) . . . . ? C17 C12 C13 C14 18.9(3) . . . . ? C12 C13 C14 C15 -54.6(3) . . . . ? C13 C14 C15 C16 66.6(2) . . . . ? C14 C15 C16 C17 -41.2(3) . . . . ? C9 N3 C17 C12 -4.2(3) . . . . ? Co1 N3 C17 C12 168.91(17) . . . . ? C9 N3 C17 C16 177.6(2) . . . . ? Co1 N3 C17 C16 -9.3(3) . . . . ? C11 C12 C17 N3 6.3(3) . . . . ? C13 C12 C17 N3 -170.9(2) . . . . ? C11 C12 C17 C16 -175.6(2) . . . . ? C13 C12 C17 C16 7.3(3) . . . . ? C15 C16 C17 N3 -177.57(19) . . . . ? C15 C16 C17 C12 4.2(3) . . . . ? C26 N5 C18 N4 178.6(2) . . . . ? Co1 N5 C18 N4 0.8(3) . . . . ? C26 N5 C18 C19 -1.1(3) . . . . ? Co1 N5 C18 C19 -178.81(17) . . . . ? C8 N4 C18 N5 4.2(4) . . . . ? C8 N4 C18 C19 -176.2(2) . . . . ? N5 C18 C19 C20 1.7(4) . . . . ? N4 C18 C19 C20 -177.9(2) . . . . ? C18 C19 C20 C21 -0.2(4) . . . . ? C19 C20 C21 C26 -1.9(4) . . . . ? C19 C20 C21 C22 178.1(2) . . . . ? C20 C21 C22 C23 158.3(2) . . . . ? C26 C21 C22 C23 -21.7(3) . . . . ? C21 C22 C23 C24 48.3(3) . . . . ? C22 C23 C24 C25 -62.3(3) . . . . ? C23 C24 C25 C26 47.5(3) . . . . ? C18 N5 C26 C21 -1.2(3) . . . . ? Co1 N5 C26 C21 176.67(18) . . . . ? C18 N5 C26 C25 174.8(2) . . . . ? Co1 N5 C26 C25 -7.4(3) . . . . ? C20 C21 C26 N5 2.7(3) . . . . ? C22 C21 C26 N5 -177.4(2) . . . . ? C20 C21 C26 C25 -173.1(2) . . . . ? C22 C21 C26 C25 6.8(3) . . . . ? C24 C25 C26 N5 164.3(2) . . . . ? C24 C25 C26 C21 -19.7(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.495 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.072 _diffrn_ambient_environment 'perfluoro polyether oil' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_specimen_support 'polyimid foil' _diffrn_detector 'CCD plate' _diffrn_detector_type CCD-PXL-KAF2 #==end== data_complex_3b _database_code_depnum_ccdc_archive 'CCDC 821502' #TrackingRef '- ga_mkr12-ga_mkr20-ga_ds12-ga_mkr14-ga_ds17.cif' _audit_creation_method SHELXL-97 _audit_block_code ga_mkr14 _audit_block_refno 957 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 Cl Fe N5 O2 S2' _chemical_melting_point ? _exptl_crystal_description irregular _exptl_crystal_colour yellow _diffrn_ambient_temperature 100(2) _chemical_formula_weight 654.06 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration . loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.838(4) _cell_length_b 16.324(7) _cell_length_c 20.602(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.207(16) _cell_angle_gamma 90.00 _cell_volume 2972(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8049 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 32.03 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 -1.00 0.00 0.0560 0.00 1.00 0.00 0.0250 0.00 0.00 -1.00 0.1670 0.00 0.00 1.00 0.1360 1.00 0.00 0.00 0.0850 -1.00 0.00 0.00 0.0030 _exptl_absorpt_coefficient_mu 0.776 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8147 _exptl_absorpt_correction_T_max 0.9791 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) SADABS (Sheldrick & Bruker AXS, 2004-2008) ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Smart 1000' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean 8.19 _diffrn_reflns_number 75048 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 32.25 _reflns_number_total 10075 _reflns_number_gt 8279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-5.631 (Bruker AXS, 2003)' _computing_cell_refinement ; SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors of the unit cell constants from Monte Carlo simulations. ; _computing_data_reduction 'SAINT (Bruker AXS, 1997-2008); SADABS (Bruker AXS, 2008)' _computing_structure_solution 'SUPERFLIP (Palatinus, 2007-2009)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0458P)^2^+1.7711P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10075 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Fe1 Fe 0.77933(2) 0.306060(11) 0.286262(9) 0.01128(5) Uani 1 1 d . . . Cl1 Cl 0.57908(4) 0.28162(2) 0.357743(16) 0.01762(7) Uani 1 1 d . . . S1 S 1.12489(4) 0.33224(2) 0.23973(2) 0.02130(8) Uani 1 1 d . . . O1 O 0.97951(11) 0.37302(6) 0.26194(5) 0.01754(19) Uani 1 1 d . . . N1 N 0.76453(13) 0.23966(7) 0.20517(5) 0.0136(2) Uani 1 1 d . . . N2 N 0.60052(13) 0.32560(7) 0.13963(6) 0.0150(2) Uani 1 1 d . . . N3 N 0.66767(12) 0.40566(7) 0.23571(5) 0.01211(19) Uani 1 1 d . . . N4 N 0.89890(13) 0.11657(7) 0.23748(6) 0.0160(2) Uani 1 1 d . . . N5 N 0.93150(13) 0.21441(7) 0.32622(6) 0.0137(2) Uani 1 1 d . . . C1 C 0.67693(15) 0.25941(8) 0.15213(6) 0.0139(2) Uani 1 1 d . . . C2 C 0.67840(16) 0.18955(8) 0.10600(6) 0.0157(2) Uani 1 1 d . . . C7 C 0.76686(16) 0.12854(9) 0.13448(7) 0.0165(2) Uani 1 1 d . . . C8 C 0.81804(15) 0.16070(8) 0.19822(6) 0.0144(2) Uani 1 1 d . . . C3 C 0.61161(18) 0.17831(9) 0.04556(7) 0.0198(3) Uani 1 1 d . . . H3 H 0.5512 0.2199 0.0262 0.024 Uiso 1 1 calc R . . C4 C 0.63646(19) 0.10374(10) 0.01420(7) 0.0233(3) Uani 1 1 d . . . H4 H 0.5921 0.0942 -0.0272 0.028 Uiso 1 1 calc R . . C5 C 0.7255(2) 0.04290(10) 0.04282(8) 0.0251(3) Uani 1 1 d . . . H5 H 0.7404 -0.0075 0.0206 0.030 Uiso 1 1 calc R . . C6 C 0.79294(18) 0.05477(9) 0.10332(7) 0.0220(3) Uani 1 1 d . . . H6 H 0.8546 0.0137 0.1225 0.026 Uiso 1 1 calc R . . C9 C 0.59748(14) 0.39650(8) 0.17764(6) 0.0134(2) Uani 1 1 d . . . C10 C 0.51239(16) 0.46102(9) 0.15081(7) 0.0165(2) Uani 1 1 d . . . H10 H 0.4586 0.4532 0.1113 0.020 Uiso 1 1 calc R . . C11 C 0.50737(16) 0.53551(9) 0.18204(7) 0.0173(3) Uani 1 1 d . . . H11 H 0.4494 0.5791 0.1642 0.021 Uiso 1 1 calc R . . C12 C 0.58733(15) 0.54711(8) 0.23992(6) 0.0146(2) Uani 1 1 d . . . C17 C 0.66251(14) 0.47962(8) 0.26599(6) 0.0124(2) Uani 1 1 d . . . C13 C 0.59072(17) 0.63045(9) 0.27149(7) 0.0197(3) Uani 1 1 d . . . H13A H 0.4882 0.6434 0.2877 0.024 Uiso 1 1 calc R . . H13B H 0.6168 0.6718 0.2382 0.024 Uiso 1 1 calc R . . C14 C 0.70287(17) 0.63747(9) 0.32760(7) 0.0190(3) Uani 1 1 d . . . H14A H 0.8064 0.6448 0.3103 0.023 Uiso 1 1 calc R . . H14B H 0.6778 0.6860 0.3543 0.023 Uiso 1 1 calc R . . C15 C 0.69708(18) 0.56058(9) 0.36943(7) 0.0190(3) Uani 1 1 d . . . H15A H 0.5929 0.5523 0.3856 0.023 Uiso 1 1 calc R . . H15B H 0.7651 0.5671 0.4074 0.023 Uiso 1 1 calc R . . C16 C 0.74590(16) 0.48613(8) 0.32981(6) 0.0155(2) Uani 1 1 d . . . H16A H 0.8559 0.4897 0.3213 0.019 Uiso 1 1 calc R . . H16B H 0.7276 0.4359 0.3555 0.019 Uiso 1 1 calc R . . C18 C 0.96064(15) 0.14216(8) 0.29642(6) 0.0139(2) Uani 1 1 d . . . C19 C 1.06454(16) 0.08656(9) 0.32350(7) 0.0169(2) Uani 1 1 d . . . H19 H 1.0776 0.0339 0.3046 0.020 Uiso 1 1 calc R . . C20 C 1.14710(16) 0.10860(9) 0.37732(7) 0.0192(3) Uani 1 1 d . A . H20 H 1.2203 0.0719 0.3947 0.023 Uiso 1 1 calc R . . C21 C 1.12397(15) 0.18476(9) 0.40674(7) 0.0162(2) Uani 1 1 d . . . C26 C 1.00999(15) 0.23414(8) 0.38120(6) 0.0140(2) Uani 1 1 d . A . C22A C 1.22175(18) 0.21146(10) 0.46330(8) 0.0229(3) Uani 0.257(5) 1 d P A 1 H22A H 1.3187 0.2332 0.4467 0.028 Uiso 0.257(5) 1 calc PR A 1 H22B H 1.2447 0.1634 0.4909 0.028 Uiso 0.257(5) 1 calc PR A 1 C22B C 1.22175(18) 0.21146(10) 0.46330(8) 0.0229(3) Uani 0.743(5) 1 d P A 2 H22C H 1.3285 0.1973 0.4541 0.028 Uiso 0.743(5) 1 calc PR A 2 H22D H 1.1908 0.1811 0.5027 0.028 Uiso 0.743(5) 1 calc PR A 2 C23A C 1.1434(7) 0.2777(4) 0.5046(3) 0.0236(16) Uani 0.257(5) 1 d P A 1 H23A H 1.0554 0.2541 0.5276 0.028 Uiso 0.257(5) 1 calc PR A 1 H23B H 1.2147 0.3001 0.5372 0.028 Uiso 0.257(5) 1 calc PR A 1 C23B C 1.2100(2) 0.30427(14) 0.47661(11) 0.0223(5) Uani 0.743(5) 1 d P A 2 H23C H 1.2606 0.3177 0.5182 0.027 Uiso 0.743(5) 1 calc PR A 2 H23D H 1.2607 0.3352 0.4416 0.027 Uiso 0.743(5) 1 calc PR A 2 C24A C 1.0926(10) 0.3440(4) 0.4590(4) 0.0229(15) Uani 0.257(5) 1 d P A 1 H24A H 1.1800 0.3629 0.4330 0.027 Uiso 0.257(5) 1 calc PR A 1 H24B H 1.0550 0.3912 0.4844 0.027 Uiso 0.257(5) 1 calc PR A 1 C24B C 1.0427(3) 0.32805(18) 0.47972(13) 0.0223(5) Uani 0.743(5) 1 d P A 2 H24C H 1.0333 0.3864 0.4922 0.027 Uiso 0.743(5) 1 calc PR A 2 H24D H 0.9911 0.2946 0.5130 0.027 Uiso 0.743(5) 1 calc PR A 2 C25A C 0.96773(17) 0.31413(9) 0.41341(7) 0.0184(3) Uani 0.257(5) 1 d P A 1 H25A H 0.8731 0.3066 0.4383 0.022 Uiso 0.257(5) 1 calc PR A 1 H25B H 0.9488 0.3561 0.3797 0.022 Uiso 0.257(5) 1 calc PR A 1 C25B C 0.96773(17) 0.31413(9) 0.41341(7) 0.0184(3) Uani 0.743(5) 1 d P A 2 H25C H 0.8565 0.3157 0.4189 0.022 Uiso 0.743(5) 1 calc PR A 2 H25D H 0.9960 0.3598 0.3842 0.022 Uiso 0.743(5) 1 calc PR A 2 C27 C 1.1526(2) 0.36508(13) 0.15870(8) 0.0338(4) Uani 1 1 d . . . H27A H 1.0755 0.3403 0.1306 0.051 Uiso 1 1 calc R . . H27B H 1.2533 0.3483 0.1441 