# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Christopher J. Ziegler' _publ_contact_author_address ; Department of Chemistry University of Akron 302 Buchtel Mall Akron OH 44325 UNITED STATES OF AMERICA ; _publ_contact_author_email ZIEGLER@UAKRON.EDU _publ_section_title ; Co(II) and Co(III) complexes of m-benziphthalocyanine ; loop_ _publ_author_name 'C. Ziegler' 'Anil Cetin' 'William S. Durfee' 'Saovalak Sripothongnak' 'Ruoqui Wu.' data_Co(mchp)py _database_code_depnum_ccdc_archive 'CCDC 641690' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H39 Co N10' _chemical_formula_weight 814.84 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' 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 P2(1)/n 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 15.4472(15) _cell_length_b 18.5201(18) _cell_length_c 16.7680(17) _cell_angle_alpha 90.00 _cell_angle_beta 116.181(2) _cell_angle_gamma 90.00 _cell_volume 4304.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9488 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.43 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 0.448 _exptl_absorpt_correction_type 'Empirical SADABS' _exptl_absorpt_correction_T_min 0.8420 _exptl_absorpt_correction_T_max 0.9783 _exptl_absorpt_process_details ? _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.860703 ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35546 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9370 _reflns_number_gt 7716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms were placed in ideal positions and were allowed for as riding atoms using the SHELXTL HFIX command, with the exception of the hydrogens on the external N atoms. The solvent disorder (half hexanes per unit cellwas refined as a diffuse contribution without specific atom positions using the SQUEEZE program, but the density, absorption coefficient and other parameters reflect the full formula. ; _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^)+(0.0632P)^2^+0.0396P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9370 _refine_ls_number_parameters 513 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.03676(11) 0.45276(8) 0.19751(10) 0.0218(3) Uani 1 1 d . . . C2 C 0.01665(12) 0.39930(8) 0.25200(11) 0.0249(3) Uani 1 1 d . . . C3 C -0.06459(13) 0.38367(9) 0.26556(12) 0.0306(4) Uani 1 1 d . . . H3 H -0.1229 0.4101 0.2360 0.037 Uiso 1 1 calc R . . C4 C -0.05673(13) 0.32772(10) 0.32425(12) 0.0339(4) Uani 1 1 d . . . H4 H -0.1106 0.3160 0.3348 0.041 Uiso 1 1 calc R . . C5 C 0.02983(13) 0.28835(9) 0.36811(12) 0.0321(4) Uani 1 1 d . . . H5 H 0.0334 0.2511 0.4083 0.038 Uiso 1 1 calc R . . C6 C 0.11014(13) 0.30316(9) 0.35351(11) 0.0296(4) Uani 1 1 d . . . H6 H 0.1681 0.2762 0.3823 0.036 Uiso 1 1 calc R . . C7 C 0.10226(12) 0.35963(8) 0.29447(11) 0.0249(3) Uani 1 1 d . . . C8 C 0.17016(11) 0.38891(8) 0.26385(10) 0.0220(3) Uani 1 1 d . . . C9 C 0.31880(11) 0.38663(8) 0.25925(10) 0.0216(3) Uani 1 1 d . . . C10 C 0.41314(11) 0.35493(8) 0.28655(10) 0.0231(3) Uani 1 1 d . . . C11 C 0.46154(12) 0.29642(8) 0.34280(11) 0.0274(4) Uani 1 1 d . . . H11 H 0.4312 0.2683 0.3707 0.033 Uiso 1 1 calc R . . C12 C 0.55493(13) 0.28151(9) 0.35573(11) 0.0301(4) Uani 1 1 d . . . H12 H 0.5887 0.2421 0.3926 0.036 Uiso 1 1 calc R . . C13 C 0.60068(13) 0.32344(9) 0.31537(11) 0.0308(4) Uani 1 1 d . . . H13 H 0.6654 0.3128 0.3274 0.037 Uiso 1 1 calc R . . C14 C 0.55326(11) 0.38008(9) 0.25830(11) 0.0255(3) Uani 1 1 d . . . H14 H 0.5840 0.4077 0.2304 0.031 Uiso 1 1 calc R . . C15 C 0.45733(11) 0.39498(8) 0.24332(10) 0.0223(3) Uani 1 1 d . . . C16 C 0.38735(11) 0.44781(8) 0.18900(10) 0.0206(3) Uani 1 1 d . . . C17 C 0.34208(10) 0.54113(8) 0.08563(10) 0.0198(3) Uani 1 1 d . . . C18 C 0.36206(11) 0.58993(8) 0.02708(10) 0.0201(3) Uani 1 1 d . . . C19 C 0.43883(11) 0.59408(8) 0.00430(10) 0.0240(3) Uani 1 1 d . . . H19 H 0.4919 0.5618 0.0292 0.029 Uiso 1 1 calc R . . C20 C 0.43495(12) 0.64720(9) -0.05621(11) 0.0268(4) Uani 1 1 d . . . H20 H 0.4864 0.6513 -0.0725 0.032 Uiso 1 1 calc R . . C21 C 0.35569(12) 0.69488(9) -0.09359(11) 0.0285(4) Uani 1 1 d . . . H21 H 0.3549 0.7307 -0.1345 0.034 Uiso 1 1 calc R . . C22 C 0.27889(11) 0.69051(9) -0.07185(10) 0.0245(3) Uani 1 1 d . . . H22 H 0.2256 0.7225 -0.0974 0.029 Uiso 1 1 calc R . . C23 C 0.28276(11) 0.63711(8) -0.01084(10) 0.0207(3) Uani 1 1 d . . . C24 C 0.21631(10) 0.61394(8) 0.02492(10) 0.0188(3) Uani 1 1 d . . . C25 C 0.05433(10) 0.62096(8) 0.01974(10) 0.0191(3) Uani 1 1 d . . . C26 C -0.03285(11) 0.65774(8) -0.03180(10) 0.0214(3) Uani 1 1 d . . . H26 H -0.0341 0.6957 -0.0704 0.026 Uiso 1 1 calc R . . C27 C -0.11649(11) 0.63840(8) -0.02589(10) 0.0222(3) Uani 1 1 d . . . H27 H -0.1760 0.6616 -0.0617 0.027 Uiso 1 1 calc R . . C28 C -0.11151(11) 0.58473(8) 0.03311(10) 0.0218(3) Uani 1 1 d . . . H28 H -0.1681 0.5705 0.0379 0.026 Uiso 1 1 calc R . . C29 C -0.02259(11) 0.55085(8) 0.08642(10) 0.0200(3) Uani 1 1 d . . . C30 C 0.06598(10) 0.56426(8) 0.08132(10) 0.0191(3) Uani 1 1 d . . . C31 C 0.28586(13) 0.55591(9) 0.34450(11) 0.0289(4) Uani 1 1 d . . . H31 H 0.2812 0.5057 0.3533 0.035 Uiso 1 1 calc R . . C32 C 0.32994(13) 0.59977(9) 0.41892(11) 0.0312(4) Uani 1 1 d . . . H32 H 0.3546 0.5797 0.4769 0.037 Uiso 1 1 calc R . . C33 C 0.33731(12) 0.67306(8) 0.40731(11) 0.0267(3) Uani 1 1 d . . . H33 H 0.3681 0.7042 0.4570 0.032 Uiso 1 1 calc R . . C34 C 0.29850(12) 0.70002(9) 0.32102(11) 0.0277(4) Uani 1 1 d . . . H34 H 0.3015 0.7502 0.3106 0.033 Uiso 1 1 calc R . . C35 C 0.25548(11) 0.65256(8) 0.25057(10) 0.0236(3) Uani 1 1 d . . . H35 H 0.2288 0.6716 0.1920 0.028 Uiso 1 1 calc R . . C36 C 0.38541(13) 0.34438(10) 0.51381(12) 0.0371(4) Uani 1 1 d . . . H36 H 0.3460 0.3314 0.4537 0.045 Uiso 1 1 calc R . . C37 C 0.41443(18) 0.41556(11) 0.53266(16) 0.0578(6) Uani 1 1 d . . . H37 H 0.3978 0.4498 0.4860 0.069 Uiso 1 1 calc R . . C38 C 0.46799(17) 0.43637(11) 0.62034(16) 0.0541(6) Uani 1 1 d . . . H38 H 0.4864 0.4853 0.6353 0.065 Uiso 1 1 calc R . . C39 C 0.49374(13) 0.38423(11) 0.68513(13) 0.0390(5) Uani 1 1 d . . . H39 H 0.5310 0.3963 0.7459 0.047 Uiso 1 1 calc R . . C40 C 0.46430(13) 0.31355(10) 0.66013(11) 0.0337(4) Uani 1 1 d . . . H40 H 0.4837 0.2777 0.7052 0.040 Uiso 1 1 calc R . . C41 C 0.27801(12) 0.48448(9) 0.81678(12) 0.0293(4) Uani 1 1 d . . . H41 H 0.2885 0.5350 0.8250 0.035 Uiso 1 1 calc R . . C42 C 0.34645(13) 0.44357(10) 0.80544(13) 0.0377(4) Uani 1 1 d . . . H42 H 0.4016 0.4657 0.8047 0.045 Uiso 1 1 calc R . . C43 C 0.33288(16) 0.36906(11) 0.79510(16) 0.0490(5) Uani 1 1 d . . . H43 H 0.3793 0.3391 0.7886 0.059 Uiso 1 1 calc R . . C44 C 0.25045(17) 0.33992(11) 0.79452(14) 0.0462(5) Uani 1 1 d . . . H44 H 0.2389 0.2894 0.7872 0.055 Uiso 1 1 calc R . . C45 C 0.18448(14) 0.38551(10) 0.80473(12) 0.0355(4) Uani 1 1 d . . . H45 H 0.1273 0.3650 0.8031 0.043 Uiso 1 1 calc R . . Co1 Co 0.187811(14) 0.508089(10) 0.147045(13) 0.01730(7) Uani 1 1 d . . . H6N H 0.1200(13) 0.6864(10) -0.0298(12) 0.027(5) Uiso 1 1 d . . . H7N H -0.0759(15) 0.5016(9) 0.1513(14) 0.029(6) Uiso 1 1 d . . . N1 N 0.12644(9) 0.44717(6) 0.20443(8) 0.0205(3) Uani 1 1 d . . . N2 N 0.25649(9) 0.36159(7) 0.28922(9) 0.0231(3) Uani 1 1 d . . . N3 N 0.30424(9) 0.44306(6) 0.20049(8) 0.0197(3) Uani 1 1 d . . . N4 N 0.40499(9) 