# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Rajeev Gupta' _publ_contact_author_email rgupta.chemistry@gmail.com loop_ _publ_author_name 'Amit Pratap Singh' 'Afsar Ali' 'Rajeev Gupta' # Attachment '2a.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 767585' #TrackingRef '2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H31 Co N11 O6 Zn, C3 H7 N O, 2(N O3), H2 O' _chemical_formula_sum 'C40 H40 Co N14 O14 Zn' _chemical_formula_weight 1065.16 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' Zn Zn 0.2839 1.4301 '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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_HALL -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.241(5) _cell_length_b 13.802(5) _cell_length_c 14.081(5) _cell_angle_alpha 116.834(5) _cell_angle_beta 93.137(5) _cell_angle_gamma 90.943(5) _cell_volume 2290.3(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9906 _cell_measurement_theta_min 0.830 _cell_measurement_theta_max 0.909 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1094 _exptl_absorpt_coefficient_mu 0.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8300 _exptl_absorpt_correction_T_max 0.9094 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48299 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 28.01 _reflns_number_total 10652 _reflns_number_gt 7802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0769P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10652 _refine_ls_number_parameters 633 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Zn Zn 0.25660(2) 0.80978(2) 0.64196(2) 0.01317(9) Uani 1 1 d . . . Co Co 0.25349(2) 0.25703(2) 0.52864(3) 0.01205(10) Uani 1 1 d . . . O1 O 0.35125(15) 0.95341(14) 0.37333(15) 0.0235(4) Uani 1 1 d . . . O3 O -0.00713(14) 0.75411(15) 0.32105(15) 0.0218(4) Uani 1 1 d . . . N8 N 0.10746(16) 0.87229(17) 0.63721(17) 0.0163(4) Uani 1 1 d . . . O2 O 0.14805(15) 0.41184(15) 0.36156(16) 0.0239(4) Uani 1 1 d . . . N5 N 0.24801(16) 0.18731(16) 0.37968(17) 0.0144(4) Uani 1 1 d . . . O1S O 0.24345(15) 0.74162(17) 0.47433(15) 0.0261(5) Uani 1 1 d . . . O1W O 0.27003(16) 0.88347(14) 0.81280(15) 0.0225(4) Uani 1 1 d . . . O4 O 0.48872(14) 0.58290(15) 0.30595(16) 0.0235(4) Uani 1 1 d . . . N10 N 0.40440(16) 0.74181(16) 0.62607(17) 0.0158(4) Uani 1 1 d . . . O2S O 0.7568(2) 0.90283(17) 0.06832(18) 0.0381(6) Uani 1 1 d . . . N7 N 0.18906(16) 0.66972(16) 0.64778(17) 0.0154(4) Uani 1 1 d . . . N3 N -0.12076(16) 0.79567(16) 0.45270(17) 0.0148(4) Uani 1 1 d . . . N4 N 0.61249(16) 0.66867(16) 0.44414(17) 0.0144(4) Uani 1 1 d . . . N1 N 0.31626(16) 1.12187(16) 0.50858(17) 0.0149(4) Uani 1 1 d . . . N9 N 0.32553(16) 0.95804(16) 0.65458(17) 0.0151(4) Uani 1 1 d . . . C18 C 0.2135(3) 0.6589(3) 0.3947(3) 0.0361(8) Uani 1 1 d . . . N6 N 0.25952(16) 0.32629(16) 0.67686(17) 0.0150(4) Uani 1 1 d . . . C20 C 0.4271(2) 1.1389(2) 0.6616(2) 0.0175(5) Uani 1 1 d . . . H20 H 0.4622 1.2006 0.6637 0.021 Uiso 1 1 calc R . . C21 C 0.3429(2) 0.3837(2) 0.7303(2) 0.0170(5) Uani 1 1 d . . . C22 C 0.34717(19) 1.08811(19) 0.5867(2) 0.0143(5) Uani 1 1 d . . . N2 N 0.18847(16) 0.37120(16) 0.50165(17) 0.0148(4) Uani 1 1 d . . . C24 C 0.17753(19) 0.3507(2) 0.3981(2) 0.0167(5) Uani 1 1 d . . . C25 C 0.5754(2) 0.6210(2) 0.5858(2) 0.0184(5) Uani 1 1 d . . . H25 H 0.6330 0.5778 0.5710 0.022 Uiso 1 1 calc R . . C26 C 0.32075(19) 1.0461(2) 0.4062(2) 0.0168(5) Uani 1 1 d . . . C27 C -0.04946(19) 0.85894(19) 0.5366(2) 0.0154(5) Uani 1 1 d . . . O9 O 0.3460(2) 0.7576(2) 0.0647(2) 0.0453(6) Uani 1 1 d . . . C29 C 0.2971(2) 0.9982(2) 0.5879(2) 0.0168(5) Uani 1 1 d . . . H29 H 0.2403 0.9644 0.5387 0.020 Uiso 1 1 calc R . . C30 C 0.20920(19) 0.2388(2) 0.3265(2) 0.0167(5) Uani 1 1 d . . . C31 C -0.0915(2) 0.7485(2) 0.3520(2) 0.0172(5) Uani 1 1 d . . . C32 C 0.3483(2) 0.4394(2) 0.8409(2) 0.0245(6) Uani 1 1 d . . . H32 H 0.4082 0.4798 0.8799 0.029 Uiso 1 1 calc R . . C33 C 0.54981(19) 0.67491(19) 0.5251(2) 0.0145(5) Uani 1 1 d . . . N11 N 0.2165(3) 0.6479(2) 0.2979(2) 0.0553(10) Uani 1 1 d . . . C35 C 0.2765(2) 0.0321(2) 0.2198(2) 0.0217(6) Uani 1 1 d . . . H35 H 0.3001 -0.0394 0.1843 0.026 Uiso 1 1 calc R . . C36 C 0.17727(19) 0.3191(2) 0.7252(2) 0.0170(5) Uani 1 1 d . . . C37 C -0.0641(2) 0.9684(2) 0.6030(2) 0.0192(6) Uani 1 1 d . . . H37 H -0.1214 1.0023 0.5901 0.023 Uiso 1 1 calc R . . C38 C 0.2017(2) 0.1887(2) 0.2162(2) 0.0226(6) Uani 1 1 d . . . H38 H 0.1740 0.2248 0.1778 0.027 Uiso 1 1 calc R . . C39 C 0.5754(2) 0.62054(19) 0.3420(2) 0.0168(5) Uani 1 1 d . . . C40 C 0.2818(2) 0.0877(2) 0.3304(2) 0.0173(5) Uani 1 1 d . . . N12 N 0.6232(3) 0.7922(3) -0.0065(2) 0.0443(8) Uani 1 1 d . . . C42 C 0.2124(2) 0.5689(2) 0.5826(2) 0.0167(5) Uani 1 1 d . . . H42 H 0.2655 0.5593 0.5368 0.020 Uiso 1 1 calc R . . O5 O 0.9202(2) 0.6930(3) 0.9573(3) 0.0694(9) Uani 1 1 d . . . C44 C 0.16295(19) 0.47586(19) 0.5777(2) 0.0144(5) Uani 1 1 d . . . C45 C 0.46290(19) 0.7348(2) 0.5486(2) 0.0158(5) Uani 1 1 d . . . H45 H 0.4444 0.7722 0.5082 0.019 Uiso 1 1 calc R . . O10 O 0.3276(3) 0.6811(2) -0.1084(2) 0.0603(8) Uani 1 1 d . . . O8 O 0.2887(3) 0.8443(2) -0.01933(19) 0.0580(8) Uani 1 1 d . . . O2W O 0.4008(3) 0.5708(3) 0.1042(3) 0.0735(9) Uani 1 1 d . . . C49 C 0.4561(2) 1.0997(2) 0.7338(2) 0.0196(6) Uani 1 1 d . . . H49 H 0.5101 1.1346 0.7866 0.024 Uiso 1 1 calc R . . C50 C 0.0903(2) 0.9771(2) 0.7030(2) 0.0188(5) Uani 1 1 d . . . H50 H 0.1379 1.0176 0.7614 0.023 Uiso 1 1 calc R . . C51 C 0.0878(2) 0.4909(2) 0.6468(2) 0.0181(5) Uani 1 1 d . . . H51 H 0.0516 0.4302 0.6454 0.022 Uiso 1 1 calc R . . C52 C 0.0055(2) 1.0271(2) 0.6880(2) 0.0186(5) Uani 1 1 d . . . H52 H -0.0048 1.1010 0.7354 0.022 Uiso 1 1 calc R . . C53 C 0.1167(2) 0.6831(2) 0.7156(2) 0.0184(5) Uani 1 1 d . . . H53 H 0.1000 0.7548 0.7632 0.022 Uiso 1 1 calc R . . C54 C 0.03827(19) 0.8156(2) 0.5584(2) 0.0161(5) Uani 1 1 d . . . H54 H 0.0491 0.7410 0.5142 0.019 Uiso 1 1 calc R . . C55 C 0.4318(2) 0.6921(2) 0.6856(2) 0.0182(5) Uani 1 1 d . . . H55 H 0.3918 0.6993 0.7422 0.022 Uiso 1 1 calc R . . N14 N 0.3215(2) 0.7599(2) -0.0218(2) 0.0297(6) Uani 1 1 d . . . C57 C 0.1770(2) 0.3726(2) 0.8345(2) 0.0247(6) Uani 1 1 d . . . H57 H 0.1192 0.3678 0.8694 0.030 Uiso 1 1 calc R . . C58 C 0.0660(2) 0.5968(2) 0.7187(2) 0.0187(5) Uani 1 1 d . . . H58 H 0.0168 0.6090 0.7691 0.022 Uiso 1 1 calc R . . C59 C 0.5168(2) 0.6307(2) 0.6669(2) 0.0219(6) Uani 1 1 d . . . H59 H 0.5344 0.5957 0.7097 0.026 Uiso 1 1 calc R . . C60 C 0.2359(2) 0.0832(2) 0.1625(2) 0.0246(6) Uani 1 1 d . . . H60 H 0.2312 0.0467 0.0867 0.029 Uiso 1 1 calc R . . C61 C 0.4043(2) 1.0085(2) 0.7268(2) 0.0174(5) Uani 1 1 d . . . H61 H 0.4249 0.9802 0.7748 0.021 Uiso 1 1 calc R . . C62 C 0.2638(2) 0.4344(3) 0.8932(2) 0.0297(7) Uani 1 1 d . . . H62 H 0.2649 0.4730 0.9687 0.036 Uiso 1 1 calc R . . C63 C 0.5602(3) 0.8738(3) -0.0172(3) 0.0420(9) Uani 1 1 d . . . H63A H 0.6015 0.9405 0.0025 0.063 Uiso 1 1 calc R . . H63B H 0.5046 0.8896 0.0301 0.063 Uiso 1 1 calc R . . H63C H 0.5325 0.8456 -0.0912 0.063 Uiso 1 1 calc R . . C64 C 0.7163(3) 0.8145(3) 0.0330(3) 0.0375(8) Uani 1 1 d . . . N13 N 1.0008(3) 0.7425(4) 0.9970(3) 0.0691(11) Uani 1 1 d . . . C66 C 0.1652(4) 0.5473(3) 0.2108(3) 0.0584(11) Uani 1 1 d . . . H66A H 0.1729 0.5472 0.1419 0.088 Uiso 1 1 calc R . . H66B H 0.0931 0.5456 0.2226 0.088 Uiso 1 1 calc R . . H66C H 0.1961 0.4832 0.2107 0.088 Uiso 1 1 calc R . . O6 O 1.0791(4) 0.6857(7) 1.0295(6) 0.180(3) Uani 1 1 d . . . O7 O 1.0206(4) 0.8537(4) 1.0089(4) 0.1102(15) Uani 1 1 d . . . C69 C 0.5750(4) 0.6828(3) -0.0407(3) 0.0529(10) Uani 1 1 d . . . H69A H 0.6261 0.6335 -0.0380 0.079 Uiso 1 1 calc R . . H69B H 0.5447 0.6551 -0.1138 0.079 Uiso 1 1 calc R . . H69C H 0.5222 0.6877 0.0072 0.079 Uiso 1 1 calc R . . C70 C 0.2294(4) 0.7405(3) 0.2778(4) 0.0578(11) Uani 1 1 d . . . H70A H 0.2300 0.7160 0.2008 0.087 Uiso 1 1 calc R . . H70B H 0.2937 0.7798 0.3131 0.087 Uiso 1 1 calc R . . H70C H 0.1735 0.7888 0.3059 0.087 Uiso 1 1 calc R . . H18 H 0.1833 0.5901 0.4029 0.050 Uiso 1 1 d . . . H64B H 0.7538 0.7434 0.0290 0.050 Uiso 1 1 d . . . H1AW H 0.2734 0.8541 0.8596 0.050 Uiso 1 1 d . . . H1BW H 0.2615 0.9540 0.8493 0.050 Uiso 1 1 d . . . H2BW H 0.4355 0.5891 0.1840 0.050 Uiso 1 1 d . . . H2AW H 0.3849 0.6295 0.0830 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.01278(16) 0.01330(14) 0.01436(16) 0.00699(11) 0.00158(11) 0.00164(11) Co 0.01085(18) 0.01222(15) 0.01399(18) 0.00672(13) 0.00098(13) 0.00079(12) O1 0.0324(11) 0.0170(9) 0.0213(10) 0.0079(8) 0.0069(9) 0.0088(8) O3 0.0164(10) 0.0281(10) 0.0257(10) 0.0159(8) 0.0063(8) 0.0013(8) N8 0.0146(11) 0.0171(10) 0.0192(11) 0.0099(9) 0.0026(9) 0.0021(8) O2 0.0276(11) 0.0247(9) 0.0239(10) 0.0148(8) 0.0005(9) 0.0063(8) N5 0.0115(10) 0.0157(10) 0.0165(11) 0.0076(8) 0.0017(8) -0.0008(8) O1S 0.0213(10) 0.0385(11) 0.0154(10) 0.0092(9) 0.0020(8) 0.0047(9) O1W 0.0352(12) 0.0176(9) 0.0146(9) 0.0074(7) 0.0006(8) 0.0001(8) O4 0.0160(10) 0.0265(10) 0.0250(10) 0.0094(8) -0.0020(8) -0.0030(8) N10 0.0143(11) 0.0157(10) 0.0166(11) 0.0067(8) 0.0010(9) 0.0008(8) O2S 0.0564(15) 0.0272(11) 0.0267(12) 0.0087(9) 0.0019(11) 0.0086(11) N7 0.0143(11) 0.0151(9) 0.0178(11) 0.0083(8) 0.0012(9) 0.0020(8) N3 0.0115(10) 0.0172(10) 0.0190(11) 0.0110(9) 0.0009(9) -0.0005(8) N4 0.0122(10) 0.0147(9) 0.0178(11) 0.0083(8) 0.0029(9) 0.0015(8) N1 0.0135(11) 0.0144(9) 0.0171(11) 0.0075(8) 0.0012(9) 0.0010(8) N9 0.0135(11) 0.0161(10) 0.0186(11) 0.0101(8) 0.0025(9) 0.0023(8) C18 0.0290(18) 0.0356(17) 0.041(2) 0.0150(15) 0.0026(15) 0.0054(14) N6 0.0150(11) 0.0143(9) 0.0173(11) 0.0084(8) 0.0019(9) 0.0036(8) C20 0.0156(13) 0.0160(11) 0.0225(14) 0.0100(10) 0.0018(11) 0.0008(10) C21 0.0159(13) 0.0175(11) 0.0202(13) 0.0111(10) -0.0010(11) 0.0009(10) C22 0.0144(12) 0.0123(10) 0.0186(13) 0.0087(9) 0.0038(10) 0.0024(9) N2 0.0132(11) 0.0145(9) 0.0183(11) 0.0090(8) -0.0002(9) 0.0007(8) C24 0.0131(12) 0.0174(11) 0.0208(13) 0.0102(10) -0.0012(10) -0.0014(10) C25 0.0120(13) 0.0192(12) 0.0269(14) 0.0129(11) 0.0024(11) 0.0021(10) C26 0.0132(13) 0.0186(11) 0.0194(13) 0.0090(10) 0.0050(10) 0.0006(10) C27 0.0132(12) 0.0159(11) 0.0196(13) 0.0101(10) 0.0025(10) -0.0006(9) O9 0.0631(17) 0.0460(14) 0.0384(14) 0.0289(12) 0.0044(12) 0.0108(13) C29 0.0185(13) 0.0160(11) 0.0140(12) 0.0051(10) 0.0012(10) 0.0027(10) C30 0.0154(13) 0.0180(11) 0.0188(13) 0.0101(10) 0.0012(10) -0.0009(10) C31 0.0163(13) 0.0191(12) 0.0218(13) 0.0140(10) 0.0031(11) 0.0017(10) C32 0.0248(15) 0.0266(13) 0.0190(14) 0.0079(11) -0.0015(12) -0.0009(12) C33 0.0121(12) 0.0133(11) 0.0172(12) 0.0064(9) -0.0002(10) -0.0029(9) N11 0.122(3) 0.0273(14) 0.0161(14) 0.0104(11) -0.0024(17) 0.0015(17) C35 0.0245(15) 0.0173(12) 0.0197(14) 0.0051(10) 0.0034(11) 0.0010(11) C36 0.0128(13) 0.0219(12) 0.0235(14) 0.0166(11) 0.0017(11) 0.0031(10) C37 0.0154(13) 0.0187(12) 0.0274(15) 0.0136(11) 0.0022(11) 0.0038(10) C38 0.0265(15) 0.0241(13) 0.0200(14) 0.0129(11) -0.0011(12) 0.0006(11) C39 0.0152(13) 0.0149(11) 0.0198(13) 0.0072(10) 0.0021(11) 0.0026(10) C40 0.0153(13) 0.0172(11) 0.0193(13) 0.0080(10) 0.0036(10) -0.0004(10) N12 0.051(2) 0.0493(18) 0.0342(16) 0.0194(14) 0.0072(15) 0.0162(15) C42 0.0153(13) 0.0202(12) 0.0163(13) 0.0097(10) 0.0006(10) 0.0024(10) O5 0.0393(17) 0.0661(19) 0.065(2) -0.0046(15) 0.0066(15) 0.0046(15) C44 0.0133(12) 0.0149(11) 0.0170(12) 0.0092(10) -0.0024(10) 0.0024(9) C45 0.0149(13) 0.0170(11) 0.0175(13) 0.0096(10) 0.0012(10) -0.0010(10) O10 0.100(2) 0.0319(13) 0.0371(15) 0.0042(11) 0.0171(15) 0.0033(14) O8 0.118(3) 0.0350(13) 0.0265(13) 0.0172(10) 0.0123(15) 0.0294(15) O2W 0.075(2) 0.0573(18) 0.073(2) 0.0171(16) -0.0072(18) 0.0113(16) C49 0.0178(14) 0.0207(12) 0.0199(14) 0.0092(11) -0.0016(11) -0.0003(10) C50 0.0161(13) 0.0169(11) 0.0210(13) 0.0066(10) 0.0003(11) -0.0017(10) C51 0.0181(13) 0.0179(11) 0.0202(13) 0.0105(10) 0.0008(11) -0.0018(10) C52 0.0184(14) 0.0144(11) 0.0223(14) 0.0073(10) 0.0035(11) 0.0012(10) C53 0.0159(13) 0.0190(12) 0.0198(13) 0.0079(10) 0.0049(11) 0.0055(10) C54 0.0142(13) 0.0156(11) 0.0192(13) 0.0081(10) 0.0042(10) 0.0005(10) C55 0.0169(13) 0.0208(12) 0.0186(13) 0.0105(10) 0.0006(11) 0.0001(10) N14 0.0416(16) 0.0243(12) 0.0256(14) 0.0124(10) 0.0105(12) 0.0057(11) C57 0.0203(15) 0.0322(15) 0.0214(14) 0.0116(12) 0.0035(12) 0.0021(12) C58 0.0157(13) 0.0223(12) 0.0190(13) 0.0095(11) 0.0060(11) 0.0051(10) C59 0.0214(14) 0.0250(13) 0.0256(15) 0.0172(12) -0.0004(12) 0.0024(11) C60 0.0300(16) 0.0249(13) 0.0180(14) 0.0092(11) 0.0010(12) -0.0011(12) C61 0.0166(13) 0.0207(12) 0.0160(13) 0.0094(10) -0.0006(10) 0.0019(10) C62 0.0312(17) 0.0409(16) 0.0153(14) 0.0114(12) 0.0005(12) 0.0005(14) C63 0.042(2) 0.0449(19) 0.0353(19) 0.0158(16) -0.0087(16) 0.0084(16) C64 0.041(2) 0.0363(18) 0.0316(18) 0.0127(14) 0.0014(15) -0.0005(15) N13 0.056(3) 0.091(3) 0.044(2) 0.016(2) 0.0088(19) 0.002(2) C66 0.077(3) 0.043(2) 0.047(2) 0.0126(18) 0.009(2) -0.015(2) O6 0.099(4) 0.271(9) 0.232(8) 0.174(7) -0.042(4) 0.012(5) O7 0.108(3) 0.115(4) 0.086(3) 0.028(3) 0.002(3) -0.013(3) C69 0.063(3) 0.042(2) 0.050(2) 0.0191(18) -0.006(2) 0.0007(19) C70 0.068(3) 0.047(2) 0.055(3) 0.021(2) 0.004(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn O1S 2.105(2) . ? Zn O1W 2.143(2) . ? Zn N7 2.154(2) . ? Zn N9 2.155(2) . ? Zn N10 2.163(2) . ? Zn N8 2.178(2) . ? Co N6 1.858(2) . ? Co N5 1.868(2) . ? Co N1 1.962(2) 1_545 ? Co N4 1.964(2) 2_666 ? Co N3 1.967(2) 2_566 ? Co N2 1.980(2) . ? O1 C26 1.232(3) . ? O3 C31 1.236(3) . ? N8 C54 1.328(3) . ? N8 C50 1.351(3) . ? O2 C24 1.229(3) . ? N5 C40 1.328(3) . ? N5 C30 1.334(3) . ? O1S C18 1.224(4) . ? O1W H1AW 0.9161 . ? O1W H1BW 0.8848 . ? O4 C39 1.234(3) . ? N10 C45 1.341(3) . ? N10 C55 1.341(3) . ? O2S C64 1.193(4) . ? N7 C42 1.329(3) . ? N7 C53 1.345(3) . ? N3 C31 1.349(3) . ? N3 C27 1.403(3) . ? N3 Co 1.967(2) 2_566 ? N4 C39 1.341(3) . ? N4 C33 1.419(3) . ? N4 Co 1.964(2) 2_666 ? N1 C26 1.351(3) . ? N1 C22 1.419(3) . ? N1 Co 1.962(2) 1_565 ? N9 C29 1.330(3) . ? N9 C61 1.352(3) . ? C18 N11 1.303(5) . ? C18 H18 1.081(4) . ? N6 C21 1.325(3) . ? N6 C36 1.341(3) . ? C20 C22 1.382(4) . ? C20 C49 1.392(4) . ? C20 H20 0.9500 . ? C21 C32 1.389(4) . ? C21 C39 1.509(4) 2_666 ? C22 C29 1.405(4) . ? N2 C24 1.352(3) . ? N2 C44 1.416(3) . ? C24 C30 1.496(3) . ? C25 C59 1.374(4) . ? C25 C33 1.396(4) . ? C25 H25 0.9500 . ? C26 C40 1.497(4) 1_565 ? C27 C37 1.396(3) . ? C27 C54 1.397(4) . ? O9 N14 1.257(3) . ? C29 H29 0.9500 . ? C30 C38 1.384(4) . ? C31 C36 1.501(4) 2_566 ? C32 C62 1.390(4) . ? C32 H32 0.9500 . ? C33 C45 1.394(4) . ? N11 C70 1.437(5) . ? N11 C66 1.494(5) . ? C35 C60 1.385(4) . ? C35 C40 1.387(4) . ? C35 H35 0.9500 . ? C36 C57 1.374(4) . ? C36 C31 1.501(4) 2_566 ? C37 C52 1.385(4) . ? C37 H37 0.9500 . ? C38 C60 1.400(4) . ? C38 H38 0.9500 . ? C39 C21 1.509(4) 2_666 ? C40 C26 1.497(4) 1_545 ? N12 C64 1.296(5) . ? N12 C63 1.468(5) . ? N12 C69 1.482(5) . ? C42 C44 1.403(4) . ? C42 H42 0.9500 . ? O5 N13 1.218(5) . ? C44 C51 1.382(4) . ? C45 H45 0.9500 . ? O10 N14 1.222(3) . ? O8 N14 1.236(3) . ? O2W H2BW 1.1051 . ? O2W H2AW 1.0030 . ? C49 C61 1.385(4) . ? C49 H49 0.9500 . ? C50 C52 1.383(4) . ? C50 H50 0.9500 . ? C51 C58 1.398(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C58 1.377(4) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C59 1.384(4) . ? C55 H55 0.9500 . ? C57 C62 1.399(4) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64B 1.087(4) . ? N13 O6 1.482(7) . ? N13 O7 1.484(7) . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 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 O1S Zn O1W 178.45(7) . . ? O1S Zn N7 94.78(8) . . ? O1W Zn N7 86.63(8) . . ? O1S Zn N9 91.37(8) . . ? O1W Zn N9 87.22(8) . . ? N7 Zn N9 173.85(8) . . ? O1S Zn N10 86.81(8) . . ? O1W Zn N10 93.81(8) . . ? N7 Zn N10 91.07(8) . . ? N9 Zn N10 89.40(8) . . ? O1S Zn N8 86.29(8) . . ? O1W Zn N8 93.07(8) . . ? N7 Zn N8 90.52(8) . . ? N9 Zn N8 89.76(8) . . ? N10 Zn N8 173.02(8) . . ? N6 Co N5 179.76(9) . . ? N6 Co N1 98.38(9) . 1_545 ? N5 Co N1 81.47(9) . 1_545 ? N6 Co N4 81.23(9) . 2_666 ? N5 Co N4 98.58(9) . 2_666 ? N1 Co N4 90.63(9) 1_545 2_666 ? N6 Co N3 81.93(9) . 2_566 ? N5 Co N3 98.25(9) . 2_566 ? N1 Co N3 91.97(9) 1_545 2_566 ? N4 Co N3 163.17(9) 2_666 2_566 ? N6 Co N2 98.83(9) . . ? N5 Co N2 81.32(9) . . ? N1 Co N2 162.79(9) 1_545 . ? N4 Co N2 91.93(9) 2_666 . ? N3 Co N2 90.49(9) 2_566 . ? C54 N8 C50 118.2(2) . . ? C54 N8 Zn 120.79(16) . . ? C50 N8 Zn 119.92(18) . . ? C40 N5 C30 122.3(2) . . ? C40 N5 Co 118.87(18) . . ? C30 N5 Co 118.83(17) . . ? C18 O1S Zn 141.9(2) . . ? Zn O1W H1AW 131.7 . . ? Zn O1W H1BW 119.1 . . ? H1AW O1W H1BW 108.3 . . ? C45 N10 C55 119.0(2) . . ? C45 N10 Zn 121.59(17) . . ? C55 N10 Zn 118.71(17) . . ? C42 N7 C53 118.0(2) . . ? C42 N7 Zn 122.35(18) . . ? C53 N7 Zn 119.53(16) . . ? C31 N3 C27 119.1(2) . . ? C31 N3 Co 115.04(17) . 2_566 ? C27 N3 Co 124.50(17) . 2_566 ? C39 N4 C33 119.4(2) . . ? C39 N4 Co 115.77(17) . 2_666 ? C33 N4 Co 124.33(17) . 2_666 ? C26 N1 C22 115.4(2) . . ? C26 N1 Co 115.53(17) . 1_565 ? C22 N1 Co 128.69(16) . 1_565 ? C29 N9 C61 118.3(2) . . ? C29 N9 Zn 121.58(18) . . ? C61 N9 Zn 119.96(17) . . ? O1S C18 N11 123.5(3) . . ? O1S C18 H18 119.7(3) . . ? N11 C18 H18 116.8(3) . . ? C21 N6 C36 122.7(2) . . ? C21 N6 Co 119.05(18) . . ? C36 N6 Co 118.19(18) . . ? C22 C20 C49 119.9(2) . . ? C22 C20 H20 120.0 . . ? C49 C20 H20 120.0 . . ? N6 C21 C32 120.3(2) . . ? N6 C21 C39 112.7(2) . 2_666 ? C32 C21 C39 127.0(2) . 2_666 ? C20 C22 C29 117.7(2) . . ? C20 C22 N1 122.6(2) . . ? C29 C22 N1 119.7(2) . . ? C24 N2 C44 116.3(2) . . ? C24 N2 Co 115.41(16) . . ? C44 N2 Co 127.82(17) . . ? O2 C24 N2 128.0(2) . . ? O2 C24 C30 121.0(2) . . ? N2 C24 C30 111.0(2) . . ? C59 C25 C33 119.7(2) . . ? C59 C25 H25 120.1 . . ? C33 C25 H25 120.1 . . ? O1 C26 N1 127.8(3) . . ? O1 C26 C40 121.0(2) . 1_565 ? N1 C26 C40 111.2(2) . 1_565 ? C37 C27 C54 117.0(2) . . ? C37 C27 N3 121.0(2) . . ? C54 C27 N3 121.9(2) . . ? N9 C29 C22 123.1(2) . . ? N9 C29 H29 118.5 . . ? C22 C29 H29 118.5 . . ? N5 C30 C38 120.4(2) . . ? N5 C30 C24 113.2(2) . . ? C38 C30 C24 126.4(2) . . ? O3 C31 N3 128.1(3) . . ? O3 C31 C36 121.0(2) . 2_566 ? N3 C31 C36 110.9(2) . 2_566 ? C21 C32 C62 118.3(3) . . ? C21 C32 H32 120.9 . . ? C62 C32 H32 120.9 . . ? C45 C33 C25 117.6(2) . . ? C45 C33 N4 122.6(2) . . ? C25 C33 N4 119.8(2) . . ? C18 N11 C70 121.4(3) . . ? C18 N11 C66 116.5(3) . . ? C70 N11 C66 117.5(3) . . ? C60 C35 C40 118.4(2) . . ? C60 C35 H35 120.8 . . ? C40 C35 H35 120.8 . . ? N6 C36 C57 120.1(3) . . ? N6 C36 C31 113.0(2) . 2_566 ? C57 C36 C31 126.9(2) . 2_566 ? C52 C37 C27 119.5(2) . . ? C52 C37 H37 120.2 . . ? C27 C37 H37 120.2 . . ? C30 C38 C60 118.3(3) . . ? C30 C38 H38 120.9 . . ? C60 C38 H38 120.9 . . ? O4 C39 N4 128.4(2) . . ? O4 C39 C21 121.4(2) . 2_666 ? N4 C39 C21 110.2(2) . 2_666 ? N5 C40 C35 120.6(2) . . ? N5 C40 C26 112.8(2) . 1_545 ? C35 C40 C26 126.6(2) . 1_545 ? C64 N12 C63 122.1(3) . . ? C64 N12 C69 120.9(3) . . ? C63 N12 C69 117.0(3) . . ? N7 C42 C44 123.6(2) . . ? N7 C42 H42 118.2 . . ? C44 C42 H42 118.2 . . ? C51 C44 C42 117.7(2) . . ? C51 C44 N2 122.2(2) . . ? C42 C44 N2 120.1(2) . . ? N10 C45 C33 122.5(2) . . ? N10 C45 H45 118.7 . . ? C33 C45 H45 118.7 . . ? H2BW O2W H2AW 122.1 . . ? C61 C49 C20 118.3(3) . . ? C61 C49 H49 120.8 . . ? C20 C49 H49 120.8 . . ? N8 C50 C52 122.0(2) . . ? N8 C50 H50 119.0 . . ? C52 C50 H50 119.0 . . ? C44 C51 C58 118.9(2) . . ? C44 C51 H51 120.5 . . ? C58 C51 H51 120.5 . . ? C50 C52 C37 119.2(2) . . ? C50 C52 H52 120.4 . . ? C37 C52 H52 120.4 . . ? N7 C53 C58 122.5(2) . . ? N7 C53 H53 118.7 . . ? C58 C53 H53 118.7 . . ? N8 C54 C27 123.9(2) . . ? N8 C54 H54 118.0 . . ? C27 C54 H54 118.0 . . ? N10 C55 C59 121.8(3) . . ? N10 C55 H55 119.1 . . ? C59 C55 H55 119.1 . . ? O10 N14 O8 118.6(3) . . ? O10 N14 O9 122.4(3) . . ? O8 N14 O9 119.0(2) . . ? C36 C57 C62 118.6(3) . . ? C36 C57 H57 120.7 . . ? C62 C57 H57 120.7 . . ? C53 C58 C51 119.2(2) . . ? C53 C58 H58 120.4 . . ? C51 C58 H58 120.4 . . ? C25 C59 C55 119.2(3) . . ? C25 C59 H59 120.4 . . ? C55 C59 H59 120.4 . . ? C35 C60 C38 120.0(3) . . ? C35 C60 H60 120.0 . . ? C38 C60 H60 120.0 . . ? N9 C61 C49 122.6(2) . . ? N9 C61 H61 118.7 . . ? C49 C61 H61 118.7 . . ? C32 C62 C57 120.0(3) . . ? C32 C62 H62 120.0 . . ? C57 C62 H62 120.0 . . ? N12 C63 H63A 109.5 . . ? N12 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N12 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O2S C64 N12 123.8(3) . . ? O2S C64 H64B 123.7(4) . . ? N12 C64 H64B 112.5(3) . . ? O5 N13 O6 117.2(5) . . ? O5 N13 O7 121.1(4) . . ? O6 N13 O7 121.6(5) . . ? N11 C66 H66A 109.5 . . ? N11 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N11 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N12 C69 H69A 109.5 . . ? N12 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N12 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N11 C70 H70A 109.5 . . ? N11 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N11 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 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 O1S Zn N8 C54 34.7(2) . . . . ? O1W Zn N8 C54 -146.8(2) . . . . ? N7 Zn N8 C54 -60.1(2) . . . . ? N9 Zn N8 C54 126.0(2) . . . . ? N10 Zn N8 C54 43.0(7) . . . . ? O1S Zn N8 C50 -133.2(2) . . . . ? O1W Zn N8 C50 45.4(2) . . . . ? N7 Zn N8 C50 132.0(2) . . . . ? N9 Zn N8 C50 -41.8(2) . . . . ? N10 Zn N8 C50 -124.9(6) . . . . ? N6 Co N5 C40 54(24) . . . . ? N1 Co N5 C40 1.75(19) 1_545 . . . ? N4 Co N5 C40 91.1(2) 2_666 . . . ? N3 Co N5 C40 -89.0(2) 2_566 . . . ? N2 Co N5 C40 -178.3(2) . . . . ? N6 Co N5 C30 -127(24) . . . . ? N1 Co N5 C30 -179.0(2) 1_545 . . . ? N4 Co N5 C30 -89.7(2) 2_666 . . . ? N3 Co N5 C30 90.2(2) 2_566 . . . ? N2 Co N5 C30 0.99(19) . . . . ? O1W Zn O1S C18 -156(3) . . . . ? N7 Zn O1S C18 -0.3(3) . . . . ? N9 Zn O1S C18 179.8(3) . . . . ? N10 Zn O1S C18 90.5(3) . . . . ? N8 Zn O1S C18 -90.5(3) . . . . ? O1S Zn N10 C45 34.32(19) . . . . ? O1W Zn N10 C45 -144.25(19) . . . . ? N7 Zn N10 C45 129.1(2) . . . . ? N9 Zn N10 C45 -57.1(2) . . . . ? N8 Zn N10 C45 26.0(7) . . . . ? O1S Zn N10 C55 -136.34(19) . . . . ? O1W Zn N10 C55 45.09(19) . . . . ? N7 Zn N10 C55 -41.60(19) . . . . ? N9 Zn N10 C55 132.26(19) . . . . ? N8 Zn N10 C55 -144.7(6) . . . . ? O1S Zn N7 C42 43.6(2) . . . . ? O1W Zn N7 C42 -137.1(2) . . . . ? N9 Zn N7 C42 -137.6(7) . . . . ? N10 Zn N7 C42 -43.3(2) . . . . ? N8 Zn N7 C42 129.9(2) . . . . ? O1S Zn N7 C53 -132.9(2) . . . . ? O1W Zn N7 C53 46.5(2) . . . . ? N9 Zn N7 C53 45.9(8) . . . . ? N10 Zn N7 C53 140.2(2) . . . . ? N8 Zn N7 C53 -46.6(2) . . . . ? O1S Zn N9 C29 36.12(19) . . . . ? O1W Zn N9 C29 -143.24(19) . . . . ? N7 Zn N9 C29 -142.7(7) . . . . ? N10 Zn N9 C29 122.9(2) . . . . ? N8 Zn N9 C29 -50.16(19) . . . . ? O1S Zn N9 C61 -139.27(18) . . . . ? O1W Zn N9 C61 41.37(18) . . . . ? N7 Zn N9 C61 41.9(8) . . . . ? N10 Zn N9 C61 -52.47(18) . . . . ? N8 Zn N9 C61 134.45(18) . . . . ? Zn O1S C18 N11 178.2(3) . . . . ? N5 Co N6 C21 34(24) . . . . ? N1 Co N6 C21 86.15(19) 1_545 . . . ? N4 Co N6 C21 -3.19(18) 2_666 . . . ? N3 Co N6 C21 176.97(19) 2_566 . . . ? N2 Co N6 C21 -93.79(19) . . . . ? N5 Co N6 C36 -149(41) . . . . ? N1 Co N6 C36 -96.24(19) 1_545 . . . ? N4 Co N6 C36 174.42(19) 2_666 . . . ? N3 Co N6 C36 -5.42(18) 2_566 . . . ? N2 Co N6 C36 83.81(19) . . . . ? C36 N6 C21 C32 0.3(4) . . . . ? Co N6 C21 C32 177.8(2) . . . . ? C36 N6 C21 C39 -179.8(2) . . . 2_666 ? Co N6 C21 C39 -2.3(3) . . . 2_666 ? C49 C20 C22 C29 0.8(4) . . . . ? C49 C20 C22 N1 -177.8(2) . . . . ? C26 N1 C22 C20 119.9(3) . . . . ? Co N1 C22 C20 -67.9(3) 1_565 . . . ? C26 N1 C22 C29 -58.6(3) . . . . ? Co N1 C22 C29 113.6(2) 1_565 . . . ? N6 Co N2 C24 175.93(18) . . . . ? N5 Co N2 C24 -3.88(18) . . . . ? N1 Co N2 C24 -3.9(4) 1_545 . . . ? N4 Co N2 C24 94.51(19) 2_666 . . . ? N3 Co N2 C24 -102.16(19) 2_566 . . . ? N6 Co N2 C44 3.8(2) . . . . ? N5 Co N2 C44 -176.0(2) . . . . ? N1 Co N2 C44 -176.0(3) 1_545 . . . ? N4 Co N2 C44 -77.6(2) 2_666 . . . ? N3 Co N2 C44 85.7(2) 2_566 . . . ? C44 N2 C24 O2 0.0(4) . . . . ? Co N2 C24 O2 -173.1(2) . . . . ? C44 N2 C24 C30 178.7(2) . . . . ? Co N2 C24 C30 5.6(3) . . . . ? C22 N1 C26 O1 -2.5(4) . . . . ? Co N1 C26 O1 -175.7(2) 1_565 . . . ? C22 N1 C26 C40 177.2(2) . . . 1_565 ? Co N1 C26 C40 3.9(3) 1_565 . . 1_565 ? C31 N3 C27 C37 120.6(3) . . . . ? Co N3 C27 C37 -73.5(3) 2_566 . . . ? C31 N3 C27 C54 -60.2(3) . . . . ? Co N3 C27 C54 105.8(2) 2_566 . . . ? C61 N9 C29 C22 2.2(4) . . . . ? Zn N9 C29 C22 -173.24(18) . . . . ? C20 C22 C29 N9 -2.6(4) . . . . ? N1 C22 C29 N9 176.0(2) . . . . ? C40 N5 C30 C38 0.8(4) . . . . ? Co N5 C30 C38 -178.4(2) . . . . ? C40 N5 C30 C24 -179.0(2) . . . . ? Co N5 C30 C24 1.8(3) . . . . ? O2 C24 C30 N5 174.0(2) . . . . ? N2 C24 C30 N5 -4.8(3) . . . . ? O2 C24 C30 C38 -5.8(4) . . . . ? N2 C24 C30 C38 175.4(3) . . . . ? C27 N3 C31 O3 -1.0(4) . . . . ? Co N3 C31 O3 -168.2(2) 2_566 . . . ? C27 N3 C31 C36 177.7(2) . . . 2_566 ? Co N3 C31 C36 10.5(3) 2_566 . . 2_566 ? N6 C21 C32 C62 -1.0(4) . . . . ? C39 C21 C32 C62 179.1(3) 2_666 . . . ? C59 C25 C33 C45 -1.6(4) . . . . ? C59 C25 C33 N4 177.4(2) . . . . ? C39 N4 C33 C45 -64.9(3) . . . . ? Co N4 C33 C45 106.6(2) 2_666 . . . ? C39 N4 C33 C25 116.1(3) . . . . ? Co N4 C33 C25 -72.4(3) 2_666 . . . ? O1S C18 N11 C70 -17.1(6) . . . . ? O1S C18 N11 C66 -172.6(4) . . . . ? C21 N6 C36 C57 0.1(4) . . . . ? Co N6 C36 C57 -177.38(19) . . . . ? C21 N6 C36 C31 178.7(2) . . . 2_566 ? Co N6 C36 C31 1.2(3) . . . 2_566 ? C54 C27 C37 C52 -2.1(4) . . . . ? N3 C27 C37 C52 177.1(2) . . . . ? N5 C30 C38 C60 -0.1(4) . . . . ? C24 C30 C38 C60 179.7(3) . . . . ? C33 N4 C39 O4 3.8(4) . . . . ? Co N4 C39 O4 -168.5(2) 2_666 . . . ? C33 N4 C39 C21 -176.0(2) . . . 2_666 ? Co N4 C39 C21 11.8(3) 2_666 . . 2_666 ? C30 N5 C40 C35 -1.0(4) . . . . ? Co N5 C40 C35 178.2(2) . . . . ? C30 N5 C40 C26 -179.3(2) . . . 1_545 ? Co N5 C40 C26 -0.1(3) . . . 1_545 ? C60 C35 C40 N5 0.5(4) . . . . ? C60 C35 C40 C26 178.6(3) . . . 1_545 ? C53 N7 C42 C44 2.7(4) . . . . ? Zn N7 C42 C44 -173.81(19) . . . . ? N7 C42 C44 C51 -1.8(4) . . . . ? N7 C42 C44 N2 176.4(2) . . . . ? C24 N2 C44 C51 119.9(3) . . . . ? Co N2 C44 C51 -68.1(3) . . . . ? C24 N2 C44 C42 -58.2(3) . . . . ? Co N2 C44 C42 113.9(2) . . . . ? C55 N10 C45 C33 2.1(4) . . . . ? Zn N10 C45 C33 -168.55(18) . . . . ? C25 C33 C45 N10 -0.1(4) . . . . ? N4 C33 C45 N10 -179.1(2) . . . . ? C22 C20 C49 C61 1.2(4) . . . . ? C54 N8 C50 C52 -2.5(4) . . . . ? Zn N8 C50 C52 165.7(2) . . . . ? C42 C44 C51 C58 -1.1(4) . . . . ? N2 C44 C51 C58 -179.2(2) . . . . ? N8 C50 C52 C37 0.0(4) . . . . ? C27 C37 C52 C50 2.3(4) . . . . ? C42 N7 C53 C58 -0.8(4) . . . . ? Zn N7 C53 C58 175.8(2) . . . . ? C50 N8 C54 C27 2.7(4) . . . . ? Zn N8 C54 C27 -165.4(2) . . . . ? C37 C27 C54 N8 -0.4(4) . . . . ? N3 C27 C54 N8 -179.7(2) . . . . ? C45 N10 C55 C59 -2.3(4) . . . . ? Zn N10 C55 C59 168.6(2) . . . . ? N6 C36 C57 C62 0.2(4) . . . . ? C31 C36 C57 C62 -178.2(3) 2_566 . . . ? N7 C53 C58 C51 -2.0(4) . . . . ? C44 C51 C58 C53 2.8(4) . . . . ? C33 C25 C59 C55 1.4(4) . . . . ? N10 C55 C59 C25 0.6(4) . . . . ? C40 C35 C60 C38 0.2(4) . . . . ? C30 C38 C60 C35 -0.4(4) . . . . ? C29 N9 C61 C49 -0.1(4) . . . . ? Zn N9 C61 C49 175.5(2) . . . . ? C20 C49 C61 N9 -1.6(4) . . . . ? C21 C32 C62 C57 1.3(5) . . . . ? C36 C57 C62 C32 -0.9(4) . . . . ? C63 N12 C64 O2S 3.7(6) . . . . ? C69 N12 C64 O2S -174.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.678 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.094 data_2 _database_code_depnum_ccdc_archive 'CCDC 767586' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C34 H22 Co N10 O4), 2(C8 H20 N), H2 O' _chemical_formula_sum 'C84 H86 Co2 N22 O9' _chemical_formula_weight 1665.61 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 _symmetry_space_group_name_HALL -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2583(7) _cell_length_b 13.8731(6) _cell_length_c 28.5219(16) _cell_angle_alpha 89.676(4) _cell_angle_beta 81.893(5) _cell_angle_gamma 80.586(5) _cell_volume 3963.