0.051 Uiso 1 1 calc R . . H27C H 1.1443 0.4249 0.1566 0.051 Uiso 1 1 calc R . . C28 C 1.27033(19) 0.39179(17) 0.27740(9) 0.0415(5) Uani 1 1 d . . . H28A H 1.2549 0.4498 0.2672 0.062 Uiso 1 1 calc R . . H28B H 1.3692 0.3742 0.2611 0.062 Uiso 1 1 calc R . . H28C H 1.2667 0.3840 0.3245 0.062 Uiso 1 1 calc R . . S2A S 0.22962(6) 0.55914(3) 0.04099(3) 0.01943(15) Uani 0.6729(15) 1 d P B 3 O2A O 0.2516(2) 0.47201(11) 0.02018(11) 0.0258(4) Uani 0.6729(15) 1 d P B 3 C31A C 0.40372(18) 0.61060(9) 0.02380(7) 0.0224(3) Uani 0.6729(15) 1 d P B 3 H31D H 0.4887 0.5772 0.0392 0.034 Uiso 0.6729(15) 1 calc PR B 3 H31E H 0.4051 0.6638 0.0459 0.034 Uiso 0.6729(15) 1 calc PR B 3 H31F H 0.4127 0.6190 -0.0231 0.034 Uiso 0.6729(15) 1 calc PR B 3 C32A C 0.1224(2) 0.60522(12) -0.02333(10) 0.0341(4) Uani 0.6729(15) 1 d P B 3 H32D H 0.1727 0.5950 -0.0649 0.051 Uiso 0.6729(15) 1 calc PR B 3 H32E H 0.1152 0.6644 -0.0160 0.051 Uiso 0.6729(15) 1 calc PR B 3 H32F H 0.0205 0.5815 -0.0244 0.051 Uiso 0.6729(15) 1 calc PR B 3 S2B S 0.27276(12) 0.53223(7) -0.00428(5) 0.0191(3) Uani 0.3271(15) 1 d P B 4 O2B O 0.2195(5) 0.4873(3) 0.0540(3) 0.0355(11) Uani 0.3271(15) 1 d P B 4 C31B C 0.40372(18) 0.61060(9) 0.02380(7) 0.0224(3) Uani 0.3271(15) 1 d P B 4 H31A H 0.4069 0.6105 0.0714 0.034 Uiso 0.3271(15) 1 calc PR B 4 H31B H 0.3699 0.6644 0.0083 0.034 Uiso 0.3271(15) 1 calc PR B 4 H31C H 0.5050 0.5991 0.0068 0.034 Uiso 0.3271(15) 1 calc PR B 4 C32B C 0.1224(2) 0.60522(12) -0.02333(10) 0.0341(4) Uani 0.3271(15) 1 d P B 4 H32A H 0.0567 0.6118 0.0145 0.051 Uiso 0.3271(15) 1 calc PR B 4 H32B H 0.0626 0.5848 -0.0601 0.051 Uiso 0.3271(15) 1 calc PR B 4 H32C H 0.1671 0.6582 -0.0347 0.051 Uiso 0.3271(15) 1 calc PR B 4 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 Fe1 0.01162(9) 0.01149(9) 0.01071(8) 0.00018(6) -0.00089(6) 0.00044(6) Cl1 0.01751(15) 0.02029(15) 0.01507(14) 0.00194(11) 0.00260(11) -0.00177(11) S1 0.01867(16) 0.01756(16) 0.02773(19) 0.00371(13) 0.00815(14) 0.00338(12) O1 0.0113(4) 0.0146(4) 0.0267(5) -0.0002(4) 0.0016(4) 0.0008(3) N1 0.0142(5) 0.0143(5) 0.0123(5) 0.0000(4) -0.0009(4) 0.0002(4) N2 0.0171(5) 0.0156(5) 0.0123(5) 0.0007(4) -0.0008(4) -0.0028(4) N3 0.0113(5) 0.0135(5) 0.0115(5) 0.0009(4) -0.0002(4) 0.0000(4) N4 0.0172(5) 0.0152(5) 0.0155(5) -0.0022(4) -0.0002(4) 0.0005(4) N5 0.0138(5) 0.0133(5) 0.0139(5) -0.0002(4) -0.0010(4) 0.0016(4) C1 0.0150(6) 0.0164(6) 0.0102(5) -0.0005(4) 0.0011(4) -0.0045(5) C2 0.0188(6) 0.0161(6) 0.0121(5) -0.0011(4) 0.0010(5) -0.0044(5) C7 0.0197(6) 0.0171(6) 0.0127(6) -0.0029(5) 0.0011(5) -0.0026(5) C8 0.0157(6) 0.0138(6) 0.0137(6) -0.0022(4) 0.0016(4) -0.0011(4) C3 0.0258(7) 0.0208(7) 0.0126(6) -0.0001(5) -0.0016(5) -0.0069(5) C4 0.0320(8) 0.0242(7) 0.0137(6) -0.0039(5) 0.0003(5) -0.0090(6) C5 0.0342(8) 0.0223(7) 0.0188(7) -0.0081(5) 0.0028(6) -0.0036(6) C6 0.0266(7) 0.0195(7) 0.0199(7) -0.0058(5) 0.0010(6) -0.0002(5) C9 0.0118(5) 0.0160(6) 0.0122(5) 0.0023(4) 0.0000(4) -0.0011(4) C10 0.0157(6) 0.0205(6) 0.0134(6) 0.0038(5) -0.0019(5) 0.0017(5) C11 0.0160(6) 0.0199(6) 0.0160(6) 0.0039(5) -0.0012(5) 0.0054(5) C12 0.0137(6) 0.0157(6) 0.0143(6) 0.0018(4) 0.0020(4) 0.0033(4) C17 0.0113(5) 0.0135(5) 0.0123(5) 0.0012(4) 0.0009(4) 0.0011(4) C13 0.0244(7) 0.0151(6) 0.0195(6) 0.0004(5) -0.0001(5) 0.0074(5) C14 0.0252(7) 0.0137(6) 0.0180(6) -0.0005(5) 0.0011(5) 0.0017(5) C15 0.0282(7) 0.0145(6) 0.0144(6) -0.0009(5) 0.0008(5) 0.0035(5) C16 0.0194(6) 0.0138(6) 0.0133(6) -0.0013(4) -0.0032(5) 0.0028(5) C18 0.0137(6) 0.0138(5) 0.0143(6) 0.0012(4) 0.0019(4) 0.0007(4) C19 0.0178(6) 0.0149(6) 0.0181(6) 0.0008(5) 0.0023(5) 0.0047(5) C20 0.0182(6) 0.0199(6) 0.0196(6) 0.0019(5) -0.0007(5) 0.0074(5) C21 0.0146(6) 0.0184(6) 0.0156(6) 0.0018(5) -0.0009(5) 0.0039(5) C26 0.0129(6) 0.0149(6) 0.0142(6) 0.0011(4) -0.0011(4) 0.0016(4) C22A 0.0213(7) 0.0261(7) 0.0214(7) -0.0019(6) -0.0085(5) 0.0080(6) C22B 0.0213(7) 0.0261(7) 0.0214(7) -0.0019(6) -0.0085(5) 0.0080(6) C23A 0.028(3) 0.024(3) 0.019(3) -0.001(2) -0.013(2) 0.003(2) C23B 0.0189(10) 0.0260(11) 0.0220(10) -0.0046(8) -0.0069(8) 0.0030(8) C24A 0.025(4) 0.022(3) 0.022(4) -0.006(3) -0.008(3) 0.002(3) C24B 0.0200(12) 0.0287(12) 0.0182(11) -0.0074(9) -0.0046(9) 0.0066(9) C25A 0.0199(6) 0.0177(6) 0.0175(6) -0.0040(5) -0.0067(5) 0.0061(5) C25B 0.0199(6) 0.0177(6) 0.0175(6) -0.0040(5) -0.0067(5) 0.0061(5) C27 0.0311(9) 0.0518(11) 0.0185(7) -0.0025(7) -0.0001(6) -0.0095(8) C28 0.0156(7) 0.0889(17) 0.0201(8) 0.0040(9) -0.0019(6) -0.0096(9) S2A 0.0215(3) 0.0221(3) 0.0147(2) 0.00216(18) 0.00137(18) -0.00199(19) O2A 0.0272(10) 0.0185(8) 0.0315(10) 0.0022(8) -0.0092(8) -0.0033(7) C31A 0.0274(7) 0.0204(7) 0.0194(7) 0.0028(5) -0.0035(6) -0.0061(6) C32A 0.0205(8) 0.0408(10) 0.0410(10) 0.0196(8) -0.0011(7) 0.0044(7) S2B 0.0149(5) 0.0223(5) 0.0200(5) 0.0019(4) -0.0032(4) -0.0023(4) O2B 0.027(2) 0.042(3) 0.037(2) 0.027(2) -0.0107(19) -0.0121(18) C31B 0.0274(7) 0.0204(7) 0.0194(7) 0.0028(5) -0.0035(6) -0.0061(6) C32B 0.0205(8) 0.0408(10) 0.0410(10) 0.0196(8) -0.0011(7) 0.0044(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 Fe1 N1 1.9955(13) . ? Fe1 O1 2.1405(12) . ? Fe1 N3 2.1667(13) . ? Fe1 N5 2.1718(13) . ? Fe1 Cl1 2.3407(9) . ? S1 O1 1.5190(12) . ? S1 C27 1.7713(19) . ? S1 C28 1.787(2) . ? N1 C1 1.3752(17) . ? N1 C8 1.3806(18) . ? N2 C1 1.2994(18) . ? N2 C9 1.3977(18) . ? N3 C9 1.3539(17) . ? N3 C17 1.3599(17) . ? N4 C8 1.2961(18) . ? N4 C18 1.3935(18) . ? N5 C18 1.3548(17) . ? N5 C26 1.3646(17) . ? C1 C2 1.4846(19) . ? C2 C3 1.388(2) . ? C2 C7 1.394(2) . ? C7 C6 1.384(2) . ? C7 C8 1.4832(19) . ? C3 C4 1.396(2) . ? C3 H3 0.9500 . ? C4 C5 1.397(2) . ? C4 H4 0.9500 . ? C5 C6 1.393(2) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C9 C10 1.4061(19) . ? C10 C11 1.376(2) . ? C10 H10 0.9500 . ? C11 C12 1.397(2) . ? C11 H11 0.9500 . ? C12 C17 1.3932(18) . ? C12 C13 1.508(2) . ? C17 C16 1.5086(19) . ? C13 C14 1.524(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.524(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.5271(19) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C18 C19 1.4051(19) . ? C19 C20 1.373(2) . ? C19 H19 0.9500 . ? C20 C21 1.398(2) . ? C20 H20 0.9500 . ? C21 C26 1.3919(18) . ? C21 C22A 1.512(2) . ? C26 C25A 1.512(2) . ? C22A C23A 1.542(6) . ? C22A H22A 0.9900 . ? C22A H22B 0.9900 . ? C23A C24A 1.500(10) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C23B C24B 1.530(4) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C24A C25A 1.527(7) . ? C24A H24A 0.9900 . ? C24A H24B 0.9900 . ? C24B H24C 0.9900 . ? C24B H24D 0.9900 . ? C25A H25A 0.9900 . ? C25A H25B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? S2A O2A 1.498(2) . ? S2A C31A 1.7895(18) . ? S2A C32A 1.7921(19) . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? S2B O2B 1.484(4) . ? 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 N1 Fe1 O1 97.65(5) . . ? N1 Fe1 N3 88.67(5) . . ? O1 Fe1 N3 83.09(5) . . ? N1 Fe1 N5 88.96(5) . . ? O1 Fe1 N5 85.95(5) . . ? N3 Fe1 N5 168.37(4) . . ? N1 Fe1 Cl1 112.75(4) . . ? O1 Fe1 Cl1 149.51(3) . . ? N3 Fe1 Cl1 94.95(4) . . ? N5 Fe1 Cl1 96.47(4) . . ? O1 S1 C27 105.74(8) . . ? O1 S1 C28 103.81(9) . . ? C27 S1 C28 98.22(9) . . ? S1 O1 Fe1 123.19(7) . . ? C1 N1 C8 109.18(11) . . ? C1 N1 Fe1 124.95(9) . . ? C8 N1 Fe1 124.93(9) . . ? C1 N2 C9 126.05(12) . . ? C9 N3 C17 119.17(11) . . ? C9 N3 Fe1 123.25(9) . . ? C17 N3 Fe1 117.49(9) . . ? C8 N4 C18 126.20(12) . . ? C18 N5 C26 119.00(12) . . ? C18 N5 Fe1 123.12(9) . . ? C26 N5 Fe1 117.66(9) . . ? N2 C1 N1 130.03(12) . . ? N2 C1 C2 121.17(12) . . ? N1 C1 C2 108.80(12) . . ? C3 C2 C7 121.27(13) . . ? C3 C2 C1 132.14(13) . . ? C7 C2 C1 106.59(12) . . ? C6 C7 C2 121.35(13) . . ? C6 C7 C8 131.89(14) . . ? C2 C7 C8 106.77(12) . . ? N4 C8 N1 129.98(12) . . ? N4 C8 C7 121.44(13) . . ? N1 C8 C7 108.59(11) . . ? C2 C3 C4 117.60(14) . . ? C2 C3 H3 121.2 . . ? C4 C3 H3 121.2 . . ? C3 C4 C5 120.94(14) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 121.15(14) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C7 C6 C5 117.68(15) . . ? C7 C6 H6 121.2 . . ? C5 C6 H6 121.2 . . ? N3 C9 N2 125.23(12) . . ? N3 C9 C10 120.48(12) . . ? N2 C9 C10 114.29(12) . . ? C11 C10 C9 119.74(13) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 120.11(13) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C17 C12 C11 117.45(13) . . ? C17 C12 C13 122.57(12) . . ? C11 C12 C13 119.98(12) . . ? N3 C17 C12 122.81(12) . . ? N3 C17 C16 116.44(11) . . ? C12 C17 C16 120.74(12) . . ? C12 C13 C14 114.00(12) . . ? C12 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? C12 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C13 110.12(12) . . ? C15 C14 H14A 109.6 . . ? C13 C14 H14A 109.6 . . ? C15 C14 H14B 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.2 . . ? C14 C15 C16 110.07(12) . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C15 112.57(11) . . ? C17 C16 H16A 109.1 . . ? C15 C16 H16A 109.1 . . ? C17 C16 H16B 109.1 . . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N5 C18 N4 125.55(12) . . ? N5 C18 C19 120.49(13) . . ? N4 C18 C19 113.93(12) . . ? C20 C19 C18 119.73(13) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.32(13) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C26 C21 C20 117.25(13) . . ? C26 C21 C22A 122.34(13) . . ? C20 C21 C22A 120.40(12) . . ? N5 C26 C21 122.82(13) . . ? N5 C26 C25A 116.26(11) . . ? C21 C26 C25A 120.92(12) . . ? C21 C22A C23A 111.7(2) . . ? C21 C22A H22A 109.3 . . ? C23A C22A H22A 109.3 . . ? C21 C22A H22B 109.3 . . ? C23A C22A H22B 109.3 . . ? H22A C22A H22B 107.9 . . ? C24A C23A C22A 107.2(5) . . ? C24A C23A H23A 110.3 . . ? C22A C23A H23A 110.3 . . ? C24A C23A H23B 110.3 . . ? C22A C23A H23B 110.3 . . ? H23A C23A H23B 108.5 . . ? C24B C23B H23C 109.9 . . ? C24B C23B H23D 109.9 . . ? H23C C23B H23D 108.3 . . ? C23A C24A C25A 111.6(6) . . ? C23A C24A H24A 109.3 . . ? C25A C24A H24A 109.3 . . ? C23A C24A H24B 109.3 . . ? C25A C24A H24B 109.3 . . ? H24A C24A H24B 108.0 . . ? C23B C24B H24C 109.7 . . ? C23B C24B H24D 109.7 . . ? H24C C24B H24D 108.2 . . ? C26 C25A C24A 111.5(3) . . ? C26 C25A H25A 109.3 . . ? C24A C25A H25A 109.3 . . ? C26 C25A H25B 109.3 . . ? C24A C25A H25B 109.3 . . ? H25A C25A H25B 108.0 . . ? S1 C27 H27A 109.5 . . ? S1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O2A S2A C31A 106.06(10) . . ? O2A S2A C32A 104.80(11) . . ? C31A S2A C32A 96.28(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C27 S1 O1 Fe1 115.27(9) . . . . ? C28 S1 O1 Fe1 -141.89(9) . . . . ? N1 Fe1 O1 S1 -52.04(8) . . . . ? N3 Fe1 O1 S1 -139.75(8) . . . . ? N5 Fe1 O1 S1 36.36(8) . . . . ? Cl1 Fe1 O1 S1 132.22(6) . . . . ? O1 Fe1 N1 C1 -95.75(11) . . . . ? N3 Fe1 N1 C1 -12.91(11) . . . . ? N5 Fe1 N1 C1 178.48(11) . . . . ? Cl1 Fe1 N1 C1 81.90(11) . . . . ? O1 Fe1 N1 C8 96.54(11) . . . . ? N3 Fe1 N1 C8 179.39(11) . . . . ? N5 Fe1 N1 C8 10.77(11) . . . . ? Cl1 Fe1 N1 C8 -85.80(11) . . . . ? N1 Fe1 N3 C9 12.72(10) . . . . ? O1 Fe1 N3 C9 110.59(11) . . . . ? N5 Fe1 N3 C9 91.0(2) . . . . ? Cl1 Fe1 N3 C9 -100.01(10) . . . . ? N1 Fe1 N3 C17 -170.61(10) . . . . ? O1 Fe1 N3 C17 -72.74(10) . . . . ? N5 Fe1 N3 C17 -92.3(2) . . . . ? Cl1 Fe1 N3 C17 76.67(9) . . . . ? N1 Fe1 N5 C18 -7.41(11) . . . . ? O1 Fe1 N5 C18 -105.16(11) . . . . ? N3 Fe1 N5 C18 -85.7(2) . . . . ? Cl1 Fe1 N5 C18 105.37(11) . . . . ? N1 Fe1 N5 C26 167.10(10) . . . . ? O1 Fe1 N5 C26 69.35(10) . . . . ? N3 Fe1 N5 C26 88.9(2) . . . . ? Cl1 Fe1 N5 C26 -80.12(10) . . . . ? C9 N2 C1 N1 4.0(2) . . . . ? C9 N2 C1 C2 -176.34(12) . . . . ? C8 N1 C1 N2 177.22(14) . . . . ? Fe1 N1 C1 N2 7.9(2) . . . . ? C8 N1 C1 C2 -2.43(15) . . . . ? Fe1 N1 C1 C2 -171.78(9) . . . . ? N2 C1 C2 C3 1.5(2) . . . . ? N1 C1 C2 C3 -178.84(15) . . . . ? N2 C1 C2 C7 -178.61(12) . . . . ? N1 C1 C2 C7 1.08(15) . . . . ? C3 C2 C7 C6 0.7(2) . . . . ? C1 C2 C7 C6 -179.21(13) . . . . ? C3 C2 C7 C8 -179.48(13) . . . . ? C1 C2 C7 C8 0.59(15) . . . . ? C18 N4 C8 N1 -4.6(2) . . . . ? C18 N4 C8 C7 175.78(13) . . . . ? C1 N1 C8 N4 -176.90(14) . . . . ? Fe1 N1 C8 N4 -7.5(2) . . . . ? C1 N1 C8 C7 2.80(15) . . . . ? Fe1 N1 C8 C7 172.15(9) . . . . ? C6 C7 C8 N4 -2.6(2) . . . . ? C2 C7 C8 N4 177.65(13) . . . . ? C6 C7 C8 N1 177.69(15) . . . . ? C2 C7 C8 N1 -2.08(15) . . . . ? C7 C2 C3 C4 -0.1(2) . . . . ? C1 C2 C3 C4 179.78(14) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? C3 C4 C5 C6 -0.3(2) . . . . ? C2 C7 C6 C5 -1.1(2) . . . . ? C8 C7 C6 C5 179.20(15) . . . . ? C4 C5 C6 C7 0.9(2) . . . . ? C17 N3 C9 N2 176.34(12) . . . . ? Fe1 N3 C9 N2 -7.04(18) . . . . ? C17 N3 C9 C10 -3.92(18) . . . . ? Fe1 N3 C9 C10 172.70(10) . . . . ? C1 N2 C9 N3 -3.9(2) . . . . ? C1 N2 C9 C10 176.36(13) . . . . ? N3 C9 C10 C11 3.7(2) . . . . ? N2 C9 C10 C11 -176.59(12) . . . . ? C9 C10 C11 C12 0.4(2) . . . . ? C10 C11 C12 C17 -4.0(2) . . . . ? C10 C11 C12 C13 175.62(13) . . . . ? C9 N3 C17 C12 0.16(19) . . . . ? Fe1 N3 C17 C12 -176.65(10) . . . . ? C9 N3 C17 C16 -178.71(11) . . . . ? Fe1 N3 C17 C16 4.48(15) . . . . ? C11 C12 C17 N3 3.8(2) . . . . ? C13 C12 C17 N3 -175.80(12) . . . . ? C11 C12 C17 C16 -177.39(12) . . . . ? C13 C12 C17 C16 3.0(2) . . . . ? C17 C12 C13 C14 9.3(2) . . . . ? C11 C12 C13 C14 -170.27(13) . . . . ? C12 C13 C14 C15 -41.77(17) . . . . ? C13 C14 C15 C16 63.10(16) . . . . ? N3 C17 C16 C15 -163.06(12) . . . . ? C12 C17 C16 C15 18.05(18) . . . . ? C14 C15 C16 C17 -50.70(16) . . . . ? C26 N5 C18 N4 -174.57(12) . . . . ? Fe1 N5 C18 N4 -0.13(19) . . . . ? C26 N5 C18 C19 3.19(19) . . . . ? Fe1 N5 C18 C19 177.63(10) . . . . ? C8 N4 C18 N5 8.4(2) . . . . ? C8 N4 C18 C19 -169.52(13) . . . . ? N5 C18 C19 C20 -5.9(2) . . . . ? N4 C18 C19 C20 172.15(13) . . . . ? C18 C19 C20 C21 2.5(2) . . . . ? C19 C20 C21 C26 3.2(2) . . . . ? C19 C20 C21 C22A -175.97(14) . . . . ? C18 N5 C26 C21 2.8(2) . . . . ? Fe1 N5 C26 C21 -171.90(11) . . . . ? C18 N5 C26 C25A -177.75(12) . . . . ? Fe1 N5 C26 C25A 7.50(16) . . . . ? C20 C21 C26 N5 -6.0(2) . . . . ? C22A C21 C26 N5 173.13(13) . . . . ? C20 C21 C26 C25A 174.61(13) . . . . ? C22A C21 C26 C25A -6.3(2) . . . . ? C26 C21 C22A C23A 23.1(3) . . . . ? C20 C21 C22A C23A -157.8(3) . . . . ? C21 C22A C23A C24A -51.5(6) . . . . ? C22A C23A C24A C25A 67.0(8) . . . . ? N5 C26 C25A C24A -160.8(4) . . . . ? C21 C26 C25A C24A 18.6(5) . . . . ? C23A C24A C25A C26 -49.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.844 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.075 _diffrn_ambient_environment 'perfluoro polyether oil' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_specimen_support 'polyimid foil' _diffrn_detector 'CCD plate' _diffrn_detector_type CCD-PXL-KAF2 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' #==end== data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 821503' #TrackingRef '- ga_mkr12-ga_mkr20-ga_ds12-ga_mkr14-ga_ds17.cif' _audit_creation_method SHELXL-97 _audit_block_code ga_ds17 _audit_block_refno 1041 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C58.53 H64.15 Co2 N10 O6.53' _chemical_melting_point ? _exptl_crystal_description box _exptl_crystal_colour orange _diffrn_ambient_temperature 100(2) _chemical_formula_weight 1129.91 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 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration . loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.578(7) _cell_length_b 14.502(7) _cell_length_c 26.573(15) _cell_angle_alpha 90.00 _cell_angle_beta 100.720(7) _cell_angle_gamma 90.00 _cell_volume 5141(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8043 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 31.78 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2366 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6560 _exptl_absorpt_correction_T_max 0.7464 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) SADABS (Sheldrick & Bruker AXS, 2004-2008) ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS Smart 1000' _diffrn_measurement_method '\f- and \w-scans' _diffrn_detector_area_resol_mean 8.19 _diffrn_reflns_number 127398 _diffrn_reflns_av_R_equivalents 0.0735 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 31.50 _reflns_number_total 16947 _reflns_number_gt 11952 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-5.631 (Bruker AXS, 2003)' _computing_cell_refinement ; SAINT (Bruker AXS, 1997-2008). Includes estimated systematic errors of the unit cell constants from Monte Carlo simulations. ; _computing_data_reduction 'SAINT (Bruker AXS, 1997-2008); SADABS (Bruker AXS, 2008)' _computing_structure_solution 'SUPERFLIP (Palatinus, 2007-2009)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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. Similarity restraints applied to disordered groups. ; _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^)+(0.0458P)^2^+7.1146P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16947 _refine_ls_number_parameters 790 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1136 