0.49304(6) 0.13468(9) 0.0201(3) Uani 1 1 d . . . N5 N 0.25027(9) 0.55734(6) 0.08121(8) 0.0188(3) Uani 1 1 d . . . N6 N 0.13093(9) 0.64579(7) 0.00258(9) 0.0209(3) Uani 1 1 d . . . N7 N -0.02965(11) 0.50047(7) 0.14627(10) 0.0230(3) Uani 1 1 d . . . N8 N 0.24935(9) 0.58083(7) 0.26050(8) 0.0206(3) Uani 1 1 d . . . N9 N 0.40993(10) 0.29324(7) 0.57570(9) 0.0257(3) Uani 1 1 d . . . N10 N 0.19759(10) 0.45725(8) 0.81687(10) 0.0316(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0227(8) 0.0185(7) 0.0234(8) -0.0019(6) 0.0095(7) -0.0028(6) C2 0.0258(8) 0.0216(8) 0.0271(8) -0.0010(6) 0.0115(7) -0.0037(6) C3 0.0285(9) 0.0288(9) 0.0364(10) 0.0021(7) 0.0160(8) -0.0022(7) C4 0.0340(10) 0.0351(10) 0.0357(10) 0.0012(8) 0.0183(8) -0.0079(8) C5 0.0369(10) 0.0296(9) 0.0271(9) 0.0048(7) 0.0118(8) -0.0089(8) C6 0.0315(9) 0.0263(9) 0.0258(8) 0.0037(7) 0.0079(7) -0.0053(7) C7 0.0252(8) 0.0226(8) 0.0231(8) -0.0013(6) 0.0072(7) -0.0061(6) C8 0.0226(8) 0.0180(7) 0.0212(8) -0.0001(6) 0.0057(6) -0.0048(6) C9 0.0229(8) 0.0163(7) 0.0200(8) 0.0000(6) 0.0044(6) -0.0003(6) C10 0.0225(8) 0.0196(8) 0.0216(8) -0.0016(6) 0.0047(7) 0.0005(6) C11 0.0308(9) 0.0215(8) 0.0256(8) 0.0016(6) 0.0085(7) 0.0027(7) C12 0.0334(9) 0.0260(9) 0.0241(8) 0.0041(7) 0.0065(7) 0.0127(7) C13 0.0265(9) 0.0322(9) 0.0289(9) 0.0003(7) 0.0079(7) 0.0109(7) C14 0.0233(8) 0.0253(8) 0.0253(8) 0.0005(6) 0.0082(7) 0.0060(7) C15 0.0225(8) 0.0195(7) 0.0189(7) -0.0025(6) 0.0036(6) 0.0023(6) C16 0.0182(7) 0.0186(7) 0.0210(8) -0.0034(6) 0.0049(6) 0.0002(6) C17 0.0174(7) 0.0178(7) 0.0211(8) -0.0042(6) 0.0058(6) -0.0017(6) C18 0.0195(7) 0.0177(7) 0.0191(7) -0.0031(6) 0.0050(6) -0.0023(6) C19 0.0205(8) 0.0249(8) 0.0248(8) -0.0031(6) 0.0084(7) -0.0004(6) C20 0.0237(8) 0.0319(9) 0.0263(8) -0.0038(7) 0.0123(7) -0.0055(7) C21 0.0290(9) 0.0300(9) 0.0260(8) 0.0048(7) 0.0117(7) -0.0009(7) C22 0.0226(8) 0.0259(8) 0.0218(8) 0.0033(6) 0.0070(7) 0.0010(6) C23 0.0197(7) 0.0202(7) 0.0193(7) -0.0031(6) 0.0060(6) -0.0012(6) C24 0.0180(7) 0.0168(7) 0.0186(7) -0.0009(6) 0.0052(6) -0.0010(6) C25 0.0159(7) 0.0194(7) 0.0191(7) -0.0039(6) 0.0049(6) -0.0007(6) C26 0.0214(8) 0.0182(7) 0.0203(7) 0.0008(6) 0.0054(6) 0.0018(6) C27 0.0179(7) 0.0206(8) 0.0229(8) -0.0040(6) 0.0042(6) 0.0017(6) C28 0.0170(7) 0.0212(8) 0.0256(8) -0.0052(6) 0.0078(6) -0.0018(6) C29 0.0206(7) 0.0153(7) 0.0220(8) -0.0026(6) 0.0076(6) -0.0013(6) C30 0.0182(7) 0.0168(7) 0.0191(7) -0.0042(6) 0.0055(6) -0.0028(6) C31 0.0393(10) 0.0181(8) 0.0248(8) 0.0000(6) 0.0099(7) -0.0037(7) C32 0.0412(10) 0.0240(8) 0.0210(8) 0.0007(6) 0.0070(8) -0.0006(7) C33 0.0272(9) 0.0225(8) 0.0251(8) -0.0064(6) 0.0067(7) -0.0038(7) C34 0.0335(9) 0.0170(8) 0.0293(9) -0.0009(6) 0.0107(7) -0.0030(7) C35 0.0240(8) 0.0209(8) 0.0216(8) 0.0011(6) 0.0062(7) 0.0012(6) C36 0.0336(10) 0.0372(10) 0.0274(9) -0.0034(8) 0.0015(8) -0.0005(8) C37 0.0659(15) 0.0298(11) 0.0544(14) 0.0092(10) 0.0053(12) 0.0022(10) C38 0.0559(14) 0.0261(10) 0.0657(15) -0.0156(10) 0.0136(12) -0.0054(9) C39 0.0299(9) 0.0513(12) 0.0315(10) -0.0204(9) 0.0096(8) -0.0069(9) C40 0.0322(9) 0.0385(10) 0.0262(9) 0.0004(7) 0.0091(8) 0.0004(8) C41 0.0261(9) 0.0268(9) 0.0320(9) 0.0000(7) 0.0102(8) -0.0028(7) C42 0.0286(9) 0.0355(10) 0.0525(12) 0.0035(9) 0.0211(9) -0.0009(8) C43 0.0553(13) 0.0341(11) 0.0759(16) -0.0007(10) 0.0458(13) 0.0045(9) C44 0.0644(14) 0.0286(10) 0.0585(13) -0.0098(9) 0.0389(12) -0.0104(9) C45 0.0353(10) 0.0379(10) 0.0363(10) -0.0073(8) 0.0184(8) -0.0127(8) Co1 0.01551(11) 0.01500(11) 0.01851(12) 0.00020(7) 0.00490(9) -0.00044(7) N1 0.0189(6) 0.0178(6) 0.0209(6) -0.0009(5) 0.0052(5) -0.0007(5) N2 0.0228(7) 0.0185(6) 0.0229(7) 0.0003(5) 0.0053(6) -0.0021(5) N3 0.0191(6) 0.0158(6) 0.0202(6) -0.0015(5) 0.0051(5) -0.0006(5) N4 0.0191(6) 0.0176(6) 0.0219(7) -0.0011(5) 0.0074(6) 0.0009(5) N5 0.0168(6) 0.0164(6) 0.0194(6) -0.0015(5) 0.0043(5) -0.0005(5) N6 0.0195(6) 0.0181(7) 0.0235(7) 0.0041(5) 0.0081(6) 0.0016(5) N7 0.0192(7) 0.0230(7) 0.0293(8) 0.0016(5) 0.0129(6) 0.0007(5) N8 0.0187(6) 0.0184(6) 0.0217(7) -0.0006(5) 0.0061(5) -0.0005(5) N9 0.0212(7) 0.0253(7) 0.0294(7) -0.0049(6) 0.0099(6) -0.0016(5) N10 0.0285(8) 0.0314(8) 0.0372(8) -0.0021(6) 0.0167(7) -0.0026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N7 1.339(2) . ? C1 N1 1.3422(19) . ? C1 C2 1.470(2) . ? C2 C3 1.401(2) . ? C2 C7 1.402(2) . ? C3 C4 1.397(2) . ? C3 H3 0.9500 . ? C4 C5 1.412(3) . ? C4 H4 0.9500 . ? C5 C6 1.394(2) . ? C5 H5 0.9500 . ? C6 C7 1.408(2) . ? C6 H6 0.9500 . ? C7 C8 1.461(2) . ? C8 N2 1.309(2) . ? C8 N1 1.4210(19) . ? C9 N2 1.349(2) . ? C9 N3 1.3849(19) . ? C9 C10 1.445(2) . ? C10 C15 1.407(2) . ? C10 C11 1.414(2) . ? C11 C12 1.389(2) . ? C11 H11 0.9500 . ? C12 C13 1.408(3) . ? C12 H12 0.9500 . ? C13 C14 1.391(2) . ? C13 H13 0.9500 . ? C14 C15 1.417(2) . ? C14 H14 0.9500 . ? C15 C16 1.444(2) . ? C16 N4 1.351(2) . ? C16 N3 1.3824(19) . ? C17 N4 1.3072(19) . ? C17 N5 1.4193(18) . ? C17 C18 1.464(2) . ? C18 C19 1.399(2) . ? C18 C23 1.407(2) . ? C19 C20 1.395(2) . ? C19 H19 0.9500 . ? C20 C21 1.412(2) . ? C20 H20 0.9500 . ? C21 C22 1.389(2) . ? C21 H21 0.9500 . ? C22 C23 1.405(2) . ? C22 H22 0.9500 . ? C23 C24 1.463(2) . ? C24 N6 1.3385(19) . ? C24 N5 1.3520(19) . ? C25 N6 1.4124(19) . ? C25 C26 1.413(2) . ? C25 C30 1.427(2) . ? C26 C27 1.386(2) . ? C26 H26 0.9500 . ? C27 C28 1.380(2) . ? C27 H27 0.9500 . ? C28 C29 1.413(2) . ? C28 H28 0.9500 . ? C29 N7 1.409(2) . ? C29 C30 1.430(2) . ? C30 Co1 2.0020(15) . ? C31 N8 1.347(2) . ? C31 C32 1.390(2) . ? C31 H31 0.9500 . ? C32 C33 1.383(2) . ? C32 H32 0.9500 . ? C33 C34 1.392(2) . ? C33 H33 0.9500 . ? C34 C35 1.384(2) . ? C34 H34 0.9500 . ? C35 N8 1.3475(19) . ? C35 H35 0.9500 . ? C36 N9 1.331(2) . ? C36 C37 1.383(3) . ? C36 H36 0.9500 . ? C37 C38 1.386(3) . ? C37 H37 0.9500 . ? C38 C39 1.375(3) . ? C38 H38 0.9500 . ? C39 C40 1.388(3) . ? C39 H39 0.9500 . ? C40 N9 1.342(2) . ? C40 H40 0.9500 . ? C41 N10 1.341(2) . ? C41 C42 1.380(2) . ? C41 H41 0.9500 . ? C42 C43 1.395(3) . ? C42 H42 0.9500 . ? C43 C44 1.379(3) . ? C43 H43 0.9500 . ? C44 C45 1.391(3) . ? C44 H44 0.9500 . ? C45 N10 1.346(2) . ? C45 H45 0.9500 . ? Co1 N1 1.9754(13) . ? Co1 N5 1.9802(13) . ? Co1 N3 2.0164(12) . ? Co1 N8 2.1775(13) . ? N6 H6N 0.899(18) . ? N7 H7N 0.76(2) . ? 