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9854 _cell_measurement_theta_min 3.0069 _cell_measurement_theta_max 33.1373 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 0.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.931 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_process_details ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.49b (release 14-10-2009 CrysAlis171 .NET) (compiled Oct 14 2009,10:37:23) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9853 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40979 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 28.28 _reflns_number_total 19658 _reflns_number_gt 12324 _reflns_threshold_expression >2sigma(I) _computing_data_collection ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.49b (release 14-10-2009 CrysAlis171 .NET) (compiled Oct 14 2009,10:37:23) ; _computing_cell_refinement ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.49b (release 14-10-2009 CrysAlis171 .NET) (compiled Oct 14 2009,10:37:23) ; _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0869P)^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 19658 _refine_ls_number_parameters 1062 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1604 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Co2 Co 0.44361(3) -0.24241(2) 0.357950(13) 0.02891(10) Uani 1 1 d . . . C01 Co 0.91318(3) -0.73260(2) 0.139890(13) 0.02970(10) Uani 1 1 d . . . O2 O 0.9189(2) -1.02294(15) 0.15252(8) 0.0539(6) Uani 1 1 d . . . O6 O 0.5648(2) -0.37958(17) 0.23121(8) 0.0542(6) Uani 1 1 d . . . O8 O 0.3425(2) 0.04507(15) 0.33314(9) 0.0528(6) Uani 1 1 d . . . O4 O 0.8780(2) -0.63778(17) 0.27511(8) 0.0550(6) Uani 1 1 d . . . C27 C 0.9854(5) -0.8810(3) -0.04349(14) 0.0721(12) Uani 1 1 d . . . H27 H 0.9729 -0.9100 -0.0715 0.087 Uiso 1 1 calc R . . N15 N 0.6191(2) -0.30384(15) 0.34266(8) 0.0289(5) Uani 1 1 d . . . N14 N 0.3680(2) -0.35506(16) 0.38497(8) 0.0354(5) Uani 1 1 d . . . N13 N 0.4646(2) -0.11053(16) 0.33622(8) 0.0344(5) Uani 1 1 d . . . N1 N 0.8090(2) -0.61506(16) 0.11754(8) 0.0356(5) Uani 1 1 d . . . N5 N 0.7729(2) -0.78814(17) 0.12295(8) 0.0331(5) Uani 1 1 d . . . N3 N 1.0401(2) -0.74801(17) 0.08029(9) 0.0386(6) Uani 1 1 d . . . N2 N 0.9753(2) -0.86777(16) 0.15612(8) 0.0356(5) Uani 1 1 d . . . N12 N 0.5064(2) -0.21698(16) 0.41769(8) 0.0348(5) Uani 1 1 d . . . O9 O 0.1657(2) -0.39611(18) 0.41921(10) 0.0657(7) Uani 1 1 d . . . O7 O 0.7008(2) -0.23804(19) 0.45205(8) 0.0606(7) Uani 1 1 d . . . N21 N 0.4772(3) -0.26902(19) 0.08235(10) 0.0492(7) Uani 1 1 d . . . N16 N 0.2667(2) -0.18191(16) 0.37235(8) 0.0331(5) Uani 1 1 d . . . N6 N 1.0482(2) -0.67546(15) 0.15972(8) 0.0328(5) Uani 1 1 d . . . O1 O 0.6045(2) -0.56137(18) 0.09267(10) 0.0667(7) Uani 1 1 d . . . O3 O 1.2528(2) -0.7181(2) 0.05042(10) 0.0750(9) Uani 1 1 d . . . N11 N 0.4345(2) -0.28736(16) 0.29358(8) 0.0334(5) Uani 1 1 d . . . N10 N 0.4709(3) -0.6462(2) 0.24884(11) 0.0586(8) Uani 1 1 d . . . C37 C 0.6587(3) -0.34798(19) 0.30036(10) 0.0324(6) Uani 1 1 d . . . C74 C 0.5977(5) -0.2694(3) 0.1061(2) 0.1048(19) Uani 1 1 d . . . H74A H 0.6698 -0.2554 0.0826 0.126 Uiso 1 1 calc R . . H74B H 0.6241 -0.3349 0.1173 0.126 Uiso 1 1 calc R . . C21 C 1.0312(3) -0.63924(19) 0.20385(10) 0.0360(6) Uani 1 1 d . . . N22 N 0.1295(3) -0.6993(2) 0.42370(11) 0.0602(8) Uani 1 1 d . . . N8 N 0.8920(3) -0.8087(2) -0.02411(11) 0.0670(9) Uani 1 1 d . . . N4 N 0.8309(2) -0.69892(16) 0.20508(8) 0.0332(5) Uani 1 1 d . . . C65 C 0.5027(3) -0.5089(2) 0.35273(11) 0.0473(8) Uani 1 1 d . . . H65 H 0.4869 -0.4913 0.3223 0.057 Uiso 1 1 calc R . . N7 N 1.3229(3) -0.9878(2) 0.15506(12) 0.0642(8) Uani 1 1 d . . . C38 C 0.7004(3) -0.3052(2) 0.37533(10) 0.0353(6) Uani 1 1 d . . . N17 N 0.1392(3) -0.3593(2) 0.25362(13) 0.0682(9) Uani 1 1 d . . . C55 C 0.1768(3) -0.2360(2) 0.39084(11) 0.0408(7) Uani 1 1 d . . . N19 N 0.7614(3) 0.0102(2) 0.32734(13) 0.0639(8) Uani 1 1 d . . . C64 C 0.4445(3) -0.4481(2) 0.39084(11) 0.0373(6) Uani 1 1 d . . . C34 C 0.5953(3) -0.6373(2) 0.23075(12) 0.0461(7) Uani 1 1 d . . . H34 H 0.6118 -0.5759 0.2209 0.055 Uiso 1 1 calc R . . C12 C 0.8983(3) -0.9336(2) 0.14688(10) 0.0382(7) Uani 1 1 d . . . C31 C 0.6763(3) -0.8049(2) 0.24070(12) 0.0494(8) Uani 1 1 d . . . H31 H 0.7451 -0.8581 0.2381 0.059 Uiso 1 1 calc R . . C29 C 0.9039(3) -0.6584(2) 0.23208(10) 0.0363(6) Uani 1 1 d . . . C32 C 0.5492(4) -0.8158(3) 0.25925(13) 0.0601(9) Uani 1 1 d . . . H32 H 0.5300 -0.8764 0.2694 0.072 Uiso 1 1 calc R . . C4 C 0.7756(3) -0.8835(2) 0.12872(10) 0.0385(7) Uani 1 1 d . . . C61 C 0.8233(4) -0.0253(3) 0.28547(16) 0.0653(11) Uani 1 1 d . . . H61 H 0.9063 -0.0084 0.2747 0.078 Uiso 1 1 calc R . . C35 C 0.8719(3) -0.4026(3) 0.32266(13) 0.0576(9) Uani 1 1 d . . . H35 H 0.9579 -0.4376 0.3161 0.069 Uiso 1 1 calc R . . C59 C 0.6522(3) -0.1128(2) 0.27308(12) 0.0499(8) Uani 1 1 d . . . H59 H 0.6148 -0.1525 0.2544 0.060 Uiso 1 1 calc R . . C54 C 0.2345(3) -0.0879(2) 0.36185(10) 0.0387(7) Uani 1 1 d . . . C20 C 1.1553(3) -0.6656(2) 0.12863(12) 0.0427(7) Uani 1 1 d . . . C36 C 0.7865(3) -0.3973(2) 0.28884(12) 0.0512(8) Uani 1 1 d . . . H36 H 0.8152 -0.4265 0.2591 0.061 Uiso 1 1 calc R . . C39 C 0.8298(3) -0.3562(2) 0.36603(13) 0.0505(8) Uani 1 1 d . . . H39 H 0.8871 -0.3591 0.3887 0.061 Uiso 1 1 calc R . . C62 C 0.6453(3) -0.0182(2) 0.34280(13) 0.0505(8) Uani 1 1 d . . . H62 H 0.6008 0.0053 0.3722 0.061 Uiso 1 1 calc R . . C53 C 0.1033(3) -0.0434(3) 0.36788(13) 0.0529(9) Uani 1 1 d . . . H53 H 0.0798 0.0215 0.3598 0.063 Uiso 1 1 calc R . . C40 C 0.5476(3) -0.3397(2) 0.27079(10) 0.0368(6) Uani 1 1 d . . . C24 C 1.0253(3) -0.7965(2) 0.03791(10) 0.0403(7) Uani 1 1 d . . . C8 C 0.8319(3) -0.4596(2) 0.15137(12) 0.0492(8) Uani 1 1 d . . . H8 H 0.7800 -0.4758 0.1788 0.059 Uiso 1 1 calc R . . C63 C 0.2360(3) -0.3385(2) 0.40027(11) 0.0431(7) Uani 1 1 d . . . C46 C 0.6354(3) -0.2499(2) 0.41968(11) 0.0396(7) Uani 1 1 d . . . C30 C 0.7012(3) -0.7138(2) 0.22580(10) 0.0361(6) Uani 1 1 d . . . N9 N 0.8801(4) -0.3750(2) 0.15186(14) 0.0756(10) Uani 1 1 d . . . C57 C 0.3531(3) -0.0427(2) 0.34226(10) 0.0380(7) Uani 1 1 d . . . C7 C 0.8531(3) -0.5233(2) 0.11395(11) 0.0404(7) Uani 1 1 d . . . C42 C 0.2608(3) -0.1954(2) 0.25334(12) 0.0480(8) Uani 1 1 d . . . H42 H 0.3011 -0.1401 0.2534 0.058 Uiso 1 1 calc R . . N20 N 0.5466(4) -0.5655(2) 0.44274(11) 0.0715(9) Uani 1 1 d . . . C18 C 1.2345(3) -0.5780(2) 0.18702(14) 0.0540(9) Uani 1 1 d . . . H18 H 1.2983 -0.5445 0.1964 0.065 Uiso 1 1 calc R . . C60 C 0.7726(4) -0.0852(3) 0.25691(14) 0.0598(9) Uani 1 1 d . . . H60 H 0.8190 -0.1065 0.2274 0.072 Uiso 1 1 calc R . . C16 C 1.3392(4) -0.9674(3) 0.19899(16) 0.0618(10) Uani 1 1 d . . . H16 H 1.4225 -0.9883 0.2082 0.074 Uiso 1 1 calc R . . C47 C 0.4267(3) -0.1676(2) 0.45830(10) 0.0363(6) Uani 1 1 d . . . C41 C 0.3163(3) -0.2804(2) 0.27245(10) 0.0351(6) Uani 1 1 d . . . C58 C 0.5865(3) -0.08115(19) 0.31759(10) 0.0351(6) Uani 1 1 d . . . C17 C 1.2033(3) -0.9554(2) 0.14293(13) 0.0514(8) Uani 1 1 d . . . H17 H 1.1898 -0.9690 0.1123 0.062 Uiso 1 1 calc R . . C6 C 0.6900(3) -0.6247(2) 0.10564(11) 0.0441(7) Uani 1 1 d . . . C13 C 1.0968(3) -0.90264(19) 0.17273(11) 0.0367(6) Uani 1 1 d . . . C23 C 1.1550(3) -0.7135(2) 0.08136(12) 0.0473(8) Uani 1 1 d . . . C3 C 0.6709(3) -0.7292(2) 0.10841(10) 0.0390(7) Uani 1 1 d . . . C75 C 0.3578(8) -0.3787(4) 0.1387(2) 0.146(3) Uani 1 1 d . . . H75A H 0.2739 -0.3781 0.1586 0.219 Uiso 1 1 calc R . . H75B H 0.4289 -0.3899 0.1577 0.219 Uiso 1 1 calc R . . H75C H 0.3704 -0.4298 0.1152 0.219 Uiso 1 1 calc R . . C1 C 0.5631(4) -0.8685(3) 0.10308(14) 0.0630(11) Uani 1 1 d . . . H1 H 0.4909 -0.8959 0.0963 0.076 Uiso 1 1 calc R . . C66 C 0.5843(4) -0.5955(2) 0.35979(13) 0.0554(9) Uani 1 1 d . . . H66 H 0.6259 -0.6359 0.3343 0.067 Uiso 1 1 calc R . . C14 C 1.1173(3) -0.8839(2) 0.21832(12) 0.0466(8) Uani 1 1 d . . . H14 H 1.0491 -0.8493 0.2397 0.056 Uiso 1 1 calc R . . C15 C 1.2408(4) -0.9173(2) 0.23183(14) 0.0594(9) Uani 1 1 d . . . H15 H 1.2570 -0.9061 0.2624 0.071 Uiso 1 1 calc R . . C56 C 0.0430(3) -0.1941(3) 0.39831(13) 0.0570(10) Uani 1 1 d . . . H56 H -0.0215 -0.2305 0.4112 0.068 Uiso 1 1 calc R . . C28 C 0.9151(3) -0.7679(3) 0.01589(11) 0.0518(8) Uani 1 1 d . . . H28 H 0.8517 -0.7165 0.0297 0.062 Uiso 1 1 calc R . . C49 C 0.2854(4) -0.1803(3) 0.53081(13) 0.0664(11) Uani 1 1 d . . . H49 H 0.2437 -0.2195 0.5527 0.080 Uiso 1 1 calc R . . C5 C 0.6689(3) -0.9259(3) 0.11872(12) 0.0521(9) Uani 1 1 d . . . H5 H 0.6695 -0.9925 0.1226 0.063 Uiso 1 1 calc R . . C19 C 1.2511(3) -0.6162(2) 0.14137(13) 0.0532(9) Uani 1 1 d . . . H19 H 1.3254 -0.6086 0.1198 0.064 Uiso 1 1 calc R . . C71 C 0.5217(9) -0.1260(4) 0.0322(2) 0.159(3) Uani 1 1 d . . . H71A H 0.4800 -0.0628 0.0233 0.238 Uiso 1 1 calc R . . H71B H 0.5491 -0.1673 0.0045 0.238 Uiso 1 1 calc R . . H71C H 0.5983 -0.1192 0.0470 0.238 Uiso 1 1 calc R . . C22 C 1.1240(3) -0.5897(2) 0.21847(12) 0.0485(8) Uani 1 1 d . . . H22 H 1.1123 -0.5644 0.2492 0.058 Uiso 1 1 calc R . . C25 C 1.1193(4) -0.8735(2) 0.01699(13) 0.0573(9) Uani 1 1 d . . . H25 H 1.1952 -0.8968 0.0307 0.069 Uiso 1 1 calc R . . C52 C 0.0067(3) -0.0978(3) 0.38640(14) 0.0628(10) Uani 1 1 d . . . H52 H -0.0829 -0.0693 0.3908 0.075 Uiso 1 1 calc R . . C45 C 0.2515(3) -0.3604(2) 0.27152(13) 0.0515(8) Uani 1 1 d . . . H45 H 0.2893 -0.4184 0.2843 0.062 Uiso 1 1 calc R . . C68 C 0.4704(4) -0.4812(2) 0.43517(12) 0.0569(9) Uani 1 1 d . . . H68 H 0.4318 -0.4418 0.4614 0.068 Uiso 1 1 calc R . . C48 C 0.3640(4) -0.2187(3) 0.49305(14) 0.0694(11) Uani 1 1 d . . . H48 H 0.3782 -0.2864 0.4896 0.083 Uiso 1 1 calc R . . C2 C 0.5634(3) -0.7686(3) 0.09733(13) 0.0558(9) Uani 1 1 d . . . H2 H 0.4923 -0.7290 0.0862 0.067 Uiso 1 1 calc R . . C50 C 0.2675(4) -0.0880(4) 0.53683(15) 0.0740(12) Uani 1 1 d . . . H50 H 0.2143 -0.0609 0.5642 0.089 Uiso 1 1 calc R . . C67 C 0.6026(4) -0.6203(3) 0.40471(14) 0.0588(9) Uani 1 1 d . . . H67 H 0.6573 -0.6790 0.4093 0.071 Uiso 1 1 calc R . . C33 C 0.4504(3) -0.7350(3) 0.26249(13) 0.0609(10) Uani 1 1 d . . . H33 H 0.3641 -0.7429 0.2750 0.073 Uiso 1 1 calc R . . C10 C 0.9521(5) -0.3544(3) 0.1121(2) 0.0879(15) Uani 1 1 d . . . H10 H 0.9870 -0.2965 0.1111 0.105 Uiso 1 1 calc R . . C80 C 0.2655(4) -0.7040(3) 0.43809(15) 0.0717(11) Uani 1 1 d . . . H80A H 0.2572 -0.7087 0.4723 0.086 Uiso 1 1 calc R . . H80B H 0.2969 -0.6431 0.4296 0.086 Uiso 1 1 calc R . . C83 C -0.1025(5) -0.5923(5) 0.4418(3) 0.144(3) Uani 1 1 d . . . H83A H -0.1486 -0.5365 0.4605 0.216 Uiso 1 1 calc R . . H83B H -0.1443 -0.6481 0.4506 0.216 Uiso 1 1 calc R . . H83C H -0.1060 -0.5795 0.4088 0.216 Uiso 1 1 calc R . . C43 C 0.1441(4) -0.1927(3) 0.23400(14) 0.0634(10) Uani 1 1 d . . . H43 H 0.1049 -0.1359 0.2206 0.076 Uiso 1 1 calc R . . C44 C 0.0871(4) -0.2762(3) 0.23493(16) 0.0691(11) Uani 1 1 d . . . H44 H 0.0086 -0.2743 0.2219 0.083 Uiso 1 1 calc R . . N18 N 0.3226(6) -0.0268(3) 0.50514(19) 0.1257(18) Uani 1 1 d . . . C78 C 0.1334(5) -0.6859(4) 0.37043(16) 0.0864(14) Uani 1 1 d . . . H78A H 0.1869 -0.7435 0.3543 0.104 Uiso 1 1 calc R . . H78B H 0.0434 -0.6817 0.3628 0.104 Uiso 1 1 calc R . . C26 C 1.0971(5) -0.9144(3) -0.02450(15) 0.0746(12) Uani 1 1 d . . . H26 H 1.1594 -0.9652 -0.0394 0.090 Uiso 1 1 calc R . . C51 C 0.4040(5) -0.0695(3) 0.46395(16) 0.0852(15) Uani 1 1 d . . . H51 H 0.4415 -0.0304 0.4410 0.102 Uiso 1 1 calc R . . C82 C 0.0750(5) -0.7928(4) 0.43389(18) 0.0930(16) Uani 1 1 d . . . H82A H -0.0071 -0.7890 0.4203 0.112 Uiso 1 1 calc R . . H82B H 0.1383 -0.8463 0.4180 0.112 Uiso 1 1 calc R . . C72 C 0.4259(5) -0.1699(3) 0.06579(17) 0.0792(13) Uani 1 1 d . . . H72A H 0.3476 -0.1737 0.0508 0.095 Uiso 1 1 calc R . . H72B H 0.3977 -0.1266 0.0932 0.095 Uiso 1 1 calc R . . C108 C 0.9278(5) -0.4975(3) 0.07363(16) 0.0950(16) Uani 1 1 d . . . H108 H 0.9442 -0.5381 0.0469 0.114 Uiso 1 1 calc R . . C70 C 0.5143(4) -0.3446(3) 0.04311(15) 0.0756(12) Uani 1 1 d . . . H70A H 0.5834 -0.3246 0.0202 0.091 Uiso 1 1 calc R . . H70B H 0.5519 -0.4058 0.0562 0.091 Uiso 1 1 calc R . . C77 C 0.1885(5) -0.5977(4) 0.35154(17) 0.0932(15) Uani 1 1 d . . . H77A H 0.1884 -0.5951 0.3179 0.140 Uiso 1 1 calc R . . H77B H 0.2783 -0.6015 0.3583 0.140 Uiso 1 1 calc R . . H77C H 0.1343 -0.5399 0.3663 0.140 Uiso 1 1 calc R . . C73 C 0.5836(5) -0.1978(4) 0.1479(2) 0.1063(19) Uani 1 1 d . . . H73A H 0.6670 -0.2038 0.1601 0.159 Uiso 1 1 calc R . . H73B H 0.5156 -0.2125 0.1723 0.159 Uiso 1 1 calc R . . H73C H 0.5595 -0.1323 0.1374 0.159 Uiso 1 1 calc R . . C81 C 0.0474(6) -0.8162(4) 0.4848(2) 0.114(2) Uani 1 1 d . . . H81A H 0.0139 -0.8769 0.4879 0.171 Uiso 1 1 calc R . . H81B H -0.0178 -0.7651 0.5008 0.171 Uiso 1 1 calc R . . H81C H 0.1283 -0.8217 0.4986 0.171 Uiso 1 1 calc R . . C79 C 0.3700(5) -0.7874(4) 0.4165(2) 0.1005(17) Uani 1 1 d . . . H79A H 0.4531 -0.7843 0.4278 0.151 Uiso 1 1 calc R . . H79B H 0.3815 -0.7826 0.3826 0.151 Uiso 1 1 calc R . . H79C H 0.3417 -0.8484 0.4254 0.151 Uiso 1 1 calc R . . C11 C 0.9783(6) -0.4122(4) 0.0727(2) 0.119(2) Uani 1 1 d . . . H11 H 1.0296 -0.3941 0.0455 0.143 Uiso 1 1 calc R . . C84 C 0.0433(5) -0.6130(4) 0.4505(2) 0.0970(16) Uani 1 1 d . . . H84A H 0.0831 -0.5553 0.4423 0.116 Uiso 1 1 calc R . . H84B H 0.0448 -0.6234 0.4841 0.116 Uiso 1 1 calc R . . C76 C 0.3581(6) -0.2899(4) 0.11674(18) 0.117(2) Uani 1 1 d . . . H76A H 0.3417 -0.2402 0.1416 0.140 Uiso 1 1 calc R . . H76B H 0.2815 -0.2793 0.0998 0.140 Uiso 1 1 calc R . . C69 C 0.4037(7) -0.3620(4) 0.0182(2) 0.133(2) Uani 1 1 d . . . H69A H 0.4364 -0.4109 -0.0062 0.199 Uiso 1 1 calc R . . H69B H 0.3669 -0.3023 0.0042 0.199 Uiso 1 1 calc R . . H69C H 0.3356 -0.3840 0.0403 0.199 Uiso 1 1 calc R . . O1W O 0.9029(4) -0.8152(3) 0.33555(16) 0.0904(11) Uani 1 1 d . . . H1A H 0.835(6) -0.834(4) 0.345(2) 0.13(3) Uiso 1 1 d . . . H1B H 0.861(6) -0.767(4) 0.321(2) 