# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email guillem.aromi@qi.ub.es _publ_contact_author_name 'Guillem Aromi' loop_ _publ_author_name 'G. A. Craig' 'J. Sanchez Costa' 'D. Aguila' 'L. A. Barrios' O.Roubeau 'S. J. Teat' 'G. Aromi' data_gac163a _database_code_depnum_ccdc_archive 'CCDC 798852' #TrackingRef '2994_web_deposit_cif_file_0_OlivierRoubeau_1288354517.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C71 H54 Co4 N12 O7, 3(C5 H5 N), 2(C H4 O)' _chemical_formula_sum 'C88 H77 Co4 N15 O9' _chemical_formula_weight 1724.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0020 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' N N -0.0031 0.0040 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0074 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Co Co 0.1760 1.1404 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 12.4549(7) _cell_length_b 12.6214(7) _cell_length_c 26.4841(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.5270(10) _cell_angle_gamma 90.00 _cell_volume 4161.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7931 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 32.04 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.376 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 1.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details 'SADABS v2.10 Bruker AXS Madison WI US' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 43906 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0658 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 33.07 _reflns_number_total 12046 _reflns_number_gt 8370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT v7.56a' _computing_data_reduction 'Bruker SAINT v7.56a' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL & local programs' _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. All non-hydrogens were refined anisotropically. One of the lattice pyridine rings was only half occupied. Both lattice pyridine molecules were refined with displacement parameters restraints. Hydrogens of the main moiety were found in difference Fourier maps. All hydrogens were placed geometrically on their carrier atom and refined with a riding model. Due the special position occupied by C2 and C37, the corresponding methyl hydrogens are also on special positions and are thus disordered by symmetry over two half occupied positions. Two residual electron density peaks remained at the en of the refinement both close to the Co1 atom. ; _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^)+(0.1163P)^2^+2.5472P] 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 12046 _refine_ls_number_parameters 542 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.2114 _refine_ls_wR_factor_gt 0.1900 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.56505(3) 0.12397(4) 0.802774(14) 0.02980(12) Uani 1 1 d . . . Co2 Co 0.69531(4) 0.25203(4) 0.913723(15) 0.03173(13) Uani 1 1 d . . . O1 O 0.5511(2) -0.0297(2) 0.78596(9) 0.0410(6) Uani 1 1 d . . . O2 O 0.6460(2) 0.3209(2) 0.97239(8) 0.0404(5) Uani 1 1 d . . . O3 O 0.1871(2) 0.3453(2) 0.57783(9) 0.0432(6) Uani 1 1 d . . . O4 O 0.5000 0.2042(3) 0.7500 0.0414(8) Uani 1 2 d S . . N1 N 0.5623(2) 0.1702(2) 0.91193(9) 0.0307(5) Uani 1 1 d . . . N2 N 0.5046(2) 0.1392(2) 0.86960(9) 0.0300(5) Uani 1 1 d . . . N3 N 0.2817(2) 0.1507(2) 0.68759(9) 0.0314(5) Uani 1 1 d . . . N4 N 0.2341(2) 0.1949(2) 0.64516(9) 0.0313(5) Uani 1 1 d . . . N5 N 0.7666(2) 0.1431(2) 0.95430(10) 0.0319(5) Uani 1 1 d . . . N6 N 0.6255(3) 0.3654(2) 0.87466(11) 0.0441(7) Uani 1 1 d . . . C1 C 0.5000 -0.0756(4) 0.7500 0.0404(11) Uani 1 2 d S . . C2 C 0.5000 -0.1929(5) 0.7500 0.0612(16) Uani 1 2 d S . . H2A H 0.4583 -0.2188 0.7206 0.092 Uiso 0.50 1 calc PR . . H2B H 0.4677 -0.2188 0.7810 0.092 Uiso 0.50 1 calc PR . . H2C H 0.5740 -0.2188 0.7484 0.092 Uiso 0.50 1 calc PR . . C3 C 0.6052(3) 0.2689(3) 1.01110(12) 0.0391(8) Uani 1 1 d . . . C4 C 0.6322(4) 0.3020(3) 1.06078(13) 0.0489(9) Uani 1 1 d . . . H4A H 0.6808 0.3592 1.0663 0.059 Uiso 1 1 calc R . . C5 C 0.5870(4) 0.2501(4) 1.10176(14) 0.0536(11) Uani 1 1 d . . . H5A H 0.6051 0.2726 1.1351 0.064 Uiso 1 1 calc R . . C6 C 0.5177(3) 0.1679(4) 1.09468(13) 0.0496(10) Uani 1 1 d . . . H6A H 0.4884 0.1333 1.1230 0.060 Uiso 1 1 calc R . . C7 C 0.4893(3) 0.1343(3) 1.04595(13) 0.0433(8) Uani 1 1 d . . . H7A H 0.4399 0.0777 1.0412 0.052 Uiso 1 1 calc R . . C8 C 0.5337(3) 0.1842(3) 1.00400(11) 0.0376(7) Uani 1 1 d . . . C9 C 0.5000(3) 0.1538(3) 0.95273(12) 0.0358(7) Uani 1 1 d . . . C10 C 0.4024(3) 0.1108(3) 0.93641(12) 0.0400(8) Uani 1 1 d . . . H10A H 0.3442 0.0905 0.9568 0.048 Uiso 1 1 calc R . . C11 C 0.4076(2) 0.1038(3) 0.88439(12) 0.0350(7) Uani 1 1 d . . . C12 C 0.3245(2) 0.0632(3) 0.84860(12) 0.0366(7) Uani 1 1 d . . . C13 C 0.2608(3) -0.0218(3) 0.86328(12) 0.0408(8) Uani 1 1 d . . . H13A H 0.2725 -0.0533 0.8955 0.049 Uiso 1 1 calc R . . C14 C 0.1803(3) -0.0606(4) 0.83102(14) 0.0480(9) Uani 1 1 d . . . H14A H 0.1376 -0.1187 0.8413 0.058 Uiso 1 1 calc R . . C15 C 0.1621(3) -0.0150(3) 0.78389(13) 0.0419(8) Uani 1 1 d . . . H15A H 0.1069 -0.0419 0.7620 0.050 Uiso 1 1 calc R . . C16 C 0.2247(2) 0.0703(3) 0.76866(12) 0.0383(7) Uani 1 1 d . . . C17 C 0.3026(3) 0.1108(3) 0.80190(13) 0.0419(8) Uani 1 1 d . . . H17A H 0.3417 0.1721 0.7926 0.050 Uiso 1 1 calc R . . C18 C 0.2018(3) 0.1190(3) 0.71861(12) 0.0351(7) Uani 1 1 d . . . C19 C 0.1034(3) 0.1423(3) 0.69590(12) 0.0398(8) Uani 1 1 d . . . H19A H 0.0346 0.1280 0.7089 0.048 Uiso 1 1 calc R . . C20 C 0.1259(3) 0.1914(3) 0.64984(11) 0.0352(7) Uani 1 1 d . . . C21 C 0.0494(3) 0.2375(3) 0.61378(12) 0.0394(8) Uani 1 1 d . . . C22 C -0.0593(3) 0.2115(4) 0.61439(14) 0.0466(9) Uani 1 1 d . . . H22A H -0.0831 0.1580 0.6367 0.056 Uiso 1 1 calc R . . C23 C -0.1336(4) 0.2629(4) 0.58276(17) 0.0595(12) Uani 1 1 d . . . H23A H -0.2076 0.2449 0.5835 0.071 Uiso 1 1 calc R . . C24 C -0.0983(4) 0.3409(5) 0.55011(19) 0.0685(14) Uani 1 1 d . . . H24A H -0.1487 0.3764 0.5285 0.082 Uiso 1 1 calc R . . C25 C 0.0078(4) 0.3670(4) 0.54871(16) 0.0579(11) Uani 1 1 d . . . H25A H 0.0301 0.4206 0.5261 0.070 Uiso 1 1 calc R . . C26 C 0.0853(3) 0.3158(3) 0.58025(13) 0.0440(8) Uani 1 1 d . . . C27 C 0.7618(3) 0.0408(3) 0.94075(12) 0.0349(7) Uani 1 1 d . . . H27A H 0.7223 0.0218 0.9109 0.042 Uiso 1 1 calc R . . C28 C 0.8128(3) -0.0382(3) 0.96901(13) 0.0403(8) Uani 1 1 d . . . H28A H 0.8084 -0.1101 0.9586 0.048 Uiso 1 1 calc R . . C29 C 0.8703(3) -0.0103(3) 1.01269(13) 0.0438(8) Uani 1 1 d . . . H29A H 0.9058 -0.0629 1.0327 0.053 Uiso 1 1 calc R . . C30 C 0.8750(3) 0.0946(3) 1.02650(12) 0.0422(8) Uani 1 1 d . . . H30A H 0.9139 0.1155 1.0562 0.051 Uiso 1 1 calc R . . C31 C 0.8227(3) 0.1696(3) 