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 N7 C1 N1 125.14(14) . . ? N7 C1 C2 122.07(14) . . ? N1 C1 C2 112.79(13) . . ? C3 C2 C7 121.40(15) . . ? C3 C2 C1 133.63(15) . . ? C7 C2 C1 104.96(14) . . ? C4 C3 C2 117.52(16) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C3 C4 C5 121.20(16) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 121.26(16) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C7 117.52(16) . . ? C5 C6 H6 121.2 . . ? C7 C6 H6 121.2 . . ? C2 C7 C6 121.08(15) . . ? C2 C7 C8 106.83(14) . . ? C6 C7 C8 132.09(15) . . ? N2 C8 N1 128.46(14) . . ? N2 C8 C7 121.92(14) . . ? N1 C8 C7 109.61(13) . . ? N2 C9 N3 127.27(14) . . ? N2 C9 C10 121.84(14) . . ? N3 C9 C10 110.88(13) . . ? C15 C10 C11 120.91(15) . . ? C15 C10 C9 105.86(13) . . ? C11 C10 C9 133.23(15) . . ? C12 C11 C10 117.63(15) . . ? C12 C11 H11 121.2 . . ? C10 C11 H11 121.2 . . ? C11 C12 C13 121.48(15) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C14 C13 C12 121.54(16) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 117.46(15) . . ? C13 C14 H14 121.3 . . ? C15 C14 H14 121.3 . . ? C10 C15 C14 120.89(14) . . ? C10 C15 C16 106.48(14) . . ? C14 C15 C16 132.62(15) . . ? N4 C16 N3 127.55(13) . . ? N4 C16 C15 121.85(14) . . ? N3 C16 C15 110.59(13) . . ? N4 C17 N5 128.70(14) . . ? N4 C17 C18 121.63(13) . . ? N5 C17 C18 109.62(12) . . ? C19 C18 C23 121.07(14) . . ? C19 C18 C17 132.20(14) . . ? C23 C18 C17 106.70(13) . . ? C20 C19 C18 117.87(15) . . ? C20 C19 H19 121.1 . . ? C18 C19 H19 121.1 . . ? C19 C20 C21 120.95(15) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C22 C21 C20 121.38(15) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 117.73(15) . . ? C21 C22 H22 121.1 . . ? C23 C22 H22 121.1 . . ? C22 C23 C18 120.99(14) . . ? C22 C23 C24 133.84(14) . . ? C18 C23 C24 105.12(13) . . ? N6 C24 N5 124.61(13) . . ? N6 C24 C23 122.60(13) . . ? N5 C24 C23 112.79(13) . . ? N6 C25 C26 112.11(13) . . ? N6 C25 C30 122.50(13) . . ? C26 C25 C30 125.37(14) . . ? C27 C26 C25 119.91(14) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 118.58(14) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C27 C28 C29 120.30(14) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? N7 C29 C28 112.67(13) . . ? N7 C29 C30 122.30(14) . . ? C28 C29 C30 125.02(14) . . ? C25 C30 C29 110.64(13) . . ? C25 C30 Co1 124.64(11) . . ? C29 C30 Co1 124.66(11) . . ? N8 C31 C32 123.51(15) . . ? N8 C31 H31 118.2 . . ? C32 C31 H31 118.2 . . ? C33 C32 C31 119.04(15) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C32 C33 C34 118.29(15) . . ? C32 C33 H33 120.9 . . ? C34 C33 H33 120.9 . . ? C35 C34 C33 118.93(15) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? N8 C35 C34 123.64(15) . . ? N8 C35 H35 118.2 . . ? C34 C35 H35 118.2 . . ? N9 C36 C37 123.23(18) . . ? N9 C36 H36 118.4 . . ? C37 C36 H36 118.4 . . ? C36 C37 C38 119.3(2) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C39 C38 C37 118.18(18) . . ? C39 C38 H38 120.9 . . ? C37 C38 H38 120.9 . . ? C38 C39 C40 118.79(17) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? N9 C40 C39 123.49(17) . . ? N9 C40 H40 118.3 . . ? C39 C40 H40 118.3 . . ? N10 C41 C42 124.04(16) . . ? N10 C41 H41 118.0 . . ? C42 C41 H41 118.0 . . ? C41 C42 C43 118.54(17) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? C44 C43 C42 118.40(18) . . ? C44 C43 H43 120.8 . . ? C42 C43 H43 120.8 . . ? C43 C44 C45 119.07(18) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? N10 C45 C44 123.26(17) . . ? N10 C45 H45 118.4 . . ? C44 C45 H45 118.4 . . ? N1 Co1 N5 172.38(5) . . ? N1 Co1 C30 91.62(6) . . ? N5 Co1 C30 91.41(6) . . ? N1 Co1 N3 88.17(5) . . ? N5 Co1 N3 87.96(5) . . ? C30 Co1 N3 172.96(5) . . ? N1 Co1 N8 92.64(5) . . ? N5 Co1 N8 94.00(5) . . ? C30 Co1 N8 95.82(5) . . ? N3 Co1 N8 91.22(5) . . ? C1 N1 C8 105.79(12) . . ? C1 N1 Co1 127.79(10) . . ? C8 N1 Co1 126.40(10) . . ? C8 N2 C9 122.53(14) . . ? C16 N3 C9 106.13(12) . . ? C16 N3 Co1 126.95(10) . . ? C9 N3 Co1 126.86(10) . . ? C17 N4 C16 122.12(13) . . ? C24 N5 C17 105.75(12) . . ? C24 N5 Co1 127.73(10) . . ? C17 N5 Co1 126.50(10) . . ? C24 N6 C25 127.59(13) . . ? C24 N6 H6N 116.0(11) . . ? C25 N6 H6N 116.3(11) . . ? C1 N7 C29 128.00(14) . . ? C1 N7 H7N 116.1(15) . . ? C29 N7 H7N 115.8(15) . . ? C31 N8 C35 116.56(13) . . ? C31 N8 Co1 121.44(10) . . ? C35 N8 Co1 121.97(10) . . ? C36 N9 C40 116.97(15) . . ? C41 N10 C45 116.65(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.681 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.062 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr 2 _platon_squeeze_void_average_x 0.500 _platon_squeeze_void_average_y 0.000 _platon_squeeze_void_average_z 1.000 _platon_squeeze_void_volume 487.7 _platon_squeeze_void_count_electrons 103.7 _platon_squeeze_details ; ; # Attachment '641691.cif' data_Co(mchp)py2 _database_code_depnum_ccdc_archive 'CCDC 641691' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H41 Co N12' _chemical_formula_weight 928.94 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' 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 P2(1)/c 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 9.9002(16) _cell_length_b 10.0469(16) _cell_length_c 44.850(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.700(3) _cell_angle_gamma 90.00 _cell_volume 4451.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2881 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 23.14 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1932 _exptl_absorpt_coefficient_mu 0.441 _exptl_absorpt_correction_type 'Empirical SADABS' _exptl_absorpt_correction_T_min 0.6374 _exptl_absorpt_correction_T_max 0.9957 _exptl_absorpt_process_details ? _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.640193 ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37698 _diffrn_reflns_av_R_equivalents 0.0990 _diffrn_reflns_av_sigmaI/netI 0.1218 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -59 _diffrn_reflns_limit_l_max 59 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 28.36 _reflns_number_total 10627 _reflns_number_gt 5951 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms were placed in ideal positions and were allowed for as riding atoms using the SHELXTL HFIX command. The solvent disorder (one pyridine per unit cell) was refined as a diffuse contribution without specific atom positions using the SQUEEZE program, but the density, absorption coefficient and other parameters reflect the full formula. ; _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^)+(0.0857P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10627 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1369 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.1835 _refine_ls_wR_factor_gt 0.1626 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3971(4) 0.3429(4) 0.80402(8) 0.0248(8) Uani 1 1 d . . . C2 C 0.4809(4) 0.4202(4) 0.78446(8) 0.0278(9) Uani 1 1 d . . . C3 C 0.4597(4) 0.4631(4) 0.75470(9) 0.0313(9) Uani 1 1 d . . . H3 H 0.3817 0.4369 0.7427 0.038 Uiso 1 1 calc R . . C4 C 0.5572(5) 0.5449(4) 0.74364(9) 0.0369(10) Uani 1 1 d . . . H4 H 0.5452 0.5762 0.7236 0.044 Uiso 1 1 calc R . . C5 C 0.6724(4) 0.5828(4) 0.76104(9) 0.0336(10) Uani 1 1 d . . . H5 H 0.7360 0.6416 0.7530 0.040 Uiso 1 1 calc R . . C6 C 0.6952(4) 0.5352(4) 0.79001(9) 0.0276(9) Uani 1 1 d . . . H6 H 0.7753 0.5575 0.8017 0.033 Uiso 1 1 calc R . . C7 C 0.5975(4) 0.4544(4) 0.80126(8) 0.0260(8) Uani 1 1 d . . . C8 C 0.5880(4) 0.3935(4) 0.83099(9) 0.0251(8) Uani 1 1 d . . . C9 C 0.6866(4) 0.3336(4) 0.87731(8) 0.0258(8) Uani 1 1 d . . . C10 C 0.8018(4) 0.3320(4) 0.89846(8) 0.0251(8) Uani 1 1 d . . . C11 C 0.9289(4) 0.3917(4) 0.89975(9) 0.0293(9) Uani 1 1 d . . . H11 H 0.9536 0.4504 0.8844 0.035 Uiso 1 1 calc R . . C12 C 1.0185(4) 0.3634(4) 0.92388(9) 0.0333(10) Uani 1 1 d . . . H12 H 1.1051 0.4045 0.9253 0.040 Uiso 1 1 calc R . . C13 C 0.9833(4) 0.2747(4) 0.94637(9) 0.0345(10) Uani 1 1 d . . . H13 H 1.0474 0.2559 0.9625 0.041 Uiso 1 1 calc R . . C14 C 0.8581(4) 0.2143(4) 0.94560(9) 0.0302(9) Uani 1 1 d . . . H14 H 0.8353 0.1548 0.9610 0.036 Uiso 1 1 calc R . . C15 C 0.7650(4) 0.2430(4) 0.92147(8) 0.0261(8) Uani 1 1 d . . . C16 C 0.6307(4) 0.2001(4) 0.91359(8) 0.0226(8) Uani 1 1 d . . . C17 C 0.4346(4) 0.0842(4) 0.92396(8) 0.0246(8) Uani 1 1 d . . . C18 C 0.3612(4) -0.0004(4) 0.94314(8) 0.0233(8) Uani 1 1 d . . . C19 C 0.4044(4) -0.0733(4) 0.96845(8) 0.0267(8) Uani 1 1 d . . . H19 H 0.4969 -0.0742 0.9756 0.032 Uiso 1 1 calc R . . C20 C 0.3074(4) -0.1447(4) 0.98292(9) 0.0345(10) Uani 1 1 d . . . H20 H 0.3341 -0.1957 1.0001 0.041 Uiso 1 1 calc R . . C21 C 0.1707(4) -0.1422(4) 0.97239(9) 0.0339(10) Uani 1 1 d . . . H21 H 0.1059 -0.1902 0.9829 0.041 Uiso 1 1 calc R . . C22 C 0.1287(4) -0.0708(4) 0.94694(9) 0.0291(9) Uani 1 1 d . . . H22 H 0.0362 -0.0691 0.9398 0.035 Uiso 1 1 calc R . . C23 C 0.2263(4) -0.0017(4) 0.93223(8) 0.0245(8) Uani 1 1 d . . . C24 C 0.2233(4) 0.0790(3) 0.90491(8) 0.0231(8) Uani 1 1 d . . . C25 C 0.1028(4) 0.1540(4) 0.85816(8) 0.0228(8) Uani 1 1 d . . . C26 C -0.0293(4) 0.1504(4) 0.84470(9) 0.0270(9) Uani 1 1 d . . . H26 H -0.1016 0.1178 0.8556 0.032 Uiso 1 1 calc R . . C27 C -0.0543(4) 0.1943(4) 0.81559(9) 0.0301(9) Uani 1 1 d . . . H27 H -0.1433 0.1932 0.8063 0.036 Uiso 1 1 calc R . . C28 C 0.0531(4) 0.2395(4) 0.80043(9) 0.0301(9) Uani 1 1 d . . . H28 H 0.0382 0.2653 0.7801 0.036 Uiso 1 1 calc R . . C29 C 0.1850(4) 0.2486(3) 0.81432(8) 0.0239(8) Uani 1 1 d . . . C30 C 0.2159(4) 0.2080(3) 0.84449(8) 0.0232(8) Uani 1 1 d . . . C31 C 0.3799(4) -0.0459(4) 0.84361(8) 0.0285(9) Uani 1 1 d . . . H31 H 0.2908 -0.0413 0.8503 0.034 Uiso 1 1 calc R . . C32 C 0.4208(4) -0.1626(4) 0.83061(9) 0.0330(10) Uani 1 1 d . . . H32 H 0.3608 -0.2362 0.8284 0.040 Uiso 1 1 calc R . . C33 C 0.5498(4) -0.1708(4) 0.82079(9) 0.0341(10) Uani 1 1 d . . . H33 H 0.5799 -0.2498 0.8116 0.041 Uiso 1 1 calc R . . C34 C 0.6347(4) -0.0616(4) 0.82458(9) 0.0320(9) Uani 1 1 d . . . H34 H 0.7246 -0.0649 0.8184 0.038 Uiso 1 1 calc R . . C35 C 0.5865(4) 0.0524(4) 0.83755(8) 0.0290(9) Uani 1 1 d . . . H35 H 0.6445 0.1276 0.8397 0.035 Uiso 1 1 calc R . . C36 C 0.2686(4) 0.4903(4) 0.86719(10) 0.0320(9) Uani 1 1 d . . . H36 H 0.2373 0.4693 0.8473 0.038 Uiso 1 1 calc R . . C37 C 0.2361(4) 0.6132(4) 0.87870(11) 0.0388(11) Uani 1 1 d . . . H37 H 0.1833 0.6746 0.8668 0.047 Uiso 1 1 calc R . . C38 C 0.2805(5) 0.6462(4) 0.90736(11) 0.0412(11) Uani 1 1 d . . . H38 H 0.2597 0.7304 0.9156 0.049 Uiso 1 1 calc R . . C39 C 0.3561(4) 0.5538(4) 0.92396(10) 0.0373(11) Uani 1 1 d . . . H39 H 0.3893 0.5745 0.9438 0.045 Uiso 1 1 calc R . . C40 C 0.3835(4) 0.4314(4) 0.91177(9) 0.0275(9) Uani 1 1 d . . . H40 H 0.4324 0.3676 0.9238 0.033 Uiso 1 1 calc R . . C41 C 0.7659(4) 0.8972(4) 0.90960(10) 0.0367(10) Uani 1 1 d . . . H41 H 0.7522 0.9639 0.9241 0.044 Uiso 1 1 calc R . . C42 C 0.6711(5) 0.7963(5) 0.90606(11) 0.0451(12) Uani 1 1 d . . . H42 H 0.5931 0.7965 0.9173 0.054 Uiso 1 1 calc R . . C43 C 0.6913(5) 0.6956(4) 0.88597(10) 0.0426(11) Uani 1 1 d . . . H43 H 0.6285 0.6244 0.8833 0.051 Uiso 1 1 calc R . . C44 C 0.8062(5) 0.7011(4) 0.86974(10) 0.0381(11) Uani 1 1 d . . . H44 H 0.8247 0.6330 0.8559 0.046 Uiso 1 1 calc R . . C45 C 0.8934(4) 0.8088(4) 0.87430(9) 0.0375(10) Uani 1 1 d . . . H45 H 0.9705 0.8131 0.8628 0.045 Uiso 1 1 calc R . . C46 C 0.0720(6) 0.6152(5) 0.79498(12) 0.0550(14) Uani 1 1 d . . . H46 H 0.0531 0.5262 0.8005 0.066 Uiso 1 1 calc R . . C47 C 0.1600(5) 0.6335(5) 0.77352(11) 0.0492(13) Uani 1 1 d . . . H47 H 0.2014 0.5598 0.7645 0.059 Uiso 1 1 calc R . . C48 C 0.1878(5) 0.7616(6) 0.76517(12) 0.0566(14) Uani 1 1 d . . . H48 H 0.2489 0.7783 0.7501 0.068 Uiso 1 1 calc R . . C49 C 0.1259(5) 0.8653(5) 0.77891(11) 0.0431(11) Uani 1 1 d . . . H49 H 0.1433 0.9549 0.7736 0.052 Uiso 1 1 calc R . . C50 C 0.0398(5) 0.8364(5) 0.80012(12) 0.0536(14) Uani 1 1 d . . . H50 H -0.0024 0.9087 0.8095 0.064 Uiso 1 1 calc R . . Co1 Co 0.39931(5) 0.22930(5) 0.865353(11) 0.02214(15) Uani 1 1 d . . . H1 H 0.031(4) 0.060(4) 0.8927(8) 0.027(11) Uiso 1 1 d . . . N1 N 0.4650(3) 0.3273(3) 0.83185(7) 0.0237(7) Uani 1 1 d . . . N2 N 0.6885(3) 0.4011(3) 0.85099(7) 0.0259(7) Uani 1 1 d . . . N3 N 0.5837(3) 0.2556(3) 0.88615(6) 0.0233(7) Uani 1 1 d . . . N4 N 0.5615(3) 0.1179(3) 0.93047(7) 0.0262(7) Uani 1 1 d . . . N5 N 0.3446(3) 0.1287(3) 0.90003(6) 0.0227(7) Uani 1 1 d . . . N6 N 0.1125(3) 0.0937(3) 0.88675(7) 0.0261(7) Uani 1 1 d . . . N7 N 0.2741(3) 0.3071(3) 0.79520(7) 0.0267(7) Uani 1 1 d . . . N8 N 0.4600(3) 0.0615(3) 0.84730(7) 0.0238(7) Uani 1 1 d . . . N9 N 0.3427(3) 0.3990(3) 0.88308(7) 0.0245(7) Uani 1 1 d . . . N10 N 0.8757(3) 0.9066(3) 0.89383(7) 0.0313(8) Uani 1 1 d . . . N11 N 0.0094(5) 0.7126(5) 0.80896(11) 0.0708(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 C1 0.031(2) 0.023(2) 0.0213(19) -0.0003(15) 0.0050(16) 0.0048(17) C2 0.031(2) 0.026(2) 0.026(2) -0.0049(16) 0.0027(17) 0.0060(17) C3 0.033(2) 0.036(2) 0.025(2) 0.0017(17) 0.0044(17) 0.0066(19) C4 0.051(3) 0.035(2) 0.025(2) 0.0020(18) 0.007(2) 0.004(2) C5 0.041(3) 0.029(2) 0.033(2) -0.0019(18) 0.0133(19) 0.0003(19) C6 0.029(2) 0.025(2) 0.030(2) -0.0009(16) 0.0065(17) 0.0018(17) C7 0.031(2) 0.022(2) 0.025(2) -0.0030(15) 0.0059(17) 0.0056(16) C8 0.027(2) 0.0164(18) 0.032(2) -0.0021(16) 0.0038(17) 0.0015(16) C9 0.030(2) 0.0220(19) 0.026(2) -0.0042(16) 0.0018(16) 0.0020(17) C10 0.025(2) 0.024(2) 0.027(2) -0.0049(16) 0.0048(16) -0.0013(16) C11 0.030(2) 0.031(2) 0.027(2) -0.0022(17) 0.0040(17) -0.0006(18) C12 0.025(2) 0.038(2) 0.037(2) -0.0074(19) -0.0013(18) -0.0048(18) C13 0.030(2) 0.041(2) 0.032(2) -0.005(2) -0.0039(18) 0.002(2) C14 0.027(2) 0.039(2) 0.025(2) -0.0008(18) -0.0010(16) 0.0026(18) C15 0.028(2) 0.029(2) 0.0218(19) -0.0056(16) 0.0036(16) 0.0028(16) C16 0.0216(19) 0.023(2) 0.0240(19) -0.0018(15) 0.0044(15) -0.0036(15) C17 0.025(2) 0.022(2) 0.027(2) -0.0025(15) 0.0032(16) -0.0014(16) C18 0.0232(19) 0.025(2) 0.0218(19) -0.0024(15) 0.0048(15) -0.0001(16) C19 0.029(2) 0.028(2) 0.0223(19) 0.0022(16) 0.0015(16) 0.0015(17) C20 0.037(2) 0.037(2) 0.030(2) 0.0045(18) 0.0029(19) 0.0018(19) C21 0.035(2) 0.031(2) 0.036(2) 0.0051(18) 0.0086(19) -0.0026(19) C22 0.028(2) 0.030(2) 0.030(2) 0.0020(17) 0.0035(17) -0.0008(17) C23 0.031(2) 0.0213(19) 0.0216(19) -0.0027(15) 0.0020(16) 0.0014(16) C24 0.027(2) 0.0186(19) 0.0236(19) -0.0049(15) 0.0024(16) -0.0029(16) C25 0.027(2) 0.0172(18) 0.025(2) -0.0002(15) 0.0035(16) 0.0010(15) C26 0.025(2) 0.024(2) 0.032(2) -0.0011(16) 0.0026(17) -0.0031(16) C27 0.033(2) 0.026(2) 0.031(2) 0.0002(16) -0.0030(18) -0.0015(17) C28 0.036(2) 0.025(2) 0.029(2) -0.0009(16) -0.0023(17) 0.0007(18) C29 0.026(2) 0.0157(19) 0.030(2) -0.0031(15) 0.0015(16) 0.0026(15) C30 0.028(2) 0.0132(18) 0.028(2) -0.0045(15) -0.0008(16) 0.0017(15) C31 0.032(2) 0.024(2) 0.029(2) 0.0014(16) -0.0012(17) -0.0013(17) C32 0.041(3) 0.024(2) 0.034(2) -0.0033(18) 0.0010(19) -0.0005(18) C33 0.039(2) 0.027(2) 0.036(2) -0.0078(18) 0.0023(19) 0.0064(19) C34 0.034(2) 0.034(2) 0.028(2) -0.0001(18) 0.0056(18) 0.0074(19) C35 0.029(2) 0.032(2) 0.026(2) -0.0003(17) -0.0032(17) -0.0010(17) C36 0.033(2) 0.024(2) 0.039(2) 0.0006(18) 0.0058(19) 0.0009(18) C37 0.042(3) 0.025(2) 0.050(3) 0.002(2) 0.010(2) 0.0051(19) C38 0.051(3) 0.022(2) 0.053(3) -0.011(2) 0.016(2) -0.003(2) C39 0.039(3) 0.036(3) 0.038(2) -0.016(2) 0.007(2) -0.012(2) C40 0.029(2) 0.024(2) 0.029(2) -0.0031(16) 0.0026(17) -0.0043(17) C41 0.042(3) 0.025(2) 0.042(3) -0.0013(19) 0.001(2) 0.002(2) C42 0.048(3) 0.038(3) 0.051(3) -0.002(2) 0.011(2) -0.009(2) C43 0.047(3) 0.029(2) 