0.12(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co2 0.03120(19) 0.02833(19) 0.0266(2) -0.00426(14) -0.00301(14) -0.00396(14) C01 0.03227(19) 0.02815(19) 0.0278(2) -0.00413(15) -0.00206(15) -0.00409(14) O2 0.0735(15) 0.0317(12) 0.0557(15) 0.0003(10) -0.0023(12) -0.0118(10) O6 0.0585(14) 0.0656(15) 0.0334(12) -0.0179(11) -0.0061(10) 0.0051(11) O8 0.0612(14) 0.0346(12) 0.0628(16) 0.0036(11) -0.0200(12) 0.0005(10) O4 0.0731(15) 0.0621(15) 0.0317(12) -0.0119(11) -0.0034(11) -0.0197(12) C27 0.100(3) 0.071(3) 0.047(2) -0.025(2) 0.002(2) -0.026(2) N15 0.0326(11) 0.0281(11) 0.0255(12) 0.0038(9) -0.0036(9) -0.0047(9) N14 0.0400(13) 0.0323(12) 0.0341(14) -0.0007(10) -0.0022(10) -0.0089(10) N13 0.0410(13) 0.0305(12) 0.0320(13) -0.0005(10) -0.0053(10) -0.0067(10) N1 0.0428(13) 0.0324(12) 0.0306(13) -0.0013(10) -0.0060(10) -0.0025(10) N5 0.0332(12) 0.0375(13) 0.0277(12) -0.0072(10) 0.0002(9) -0.0066(10) N3 0.0412(13) 0.0390(13) 0.0349(14) -0.0070(11) 0.0038(10) -0.0123(10) N2 0.0412(13) 0.0278(12) 0.0368(14) -0.0038(10) -0.0061(10) -0.0021(10) N12 0.0393(13) 0.0365(13) 0.0292(13) -0.0051(10) -0.0083(10) -0.0046(10) O9 0.0554(14) 0.0585(15) 0.082(2) 0.0027(14) 0.0128(13) -0.0248(12) O7 0.0578(14) 0.0810(17) 0.0454(14) -0.0132(13) -0.0239(12) -0.0040(12) N21 0.0575(16) 0.0443(15) 0.0442(16) 0.0006(12) -0.0074(13) -0.0029(12) N16 0.0349(12) 0.0359(13) 0.0269(12) -0.0057(10) -0.0038(9) -0.0016(10) N6 0.0343(12) 0.0266(11) 0.0369(14) -0.0030(10) -0.0056(10) -0.0023(9) O1 0.0618(15) 0.0565(15) 0.081(2) -0.0016(13) -0.0335(14) 0.0118(12) O3 0.0601(15) 0.096(2) 0.0665(18) -0.0324(15) 0.0288(13) -0.0366(14) N11 0.0393(12) 0.0326(12) 0.0279(12) -0.0069(10) -0.0044(10) -0.0043(9) N10 0.0443(16) 0.0636(19) 0.063(2) -0.0065(16) 0.0017(14) -0.0028(13) C37 0.0368(14) 0.0315(14) 0.0271(14) -0.0008(11) -0.0004(11) -0.0038(11) C74 0.096(3) 0.073(3) 0.148(5) -0.028(3) -0.069(4) 0.024(3) C21 0.0440(16) 0.0272(14) 0.0374(16) -0.0010(12) -0.0132(13) -0.0005(11) N22 0.077(2) 0.0609(19) 0.0522(19) 0.0033(15) -0.0149(16) -0.0342(16) N8 0.082(2) 0.081(2) 0.0407(17) -0.0139(16) -0.0065(15) -0.0216(18) N4 0.0367(12) 0.0308(12) 0.0309(13) -0.0042(10) -0.0032(10) -0.0034(9) C65 0.066(2) 0.0407(17) 0.0344(18) 0.0051(13) -0.0069(15) -0.0070(15) N7 0.0492(17) 0.066(2) 0.071(2) -0.0016(17) -0.0093(16) 0.0098(14) C38 0.0345(14) 0.0361(15) 0.0364(16) 0.0018(12) -0.0063(12) -0.0081(11) N17 0.0578(19) 0.069(2) 0.084(2) -0.0183(19) -0.0204(17) -0.0217(16) C55 0.0364(15) 0.0482(18) 0.0373(17) -0.0118(14) -0.0016(12) -0.0080(13) N19 0.0519(17) 0.0597(19) 0.085(3) 0.0012(17) -0.0131(17) -0.0208(14) C64 0.0428(16) 0.0338(15) 0.0378(17) 0.0016(12) -0.0040(13) -0.0149(12) C34 0.0476(18) 0.0393(17) 0.048(2) -0.0027(14) -0.0020(15) -0.0012(13) C12 0.0513(17) 0.0329(15) 0.0283(15) -0.0060(12) 0.0054(12) -0.0105(13) C31 0.059(2) 0.0382(17) 0.048(2) 0.0039(14) -0.0008(16) -0.0061(14) C29 0.0490(17) 0.0292(14) 0.0296(16) -0.0016(11) -0.0077(12) -0.0011(12) C32 0.068(2) 0.058(2) 0.056(2) 0.0086(18) 0.0030(18) -0.0263(18) C4 0.0438(16) 0.0393(16) 0.0309(16) -0.0073(12) 0.0058(12) -0.0113(12) C61 0.046(2) 0.054(2) 0.095(3) 0.017(2) -0.003(2) -0.0112(16) C35 0.0355(17) 0.069(2) 0.060(2) -0.0101(19) -0.0033(16) 0.0116(15) C59 0.061(2) 0.0422(18) 0.046(2) 0.0000(15) -0.0044(16) -0.0110(15) C54 0.0408(16) 0.0386(16) 0.0353(17) -0.0106(13) -0.0113(13) 0.0031(12) C20 0.0364(15) 0.0373(16) 0.053(2) -0.0066(14) -0.0021(14) -0.0061(12) C36 0.0453(18) 0.059(2) 0.0418(19) -0.0114(16) 0.0045(15) 0.0039(15) C39 0.0387(17) 0.057(2) 0.056(2) -0.0014(17) -0.0132(15) -0.0045(14) C62 0.0520(19) 0.0497(19) 0.052(2) -0.0009(16) -0.0108(16) -0.0120(15) C53 0.0462(18) 0.0494(19) 0.060(2) -0.0117(17) -0.0149(16) 0.0084(15) C40 0.0439(16) 0.0353(15) 0.0312(16) -0.0054(12) -0.0050(12) -0.0068(12) C24 0.0490(17) 0.0384(16) 0.0316(16) -0.0058(13) 0.0086(13) -0.0136(13) C8 0.064(2) 0.0412(18) 0.046(2) 0.0037(15) -0.0111(16) -0.0144(15) C63 0.0428(16) 0.0476(18) 0.0394(18) -0.0060(14) 0.0007(13) -0.0141(14) C46 0.0442(16) 0.0387(16) 0.0374(17) -0.0017(13) -0.0113(13) -0.0060(13) C30 0.0440(16) 0.0388(16) 0.0247(15) -0.0034(12) -0.0033(12) -0.0054(12) N9 0.090(3) 0.055(2) 0.093(3) 0.0051(19) -0.035(2) -0.0259(18) C57 0.0467(17) 0.0344(16) 0.0341(16) -0.0046(12) -0.0135(13) -0.0035(12) C7 0.0460(17) 0.0344(16) 0.0381(17) 0.0037(13) -0.0055(13) 0.0008(12) C42 0.0498(18) 0.0461(18) 0.049(2) -0.0035(15) -0.0142(15) -0.0039(14) N20 0.112(3) 0.0516(19) 0.050(2) 0.0025(15) -0.0271(19) 0.0046(17) C18 0.0482(19) 0.050(2) 0.070(3) -0.0073(18) -0.0211(17) -0.0159(15) C60 0.062(2) 0.050(2) 0.061(2) 0.0080(17) 0.0108(18) -0.0063(17) C16 0.052(2) 0.052(2) 0.085(3) 0.010(2) -0.028(2) -0.0017(16) C47 0.0427(15) 0.0363(15) 0.0305(16) -0.0077(12) -0.0103(12) -0.0031(12) C41 0.0377(15) 0.0365(15) 0.0303(15) -0.0086(12) -0.0036(12) -0.0042(12) C58 0.0427(15) 0.0300(14) 0.0335(16) 0.0058(11) -0.0104(12) -0.0038(11) C17 0.0515(19) 0.0493(19) 0.049(2) -0.0049(16) -0.0069(15) 0.0052(15) C6 0.0474(18) 0.0447(18) 0.0369(18) -0.0098(14) -0.0097(14) 0.0057(14) C13 0.0433(16) 0.0263(14) 0.0392(17) 0.0022(12) -0.0050(13) -0.0032(11) C23 0.0430(17) 0.0455(18) 0.052(2) -0.0102(15) 0.0058(14) -0.0125(13) C3 0.0379(15) 0.0490(18) 0.0285(15) -0.0071(13) -0.0017(12) -0.0048(13) C75 0.223(7) 0.097(4) 0.110(5) -0.010(4) 0.052(5) -0.070(5) C1 0.049(2) 0.079(3) 0.066(3) -0.020(2) -0.0012(18) -0.0300(19) C66 0.071(2) 0.0366(17) 0.053(2) -0.0034(15) 0.0007(18) -0.0010(15) C14 0.059(2) 0.0380(17) 0.0422(19) 0.0013(14) -0.0094(15) -0.0029(14) C15 0.080(3) 0.047(2) 0.057(2) 0.0059(17) -0.028(2) -0.0100(18) C56 0.0344(16) 0.073(2) 0.060(2) -0.0202(19) 0.0050(15) -0.0073(16) C28 0.063(2) 0.057(2) 0.0344(18) -0.0123(15) 0.0007(15) -0.0130(16) C49 0.091(3) 0.050(2) 0.045(2) -0.0056(17) 0.0273(19) -0.0029(19) C5 0.057(2) 0.052(2) 0.051(2) -0.0069(16) -0.0018(16) -0.0260(16) C19 0.0370(16) 0.053(2) 0.068(2) -0.0073(18) 0.0024(15) -0.0124(14) C71 0.291(10) 0.086(4) 0.105(5) 0.030(4) -0.001(6) -0.072(5) C22 0.062(2) 0.0429(18) 0.047(2) -0.0049(15) -0.0215(16) -0.0131(15) C25 0.065(2) 0.050(2) 0.052(2) -0.0137(17) 0.0044(17) -0.0055(16) C52 0.0348(17) 0.072(3) 0.075(3) -0.022(2) -0.0047(17) 0.0074(16) C45 0.0512(19) 0.0450(19) 0.061(2) -0.0061(16) -0.0127(16) -0.0114(14) C68 0.089(3) 0.0430(19) 0.0368(19) -0.0032(15) -0.0090(18) -0.0042(17) C48 0.106(3) 0.0409(19) 0.050(2) -0.0009(17) 0.018(2) -0.0018(19) C2 0.0385(17) 0.073(2) 0.057(2) -0.0137(19) -0.0104(15) -0.0074(16) C50 0.080(3) 0.091(3) 0.041(2) -0.012(2) 0.0120(19) 0.000(2) C67 0.075(2) 0.0408(19) 0.058(2) 0.0035(16) -0.0142(19) 0.0010(16) C33 0.0456(19) 0.080(3) 0.057(2) -0.005(2) 0.0061(16) -0.0214(18) C10 0.081(3) 0.058(3) 0.131(5) 0.019(3) -0.018(3) -0.032(2) C80 0.079(3) 0.087(3) 0.062(3) 0.005(2) -0.028(2) -0.034(2) C83 0.077(4) 0.151(6) 0.203(8) 0.056(5) -0.011(4) -0.023(4) C43 0.061(2) 0.064(2) 0.063(3) -0.0033(19) -0.0245(19) 0.0086(18) C44 0.050(2) 0.081(3) 0.078(3) -0.021(2) -0.026(2) -0.003(2) N18 0.173(5) 0.079(3) 0.107(4) -0.045(3) 0.005(3) 0.012(3) C78 0.110(4) 0.105(4) 0.063(3) 0.011(3) -0.046(3) -0.045(3) C26 0.094(3) 0.058(2) 0.063(3) -0.030(2) 0.017(2) -0.009(2) C51 0.136(4) 0.043(2) 0.067(3) -0.013(2) 0.027(3) -0.021(2) C82 0.107(4) 0.097(4) 0.095(4) 0.023(3) -0.036(3) -0.058(3) C72 0.094(3) 0.054(2) 0.087(3) -0.011(2) -0.030(3) 0.011(2) C108 0.151(5) 0.065(3) 0.061(3) -0.001(2) 0.035(3) -0.036(3) C70 0.091(3) 0.063(3) 0.065(3) -0.017(2) -0.002(2) 0.001(2) C77 0.122(4) 0.101(4) 0.064(3) 0.019(3) -0.020(3) -0.038(3) C73 0.129(4) 0.077(3) 0.127(5) -0.015(3) -0.077(4) -0.009(3) C81 0.117(4) 0.142(5) 0.103(5) 0.061(4) -0.035(4) -0.062(4) C79 0.087(3) 0.084(3) 0.134(5) 0.001(3) -0.024(3) -0.014(3) C11 0.159(5) 0.081(4) 0.110(5) 0.019(3) 0.048(4) -0.057(4) C84 0.088(3) 0.095(4) 0.104(4) -0.005(3) 0.008(3) -0.024(3) C76 0.177(6) 0.120(5) 0.063(3) -0.020(3) 0.025(3) -0.088(4) C69 0.193(7) 0.123(5) 0.084(4) -0.043(4) -0.060(4) 0.009(4) O1W 0.091(3) 0.095(3) 0.100(3) 0.008(2) -0.042(2) -0.035(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co2 N15 1.854(2) . ? Co2 N16 1.860(2) . ? Co2 N12 1.958(2) . ? Co2 N11 1.962(2) . ? Co2 N14 1.963(2) . ? Co2 N13 1.964(2) . ? C01 N6 1.858(2) . ? C01 N5 1.860(2) . ? C01 N1 1.954(2) . ? C01 N2 1.954(2) . ? C01 N4 1.956(2) . ? C01 N3 1.980(2) . ? O2 C12 1.237(3) . ? O6 C40 1.237(3) . ? O8 C57 1.234(3) . ? O4 C29 1.243(3) . ? C27 N8 1.331(5) . ? C27 C26 1.350(6) . ? C27 H27 0.9300 . ? N15 C38 1.334(3) . ? N15 C37 1.336(3) . ? N14 C63 1.345(4) . ? N14 C64 1.419(4) . ? N13 C57 1.349(4) . ? N13 C58 1.410(3) . ? N1 C6 1.339(4) . ? N1 C7 1.418(4) . ? N5 C4 1.328(4) . ? N5 C3 1.331(4) . ? N3 C23 1.347(4) . ? N3 C24 1.425(3) . ? N2 C12 1.350(3) . ? N2 C13 1.407(4) . ? N12 C46 1.336(4) . ? N12 C47 1.427(3) . ? O9 C63 1.235(4) . ? O7 C46 1.241(3) . ? N21 C72 1.489(5) . ? N21 C74 1.491(5) . ? N21 C70 1.503(4) . ? N21 C76 1.521(5) . ? N16 C55 1.333(4) . ? N16 C54 1.335(4) . ? N6 C21 1.335(3) . ? N6 C20 1.336(4) . ? O1 C6 1.231(4) . ? O3 C23 1.232(4) . ? N11 C40 1.346(3) . ? N11 C41 1.418(4) . ? N10 C33 1.330(5) . ? N10 C34 1.331(4) . ? C37 C36 1.373(4) . ? C37 C40 1.500(4) . ? C74 C73 1.530(6) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C21 C22 1.372(4) . ? C21 C29 1.495(4) . ? N22 C80 1.500(5) . ? N22 C82 1.506(5) . ? N22 C84 1.507(5) . ? N22 C78 1.525(5) . ? N8 C28 1.343(4) . ? N4 C29 1.333(3) . ? N4 C30 1.425(3) . ? C65 C66 1.378(4) . ? C65 C64 1.383(4) . ? C65 H65 0.9300 . ? N7 C16 1.325(5) . ? N7 C17 1.329(4) . ? C38 C39 1.389(4) . ? C38 C46 1.496(4) . ? N17 C45 1.322(4) . ? N17 C44 1.331(5) . ? C55 C56 1.388(4) . ? C55 C63 1.491(4) . ? N19 C61 1.327(5) . ? N19 C62 1.331(4) . ? C64 C68 1.389(4) . ? C34 C30 1.381(4) . ? C34 H34 0.9300 . ? C12 C4 1.493(4) . ? C31 C32 1.368(5) . ? C31 C30 1.383(4) . ? C31 H31 0.9300 . ? C32 C33 1.377(5) . ? C32 H32 0.9300 . ? C4 C5 1.388(4) . ? C61 C60 1.376(5) . ? C61 H61 0.9300 . ? C35 C39 1.378(5) . ? C35 C36 1.385(5) . ? C35 H35 0.9300 . ? C59 C60 1.370(5) . ? C59 C58 1.388(4) . ? C59 H59 0.9300 . ? C54 C53 1.374(4) . ? C54 C57 1.496(4) . ? C20 C19 1.375(4) . ? C20 C23 1.507(4) . ? C36 H36 0.9300 . ? C39 H39 0.9300 . ? C62 C58 1.395(4) . ? C62 H62 0.9300 . ? C53 C52 1.386(5) . ? C53 H53 0.9300 . ? C24 C28 1.372(5) . ? C24 C25 1.390(4) . ? C8 N9 1.347(4) . ? C8 C7 1.359(4) . ? C8 H8 0.9300 . ? N9 C10 1.320(6) . ? C7 C108 1.369(5) . ? C42 C41 1.368(4) . ? C42 C43 1.382(5) . ? C42 H42 0.9300 . ? N20 C68 1.331(5) . ? N20 C67 1.332(5) . ? C18 C22 1.374(5) . ? C18 C19 1.386(5) . ? C18 H18 0.9300 . ? C60 H60 0.9300 . ? C16 C15 1.375(5) . ? C16 H16 0.9300 . ? C47 C51 1.350(4) . ? C47 C48 1.364(5) . ? C41 C45 1.387(4) . ? C17 C13 1.391(4) . ? C17 H17 0.9300 . ? C6 C3 1.494(4) . ? C13 C14 1.379(4) . ? C3 C2 1.383(4) . ? C75 C76 1.379(8) . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C1 C5 1.365(5) . ? C1 C2 1.395(5) . ? C1 H1 0.9300 . ? C66 C67 1.356(5) . ? C66 H66 0.9300 . ? C14 C15 1.383(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C56 C52 1.382(5) . ? C56 H56 0.9300 . ? C28 H28 0.9300 . ? C49 C50 1.273(5) . ? C49 C48 1.310(5) . ? C49 H49 0.9300 . ? C5 H5 0.9300 . ? C19 H19 0.9300 . ? C71 C72 1.476(7) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C22 H22 0.9300 . ? C25 C26 1.378(5) . ? C25 H25 0.9300 . ? C52 H52 0.9300 . ? C45 H45 0.9300 . ? C68 H68 0.9300 . ? C48 H48 0.9300 . ? C2 H2 0.9300 . ? C50 N18 1.365(6) . ? C50 H50 0.9300 . ? C67 H67 0.9300 . ? C33 H33 0.9300 . ? C10 C11 1.355(7) . ? C10 H10 0.9300 . ? C80 C79 1.512(6) . ? C80 H80A 0.9700 . ? C80 H80B 0.9700 . ? C83 C84 1.532(7) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C43 C44 1.379(5) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? N18 C51 1.413(6) . ? C78 C77 1.498(6) . ? C78 H78A 0.9700 . ? C78 H78B 0.9700 . ? C26 H26 0.9300 . ? C51 H51 0.9300 . ? C82 C81 1.484(7) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C72 H72A 0.9700 . ? C72 H72B 0.9700 . ? C108 C11 1.367(6) . ? C108 H108 0.9300 . ? C70 C69 1.473(6) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C11 H11 0.9300 . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C76 H76A 0.9700 . ? C76 H76B 0.9700 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? O1W H1A 0.79(6) . ? O1W H1B 0.87(6) . ? 