0.99686(12) 0.0375(7) Uani 1 1 d . . . H31A H 0.8262 0.2419 1.0067 0.045 Uiso 1 1 calc R . . C32 C 0.5243(4) 0.3929(4) 0.88427(15) 0.0547(11) Uani 1 1 d . . . H32A H 0.4851 0.3526 0.9078 0.066 Uiso 1 1 calc R . . C33 C 0.4743(6) 0.4806(4) 0.86020(17) 0.0776(18) Uani 1 1 d . . . H33A H 0.4023 0.4993 0.8673 0.093 Uiso 1 1 calc R . . C34 C 0.5317(7) 0.5377(4) 0.8267(2) 0.088(2) Uani 1 1 d . . . H34A H 0.5002 0.5978 0.8106 0.106 Uiso 1 1 calc R . . C35 C 0.6372(6) 0.5080(4) 0.8160(2) 0.0797(17) Uani 1 1 d . . . H35A H 0.6781 0.5455 0.7920 0.096 Uiso 1 1 calc R . . C36 C 0.6783(5) 0.4224(4) 0.84159(16) 0.0590(11) Uani 1 1 d . . . H36A H 0.7502 0.4024 0.8351 0.071 Uiso 1 1 calc R . . C37 C 0.5000 0.3135(6) 0.7500 0.093(3) Uani 1 2 d SU . . H37A H 0.4624 0.3394 0.7195 0.140 Uiso 0.50 1 calc PR . . H37B H 0.5742 0.3394 0.7506 0.140 Uiso 0.50 1 calc PR . . H37C H 0.4634 0.3394 0.7799 0.140 Uiso 0.50 1 calc PR . . N1S N 0.9630(4) 0.7982(5) 0.87834(18) 0.0766(13) Uani 1 1 d . . . C2S C 0.9223(6) 0.7112(6) 0.8995(2) 0.0884(19) Uani 1 1 d . . . H2SA H 0.9708 0.6679 0.9187 0.106 Uiso 1 1 calc R . . C3S C 0.8193(6) 0.6793(6) 0.8963(2) 0.088(2) Uani 1 1 d . . . H3SA H 0.7959 0.6159 0.9120 0.106 Uiso 1 1 calc R . . C4S C 0.7483(5) 0.7446(6) 0.8686(3) 0.0908(18) Uani 1 1 d U . . H4SA H 0.6743 0.7266 0.8659 0.109 Uiso 1 1 calc R . . C5S C 0.7851(4) 0.8356(6) 0.8448(2) 0.0813(15) Uani 1 1 d U . . H5SA H 0.7386 0.8800 0.8252 0.098 Uiso 1 1 calc R . . C6S C 0.8939(4) 0.8576(5) 0.85157(19) 0.0695(14) Uani 1 1 d . . . H6SA H 0.9210 0.9195 0.8359 0.083 Uiso 1 1 calc R . . O1S O 0.7300(3) 0.5251(3) 0.9826(2) 0.0908(14) Uani 1 1 d . . . H1S H 0.7176 0.4698 0.9657 0.136 Uiso 1 1 calc R . . C1S C 0.6343(4) 0.5766(4) 0.9914(2) 0.0611(12) Uani 1 1 d . . . H1S1 H 0.6494 0.6478 1.0046 0.092 Uiso 1 1 calc R . . H1S2 H 0.5937 0.5364 1.0162 0.092 Uiso 1 1 calc R . . H1S3 H 0.5921 0.5821 0.9598 0.092 Uiso 1 1 calc R . . N2S N 0.1930(11) 0.6668(11) 0.7835(5) 0.147(4) Uani 0.50 1 d PGU . . C7S C 0.2440(8) 0.5823(13) 0.8077(5) 0.147(4) Uani 0.50 1 d PGU . . H7S H 0.3200 0.5821 0.8120 0.176 Uiso 0.50 1 calc PR . . C8S C 0.1839(12) 0.4983(11) 0.8257(5) 0.164(4) Uani 0.50 1 d PGU . . H8S H 0.2188 0.4405 0.8423 0.196 Uiso 0.50 1 calc PR . . C9S C 0.0728(12) 0.4987(12) 0.8195(6) 0.164(4) Uani 0.50 1 d PGU . . H9S H 0.0317 0.4412 0.8317 0.197 Uiso 0.50 1 calc PR . . C10S C 0.0217(8) 0.5832(14) 0.7952(6) 0.165(4) Uani 0.50 1 d PGU . . H10S H -0.0543 0.5834 0.7909 0.199 Uiso 0.50 1 calc PR . . C11S C 0.0818(11) 0.6672(11) 0.7772(5) 0.159(4) Uani 0.50 1 d PGU . . H11S H 0.0469 0.7250 0.7607 0.190 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0258(2) 0.0463(3) 0.01760(19) -0.00261(16) 0.00641(13) -0.00134(16) Co2 0.0393(2) 0.0379(2) 0.0181(2) -0.00355(16) 0.00292(15) 0.00001(17) O1 0.0418(13) 0.0523(15) 0.0290(12) -0.0036(10) 0.0054(9) -0.0025(11) O2 0.0555(15) 0.0443(13) 0.0216(10) -0.0057(9) 0.0040(10) 0.0088(11) O3 0.0553(15) 0.0452(14) 0.0292(12) 0.0089(10) 0.0018(10) 0.0116(12) O4 0.0475(19) 0.049(2) 0.0283(16) 0.000 0.0066(14) 0.000 N1 0.0326(12) 0.0426(14) 0.0173(11) -0.0007(10) 0.0063(9) 0.0057(11) N2 0.0292(12) 0.0427(15) 0.0183(11) 0.0001(10) 0.0060(9) 0.0037(10) N3 0.0313(12) 0.0455(15) 0.0176(11) 0.0040(10) 0.0039(9) 0.0028(11) N4 0.0342(13) 0.0420(15) 0.0177(11) 0.0022(10) 0.0020(9) 0.0073(11) N5 0.0304(12) 0.0447(15) 0.0209(11) -0.0006(10) 0.0060(9) 0.0013(10) N6 0.067(2) 0.0386(16) 0.0268(14) -0.0043(11) -0.0034(13) 0.0029(14) C1 0.045(3) 0.053(3) 0.023(2) 0.000 0.0047(18) 0.000 C2 0.086(5) 0.058(4) 0.039(3) 0.000 -0.008(3) 0.000 C3 0.0482(19) 0.049(2) 0.0200(14) -0.0026(12) 0.0035(12) 0.0177(15) C4 0.064(2) 0.056(2) 0.0260(16) -0.0082(15) -0.0022(15) 0.0178(19) C5 0.069(3) 0.072(3) 0.0201(16) -0.0058(16) 0.0038(15) 0.031(2) C6 0.055(2) 0.074(3) 0.0203(15) 0.0060(16) 0.0082(14) 0.025(2) C7 0.0383(17) 0.066(2) 0.0263(15) 0.0076(15) 0.0086(12) 0.0169(16) C8 0.0390(16) 0.055(2) 0.0187(13) 0.0010(13) 0.0056(11) 0.0176(15) C9 0.0346(15) 0.0517(19) 0.0214(14) 0.0020(12) 0.0072(11) 0.0108(14) C10 0.0292(14) 0.068(2) 0.0232(14) 0.0088(14) 0.0066(11) 0.0061(15) C11 0.0289(14) 0.0518(19) 0.0247(14) 0.0071(13) 0.0058(11) 0.0043(13) C12 0.0286(14) 0.058(2) 0.0234(14) 0.0081(13) 0.0050(11) 0.0037(13) C13 0.0314(15) 0.067(2) 0.0241(15) 0.0129(14) 0.0057(11) 0.0022(15) C14 0.0332(16) 0.077(3) 0.0342(18) 0.0167(18) 0.0042(13) -0.0098(17) C15 0.0274(14) 0.070(2) 0.0283(15) 0.0105(15) 0.0031(11) -0.0044(15) C16 0.0280(14) 0.065(2) 0.0221(14) 0.0110(14) 0.0053(11) 0.0028(14) C17 0.0362(16) 0.064(2) 0.0258(15) 0.0107(15) 0.0055(12) -0.0040(15) C18 0.0302(14) 0.053(2) 0.0222(14) 0.0067(13) 0.0045(11) 0.0034(13) C19 0.0301(15) 0.068(2) 0.0220(14) 0.0061(14) 0.0037(11) 0.0057(14) C20 0.0325(15) 0.053(2) 0.0200(13) 0.0014(13) 0.0023(11) 0.0094(13) C21 0.0404(17) 0.055(2) 0.0228(14) -0.0015(13) -0.0005(12) 0.0133(15) C22 0.0428(19) 0.067(2) 0.0296(17) -0.0007(16) -0.0054(14) 0.0120(17) C23 0.046(2) 0.083(3) 0.049(2) -0.001(2) -0.0131(18) 0.016(2) C24 0.062(3) 0.089(4) 0.054(3) 0.008(2) -0.018(2) 0.029(3) C25 0.070(3) 0.065(3) 0.038(2) 0.0091(18) -0.0096(19) 0.023(2) C26 0.050(2) 0.055(2) 0.0268(16) 0.0018(14) -0.0022(14) 0.0191(17) C27 0.0325(15) 0.0470(18) 0.0258(14) 0.0000(13) 0.0094(11) 0.0013(13) C28 0.0371(16) 0.050(2) 0.0344(17) 0.0054(14) 0.0118(13) 0.0054(14) C29 0.0337(16) 0.065(2) 0.0329(17) 0.0120(16) 0.0111(13) 0.0094(16) C30 0.0338(16) 0.070(2) 0.0231(15) 0.0042(15) 0.0050(12) 0.0020(16) C31 0.0340(15) 0.057(2) 0.0214(14) -0.0049(13) 0.0048(11) 0.0006(14) C32 0.083(3) 0.052(2) 0.0287(18) -0.0052(16) -0.0055(18) 0.026(2) C33 0.125(5) 0.070(3) 0.037(2) -0.005(2) -0.007(3) 0.052(3) C34 0.166(7) 0.049(3) 0.049(3) 0.004(2) -0.016(3) 0.025(3) C35 0.132(6) 0.053(3) 0.054(3) 0.013(2) -0.002(3) -0.003(3) C36 0.092(3) 0.047(2) 0.038(2) 0.0043(17) -0.003(2) -0.010(2) C37 0.165(8) 0.060(4) 0.052(4) 0.000 -0.039(5) 0.000 N1S 0.059(2) 0.108(4) 0.063(3) 0.016(3) -0.001(2) -0.012(2) C2S 0.091(4) 0.113(5) 0.061(3) 0.021(3) -0.002(3) -0.025(4) C3S 0.092(4) 0.111(5) 0.062(3) -0.007(3) 0.023(3) -0.041(4) C4S 0.054(3) 0.126(4) 0.094(4) -0.054(3) 0.018(3) -0.027(3) C5S 0.061(3) 0.105(4) 0.078(4) -0.043(3) -0.003(2) 0.005(3) C6S 0.066(3) 0.098(4) 0.045(2) -0.004(2) 0.006(2) -0.007(3) O1S 0.0537(19) 0.060(2) 0.158(4) -0.051(2) -0.009(2) -0.0064(16) C1S 0.048(2) 0.070(3) 0.065(3) -0.016(2) 0.004(2) -0.007(2) N2S 0.129(6) 0.175(7) 0.137(7) 0.002(6) 0.001(6) 0.000(5) C7S 0.128(6) 0.178(7) 0.132(7) 0.002(6) -0.021(6) -0.012(5) C8S 0.142(6) 0.197(7) 0.150(7) 0.027(6) -0.030(6) -0.020(6) C9S 0.138(6) 0.192(7) 0.161(7) 0.031(6) -0.013(6) -0.018(6) C10S 0.136(6) 0.189(7) 0.171(7) 0.026(6) -0.006(6) -0.009(5) C11S 