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.61921(16) 0.50265(14) 0.14834(8) 0.0131(4) Uani 1 1 d . . . C2 C 0.62036(16) 0.56516(14) 0.19239(8) 0.0139(4) Uani 1 1 d . . . C7 C 0.62017(16) 0.51022(14) 0.23516(8) 0.0136(4) Uani 1 1 d . . . C8 C 0.62037(15) 0.41356(14) 0.21769(8) 0.0128(4) Uani 1 1 d . . . C3 C 0.62163(17) 0.66068(15) 0.19590(9) 0.0171(4) Uani 1 1 d . . . H3 H 0.6220 0.6983 0.1666 0.021 Uiso 1 1 calc R . . C4 C 0.62241(18) 0.69919(15) 0.24387(9) 0.0196(4) Uani 1 1 d . . . H4 H 0.6236 0.7644 0.2476 0.024 Uiso 1 1 calc R . . C5 C 0.62142(17) 0.64369(15) 0.28666(9) 0.0186(4) Uani 1 1 d . . . H5 H 0.6214 0.6717 0.3190 0.022 Uiso 1 1 calc R . . C6 C 0.62040(16) 0.54822(15) 0.28274(8) 0.0163(4) Uani 1 1 d . . . H6 H 0.6199 0.5103 0.3119 0.020 Uiso 1 1 calc R . . C9 C 0.61912(15) 0.48191(14) 0.05938(8) 0.0128(4) Uani 1 1 d . . . C10 C 0.62629(16) 0.53379(15) 0.01556(8) 0.0147(4) Uani 1 1 d . . . H10 H 0.6307 0.5991 0.0175 0.018 Uiso 1 1 calc R . . C11 C 0.62686(17) 0.49003(15) -0.02987(9) 0.0171(4) Uani 1 1 d . A . H11 H 0.6339 0.5248 -0.0593 0.021 Uiso 1 1 calc R . . C12 C 0.61706(17) 0.39416(15) -0.03323(8) 0.0155(4) Uani 1 1 d D . . C17 C 0.60816(16) 0.34655(14) 0.01087(8) 0.0136(4) Uani 1 1 d D A . C13A C 0.6105(9) 0.3458(5) -0.0841(3) 0.0180(17) Uani 0.690(9) 1 d PD A 1 H13A H 0.6785 0.3414 -0.0923 0.022 Uiso 0.690(9) 1 calc PR A 1 H13B H 0.5691 0.3836 -0.1111 0.022 Uiso 0.690(9) 1 calc PR A 1 C14A C 0.5656(4) 0.2498(2) -0.08504(13) 0.0220(10) Uani 0.690(9) 1 d PD A 1 H14A H 0.4924 0.2544 -0.0866 0.026 Uiso 0.690(9) 1 calc PR A 1 H14B H 0.5772 0.2165 -0.1160 0.026 Uiso 0.690(9) 1 calc PR A 1 C15A C 0.6130(4) 0.1965(3) -0.03746(14) 0.0209(9) Uani 0.690(9) 1 d PD A 1 H15A H 0.5844 0.1335 -0.0392 0.025 Uiso 0.690(9) 1 calc PR A 1 H15B H 0.6860 0.1909 -0.0366 0.025 Uiso 0.690(9) 1 calc PR A 1 C16A C 0.5960(7) 0.2425(4) 0.0107(3) 0.0143(14) Uani 0.690(9) 1 d PD A 1 H16A H 0.6437 0.2166 0.0400 0.017 Uiso 0.690(9) 1 calc PR A 1 H16B H 0.5274 0.2277 0.0159 0.017 Uiso 0.690(9) 1 calc PR A 1 C13B C 0.628(3) 0.3466(10) -0.0827(7) 0.0180(17) Uani 0.310(9) 1 d PD A 2 H13C H 0.6904 0.3690 -0.0932 0.022 Uiso 0.310(9) 1 calc PR A 2 H13D H 0.5712 0.3639 -0.1099 0.022 Uiso 0.310(9) 1 calc PR A 2 C14B C 0.6330(10) 0.2420(6) -0.0784(3) 0.030(3) Uani 0.310(9) 1 d PD A 2 H14C H 0.6159 0.2141 -0.1129 0.037 Uiso 0.310(9) 1 calc PR A 2 H14D H 0.7018 0.2226 -0.0628 0.037 Uiso 0.310(9) 1 calc PR A 2 C15B C 0.5597(10) 0.2089(8) -0.0456(4) 0.032(3) Uani 0.310(9) 1 d PD A 2 H15C H 0.4910 0.2259 -0.0627 0.039 Uiso 0.310(9) 1 calc PR A 2 H15D H 0.5629 0.1407 -0.0437 0.039 Uiso 0.310(9) 1 calc PR A 2 C16B C 0.5775(19) 0.2465(10) 0.0078(7) 0.0143(14) Uani 0.310(9) 1 d PD A 2 H16C H 0.6306 0.2096 0.0294 0.017 Uiso 0.310(9) 1 calc PR A 2 H16D H 0.5154 0.2395 0.0219 0.017 Uiso 0.310(9) 1 calc PR A 2 C18 C 0.62328(16) 0.25220(14) 0.23758(8) 0.0134(4) Uani 1 1 d . . . C19 C 0.63276(17) 0.19401(15) 0.28031(8) 0.0164(4) Uani 1 1 d . . . H19 H 0.6369 0.2194 0.3136 0.020 Uiso 1 1 calc R . . C20 C 0.63597(17) 0.10054(15) 0.27386(8) 0.0172(4) Uani 1 1 d . . . H20 H 0.6439 0.0610 0.3028 0.021 Uiso 1 1 calc R . . C21 C 0.62764(16) 0.06325(14) 0.22500(8) 0.0144(4) Uani 1 1 d . . . C26 C 0.61574(16) 0.12419(14) 0.18381(8) 0.0138(4) Uani 1 1 d . . . C22 C 0.63133(18) -0.03985(15) 0.21804(9) 0.0185(4) Uani 1 1 d . . . H22A H 0.5670 -0.0669 0.2232 0.022 Uiso 1 1 calc R . . H22B H 0.6852 -0.0657 0.2445 0.022 Uiso 1 1 calc R . . C23 C 0.6500(2) -0.06760(16) 0.16539(10) 0.0255(5) Uani 1 1 d . . . H23A H 0.7205 -0.0544 0.1629 0.031 Uiso 1 1 calc R . . H23B H 0.6382 -0.1346 0.1601 0.031 Uiso 1 1 calc R . . C24 C 0.5801(2) -0.01407(16) 0.12463(9) 0.0251(5) Uani 1 1 d . . . H24A H 0.5098 -0.0251 0.1283 0.030 Uiso 1 1 calc R . . H24B H 0.5880 -0.0358 0.0903 0.030 Uiso 1 1 calc R . . C25 C 0.6029(2) 0.08904(15) 0.12953(9) 0.0212(5) Uani 1 1 d . . . H25A H 0.6651 0.1017 0.1163 0.025 Uiso 1 1 calc R . . H25B H 0.5477 0.1234 0.1079 0.025 Uiso 1 1 calc R . . C27 C 0.83787(18) 0.28282(19) 0.13827(10) 0.0254(5) Uani 1 1 d . . . C28 C 0.85051(19) 0.33998(18) 0.18640(10) 0.0253(5) Uani 1 1 d . D . H28A H 0.9216 0.3420 0.2025 0.038 Uiso 1 1 calc R . . H28B H 0.8118 0.3124 0.2102 0.038 Uiso 1 1 calc R . . H28C H 0.8264 0.4028 0.1778 0.038 Uiso 1 1 calc R . . C51 C 0.12839(16) 0.49389(14) 0.09877(8) 0.0147(4) Uani 1 1 d . . . C52 C 0.12352(16) 0.55466(15) 0.14287(9) 0.0163(4) Uani 1 1 d . . . C57 C 0.11994(16) 0.49752(15) 0.18454(8) 0.0158(4) Uani 1 1 d . . . C58 C 0.12504(16) 0.40176(15) 0.16644(8) 0.0149(4) Uani 1 1 d . . . C53 C 0.12098(18) 0.64981(15) 0.14755(9) 0.0195(4) Uani 1 1 d . . . H53 H 0.1234 0.6889 0.1191 0.023 Uiso 1 1 calc R . . C54 C 0.11473(18) 0.68612(16) 0.19539(10) 0.0228(5) Uani 1 1 d . . . H54 H 0.1134 0.7511 0.1997 0.027 Uiso 1 1 calc R . . C55 C 0.11039(18) 0.62860(17) 0.23703(10) 0.0224(5) Uani 1 1 d . . . H55 H 0.1057 0.6550 0.2692 0.027 Uiso 1 1 calc R . . C56 C 0.11286(17) 0.53320(16) 0.23213(9) 0.0198(4) Uani 1 1 d . . . H56 H 0.1098 0.4939 0.2604 0.024 Uiso 1 1 calc R . . C59 C 0.13150(16) 0.47548(15) 0.00961(8) 0.0144(4) Uani 1 1 d . B . C60 C 0.11624(18) 0.52728(16) -0.03544(9) 0.0202(5) Uani 1 1 d . . . H60 H 0.1041 0.5917 -0.0342 0.024 Uiso 1 1 calc R . . C61 C 0.11869(18) 0.48547(17) -0.08133(9) 0.0204(5) Uani 1 1 d . B . H61 H 0.1062 0.5206 -0.1120 0.024 Uiso 1 1 calc R . . C62 C 0.13955(17) 0.39127(16) -0.08318(9) 0.0173(4) Uani 1 1 d D . . C67 C 0.15511(16) 0.34331(15) -0.03725(8) 0.0158(4) Uani 1 1 d D B . C63A C 0.1463(18) 0.3465(7) -0.1336(2) 0.0208(5) Uani 0.822(6) 1 d PD B 3 H63A H 0.2079 0.3684 -0.1447 0.025 Uiso 0.822(6) 1 calc PR B 3 H63B H 0.0883 0.3665 -0.1596 0.025 Uiso 0.822(6) 1 calc PR B 3 C64A C 0.1481(3) 0.2407(2) -0.13158(12) 0.0250(8) Uani 0.822(6) 1 d PD B 3 H64A H 0.0804 0.2167 -0.1300 0.030 Uiso 0.822(6) 1 calc PR B 3 H64B H 0.1687 0.2156 -0.1627 0.030 Uiso 0.822(6) 1 calc PR B 3 C65A C 0.2221(3) 0.2116(2) -0.08422(11) 0.0255(8) Uani 0.822(6) 1 d PD B 3 H65A H 0.2883 0.2398 -0.0847 0.031 Uiso 0.822(6) 1 calc PR B 3 H65B H 0.2301 0.1438 -0.0839 0.031 Uiso 0.822(6) 1 calc PR B 3 C66A C 0.1842(15) 0.2426(4) -0.0359(2) 0.0236(11) Uani 0.822(6) 1 d PD B 3 H66A H 0.1254 0.2047 -0.0320 0.028 Uiso 0.822(6) 1 calc PR B 3 H66B H 0.2374 0.2314 -0.0056 0.028 Uiso 0.822(6) 1 calc PR B 3 C63B C 0.145(8) 0.350(3) -0.1347(8) 0.0208(5) Uani 0.178(6) 1 d PD B 4 H63C H 0.1848 0.3902 -0.1533 0.025 Uiso 0.178(6) 1 calc PR B 4 H63D H 0.0767 0.3438 -0.1554 0.025 Uiso 0.178(6) 1 calc PR B 4 C64B C 0.1943(14) 0.2548(11) -0.1256(6) 0.0250(8) Uani 0.178(6) 1 d PD B 4 H64C H 0.1874 0.2210 -0.1585 0.030 Uiso 0.178(6) 1 calc PR B 4 H64D H 0.2666 0.2619 -0.1113 0.030 Uiso 0.178(6) 1 calc PR B 4 C65B C 0.1444(12) 0.2018(10) -0.0889(5) 0.027(4) Uani 0.178(6) 1 d PD B 4 H65C H 0.1626 0.1358 -0.0894 0.033 Uiso 0.178(6) 1 calc PR B 4 H65D H 0.0707 0.2071 -0.0989 0.033 Uiso 0.178(6) 1 calc PR B 4 C66B C 0.179(7) 0.2415(19) -0.0351(10) 0.0236(11) Uani 0.178(6) 1 d PD B 4 H66C H 0.1439 0.2103 -0.0104 0.028 Uiso 0.178(6) 1 calc PR B 4 H66D H 0.2521 0.2320 -0.0239 0.028 Uiso 0.178(6) 1 calc PR B 4 C68 C 0.13012(16) 0.24015(15) 0.18385(8) 0.0153(4) Uani 1 1 d . B . C69 C 0.11739(18) 0.17926(17) 0.22333(9) 0.0210(5) Uani 1 1 d . . . H69 H 0.1070 0.2027 0.2553 0.025 Uiso 1 1 calc R . . C70 C 0.12002(19) 0.08598(17) 0.21552(10) 0.0237(5) Uani 1 1 d . . . H70 H 0.1103 0.0447 0.2419 0.028 Uiso 1 1 calc R . . C71 C 0.13684(18) 0.05163(16) 0.16902(9) 0.0211(5) Uani 1 1 d D . . C76 C 0.14996(17) 0.11498(15) 0.13152(9) 0.0171(4) Uani 1 1 d D B . C72A C 0.149(3) -0.0500(7) 0.1590(7) 0.024(3) Uani 0.508(10) 1 d PD B 5 H72A H 0.1919 -0.0768 0.1898 0.029 Uiso 0.508(10) 1 calc PR B 5 H72B H 0.0824 -0.0792 0.1556 0.029 Uiso 0.508(10) 1 calc PR B 5 C73A C 0.1930(6) -0.0776(3) 0.1132(2) 0.0281(15) Uani 0.508(10) 1 d PD B 5 H73A H 0.1786 -0.1435 0.1053 0.034 Uiso 0.508(10) 1 calc PR B 5 H73B H 0.2667 -0.0694 0.1209 0.034 Uiso 0.508(10) 1 calc PR B 5 C74A C 0.1484(6) -0.0191(4) 0.0674(2) 0.0279(15) Uani 0.508(10) 1 d PD B 5 H74A H 0.0749 -0.0285 0.0589 0.033 Uiso 0.508(10) 1 calc PR B 5 H74B H 0.1774 -0.0371 0.0373 0.033 Uiso 0.508(10) 1 calc PR B 5 C75A C 0.172(3) 0.0827(8) 0.0807(7) 0.0257(6) Uani 0.508(10) 1 d PD B 5 H75A H 0.2439 0.0935 0.0806 0.031 Uiso 0.508(10) 1 calc PR B 5 H75B H 0.1331 0.1214 0.0533 0.031 Uiso 0.508(10) 1 calc PR B 5 C72B C 0.133(3) -0.0525(8) 0.1630(7) 0.024(3) Uani 0.492(10) 1 d PD B 6 H72C H 0.1929 -0.0803 0.1849 0.029 Uiso 0.492(10) 1 calc PR B 6 H72D H 0.0728 -0.0769 0.1742 0.029 Uiso 0.492(10) 1 calc PR B 6 C73B C 0.1310(7) -0.0781(4) 0.1077(2) 0.0350(19) Uani 0.492(10) 1 d PD B 6 H73C H 0.0620 -0.0704 0.0882 0.042 Uiso 0.492(10) 1 calc PR B 6 H73D H 0.1498 -0.1438 0.1058 0.042 Uiso 0.492(10) 1 calc PR B 6 C74B C 0.2023(7) -0.0190(4) 0.0836(3) 0.0336(17) Uani 0.492(10) 1 d PD B 6 H74C H 0.2036 -0.0418 0.0486 0.040 Uiso 0.492(10) 1 calc PR B 6 H74D H 0.2709 -0.0244 0.1040 0.040 Uiso 0.492(10) 1 calc PR B 6 C75B C 0.170(3) 0.0823(8) 0.0809(7) 0.0257(6) Uani 0.492(10) 1 d PD B 6 H75C H 0.2240 0.1205 0.0708 0.031 Uiso 0.492(10) 1 calc PR B 6 H75D H 0.1091 0.0898 0.0544 0.031 Uiso 0.492(10) 1 calc PR B 6 C77 C 0.38144(16) 0.29650(14) 0.10589(8) 0.0127(4) Uani 1 1 d . B . C78 C 0.37846(18) 0.35839(16) 0.15130(9) 0.0186(4) Uani 1 1 d . . . H78A H 0.4340 0.3427 0.1791 0.028 Uiso 1 1 calc R . . H78B H 0.3147 0.3498 0.1630 0.028 Uiso 1 1 calc R . . H78C H 0.3847 0.4229 0.1413 0.028 Uiso 1 1 calc R . . C79 C -0.0561(2) 0.24328(19) -0.00175(10) 0.0284(6) Uani 1 1 d . B . H79A H -0.0454 0.2981 -0.0216 0.043 Uiso 1 1 calc R . . H79B H -0.1258 0.2419 0.0033 0.043 Uiso 1 1 calc R . . H79C H -0.0422 0.1878 -0.0203 0.043 Uiso 1 1 calc R . . C91 C 0.8755(3) 0.0502(3) 0.0885(3) 0.094(2) Uani 1 1 d . . . H91A H 0.9345 0.0891 0.0998 0.140 Uiso 1 1 calc R . . H91B H 0.8936 -0.0016 0.0684 0.140 Uiso 1 1 calc R . . H91C H 0.8512 0.0266 0.1185 0.140 Uiso 1 1 calc R . . Co1 Co 0.61105(2) 0.303809(19) 0.122846(11) 0.01111(6) Uani 1 1 d . . . Co2 Co 0.15266(2) 0.298007(19) 0.073770(11) 0.01254(7) Uani 1 1 d . B . N1 N 0.61925(14) 0.41276(12) 0.16582(7) 0.0132(3) Uani 1 1 d . D . N2 N 0.62000(14) 0.53436(12) 0.10325(7) 0.0149(3) Uani 1 1 d . . . N3 N 0.61056(13) 0.38880(12) 0.05694(7) 0.0124(3) Uani 1 1 d . A . N4 N 0.62186(14) 0.34574(12) 0.24965(7) 0.0143(3) Uani 1 1 d . . . N5 N 0.61503(13) 0.21772(12) 0.18965(7) 0.0121(3) Uani 1 1 d . D . N51 N 0.12947(14) 0.40314(12) 0.11510(7) 0.0148(3) Uani 1 1 d . . . N52 N 0.12928(14) 0.52673(13) 0.05371(7) 0.0167(4) Uani 1 1 d . . . N53 N 0.14807(14) 0.38288(12) 0.00848(7) 0.0144(3) Uani 1 1 d . . . N54 N 0.12583(14) 0.33264(13) 0.19723(7) 0.0165(4) Uani 1 1 d . . . N55 N 0.14596(14) 0.20835(12) 0.13846(7) 0.0146(3) Uani 1 1 d . . . O1 O 0.75035(12) 0.25918(11) 0.11570(6) 0.0198(3) Uani 1 1 d . D . O3 O 0.46453(11) 0.27173(10) 0.09618(6) 0.0152(3) Uani 1 1 d . B . O4 O 0.29996(11) 0.27135(11) 0.07827(6) 0.0175(3) Uani 1 1 d . . . O5 O 0.00984(12) 0.24618(11) 0.04713(6) 0.0208(3) Uani 1 1 d . . . H5O H -0.0241 0.2447 0.0723 0.025 Uiso 1 1 d R B . O91 O 0.7985(2) 0.1036(2) 0.05775(11) 0.0649(8) Uani 1 1 d . . . H91 H 0.7880 0.1515 0.0737 0.097 Uiso 1 1 calc R . . C92 C 0.3880(4) 0.0634(3) 0.0200(2) 0.0280(12) Uani 0.535(5) 1 d P C 9 H92A H 0.3940 0.1295 0.0275 0.042 Uiso 0.535(5) 1 calc PR C 9 H92B H 0.4472 0.0423 0.0071 0.042 Uiso 0.535(5) 1 calc PR C 9 H92C H 0.3830 0.0295 0.0514 0.042 Uiso 0.535(5) 1 calc PR C 9 O92 O 0.3037(4) 0.0476(3) -0.01626(19) 0.0509(14) Uani 0.535(5) 1 d P C 9 H92 H 0.2972 -0.0093 -0.0218 0.076 Uiso 0.535(5) 1 calc PR C 9 O2A O 0.9160(2) 0.2710(8) 0.12130(17) 0.033(2) Uani 0.70(2) 1 d P D 7 O2B O 0.9073(8) 0.2242(14) 0.1256(4) 0.034(3) Uani 0.30(2) 1 d P D 8 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 0.0145(9) 0.0107(9) 0.0143(10) -0.0018(7) 0.0032(7) -0.0010(7) C2 0.0155(10) 0.0109(9) 0.0149(10) -0.0017(7) 0.0022(8) -0.0009(7) C7 0.0140(9) 0.0111(9) 0.0156(10) -0.0029(7) 0.0022(7) -0.0002(7) C8 0.0133(9) 0.0116(9) 0.0134(9) -0.0022(7) 0.0020(7) -0.0006(7) C3 0.0214(11) 0.0100(9) 0.0206(11) -0.0019(8) 0.0053(8) -0.0011(8) C4 0.0243(11) 0.0106(9) 0.0241(11) -0.0063(9) 0.0049(9) -0.0010(8) C5 0.0205(11) 0.0162(10) 0.0189(11) -0.0070(8) 0.0033(8) 0.0007(8) C6 0.0181(10) 0.0157(10) 0.0152(10) -0.0024(8) 0.0031(8) 0.0004(8) C9 0.0135(9) 0.0108(9) 0.0137(10) 0.0007(7) 0.0019(7) -0.0010(7) C10 0.0160(10) 0.0120(9) 0.0159(10) 0.0016(8) 0.0025(8) -0.0014(7) C11 0.0212(11) 0.0154(10) 0.0149(10) 0.0046(8) 0.0037(8) -0.0013(8) C12 0.0193(10) 0.0150(10) 0.0120(10) 0.0004(8) 0.0020(8) 0.0004(8) C17 0.0155(10) 0.0125(9) 0.0123(9) -0.0008(7) 0.0012(7) -0.0002(7) C13A 0.023(5) 0.0195(11) 0.0130(11) -0.0003(9) 0.0059(19) 0.0002(14) C14A 0.030(2) 0.0220(18) 0.0136(16) -0.0048(13) 0.0041(15) -0.0043(15) C15A 0.035(2) 0.0143(16) 0.0145(17) -0.0016(13) 0.0072(16) -0.0003(17) C16A 0.018(4) 0.0118(11) 0.0127(13) -0.0005(10) 0.0009(18) 0.0008(16) C13B 0.023(5) 0.0195(11) 0.0130(11) -0.0003(9) 0.0059(19) 0.0002(14) C14B 0.058(8) 0.021(4) 0.013(4) -0.006(3) 0.010(4) 0.001(4) C15B 0.054(7) 0.026(5) 0.016(4) -0.008(3) 0.004(5) -0.012(5) C16B 0.018(4) 0.0118(11) 0.0127(13) -0.0005(10) 0.0009(18) 0.0008(16) C18 0.0148(10) 0.0108(9) 0.0151(10) -0.0002(7) 0.0038(8) -0.0004(7) C19 0.0223(11) 0.0160(10) 0.0108(9) -0.0004(8) 0.0034(8) 0.0000(8) C20 0.0216(11) 0.0152(10) 0.0149(10) 0.0039(8) 0.0036(8) 0.0010(8) C21 0.0171(10) 0.0103(9) 0.0161(10) 0.0019(7) 0.0042(8) 0.0010(7) C26 0.0156(10) 0.0101(9) 0.0161(10) -0.0012(7) 0.0041(8) -0.0005(7) C22 0.0262(12) 0.0102(9) 0.0193(11) 0.0019(8) 0.0047(9) 0.0015(8) C23 0.0399(15) 0.0114(10) 0.0269(13) -0.0009(9) 0.0103(11) 0.0035(9) C24 0.0428(15) 0.0133(10) 0.0191(12) -0.0036(9) 0.0052(10) -0.0020(10) C25 0.0367(14) 0.0115(10) 0.0157(11) -0.0014(8) 0.0059(9) -0.0001(9) C27 0.0190(11) 0.0379(15) 0.0201(12) 0.0052(10) 0.0058(9) 0.0052(10) C28 0.0200(12) 0.0284(13) 0.0268(13) 0.0014(10) 0.0020(9) -0.0033(9) C51 0.0137(9) 0.0122(9) 0.0175(10) -0.0001(8) 0.0012(8) 0.0010(7) C52 0.0153(10) 0.0144(10) 0.0191(11) -0.0027(8) 0.0028(8) 0.0014(8) C57 0.0143(10) 0.0151(10) 0.0177(10) -0.0030(8) 0.0019(8) 0.0000(8) C58 0.0128(9) 0.0159(10) 0.0163(10) -0.0019(8) 0.0033(8) 0.0012(7) C53 0.0226(11) 0.0125(10) 0.0226(12) -0.0011(8) 0.0021(9) 0.0011(8) C54 0.0243(12) 0.0154(11) 0.0275(12) -0.0059(9) 0.0015(9) 0.0020(9) C55 0.0226(12) 0.0221(11) 0.0222(12) -0.0082(9) 0.0031(9) 0.0012(9) C56 0.0207(11) 0.0200(11) 0.0189(11) -0.0040(9) 0.0045(9) 0.0016(8) C59 0.0136(9) 0.0150(10) 0.0148(10) 0.0007(8) 0.0030(7) 0.0006(7) C60 0.0236(12) 0.0165(10) 0.0207(11) 0.0038(9) 0.0046(9) 0.0038(8) C61 0.0234(12) 0.0224(11) 0.0158(10) 0.0063(9) 0.0046(9) 0.0014(9) C62 0.0163(10) 0.0201(11) 0.0157(10) 0.0001(8) 0.0037(8) -0.0009(8) C67 0.0158(10) 0.0166(10) 0.0150(10) -0.0006(8) 0.0028(8) -0.0014(8) C63A 0.0227(13) 0.0249(14) 0.0151(11) 0.0000(9) 0.0046(10) -0.0012(13) C64A 0.035(2) 0.0229(15) 0.0172(14) -0.0058(11) 0.0047(14) 0.0015(15) C65A 0.0333(19) 0.0227(15) 0.0203(15) -0.0023(11) 0.0045(12) 0.0076(12) C66A 0.037(3) 0.0156(11) 0.0184(12) -0.0016(9) 0.0057(11) 0.0012(11) C63B 0.0227(13) 0.0249(14) 0.0151(11) 0.0000(9) 0.0046(10) -0.0012(13) C64B 0.035(2) 0.0229(15) 0.0172(14) -0.0058(11) 0.0047(14) 0.0015(15) C65B 0.041(10) 0.020(7) 0.018(7) -0.005(5) -0.002(6) 0.006(6) C66B 0.037(3) 0.0156(11) 0.0184(12) -0.0016(9) 0.0057(11) 0.0012(11) C68 0.0149(10) 0.0151(10) 0.0159(10) 0.0018(8) 0.0030(8) -0.0002(8) C69 0.0216(11) 0.0233(12) 0.0186(11) 0.0033(9) 0.0052(9) -0.0013(9) C70 0.0258(12) 0.0216(12) 0.0234(12) 0.0085(9) 0.0041(10) -0.0032(9) C71 0.0228(12) 0.0147(10) 0.0236(12) 0.0029(9) -0.0012(9) -0.0038(8) C76 0.0171(10) 0.0134(10) 0.0197(11) 0.0010(8) 0.0008(8) 0.0001(8) C72A 0.028(9) 0.0130(12) 0.031(3) 0.0063(13) 0.0040(19) -0.0079(18) C73A 0.040(4) 0.011(2) 0.031(3) -0.0035(19) 0.001(3) -0.002(2) C74A 0.050(4) 0.015(2) 0.017(3) -0.0018(19) 0.003(3) -0.003(2) C75A 0.0409(16) 0.0126(10) 0.0238(12) -0.0009(9) 0.0065(11) 0.0032(10) C72B 0.028(9) 0.0130(12) 0.031(3) 0.0063(13) 0.0040(19) -0.0079(18) C73B 0.058(5) 0.012(2) 0.032(3) -0.004(2) 0.002(3) -0.003(3) C74B 0.060(5) 0.017(3) 0.022(3) -0.003(2) 0.004(3) 0.010(3) C75B 0.0409(16) 0.0126(10) 0.0238(12) -0.0009(9) 0.0065(11) 0.0032(10) C77 0.0177(9) 0.0082(8) 0.0120(9) 0.0041(7) 0.0024(7) 0.0002(7) C78 0.0223(11) 0.0174(10) 0.0161(10) -0.0031(8) 0.0038(8) -0.0010(8) C79 0.0256(13) 0.0269(13) 0.0285(13) -0.0037(10) -0.0057(10) -0.0030(10) C91 0.036(2) 0.052(3) 0.188(6) 0.015(3) 0.010(3) -0.0030(19) Co1 0.01333(13) 0.00832(12) 0.01177(13) -0.00171(10) 0.00258(10) -0.00061(10) Co2 0.01333(13) 0.01013(13) 0.01398(14) -0.00091(10) 0.00205(10) -0.00009(10) N1 0.0172(9) 0.0093(8) 0.0131(8) -0.0007(6) 0.0029(7) -0.0012(6) N2 0.0191(9) 0.0103(8) 0.0155(9) -0.0012(7) 0.0038(7) -0.0015(6) N3 0.0134(8) 0.0115(8) 0.0118(8) -0.0010(6) 0.0014(6) -0.0009(6) N4 0.0180(9) 0.0118(8) 