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 N15 Co2 N16 178.95(9) . . ? N15 Co2 N12 81.86(9) . . ? N16 Co2 N12 99.16(9) . . ? N15 Co2 N11 81.39(9) . . ? N16 Co2 N11 97.59(9) . . ? N12 Co2 N11 163.25(9) . . ? N15 Co2 N14 98.05(9) . . ? N16 Co2 N14 81.68(10) . . ? N12 Co2 N14 91.16(10) . . ? N11 Co2 N14 90.90(9) . . ? N15 Co2 N13 98.92(9) . . ? N16 Co2 N13 81.36(10) . . ? N12 Co2 N13 90.81(10) . . ? N11 Co2 N13 92.05(10) . . ? N14 Co2 N13 163.03(10) . . ? N6 C01 N5 177.15(10) . . ? N6 C01 N1 98.32(10) . . ? N5 C01 N1 81.43(10) . . ? N6 C01 N2 98.68(10) . . ? N5 C01 N2 81.59(10) . . ? N1 C01 N2 163.01(9) . . ? N6 C01 N4 81.20(9) . . ? N5 C01 N4 95.95(9) . . ? N1 C01 N4 90.26(10) . . ? N2 C01 N4 92.28(10) . . ? N6 C01 N3 81.31(10) . . ? N5 C01 N3 101.53(9) . . ? N1 C01 N3 92.19(10) . . ? N2 C01 N3 90.42(10) . . ? N4 C01 N3 162.51(9) . . ? N8 C27 C26 123.2(3) . . ? N8 C27 H27 118.4 . . ? C26 C27 H27 118.4 . . ? C38 N15 C37 122.2(2) . . ? C38 N15 Co2 118.23(18) . . ? C37 N15 Co2 119.48(18) . . ? C63 N14 C64 120.1(2) . . ? C63 N14 Co2 115.8(2) . . ? C64 N14 Co2 124.07(18) . . ? C57 N13 C58 118.6(2) . . ? C57 N13 Co2 116.03(19) . . ? C58 N13 Co2 125.32(18) . . ? C6 N1 C7 120.3(2) . . ? C6 N1 C01 116.3(2) . . ? C7 N1 C01 123.38(18) . . ? C4 N5 C3 123.3(2) . . ? C4 N5 C01 118.4(2) . . ? C3 N5 C01 118.19(19) . . ? C23 N3 C24 117.4(2) . . ? C23 N3 C01 115.8(2) . . ? C24 N3 C01 126.71(17) . . ? C12 N2 C13 118.0(2) . . ? C12 N2 C01 116.1(2) . . ? C13 N2 C01 125.72(18) . . ? C46 N12 C47 118.6(2) . . ? C46 N12 Co2 115.72(18) . . ? C47 N12 Co2 125.69(18) . . ? C72 N21 C74 111.9(3) . . ? C72 N21 C70 113.3(3) . . ? C74 N21 C70 107.1(3) . . ? C72 N21 C76 101.5(4) . . ? C74 N21 C76 111.9(4) . . ? C70 N21 C76 111.2(3) . . ? C55 N16 C54 123.0(2) . . ? C55 N16 Co2 118.1(2) . . ? C54 N16 Co2 118.83(19) . . ? C21 N6 C20 121.7(2) . . ? C21 N6 C01 118.89(19) . . ? C20 N6 C01 119.24(19) . . ? C40 N11 C41 118.4(2) . . ? C40 N11 Co2 115.81(18) . . ? C41 N11 Co2 125.22(17) . . ? C33 N10 C34 116.6(3) . . ? N15 C37 C36 120.7(3) . . ? N15 C37 C40 112.1(2) . . ? C36 C37 C40 127.2(3) . . ? N21 C74 C73 116.6(4) . . ? N21 C74 H74A 108.1 . . ? C73 C74 H74A 108.1 . . ? N21 C74 H74B 108.1 . . ? C73 C74 H74B 108.1 . . ? H74A C74 H74B 107.3 . . ? N6 C21 C22 120.4(3) . . ? N6 C21 C29 112.3(2) . . ? C22 C21 C29 127.3(3) . . ? C80 N22 C82 111.9(3) . . ? C80 N22 C84 105.7(3) . . ? C82 N22 C84 112.2(4) . . ? C80 N22 C78 111.4(3) . . ? C82 N22 C78 105.0(3) . . ? C84 N22 C78 110.6(4) . . ? C27 N8 C28 116.4(3) . . ? C29 N4 C30 117.8(2) . . ? C29 N4 C01 116.31(19) . . ? C30 N4 C01 125.85(17) . . ? C66 C65 C64 120.1(3) . . ? C66 C65 H65 119.9 . . ? C64 C65 H65 119.9 . . ? C16 N7 C17 116.2(3) . . ? N15 C38 C39 119.5(3) . . ? N15 C38 C46 113.0(2) . . ? C39 C38 C46 127.5(3) . . ? C45 N17 C44 117.3(3) . . ? N16 C55 C56 118.9(3) . . ? N16 C55 C63 113.6(2) . . ? C56 C55 C63 127.5(3) . . ? C61 N19 C62 116.6(3) . . ? C65 C64 C68 116.2(3) . . ? C65 C64 N14 122.1(3) . . ? C68 C64 N14 121.7(3) . . ? N10 C34 C30 124.0(3) . . ? N10 C34 H34 118.0 . . ? C30 C34 H34 118.0 . . ? O2 C12 N2 127.9(3) . . ? O2 C12 C4 121.8(3) . . ? N2 C12 C4 110.3(2) . . ? C32 C31 C30 119.2(3) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? O4 C29 N4 128.1(3) . . ? O4 C29 C21 120.8(3) . . ? N4 C29 C21 111.0(2) . . ? C31 C32 C33 118.4(3) . . ? C31 C32 H32 120.8 . . ? C33 C32 H32 120.8 . . ? N5 C4 C5 119.6(3) . . ? N5 C4 C12 113.5(2) . . ? C5 C4 C12 126.9(3) . . ? N19 C61 C60 124.3(3) . . ? N19 C61 H61 117.8 . . ? C60 C61 H61 117.8 . . ? C39 C35 C36 120.3(3) . . ? C39 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C60 C59 C58 119.5(3) . . ? C60 C59 H59 120.2 . . ? C58 C59 H59 120.2 . . ? N16 C54 C53 120.3(3) . . ? N16 C54 C57 112.9(2) . . ? C53 C54 C57 126.7(3) . . ? N6 C20 C19 120.3(3) . . ? N6 C20 C23 112.6(2) . . ? C19 C20 C23 127.1(3) . . ? C37 C36 C35 118.3(3) . . ? C37 C36 H36 120.8 . . ? C35 C36 H36 120.8 . . ? C35 C39 C38 118.9(3) . . ? C35 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? N19 C62 C58 124.0(3) . . ? N19 C62 H62 118.0 . . ? C58 C62 H62 118.0 . . ? C54 C53 C52 118.3(3) . . ? C54 C53 H53 120.9 . . ? C52 C53 H53 120.9 . . ? O6 C40 N11 127.8(3) . . ? O6 C40 C37 121.0(3) . . ? N11 C40 C37 111.2(2) . . ? C28 C24 C25 117.0(3) . . ? C28 C24 N3 120.2(3) . . ? C25 C24 N3 122.8(3) . . ? N9 C8 C7 125.2(3) . . ? N9 C8 H8 117.4 . . ? C7 C8 H8 117.4 . . ? O9 C63 N14 128.3(3) . . ? O9 C63 C55 120.9(3) . . ? N14 C63 C55 110.7(3) . . ? O7 C46 N12 128.2(3) . . ? O7 C46 C38 120.8(3) . . ? N12 C46 C38 111.0(2) . . ? C34 C30 C31 117.8(3) . . ? C34 C30 N4 120.6(3) . . ? C31 C30 N4 121.5(3) . . ? C10 N9 C8 115.5(4) . . ? O8 C57 N13 127.8(3) . . ? O8 C57 C54 121.6(3) . . ? N13 C57 C54 110.6(2) . . ? C8 C7 C108 116.6(3) . . ? C8 C7 N1 121.8(3) . . ? C108 C7 N1 121.4(3) . . ? C41 C42 C43 119.3(3) . . ? C41 C42 H42 120.4 . . ? C43 C42 H42 120.4 . . ? C68 N20 C67 116.9(3) . . ? C22 C18 C19 120.0(3) . . ? C22 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C59 C60 C61 118.3(4) . . ? C59 C60 H60 120.9 . . ? C61 C60 H60 120.9 . . ? N7 C16 C15 124.3(3) . . ? N7 C16 H16 117.9 . . ? C15 C16 H16 117.9 . . ? C51 C47 C48 116.2(3) . . ? C51 C47 N12 123.2(3) . . ? C48 C47 N12 120.6(3) . . ? C42 C41 C45 117.8(3) . . ? C42 C41 N11 122.0(3) . . ? C45 C41 N11 120.2(3) . . ? C59 C58 C62 117.2(3) . . ? C59 C58 N13 121.3(2) . . ? C62 C58 N13 121.5(3) . . ? N7 C17 C13 124.8(3) . . ? N7 C17 H17 117.6 . . ? C13 C17 H17 117.6 . . ? O1 C6 N1 128.5(3) . . ? O1 C6 C3 121.1(3) . . ? N1 C6 C3 110.4(3) . . ? C14 C13 C17 117.2(3) . . ? C14 C13 N2 122.0(3) . . ? C17 C13 N2 120.8(3) . . ? O3 C23 N3 129.1(3) . . ? O3 C23 C20 120.1(3) . . ? N3 C23 C20 110.8(3) . . ? N5 C3 C2 119.1(3) . . ? N5 C3 C6 113.3(2) . . ? C2 C3 C6 127.6(3) . . ? C76 C75 H75A 109.5 . . ? C76 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C76 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C5 C1 C2 119.9(3) . . ? C5 C1 H1 120.1 . . ? C2 C1 H1 120.1 . . ? C67 C66 C65 118.5(3) . . ? C67 C66 H66 120.7 . . ? C65 C66 H66 120.7 . . ? C13 C14 C15 119.1(3) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 118.5(3) . . ? C16 C15 H15 120.8 . . ? C14 C15 H15 120.8 . . ? C52 C56 C55 119.2(3) . . ? C52 C56 H56 120.4 . . ? C55 C56 H56 120.4 . . ? N8 C28 C24 124.8(3) . . ? N8 C28 H28 117.6 . . ? C24 C28 H28 117.6 . . ? C50 C49 C48 118.3(4) . . ? C50 C49 H49 120.8 . . ? C48 C49 H49 120.8 . . ? C1 C5 C4 119.1(3) . . ? C1 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C20 C19 C18 118.6(3) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C72 C71 H71A 109.5 . . ? C72 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C72 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C21 C22 C18 119.0(3) . . ? C21 C22 H22 120.5 . . ? C18 C22 H22 120.5 . . ? C26 C25 C24 118.4(4) . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 120.8 . . ? C56 C52 C53 120.2(3) . . ? C56 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? N17 C45 C41 124.0(3) . . ? N17 C45 H45 118.0 . . ? C41 C45 H45 118.0 . . ? N20 C68 C64 124.5(3) . . ? N20 C68 H68 117.7 . . ? C64 C68 H68 117.7 . . ? C49 C48 C47 125.4(3) . . ? C49 C48 H48 117.3 . . ? C47 C48 H48 117.3 . . ? C3 C2 C1 119.0(3) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C49 C50 N18 123.3(4) . . ? C49 C50 H50 118.4 . . ? N18 C50 H50 118.4 . . ? N20 C67 C66 123.8(3) . . ? N20 C67 H67 118.1 . . ? C66 C67 H67 118.1 . . ? N10 C33 C32 123.9(3) . . ? N10 C33 H33 118.0 . . ? C32 C33 H33 118.0 . . ? N9 C10 C11 124.1(4) . . ? N9 C10 H10 117.9 . . ? C11 C10 H10 117.9 . . ? N22 C80 C79 115.6(3) . . ? N22 C80 H80A 108.4 . . ? C79 C80 H80A 108.4 . . ? N22 C80 H80B 108.4 . . ? C79 C80 H80B 108.4 . . ? H80A C80 H80B 107.4 . . ? C84 C83 H83A 109.5 . . ? C84 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C84 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C44 C43 C42 118.5(4) . . ? C44 C43 H43 120.7 . . ? C42 C43 H43 120.7 . . ? N17 C44 C43 123.0(3) . . ? N17 C44 H44 118.5 . . ? C43 C44 H44 118.5 . . ? C50 N18 C51 117.4(4) . . ? C77 C78 N22 114.8(3) . . ? C77 C78 H78A 108.6 . . ? N22 C78 H78A 108.6 . . ? C77 C78 H78B 108.6 . . ? N22 C78 H78B 108.6 . . ? H78A C78 H78B 107.6 . . ? C27 C26 C25 120.2(3) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C47 C51 N18 119.4(4) . . ? C47 C51 H51 120.3 . . ? N18 C51 H51 120.3 . . ? C81 C82 N22 115.2(4) . . ? C81 C82 H82A 108.5 . . ? N22 C82 H82A 108.5 . . ? C81 C82 H82B 108.5 . . ? N22 C82 H82B 108.5 . . ? H82A C82 H82B 107.5 . . ? C71 C72 N21 115.3(4) . . ? C71 C72 H72A 108.5 . . ? N21 C72 H72A 108.5 . . ? C71 C72 H72B 108.5 . . ? N21 C72 H72B 108.5 . . ? H72A C72 H72B 107.5 . . ? C11 C108 C7 120.0(4) . . ? C11 C108 H108 120.0 . . ? C7 C108 H108 120.0 . . ? C69 C70 N21 115.2(4) . . ? C69 C70 H70A 108.5 . . ? N21 C70 H70A 108.5 . . ? C69 C70 H70B 108.5 . . ? N21 C70 H70B 108.5 . . ? H70A C70 H70B 107.5 . . ? C78 C77 H77A 109.5 . . ? C78 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C78 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C74 C73 H73A 109.5 . . ? C74 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C74 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C82 C81 H81A 109.5 . . ? C82 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C82 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C80 C79 H79A 109.5 . . ? C80 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C80 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C10 C11 C108 118.5(5) . . ? C10 C11 H11 120.7 . . ? C108 C11 H11 120.7 . . ? N22 C84 C83 116.0(5) . . ? N22 C84 H84A 108.3 . . ? C83 C84 H84A 108.3 . . ? N22 C84 H84B 108.3 . . ? C83 C84 H84B 108.3 . . ? H84A C84 H84B 107.4 . . ? C75 C76 N21 121.8(6) . . ? C75 C76 H76A 106.9 . . ? N21 C76 H76A 106.9 . . ? C75 C76 H76B 106.9 . . ? N21 C76 H76B 106.9 . . ? H76A C76 H76B 106.7 . . ? C70 C69 H69A 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C70 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? H1A O1W H1B 91(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 N12 Co2 N15 C38 1.1(2) . . . . ? N11 Co2 N15 C38 -178.6(2) . . . . ? N14 Co2 N15 C38 -88.9(2) . . . . ? N13 Co2 N15 C38 90.6(2) . . . . ? N12 Co2 N15 C37 178.8(2) . . . . ? N11 Co2 N15 C37 -1.0(2) . . . . ? N14 Co2 N15 C37 88.7(2) . . . . ? N13 Co2 N15 C37 -91.7(2) . . . . ? N15 Co2 N14 C63 -179.3(2) . . . . ? N16 Co2 N14 C63 -0.3(2) . . . . ? N12 Co2 N14 C63 98.8(2) . . . . ? N11 Co2 N14 C63 -97.8(2) . . . . ? N13 Co2 N14 C63 2.2(4) . . . . ? N15 Co2 N14 C64 3.7(2) . . . . ? N16 Co2 N14 C64 -177.4(2) . . . . ? N12 Co2 N14 C64 -78.3(2) . . . . ? N11 Co2 N14 C64 85.1(2) . . . . ? N13 Co2 N14 C64 -174.8(3) . . . . ? N15 Co2 N13 C57 -179.5(2) . . . . ? N16 Co2 N13 C57 1.6(2) . . . . ? N12 Co2 N13 C57 -97.6(2) . . . . ? N11 Co2 N13 C57 98.9(2) . . . . ? N14 Co2 N13 C57 -0.9(4) . . . . ? N15 Co2 N13 C58 -3.1(2) . . . . ? N16 Co2 N13 C58 178.0(2) . . . . ? N12 Co2 N13 C58 78.8(2) . . . . ? N11 Co2 N13 C58 -84.7(2) . . . . ? N14 Co2 N13 C58 175.5(3) . . . . ? N6 C01 N1 C6 -171.5(2) . . . . ? N5 C01 N1 C6 5.6(2) . . . . ? N2 C01 N1 C6 8.3(5) . . . . ? N4 C01 N1 C6 -90.4(2) . . . . ? N3 C01 N1 C6 106.9(2) . . . . ? N6 C01 N1 C7 8.1(2) . . . . ? N5 C01 N1 C7 -174.8(2) . . . . ? N2 C01 N1 C7 -172.1(3) . . . . ? N4 C01 N1 C7 89.2(2) . . . . ? N3 C01 N1 C7 -73.5(2) . . . . ? N1 C01 N5 C4 179.4(2) . . . . ? N2 C01 N5 C4 0.2(2) . . . . ? N4 C01 N5 C4 -91.2(2) . . . . ? N3 C01 N5 C4 88.9(2) . . . . ? N1 C01 N5 C3 -4.7(2) . . . . ? N2 C01 N5 C3 176.1(2) . . . . ? N4 C01 N5 C3 84.7(2) . . . . ? N3 C01 N5 C3 -95.2(2) . . . . ? N6 C01 N3 C23 0.1(2) . . . . ? N5 C01 N3 C23 179.9(2) . . . . ? N1 C01 N3 C23 98.2(2) . . . . ? N2 C01 N3 C23 -98.6(2) . . . . ? N4 C01 N3 C23 0.4(5) . . . . ? N6 C01 N3 C24 176.1(3) . . . . ? N5 C01 N3 C24 -4.1(3) . . . . ? N1 C01 N3 C24 -85.8(3) . . . . ? N2 C01 N3 C24 77.4(3) . . . . ? N4 C01 N3 C24 176.3(3) . . . . ? N6 C01 N2 C12 179.3(2) . . . . ? N5 C01 N2 C12 2.2(2) . . . . ? N1 C01 N2 C12 -0.5(5) . . . . ? N4 C01 N2 C12 97.9(2) . . . . ? N3 C01 N2 C12 -99.4(2) . . . . ? N6 C01 N2 C13 -6.1(2) . . . . ? N5 C01 N2 C13 176.8(2) . . . . ? N1 C01 N2 C13 174.1(3) . . . . ? N4 C01 N2 C13 -87.5(2) . . . . ? N3 C01 N2 C13 75.2(2) . . . . ? N15 Co2 N12 C46 1.6(2) . . . . ? N16 Co2 N12 C46 -178.7(2) . . . . ? N11 Co2 N12 C46 2.5(5) . . . . ? N14 Co2 N12 C46 99.6(2) . . . . ? N13 Co2 N12 C46 -97.3(2) . . . . ? N15 Co2 N12 C47 -178.1(2) . . . . ? N16 Co2 N12 C47 1.6(2) . . . . ? N11 Co2 N12 C47 -177.2(3) . . . . ? N14 Co2 N12 C47 -80.1(2) . . . . ? N13 Co2 N12 C47 83.0(2) . . . . ? N12 Co2 N16 C55 -91.9(2) . . . . ? N11 Co2 N16 C55 87.7(2) . . . . ? N14 Co2 N16 C55 -2.1(2) . . . . ? N13 Co2 N16 C55 178.6(2) . . . . ? N12 Co2 N16 C54 91.0(2) . . . . ? N11 Co2 N16 C54 -89.4(2) . . . . ? N14 Co2 N16 C54 -179.2(2) . . . . ? N13 Co2 N16 C54 1.5(2) . . . . ? N1 C01 N6 C21 87.8(2) . . . . ? N2 C01 N6 C21 -92.2(2) . . . . ? N4 C01 N6 C21 -1.2(2) . . . . ? N3 C01 N6 C21 178.7(2) . . . . ? N1 C01 N6 C20 -87.6(2) . . . . ? N2 C01 N6 C20 92.4(2) . . . . ? N4 C01 N6 C20 -176.6(2) . . . . ? N3 C01 N6 C20 3.3(2) . . . . ? N15 Co2 N11 C40 1.9(2) . . . . ? N16 Co2 N11 C40 -177.8(2) . . . . ? N12 Co2 N11 C40 1.0(5) . . . . ? N14 Co2 N11 C40 -96.1(2) . . . . ? N13 Co2 N11 C40 100.6(2) . . . . ? N15 Co2 N11 C41 173.0(2) . . . . ? N16 Co2 N11 C41 -6.7(2) . . . . ? N12 Co2 N11 C41 172.1(3) . . . . ? N14 Co2 N11 C41 75.0(2) . . . . ? N13 Co2 N11 C41 -88.3(2) . . . . ? C38 N15 C37 C36 0.2(4) . . . . ? Co2 N15 C37 C36 -177.4(2) . . . . ? C38 N15 C37 C40 177.5(2) . . . . ? Co2 N15 C37 C40 0.0(3) . . . . ? C72 N21 C74 C73 55.5(6) . . . . ? C70 N21 C74 C73 -179.8(5) . . . . ? C76 N21 C74 C73 -57.7(6) . . . . ? C20 N6 C21 C22 0.5(4) . . . . ? C01 N6 C21 C22 -174.8(2) . . . . ? C20 N6 C21 C29 179.6(3) . . . . ? C01 N6 C21 C29 4.3(3) . . . . ? C26 C27 N8 C28 1.0(6) . . . . ? N6 C01 N4 C29 -2.6(2) . . . . ? N5 C01 N4 C29 177.6(2) . . . . ? N1 C01 N4 C29 -101.0(2) . . . . ? N2 C01 N4 C29 95.8(2) . . . . ? N3 C01 N4 C29 -2.9(5) . . . . ? N6 C01 N4 C30 177.3(2) . . . . ? N5 C01 N4 C30 -2.5(2) . . . . ? N1 C01 N4 C30 78.9(2) . . . . ? N2 C01 N4 C30 -84.3(2) . . . . ? N3 C01 N4 C30 177.0(3) . . . . ? C37 N15 C38 C39 -1.9(4) . . . . ? Co2 N15 C38 C39 175.7(2) . . . . ? C37 N15 C38 C46 179.2(2) . . . . ? Co2 N15 C38 C46 -3.2(3) . . . . ? C54 N16 C55 C56 2.0(4) . . . . ? Co2 N16 C55 C56 -175.0(2) . . . . ? C54 N16 C55 C63 -179.1(2) . . . . ? Co2 N16 C55 C63 3.9(3) . . . . ? C66 C65 C64 C68 -1.8(5) . . . . ? C66 C65 C64 N14 175.2(3) . . . . ? C63 N14 C64 C65 113.0(3) . . . . ? Co2 N14 C64 C65 -70.1(3) . . . . ? C63 N14 C64 C68 -70.2(4) . . . . ? Co2 N14 C64 C68 106.7(3) . . . . ? C33 N10 C34 C30 -0.3(5) . . . . ? C13 N2 C12 O2 2.4(4) . . . . ? C01 N2 C12 O2 177.4(2) . . . . ? C13 N2 C12 C4 -178.8(2) . . . . ? C01 N2 C12 C4 -3.8(3) . . . . ? C30 N4 C29 O4 6.2(4) . . . . ? C01 N4 C29 O4 -173.9(3) . . . . ? C30 N4 C29 C21 -174.6(2) . . . . ? C01 N4 C29 C21 5.3(3) . . . . ? N6 C21 C29 O4 173.3(3) . . . . ? C22 C21 C29 O4 -7.8(5) . . . . ? N6 C21 C29 N4 -6.0(3) . . . . ? C22 C21 C29 N4 172.9(3) . . . . ? C30 C31 C32 C33 -0.2(5) . . . . ? C3 N5 C4 C5 0.9(4) . . . . ? C01 N5 C4 C5 176.6(2) . . . . ? C3 N5 C4 C12 -178.0(2) . . . . ? C01 N5 C4 C12 -2.3(3) . . . . ? O2 C12 C4 N5 -177.2(3) . . . . ? N2 C12 C4 N5 3.9(3) . . . . ? O2 C12 C4 C5 4.0(5) . . . . ? N2 C12 C4 C5 -175.0(3) . . . . ? C62 N19 C61 C60 2.7(6) . . . . ? C55 N16 C54 C53 -3.0(4) . . . . ? Co2 N16 C54 C53 173.9(2) . . . . ? C55 N16 C54 C57 179.1(2) . . . . ? Co2 N16 C54 C57 -4.0(3) . . . . ? C21 N6 C20 C19 -0.8(5) . . . . ? C01 N6 C20 C19 