0.132(6) 0.180(7) 0.163(7) 0.022(6) -0.007(6) -0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 1.891(2) . ? Co1 N3 1.949(3) 2_656 ? Co1 N2 1.951(2) . ? Co1 O1 1.997(3) . ? Co2 O3 1.888(3) 2_656 ? Co2 O2 1.897(2) . ? Co2 N5 1.945(3) . ? Co2 N4 1.949(3) 2_656 ? Co2 N1 1.952(3) . ? Co2 N6 1.956(3) . ? O1 C1 1.271(4) . ? O2 C3 1.329(4) . ? O3 C26 1.325(5) . ? O3 Co2 1.888(3) 2_656 ? O4 C37 1.380(9) . ? O4 Co1 1.891(2) 2_656 ? N1 C9 1.363(4) . ? N1 N2 1.372(4) . ? N2 C11 1.356(4) . ? N3 C18 1.366(4) . ? N3 N4 1.375(3) . ? N3 Co1 1.949(3) 2_656 ? N4 C20 1.357(4) . ? N4 Co2 1.949(3) 2_656 ? N5 C27 1.341(4) . ? N5 C31 1.352(4) . ? N6 C36 1.322(6) . ? N6 C32 1.338(6) . ? C1 O1 1.271(4) 2_656 ? C1 C2 1.481(9) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C8 1.401(6) . ? C3 C4 1.412(5) . ? C4 C5 1.399(6) . ? C4 H4A 0.9500 . ? C5 C6 1.359(7) . ? C5 H5A 0.9500 . ? C6 C7 1.395(5) . ? C6 H6A 0.9500 . ? C7 C8 1.403(5) . ? C7 H7A 0.9500 . ? C8 C9 1.462(4) . ? C9 C10 1.390(5) . ? C10 C11 1.384(4) . ? C10 H10A 0.9500 . ? C11 C12 1.476(5) . ? C12 C17 1.395(4) . ? C12 C13 1.396(5) . ? C13 C14 1.388(5) . ? C13 H13A 0.9500 . ? C14 C15 1.388(5) . ? C14 H14A 0.9500 . ? C15 C16 1.396(5) . ? C15 H15A 0.9500 . ? C16 C17 1.390(5) . ? C16 C18 1.482(4) . ? C17 H17A 0.9500 . ? C18 C19 1.382(4) . ? C19 C20 1.403(4) . ? C19 H19A 0.9500 . ? C20 C21 1.452(4) . ? C21 C22 1.394(5) . ? C21 C26 1.409(5) . ? C22 C23 1.392(5) . ? C22 H22A 0.9500 . ? C23 C24 1.389(8) . ? C23 H23A 0.9500 . ? C24 C25 1.364(7) . ? C24 H24A 0.9500 . ? C25 C26 1.416(5) . ? C25 H25A 0.9500 . ? C27 C28 1.390(5) . ? C27 H27A 0.9500 . ? C28 C29 1.389(5) . ? C28 H28A 0.9500 . ? C29 C30 1.375(6) . ? C29 H29A 0.9500 . ? C30 C31 1.381(5) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C33 1.413(6) . ? C32 H32A 0.9500 . ? C33 C34 1.360(9) . ? C33 H33A 0.9500 . ? C34 C35 1.403(10) . ? C34 H34A 0.9500 . ? C35 C36 1.369(7) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? N1S C6S 1.331(7) . ? N1S C2S 1.339(8) . ? C2S C3S 1.345(9) . ? C2S H2SA 0.9500 . ? C3S C4S 1.403(10) . ? C3S H3SA 0.9500 . ? C4S C5S 1.393(10) . ? C4S H4SA 0.9500 . ? C5S C6S 1.391(8) . ? C5S H5SA 0.9500 . ? C6S H6SA 0.9500 . ? O1S C1S 1.383(6) . ? O1S H1S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? N2S C7S 1.3900 . ? N2S C11S 1.3900 . ? C7S C8S 1.3900 . ? C7S H7S 0.9500 . ? C8S C9S 1.3900 . ? C8S H8S 0.9500 . ? C9S C10S 1.3900 . ? C9S H9S 0.9500 . ? C10S C11S 1.3900 . ? C10S H10S 0.9500 . ? C11S H11S 0.9500 . ? 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 O4 Co1 N3 113.77(10) . 2_656 ? O4 Co1 N2 116.72(9) . . ? N3 Co1 N2 105.33(11) 2_656 . ? O4 Co1 O1 108.81(12) . . ? N3 Co1 O1 106.04(11) 2_656 . ? N2 Co1 O1 105.36(11) . . ? O3 Co2 O2 83.36(11) 2_656 . ? O3 Co2 N5 91.94(12) 2_656 . ? O2 Co2 N5 91.38(11) . . ? O3 Co2 N4 87.73(11) 2_656 2_656 ? O2 Co2 N4 171.07(12) . 2_656 ? N5 Co2 N4 88.38(11) . 2_656 ? O3 Co2 N1 171.21(11) 2_656 . ? O2 Co2 N1 88.23(11) . . ? N5 Co2 N1 90.81(11) . . ? N4 Co2 N1 100.70(11) 2_656 . ? O3 Co2 N6 86.50(14) 2_656 . ? O2 Co2 N6 87.07(12) . . ? N5 Co2 N6 177.92(12) . . ? N4 Co2 N6 92.94(13) 2_656 . ? N1 Co2 N6 90.53(13) . . ? C1 O1 Co1 130.4(3) . . ? C3 O2 Co2 123.0(2) . . ? C26 O3 Co2 124.0(2) . 2_656 ? C37 O4 Co1 122.38(10) . 2_656 ? C37 O4 Co1 122.38(10) . . ? Co1 O4 Co1 115.2(2) 2_656 . ? C9 N1 N2 107.9(3) . . ? C9 N1 Co2 124.2(2) . . ? N2 N1 Co2 126.58(19) . . ? C11 N2 N1 108.0(2) . . ? C11 N2 Co1 126.7(2) . . ? N1 N2 Co1 124.28(19) . . ? C18 N3 N4 107.8(2) . . ? C18 N3 Co1 126.6(2) . 2_656 ? N4 N3 Co1 125.21(19) . 2_656 ? C20 N4 N3 108.6(2) . . ? C20 N4 Co2 123.7(2) . 2_656 ? N3 N4 Co2 127.6(2) . 2_656 ? C27 N5 C31 118.6(3) . . ? C27 N5 Co2 121.1(2) . . ? C31 N5 Co2 120.3(3) . . ? C36 N6 C32 118.2(4) . . ? C36 N6 Co2 121.7(3) . . ? C32 N6 Co2 119.8(3) . . ? O1 C1 O1 125.8(5) . 2_656 ? O1 C1 C2 117.1(3) . . ? O1 C1 C2 117.1(3) 2_656 . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O2 C3 C8 121.8(3) . . ? O2 C3 C4 119.1(4) . . ? C8 C3 C4 119.0(3) . . ? C5 C4 C3 119.5(4) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C6 C5 C4 121.2(4) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C7 120.2(4) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C6 C7 C8 120.1(4) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C3 C8 C7 119.9(3) . . ? C3 C8 C9 119.4(3) . . ? C7 C8 C9 120.6(4) . . ? N1 C9 C10 108.9(3) . . ? N1 C9 C8 122.8(3) . . ? C10 C9 C8 128.2(3) . . ? C11 C10 C9 105.7(3) . . ? C11 C10 H10A 127.1 . . ? C9 C10 H10A 127.1 . . ? N2 C11 C10 109.4(3) . . ? N2 C11 C12 123.0(3) . . ? C10 C11 C12 127.7(3) . . ? C17 C12 C13 118.6(3) . . ? C17 C12 C11 122.5(3) . . ? C13 C12 C11 118.8(3) . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 120.0(3) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C17 C16 C15 119.1(3) . . ? C17 C16 C18 121.9(3) . . ? C15 C16 C18 118.9(3) . . ? C16 C17 C12 121.3(3) . . ? C16 C17 H17A 119.3 . . ? C12 C17 H17A 119.3 . . ? N3 C18 C19 109.1(3) . . ? N3 C18 C16 122.2(3) . . ? C19 C18 C16 128.6(3) . . ? C18 C19 C20 106.1(3) . . ? C18 C19 H19A 127.0 . . ? C20 C19 H19A 127.0 . . ? N4 C20 C19 108.4(3) . . ? N4 C20 C21 124.2(3) . . ? C19 C20 C21 127.3(3) . . ? C22 C21 C26 119.8(3) . . ? C22 C21 C20 121.3(3) . . ? C26 C21 C20 118.8(3) . . ? C23 C22 C21 120.9(4) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C24 C23 C22 119.3(4) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C25 C24 C23 120.7(4) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C24 C25 C26 121.3(4) . . ? C24 C25 H25A 119.3 . . ? C26 C25 H25A 119.3 . . ? O3 C26 C21 123.2(3) . . ? O3 C26 C25 118.8(4) . . ? C21 C26 C25 118.0(4) . . ? N5 C27 C28 122.0(3) . . ? N5 C27 H27A 119.0 . . ? C28 C27 H27A 119.0 . . ? C29 C28 C27 119.0(4) . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? C30 C29 C28 118.9(3) . . ? C30 C29 H29A 120.6 . . ? C28 C29 H29A 120.6 . . ? C29 C30 C31 119.5(3) . . ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? N5 C31 C30 122.0(4) . . ? N5 C31 H31A 119.0 . . ? C30 C31 H31A 119.0 . . ? N6 C32 C33 121.5(5) . . ? N6 C32 H32A 119.2 . . ? C33 C32 H32A 119.2 . . ? C34 C33 C32 118.4(6) . . ? C34 C33 H33A 120.8 . . ? C32 C33 H33A 120.8 . . ? C33 C34 C35 120.1(5) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C36 C35 C34 116.8(6) . . ? C36 C35 H35A 121.6 . . ? C34 C35 H35A 121.6 . . ? N6 C36 C35 124.8(6) . . ? N6 C36 H36A 117.6 . . ? C35 C36 H36A 117.6 . . ? O4 C37 H37A 109.5 . . ? O4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C6S N1S C2S 116.0(5) . . ? N1S C2S C3S 126.1(7) . . ? N1S C2S H2SA 116.9 . . ? C3S C2S H2SA 116.9 . . ? C2S C3S C4S 116.4(6) . . ? C2S C3S H3SA 121.8 . . ? C4S C3S H3SA 121.8 . . ? C5S C4S C3S 120.7(5) . . ? C5S C4S H4SA 119.6 . . ? C3S C4S H4SA 119.6 . . ? C6S C5S C4S 115.9(6) . . ? C6S C5S H5SA 122.0 . . ? C4S C5S H5SA 122.0 . . ? N1S C6S C5S 124.8(6) . . ? N1S C6S H6SA 117.6 . . ? C5S C6S H6SA 117.6 . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C7S N2S C11S 120.0 . . ? N2S C7S C8S 120.0 . . ? N2S C7S H7S 120.0 . . ? C8S C7S H7S 120.0 . . ? C9S C8S C7S 120.0 . . ? C9S C8S H8S 120.0 . . ? C7S C8S H8S 120.0 . . ? C10S C9S C8S 120.0 . . ? C10S C9S H9S 120.0 . . ? C8S C9S H9S 120.0 . . ? C11S C10S C9S 120.0 . . ? C11S C10S H10S 120.0 . . ? C9S C10S H10S 120.0 . . ? C10S C11S N2S 120.0 . . ? C10S C11S H11S 120.0 . . ? N2S C11S H11S 120.0 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 33.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.513 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.106 # Attachment '2995_web_deposit_cif_file_1_OlivierRoubeau_1288354517.cif' data_gac183 _database_code_depnum_ccdc_archive 'CCDC 798853' #TrackingRef '2995_web_deposit_cif_file_1_OlivierRoubeau_1288354517.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C70 H52 Co4 N12 O7), C5 H5 N' _chemical_formula_sum 'C145 H109 Co8 N25 O14' _chemical_formula_weight 2897.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0018 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' H H 0.0000 0.0000 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' N N -0.0031 0.0036 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' O O -0.0041 0.0066 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' Co Co 0.1916 1.0462 'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.133(3) _cell_length_b 23.373(5) _cell_length_c 23.517(5) _cell_angle_alpha 88.14(3) _cell_angle_beta 76.50(3) _cell_angle_gamma 80.03(3) _cell_volume 8492(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 36672 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 25.87 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2964 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details 'HKL2000, Otwinoski, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.73830 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'ESRF BM16' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Single-axis HUBER diffractometer' _diffrn_measurement_method 'phi rotation at various kappa' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 26563 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.74 _reflns_number_total 26563 _reflns_number_gt 17900 _reflns_threshold_expression >2sigma(I) _computing_data_collection MxCube _computing_cell_refinement 'HKL-2000 (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL-2000 (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non-hydrogens were refined anisotropically. Hydrogens were placed geometrically at calculated positions on their carrier atom and refined with a riding model, except for the hydroxide hydrogen on O3 and O3B that are omitted in the structural model as they could not be found in difference Fourier maps nor fixed. Apart from the lattice pyridine molecule, there remained at the end of the refinement one large area of the cell that contained only weak electron density peaks that could not be modeled in any way as solvent molecules. Such diffuse/disordered solvent area is likely related to the observed damaging of the crystals (even in grease at RT) once taken out of their mother liquor. The remaining voids were analyzed and taken into account by PLATON/SQUEEZE that recovered 507 electrons in one large void of 3042 cubic angstrom. These figures would agree with 12 diffuse/disordered pyridine molecules per cell. The SQUEEZE treatment resulted in decrease of R1 by ca. 7%. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.012 0.012 0.002 3042 507 ' ' 2 0.000 0.000 0.500 193 36 ' ' _platon_squeeze_details ; ; _vrf_PLAT029_gac183 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.92 RESPONSE: The low completeness is likely due both to poor diffraction of the crystal that showed rapid damage even in oil and to geometrical limitations of the single-axis goniometer set-up on BM16, with a best resolution of 0.79 angstroms and important blind area. In the present case two full-sphere datasets were collected for two kappa positions of the crystal. ; _vrf_PLAT082_gac183 ; PROBLEM: High R1 Value .................................. 0.16 RESPONSE: Crystals damaged very fast as soon as they were taken out of their mother liquor, even when preventing contact with by using the oil-drop method. Damage continued when kept in grease. Even realizing the mounting as fast as possible, crystals repeatedly showed very poor diffraction, especially at high angles, but also globally. Because there are two similar [Co4] molecules in the asymmetric unit, we attempted to switch the structure to a higher symmetry, without success. PLATON/ADSYM indeed does not indicated any probable higher symmetry space. Overall, we believe the poor quality of the structural model is solely related to the damaging of crystals and disordered solvent area, and that with the crystals at hand this the best model accessible. ; _vrf_RFACG01_gac183 ; PROBLEM: The value of the R factor is > 0.15 RESPONSE: Crystals damaged very fast as soon as they were taken out of their mother liquor, even when preventing contact with by using the oil-drop method. Damage continued when kept in grease. Even realizing the mounting as fast as possible, crystals repeatedly showed very poor diffraction, especially at high angles, but also globally. Because there are two similar [Co4] molecules in the asymmetric unit, we attempted to switch the structure to a higher symmetry, without success. PLATON/ADSYM indeed does not indicated any probable higher symmetry space. Overall, we believe the poor quality of the structural model is solely related to the damaging of crystals and disordered solvent area, and that with the crystals at hand this the best model accessible. ; _vrf_RFACR01_gac183 ; PROBLEM: The value of the weighted R factor is > 0.35 RESPONSE: Crystals damaged very fast as soon as they were taken out of their mother liquor, even when preventing contact with by using the oil-drop method. Damage continued when kept in grease. Even realizing the mounting as fast as possible, crystals repeatedly showed very poor diffraction, especially at high angles, but also globally. Because there are two similar [Co4] molecules in the asymmetric unit, we attempted to switch the structure to a higher symmetry, without success. PLATON/ADSYM indeed does not indicated any probable higher symmetry space. Overall, we believe the poor quality of the structural model is solely related to the damaging of crystals and disordered solvent area, and that with the crystals at hand this is the best model accessible. ; _vrf_PLAT084_gac183 ; PROBLEM: High wR2 Value ................................. 