0.050(3) -0.002(2) -0.007(2) -0.008(2) C44 0.043(3) 0.028(2) 0.041(3) 0.0001(19) -0.008(2) -0.0003(19) C45 0.039(3) 0.041(3) 0.033(2) 0.0037(19) 0.000(2) 0.005(2) C46 0.076(4) 0.032(3) 0.058(3) 0.000(2) 0.007(3) -0.005(3) C47 0.040(3) 0.053(3) 0.055(3) -0.016(3) -0.003(2) 0.014(2) C48 0.048(3) 0.078(4) 0.044(3) -0.004(3) 0.010(2) -0.009(3) C49 0.039(3) 0.039(3) 0.052(3) 0.002(2) 0.005(2) -0.011(2) C50 0.053(3) 0.032(3) 0.078(4) -0.010(3) 0.024(3) -0.004(2) Co1 0.0254(3) 0.0184(2) 0.0225(3) -0.0023(2) 0.0012(2) 0.0003(2) N1 0.0247(17) 0.0199(16) 0.0263(17) -0.0010(13) 0.0010(13) 0.0020(13) N2 0.0272(17) 0.0244(17) 0.0264(17) -0.0007(13) 0.0030(14) -0.0044(14) N3 0.0287(17) 0.0215(17) 0.0198(15) -0.0003(12) 0.0016(13) -0.0003(13) N4 0.0254(17) 0.0302(18) 0.0231(17) 0.0015(14) 0.0006(13) 0.0003(14) N5 0.0246(17) 0.0225(17) 0.0207(16) -0.0034(13) -0.0002(13) 0.0016(13) N6 0.0223(17) 0.0271(18) 0.0290(18) 0.0004(14) 0.0025(14) -0.0033(14) N7 0.0292(18) 0.0250(17) 0.0255(17) 0.0015(13) -0.0011(14) 0.0052(14) N8 0.0240(17) 0.0240(17) 0.0228(16) 0.0025(13) -0.0018(13) 0.0021(13) N9 0.0270(17) 0.0228(17) 0.0239(17) 0.0009(13) 0.0037(13) -0.0037(14) N10 0.0302(19) 0.0273(19) 0.0360(19) -0.0011(15) -0.0014(15) -0.0023(15) N11 0.093(4) 0.041(3) 0.083(3) -0.010(2) 0.046(3) -0.012(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 N7 1.306(5) . ? C1 N1 1.388(5) . ? C1 C2 1.468(5) . ? C2 C7 1.381(5) . ? C2 C3 1.405(5) . ? C3 C4 1.385(6) . ? C3 H3 0.9500 . ? C4 C5 1.393(6) . ? C4 H4 0.9500 . ? C5 C6 1.389(6) . ? C5 H5 0.9500 . ? C6 C7 1.382(5) . ? C6 H6 0.9500 . ? C7 C8 1.476(5) . ? C8 N2 1.298(5) . ? C8 N1 1.390(5) . ? C9 N2 1.363(5) . ? C9 N3 1.364(5) . ? C9 C10 1.435(5) . ? C10 C11 1.392(5) . ? C10 C15 1.430(5) . ? C11 C12 1.384(6) . ? C11 H11 0.9500 . ? C12 C13 1.407(6) . ? C12 H12 0.9500 . ? C13 C14 1.379(6) . ? C13 H13 0.9500 . ? C14 C15 1.405(5) . ? C14 H14 0.9500 . ? C15 C16 1.421(5) . ? C16 N4 1.339(5) . ? C16 N3 1.403(5) . ? C17 N4 1.316(5) . ? C17 N5 1.422(5) . ? C17 C18 1.439(5) . ? C18 C23 1.393(5) . ? C18 C19 1.395(5) . ? C19 C20 1.392(5) . ? C19 H19 0.9500 . ? C20 C21 1.405(6) . ? C20 H20 0.9500 . ? C21 C22 1.390(6) . ? C21 H21 0.9500 . ? C22 C23 1.390(5) . ? C22 H22 0.9500 . ? C23 C24 1.468(5) . ? C24 N6 1.331(5) . ? C24 N5 1.331(5) . ? C25 C26 1.405(5) . ? C25 N6 1.416(5) . ? C25 C30 1.419(5) . ? C26 C27 1.385(5) . ? C26 H26 0.9500 . ? C27 C28 1.376(5) . ? C27 H27 0.9500 . ? C28 C29 1.413(5) . ? C28 H28 0.9500 . ? C29 N7 1.399(5) . ? C29 C30 1.427(5) . ? C30 Co1 2.000(4) . ? C31 N8 1.343(5) . ? C31 C32 1.382(5) . ? C31 H31 0.9500 . ? C32 C33 1.380(6) . ? C32 H32 0.9500 . ? C33 C34 1.386(6) . ? C33 H33 0.9500 . ? C34 C35 1.384(5) . ? C34 H34 0.9500 . ? C35 N8 1.355(5) . ? C35 H35 0.9500 . ? C36 N9 1.349(5) . ? C36 C37 1.385(6) . ? C36 H36 0.9500 . ? C37 C38 1.372(6) . ? C37 H37 0.9500 . ? C38 C39 1.380(6) . ? C38 H38 0.9500 . ? C39 C40 1.380(5) . ? C39 H39 0.9500 . ? C40 N9 1.363(5) . ? C40 H40 0.9500 . ? C41 N10 1.338(5) . ? C41 C42 1.384(6) . ? C41 H41 0.9500 . ? C42 C43 1.378(6) . ? C42 H42 0.9500 . ? C43 C44 1.391(6) . ? C43 H43 0.9500 . ? C44 C45 1.392(6) . ? C44 H44 0.9500 . ? C45 N10 1.335(5) . ? C45 H45 0.9500 . ? C46 N11 1.336(6) . ? C46 C47 1.352(7) . ? C46 H46 0.9500 . ? C47 C48 1.373(7) . ? C47 H47 0.9500 . ? C48 C49 1.374(7) . ? C48 H48 0.9500 . ? C49 C50 1.350(6) . ? C49 H49 0.9500 . ? C50 N11 1.345(6) . ? C50 H50 0.9500 . ? Co1 N1 1.943(3) . ? Co1 N5 1.960(3) . ? Co1 N9 1.978(3) . ? Co1 N8 1.981(3) . ? Co1 N3 2.013(3) . ? N6 H1 0.93(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 N7 C1 N1 129.0(3) . . ? N7 C1 C2 121.1(3) . . ? N1 C1 C2 109.7(3) . . ? C7 C2 C3 120.7(4) . . ? C7 C2 C1 106.9(3) . . ? C3 C2 C1 132.4(4) . . ? C4 C3 C2 117.2(4) . . ? C4 C3 H3 121.4 . . ? C2 C3 H3 121.4 . . ? C3 C4 C5 121.7(4) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 120.5(4) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.8 . . ? C7 C6 C5 117.9(4) . . ? C7 C6 H6 121.0 . . ? C5 C6 H6 121.0 . . ? C2 C7 C6 121.8(4) . . ? C2 C7 C8 106.9(3) . . ? C6 C7 C8 131.3(4) . . ? N2 C8 N1 130.0(4) . . ? N2 C8 C7 120.6(3) . . ? N1 C8 C7 109.3(3) . . ? N2 C9 N3 126.1(3) . . ? N2 C9 C10 121.6(3) . . ? N3 C9 C10 112.2(3) . . ? C11 C10 C15 120.7(4) . . ? C11 C10 C9 134.5(4) . . ? C15 C10 C9 104.8(3) . . ? C12 C11 C10 118.5(4) . . ? C12 C11 H11 120.8 . . ? C10 C11 H11 120.8 . . ? C11 C12 C13 121.0(4) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 121.7(4) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 118.2(4) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? C14 C15 C16 133.3(4) . . ? C14 C15 C10 120.0(4) . . ? C16 C15 C10 106.7(3) . . ? N4 C16 N3 126.0(3) . . ? N4 C16 C15 123.5(3) . . ? N3 C16 C15 110.5(3) . . ? N4 C17 N5 129.0(3) . . ? N4 C17 C18 122.1(3) . . ? N5 C17 C18 108.7(3) . . ? C23 C18 C19 121.2(4) . . ? C23 C18 C17 107.8(3) . . ? C19 C18 C17 131.0(4) . . ? C20 C19 C18 117.8(4) . . ? C20 C19 H19 121.1 . . ? C18 C19 H19 121.1 . . ? C19 C20 C21 120.8(4) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 121.1(4) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 117.8(4) . . ? C21 C22 H22 121.1 . . ? C23 C22 H22 121.1 . . ? C22 C23 C18 121.2(3) . . ? C22 C23 C24 134.0(4) . . ? C18 C23 C24 104.8(3) . . ? N6 C24 N5 125.0(3) . . ? N6 C24 C23 122.9(3) . . ? N5 C24 C23 112.0(3) . . ? C26 C25 N6 112.7(3) . . ? C26 C25 C30 124.3(3) . . ? N6 C25 C30 123.1(3) . . ? C27 C26 C25 120.1(4) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 118.3(4) . . ? C28 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C27 C28 C29 121.7(4) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? N7 C29 C28 111.0(3) . . ? N7 C29 C30 126.6(3) . . ? C28 C29 C30 122.4(4) . . ? C25 C30 C29 113.1(3) . . ? C25 C30 Co1 123.8(3) . . ? C29 C30 Co1 123.1(3) . . ? N8 C31 C32 123.1(4) . . ? N8 C31 H31 118.4 . . ? C32 C31 H31 118.4 . . ? C33 C32 C31 119.2(4) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 118.6(4) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C35 C34 C33 118.9(4) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? N8 C35 C34 122.9(4) . . ? N8 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? N9 C36 C37 122.7(4) . . ? N9 C36 H36 118.6 . . ? C37 C36 H36 118.6 . . ? C38 C37 C36 119.8(4) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C39 118.2(4) . . ? C37 C38 H38 120.9 . . ? C39 C38 H38 120.9 . . ? C38 C39 C40 120.0(4) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? N9 C40 C39 122.2(4) . . ? N9 C40 H40 118.9 . . ? C39 C40 H40 118.9 . . ? N10 C41 C42 124.0(4) . . ? N10 C41 H41 118.0 . . ? C42 C41 H41 118.0 . . ? C43 C42 C41 119.1(4) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C42 C43 C44 118.1(4) . . ? C42 C43 H43 120.9 . . ? C44 C43 H43 120.9 . . ? C43 C44 C45 118.3(4) . . ? C43 C44 H44 120.8 . . ? C45 C44 H44 120.8 . . ? N10 C45 C44 124.2(4) . . ? N10 C45 H45 117.9 . . ? C44 C45 H45 117.9 . . ? N11 C46 C47 125.0(5) . . ? N11 C46 H46 117.5 . . ? C47 C46 H46 117.5 . . ? C46 C47 C48 118.1(5) . . ? C46 C47 H47 120.9 . . ? C48 C47 H47 120.9 . . ? C47 C48 C49 119.0(5) . . ? C47 C48 H48 120.5 . . ? C49 C48 H48 120.5 . . ? C50 C49 C48 118.2(5) . . ? C50 C49 H49 120.9 . . ? C48 C49 H49 120.9 . . ? N11 C50 C49 124.8(5) . . ? N11 C50 H50 117.6 . . ? C49 C50 H50 