174.5(2) . . . . ? C21 N6 C20 C23 179.0(3) . . . . ? C01 N6 C20 C23 -5.7(3) . . . . ? N15 C37 C36 C35 1.9(5) . . . . ? C40 C37 C36 C35 -175.0(3) . . . . ? C39 C35 C36 C37 -2.3(5) . . . . ? C36 C35 C39 C38 0.6(5) . . . . ? N15 C38 C39 C35 1.4(5) . . . . ? C46 C38 C39 C35 -179.8(3) . . . . ? C61 N19 C62 C58 -0.6(5) . . . . ? N16 C54 C53 C52 2.0(5) . . . . ? C57 C54 C53 C52 179.5(3) . . . . ? C41 N11 C40 O6 4.5(5) . . . . ? Co2 N11 C40 O6 176.3(3) . . . . ? C41 N11 C40 C37 -174.1(2) . . . . ? Co2 N11 C40 C37 -2.3(3) . . . . ? N15 C37 C40 O6 -177.2(3) . . . . ? C36 C37 C40 O6 0.0(5) . . . . ? N15 C37 C40 N11 1.5(3) . . . . ? C36 C37 C40 N11 178.7(3) . . . . ? C23 N3 C24 C28 -127.2(3) . . . . ? C01 N3 C24 C28 56.8(4) . . . . ? C23 N3 C24 C25 52.8(4) . . . . ? C01 N3 C24 C25 -123.2(3) . . . . ? C64 N14 C63 O9 -1.5(5) . . . . ? Co2 N14 C63 O9 -178.6(3) . . . . ? C64 N14 C63 C55 179.5(2) . . . . ? Co2 N14 C63 C55 2.3(3) . . . . ? N16 C55 C63 O9 176.9(3) . . . . ? C56 C55 C63 O9 -4.3(5) . . . . ? N16 C55 C63 N14 -3.9(4) . . . . ? C56 C55 C63 N14 174.8(3) . . . . ? C47 N12 C46 O7 -5.1(5) . . . . ? Co2 N12 C46 O7 175.2(3) . . . . ? C47 N12 C46 C38 176.2(2) . . . . ? Co2 N12 C46 C38 -3.5(3) . . . . ? N15 C38 C46 O7 -174.6(3) . . . . ? C39 C38 C46 O7 6.6(5) . . . . ? N15 C38 C46 N12 4.3(4) . . . . ? C39 C38 C46 N12 -174.6(3) . . . . ? N10 C34 C30 C31 -0.2(5) . . . . ? N10 C34 C30 N4 178.5(3) . . . . ? C32 C31 C30 C34 0.4(5) . . . . ? C32 C31 C30 N4 -178.3(3) . . . . ? C29 N4 C30 C34 79.2(4) . . . . ? C01 N4 C30 C34 -100.7(3) . . . . ? C29 N4 C30 C31 -102.1(3) . . . . ? C01 N4 C30 C31 78.0(3) . . . . ? C7 C8 N9 C10 0.6(6) . . . . ? C58 N13 C57 O8 0.3(4) . . . . ? Co2 N13 C57 O8 177.0(2) . . . . ? C58 N13 C57 C54 179.5(2) . . . . ? Co2 N13 C57 C54 -3.9(3) . . . . ? N16 C54 C57 O8 -175.9(3) . . . . ? C53 C54 C57 O8 6.4(5) . . . . ? N16 C54 C57 N13 4.9(3) . . . . ? C53 C54 C57 N13 -172.8(3) . . . . ? N9 C8 C7 C108 -1.1(6) . . . . ? N9 C8 C7 N1 174.3(3) . . . . ? C6 N1 C7 C8 93.4(4) . . . . ? C01 N1 C7 C8 -86.2(3) . . . . ? C6 N1 C7 C108 -91.5(4) . . . . ? C01 N1 C7 C108 88.9(4) . . . . ? C58 C59 C60 C61 -1.0(5) . . . . ? N19 C61 C60 C59 -2.0(6) . . . . ? C17 N7 C16 C15 1.1(6) . . . . ? C46 N12 C47 C51 94.7(4) . . . . ? Co2 N12 C47 C51 -85.6(4) . . . . ? C46 N12 C47 C48 -88.2(4) . . . . ? Co2 N12 C47 C48 91.5(4) . . . . ? C43 C42 C41 C45 -0.2(5) . . . . ? C43 C42 C41 N11 -178.8(3) . . . . ? C40 N11 C41 C42 -108.9(3) . . . . ? Co2 N11 C41 C42 80.2(3) . . . . ? C40 N11 C41 C45 72.4(4) . . . . ? Co2 N11 C41 C45 -98.4(3) . . . . ? C60 C59 C58 C62 2.8(5) . . . . ? C60 C59 C58 N13 -177.8(3) . . . . ? N19 C62 C58 C59 -2.1(5) . . . . ? N19 C62 C58 N13 178.5(3) . . . . ? C57 N13 C58 C59 -112.5(3) . . . . ? Co2 N13 C58 C59 71.1(3) . . . . ? C57 N13 C58 C62 66.8(4) . . . . ? Co2 N13 C58 C62 -109.6(3) . . . . ? C16 N7 C17 C13 0.1(5) . . . . ? C7 N1 C6 O1 -3.0(5) . . . . ? C01 N1 C6 O1 176.6(3) . . . . ? C7 N1 C6 C3 175.2(2) . . . . ? C01 N1 C6 C3 -5.2(3) . . . . ? N7 C17 C13 C14 -0.8(5) . . . . ? N7 C17 C13 N2 177.3(3) . . . . ? C12 N2 C13 C14 -111.3(3) . . . . ? C01 N2 C13 C14 74.2(3) . . . . ? C12 N2 C13 C17 70.7(4) . . . . ? C01 N2 C13 C17 -103.8(3) . . . . ? C24 N3 C23 O3 -0.5(6) . . . . ? C01 N3 C23 O3 175.9(3) . . . . ? C24 N3 C23 C20 -179.3(3) . . . . ? C01 N3 C23 C20 -2.9(3) . . . . ? N6 C20 C23 O3 -173.6(3) . . . . ? C19 C20 C23 O3 6.3(6) . . . . ? N6 C20 C23 N3 5.3(4) . . . . ? C19 C20 C23 N3 -174.8(3) . . . . ? C4 N5 C3 C2 -1.9(4) . . . . ? C01 N5 C3 C2 -177.6(2) . . . . ? C4 N5 C3 C6 178.8(2) . . . . ? C01 N5 C3 C6 3.1(3) . . . . ? O1 C6 C3 N5 179.8(3) . . . . ? N1 C6 C3 N5 1.5(4) . . . . ? O1 C6 C3 C2 0.6(5) . . . . ? N1 C6 C3 C2 -177.7(3) . . . . ? C64 C65 C66 C67 1.8(5) . . . . ? C17 C13 C14 C15 0.5(5) . . . . ? N2 C13 C14 C15 -177.6(3) . . . . ? N7 C16 C15 C14 -1.4(6) . . . . ? C13 C14 C15 C16 0.5(5) . . . . ? N16 C55 C56 C52 0.0(5) . . . . ? C63 C55 C56 C52 -178.6(3) . . . . ? C27 N8 C28 C24 -1.0(5) . . . . ? C25 C24 C28 N8 -0.1(5) . . . . ? N3 C24 C28 N8 179.9(3) . . . . ? C2 C1 C5 C4 0.0(5) . . . . ? N5 C4 C5 C1 0.0(5) . . . . ? C12 C4 C5 C1 178.8(3) . . . . ? N6 C20 C19 C18 0.7(5) . . . . ? C23 C20 C19 C18 -179.2(3) . . . . ? C22 C18 C19 C20 -0.2(5) . . . . ? N6 C21 C22 C18 0.0(5) . . . . ? C29 C21 C22 C18 -178.9(3) . . . . ? C19 C18 C22 C21 -0.1(5) . . . . ? C28 C24 C25 C26 1.2(5) . . . . ? N3 C24 C25 C26 -178.8(3) . . . . ? C55 C56 C52 C53 -1.0(5) . . . . ? C54 C53 C52 C56 0.0(5) . . . . ? C44 N17 C45 C41 0.9(5) . . . . ? C42 C41 C45 N17 -0.5(5) . . . . ? N11 C41 C45 N17 178.2(3) . . . . ? C67 N20 C68 C64 0.9(6) . . . . ? C65 C64 C68 N20 0.4(5) . . . . ? N14 C64 C68 N20 -176.6(3) . . . . ? C50 C49 C48 C47 -1.9(7) . . . . ? C51 C47 C48 C49 -0.3(7) . . . . ? N12 C47 C48 C49 -177.6(4) . . . . ? N5 C3 C2 C1 1.9(5) . . . . ? C6 C3 C2 C1 -178.9(3) . . . . ? C5 C1 C2 C3 -1.0(5) . . . . ? C48 C49 C50 N18 2.2(8) . . . . ? C68 N20 C67 C66 -0.9(6) . . . . ? C65 C66 C67 N20 -0.4(6) . . . . ? C34 N10 C33 C32 0.5(6) . . . . ? C31 C32 C33 N10 -0.3(6) . . . . ? C8 N9 C10 C11 0.0(7) . . . . ? C82 N22 C80 C79 55.9(5) . . . . ? C84 N22 C80 C79 178.5(4) . . . . ? C78 N22 C80 C79 -61.3(5) . . . . ? C41 C42 C43 C44 0.4(5) . . . . ? C45 N17 C44 C43 -0.6(6) . . . . ? C42 C43 C44 N17 0.0(6) . . . . ? C49 C50 N18 C51 -0.4(8) . . . . ? C80 N22 C78 C77 -57.0(5) . . . . ? C82 N22 C78 C77 -178.4(4) . . . . ? C84 N22 C78 C77 60.3(5) . . . . ? N8 C27 C26 C25 0.1(7) . . . . ? C24 C25 C26 C27 -1.2(6) . . . . ? C48 C47 C51 N18 2.2(6) . . . . ? N12 C47 C51 N18 179.4(4) . . . . ? C50 N18 C51 C47 -1.9(8) . . . . ? C80 N22 C82 C81 65.5(6) . . . . ? C84 N22 C82 C81 -53.2(6) . . . . ? C78 N22 C82 C81 -173.5(5) . . . . ? C74 N21 C72 C71 58.6(5) . . . . ? C70 N21 C72 C71 -62.7(5) . . . . ? C76 N21 C72 C71 178.1(4) . . . . ? C8 C7 C108 C11 0.9(7) . . . . ? N1 C7 C108 C11 -174.5(5) . . . . ? C72 N21 C70 C69 -61.8(5) . . . . ? C74 N21 C70 C69 174.3(5) . . . . ? C76 N21 C70 C69 51.7(6) . . . . ? N9 C10 C11 C108 -0.1(9) . . . . ? C7 C108 C11 C10 -0.4(9) . . . . ? C80 N22 C84 C83 180.0(4) . . . . ? C82 N22 C84 C83 -57.7(6) . . . . ? C78 N22 C84 C83 59.3(5) . . . . ? C72 N21 C76 C75 175.7(5) . . . . ? C74 N21 C76 C75 -64.9(6) . . . . ? C70 N21 C76 C75 54.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.597 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.065 # Attachment '3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 767587' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H22 Co N10 O4, C8 H20 N' _chemical_formula_sum 'C42 H42 Co N11 O4' _chemical_formula_weight 823.80 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 'C 2/c' _symmetry_space_group_name_HALL '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.101(5) _cell_length_b 10.454(5) _cell_length_c 23.321(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.893(5) _cell_angle_gamma 90.000(5) _cell_volume 4169(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7216 _cell_measurement_theta_min 3.4578 _cell_measurement_theta_max 34.7799 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.467 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.902 _exptl_absorpt_correction_T_max 0.937 _exptl_absorpt_process_details ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.49b (release 14-10-2009 CrysAlis171 .NET) (compiled Oct 14 2009,10:37:23) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9853 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9323 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 25.49 _reflns_number_total 3826 _reflns_number_gt 3372 _reflns_threshold_expression >2sigma(I) _computing_data_collection ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.49b (release 14-10-2009 CrysAlis171 .NET) (compiled Oct 14 2009,10:37:23) ; _computing_cell_refinement ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.49b (release 14-10-2009 CrysAlis171 .NET) (compiled Oct 14 2009,10:37:23) ; _computing_data_reduction ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.49b (release 14-10-2009 CrysAlis171 .NET) (compiled Oct 14 2009,10:37:23) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1563P)^2^+15.9281P] 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 3826 _refine_ls_number_parameters 264 _refine_ls_number_restraints 183 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.2383 _refine_ls_wR_factor_gt 0.2308 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.05800(7) 0.7500 0.0267(3) Uani 1 2 d SU . . N5 N 0.38936(19) 0.0647(3) 0.74901(15) 0.0264(7) Uani 1 1 d U . . O2 O 0.3872(2) 0.3146(3) 0.84852(16) 0.0493(9) Uani 1 1 d U . . O1 O 0.3715(2) -0.1865(3) 0.65158(15) 0.0467(9) Uani 1 1 d U . . N2 N 0.48486(19) 0.1911(3) 0.80880(15) 0.0297(7) Uani 1 1 d U . . N1 N 0.4774(2) -0.0785(3) 0.69225(15) 0.0290(7) Uani 1 1 d U . . C5 C 0.3538(2) 0.1515(4) 0.78168(18) 0.0306(9) Uani 1 1 d U . . C13 C 0.4099(2) 0.2290(4) 0.81678(19) 0.0339(9) Uani 1 1 d U . . C4 C 0.3491(2) -0.0128(4) 0.71372(18) 0.0305(9) Uani 1 1 d U . . C7 C 0.4006(2) -0.1034(4) 0.68242(18) 0.0301(9) Uani 1 1 d U . . C8 C 0.5320(2) -0.1589(4) 0.66526(18) 0.0325(9) Uani 1 1 d U . . C3 C 0.2685(3) -0.0026(5) 0.7088(2) 0.0401(10) Uani 1 1 d U . . H3 H 0.2399 -0.0546 0.6824 0.048 Uiso 1 1 calc R . . C6 C 0.2726(3) 0.1633(5) 0.7801(2) 0.0406(10) Uani 1 1 d U . . H6 H 0.2469 0.2235 0.8038 0.049 Uiso 1 1 calc R . . C14 C 0.5434(2) 0.2551(4) 0.84150(19) 0.0343(9) Uani 1 1 d U . . N9 N 0.6398(3) -0.3167(6) 0.6093(2) 0.0693(15) Uani 1 1 d U . . C2 C 0.2304(3) 0.0847(5) 0.7430(2) 0.0463(12) Uani 1 1 d U . . H2 H 0.1750 0.0910 0.7411 0.056 Uiso 1 1 calc R . . C9 C 0.5275(3) -0.2921(5) 0.6681(2) 0.0462(11) Uani 1 1 d U . . H9 H 0.4875 -0.3322 0.6894 0.055 Uiso 1 1 calc R . . C12 C 0.5935(3) -0.1067(6) 0.6347(2) 0.0501(12) Uani 1 1 d U . . H12 H 0.5998 -0.0166 0.6322 0.060 Uiso 1 1 calc R . . C11 C 0.6454(4) -0.1879(7) 0.6081(3) 0.0686(17) Uani 1 1 d U . . H11 H 0.6875 -0.1509 0.5878 0.082 Uiso 1 1 calc R . . C10 C 0.5817(4) -0.3650(6) 0.6396(3) 0.0635(16) Uani 1 1 d U . . H10 H 0.5771 -0.4555 0.6417 0.076 Uiso 1 1 calc R . . N11 N 0.2500 0.2500 1.0000 0.167(6) Uani 1 2 d SDU . . C15 C 0.5699(4) 0.3750(7) 0.8251(3) 0.0704(17) Uani 1 1 d U . . H15 H 0.5512 0.4125 0.7904 0.084 Uiso 1 1 calc R . . N7 N 0.6568(3) 0.3860(7) 0.9064(3) 0.0775(16) Uani 1 1 d U . . C18 C 0.5753(5) 0.2053(7) 0.8894(3) 0.082(2) Uani 1 1 d U . . H18 H 0.5605 0.1222 0.9017 0.098 Uiso 1 1 calc R . . C16 C 0.6227(5) 0.4386(8) 0.8587(3) 0.083(2) Uani 1 1 d U . . H16 H 0.6365 0.5235 0.8484 0.100 Uiso 1 1 calc R . . C17 C 0.6299(5) 0.2751(9) 0.9211(4) 0.095(2) Uani 1 1 d U . . H17 H 0.6487 0.2391 0.9561 0.114 Uiso 1 1 calc R . . C35 C 0.2518(8) 0.3458(12) 0.9481(5) 0.123(4) Uani 1 1 d DU . . H35A H 0.3058 0.3531 0.9339 0.147 Uiso 1 1 calc R . . H35B H 0.2180 0.3132 0.9165 0.147 Uiso 1 1 calc R . . C36 C 0.2229(9) 0.4761(16) 0.9671(7) 0.164(5) Uani 1 1 d U . . H36A H 0.2241 0.5355 0.9346 0.246 Uiso 1 1 calc R . . H36B H 0.2569 0.5085 0.9981 0.246 Uiso 1 1 calc R . . H36C H 0.1693 0.4686 0.9808 0.246 Uiso 1 1 calc R . . C37 C 0.3355(16) 0.190(4) 0.9960(18) 0.47(3) Uani 1 1 d DU . . H37A H 0.3244 0.1469 0.9590 0.565 Uiso 1 1 calc R . . H37B H 0.3597 0.2719 0.9841 0.565 Uiso 1 1 calc R . . C38 C 0.416(2) 0.121(5) 1.006(2) 0.48(3) Uani 1 1 d DU . . H38A H 0.4373 0.0971 0.9683 0.721 Uiso 1 1 calc R . . H38B H 0.4081 0.0439 1.0287 0.721 Uiso 1 1 calc R . . H38C H 0.4522 0.1787 1.0255 0.721 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 0.0223(4) 0.0231(4) 0.0346(5) 0.000 0.0004(3) 0.000 N5 0.0218(15) 0.0258(16) 0.0316(16) 0.0024(13) 0.0013(12) -0.0010(12) O2 0.0407(17) 0.0451(18) 0.062(2) -0.0219(16) 0.0064(15) 0.0052(14) O1 0.0402(17) 0.0475(19) 0.0521(19) -0.0174(15) -0.0038(14) -0.0060(14) N2 0.0270(16) 0.0252(16) 0.0368(17) -0.0036(13) 0.0012(13) 0.0008(13) N1 0.0277(16) 0.0251(16) 0.0340(17) -0.0005(13) -0.0013(13) 0.0003(13) C5 0.0260(18) 0.0262(18) 0.040(2) 0.0026(16) 0.0038(16) 0.0022(15) C13 0.0292(19) 0.028(2) 0.044(2) -0.0021(17) 0.0037(16) 0.0018(16) C4 0.0261(18) 0.0304(19) 0.0349(19) 0.0008(16) -0.0021(15) -0.0022(16) C7 0.0278(19) 0.0284(19) 0.0341(19) -0.0013(16) -0.0033(15) -0.0053(16) C8 0.0311(19) 0.031(2) 0.035(2) -0.0048(16) -0.0035(16) 0.0036(16) C3 0.028(2) 0.043(2) 0.049(2) -0.0046(19) -0.0063(18) -0.0045(18) C6 0.030(2) 0.039(2) 0.052(2) -0.0036(19) 0.0049(18) 0.0056(18) C14 0.0282(19) 0.036(2) 0.039(2) -0.0087(17) 0.0015(16) 0.0016(16) N9 0.062(3) 0.068(3) 0.078(3) -0.022(2) 0.010(2) 0.018(2) C2 0.025(2) 0.053(3) 0.061(3) -0.001(2) -0.0002(19) 0.0017(19) C9 0.051(3) 0.037(2) 0.050(2) -0.003(2) 0.002(2) 0.006(2) C12 0.044(2) 0.050(3) 0.056(3) -0.012(2) 0.013(2) -0.004(2) C11 0.056(3) 0.077(4) 0.073(3) -0.015(3) 0.019(3) 0.005(3) C10 0.071(3) 0.049(3) 0.071(3) -0.011(3) -0.002(3) 0.016(3) N11 0.180(8) 0.158(8) 0.162(8) -0.009(5) -0.007(5) 0.010(5) C15 0.080(3) 0.073(3) 0.057(3) 0.004(3) -0.008(3) -0.035(3) N7 0.062(3) 0.085(3) 0.085(3) -0.021(3) -0.018(3) -0.009(3) C18 0.099(4) 0.061(3) 0.084(4) 0.003(3) -0.041(3) -0.010(3) C16 0.087(4) 0.082(4) 0.081(4) -0.008(3) -0.001(3) -0.035(3) C17 0.103(4) 0.090(4) 0.091(4) -0.002(3) -0.046(4) 0.008(4) C35 0.129(5) 0.133(6) 0.106(5) -0.006(4) 0.005(4) 0.008(4) C36 0.167(7) 0.164(7) 0.160(7) 0.005(5) -0.002(5) 0.010(5) C37 0.47(3) 0.47(3) 0.47(3) -0.001(5) 0.009(6) 0.000(5) C38 0.48(3) 0.48(3) 0.48(3) 0.000(5) 0.007(5) 0.001(5) _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 N5 1.893(3) . ? Co1 N5 1.893(3) 2_656 ? Co1 N2 1.974(3) . ? Co1 N2 1.974(3) 2_656 ? Co1 N1 1.996(3) . ? Co1 N1 1.996(3) 2_656 ? N5 C5 1.337(5) . ? N5 C4 1.338(5) . ? O2 C13 1.228(5) . ? O1 C7 1.228(5) . ? N2 C13 1.358(5) . ? N2 C14 1.417(5) . ? N1 C7 1.356(5) . ? N1 C8 1.410(5) . ? C5 C6 1.394(6) . ? C5 C13 1.491(6) . ? C4 C3 1.386(6) . ? C4 C7 1.492(6) . ? C8 C12 1.391(7) . ? C8 C9 1.397(7) . ? C3 C2 1.382(7) . ? C3 H3 0.9500 . ? C6 C2 1.388(7) . ? C6 H6 0.9500 . ? C14 C18 1.341(8) . ? C14 C15 1.389(8) . ? N9 C10 1.327(9) . ? N9 C11 1.350(9) . ? C2 H2 0.9500 . ? C9 C10 1.378(8) . ? C9 H9 0.9500 . ? C12 C11 1.382(8) . ? C12 H12 0.9500 . ? C11 H11 0.9500 . ? C10 H10 0.9500 . ? N11 C35 1.571(12) 7_557 ? N11 C35 1.571(12) . ? N11 C37 1.594(19) 7_557 ? N11 C37 1.594(19) . ? C15 C16 1.359(9) . ? C15 H15 0.9500 . ? N7 C17 1.296(11) . ? N7 C16 1.363(10) . ? C18 C17 1.389(11) . ? C18 H18 0.9500 . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C35 C36 1.517(17) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.56(2) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 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 N5 Co1 N5 175.8(2) . 2_656 ? N5 Co1 N2 80.83(14) . . ? N5 Co1 N2 96.17(14) 2_656 . ? N5 Co1 N2 96.17(14) . 2_656 ? N5 Co1 N2 80.83(14) 2_656 2_656 ? N2 Co1 N2 90.3(2) . 2_656 ? N5 Co1 N1 80.54(14) . . ? N5 Co1 N1 102.54(14) 2_656 . ? N2 Co1 N1 161.27(14) . . ? N2 Co1 N1 93.53(15) 2_656 . ? N5 Co1 N1 102.54(14) . 2_656 ? N5 Co1 N1 80.54(14) 2_656 2_656 ? N2 Co1 N1 93.53(15) . 2_656 ? N2 Co1 N1 161.27(14) 2_656 2_656 ? N1 Co1 N1 88.7(2) . 2_656 ? C5 N5 C4 121.8(3) . . ? C5 N5 Co1 118.8(3) . . ? C4 N5 Co1 119.3(3) . . ? C13 N2 C14 116.7(3) . . ? C13 N2 Co1 115.8(3) . . ? C14 N2 Co1 127.4(3) . . ? C7 N1 C8 117.1(3) . . ? C7 N1 Co1 115.3(3) . . ? C8 N1 Co1 127.2(3) . . ? N5 C5 C6 120.5(4) . . ? N5 C5 C13 112.8(3) . . ? C6 C5 C13 126.7(4) . . ? O2 C13 N2 127.1(4) . . ? O2 C13 C5 121.4(4) . . ? N2 C13 C5 111.5(4) . . ? N5 C4 C3 120.4(4) . . ? N5 C4 C7 112.5(3) . . ? C3 C4 C7 127.1(4) . . ? O1 C7 N1 128.1(4) . . ? O1 C7 C4 119.9(4) . . ? N1 C7 C4 111.9(3) . . ? C12 C8 C9 117.2(4) . . ? C12 C8 N1 120.4(4) . . ? C9 C8 N1 122.4(4) . . ? C2 C3 C4 118.7(4) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C2 C6 C5 118.2(4) . . ? C2 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? C18 C14 C15 116.7(5) . . ? C18 C14 N2 122.7(5) . . ? C15 C14 N2 120.6(4) . . ? C10 N9 C11 116.4(5) . . ? C3 C2 C6 120.4(4) . . ? C3 C2 H2 119.8 . . ? C6 C2 H2 119.8 . . ? C10 C9 C8 119.5(5) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C12 C8 119.1(6) . . ? C11 C12 H12 120.5 . . ? C8 C12 H12 120.5 . . ? N9 C11 C12 123.8(6) . . ? N9 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? N9 C10 C9 124.1(6) . . ? N9 C10 H10 118.0 . . ? C9 C10 H10 118.0 . . ? C35 N11 C35 180.000(4) 7_557 . ? C35 N11 C37 100.1(12) 7_557 7_557 ? C35 N11 C37 79.9(12) . 7_557 ? C35 N11 C37 79.9(12) 7_557 . ? C35 N11 C37 100.1(12) . . ? C37 N11 C37 180(3) 7_557 . ? C16 C15 C14 120.0(6) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 N7 C16 115.3(6) . . ? C14 C18 C17 120.0(7) . . ? C14 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C15 C16 N7 123.0(7) . . ? C15 C16 H16 118.5 . . ? N7 C16 H16 118.5 . . ? N7 C17 C18 124.6(7) . . ? N7 C17 H17 117.7 . . ? C18 C17 H17 117.7 . . ? C36 C35 N11 109.8(9) . . ? C36 C35 H35A 109.7 . . ? N11 C35 H35A 109.7 . . ? C36 C35 H35B 109.7 . . ? N11 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 N11 168(3) . . ? C38 C37 H37A 93.9 . . ? N11 C37 H37A 93.9 . . ? C38 C37 H37B 93.9 . . ? N11 C37 H37B 93.9 . . ? H37A C37 H37B 103.1 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.202 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.118 # Attachment '3a.cif' data_3a _database_code_depnum_ccdc_archive 'CCDC 767588' #TrackingRef '3a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C204 H144 Co6 N60 O30 Zn5, 6(N O3), 8(O)' _chemical_formula_sum 'C204 H144 Co6 N66 O56 Zn5' _chemical_formula_weight 5096.28 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_HALL '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 38.9152(14) _cell_length_b 38.9152(14) _cell_length_c 14.4944(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 19009.4(13) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9903 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 28.4 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.324 _exptl_crystal_size_mid 0.168 _exptl_crystal_size_min 0.109 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7770 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.903 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 148473 _diffrn_reflns_av_R_equivalents 0.1181 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.39 _reflns_number_total 10468 _reflns_number_gt 5960 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Output of the Platon SQUEEZE routine has been appended to the CIF. Four of the highly disordered uncoordinated water molecules (O5W, O6W, O7W, and O8W) were removed by the 'SQUEEZE' routine of the PLATON program successfully and the remaining structure was then refined again with the new solvent free reflection data to give a converged improved model. As a result of the solvent removal, the final structure shows solvent accessible voids of volume 564 A^3^ (Z = 3)which correspond to 4.5 water molecules. ; _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^)+(0.2000P)^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 10468 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1614 _refine_ls_R_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.3291 _refine_ls_wR_factor_gt 0.2756 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _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 Zn1 Zn 0.3333 0.1667 0.6667 0.0252(3) Uani 1 2 d S . . Zn2 Zn 0.0000 0.0000 0.3109(2) 0.1032(9) Uani 1 3 d S . . Co Co 0.21530(2) 0.04885(2) 0.25470(5) 0.0291(2) Uani 1 1 d . . . O1 O 0.13278(16) -0.01998(17) 0.0681(4) 0.0663(15) Uani 1 1 d . . . O2 O 0.31818(15) 0.04799(18) 0.2702(4) 0.0606(14) Uani 1 1 d . . . O3 O 0.18260(15) 0.19381(15) 0.4837(3) 0.0478(12) Uani 1 1 d . . . O4 O 0.2214(2) 0.15093(17) 0.1781(3) 0.0747(19) Uani 1 1 d . . . O5 O 0.1664(7) 0.0690(11) 0.7282(17) 0.33(2) Uani 1 1 d . . . O6 O 0.121(2) 0.0055(13) 0.699(3) 0.62(5) Uani 1 1 d . . . O7 O 0.1278(8) 0.0407(7) 0.8624(16) 0.354(18) Uani 1 1 d . . . N1 N 0.16289(15) 0.02099(15) 0.1926(4) 0.0388(12) Uani 1 1 d . . . N2 N 0.27059(14) 0.06683(13) 0.2905(3) 0.0303(10) Uani 1 1 d . . . N3 N 0.18769(14) 0.19905(14) 0.6432(3) 0.0303(10) Uani 1 1 d . . . N4 N 0.22819(17) 0.09551(15) 0.1793(3) 0.0387(12) Uani 1 1 d . . . N5 N 0.22627(15) 0.01953(14) 0.1703(3) 0.0324(10) Uani 1 1 d . . . N6 N 0.20542(15) 0.07797(14) 0.3409(3) 0.0352(11) Uani 1 1 d . . . N7 N 0.31637(13) 0.13453(13) 0.5342(3) 0.0294(10) Uani 1 1 d . . . N8 N 0.28484(13) 0.17966(13) 0.6557(3) 0.0282(10) Uani 1 1 d . . . N9 N 0.0550(2) 0.0113(2) 0.2700(7) 0.079(2) Uani 1 1 d . . . N10 N 0.26399(19) 0.10551(16) -0.0969(4) 0.0481(14) Uani 1 1 d . . . N11 N 0.144(3) 0.045(2) 0.760(4) 0.62(6) Uani 1 1 d . . . C1 C 0.2412(3) -0.0246(2) 0.0489(5) 0.057(2) Uani 1 1 d . . . H1 H 0.2465 -0.0396 0.0077 0.069 Uiso 1 1 calc R . . C2 C 0.2056(2) -0.0249(2) 0.0429(5) 0.0509(17) Uani 1 1 d . . . H2 H 0.1869 -0.0397 -0.0021 0.061 Uiso 1 1 calc R . . C3 C 0.19874(19) -0.00207(17) 0.1076(4) 0.0366(13) Uani 1 1 d . . . C4 C 0.26063(19) 0.02045(18) 0.1761(4) 0.0397(14) Uani 1 1 d . . . C5 C 0.2689(2) -0.0022(2) 0.1150(5) 0.0544(18) Uani 1 1 d . . . H5 H 0.2928 -0.0022 0.1189 0.065 Uiso 1 1 calc R . . C6 C 0.1610(2) -0.0007(2) 0.1191(5) 0.0466(16) Uani 1 1 d . . . C7 C 0.28665(18) 0.04661(19) 0.2516(4) 0.0392(14) Uani 1 1 d . . . C9 C 0.1274(2) 0.0197(2) 0.2198(6) 0.0536(18) Uani 1 1 d . . . C10 C 0.1060(4) 0.0291(5) 0.1640(10) 0.123(5) Uani 1 1 d . . . H10 H 0.1149 0.0378 0.1043 0.148 Uiso 1 1 calc R . . C11 C 0.0711(4) 0.0262(6) 0.1935(13) 0.144(7) Uani 1 1 d . . . H11 H 0.0587 0.0358 0.1549 0.173 Uiso 1 1 calc R . . C12 C 0.0769(3) 0.0066(4) 0.3305(10) 0.105(4) Uani 1 1 d . . . H12 H 0.0680 0.0012 0.3912 0.127 Uiso 1 1 calc R . . C13 C 0.1126(3) 0.0090(3) 0.3095(7) 0.074(2) Uani 1 1 d . . . H13 H 0.1265 0.0037 0.3540 0.089 Uiso 1 1 calc R . . C14 C 0.28895(17) 0.09008(16) 0.3707(4) 0.0322(12) Uani 1 1 d . . . C15 C 0.29419(19) 0.12835(17) 0.3780(4) 0.0372(13) Uani 1 1 d . . . H15 H 0.2891 0.1400 0.3276 0.045 Uiso 1 1 calc R . . C16 C 0.30675(17) 0.14837(16) 0.4592(4) 0.0336(12) Uani 1 1 d . . . H16 H 0.3088 0.1732 0.4632 0.040 Uiso 1 1 calc R . . C17 C 0.31388(16) 0.09871(16) 0.5245(4) 0.0305(12) Uani 1 1 d . . . H17 H 0.3219 0.0890 0.5736 0.037 Uiso 1 1 calc R . . C18 C 0.30020(17) 0.07598(16) 0.4464(4) 0.0322(12) Uani 1 1 d . . . H18 H 0.2984 0.0513 0.4440 0.039 Uiso 1 1 calc R . . C19 C 0.2022(3) 0.1347(2) 0.3791(5) 0.066(2) Uani 1 1 d . . . H19 H 0.2035 0.1584 0.3620 0.079 Uiso 1 1 calc R . . C20 C 0.2071(2) 0.1116(2) 0.3150(5) 0.0470(16) Uani 1 1 d . . . C21 C 0.2187(2) 0.1213(2) 0.2153(4) 0.0486(17) Uani 1 1 d . . . C22 C 0.2399(2) 0.09983(17) 0.0863(4) 0.0392(14) Uani 1 1 d . . . C23 C 0.2740(2) 0.0999(2) 0.0631(4) 0.0457(16) Uani 1 1 d . . . H23 H 0.2902 0.0986 0.1085 0.055 Uiso 1 1 calc R . . C24 C 0.2840(2) 0.1019(2) -0.0291(5) 0.0493(17) Uani 1 1 d . . . H24 H 0.3066 0.1005 -0.0438 0.059 Uiso 1 1 calc R . . C25 C 0.2311(3) 0.1056(2) -0.0742(5) 0.059(2) Uani 1 1 d . . . H25 H 0.2159 0.1075 -0.1214 0.071 Uiso 1 1 calc R . . C26 C 0.2179(3) 0.1029(2) 0.0154(5) 0.0524(18) Uani 1 1 d . . . H26 H 0.1946 0.1033 0.0278 0.063 Uiso 1 1 calc R . . C27 C 0.28670(19) 0.21024(18) 0.6064(5) 0.0406(14) Uani 1 1 d . . . H27 H 0.3101 0.2271 0.5753 0.049 Uiso 1 1 calc R . . C28 C 0.25497(19) 0.21734(19) 0.6006(5) 0.0427(15) Uani 1 1 d . . . H28 H 0.2573 0.2383 0.5650 0.051 Uiso 1 1 calc R . . C29 C 0.22123(17) 0.19408(16) 0.6461(4) 0.0296(12) Uani 1 1 d . . . C30 C 0.21883(18) 0.16266(19) 0.6983(5) 0.0418(15) Uani 1 1 d . . . H30 H 0.1961 0.1462 0.7320 0.050 Uiso 1 1 calc R . . C31 C 0.25083(18) 0.15679(19) 0.6987(4) 0.0397(14) Uani 1 1 d . . . H31 H 0.2484 0.1352 0.7315 0.048 Uiso 1 1 calc R . . C32 C 0.1708(2) 0.19766(18) 0.5594(4) 0.0379(14) Uani 1 1 d . . . C33 C 0.13363(19) 0.1988(2) 0.5716(4) 0.0399(14) Uani 1 1 d . . . C34 C 0.1063(2) 0.1932(3) 0.5043(5) 0.056(2) Uani 1 1 d . . . H34 H 0.1101 0.1882 0.4435 0.068 Uiso 1 1 calc R . . C35 C 0.0732(3) 0.1952(3) 0.5302(6) 0.073(3) Uani 1 1 d . . . H35 H 0.0544 0.1918 0.4859 0.087 Uiso 1 1 calc R . . O1W O 0.29671(12) 0.11259(13) 0.7349(3) 0.0314(9) Uani 1 1 d . . . O2W O 0.0000 0.0000 0.5000 0.078(5) Uani 1 6 d S . . O3W O 0.0000 0.0000 0.0000 0.232(18) Uani 1 6 d S . . O4W O 0.2339(3) 0.0473(2) 0.6728(5) 0.122(4) Uani 1 1 d . . . H1W1 H 0.282(2) 0.089(3) 0.714(5) 0.05(2) Uiso 1 1 d . . . H2W1 H 0.289(2) 0.113(2) 0.789(6) 0.05(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0290(5) 0.0267(4) 0.0204(4) 0.0018(3) 0.0018(3) 0.0143(4) Zn2 0.0567(7) 0.0567(7) 0.196(3) 0.000 0.000 0.0284(4) Co 0.0400(5) 0.0281(4) 0.0204(4) -0.0027(3) 0.0002(3) 0.0181(3) O1 0.059(3) 0.078(4) 0.065(4) -0.032(3) -0.029(3) 0.036(3) O2 0.050(3) 0.089(4) 0.051(3) -0.032(3) -0.011(2) 0.041(3) O3 0.075(3) 0.071(3) 0.026(2) -0.013(2) -0.008(2) 0.058(3) O4 0.159(6) 0.066(3) 0.036(3) 0.007(2) 0.007(3) 0.084(4) O5 0.209(18) 0.44(4) 0.168(17) 0.05(2) 0.092(15) 0.04(2) O6 1.04(14) 0.38(5) 0.41(5) -0.15(4) 0.14(7) 0.33(7) O7 0.33(3) 0.25(2) 0.211(17) 0.071(16) -0.127(18) -0.055(18) N1 0.041(3) 0.043(3) 0.038(3) -0.012(2) -0.008(2) 0.025(2) N2 0.038(3) 0.030(2) 0.020(2) -0.0005(18) 0.0019(19) 0.016(2) N3 0.039(3) 0.040(3) 0.023(2) -0.0061(19) -0.0091(19) 0.028(2) N4 0.061(3) 0.037(3) 0.025(2) 0.002(2) 0.002(2) 0.030(3) N5 0.045(3) 0.032(2) 0.021(2) -0.0014(18) 0.001(2) 0.020(2) N6 0.049(3) 0.031(2) 0.025(2) -0.0068(19) 0.002(2) 0.019(2) N7 0.032(2) 0.029(2) 0.025(2) 0.0003(18) 0.0008(18) 0.0131(19) N8 0.034(2) 0.032(2) 0.021(2) -0.0012(18) 0.0012(18) 0.018(2) N9 0.072(5) 0.064(5) 0.111(7) -0.005(4) -0.005(5) 0.041(4) N10 0.065(4) 0.045(3) 0.026(3) 0.011(2) 0.010(3) 0.022(3) N11 1.09(14) 0.94(13) 0.35(5) -0.38(7) -0.50(7) 0.91(13) C1 0.080(5) 0.061(4) 0.047(4) -0.022(3) 0.004(4) 0.047(4) C2 0.063(4) 0.048(4) 0.038(4) -0.014(3) -0.001(3) 0.025(3) C3 0.046(3) 0.030(3) 0.030(3) -0.005(2) 0.001(3) 0.016(3) C4 0.045(3) 0.039(3) 0.038(3) -0.006(3) 0.004(3) 0.023(3) C5 0.058(4) 0.070(5) 0.046(4) -0.017(4) 0.005(3) 0.040(4) C6 0.056(4) 0.053(4) 0.039(4) -0.008(3) -0.012(3) 0.034(3) C7 0.038(3) 0.043(3) 0.029(3) -0.007(3) 0.004(2) 0.016(3) C9 0.051(4) 0.057(4) 0.060(5) -0.007(4) -0.005(4) 0.033(4) C10 0.106(9) 0.199(15) 0.111(9) 0.069(10) 0.025(7) 0.110(10) C11 0.113(10) 0.217(18) 0.154(14) 0.093(13) 0.042(10) 0.122(12) C12 0.085(7) 0.151(12) 0.109(9) 0.015(8) 0.020(7) 0.080(8) C13 0.069(5) 0.097(7) 0.069(6) -0.001(5) 0.004(5) 0.051(5) C14 0.035(3) 0.031(3) 0.024(3) 0.001(2) 0.006(2) 0.012(2) C15 0.050(4) 0.027(3) 0.028(3) 0.003(2) -0.008(3) 0.014(3) C16 0.037(3) 0.025(3) 0.033(3) 0.002(2) 0.000(2) 0.012(2) C17 0.036(3) 0.029(3) 0.026(3) 0.000(2) 0.001(2) 0.016(2) C18 0.036(3) 0.025(3) 0.032(3) 0.001(2) 0.002(2) 0.013(2) C19 0.120(7) 0.057(5) 0.045(4) -0.002(3) 0.009(4) 0.062(5) C20 0.075(5) 0.043(4) 0.034(3) -0.003(3) -0.001(3) 0.038(4) C21 0.089(5) 0.044(4) 0.029(3) -0.005(3) -0.002(3) 0.045(4) C22 0.066(4) 0.031(3) 0.026(3) 0.001(2) 0.002(3) 0.028(3) C23 0.058(4) 0.050(4) 0.030(3) 0.011(3) 0.001(3) 0.028(3) C24 0.056(4) 0.047(4) 0.036(4) 0.017(3) 0.015(3) 0.019(3) C25 0.084(6) 0.072(5) 0.026(3) 0.017(3) 0.004(3) 0.042(4) C26 0.079(5) 0.058(4) 0.033(3) 0.005(3) 0.000(3) 0.044(4) C27 0.044(3) 0.035(3) 0.050(4) 0.014(3) 0.014(3) 0.025(3) C28 0.049(4) 0.040(3) 0.048(4) 0.013(3) 0.009(3) 0.030(3) C29 0.040(3) 0.034(3) 0.023(3) -0.004(2) -0.007(2) 0.025(3) C30 0.033(3) 0.044(3) 0.051(4) 0.017(3) 0.009(3) 0.021(3) C31 0.043(3) 0.046(3) 0.039(3) 0.015(3) 0.010(3) 0.029(3) C32 0.058(4) 0.040(3) 0.028(3) -0.008(2) -0.007(3) 0.034(3) C33 0.050(4) 0.052(4) 0.031(3) -0.009(3) -0.013(3) 0.035(3) C34 0.071(5) 0.092(6) 0.030(3) -0.014(4) -0.019(3) 0.058(5) C35 0.068(5) 0.128(8) 0.046(5) -0.012(5) -0.024(4) 0.067(6) O1W 0.033(2) 0.029(2) 0.032(2) 0.0067(17) 0.0051(18) 0.0149(18) O2W 0.022(3) 0.022(3) 0.189(17) 0.000 0.000 0.0109(16) O3W 0.21(2) 0.21(2) 0.28(5) 0.000 0.000 0.105(11) O4W 0.132(6) 0.075(4) 0.052(4) 0.006(3) -0.023(4) -0.028(4) _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 Zn1 O1W 2.107(4) . ? Zn1 O1W 2.107(4) 13_556 ? Zn1 N8 2.190(4) 13_556 ? Zn1 N8 2.190(4) . ? Zn1 N7 2.205(5) . ? Zn1 N7 2.205(5) 13_556 ? Zn2 N9 2.047(8) 2 ? Zn2 N9 2.047(8) 3 ? Zn2 N9 2.047(8) . ? Co N6 1.851(5) . ? Co N5 1.862(5) . ? Co N3 1.949(4) 11_556 ? Co N4 1.957(5) . ? Co N2 1.971(5) . ? Co N1 1.984(5) . ? O1 C6 1.221(8) . ? O2 C7 1.231(8) . ? O3 C32 1.226(7) . ? O4 C21 1.229(8) . ? O5 N11 1.02(11) . ? O6 N11 1.60(7) . ? O7 N11 1.59(7) . ? N1 C6 1.338(8) . ? N1 C9 1.412(9) . ? N2 C7 1.349(8) . ? N2 C14 1.426(7) . ? N3 C32 1.368(7) . ? N3 C29 1.412(7) . ? N3 Co 1.949(4) 12_556 ? N4 C21 1.335(8) . ? N4 C22 1.405(8) . ? N5 C4 1.323(8) . ? N5 C3 1.334(8) . ? N6 C20 1.334(8) . ? N6 C33 1.340(8) 11_556 ? N7 C16 1.347(7) . ? N7 C17 1.355(7) . ? N8 C31 1.324(7) . ? N8 C27 1.359(7) . ? N9 C11 1.263(16) . ? N9 C12 1.298(14) . ? N10 C24 1.305(9) . ? N10 C25 1.324(10) . ? C1 C5 1.380(11) . ? C1 C2 1.380(11) . ? C1 H1 0.9300 . ? C2 C3 1.407(9) . ? C2 H2 0.9300 . ? C3 C6 1.505(9) . ? C4 C5 1.396(9) . ? C4 C7 1.492(9) . ? C5 H5 0.9300 . ? C9 C10 1.337(12) . ? C9 C13 1.398(12) . ? C10 C11 1.373(16) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.377(13) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C18 1.392(8) . ? C14 C15 1.403(8) . ? C15 C16 1.360(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.369(8) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.370(10) . ? C19 C35 1.383(11) 11_556 ? C19 H19 0.9300 . ? C20 C21 1.504(9) . ? C22 C23 1.368(10) . ? C22 C26 1.382(9) . ? C23 C24 1.383(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.382(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.396(9) . ? C27 H27 0.9300 . ? C28 C29 1.338(9) . ? C28 H28 0.9300 . ? C29 C30 1.401(8) . ? C30 C31 1.374(8) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.482(9) . ? C33 N6 1.340(8) 12_556 ? C33 C34 1.377(9) . ? C34 C35 1.383(11) . ? C34 H34 0.9300 . ? C35 C19 1.383(11) 12_556 ? C35 H35 0.9300 . ? O1W H1W1 0.85(9) . ? O1W H2W1 0.85(8) . ? 