0.44 RESPONSE: Crystals damaged very fast as soon as they were taken out of their mother liquor, even when preventing contact with by using the oil-drop method. Damage continued when kept in grease. Even realizing the mounting as fast as possible, crystals repeatedly showed very poor diffraction, especially at high angles, but also globally. Because there are two similar [Co4] molecules in the asymmetric unit, we attempted to switch the structure to a higher symmetry, without success. PLATON/ADSYM indeed does not indicated any probable higher symmetry space. Overall, we believe the poor quality of the structural model is solely related to the damaging of crystals and disordered solvent area, and that with the crystals at hand this is the best model accessible. ; _vrf_DIFMX02_gac183 ; PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75 RESPONSE: The two largest residual electron density peaks remaining at the end of the refinement were close to the Co3B and Co3 atoms. ; _vrf_PLAT097_gac183 ; PROBLEM: Large Reported Max. (Positive) Residual Density 2.49 eA-3 RESPONSE: The two largest residual electron density peaks remaining at the end of the refinement were close to the Co3B and Co3 atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26563 _refine_ls_number_parameters 1717 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1792 _refine_ls_R_factor_gt 0.1561 _refine_ls_wR_factor_ref 0.4437 _refine_ls_wR_factor_gt 0.4118 _refine_ls_goodness_of_fit_ref 1.741 _refine_ls_restrained_S_all 1.741 _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 1.07548(8) 0.15742(5) 0.13262(5) 0.067 Uani 1 1 d . . . Co2 Co 0.87694(8) 0.24746(5) 0.21292(4) 0.063 Uani 1 1 d . . . Co3 Co 0.76336(8) 0.35789(5) 0.28052(4) 0.065 Uani 1 1 d . . . Co4 Co 0.72800(8) 0.50727(5) 0.33397(4) 0.065 Uani 1 1 d . . . O1 O 0.7596(4) 0.2269(3) 0.2357(2) 0.068 Uani 1 1 d . . . O2 O 0.6834(4) 0.3020(2) 0.2893(2) 0.067 Uani 1 1 d . . . O3 O 0.8784(4) 0.3257(3) 0.2381(2) 0.078 Uani 1 1 d . . . O4 O 1.1517(4) 0.1655(3) 0.0599(2) 0.076 Uani 1 1 d . . . O5 O 0.7146(4) 0.5825(3) 0.2985(2) 0.076 Uani 1 1 d . . . O6 O 1.1753(4) 0.1171(3) 0.1556(3) 0.071 Uani 1 1 d . . . O7 O 0.7782(4) 0.5450(3) 0.3845(2) 0.080 Uani 1 1 d . . . N1 N 0.9831(5) 0.1988(3) 0.0989(3) 0.067 Uani 1 1 d . . . N2 N 0.9086(5) 0.2349(3) 0.1287(3) 0.067 Uani 1 1 d . . . N3 N 0.7024(4) 0.4266(3) 0.2476(3) 0.058 Uani 1 1 d . . . N4 N 0.6755(4) 0.4790(3) 0.2753(3) 0.063 Uani 1 1 d . . . N5 N 1.0119(4) 0.1462(3) 0.2113(3) 0.065 Uani 1 1 d . . . N6 N 0.9467(5) 0.1831(3) 0.2453(3) 0.066 Uani 1 1 d . . . N7 N 0.7607(5) 0.3816(3) 0.3602(3) 0.071 Uani 1 1 d . . . N8 N 0.7484(5) 0.4378(3) 0.3796(3) 0.075 Uani 1 1 d . . . N9 N 1.0473(5) 0.0862(3) 0.1082(3) 0.074 Uani 1 1 d . . . N10 N 1.1015(5) 0.2302(3) 0.1571(3) 0.069 Uani 1 1 d . . . N11 N 0.8397(5) 0.4878(3) 0.2779(3) 0.068 Uani 1 1 d . . . N12 N 0.6159(5) 0.5262(3) 0.3847(3) 0.071 Uani 1 1 d . . . C1 C 0.6927(6) 0.2523(4) 0.2678(4) 0.075 Uani 1 1 d . . . C2 C 0.6152(6) 0.2209(5) 0.2826(5) 0.088 Uani 1 1 d . . . H2A H 0.6309 0.1827 0.2634 0.131 Uiso 1 1 calc R . . H2B H 0.5668 0.2437 0.2690 0.131 Uiso 1 1 calc R . . H2C H 0.5982 0.2160 0.3251 0.131 Uiso 1 1 calc R . . C3 C 1.1349(6) 0.1554(4) 0.0088(4) 0.075 Uani 1 1 d . . . C4 C 1.2032(6) 0.1300(4) -0.0372(4) 0.080 Uani 1 1 d . . . H4A H 1.2595 0.1191 -0.0303 0.097 Uiso 1 1 calc R . . C5 C 1.1906(7) 0.1209(5) -0.0909(5) 0.097 Uani 1 1 d . . . H5A H 1.2387 0.1056 -0.1212 0.116 Uiso 1 1 calc R . . C6 C 1.1093(7) 0.1335(5) -0.1025(5) 0.094 Uani 1 1 d . . . H6A H 1.1008 0.1253 -0.1398 0.113 Uiso 1 1 calc R . . C7 C 1.0385(6) 0.1593(4) -0.0572(4) 0.072 Uani 1 1 d . . . H7A H 0.9823 0.1694 -0.0644 0.087 Uiso 1 1 calc R . . C8 C 1.0520(5) 0.1695(4) -0.0024(4) 0.067 Uani 1 1 d . . . C9 C 0.9810(5) 0.1982(3) 0.0421(3) 0.062 Uani 1 1 d . . . C10 C 0.9056(6) 0.2327(4) 0.0346(4) 0.077 Uani 1 1 d . . . H10A H 0.8877 0.2393 -0.0011 0.092 Uiso 1 1 calc R . . C11 C 0.8608(5) 0.2561(4) 0.0893(4) 0.065 Uani 1 1 d . . . C12 C 0.7763(5) 0.2944(4) 0.1061(4) 0.064 Uani 1 1 d . . . C13 C 0.7093(6) 0.2847(4) 0.0842(4) 0.075 Uani 1 1 d . . . H13A H 0.7177 0.2528 0.0582 0.090 Uiso 1 1 calc R . . C14 C 0.6267(6) 0.3209(4) 0.0992(4) 0.076 Uani 1 1 d . . . H14A H 0.5815 0.3151 0.0815 0.091 Uiso 1 1 calc R . . C15 C 0.6139(6) 0.3650(4) 0.1402(4) 0.071 Uani 1 1 d . . . H15A H 0.5578 0.3872 0.1537 0.085 Uiso 1 1 calc R . . C16 C 0.6805(5) 0.3765(3) 0.1610(3) 0.062 Uani 1 1 d . . . C17 C 0.7638(5) 0.3415(3) 0.1440(3) 0.063 Uani 1 1 d . . . H17A H 0.8107 0.3502 0.1584 0.076 Uiso 1 1 calc R . . C18 C 0.6664(5) 0.4273(4) 0.2005(4) 0.068 Uani 1 1 d . . . C19 C 0.6170(5) 0.4800(4) 0.1994(4) 0.068 Uani 1 1 d . . . H19A H 0.5823 0.4925 0.1723 0.082 Uiso 1 1 calc R . . C20 C 0.6262(5) 0.5118(4) 0.2441(4) 0.064 Uani 1 1 d . . . C21 C 0.5949(5) 0.5758(4) 0.2570(4) 0.065 Uani 1 1 d . . . C22 C 0.5184(6) 0.6039(4) 0.2392(4) 0.077 Uani 1 1 d . . . H22A H 0.4858 0.5819 0.2223 0.092 Uiso 1 1 calc R . . C23 C 0.4936(6) 0.6618(4) 0.2468(4) 0.073 Uani 1 1 d . . . H23A H 0.4445 0.6813 0.2340 0.087 Uiso 1 1 calc R . . C24 C 0.5414(6) 0.6932(5) 0.2742(4) 0.083 Uani 1 1 d . . . H24A H 0.5234 0.7338 0.2806 0.099 Uiso 1 1 calc R . . C25 C 0.6108(6) 0.6665(4) 0.2907(4) 0.072 Uani 1 1 d . . . H25A H 0.6419 0.6890 0.3083 0.087 Uiso 1 1 calc R . . C26 C 0.6405(5) 0.6073(4) 0.2837(4) 0.063 Uani 1 1 d . . . C27 C 1.1760(6) 0.0667(4) 0.1819(4) 0.078 Uani 1 1 d . . . C28 C 1.2501(7) 0.0260(5) 0.1698(5) 0.086 Uani 1 1 d . . . H28A H 1.2979 0.0349 0.1409 0.104 Uiso 1 1 calc R . . C29 C 1.2599(8) -0.0280(5) 0.1973(5) 0.102 Uani 1 1 d . . . H29A H 1.3129 -0.0546 0.1883 0.123 Uiso 1 1 calc R . . C30 C 1.1866(6) -0.0413(4) 0.2396(4) 0.080 Uani 1 1 d . . . H30A H 1.1893 -0.0782 0.2578 0.096 Uiso 1 1 calc R . . C31 C 1.1116(6) -0.0005(4) 0.2539(5) 0.084 Uani 1 1 d . . . H31A H 1.0646 -0.0090 0.2838 0.101 Uiso 1 1 calc R . . C32 C 1.1032(6) 0.0535(4) 0.2254(4) 0.078 Uani 1 1 d . . . C33 C 1.0293(6) 0.0994(4) 0.2456(4) 0.080 Uani 1 1 d . . . C34 C 0.9776(6) 0.1073(4) 0.3006(4) 0.073 Uani 1 1 d . . . H34A H 0.9778 0.0818 0.3329 0.087 Uiso 1 1 calc R . . C35 C 0.9247(6) 0.1605(4) 0.2993(4) 0.071 Uani 1 1 d . . . C36 C 0.8582(5) 0.1909(4) 0.3463(4) 0.064 Uani 1 1 d . . . C37 C 0.8016(6) 0.1607(4) 0.3834(4) 0.080 Uani 1 1 d . . . H37A H 0.8079 0.1197 0.3801 0.096 Uiso 1 1 calc R . . C38 C 0.7344(7) 0.1916(5) 0.4263(5) 0.089 Uani 1 1 d . . . H38A H 0.6945 0.1709 0.4511 0.107 Uiso 1 1 calc R . . C39 C 0.7243(6) 0.2514(4) 