117.6 . . ? N1 Co1 N5 176.50(13) . . ? N1 Co1 N9 89.52(13) . . ? N5 Co1 N9 91.47(13) . . ? N1 Co1 N8 89.41(13) . . ? N5 Co1 N8 89.54(13) . . ? N9 Co1 N8 178.62(14) . . ? N1 Co1 C30 91.80(14) . . ? N5 Co1 C30 91.55(14) . . ? N9 Co1 C30 90.45(14) . . ? N8 Co1 C30 90.47(14) . . ? N1 Co1 N3 87.30(13) . . ? N5 Co1 N3 89.37(12) . . ? N9 Co1 N3 88.44(13) . . ? N8 Co1 N3 90.63(12) . . ? C30 Co1 N3 178.57(14) . . ? C1 N1 C8 107.2(3) . . ? C1 N1 Co1 125.9(3) . . ? C8 N1 Co1 127.0(3) . . ? C8 N2 C9 121.1(3) . . ? C9 N3 C16 105.7(3) . . ? C9 N3 Co1 127.8(2) . . ? C16 N3 Co1 126.4(2) . . ? C17 N4 C16 123.4(3) . . ? C24 N5 C17 106.6(3) . . ? C24 N5 Co1 128.5(3) . . ? C17 N5 Co1 124.7(2) . . ? C24 N6 C25 127.3(3) . . ? C24 N6 H1 119(2) . . ? C25 N6 H1 114(2) . . ? C1 N7 C29 122.9(3) . . ? C31 N8 C35 117.2(3) . . ? C31 N8 Co1 122.8(3) . . ? C35 N8 Co1 120.0(3) . . ? C36 N9 C40 117.0(3) . . ? C36 N9 Co1 122.2(3) . . ? C40 N9 Co1 120.7(3) . . ? C45 N10 C41 116.2(4) . . ? C46 N11 C50 114.8(4) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.36 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.574 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.082 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr 2 _platon_squeeze_void_average_x -0.051 _platon_squeeze_void_average_y 1.000 _platon_squeeze_void_average_z 0.500 _platon_squeeze_void_volume 336.7 _platon_squeeze_void_count_electrons 47.6 _platon_squeeze_details ; ? ; # Attachment '641692.cif' data_Co(mchpOH)py2 _database_code_depnum_ccdc_archive 'CCDC 641692' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H46 Co N9 O' _chemical_formula_weight 919.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5789(11) _cell_length_b 13.3090(12) _cell_length_c 15.3136(13) _cell_angle_alpha 75.725(1) _cell_angle_beta 76.522(1) _cell_angle_gamma 69.353(1) _cell_volume 2294.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6780 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour dark _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.426 _exptl_absorpt_correction_type 'Empirical SADABS' _exptl_absorpt_correction_T_min 0.7065 _exptl_absorpt_correction_T_max 0.9667 _exptl_absorpt_process_details ? _exptl_special_details ; Ratio of minimum to maximum apparent transmission: 0.730830 ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17911 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8946 _reflns_number_gt 6891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms were placed in ideal positions and were allowed for as riding atoms using the SHELXTL HFIX command. ; _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^)+(0.1622P)^2^+3.6794P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8946 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1158 _refine_ls_R_factor_gt 0.0946 _refine_ls_wR_factor_ref 0.2722 _refine_ls_wR_factor_gt 0.2567 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0485(4) 0.5239(4) 0.6077(3) 0.0394(11) Uani 1 1 d . . . C2 C 1.1586(4) 0.4285(4) 0.6101(3) 0.0343(10) Uani 1 1 d . . . C3 C 1.2001(4) 0.3409(4) 0.5638(3) 0.0387(10) Uani 1 1 d . . . H3 H 1.1561 0.3310 0.5257 0.046 Uiso 1 1 calc R . . C4 C 1.3097(4) 0.2682(4) 0.5759(4) 0.0425(11) Uani 1 1 d . . . H4 H 1.3405 0.2075 0.5454 0.051 Uiso 1 1 calc R . . C5 C 1.3747(4) 0.2824(4) 0.6312(4) 0.0431(11) Uani 1 1 d . . . H5 H 1.4493 0.2322 0.6368 0.052 Uiso 1 1 calc R . . C6 C 1.3314(5) 0.3700(4) 0.6789(4) 0.0426(11) Uani 1 1 d . . . H6 H 1.3743 0.3798 0.7179 0.051 Uiso 1 1 calc R . . C7 C 1.2230(4) 0.4414(4) 0.6662(3) 0.0353(10) Uani 1 1 d . . . C8 C 1.1504(4) 0.5422(3) 0.7045(3) 0.0348(10) Uani 1 1 d . . . C9 C 1.1408(4) 0.6819(4) 0.7719(3) 0.0334(9) Uani 1 1 d . . . C10 C 1.1981(4) 0.7408(4) 0.8053(3) 0.0367(10) Uani 1 1 d . . . C11 C 1.2999(5) 0.7066(4) 0.8364(4) 0.0474(12) Uani 1 1 d . . . H11 H 1.3457 0.6320 0.8445 0.057 Uiso 1 1 calc R . . C12 C 1.3342(5) 0.7875(5) 0.8559(4) 0.0558(15) Uani 1 1 d . . . H12 H 1.4047 0.7674 0.8780 0.067 Uiso 1 1 calc R . . C13 C 1.2667(5) 0.8959(5) 0.8432(5) 0.0568(15) Uani 1 1 d . . . H13 H 1.2939 0.9491 0.8542 0.068 Uiso 1 1 calc R . . C14 C 1.1599(5) 0.9296(4) 0.8148(4) 0.0479(12) Uani 1 1 d . . . H14 H 1.1128 1.0038 0.8080 0.057 Uiso 1 1 calc R . . C15 C 1.1267(4) 0.8506(4) 0.7974(3) 0.0367(10) Uani 1 1 d . . . C16 C 1.0213(4) 0.8529(3) 0.7713(3) 0.0305(9) Uani 1 1 d . . . C17 C 0.8232(4) 0.9277(4) 0.7667(3) 0.0356(10) Uani 1 1 d . . . C18 C 0.7314(5) 1.0236(5) 0.7848(4) 0.0490(12) Uani 1 1 d . . . H18 H 0.7494 1.0863 0.7872 0.059 Uiso 1 1 calc R . . C19 C 0.6172(5) 1.0291(5) 0.7990(5) 0.0605(16) Uani 1 1 d . . . H19 H 0.5575 1.0922 0.8154 0.073 Uiso 1 1 calc R . . C20 C 0.5927(5) 0.9403(5) 0.7887(4) 0.0535(14) Uani 1 1 d . . . H20 H 0.5150 0.9413 0.7987 0.064 Uiso 1 1 calc R . . C21 C 0.6838(4) 0.8458(4) 0.7628(3) 0.0392(10) Uani 1 1 d . . . C22 C 0.8001(4) 0.8359(4) 0.7524(3) 0.0356(10) Uani 1 1 d . . . C23 C 0.7027(4) 0.6877(4) 0.7090(3) 0.0350(10) Uani 1 1 d . . . C24 C 0.6514(4) 0.6149(4) 0.6852(3) 0.0404(11) Uani 1 1 d . . . C25 C 0.5386(5) 0.6231(4) 0.6889(4) 0.0491(12) Uani 1 1 d . . . H25 H 0.4773 0.6821 0.7105 0.059 Uiso 1 1 calc R . . C26 C 0.5174(5) 0.5421(5) 0.6599(4) 0.0555(14) Uani 1 1 d . . . H26 H 0.4403 0.5459 0.6607 0.067 Uiso 1 1 calc R . . C27 C 0.6074(5) 0.4559(5) 0.6299(5) 0.0582(15) Uani 1 1 d . . . H27 H 0.5908 0.4006 0.6115 0.070 Uiso 1 1 calc R . . C28 C 0.7208(5) 0.4481(4) 0.6258(4) 0.0484(12) Uani 1 1 d . . . H28 H 0.7823 0.3884 0.6055 0.058 Uiso 1 1 calc R . . C29 C 0.7414(4) 0.5315(4) 0.6528(3) 0.0392(10) Uani 1 1 d . . . C30 C 0.8483(4) 0.5555(4) 0.6504(3) 0.0341(9) Uani 1 1 d . . . C31 C 0.8600(4) 0.8427(4) 0.5456(3) 0.0381(10) Uani 1 1 d . . . H31 H 0.7854 0.8397 0.5742 0.046 Uiso 1 1 calc R . . C32 C 0.8756(5) 0.8941(4) 0.4552(3) 0.0448(12) Uani 1 1 d . . . H32 H 0.8129 0.9242 0.4222 0.054 Uiso 1 1 calc R . . C33 C 0.9824(5) 0.9010(4) 0.4142(4) 0.0466(12) Uani 1 1 d . . . H33 H 0.9946 0.9358 0.3523 0.056 Uiso 1 1 calc R . . C34 C 1.0710(5) 0.8573(4) 0.4631(3) 0.0463(12) Uani 1 1 d . . . H34 H 1.1455 0.8621 0.4360 0.056 Uiso 1 1 calc R . . C35 C 1.0508(4) 0.8055(4) 0.5534(3) 0.0410(11) Uani 1 1 d . . . H35 H 1.1126 0.7750 0.5875 0.049 Uiso 1 1 calc R . . C36 C 0.8751(4) 0.6711(4) 0.9166(3) 0.0354(10) Uani 1 1 d . . . H36 H 0.8773 0.7436 0.9080 0.042 Uiso 1 1 calc R . . C37 C 0.8473(4) 0.6194(4) 1.0032(3) 0.0379(10) Uani 1 1 d . . . H37 H 0.8306 0.6556 1.0534 0.046 Uiso 1 1 calc R . . C38 C 0.8434(4) 0.5143(4) 1.0177(3) 0.0394(10) Uani 1 1 d . . . H38 H 0.8210 0.4780 1.0772 0.047 Uiso 1 1 calc R . . C39 C 0.8730(4) 0.4630(4) 0.9429(3) 0.0366(10) Uani 1 1 d . . . H39 H 0.8744 0.3895 0.9509 0.044 Uiso 1 1 calc R . . C40 C 0.9003(4) 0.5193(3) 0.8571(3) 0.0322(9) Uani 1 1 d . . . H40 H 0.9204 0.4834 0.8064 0.039 Uiso 1 1 calc R . . C41 C 1.0304(8) 0.7903(5) 0.1381(5) 0.079(2) Uani 1 1 d . . . C42 C 0.9360(11) 0.7711(5) 0.1918(5) 0.088(3) Uani 1 1 d . . . H42 H 0.9410 0.7320 0.2525 0.105 Uiso 1 1 calc R . . C43 C 0.8327(9) 0.8068(6) 0.1609(6) 0.088(3) Uani 1 1 d . . . H43 H 0.7680 0.7917 0.2011 0.105 Uiso 1 1 calc R . . C44 C 0.8185(7) 0.8653(6) 0.0716(5) 0.073(2) Uani 1 1 d . . . C45 C 0.9143(6) 0.8842(5) 0.0179(4) 0.0604(16) Uani 1 1 d . . . H45 H 0.9097 0.9238 -0.0427 0.072 Uiso 