0.0132(8) -0.0016(6) 0.0027(7) 0.0000(7) N5 0.0155(8) 0.0096(8) 0.0112(8) -0.0001(6) 0.0023(6) -0.0003(6) N51 0.0160(9) 0.0133(8) 0.0150(9) 0.0009(7) 0.0025(7) 0.0019(7) N52 0.0179(9) 0.0142(8) 0.0182(9) -0.0003(7) 0.0036(7) 0.0009(7) N53 0.0164(9) 0.0132(8) 0.0137(8) -0.0005(7) 0.0032(7) -0.0012(6) N54 0.0167(9) 0.0160(8) 0.0170(9) -0.0010(7) 0.0039(7) 0.0003(7) N55 0.0155(8) 0.0123(8) 0.0156(9) 0.0012(7) 0.0016(7) 0.0003(6) O1 0.0189(8) 0.0196(8) 0.0213(8) -0.0012(6) 0.0049(6) 0.0026(6) O3 0.0133(7) 0.0139(7) 0.0182(8) -0.0025(6) 0.0025(6) -0.0011(5) O4 0.0147(7) 0.0177(7) 0.0199(8) -0.0034(6) 0.0028(6) -0.0005(6) O5 0.0189(8) 0.0229(8) 0.0192(8) 0.0000(6) 0.0003(6) -0.0045(6) O91 0.0419(15) 0.091(2) 0.0614(18) -0.0217(16) 0.0085(13) -0.0070(15) C92 0.026(2) 0.021(2) 0.037(3) -0.011(2) 0.006(2) -0.0052(18) O92 0.057(3) 0.037(2) 0.055(3) -0.006(2) 0.001(2) -0.003(2) O2A 0.0176(14) 0.055(5) 0.0276(18) -0.014(2) 0.0073(11) -0.0029(16) O2B 0.025(4) 0.023(7) 0.061(6) 0.003(4) 0.025(4) 0.007(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 C1 N2 1.285(3) . ? C1 N1 1.384(3) . ? C1 C2 1.478(3) . ? C2 C7 1.388(3) . ? C2 C3 1.388(3) . ? C7 C6 1.379(3) . ? C7 C8 1.477(3) . ? C8 N4 1.297(3) . ? C8 N1 1.376(3) . ? C3 C4 1.390(3) . ? C3 H3 0.9500 . ? C4 C5 1.395(3) . ? C4 H4 0.9500 . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C9 N3 1.356(3) . ? C9 N2 1.390(3) . ? C9 C10 1.405(3) . ? C10 C11 1.365(3) . ? C10 H10 0.9500 . ? C11 C12 1.398(3) . ? C11 H11 0.9500 . ? C12 C17 1.385(3) . ? C12 C13A 1.510(7) . ? C12 C13B 1.518(14) . ? C17 N3 1.364(3) . ? C17 C16B 1.508(14) . ? C17 C16A 1.517(6) . ? C13A C14A 1.519(8) . ? C13A H13A 0.9900 . ? C13A H13B 0.9900 . ? C14A C15A 1.519(6) . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A C16A 1.500(7) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C13B C14B 1.521(15) . ? C13B H13C 0.9900 . ? C13B H13D 0.9900 . ? C14B C15B 1.517(13) . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B C16B 1.496(14) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? C18 N5 1.353(3) . ? C18 N4 1.395(3) . ? C18 C19 1.401(3) . ? C19 C20 1.368(3) . ? C19 H19 0.9500 . ? C20 C21 1.392(3) . ? C20 H20 0.9500 . ? C21 C26 1.392(3) . ? C21 C22 1.509(3) . ? C26 N5 1.365(3) . ? C26 C25 1.509(3) . ? C22 C23 1.522(3) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.515(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.528(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C27 O2A 1.239(4) . ? C27 O1 1.274(3) . ? C27 O2B 1.357(10) . ? C27 C28 1.507(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C51 N52 1.291(3) . ? C51 N51 1.385(3) . ? C51 C52 1.477(3) . ? C52 C53 1.387(3) . ? C52 C57 1.391(3) . ? C57 C56 1.386(3) . ? C57 C58 1.476(3) . ? C58 N54 1.293(3) . ? C58 N51 1.377(3) . ? C53 C54 1.393(3) . ? C53 H53 0.9500 . ? C54 C55 1.396(4) . ? C54 H54 0.9500 . ? C55 C56 1.391(3) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C59 N53 1.363(3) . ? C59 N52 1.393(3) . ? C59 C60 1.396(3) . ? C60 C61 1.368(3) . ? C60 H60 0.9500 . ? C61 C62 1.398(3) . ? C61 H61 0.9500 . ? C62 C67 1.387(3) . ? C62 C63A 1.507(5) . ? C62 C63B 1.508(17) . ? C67 N53 1.363(3) . ? C67 C66B 1.510(17) . ? C67 C66A 1.512(5) . ? C63A C64A 1.536(10) . ? C63A H63A 0.9900 . ? C63A H63B 0.9900 . ? C64A C65A 1.517(5) . ? C64A H64A 0.9900 . ? C64A H64B 0.9900 . ? C65A C66A 1.537(12) . ? C65A H65A 0.9900 . ? C65A H65B 0.9900 . ? C66A H66A 0.9900 . ? C66A H66B 0.9900 . ? C63B C64B 1.534(19) . ? C63B H63C 0.9900 . ? C63B H63D 0.9900 . ? C64B C65B 1.500(15) . ? C64B H64C 0.9900 . ? C64B H64D 0.9900 . ? C65B C66B 1.53(2) . ? C65B H65C 0.9900 . ? C65B H65D 0.9900 . ? C66B H66C 0.9900 . ? C66B H66D 0.9900 . ? C68 N55 1.345(3) . ? C68 N54 1.392(3) . ? C68 C69 1.406(3) . ? C69 C70 1.370(3) . ? C69 H69 0.9500 . ? C70 C71 1.390(4) . ? C70 H70 0.9500 . ? C71 C76 1.391(3) . ? C71 C72A 1.512(10) . ? C71 C72B 1.518(11) . ? C76 N55 1.369(3) . ? C76 C75B 1.501(11) . ? C76 C75A 1.511(10) . ? C72A C73A 1.505(12) . ? C72A H72A 0.9900 . ? C72A H72B 0.9900 . ? C73A C74A 1.515(8) . ? C73A H73A 0.9900 . ? C73A H73B 0.9900 . ? C74A C75A 1.539(14) . ? C74A H74A 0.9900 . ? C74A H74B 0.9900 . ? C75A H75A 0.9900 . ? C75A H75B 0.9900 . ? C72B C73B 1.510(14) . ? C72B H72C 0.9900 . ? C72B H72D 0.9900 . ? C73B C74B 1.522(10) . ? C73B H73C 0.9900 . ? C73B H73D 0.9900 . ? C74B C75B 1.530(14) . ? C74B H74C 0.9900 . ? C74B H74D 0.9900 . ? C75B H75C 0.9900 . ? C75B H75D 0.9900 . ? C77 O3 1.256(3) . ? C77 O4 1.262(3) . ? C77 C78 1.510(3) . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 O5 1.435(3) . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C91 O91 1.429(5) . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? Co1 N1 1.9405(19) . ? Co1 O3 2.0377(18) . ? Co1 O1 2.0412(19) . ? Co1 N3 2.140(2) . ? Co1 N5 2.163(2) . ? Co2 N51 1.939(2) . ? Co2 O4 2.0188(19) . ? Co2 O5 2.0774(18) . ? Co2 N53 2.119(2) . ? Co2 N55 2.171(2) . ? O5 H5O 0.8809 . ? O91 H91 0.8400 . ? C92 O92 1.372(6) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? O92 H92 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 130.57(19) . . ? N2 C1 C2 121.20(19) . . ? N1 C1 C2 108.21(18) . . ? C7 C2 C3 121.3(2) . . ? C7 C2 C1 107.15(18) . . ? C3 C2 C1 131.5(2) . . ? C6 C7 C2 121.4(2) . . ? C6 C7 C8 131.9(2) . . ? C2 C7 C8 106.69(18) . . ? N4 C8 N1 130.21(19) . . ? N4 C8 C7 120.97(19) . . ? N1 C8 C7 108.82(18) . . ? C2 C3 C4 117.4(2) . . ? C2 C3 H3 121.3 . . ? C4 C3 H3 121.3 . . ? C3 C4 C5 121.1(2) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 121.0(2) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C7 C6 C5 117.8(2) . . ? C7 C6 H6 121.1 . . ? C5 C6 H6 121.1 . . ? N3 C9 N2 124.91(19) . . ? N3 C9 C10 120.82(19) . . ? N2 C9 C10 114.27(19) . . ? C11 C10 C9 119.8(2) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 120.2(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C17 C12 C11 117.7(2) . . ? C17 C12 C13A 121.7(3) . . ? C11 C12 C13A 120.5(3) . . ? C17 C12 C13B 123.1(7) . . ? C11 C12 C13B 118.9(7) . . ? C13A C12 C13B 9.1(17) . . ? N3 C17 C12 122.99(19) . . ? N3 C17 C16B 116.2(7) . . ? C12 C17 C16B 120.0(7) . . ? N3 C17 C16A 115.7(3) . . ? C12 C17 C16A 121.4(3) . . ? C16B C17 C16A 9.7(13) . . ? C12 C13A C14A 113.4(5) . . ? C12 C13A H13A 108.9 . . ? C14A C13A H13A 108.9 . . ? C12 C13A H13B 108.9 . . ? C14A C13A H13B 108.9 . . ? H13A C13A H13B 107.7 . . ? C15A C14A C13A 110.3(5) . . ? C15A C14A H14A 109.6 . . ? C13A C14A H14A 109.6 . . ? C15A C14A H14B 109.6 . . ? C13A C14A H14B 109.6 . . ? H14A C14A H14B 108.1 . . ? C16A C15A C14A 112.1(4) . . ? C16A C15A H15A 109.2 . . ? C14A C15A H15A 109.2 . . ? C16A C15A H15B 109.2 . . ? C14A C15A H15B 109.2 . . ? H15A C15A H15B 107.9 . . ? C15A C16A C17 114.2(5) . . ? C15A C16A H16A 108.7 . . ? C17 C16A H16A 108.7 . . ? C15A C16A H16B 108.7 . . ? C17 C16A H16B 108.7 . . ? H16A C16A H16B 107.6 . . ? C12 C13B C14B 113.3(12) . . ? C12 C13B H13C 108.9 . . ? C14B C13B H13C 108.9 . . ? C12 C13B H13D 108.9 . . ? C14B C13B H13D 108.9 . . ? H13C C13B H13D 107.7 . . ? C15B C14B C13B 109.8(12) . . ? C15B C14B H14C 109.7 . . ? C13B C14B H14C 109.7 . . ? C15B C14B H14D 109.7 . . ? C13B C14B H14D 109.7 . . ? H14C C14B H14D 108.2 . . ? C16B C15B C14B 114.9(12) . . ? C16B C15B H15C 108.5 . . ? C14B C15B H15C 108.5 . . ? C16B C15B H15D 108.5 . . ? C14B C15B H15D 108.5 . . ? H15C C15B H15D 107.5 . . ? C15B C16B C17 113.4(12) . . ? C15B C16B H16C 108.9 . . ? C17 C16B H16C 108.9 . . ? C15B C16B H16D 108.9 . . ? C17 C16B H16D 108.9 . . ? H16C C16B H16D 107.7 . . ? N5 C18 N4 125.00(19) . . ? N5 C18 C19 121.28(19) . . ? N4 C18 C19 113.72(19) . . ? C20 C19 C18 119.7(2) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 120.2(2) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C26 117.7(2) . . ? C20 C21 C22 120.05(19) . . ? C26 C21 C22 122.3(2) . . ? N5 C26 C21 122.9(2) . . ? N5 C26 C25 116.24(18) . . ? C21 C26 C25 120.85(19) . . ? C21 C22 C23 112.94(19) . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C24 C23 C22 109.4(2) . . ? C24 C23 H23A 109.8 . . ? C22 C23 H23A 109.8 . . ? C24 C23 H23B 109.8 . . ? C22 C23 H23B 109.8 . . ? H23A C23 H23B 108.2 . . ? C23 C24 C25 110.5(2) . . ? C23 C24 H24A 109.6 . . ? C25 C24 H24A 109.6 . . ? C23 C24 H24B 109.6 . . ? C25 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C24 113.42(19) . . ? C26 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? C26 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? O2A C27 O1 125.3(3) . . ? O2A C27 O2B 30.9(4) . . ? O1 C27 O2B 110.2(8) . . ? O2A C27 C28 114.5(3) . . ? O1 C27 C28 119.8(2) . . ? O2B C27 C28 125.5(6) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N52 C51 N51 129.8(2) . . ? N52 C51 C52 121.7(2) . . ? N51 C51 C52 108.52(19) . . ? C53 C52 C57 121.1(2) . . ? C53 C52 C51 132.1(2) . . ? C57 C52 C51 106.82(19) . . ? C56 C57 C52 121.5(2) . . ? C56 C57 C58 131.6(2) . . ? C52 C57 C58 106.88(19) . . ? N54 C58 N51 129.9(2) . . ? N54 C58 C57 121.2(2) . . ? N51 C58 C57 108.83(19) . . ? C52 C53 C54 117.7(2) . . ? C52 C53 H53 121.1 . . ? C54 C53 H53 121.1 . . ? C53 C54 C55 121.1(2) . . ? C53 C54 H54 119.5 . . ? C55 C54 H54 119.5 . . ? C56 C55 C54 121.0(2) . . ? C56 C55 H55 119.5 . . ? C54 C55 H55 119.5 . . ? C57 C56 C55 117.6(2) . . ? C57 C56 H56 121.2 . . ? C55 C56 H56 121.2 . . ? N53 C59 N52 125.01(19) . . ? N53 C59 C60 120.7(2) . . ? N52 C59 C60 114.3(2) . . ? C61 C60 C59 120.1(2) . . ? C61 C60 H60 119.9 . . ? C59 C60 H60 119.9 . . ? C60 C61 C62 120.2(2) . . ? C60 C61 H61 119.9 . . ? C62 C61 H61 119.9 . . ? C67 C62 C61 117.2(2) . . ? C67 C62 C63A 122.8(3) . . ? C61 C62 C63A 119.9(3) . . ? C67 C62 C63B 125.1(12) . . ? C61 C62 C63B 117.7(12) . . ? C63A C62 C63B 2.2(11) . . ? N53 C67 C62 123.3(2) . . ? N53 C67 C66B 115.3(13) . . ? C62 C67 C66B 121.4(13) . . ? N53 C67 C66A 116.5(3) . . ? C62 C67 C66A 120.2(3) . . ? C66B C67 C66A 3(5) . . ? C62 C63A C64A 113.7(6) . . ? C62 C63A H63A 108.8 . . ? C64A C63A H63A 108.8 . . ? C62 C63A H63B 108.8 . . ? C64A C63A H63B 108.8 . . ? H63A C63A H63B 107.7 . . ? C65A C64A C63A 108.1(6) . . ? C65A C64A H64A 110.1 . . ? C63A C64A H64A 110.1 . . ? C65A C64A H64B 110.1 . . ? C63A C64A H64B 110.1 . . ? H64A C64A H64B 108.4 . . ? C64A C65A C66A 109.8(5) . . ? C64A C65A H65A 109.7 . . ? C66A C65A H65A 109.7 . . ? C64A C65A H65B 109.7 . . ? C66A C65A H65B 109.7 . . ? H65A C65A H65B 108.2 . . ? C67 C66A C65A 112.9(6) . . ? C67 C66A H66A 109.0 . . ? C65A C66A H66A 109.0 . . ? C67 C66A H66B 109.0 . . ? C65A C66A H66B 109.0 . . ? H66A C66A H66B 107.8 . . ? C62 C63B C64B 108.0(16) . . ? C62 C63B H63C 110.1 . . ? C64B C63B H63C 110.1 . . ? C62 C63B H63D 110.1 . . ? C64B C63B H63D 110.1 . . ? H63C C63B H63D 108.4 . . ? C65B C64B C63B 109(3) . . ? C65B C64B H64C 109.9 . . ? C63B C64B H64C 109.9 . . ? C65B C64B H64D 109.9 . . ? C63B C64B H64D 109.9 . . ? H64C C64B H64D 108.3 . . ? C64B C65B C66B 109(3) . . ? C64B C65B H65C 110.0 . . ? C66B C65B H65C 110.0 . . ? C64B C65B H65D 110.0 . . ? C66B C65B H65D 110.0 . . ? H65C C65B H65D 108.4 . . ? C67 C66B C65B 107.7(16) . . ? C67 C66B H66C 110.2 . . ? C65B C66B H66C 110.2 . . ? C67 C66B H66D 110.2 . . ? C65B C66B H66D 110.2 . . ? H66C C66B H66D 108.5 . . ? N55 C68 N54 125.51(19) . . ? N55 C68 C69 121.1(2) . . ? N54 C68 C69 113.4(2) . . ? C70 C69 C68 119.8(2) . . ? C70 C69 H69 120.1 . . ? C68 C69 H69 120.1 . . ? C69 C70 C71 120.1(2) . . ? C69 C70 H70 119.9 . . ? C71 C70 H70 119.9 . . ? C70 C71 C76 117.7(2) . . ? C70 C71 C72A 123.2(5) . . ? C76 C71 C72A 118.9(5) . . ? C70 C71 C72B 116.3(5) . . ? C76 C71 C72B 126.0(5) . . ? C72A C71 C72B 9.9(18) . . ? N55 C76 C71 122.9(2) . . ? N55 C76 C75B 116.8(5) . . ? C71 C76 C75B 120.3(5) . . ? N55 C76 C75A 116.5(5) . . ? C71 C76 C75A 120.6(5) . . ? C75B C76 C75A 1(3) . . ? C73A C72A C71 118.4(9) . . ? C73A C72A H72A 107.7 . . ? C71 C72A H72A 107.7 . . ? C73A C72A H72B 107.7 . . ? C71 C72A H72B 107.7 . . ? H72A C72A H72B 107.1 . . ? C72A C73A C74A 110.0(11) . . ? C72A C73A H73A 109.7 . . ? C74A C73A H73A 109.7 . . ? C72A C73A H73B 109.7 . . ? C74A C73A H73B 109.7 . . ? H73A C73A H73B 108.2 . . ? C73A C74A C75A 108.5(11) . . ? C73A C74A H74A 110.0 . . ? C75A C74A H74A 110.0 . . ? C73A C74A H74B 110.0 . . ? C75A C74A H74B 110.0 . . ? H74A C74A H74B 108.4 . . ? C76 C75A C74A 115.8(10) . . ? C76 C75A H75A 108.3 . . ? C74A C75A H75A 108.3 . . ? C76 C75A H75B 108.3 . . ? C74A C75A H75B 108.3 . . ? H75A C75A H75B 107.4 . . ? C73B C72B C71 110.0(10) . . ? C73B C72B H72C 109.7 . . ? C71 C72B H72C 109.7 . . ? C73B C72B H72D 109.7 . . ? C71 C72B H72D 109.7 . . ? H72C C72B H72D 108.2 . . ? C72B C73B C74B 111.9(10) . . ? C72B C73B H73C 109.2 . . ? C74B C73B H73C 109.2 . . ? C72B C73B H73D 109.2 . . ? C74B C73B H73D 109.2 . . ? H73C C73B H73D 107.9 . . ? C73B C74B C75B 111.3(12) . . ? C73B C74B H74C 109.4 . . ? C75B C74B H74C 109.4 . . ? C73B C74B H74D 109.4 . . ? C75B C74B H74D 109.4 . . ? H74C C74B H74D 108.0 . . ? C76 C75B C74B 111.0(10) . . ? C76 C75B H75C 109.4 . . ? C74B C75B H75C 109.4 . . ? C76 C75B H75D 109.4 . . ? C74B C75B H75D 109.4 . . ? H75C C75B H75D 108.0 . . ? O3 C77 O4 121.4(2) . . ? O3 C77 C78 119.52(19) . . ? O4 C77 C78 119.03(19) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? O5 C79 H79A 109.5 . . ? O5 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? O5 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O91 C91 H91A 109.5 . . ? O91 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? O91 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? N1 Co1 O3 109.63(7) . . ? N1 Co1 O1 111.11(7) . . ? O3 Co1 O1 139.20(7) . . ? N1 Co1 N3 90.21(8) . . ? O3 Co1 N3 89.58(7) . . ? O1 Co1 N3 88.19(7) . . ? N1 Co1 N5 89.84(8) . . ? O3 Co1 N5 91.57(7) . . ? O1 Co1 N5 90.64(7) . . ? N3 Co1 N5 178.76(7) . . ? N51 Co2 O4 112.37(7) . . ? N51 Co2 O5 103.76(8) . . ? O4 Co2 O5 143.39(7) . . ? N51 Co2 N53 91.37(8) . . ? O4 Co2 N53 92.16(7) . . ? O5 Co2 N53 92.74(7) . . ? N51 Co2 N55 89.27(8) . . ? O4 Co2 N55 91.45(7) . . ? O5 Co2 N55 83.06(7) . . ? N53 Co2 N55 175.78(7) . . ? C8 N1 C1 109.12(17) . . ? C8 N1 Co1 125.81(14) . . ? C1 N1 Co1 124.97(15) . . ? C1 N2 C9 125.85(19) . . ? C9 N3 C17 118.54(18) . . ? C9 N3 Co1 123.17(14) . . ? C17 N3 Co1 118.15(14) . . ? C8 N4 C18 125.87(19) . . ? C18 N5 C26 118.22(18) . . ? C18 N5 Co1 122.97(14) . . ? C26 N5 Co1 118.67(14) . . ? C58 N51 C51 108.93(18) . . ? C58 N51 Co2 126.27(15) . . ? C51 N51 Co2 124.27(15) . . ? C51 N52 C59 126.09(19) . . ? C59 N53 C67 118.28(19) . . ? C59 N53 Co2 122.29(15) . . ? C67 N53 Co2 119.28(15) . . ? C58 N54 C68 125.5(2) . . ? C68 N55 C76 118.47(19) . . ? C68 N55 Co2 122.80(15) . . ? C76 N55 Co2 118.51(15) . . ? C27 O1 Co1 132.07(17) . . ? C77 O3 Co1 136.02(14) . . ? C77 O4 Co2 136.94(15) . . ? C79 O5 Co2 134.83(16) . . ? C79 O5 H5O 111.2 . . ? Co2 O5 H5O 109.7 . . ? C91 O91 H91 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C1 C2 C7 -179.4(2) . . . . ? N1 C1 C2 C7 -0.5(2) . . . . ? N2 C1 C2 C3 0.5(4) . . . . ? N1 C1 C2 C3 179.4(2) . . . . ? C3 C2 C7 C6 0.5(3) . . . . ? C1 C2 C7 C6 -179.6(2) . . . . ? C3 C2 C7 C8 -179.1(2) . . . . ? C1 C2 C7 C8 0.8(2) . . . . ? C6 C7 C8 N4 -0.7(4) . . . . ? C2 C7 C8 N4 178.9(2) . . . . ? C6 C7 C8 N1 179.6(2) . . . . ? C2 C7 C8 N1 -0.8(2) . . . . ? C7 C2 C3 C4 -0.2(3) . . . . ? C1 C2 C3 C4 179.9(2) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C3 C4 C5 C6 0.5(4) . . . . ? C2 C7 C6 C5 -0.4(3) . . . . ? C8 C7 C6 C5 179.2(2) . . . . ? C4 C5 C6 C7 -0.2(3) . . . . ? N3 C9 C10 C11 -1.4(3) . . . . ? N2 C9 C10 C11 179.6(2) . . . . ? C9 C10 C11 C12 2.1(3) . . . . ? C10 C11 C12 C17 -0.8(3) . . . . ? C10 C11 C12 C13A 175.8(6) . . . . ? C10 C11 C12 C13B -173.9(15) . . . . ? C11 C12 C17 N3 -1.3(3) . . . . ? C13A C12 C17 N3 -177.8(6) . . . . ? C13B C12 C17 N3 171.5(15) . . . . ? C11 C12 C17 C16B 168.1(12) . . . . ? C13A C12 C17 C16B -8.4(13) . . . . ? C13B C12 C17 C16B -19.0(19) . . . . ? C11 C12 C17 C16A 179.3(4) . . . . ? C13A C12 C17 C16A 2.8(8) . . . . ? C13B C12 C17 C16A -7.8(16) . . . . ? C17 C12 C13A C14A 16.0(10) . . . . ? C11 C12 C13A C14A -160.4(5) . . . . ? C13B C12 C13A C14A 117(7) . . . . ? C12 C13A C14A C15A -46.5(9) . . . . ? C13A C14A C15A C16A 60.5(6) . . . . ? C14A C15A C16A C17 -41.9(7) . . . . ? N3 C17 C16A C15A -169.0(4) . . . . ? C12 C17 C16A C15A 10.4(8) . . . . ? C16B C17 C16A C15A 95(6) . . . . ? C17 C12 C13B C14B -2(3) . . . . ? C11 C12 C13B C14B 170.6(14) . . . . ? C13A C12 C13B C14B -87(6) . . . . ? C12 C13B C14B C15B 39(3) . . . . ? C13B C14B C15B C16B -59(2) . . . . ? C14B C15B C16B C17 39(2) . . . . ? N3 C17 C16B C15B 170.3(12) . . . . ? C12 C17 C16B C15B 0(2) . . . . ? C16A C17 C16B C15B -101(6) . . . . ? N5 C18 C19 C20 1.4(3) . . . . ? N4 C18 C19 C20 -179.5(2) . . . . ? C18 C19 C20 C21 -1.4(3) . . . . ? C19 C20 C21 C26 -0.2(3) . . . . ? C19 C20 C21 C22 179.9(2) . . . . ? C20 C21 C26 N5 2.0(3) . . . . ? C22 C21 C26 N5 -178.2(2) . . . . ? C20 C21 C26 C25 -178.1(2) . . . . ? C22 C21 C26 C25 1.7(3) . . . . ? C20 C21 C22 C23 -164.2(2) . . . . ? C26 