0.4338(4) 0.073 Uani 1 1 d . . . H39A H 0.6787 0.2713 0.4633 0.088 Uiso 1 1 calc R . . C40 C 0.7818(6) 0.2808(4) 0.3975(4) 0.072 Uani 1 1 d . . . C41 C 0.8492(5) 0.2507(4) 0.3540(4) 0.066 Uani 1 1 d . . . H41A H 0.8892 0.2715 0.3296 0.079 Uiso 1 1 calc R . . C42 C 0.7713(6) 0.3446(4) 0.4049(4) 0.072 Uani 1 1 d . . . C43 C 0.7722(5) 0.3765(4) 0.4525(4) 0.067 Uani 1 1 d . . . H43A H 0.7799 0.3619 0.4895 0.081 Uiso 1 1 calc R . . C44 C 0.7597(5) 0.4344(4) 0.4361(4) 0.070 Uani 1 1 d . . . C45 C 0.7542(6) 0.4869(4) 0.4701(4) 0.073 Uani 1 1 d . . . C46 C 0.7433(6) 0.4855(4) 0.5310(4) 0.078 Uani 1 1 d . . . H46A H 0.7425 0.4489 0.5498 0.093 Uiso 1 1 calc R . . C47 C 0.7337(6) 0.5334(4) 0.5648(5) 0.087 Uani 1 1 d . . . H47A H 0.7290 0.5304 0.6058 0.104 Uiso 1 1 calc R . . C48 C 0.7311(6) 0.5889(4) 0.5362(4) 0.081 Uani 1 1 d . . . H48A H 0.7221 0.6236 0.5584 0.097 Uiso 1 1 calc R . . C49 C 0.7415(6) 0.5911(4) 0.4774(4) 0.080 Uani 1 1 d . . . H49A H 0.7372 0.6281 0.4593 0.096 Uiso 1 1 calc R . . C50 C 0.7588(6) 0.5399(4) 0.4410(5) 0.083 Uani 1 1 d . . . C51 C 0.9673(5) 0.0766(4) 0.1202(3) 0.062 Uani 1 1 d . . . H51A H 0.9231 0.1048 0.1424 0.074 Uiso 1 1 calc R . . C52 C 0.9444(7) 0.0257(5) 0.1014(5) 0.085 Uani 1 1 d . . . H52A H 0.8865 0.0187 0.1111 0.102 Uiso 1 1 calc R . . C53 C 1.0105(6) -0.0127(5) 0.0682(4) 0.086 Uani 1 1 d . . . H53A H 0.9970 -0.0468 0.0541 0.103 Uiso 1 1 calc R . . C54 C 1.0956(7) -0.0045(5) 0.0541(5) 0.089 Uani 1 1 d . . . H54A H 1.1406 -0.0320 0.0316 0.106 Uiso 1 1 calc R . . C55 C 1.1107(5) 0.0461(4) 0.0749(4) 0.066 Uani 1 1 d . . . H55A H 1.1683 0.0536 0.0658 0.079 Uiso 1 1 calc R . . C56 C 1.1000(6) 0.2759(4) 0.1224(4) 0.077 Uani 1 1 d . . . H56A H 1.0816 0.2732 0.0872 0.092 Uiso 1 1 calc R . . C57 C 1.1240(6) 0.3276(4) 0.1347(4) 0.082 Uani 1 1 d . . . H57A H 1.1196 0.3598 0.1092 0.098 Uiso 1 1 calc R . . C58 C 1.1536(7) 0.3315(5) 0.1833(5) 0.087 Uani 1 1 d . . . H58A H 1.1738 0.3655 0.1914 0.104 Uiso 1 1 calc R . . C59 C 1.1540(7) 0.2856(5) 0.2206(5) 0.090 Uani 1 1 d . . . H59A H 1.1696 0.2879 0.2569 0.108 Uiso 1 1 calc R . . C60 C 1.1307(6) 0.2352(4) 0.2036(4) 0.082 Uani 1 1 d . . . H60A H 1.1365 0.2020 0.2278 0.098 Uiso 1 1 calc R . . C61 C 0.8462(6) 0.5032(4) 0.2210(4) 0.073 Uani 1 1 d . . . H61A H 0.7969 0.5235 0.2091 0.087 Uiso 1 1 calc R . . C62 C 0.9257(6) 0.4893(4) 0.1792(4) 0.078 Uani 1 1 d . . . H62A H 0.9301 0.5015 0.1399 0.093 Uiso 1 1 calc R . . C63 C 0.9954(7) 0.4586(5) 0.1956(5) 0.085 Uani 1 1 d . . . H63A H 1.0487 0.4490 0.1676 0.103 Uiso 1 1 calc R . . C64 C 0.9891(6) 0.4410(4) 0.2537(4) 0.082 Uani 1 1 d . . . H64A H 1.0368 0.4187 0.2660 0.099 Uiso 1 1 calc R . . C65 C 0.9094(6) 0.4579(4) 0.2927(4) 0.075 Uani 1 1 d . . . H65A H 0.9045 0.4472 0.3325 0.090 Uiso 1 1 calc R . . C66 C 0.5627(5) 0.4867(4) 0.3966(4) 0.068 Uani 1 1 d . . . H66A H 0.5824 0.4483 0.3815 0.082 Uiso 1 1 calc R . . C67 C 0.4797(6) 0.5016(5) 0.4307(4) 0.085 Uani 1 1 d . . . H67A H 0.4414 0.4742 0.4363 0.102 Uiso 1 1 calc R . . C68 C 0.4518(6) 0.5556(4) 0.4565(4) 0.080 Uani 1 1 d . . . H68A H 0.3954 0.5648 0.4812 0.097 Uiso 1 1 calc R . . C69 C 0.5039(5) 0.5951(4) 0.4469(4) 0.072 Uani 1 1 d . . . H69A H 0.4860 0.6330 0.4636 0.086 Uiso 1 1 calc R . . C70 C 0.5877(6) 0.5773(4) 0.4105(4) 0.079 Uani 1 1 d . . . H70A H 0.6264 0.6045 0.4043 0.094 Uiso 1 1 calc R . . Co1B Co -0.12029(8) 0.86701(5) 0.39778(5) 0.069 Uani 1 1 d . . . Co2B Co 0.07919(8) 0.78262(5) 0.31251(4) 0.065 Uani 1 1 d . . . Co3B Co 0.19516(8) 0.67372(5) 0.24246(4) 0.064 Uani 1 1 d . . . Co4B Co 0.23991(7) 0.52541(5) 0.18440(4) 0.061 Uani 1 1 d . . . O1B O 0.1940(4) 0.8062(3) 0.2875(2) 0.079 Uani 1 1 d . . . O2B O 0.2736(4) 0.7304(2) 0.2339(2) 0.065 Uani 1 1 d . . . O3B O 0.0804(4) 0.7050(3) 0.2882(3) 0.074 Uani 1 1 d . . . O4B O -0.1915(4) 0.8555(3) 0.4714(2) 0.076 Uani 1 1 d . . . O5B O 0.2566(3) 0.4502(2) 0.2161(2) 0.059 Uani 1 1 d . . . O6B O -0.2248(4) 0.9022(3) 0.3784(3) 0.090 Uani 1 1 d . . . O7B O 0.1902(4) 0.4883(2) 0.1321(2) 0.065 Uani 1 1 d . . . N1B N -0.0224(5) 0.8275(3) 0.4278(3) 0.066 Uani 1 1 d . . . N2B N 0.0512(4) 0.7941(3) 0.3968(3) 0.062 Uani 1 1 d . . . N3B N 0.2601(4) 0.6063(3) 0.2738(3) 0.065 Uani 1 1 d . . . N4B N 0.2875(5) 0.5535(3) 0.2450(3) 0.069 Uani 1 1 d . . . N5B N -0.0639(5) 0.8817(3) 0.3182(4) 0.085 Uani 1 1 d . . . N6B N 0.0056(5) 0.8456(3) 0.2835(3) 0.069 Uani 1 1 d . . . N7B N 0.1999(5) 0.6533(3) 0.1617(3) 0.075 Uani 1 1 d . . . N8B N 0.2169(4) 0.5956(3) 0.1400(3) 0.061 Uani 1 1 d . . . N9B N -0.0997(6) 0.9399(3) 0.4241(3) 0.083 Uani 1 1 d . . . N10B N -0.1419(5) 0.7936(3) 0.3728(4) 0.085 Uani 1 1 d . . . N11B N 0.3531(5) 0.5116(3) 0.1339(3) 0.068 Uani 1 1 d . . . N12B N 0.1280(4) 0.5414(3) 0.2389(3) 0.064 Uani 1 1 d . . . C1B C 0.2643(5) 0.7809(4) 0.2548(4) 0.064 Uani 1 1 d . . . C2B C 0.3395(7) 0.8119(5) 0.2426(5) 0.098 Uani 1 1 d . . . H2BA H 0.3891 0.7879 0.2169 0.148 Uiso 1 1 calc R . . H2BB H 0.3544 0.8195 0.2794 0.148 Uiso 1 1 calc R . . H2BC H 0.3247 0.8488 0.2233 0.148 Uiso 1 1 calc R . . C3B C -0.1738(5) 0.8648(4) 0.5223(4) 0.070 Uani 1 1 d . . . C4B C -0.2435(7) 0.8887(5) 0.5693(5) 0.087 Uani 1 1 d . . . H4BA H -0.3000 0.8989 0.5625 0.105 Uiso 1 1 calc R . . C5B C -0.2312(7) 0.8973(5) 0.6230(5) 0.094 Uani 1 1 d . . . H5BA H -0.2794 0.9112 0.6540 0.113 Uiso 1 1 calc R . . C6B C -0.1473(7) 0.8858(5) 0.6334(5) 0.089 Uani 1 1 d . . . H6BA H -0.1375 0.8929 0.6706 0.107 Uiso 1 1 calc R . . C7B C -0.0796(6) 0.8636(4) 0.5872(4) 0.070 Uani 1 1 d . . . H7BA H -0.0229 0.8547 0.5939 0.084 Uiso 1 1 calc R . . C8B C -0.0905(5) 0.8537(4) 0.5313(4) 0.064 Uani 1 1 d . . . C9B C -0.0175(5) 0.8258(4) 0.4849(4) 0.066 Uani 1 1 d . . . C10B C 0.0619(5) 0.7949(3) 0.4903(4) 0.064 Uani 1 1 d . . . H10B H 0.0834 0.7883 0.5247 0.077 Uiso 1 1 calc R . . C11B C 0.1029(5) 0.7756(3) 0.4334(3) 0.062 Uani 1 1 d . . . C12B C 0.1889(5) 0.7388(3) 0.4133(3) 0.062 Uani 1 1 d . . . C13B C 0.2555(6) 0.7535(4) 0.4318(4) 0.081 Uani 1 1 d . . . H13B H 0.2469 0.7856 0.4575 0.097 Uiso 1 1 calc R . . C14B C 0.3392(6) 0.7194(4) 0.4116(4) 0.082 Uani 1 1 d . . . H14B H 0.3876 0.7302 0.4224 0.098 Uiso 1 1 calc R . . C15B C 0.3509(6) 0.6715(4) 0.3771(4) 0.073 Uani 1 1 d . . . H15B H 0.4065 0.6482 0.3656 0.087 Uiso 1 1 calc R . . C16B C 0.2818(5) 0.6569(4) 0.3588(4) 0.067 Uani 1 1 d . . . C17B C 0.2006(5) 0.6894(3) 0.3782(3) 0.061 Uani 1 1 d . . . H17B H 0.1522 0.6782 0.3677 0.073 Uiso 1 1 calc R . . C18B C 0.2956(5) 0.6056(4) 0.3193(4) 0.064 Uani 1 1 d . . . C19B C 0.3489(5) 0.5518(3) 0.3206(4) 0.064 Uani 1 1 d . . . H19B H 0.3839 0.5399 0.3477 0.076 Uiso 1 1 calc R . . C20B C 0.3408(5) 0.5197(4) 0.2750(4) 0.065 Uani 1 1 d . . . C21B C 0.3718(5) 0.4587(4) 0.2625(4) 0.066 