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 O1W Zn1 O1W 179.995(1) . 13_556 ? O1W Zn1 N8 88.06(16) . 13_556 ? O1W Zn1 N8 91.95(16) 13_556 13_556 ? O1W Zn1 N8 91.94(16) . . ? O1W Zn1 N8 88.05(16) 13_556 . ? N8 Zn1 N8 179.998(1) 13_556 . ? O1W Zn1 N7 88.90(18) . . ? O1W Zn1 N7 91.10(18) 13_556 . ? N8 Zn1 N7 88.86(16) 13_556 . ? N8 Zn1 N7 91.14(16) . . ? O1W Zn1 N7 91.10(18) . 13_556 ? O1W Zn1 N7 88.90(18) 13_556 13_556 ? N8 Zn1 N7 91.14(16) 13_556 13_556 ? N8 Zn1 N7 88.86(16) . 13_556 ? N7 Zn1 N7 179.996(1) . 13_556 ? N9 Zn2 N9 112.0(3) 2 3 ? N9 Zn2 N9 112.0(3) 2 . ? N9 Zn2 N9 112.0(3) 3 . ? N6 Co N5 178.4(2) . . ? N6 Co N3 81.8(2) . 11_556 ? N5 Co N3 97.37(19) . 11_556 ? N6 Co N4 81.0(2) . . ? N5 Co N4 99.8(2) . . ? N3 Co N4 162.81(19) 11_556 . ? N6 Co N2 97.4(2) . . ? N5 Co N2 81.2(2) . . ? N3 Co N2 87.3(2) 11_556 . ? N4 Co N2 95.1(2) . . ? N6 Co N1 99.8(2) . . ? N5 Co N1 81.7(2) . . ? N3 Co N1 94.3(2) 11_556 . ? N4 Co N1 88.3(2) . . ? N2 Co N1 162.8(2) . . ? C6 N1 C9 117.1(6) . . ? C6 N1 Co 115.1(4) . . ? C9 N1 Co 127.7(4) . . ? C7 N2 C14 118.7(5) . . ? C7 N2 Co 115.1(4) . . ? C14 N2 Co 123.5(4) . . ? C32 N3 C29 118.6(5) . . ? C32 N3 Co 114.5(4) . 12_556 ? C29 N3 Co 126.4(3) . 12_556 ? C21 N4 C22 118.6(5) . . ? C21 N4 Co 116.1(4) . . ? C22 N4 Co 124.3(4) . . ? C4 N5 C3 122.9(5) . . ? C4 N5 Co 118.7(4) . . ? C3 N5 Co 118.4(4) . . ? C20 N6 C33 122.5(5) . 11_556 ? C20 N6 Co 119.2(4) . . ? C33 N6 Co 118.1(4) 11_556 . ? C16 N7 C17 115.9(5) . . ? C16 N7 Zn1 122.7(4) . . ? C17 N7 Zn1 121.4(4) . . ? C31 N8 C27 115.7(5) . . ? C31 N8 Zn1 119.9(4) . . ? C27 N8 Zn1 124.4(4) . . ? C11 N9 C12 116.6(10) . . ? C11 N9 Zn2 125.4(8) . . ? C12 N9 Zn2 117.6(8) . . ? C24 N10 C25 116.3(6) . . ? O5 N11 O7 129(5) . . ? O5 N11 O6 117(5) . . ? O7 N11 O6 115(7) . . ? C5 C1 C2 121.1(6) . . ? C5 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C1 C2 C3 117.2(6) . . ? C1 C2 H2 121.4 . . ? C3 C2 H2 121.4 . . ? N5 C3 C2 120.4(6) . . ? N5 C3 C6 113.2(5) . . ? C2 C3 C6 126.3(6) . . ? N5 C4 C5 119.5(6) . . ? N5 C4 C7 113.4(5) . . ? C5 C4 C7 127.1(6) . . ? C1 C5 C4 118.9(7) . . ? C1 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? O1 C6 N1 128.2(7) . . ? O1 C6 C3 120.3(6) . . ? N1 C6 C3 111.3(5) . . ? O2 C7 N2 128.7(6) . . ? O2 C7 C4 120.8(6) . . ? N2 C7 C4 110.5(5) . . ? C10 C9 C13 114.9(8) . . ? C10 C9 N1 123.6(9) . . ? C13 C9 N1 121.5(7) . . ? C9 C10 C11 121.0(12) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? N9 C11 C10 123.7(12) . . ? N9 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? N9 C12 C13 123.4(12) . . ? N9 C12 H12 118.3 . . ? C13 C12 H12 118.3 . . ? C12 C13 C9 118.6(9) . . ? C12 C13 H13 120.7 . . ? C9 C13 H13 120.7 . . ? C18 C14 C15 116.9(5) . . ? C18 C14 N2 123.3(5) . . ? C15 C14 N2 119.7(5) . . ? C16 C15 C14 119.5(5) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? N7 C16 C15 124.2(5) . . ? N7 C16 H16 117.9 . . ? C15 C16 H16 117.9 . . ? N7 C17 C18 123.7(5) . . ? N7 C17 H17 118.1 . . ? C18 C17 H17 118.1 . . ? C17 C18 C14 119.6(5) . . ? C17 C18 H18 120.2 . . ? C14 C18 H18 120.2 . . ? C20 C19 C35 118.5(7) . 11_556 ? C20 C19 H19 120.7 . . ? C35 C19 H19 120.7 11_556 . ? N6 C20 C19 119.9(6) . . ? N6 C20 C21 112.1(5) . . ? C19 C20 C21 127.7(6) . . ? O4 C21 N4 127.5(6) . . ? O4 C21 C20 121.9(6) . . ? N4 C21 C20 110.5(5) . . ? C23 C22 C26 117.4(6) . . ? C23 C22 N4 119.5(6) . . ? C26 C22 N4 123.1(6) . . ? C22 C23 C24 118.9(6) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? N10 C24 C23 124.5(7) . . ? N10 C24 H24 117.7 . . ? C23 C24 H24 117.7 . . ? N10 C25 C26 123.9(7) . . ? N10 C25 H25 118.1 . . ? C26 C25 H25 118.1 . . ? C22 C26 C25 118.8(7) . . ? C22 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? N8 C27 C28 122.7(6) . . ? N8 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C29 C28 C27 120.1(6) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 118.1(5) . . ? C28 C29 N3 123.7(5) . . ? C30 C29 N3 118.2(5) . . ? C31 C30 C29 118.5(6) . . ? C31 C30 H30 120.8 . . ? C29 C30 H30 120.8 . . ? N8 C31 C30 124.8(5) . . ? N8 C31 H31 117.6 . . ? C30 C31 H31 117.6 . . ? O3 C32 N3 126.7(6) . . ? O3 C32 C33 122.7(5) . . ? N3 C32 C33 110.4(5) . . ? N6 C33 C34 120.2(6) 12_556 . ? N6 C33 C32 113.0(5) 12_556 . ? C34 C33 C32 126.8(6) . . ? C33 C34 C35 117.8(7) . . ? C33 C34 H34 121.1 . . ? C35 C34 H34 121.1 . . ? C34 C35 C19 121.0(7) . 12_556 ? C34 C35 H35 119.5 . . ? C19 C35 H35 119.5 12_556 . ? Zn1 O1W H1W1 131(5) . . ? Zn1 O1W H2W1 119(5) . . ? H1W1 O1W H2W1 108(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Co N1 C6 174.6(5) . . . . ? N5 Co N1 C6 -6.2(5) . . . . ? N3 Co N1 C6 -103.1(5) 11_556 . . . ? N4 Co N1 C6 94.0(5) . . . . ? N2 Co N1 C6 -8.0(10) . . . . ? N6 Co N1 C9 -9.4(6) . . . . ? N5 Co N1 C9 169.8(6) . . . . ? N3 Co N1 C9 73.0(6) 11_556 . . . ? N4 Co N1 C9 -90.0(6) . . . . ? N2 Co N1 C9 168.0(6) . . . . ? N6 Co N2 C7 169.6(4) . . . . ? N5 Co N2 C7 -9.6(4) . . . . ? N3 Co N2 C7 88.2(4) 11_556 . . . ? N4 Co N2 C7 -108.8(4) . . . . ? N1 Co N2 C7 -7.8(9) . . . . ? N6 Co N2 C14 8.6(4) . . . . ? N5 Co N2 C14 -170.7(4) . . . . ? N3 Co N2 C14 -72.8(4) 11_556 . . . ? N4 Co N2 C14 90.2(4) . . . . ? N1 Co N2 C14 -168.9(6) . . . . ? N6 Co N4 C21 -9.8(5) . . . . ? N5 Co N4 C21 171.6(5) . . . . ? N3 Co N4 C21 -8.8(11) 11_556 . . . ? N2 Co N4 C21 -106.5(5) . . . . ? N1 Co N4 C21 90.4(5) . . . . ? N6 Co N4 C22 -178.3(6) . . . . ? N5 Co N4 C22 3.1(6) . . . . ? N3 Co N4 C22 -177.3(6) 11_556 . . . ? N2 Co N4 C22 85.0(5) . . . . ? N1 Co N4 C22 -78.1(5) . . . . ? N3 Co N5 C4 -80.4(5) 11_556 . . . ? N4 Co N5 C4 99.4(5) . . . . ? N2 Co N5 C4 5.7(4) . . . . ? N1 Co N5 C4 -173.8(5) . . . . ? N3 Co N5 C3 98.3(4) 11_556 . . . ? N4 Co N5 C3 -81.8(5) . . . . ? N2 Co N5 C3 -175.5(4) . . . . ? N1 Co N5 C3 5.0(4) . . . . ? N3 Co N6 C20 -173.5(6) 11_556 . . . ? N4 Co N6 C20 6.2(5) . . . . ? N2 Co N6 C20 100.3(5) . . . . ? N1 Co N6 C20 -80.5(5) . . . . ? N3 Co N6 C33 9.8(5) 11_556 . . 11_556 ? N4 Co N6 C33 -170.5(5) . . . 11_556 ? N2 Co N6 C33 -76.4(5) . . . 11_556 ? N1 Co N6 C33 102.8(5) . . . 11_556 ? O1W Zn1 N7 C16 135.9(4) . . . . ? O1W Zn1 N7 C16 -44.1(4) 13_556 . . . ? N8 Zn1 N7 C16 -136.0(4) 13_556 . . . ? O1W Zn1 N7 C17 -42.1(4) . . . . ? O1W Zn1 N7 C17 137.9(4) 13_556 . . . ? N8 Zn1 N7 C17 46.0(4) 13_556 . . . ? N8 Zn1 N7 C17 -134.0(4) . . . . ? O1W Zn1 N8 C31 7.9(5) . . . . ? O1W Zn1 N8 C31 -172.1(5) 13_556 . . . ? N7 Zn1 N8 C31 96.8(5) . . . . ? N7 Zn1 N8 C31 -83.2(5) 13_556 . . . ? O1W Zn1 N8 C27 -171.8(5) . . . . ? O1W Zn1 N8 C27 8.2(5) 13_556 . . . ? N7 Zn1 N8 C27 -82.8(5) . . . . ? N7 Zn1 N8 C27 97.2(5) 13_556 . . . ? N9 Zn2 N9 C11 -38.8(15) 2 . . . ? N9 Zn2 N9 C11 87.8(13) 3 . . . ? N9 Zn2 N9 C12 133.9(9) 2 . . . ? N9 Zn2 N9 C12 -99.4(10) 3 . . . ? C5 C1 C2 C3 -0.9(11) . . . . ? C4 N5 C3 C2 -0.8(9) . . . . ? Co N5 C3 C2 -179.6(5) . . . . ? C4 N5 C3 C6 175.7(6) . . . . ? Co N5 C3 C6 -3.1(7) . . . . ? C1 C2 C3 N5 1.5(10) . . . . ? C1 C2 C3 C6 -174.5(7) . . . . ? C3 N5 C4 C5 -0.5(9) . . . . ? Co N5 C4 C5 178.2(5) . . . . ? C3 N5 C4 C7 -179.9(5) . . . . ? Co N5 C4 C7 -1.2(7) . . . . ? C2 C1 C5 C4 -0.4(12) . . . . ? N5 C4 C5 C1 1.1(11) . . . . ? C7 C4 C5 C1 -179.6(7) . . . . ? C9 N1 C6 O1 5.1(11) . . . . ? Co N1 C6 O1 -178.4(7) . . . . ? C9 N1 C6 C3 -170.4(6) . . . . ? Co N1 C6 C3 6.1(7) . . . . ? N5 C3 C6 O1 -178.1(6) . . . . ? C2 C3 C6 O1 -1.8(11) . . . . ? N5 C3 C6 N1 -2.2(8) . . . . ? C2 C3 C6 N1 174.1(6) . . . . ? C14 N2 C7 O2 -7.8(10) . . . . ? Co N2 C7 O2 -169.7(6) . . . . ? C14 N2 C7 C4 173.1(5) . . . . ? Co N2 C7 C4 11.1(6) . . . . ? N5 C4 C7 O2 174.1(6) . . . . ? C5 C4 C7 O2 -5.2(11) . . . . ? N5 C4 C7 N2 -6.7(8) . . . . ? C5 C4 C7 N2 174.0(7) . . . . ? C6 N1 C9 C10 -57.0(13) . . . . ? Co N1 C9 C10 127.1(11) . . . . ? C6 N1 C9 C13 124.5(9) . . . . ? Co N1 C9 C13 -51.5(10) . . . . ? C13 C9 C10 C11 -3(2) . . . . ? N1 C9 C10 C11 178.1(14) . . . . ? C12 N9 C11 C10 15(3) . . . . ? Zn2 N9 C11 C10 -172.1(14) . . . . ? C9 C10 C11 N9 -7(3) . . . . ? C11 N9 C12 C13 -14(2) . . . . ? Zn2 N9 C12 C13 172.8(10) . . . . ? N9 C12 C13 C9 4.2(19) . . . . ? C10 C9 C13 C12 4.3(16) . . . . ? N1 C9 C13 C12 -177.1(9) . . . . ? C7 N2 C14 C18 -47.8(8) . . . . ? Co N2 C14 C18 112.6(6) . . . . ? C7 N2 C14 C15 136.1(6) . . . . ? Co N2 C14 C15 -63.5(6) . . . . ? C18 C14 C15 C16 -5.0(9) . . . . ? N2 C14 C15 C16 171.2(5) . . . . ? C17 N7 C16 C15 1.6(8) . . . . ? Zn1 N7 C16 C15 -176.4(5) . . . . ? C14 C15 C16 N7 2.9(9) . . . . ? C16 N7 C17 C18 -4.0(8) . . . . ? Zn1 N7 C17 C18 174.1(4) . . . . ? N7 C17 C18 C14 1.7(9) . . . . ? C15 C14 C18 C17 2.9(8) . . . . ? N2 C14 C18 C17 -173.3(5) . . . . ? C33 N6 C20 C19 0.4(11) 11_556 . . . ? Co N6 C20 C19 -176.1(7) . . . . ? C33 N6 C20 C21 174.5(6) 11_556 . . . ? Co N6 C20 C21 -2.1(8) . . . . ? C35 C19 C20 N6 -0.6(14) 11_556 . . . ? C35 C19 C20 C21 -173.6(9) 11_556 . . . ? C22 N4 C21 O4 -5.3(12) . . . . ? Co N4 C21 O4 -174.5(7) . . . . ? C22 N4 C21 C20 180.0(6) . . . . ? Co N4 C21 C20 10.8(8) . . . . ? N6 C20 C21 O4 179.1(8) . . . . ? C19 C20 C21 O4 -7.4(14) . . . . ? N6 C20 C21 N4 -5.8(9) . . . . ? C19 C20 C21 N4 167.7(8) . . . . ? C21 N4 C22 C23 130.0(7) . . . . ? Co N4 C22 C23 -61.8(8) . . . . ? C21 N4 C22 C26 -51.9(9) . . . . ? Co N4 C22 C26 116.3(6) . . . . ? C26 C22 C23 C24 -1.9(10) . . . . ? N4 C22 C23 C24 176.3(6) . . . . ? C25 N10 C24 C23 -2.9(11) . . . . ? C22 C23 C24 N10 3.2(11) . . . . ? C24 N10 C25 C26 1.5(11) . . . . ? C23 C22 C26 C25 0.6(10) . . . . ? N4 C22 C26 C25 -177.5(7) . . . . ? N10 C25 C26 C22 -0.4(12) . . . . ? C31 N8 C27 C28 -0.2(9) . . . . ? Zn1 N8 C27 C28 179.5(5) . . . . ? N8 C27 C28 C29 1.3(10) . . . . ? C27 C28 C29 C30 -0.5(10) . . . . ? C27 C28 C29 N3 -179.4(6) . . . . ? C32 N3 C29 C28 58.0(8) . . . . ? Co N3 C29 C28 -112.7(6) 12_556 . . . ? C32 N3 C29 C30 -120.9(6) . . . . ? Co N3 C29 C30 68.4(7) 12_556 . . . ? C28 C29 C30 C31 -1.3(9) . . . . ? N3 C29 C30 C31 177.6(6) . . . . ? C27 N8 C31 C30 -1.8(9) . . . . ? Zn1 N8 C31 C30 178.5(5) . . . . ? C29 C30 C31 N8 2.7(10) . . . . ? C29 N3 C32 O3 -2.7(9) . . . . ? Co N3 C32 O3 169.1(5) 12_556 . . . ? C29 N3 C32 C33 173.5(5) . . . . ? Co N3 C32 C33 -14.7(6) 12_556 . . . ? O3 C32 C33 N6 -176.5(6) . . . 12_556 ? N3 C32 C33 N6 7.1(8) . . . 12_556 ? O3 C32 C33 C34 4.8(11) . . . . ? N3 C32 C33 C34 -171.6(7) . . . . ? N6 C33 C34 C35 0.9(12) 12_556 . . . ? C32 C33 C34 C35 179.6(8) . . . . ? C33 C34 C35 C19 -0.8(15) . . . 12_556 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.919 _refine_diff_density_min -1.650 _refine_diff_density_rms 0.182 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.333 0.815 573.6 27.4 2 0.000 0.667 0.723 570.9 28.4 3 0.018 0.083 1.002 10.6 0.4 4 0.049 0.949 0.492 24.7 1.2 5 0.051 0.101 0.492 25.3 1.3 6 0.064 0.982 0.002 10.7 0.4 7 0.104 0.052 0.510 21.2 0.8 8 0.083 0.064 0.998 10.7 0.5 9 0.334 0.333 0.182 571.0 28.3 10 0.334 0.000 0.810 569.0 27.4 11 0.233 0.617 0.159 23.1 1.2 12 0.250 0.602 0.669 11.4 0.4 13 0.287 0.722 0.180 21.7 1.1 14 0.285 0.564 0.171 21.4 1.1 15 0.269 0.685 0.665 11.0 0.5 16 0.315 0.584 0.665 11.0 0.4 17 0.388 0.619 0.162 21.9 0.8 18 0.352 0.750 0.669 11.3 0.5 19 0.389 0.769 0.154 21.9 0.8 20 0.398 0.648 0.669 11.3 0.5 21 0.438 0.718 0.176 20.5 1.1 22 0.416 0.731 0.665 11.0 0.5 23 0.667 0.999 0.847 568.3 28.4 24 0.667 0.667 0.419 566.9 27.4 25 0.566 0.284 0.825 23.0 1.3 26 0.584 0.269 0.335 10.9 0.5 27 0.620 0.389 0.846 21.7 1.0 28 0.619 0.231 0.838 21.4 0.8 29 0.602 0.352 0.331 11.3 0.4 30 0.648 0.250 0.331 11.5 0.4 31 0.721 0.285 0.829 22.1 1.1 32 0.685 0.416 0.335 10.9 0.5 33 0.722 0.435 0.820 22.0 1.0 34 0.731 0.315 0.335 11.0 0.5 35 0.771 0.385 0.843 20.3 0.8 36 0.750 0.398 0.331 11.4 0.5 37 0.899 0.951 0.492 24.1 1.2 38 0.948 0.052 0.510 19.9 0.5 39 0.917 0.935 0.002 10.7 0.4 40 0.948 0.896 0.510 20.1 0.6 41 0.935 0.018 -0.002 10.6 0.4 42 0.982 0.917 0.998 10.8 0.4 _platon_squeeze_details ; ? ;