1 1 calc R . . C46 C 1.0172(7) 0.8476(4) 0.0489(4) 0.0611(17) Uani 1 1 d . . . H46 H 1.0824 0.8614 0.0086 0.073 Uiso 1 1 calc R . . C47 C 1.1406(12) 0.7516(7) 0.1738(9) 0.134(5) Uani 1 1 d . . . H47A H 1.1332 0.7911 0.2222 0.201 Uiso 1 1 calc R . . H47B H 1.2020 0.7650 0.1242 0.201 Uiso 1 1 calc R . . H47C H 1.1595 0.6733 0.1985 0.201 Uiso 1 1 calc R . . C48 C 0.7055(8) 0.9056(9) 0.0359(8) 0.122(4) Uani 1 1 d . . . H48A H 0.6798 0.9856 0.0218 0.183 Uiso 1 1 calc R . . H48B H 0.6475 0.8807 0.0824 0.183 Uiso 1 1 calc R . . H48C H 0.7158 0.8768 -0.0196 0.183 Uiso 1 1 calc R . . C49 C 0.5595(5) 0.0074(5) 0.5610(4) 0.0559(14) Uani 1 1 d . . . H49 H 0.6013 0.0112 0.6037 0.067 Uiso 1 1 calc R . . C50 C 0.5702(5) 0.0686(5) 0.4733(4) 0.0519(13) Uani 1 1 d . . . C51 C 0.5102(5) 0.0588(5) 0.4122(4) 0.0576(15) Uani 1 1 d . . . H51 H 0.5171 0.0980 0.3514 0.069 Uiso 1 1 calc R . . C52 C 0.6436(6) 0.1443(5) 0.4465(5) 0.0659(17) Uani 1 1 d . . . H52A H 0.6801 0.1447 0.3825 0.099 Uiso 1 1 calc R . . H52B H 0.7032 0.1187 0.4854 0.099 Uiso 1 1 calc R . . H52C H 0.5949 0.2185 0.4543 0.099 Uiso 1 1 calc R . . C53 C 0.5595(6) 0.4727(8) 0.9173(5) 0.083(2) Uani 1 1 d . . . H53 H 0.6018 0.4552 0.8600 0.099 Uiso 1 1 calc R . . C54 C 0.5657(6) 0.5597(8) 0.9455(6) 0.087(3) Uani 1 1 d . . . H54 H 0.6117 0.6016 0.9067 0.105 Uiso 1 1 calc R . . C55 C 0.5063(6) 0.5899(8) 1.0305(6) 0.086(2) Uani 1 1 d . . . C56 C 0.5129(10) 0.6842(11) 1.0621(10) 0.135(4) Uani 1 1 d . . . H56A H 0.4359 0.7375 1.0707 0.203 Uiso 1 1 calc R . . H56B H 0.5646 0.7184 1.0164 0.203 Uiso 1 1 calc R . . H56C H 0.5425 0.6587 1.1201 0.203 Uiso 1 1 calc R . . Co1 Co 0.92512(5) 0.70780(4) 0.71738(4) 0.0311(2) Uani 1 1 d . . . N1 N 1.0519(3) 0.5827(3) 0.6781(2) 0.0304(8) Uani 1 1 d . . . N2 N 1.1975(3) 0.5806(3) 0.7567(2) 0.0358(8) Uani 1 1 d . . . N3 N 1.0349(3) 0.7481(3) 0.7559(2) 0.0298(8) Uani 1 1 d . . . N4 N 0.9298(3) 0.9356(3) 0.7715(2) 0.0299(8) Uani 1 1 d . . . N5 N 0.6393(4) 0.7692(3) 0.7467(3) 0.0420(9) Uani 1 1 d . . . N6 N 0.8201(3) 0.6517(3) 0.6832(2) 0.0330(8) Uani 1 1 d . . . N7 N 0.9506(3) 0.4907(3) 0.6209(2) 0.0333(8) Uani 1 1 d . . . N8 N 0.9465(3) 0.7974(3) 0.5938(3) 0.0357(8) Uani 1 1 d . . . N9 N 0.8996(3) 0.6244(3) 0.8423(2) 0.0317(8) Uani 1 1 d . . . O1 O 1.0520(3) 0.6012(3) 0.5230(2) 0.0403(8) Uani 1 1 d . . . H1 H 1.0555 0.5714 0.4795 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(3) 0.036(2) 0.040(3) -0.021(2) 0.001(2) -0.010(2) C2 0.037(2) 0.030(2) 0.036(2) -0.0112(18) 0.0057(18) -0.0143(18) C3 0.043(3) 0.031(2) 0.042(3) -0.016(2) 0.001(2) -0.012(2) C4 0.047(3) 0.030(2) 0.050(3) -0.017(2) 0.002(2) -0.011(2) C5 0.034(2) 0.036(3) 0.053(3) -0.014(2) 0.000(2) -0.004(2) C6 0.056(3) 0.034(2) 0.044(3) -0.007(2) -0.006(2) -0.022(2) C7 0.039(2) 0.026(2) 0.038(2) -0.0111(18) 0.0072(18) -0.0105(18) C8 0.056(3) 0.024(2) 0.026(2) -0.0098(16) 0.0096(19) -0.021(2) C9 0.049(3) 0.029(2) 0.0205(19) -0.0058(16) -0.0003(17) -0.0132(19) C10 0.051(3) 0.030(2) 0.030(2) -0.0097(18) -0.0028(19) -0.013(2) C11 0.054(3) 0.041(3) 0.052(3) -0.020(2) -0.003(2) -0.016(2) C12 0.050(3) 0.055(3) 0.075(4) -0.035(3) -0.015(3) -0.012(3) C13 0.058(3) 0.051(3) 0.076(4) -0.036(3) -0.007(3) -0.021(3) C14 0.052(3) 0.039(3) 0.054(3) -0.017(2) -0.001(2) -0.015(2) C15 0.040(2) 0.041(3) 0.032(2) -0.0113(19) 0.0004(18) -0.016(2) C16 0.046(2) 0.026(2) 0.0193(19) -0.0057(15) 0.0007(16) -0.0139(18) C17 0.051(3) 0.027(2) 0.031(2) -0.0091(17) -0.0062(19) -0.014(2) C18 0.044(3) 0.043(3) 0.063(3) -0.017(2) -0.011(2) -0.010(2) C19 0.049(3) 0.046(3) 0.085(5) -0.036(3) -0.006(3) 0.000(3) C20 0.054(3) 0.052(3) 0.061(3) -0.028(3) -0.003(3) -0.016(3) C21 0.050(3) 0.037(2) 0.035(2) -0.0130(19) -0.002(2) -0.017(2) C22 0.058(3) 0.026(2) 0.024(2) -0.0053(16) -0.0051(19) -0.015(2) C23 0.040(2) 0.034(2) 0.034(2) -0.0059(18) -0.0054(18) -0.0156(19) C24 0.055(3) 0.029(2) 0.037(2) -0.0075(19) -0.007(2) -0.012(2) C25 0.052(3) 0.042(3) 0.057(3) -0.011(2) -0.007(2) -0.020(2) C26 0.052(3) 0.051(3) 0.073(4) -0.018(3) -0.011(3) -0.022(3) C27 0.054(3) 0.057(4) 0.078(4) -0.032(3) -0.003(3) -0.027(3) C28 0.052(3) 0.040(3) 0.059(3) -0.019(2) -0.001(2) -0.019(2) C29 0.045(3) 0.038(2) 0.038(2) -0.010(2) -0.005(2) -0.017(2) C30 0.044(3) 0.029(2) 0.032(2) -0.0066(18) -0.0065(18) -0.0150(19) C31 0.049(3) 0.027(2) 0.035(2) -0.0056(18) -0.006(2) -0.0096(19) C32 0.063(3) 0.029(2) 0.039(3) -0.004(2) -0.010(2) -0.011(2) C33 0.073(4) 0.033(2) 0.036(3) -0.002(2) -0.010(2) -0.022(2) C34 0.062(3) 0.045(3) 0.037(3) -0.010(2) 0.003(2) -0.030(3) C35 0.051(3) 0.040(3) 0.038(3) -0.012(2) -0.008(2) -0.019(2) C36 0.051(3) 0.027(2) 0.029(2) -0.0114(17) -0.0027(19) -0.0129(19) C37 0.050(3) 0.039(2) 0.027(2) -0.0123(18) -0.0020(19) -0.014(2) C38 0.049(3) 0.042(3) 0.025(2) -0.0010(19) -0.0025(19) -0.019(2) C39 0.048(3) 0.029(2) 0.034(2) -0.0039(18) -0.0070(19) -0.014(2) C40 0.046(2) 0.024(2) 0.028(2) -0.0063(16) -0.0048(18) -0.0117(18) C41 0.148(7) 0.029(3) 0.070(5) -0.015(3) -0.026(5) -0.030(4) C42 0.183(10) 0.039(3) 0.045(4) -0.008(3) -0.006(5) -0.048(5) C43 0.135(8) 0.067(5) 0.072(5) -0.034(4) 0.041(5) -0.068(5) C44 0.096(5) 0.070(4) 0.070(4) -0.043(4) 0.018(4) -0.045(4) C45 0.100(5) 0.038(3) 0.041(3) -0.017(2) 0.003(3) -0.022(3) C46 0.096(5) 0.033(3) 0.054(3) -0.020(3) 0.007(3) -0.025(3) C47 0.217(13) 0.054(5) 0.164(10) -0.026(6) -0.117(10) -0.023(6) C48 0.101(7) 0.136(9) 0.158(10) -0.105(8) 0.009(6) -0.040(6) C49 0.052(3) 0.049(3) 0.059(4) -0.013(3) -0.020(3) 0.002(3) C50 0.042(3) 0.044(3) 0.056(3) -0.015(2) -0.009(2) 0.006(2) C51 0.059(3) 0.048(3) 0.054(3) -0.009(3) -0.012(3) 0.000(3) C52 0.065(4) 0.049(3) 0.072(4) -0.002(3) -0.018(3) -0.005(3) C53 0.057(4) 0.099(6) 0.065(4) 0.014(4) -0.014(3) -0.007(4) C54 0.050(4) 0.097(6) 0.081(5) 0.029(5) 0.000(3) -0.018(4) C55 0.056(4) 0.101(6) 0.086(6) 0.017(5) -0.027(4) -0.019(4) C56 0.099(7) 0.138(10) 0.174(12) -0.025(9) -0.056(8) -0.024(7) Co1 0.0497(4) 0.0229(3) 0.0220(3) -0.0084(2) 0.0004(2) -0.0138(3) N1 0.038(2) 0.0279(18) 0.0278(18) -0.0101(14) 0.0017(15) -0.0140(15) N2 0.053(2) 0.0263(18) 0.0273(18) -0.0053(15) -0.0019(16) -0.0140(17) N3 0.040(2) 0.0238(17) 0.0257(17) -0.0080(14) -0.0017(14) -0.0104(15) N4 0.041(2) 0.0211(17) 0.0265(18) -0.0051(13) -0.0036(14) -0.0097(15) N5 0.056(3) 0.035(2) 0.039(2) -0.0123(17) -0.0005(18) -0.0190(19) N6 0.056(2) 0.0214(17) 0.0233(17) -0.0055(13) -0.0069(16) -0.0132(16) N7 0.054(2) 0.0259(18) 0.0235(17) -0.0092(14) -0.0019(15) -0.0155(16) N8 0.048(2) 0.0306(19) 0.0328(19) -0.0130(15) 0.0001(16) -0.0171(17) N9 0.046(2) 0.0239(17) 0.0256(18) -0.0075(14) -0.0010(15) -0.0125(15) O1 0.058(2) 0.0345(17) 0.0299(16) -0.0096(13) -0.0019(14) -0.0166(15) _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 N7 1.405(6) . ? C1 O1 1.446(6) . ? C1 N1 1.496(5) . ? C1 C2 1.515(7) . ? C2 C7 1.385(7) . ? C2 C3 1.393(6) . ? C3 C4 1.400(7) . ? C3 H3 0.9500 . ? C4 C5 1.389(7) . ? C4 H4 0.9500 . ? C5 C6 1.407(7) . ? C5 H5 0.9500 . ? C6 C7 1.385(7) . ? C6 H6 0.9500 . ? C7 C8 1.501(6) . ? C8 N1 1.282(6) . ? C8 N2 1.375(6) . ? C9 N2 1.334(6) . ? C9 N3 1.353(6) . ? C9 C10 1.470(6) . ? C10 C11 1.357(7) . ? C10 C15 1.412(7) . ? C11 C12 1.406(7) . ? C11 H11 0.9500 . ? C12 C13 1.384(8) . ? C12 H12 0.9500 . ? C13 C14 1.395(8) . ? C13 H13 0.9500 . ? C14 C15 