Uani 1 1 d . . . C22B C 0.4438(5) 0.4297(4) 0.2828(4) 0.067 Uani 1 1 d . . . H22B H 0.4743 0.4517 0.3015 0.080 Uiso 1 1 calc R . . C23B C 0.4715(6) 0.3701(4) 0.2763(4) 0.073 Uani 1 1 d . . . H23B H 0.5199 0.3509 0.2900 0.087 Uiso 1 1 calc R . . C24B C 0.4254(6) 0.3405(5) 0.2492(4) 0.083 Uani 1 1 d . . . H24B H 0.4411 0.2994 0.2457 0.100 Uiso 1 1 calc R . . C25B C 0.3583(6) 0.3671(4) 0.2272(4) 0.078 Uani 1 1 d . . . H25B H 0.3308 0.3445 0.2068 0.093 Uiso 1 1 calc R . . C26B C 0.3286(5) 0.4261(4) 0.2336(4) 0.066 Uani 1 1 d . . . C27B C -0.2337(7) 0.9545(5) 0.3512(5) 0.088 Uani 1 1 d . . . C28B C -0.3097(9) 0.9939(6) 0.3695(7) 0.124 Uani 1 1 d . . . H28B H -0.3553 0.9848 0.4002 0.149 Uiso 1 1 calc R . . C29B C -0.3168(8) 1.0487(5) 0.3402(5) 0.101 Uani 1 1 d . . . H29B H -0.3690 1.0755 0.3529 0.121 Uiso 1 1 calc R . . C30B C -0.2557(9) 1.0656(7) 0.2962(7) 0.125 Uani 1 1 d . . . H30B H -0.2643 1.1020 0.2774 0.150 Uiso 1 1 calc R . . C31B C -0.1767(8) 1.0244(5) 0.2798(5) 0.103 Uani 1 1 d . . . H31B H -0.1302 1.0345 0.2505 0.123 Uiso 1 1 calc R . . C32B C -0.1665(6) 0.9693(5) 0.3062(5) 0.084 Uani 1 1 d . . . C33B C -0.0908(6) 0.9267(4) 0.2858(4) 0.071 Uani 1 1 d . . . C34B C -0.0376(6) 0.9191(4) 0.2286(4) 0.078 Uani 1 1 d . . . H34B H -0.0402 0.9447 0.1966 0.093 Uiso 1 1 calc R . . C35B C 0.0181(5) 0.8679(4) 0.2282(4) 0.069 Uani 1 1 d . . . C36B C 0.0872(5) 0.8398(4) 0.1789(4) 0.068 Uani 1 1 d . . . C37B C 0.1319(6) 0.8739(4) 0.1386(4) 0.076 Uani 1 1 d . . . H37B H 0.1191 0.9150 0.1423 0.092 Uiso 1 1 calc R . . C38B C 0.1948(6) 0.8482(4) 0.0934(4) 0.078 Uani 1 1 d . . . H38B H 0.2268 0.8720 0.0665 0.093 Uiso 1 1 calc R . . C39B C 0.2146(6) 0.7865(4) 0.0850(4) 0.074 Uani 1 1 d . . . H39B H 0.2588 0.7692 0.0531 0.089 Uiso 1 1 calc R . . C40B C 0.1669(5) 0.7528(4) 0.1249(4) 0.066 Uani 1 1 d . . . C41B C 0.1036(5) 0.7791(4) 0.1709(4) 0.066 Uani 1 1 d . . . H41B H 0.0703 0.7558 0.1977 0.079 Uiso 1 1 calc R . . C42B C 0.1870(5) 0.6897(4) 0.1171(4) 0.068 Uani 1 1 d . . . C43B C 0.1994(5) 0.6563(4) 0.0672(4) 0.071 Uani 1 1 d . . . H43B H 0.1975 0.6700 0.0290 0.085 Uiso 1 1 calc R . . C44B C 0.2150(5) 0.5989(4) 0.0842(4) 0.062 Uani 1 1 d . . . C45B C 0.2261(5) 0.5475(4) 0.0468(4) 0.065 Uani 1 1 d . . . C46B C 0.2447(5) 0.5495(4) -0.0129(4) 0.065 Uani 1 1 d . . . H46B H 0.2533 0.5857 -0.0307 0.078 Uiso 1 1 calc R . . C47B C 0.2520(6) 0.5034(4) -0.0486(4) 0.073 Uani 1 1 d . . . H47B H 0.2639 0.5069 -0.0900 0.088 Uiso 1 1 calc R . . C48B C 0.2408(6) 0.4498(4) -0.0203(4) 0.077 Uani 1 1 d . . . H48B H 0.2459 0.4161 -0.0433 0.092 Uiso 1 1 calc R . . C49B C 0.2231(6) 0.4455(4) 0.0387(4) 0.078 Uani 1 1 d . . . H49B H 0.2175 0.4088 0.0562 0.093 Uiso 1 1 calc R . . C50B C 0.2128(5) 0.4943(4) 0.0746(4) 0.063 Uani 1 1 d . . . C51B C -0.0201(5) 0.9543(4) 0.4090(4) 0.064 Uani 1 1 d . . . H51B H 0.0265 0.9282 0.3861 0.077 Uiso 1 1 calc R . . C52B C -0.0054(6) 1.0085(4) 0.4274(4) 0.072 Uani 1 1 d . . . H52B H 0.0511 1.0179 0.4172 0.087 Uiso 1 1 calc R . . C53B C -0.0705(6) 1.0457(5) 0.4586(5) 0.087 Uani 1 1 d . . . H53B H -0.0606 1.0816 0.4713 0.104 Uiso 1 1 calc R . . C54B C -0.1536(6) 1.0317(4) 0.4726(4) 0.080 Uani 1 1 d . . . H54B H -0.2015 1.0586 0.4930 0.096 Uiso 1 1 calc R . . C55B C -0.1649(7) 0.9762(5) 0.4556(5) 0.086 Uani 1 1 d . . . H55B H -0.2203 0.9651 0.4672 0.103 Uiso 1 1 calc R . . C56B C -0.1695(7) 0.7891(5) 0.3268(5) 0.100 Uani 1 1 d . . . H56B H -0.1741 0.8222 0.3024 0.119 Uiso 1 1 calc R . . C57B C -0.1938(7) 0.7382(5) 0.3095(5) 0.098 Uani 1 1 d . . . H57B H -0.2150 0.7371 0.2753 0.117 Uiso 1 1 calc R . . C58B C -0.1850(7) 0.6896(5) 0.3453(5) 0.099 Uani 1 1 d . . . H58B H -0.2036 0.6551 0.3367 0.119 Uiso 1 1 calc R . . C59B C -0.1508(7) 0.6916(5) 0.3913(5) 0.094 Uani 1 1 d . . . H59B H -0.1402 0.6582 0.4144 0.113 Uiso 1 1 calc R . . C60B C -0.1307(6) 0.7464(4) 0.4044(5) 0.083 Uani 1 1 d . . . H60B H -0.1081 0.7489 0.4379 0.100 Uiso 1 1 calc R . . C61B C 0.4046(5) 0.5516(4) 0.1251(3) 0.063 Uani 1 1 d . . . H61B H 0.3842 0.5884 0.1438 0.075 Uiso 1 1 calc R . . C62B C 0.4867(6) 0.5405(4) 0.0895(4) 0.080 Uani 1 1 d . . . H62B H 0.5214 0.5701 0.0836 0.096 Uiso 1 1 calc R . . C63B C 0.5182(6) 0.4893(4) 0.0632(4) 0.081 Uani 1 1 d . . . H63B H 0.5748 0.4827 0.0386 0.097 Uiso 1 1 calc R . . C64B C 0.4693(6) 0.4461(4) 0.0714(4) 0.080 Uani 1 1 d . . . H64B H 0.4912 0.4090 0.0535 0.096 Uiso 1 1 calc R . . C65B C 0.3866(5) 0.4587(3) 0.1067(3) 0.061 Uani 1 1 d . . . H65B H 0.3514 0.4294 0.1123 0.074 Uiso 1 1 calc R . . C66B C 0.0581(6) 0.5722(4) 0.2239(4) 0.073 Uani 1 1 d . . . H66B H 0.0626 0.5844 0.1845 0.088 Uiso 1 1 calc R . . C67B C -0.0201(7) 0.5867(4) 0.2638(4) 0.084 Uani 1 1 d . . . H67B H -0.0684 0.6091 0.2523 0.101 Uiso 1 1 calc R . . C68B C -0.0269(6) 0.5682(4) 0.3202(4) 0.078 Uani 1 1 d . . . H68B H -0.0803 0.5778 0.3482 0.094 Uiso 1 1 calc R . . C69B C 0.0432(6) 0.5357(4) 0.3366(5) 0.084 Uani 1 1 d . . . H69B H 0.0399 0.5218 0.3754 0.101 Uiso 1 1 calc R . . C70B C 0.1171(6) 0.5245(4) 0.2945(4) 0.074 Uani 1 1 d . . . H70B H 0.1660 0.5026 0.3057 0.088 Uiso 1 1 calc R . . N1S N 0.0846(5) 0.3793(3) 0.3540(3) 0.093 Uani 1 1 d G . . C1S C 0.0331(4) 0.3371(4) 0.3720(4) 0.137 Uani 1 1 d G . . H1S H -0.0275 0.3463 0.3755 0.164 Uiso 1 1 calc R . . C2S C 0.0705(5) 0.2816(3) 0.3849(5) 0.154 Uani 1 1 d G . . H2S H 0.0353 0.2527 0.3972 0.185 Uiso 1 1 calc R . . C3S C 0.1593(5) 0.2681(3) 0.3798(4) 0.111 Uani 1 1 d G . . H3S H 0.1848 0.2301 0.3887 0.133 Uiso 1 1 calc R . . C4S C 0.2108(4) 0.3103(3) 0.3618(4) 0.100 Uani 1 1 d G . . H4S H 0.2715 0.3011 0.3583 0.120 Uiso 1 1 calc R . . C5S C 0.1734(4) 0.3659(3) 0.3489(4) 0.148 Uani 1 1 d G . . H5S H 0.2086 0.3947 0.3366 0.178 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 0.085 0.063 0.048 0.000 -0.020 0.000 Co2 0.086 0.061 0.042 0.001 -0.020 -0.002 Co3 0.087 0.065 0.042 0.000 -0.020 0.001 Co4 0.086 0.067 0.040 -0.002 -0.016 -0.004 O1 0.071 0.076 0.055 -0.005 -0.018 -0.005 O2 0.079 0.064 0.055 -0.001 -0.018 0.002 O3 0.104 0.083 0.038 -0.005 -0.013 0.001 O4 0.099 0.075 0.049 -0.003 -0.017 0.003 O5 0.097 0.067 0.057 -0.008 -0.014 -0.003 O6 0.069 0.070 0.079 0.010 -0.028 -0.010 O7 0.122 0.085 0.037 0.002 -0.025 -0.021 N1 0.097 0.054 0.039 -0.007 -0.009 0.006 N2 0.089 0.065 0.045 -0.003 -0.017 -0.008 N3 0.087 0.047 0.045 -0.001 -0.028 -0.006 N4 0.076 0.059 0.057 0.007 -0.023 -0.005 N5 0.071 0.067 0.054 0.005 -0.018 0.002 N6 0.085 0.068 0.047 -0.002 -0.030 0.000 N7 0.108 0.056 0.043 -0.004 -0.020 0.010 N8 0.094 0.085 0.045 -0.003 -0.014 -0.018 N9 0.101 0.075 0.038 -0.007 -0.012 0.002 N10 0.089 0.068 0.047 -0.006 -0.021 0.005 N11 0.078 0.074 0.057 0.002 -0.023 -0.017 N12 0.100 0.074 0.039 -0.012 -0.020 -0.007 C1 0.075 