C21 C22 C23 16.0(3) . . . . ? C21 C22 C23 C24 -48.1(3) . . . . ? C22 C23 C24 C25 64.0(3) . . . . ? N5 C26 C25 C24 -166.6(2) . . . . ? C21 C26 C25 C24 13.5(3) . . . . ? C23 C24 C25 C26 -46.2(3) . . . . ? N52 C51 C52 C53 -1.3(4) . . . . ? N51 C51 C52 C53 179.8(2) . . . . ? N52 C51 C52 C57 177.8(2) . . . . ? N51 C51 C52 C57 -1.1(2) . . . . ? C53 C52 C57 C56 0.6(3) . . . . ? C51 C52 C57 C56 -178.7(2) . . . . ? C53 C52 C57 C58 -179.5(2) . . . . ? C51 C52 C57 C58 1.3(2) . . . . ? C56 C57 C58 N54 -1.8(4) . . . . ? C52 C57 C58 N54 178.2(2) . . . . ? C56 C57 C58 N51 178.8(2) . . . . ? C52 C57 C58 N51 -1.2(2) . . . . ? C57 C52 C53 C54 0.0(3) . . . . ? C51 C52 C53 C54 179.0(2) . . . . ? C52 C53 C54 C55 -0.5(4) . . . . ? C53 C54 C55 C56 0.4(4) . . . . ? C52 C57 C56 C55 -0.6(3) . . . . ? C58 C57 C56 C55 179.4(2) . . . . ? C54 C55 C56 C57 0.1(4) . . . . ? N53 C59 C60 C61 -0.6(3) . . . . ? N52 C59 C60 C61 178.7(2) . . . . ? C59 C60 C61 C62 -2.0(4) . . . . ? C60 C61 C62 C67 1.3(3) . . . . ? C60 C61 C62 C63A -177.5(11) . . . . ? C60 C61 C62 C63B -178(5) . . . . ? C61 C62 C67 N53 2.0(3) . . . . ? C63A C62 C67 N53 -179.2(11) . . . . ? C63B C62 C67 N53 -179(5) . . . . ? C61 C62 C67 C66B -179(4) . . . . ? C63A C62 C67 C66B -1(5) . . . . ? C63B C62 C67 C66B 0(7) . . . . ? C61 C62 C67 C66A -176.3(9) . . . . ? C63A C62 C67 C66A 2.5(15) . . . . ? C63B C62 C67 C66A 3(5) . . . . ? C67 C62 C63A C64A 13(2) . . . . ? C61 C62 C63A C64A -168.2(8) . . . . ? C63B C62 C63A C64A -160(100) . . . . ? C62 C63A C64A C65A -46.2(16) . . . . ? C63A C64A C65A C66A 65.3(10) . . . . ? N53 C67 C66A C65A -162.1(7) . . . . ? C62 C67 C66A C65A 16.3(15) . . . . ? C66B C67 C66A C65A 131(26) . . . . ? C64A C65A C66A C67 -50.6(13) . . . . ? C67 C62 C63B C64B -13(9) . . . . ? C61 C62 C63B C64B 166(4) . . . . ? C63A C62 C63B C64B -7(100) . . . . ? C62 C63B C64B C65B 49(7) . . . . ? C63B C64B C65B C66B -74(4) . . . . ? N53 C67 C66B C65B 158(4) . . . . ? C62 C67 C66B C65B -20(8) . . . . ? C66A C67 C66B C65B -87(23) . . . . ? C64B C65B C66B C67 56(6) . . . . ? N55 C68 C69 C70 -0.7(4) . . . . ? N54 C68 C69 C70 -179.9(2) . . . . ? C68 C69 C70 C71 1.1(4) . . . . ? C69 C70 C71 C76 -0.4(4) . . . . ? C69 C70 C71 C72A 174.8(16) . . . . ? C69 C70 C71 C72B -177.1(15) . . . . ? C70 C71 C76 N55 -0.7(4) . . . . ? C72A C71 C76 N55 -176.1(15) . . . . ? C72B C71 C76 N55 175.6(17) . . . . ? C70 C71 C76 C75B 178.8(17) . . . . ? C72A C71 C76 C75B 3(2) . . . . ? C72B C71 C76 C75B -5(2) . . . . ? C70 C71 C76 C75A 177.9(16) . . . . ? C72A C71 C76 C75A 2(2) . . . . ? C72B C71 C76 C75A -6(2) . . . . ? C70 C71 C72A C73A -164.4(14) . . . . ? C76 C71 C72A C73A 11(3) . . . . ? C72B C71 C72A C73A 148(15) . . . . ? C71 C72A C73A C74A -43(3) . . . . ? C72A C73A C74A C75A 59.4(17) . . . . ? N55 C76 C75A C74A -164.0(15) . . . . ? C71 C76 C75A C74A 17(3) . . . . ? C75B C76 C75A C74A -50(100) . . . . ? C73A C74A C75A C76 -48(3) . . . . ? C70 C71 C72B C73B 168.2(13) . . . . ? C76 C71 C72B C73B -8(3) . . . . ? C72A C71 C72B C73B -55(11) . . . . ? C71 C72B C73B C74B 41(2) . . . . ? C72B C73B C74B C75B -64.5(18) . . . . ? N55 C76 C75B C74B 163.7(13) . . . . ? C71 C76 C75B C74B -16(3) . . . . ? C75A C76 C75B C74B 97(100) . . . . ? C73B C74B C75B C76 49(3) . . . . ? N4 C8 N1 C1 -179.2(2) . . . . ? C7 C8 N1 C1 0.5(2) . . . . ? N4 C8 N1 Co1 4.2(3) . . . . ? C7 C8 N1 Co1 -176.14(14) . . . . ? N2 C1 N1 C8 178.7(2) . . . . ? C2 C1 N1 C8 0.0(2) . . . . ? N2 C1 N1 Co1 -4.6(3) . . . . ? C2 C1 N1 Co1 176.67(14) . . . . ? O3 Co1 N1 C8 88.64(18) . . . . ? O1 Co1 N1 C8 -93.60(18) . . . . ? N3 Co1 N1 C8 178.27(17) . . . . ? N5 Co1 N1 C8 -2.97(18) . . . . ? O3 Co1 N1 C1 -87.50(18) . . . . ? O1 Co1 N1 C1 90.27(18) . . . . ? N3 Co1 N1 C1 2.13(17) . . . . ? N5 Co1 N1 C1 -179.11(17) . . . . ? N1 C1 N2 C9 1.4(4) . . . . ? C2 C1 N2 C9 180.0(2) . . . . ? N3 C9 N2 C1 4.6(3) . . . . ? C10 C9 N2 C1 -176.4(2) . . . . ? N2 C9 N3 C17 178.31(19) . . . . ? C10 C9 N3 C17 -0.6(3) . . . . ? N2 C9 N3 Co1 -6.2(3) . . . . ? C10 C9 N3 Co1 174.95(15) . . . . ? C12 C17 N3 C9 2.0(3) . . . . ? C16B C17 N3 C9 -167.8(11) . . . . ? C16A C17 N3 C9 -178.6(4) . . . . ? C12 C17 N3 Co1 -173.77(16) . . . . ? C16B C17 N3 Co1 16.4(11) . . . . ? C16A C17 N3 Co1 5.7(4) . . . . ? N1 Co1 N3 C9 2.66(17) . . . . ? O3 Co1 N3 C9 112.29(17) . . . . ? O1 Co1 N3 C9 -108.46(17) . . . . ? N5 Co1 N3 C9 -89(3) . . . . ? N1 Co1 N3 C17 178.20(16) . . . . ? O3 Co1 N3 C17 -72.17(15) . . . . ? O1 Co1 N3 C17 67.08(15) . . . . ? N5 Co1 N3 C17 86(3) . . . . ? N1 C8 N4 C18 0.4(4) . . . . ? C7 C8 N4 C18 -179.3(2) . . . . ? N5 C18 N4 C8 -5.7(3) . . . . ? C19 C18 N4 C8 175.2(2) . . . . ? N4 C18 N5 C26 -178.7(2) . . . . ? C19 C18 N5 C26 0.3(3) . . . . ? N4 C18 N5 Co1 5.6(3) . . . . ? C19 C18 N5 Co1 -175.42(16) . . . . ? C21 C26 N5 C18 -2.0(3) . . . . ? C25 C26 N5 C18 178.07(19) . . . . ? C21 C26 N5 Co1 173.84(16) . . . . ? C25 C26 N5 Co1 -6.1(3) . . . . ? N1 Co1 N5 C18 -1.42(17) . . . . ? O3 Co1 N5 C18 -111.06(17) . . . . ? O1 Co1 N5 C18 109.69(17) . . . . ? N3 Co1 N5 C18 91(3) . . . . ? N1 Co1 N5 C26 -177.08(16) . . . . ? O3 Co1 N5 C26 73.28(16) . . . . ? O1 Co1 N5 C26 -65.97(16) . . . . ? N3 Co1 N5 C26 -85(3) . . . . ? N54 C58 N51 C51 -178.8(2) . . . . ? C57 C58 N51 C51 0.5(2) . . . . ? N54 C58 N51 Co2 -6.9(3) . . . . ? C57 C58 N51 Co2 172.36(14) . . . . ? N52 C51 N51 C58 -178.4(2) . . . . ? C52 C51 N51 C58 0.3(2) . . . . ? N52 C51 N51 Co2 9.5(3) . . . . ? C52 C51 N51 Co2 -171.74(14) . . . . ? O4 Co2 N51 C58 -85.28(18) . . . . ? O5 Co2 N51 C58 88.66(18) . . . . ? N53 Co2 N51 C58 -178.18(18) . . . . ? N55 Co2 N51 C58 5.98(18) . . . . ? O4 Co2 N51 C51 85.41(18) . . . . ? O5 Co2 N51 C51 -100.64(17) . . . . ? N53 Co2 N51 C51 -7.49(17) . . . . ? N55 Co2 N51 C51 176.68(17) . . . . ? N51 C51 N52 C59 0.1(4) . . . . ? C52 C51 N52 C59 -178.5(2) . . . . ? N53 C59 N52 C51 -10.3(4) . . . . ? C60 C59 N52 C51 170.5(2) . . . . ? N52 C59 N53 C67 -175.4(2) . . . . ? C60 C59 N53 C67 3.7(3) . . . . ? N52 C59 N53 Co2 9.1(3) . . . . ? C60 C59 N53 Co2 -171.76(16) . . . . ? C62 C67 N53 C59 -4.5(3) . . . . ? C66B C67 N53 C59 177(4) . . . . ? C66A C67 N53 C59 173.8(9) . . . . ? C62 C67 N53 Co2 171.12(17) . . . . ? C66B C67 N53 Co2 -8(4) . . . . ? C66A C67 N53 Co2 -10.6(9) . . . . ? N51 Co2 N53 C59 -0.78(17) . . . . ? O4 Co2 N53 C59 -113.23(17) . . . . ? O5 Co2 N53 C59 103.07(17) . . . . ? N55 Co2 N53 C59 98.0(10) . . . . ? N51 Co2 N53 C67 -176.23(16) . . . . ? O4 Co2 N53 C67 71.32(16) . . . . ? O5 Co2 N53 C67 -72.39(17) . . . . ? N55 Co2 N53 C67 -77.5(10) . . . . ? N51 C58 N54 C68 -1.0(4) . . . . ? C57 C58 N54 C68 179.8(2) . . . . ? N55 C68 N54 C58 8.3(4) . . . . ? C69 C68 N54 C58 -172.5(2) . . . . ? N54 C68 N55 C76 178.8(2) . . . . ? C69 C68 N55 C76 -0.3(3) . . . . ? N54 C68 N55 Co2 -6.6(3) . . . . ? C69 C68 N55 Co2 174.28(16) . . . . ? C71 C76 N55 C68 1.0(3) . . . . ? C75B C76 N55 C68 -178.5(16) . . . . ? C75A C76 N55 C68 -177.6(16) . . . . ? C71 C76 N55 Co2 -173.81(17) . . . . ? C75B C76 N55 Co2 6.7(16) . . . . ? C75A C76 N55 Co2 7.5(16) . . . . ? N51 Co2 N55 C68 0.08(17) . . . . ? O4 Co2 N55 C68 112.44(17) . . . . ? O5 Co2 N55 C68 -103.88(17) . . . . ? N53 Co2 N55 C68 -98.7(10) . . . . ? N51 Co2 N55 C76 174.67(16) . . . . ? O4 Co2 N55 C76 -72.98(16) . . . . ? O5 Co2 N55 C76 70.71(16) . . . . ? N53 Co2 N55 C76 75.8(10) . . . . ? O2A C27 O1 Co1 -157.9(7) . . . . ? O2B C27 O1 Co1 171.4(7) . . . . ? C28 C27 O1 Co1 14.2(4) . . . . ? N1 Co1 O1 C27 9.2(2) . . . . ? O3 Co1 O1 C27 -174.06(19) . . . . ? N3 Co1 O1 C27 98.7(2) . . . . ? N5 Co1 O1 C27 -80.9(2) . . . . ? O4 C77 O3 Co1 171.68(15) . . . . ? C78 C77 O3 Co1 -7.8(3) . . . . ? N1 Co1 O3 C77 -11.8(2) . . . . ? O1 Co1 O3 C77 171.42(18) . . . . ? N3 Co1 O3 C77 -101.8(2) . . . . ? N5 Co1 O3 C77 78.6(2) . . . . ? O3 C77 O4 Co2 -174.31(15) . . . . ? C78 C77 O4 Co2 5.2(3) . . . . ? N51 Co2 O4 C77 12.0(2) . . . . ? O5 Co2 O4 C77 -158.07(18) . . . . ? N53 Co2 O4 C77 104.4(2) . . . . ? N55 Co2 O4 C77 -77.8(2) . . . . ? N51 Co2 O5 C79 109.4(2) . . . . ? O4 Co2 O5 C79 -80.0(2) . . . . ? N53 Co2 O5 C79 17.3(2) . . . . ? N55 Co2 O5 C79 -163.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.980 _refine_diff_density_min -0.925 _refine_diff_density_rms 0.089 _diffrn_ambient_environment 'perfluoro polyether oil' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_specimen_support 'polyimid foil' _diffrn_detector 'CCD plate' _diffrn_detector_type CCD-PXL-KAF2 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'