1.361(7) . ? C14 H14 0.9500 . ? C15 C16 1.459(6) . ? C16 N4 1.282(6) . ? C16 N3 1.416(5) . ? C17 N4 1.401(6) . ? C17 C18 1.423(7) . ? C17 C22 1.427(6) . ? C18 C19 1.379(8) . ? C18 H18 0.9500 . ? C19 C20 1.375(8) . ? C19 H19 0.9500 . ? C20 C21 1.439(7) . ? C20 H20 0.9500 . ? C21 C22 1.396(7) . ? C21 N5 1.416(6) . ? C22 Co1 1.958(5) . ? C23 N5 1.278(6) . ? C23 N6 1.375(6) . ? C23 C24 1.487(6) . ? C24 C25 1.373(8) . ? C24 C29 1.373(7) . ? C25 C26 1.387(7) . ? C25 H25 0.9500 . ? C26 C27 1.382(8) . ? C26 H26 0.9500 . ? C27 C28 1.381(8) . ? C27 H27 0.9500 . ? C28 C29 1.396(7) . ? C28 H28 0.9500 . ? C29 C30 1.478(6) . ? C30 N7 1.320(6) . ? C30 N6 1.389(5) . ? C31 N8 1.335(6) . ? C31 C32 1.387(7) . ? C31 H31 0.9500 . ? C32 C33 1.368(8) . ? C32 H32 0.9500 . ? C33 C34 1.364(8) . ? C33 H33 0.9500 . ? C34 C35 1.394(7) . ? C34 H34 0.9500 . ? C35 N8 1.343(6) . ? C35 H35 0.9500 . ? C36 N9 1.351(5) . ? C36 C37 1.364(6) . ? C36 H36 0.9500 . ? C37 C38 1.378(7) . ? C37 H37 0.9500 . ? C38 C39 1.387(7) . ? C38 H38 0.9500 . ? C39 C40 1.375(6) . ? C39 H39 0.9500 . ? C40 N9 1.357(5) . ? C40 H40 0.9500 . ? C41 C42 1.344(13) . ? C41 C46 1.407(9) . ? C41 C47 1.482(13) . ? C42 C43 1.371(13) . ? C42 H42 0.9500 . ? C43 C44 1.414(12) . ? C43 H43 0.9500 . ? C44 C45 1.358(9) . ? C44 C48 1.512(13) . ? C45 C46 1.366(10) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C51 1.383(9) 2_656 ? C49 C50 1.392(9) . ? C49 H49 0.9500 . ? C50 C51 1.386(8) . ? C50 C52 1.521(9) . ? C51 C49 1.383(9) 2_656 ? C51 H51 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.364(13) . ? C53 C55 1.366(11) 2_667 ? C53 H53 0.9500 . ? C54 C55 1.416(13) . ? C54 H54 0.9500 . ? C55 C53 1.366(11) 2_667 ? C55 C56 1.486(15) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? Co1 N3 1.897(4) . ? Co1 N6 1.946(4) . ? Co1 N1 1.963(4) . ? Co1 N9 1.979(4) . ? Co1 N8 1.988(4) . ? O1 H1 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 N7 C1 O1 108.9(4) . . ? N7 C1 N1 115.7(4) . . ? O1 C1 N1 104.5(3) . . ? N7 C1 C2 112.5(4) . . ? O1 C1 C2 111.8(4) . . ? N1 C1 C2 103.1(4) . . ? C7 C2 C3 121.1(4) . . ? C7 C2 C1 108.7(4) . . ? C3 C2 C1 130.1(4) . . ? C2 C3 C4 116.9(5) . . ? C2 C3 H3 121.6 . . ? C4 C3 H3 121.6 . . ? C5 C4 C3 121.9(4) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 120.9(5) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C7 C6 C5 116.6(5) . . ? C7 C6 H6 121.7 . . ? C5 C6 H6 121.7 . . ? C2 C7 C6 122.7(4) . . ? C2 C7 C8 105.6(4) . . ? C6 C7 C8 131.7(5) . . ? N1 C8 N2 129.7(4) . . ? N1 C8 C7 111.9(4) . . ? N2 C8 C7 118.3(4) . . ? N2 C9 N3 130.2(4) . . ? N2 C9 C10 119.8(4) . . ? N3 C9 C10 109.9(4) . . ? C11 C10 C15 122.1(4) . . ? C11 C10 C9 131.3(4) . . ? C15 C10 C9 106.6(4) . . ? C10 C11 C12 116.5(5) . . ? C10 C11 H11 121.7 . . ? C12 C11 H11 121.7 . . ? C13 C12 C11 121.0(5) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 122.0(5) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C15 C14 C13 116.5(5) . . ? C15 C14 H14 121.7 . . ? C13 C14 H14 121.7 . . ? C14 C15 C10 121.7(5) . . ? C14 C15 C16 132.3(5) . . ? C10 C15 C16 106.0(4) . . ? N4 C16 N3 127.3(4) . . ? N4 C16 C15 123.5(4) . . ? N3 C16 C15 109.0(4) . . ? N4 C17 C18 111.7(4) . . ? N4 C17 C22 127.7(4) . . ? C18 C17 C22 120.5(4) . . ? C19 C18 C17 122.6(5) . . ? C19 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C20 C19 C18 117.7(5) . . ? C20 C19 H19 121.1 . . ? C18 C19 H19 121.1 . . ? C19 C20 C21 120.6(5) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C22 C21 N5 126.0(4) . . ? C22 C21 C20 122.8(4) . . ? N5 C21 C20 111.2(4) . . ? C21 C22 C17 115.4(4) . . ? C21 C22 Co1 123.3(3) . . ? C17 C22 Co1 121.3(4) . . ? N5 C23 N6 130.0(4) . . ? N5 C23 C24 120.9(4) . . ? N6 C23 C24 109.1(4) . . ? C25 C24 C29 122.3(5) . . ? C25 C24 C23 131.0(5) . . ? C29 C24 C23 106.7(4) . . ? C24 C25 C26 117.6(5) . . ? C24 C25 H25 121.2 . . ? C26 C25 H25 121.2 . . ? C27 C26 C25 120.6(5) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C26 121.7(5) . . ? C28 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? C27 C28 C29 117.3(5) . . ? C27 C28 H28 121.4 . . ? C29 C28 H28 121.4 . . ? C24 C29 C28 120.5(5) . . ? C24 C29 C30 107.0(4) . . ? C28 C29 C30 132.5(5) . . ? N7 C30 N6 129.2(4) . . ? N7 C30 C29 121.8(4) . . ? N6 C30 C29 109.0(4) . . ? N8 C31 C32 122.2(5) . . ? N8 C31 H31 118.9 . . ? C32 C31 H31 118.9 . . ? C33 C32 C31 119.2(5) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C34 C33 C32 119.3(5) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 119.0(5) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? N8 C35 C34 122.0(5) . . ? N8 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? N9 C36 C37 123.2(4) . . ? N9 C36 H36 118.4 . . ? C37 C36 H36 118.4 . . ? C36 C37 C38 119.6(4) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C37 C38 C39 118.2(4) . . ? C37 C38 H38 120.9 . . ? C39 C38 H38 120.9 . . ? C40 C39 C38 119.5(4) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? N9 C40 C39 122.4(4) . . ? N9 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? C42 C41 C46 116.4(8) . . ? C42 C41 C47 120.1(9) . . ? C46 C41 C47 123.6(9) . . ? C41 C42 C43 121.3(7) . . ? C41 C42 H42 119.3 . . ? C43 C42 H42 119.3 . . ? C42 C43 C44 122.7(7) . . ? C42 C43 H43 118.7 . . ? C44 C43 H43 118.7 . . ? C45 C44 C43 115.5(8) . . ? C45 C44 C48 120.8(8) . . ? C43 C44 C48 123.6(8) . . ? C44 C45 C46 121.5(7) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C45 C46 C41 122.6(7) . . ? C45 C46 H46 118.7 . . ? C41 C46 H46 118.7 . . ? C41 C47 H47A 109.5 . . ? C41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 C48 H48A 109.5 . . ? C44 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C44 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C51 C49 C50 122.0(6) 2_656 . ? C51 C49 H49 119.0 2_656 . ? C50 C49 H49 119.0 . . ? C51 C50 C49 117.4(6) . . ? C51 C50 C52 121.5(6) . . ? C49 C50 C52 121.1(6) . . ? C49 C51 C50 120.6(6) 2_656 . ? C49 C51 H51 119.7 2_656 . ? C50 C51 H51 119.7 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C55 121.4(9) . 2_667 ? C54 C53 H53 119.3 . . ? C55 C53 H53 119.3 2_667 . ? C53 C54 C55 122.5(8) . . ? C53 C54 H54 118.7 . . ? C55 C54 H54 118.7 . . ? C53 C55 C54 116.0(9) 2_667 . ? C53 C55 C56 121.0(10) 2_667 . ? C54 C55 C56 123.0(9) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N3 Co1 N6 174.34(15) . . ? N3 Co1 C22 92.04(18) . . ? N6 Co1 C22 92.24(18) . . ? N3 Co1 N1 87.74(15) . . ? N6 Co1 N1 88.11(15) . . ? C22 Co1 N1 177.93(16) . . ? N3 Co1 N9 87.67(15) . . ? N6 Co1 N9 88.60(15) . . ? C22 Co1 N9 90.36(16) . . ? N1 Co1 N9 91.70(15) . . ? N3 Co1 N8 91.87(15) . . ? N6 Co1 N8 92.03(15) . . ? C22 Co1 N8 87.26(17) . . ? N1 Co1 N8 90.68(15) . . ? N9 Co1 N8 177.56(15) . . ? C8 N1 C1 109.9(4) . . ? C8 N1 Co1 126.3(3) . . ? C1 N1 Co1 123.8(3) . . ? C9 N2 C8 115.8(4) . . ? C9 N3 C16 108.0(4) . . ? C9 N3 Co1 125.8(3) . . ? C16 N3 Co1 126.2(3) . . ? C16 N4 C17 121.9(4) . . ? C23 N5 C21 122.4(4) . . ? C23 N6 C30 107.9(4) . . ? C23 N6 Co1 123.5(3) . . ? C30 N6 Co1 126.9(3) . . ? C30 N7 C1 119.9(4) . . ? C31 N8 C35 118.2(4) . . ? C31 N8 Co1 120.8(3) . . ? C35 N8 Co1 120.7(3) . . ? C36 N9 C40 117.0(4) . . ? C36 N9 Co1 121.4(3) . . ? C40 N9 Co1 121.5(3) . . ? C1 O1 H1 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 4.570 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.149