0.075 0.075 0.001 -0.017 -0.013 C2 0.088 0.088 0.088 0.001 -0.020 -0.015 C3 0.075 0.075 0.075 0.001 -0.017 -0.013 C4 0.080 0.080 0.080 0.001 -0.019 -0.014 C5 0.097 0.097 0.097 0.001 -0.022 -0.017 C6 0.094 0.094 0.094 0.001 -0.022 -0.016 C7 0.072 0.072 0.072 0.001 -0.017 -0.012 C8 0.067 0.067 0.067 0.001 -0.016 -0.011 C9 0.062 0.062 0.062 0.001 -0.014 -0.011 C10 0.077 0.077 0.077 0.001 -0.018 -0.013 C11 0.065 0.065 0.065 0.001 -0.015 -0.011 C12 0.064 0.064 0.064 0.001 -0.015 -0.011 C13 0.075 0.075 0.075 0.001 -0.017 -0.013 C14 0.076 0.076 0.076 0.001 -0.018 -0.013 C15 0.071 0.071 0.071 0.001 -0.016 -0.012 C16 0.062 0.062 0.062 0.001 -0.014 -0.010 C17 0.063 0.063 0.063 0.001 -0.015 -0.011 C18 0.068 0.068 0.068 0.001 -0.016 -0.012 C19 0.068 0.068 0.068 0.001 -0.016 -0.012 C20 0.064 0.064 0.064 0.001 -0.015 -0.011 C21 0.065 0.065 0.065 0.001 -0.015 -0.011 C22 0.077 0.077 0.077 0.001 -0.018 -0.013 C23 0.073 0.073 0.073 0.001 -0.017 -0.012 C24 0.083 0.083 0.083 0.001 -0.019 -0.014 C25 0.072 0.072 0.072 0.001 -0.017 -0.012 C26 0.063 0.063 0.063 0.001 -0.015 -0.011 C27 0.078 0.078 0.078 0.001 -0.018 -0.013 C28 0.086 0.086 0.086 0.001 -0.020 -0.015 C29 0.102 0.102 0.102 0.001 -0.024 -0.017 C30 0.080 0.080 0.080 0.001 -0.019 -0.014 C31 0.084 0.084 0.084 0.001 -0.019 -0.014 C32 0.078 0.078 0.078 0.001 -0.018 -0.013 C33 0.080 0.080 0.080 0.001 -0.019 -0.014 C34 0.073 0.073 0.073 0.001 -0.017 -0.012 C35 0.071 0.071 0.071 0.001 -0.016 -0.012 C36 0.064 0.064 0.064 0.001 -0.015 -0.011 C37 0.080 0.080 0.080 0.001 -0.018 -0.014 C38 0.089 0.089 0.089 0.001 -0.021 -0.015 C39 0.073 0.073 0.073 0.001 -0.017 -0.012 C40 0.072 0.072 0.072 0.001 -0.017 -0.012 C41 0.066 0.066 0.066 0.001 -0.015 -0.011 C42 0.072 0.072 0.072 0.001 -0.017 -0.012 C43 0.067 0.067 0.067 0.001 -0.016 -0.011 C44 0.070 0.070 0.070 0.001 -0.016 -0.012 C45 0.073 0.073 0.073 0.001 -0.017 -0.012 C46 0.078 0.078 0.078 0.001 -0.018 -0.013 C47 0.087 0.087 0.087 0.001 -0.020 -0.015 C48 0.081 0.081 0.081 0.001 -0.019 -0.014 C49 0.080 0.080 0.080 0.001 -0.019 -0.014 C50 0.083 0.083 0.083 0.001 -0.019 -0.014 C51 0.062 0.062 0.062 0.001 -0.014 -0.011 C52 0.085 0.085 0.085 0.001 -0.020 -0.015 C53 0.086 0.086 0.086 0.001 -0.020 -0.015 C54 0.089 0.089 0.089 0.001 -0.021 -0.015 C55 0.066 0.066 0.066 0.001 -0.015 -0.011 C56 0.077 0.077 0.077 0.001 -0.018 -0.013 C57 0.082 0.082 0.082 0.001 -0.019 -0.014 C58 0.087 0.087 0.087 0.001 -0.020 -0.015 C59 0.090 0.090 0.090 0.001 -0.021 -0.015 C60 0.082 0.082 0.082 0.001 -0.019 -0.014 C61 0.073 0.073 0.073 0.001 -0.017 -0.012 C62 0.078 0.078 0.078 0.001 -0.018 -0.013 C63 0.085 0.085 0.085 0.001 -0.020 -0.015 C64 0.082 0.082 0.082 0.001 -0.019 -0.014 C65 0.075 0.075 0.075 0.001 -0.017 -0.013 C66 0.068 0.068 0.068 0.001 -0.016 -0.012 C67 0.085 0.085 0.085 0.001 -0.020 -0.014 C68 0.080 0.080 0.080 0.001 -0.019 -0.014 C69 0.072 0.072 0.072 0.001 -0.017 -0.012 C70 0.079 0.079 0.079 0.001 -0.018 -0.013 Co1B 0.084 0.061 0.061 -0.009 -0.022 0.002 Co2B 0.089 0.059 0.043 -0.001 -0.022 0.003 Co3B 0.090 0.057 0.042 0.001 -0.024 0.003 Co4B 0.081 0.058 0.042 0.002 -0.019 0.001 O1B 0.109 0.074 0.052 0.004 -0.015 -0.016 O2B 0.089 0.055 0.043 -0.008 -0.016 0.010 O3B 0.085 0.070 0.063 0.003 -0.007 -0.016 O4B 0.083 0.087 0.051 -0.010 -0.012 0.004 O5B 0.062 0.059 0.057 0.008 -0.017 -0.005 O6B 0.097 0.068 0.100 -0.013 -0.025 0.008 O7B 0.085 0.067 0.039 -0.001 -0.014 -0.003 N1B 0.082 0.062 0.049 -0.001 -0.014 0.001 N2B 0.066 0.061 0.059 0.000 -0.023 0.001 N3B 0.081 0.047 0.061 -0.002 -0.022 0.012 N4B 0.098 0.068 0.038 0.007 -0.019 -0.006 N5B 0.095 0.070 0.090 -0.010 -0.037 0.007 N6B 0.096 0.056 0.046 0.000 -0.013 0.005 N7B 0.101 0.062 0.046 0.005 -0.010 0.022 N8B 0.090 0.048 0.041 -0.010 -0.017 0.002 N9B 0.129 0.066 0.050 -0.001 -0.023 -0.003 N10B 0.094 0.068 0.081 -0.012 -0.020 0.025 N11B 0.089 0.070 0.045 0.004 -0.020 -0.011 N12B 0.080 0.066 0.045 0.001 -0.023 0.005 C1B 0.064 0.064 0.064 0.001 -0.015 -0.011 C2B 0.098 0.098 0.098 0.001 -0.023 -0.017 C3B 0.070 0.070 0.070 0.001 -0.016 -0.012 C4B 0.087 0.087 0.087 0.001 -0.020 -0.015 C5B 0.094 0.094 0.094 0.001 -0.022 -0.016 C6B 0.089 0.089 0.089 0.001 -0.021 -0.015 C7B 0.070 0.070 0.070 0.001 -0.016 -0.012 C8B 0.064 0.064 0.064 0.001 -0.015 -0.011 C9B 0.066 0.066 0.066 0.001 -0.015 -0.011 C10B 0.064 0.064 0.064 0.001 -0.015 -0.011 C11B 0.062 0.062 0.062 0.001 -0.014 -0.011 C12B 0.062 0.062 0.062 0.001 -0.014 -0.011 C13B 0.081 0.081 0.081 0.001 -0.019 -0.014 C14B 0.082 0.082 0.082 0.001 -0.019 -0.014 C15B 0.073 0.073 0.073 0.001 -0.017 -0.012 C16B 0.067 0.067 0.067 0.001 -0.015 -0.011 C17B 0.061 0.061 0.061 0.001 -0.014 -0.010 C18B 0.064 0.064 0.064 0.001 -0.015 -0.011 C19B 0.064 0.064 0.064 0.001 -0.015 -0.011 C20B 0.065 0.065 0.065 0.001 -0.015 -0.011 C21B 0.066 0.066 0.066 0.001 -0.015 -0.011 C22B 0.067 0.067 0.067 0.001 -0.015 -0.011 C23B 0.073 0.073 0.073 0.001 -0.017 -0.012 C24B 0.083 0.083 0.083 0.001 -0.019 -0.014 C25B 0.078 0.078 0.078 0.001 -0.018 -0.013 C26B 0.066 0.066 0.066 0.001 -0.015 -0.011 C27B 0.088 0.088 0.088 0.001 -0.020 -0.015 C28B 0.124 0.124 0.124 0.001 -0.029 -0.021 C29B 0.101 0.101 0.101 0.001 -0.023 -0.017 C30B 0.125 0.125 0.125 0.001 -0.029 -0.021 C31B 0.103 0.103 0.103 0.001 -0.024 -0.018 C32B 0.084 0.084 0.084 0.001 -0.019 -0.014 C33B 0.071 0.071 0.071 0.001 -0.016 -0.012 C34B 0.078 0.078 0.078 0.001 -0.018 -0.013 C35B 0.069 0.069 0.069 0.001 -0.016 -0.012 C36B 0.068 0.068 0.068 0.001 -0.016 -0.012 C37B 0.076 0.076 0.076 0.001 -0.018 -0.013 C38B 0.078 0.078 0.078 0.001 -0.018 -0.013 C39B 0.074 0.074 0.074 0.001 -0.017 -0.013 C40B 0.066 0.066 0.066 0.001 -0.015 -0.011 C41B 0.066 0.066 0.066 0.001 -0.015 -0.011 C42B 0.068 0.068 0.068 0.001 -0.016 -0.012 C43B 0.071 0.071 0.071 0.001 -0.016 -0.012 C44B 0.062 0.062 0.062 0.001 -0.014 -0.011 C45B 0.065 0.065 0.065 0.001 -0.015 -0.011 C46B 0.065 0.065 0.065 0.001 -0.015 -0.011 C47B 0.073 0.073 0.073 0.001 -0.017 -0.012 C48B 0.077 0.077 0.077 0.001 -0.018 -0.013 C49B 0.078 0.078 0.078 0.001 -0.018 -0.013 C50B 0.063 0.063 0.063 0.001 -0.015 -0.011 C51B 0.064 0.064 0.064 0.001 -0.015 -0.011 C52B 0.072 0.072 0.072 0.001 -0.017 -0.012 C53B 0.087 0.087 0.087 0.001 -0.020 -0.015 C54B 0.080 0.080 0.080 0.001 -0.019 -0.014 C55B 0.086 0.086 0.086 0.001 -0.020 -0.015 C56B 0.100 0.100 0.100 0.001 -0.023 -0.017 C57B 0.098 0.098 0.098 0.001 -0.023 -0.017 C58B 0.099 0.099 0.099 0.001 -0.023 -0.017 C59B 0.094 0.094 0.094 0.001 -0.022 -0.016 C60B 0.083 0.083 0.083 0.001 -0.019 -0.014 C61B 0.063 0.063 0.063 0.001 -0.015 -0.011 C62B 0.080 0.080 0.080 0.001 -0.018 -0.014 C63B 0.081 0.081 0.081 0.001 -0.019 -0.014 C64B 0.080 0.080 0.080 0.001 -0.019 -0.014 C65B 0.061 0.061 0.061 0.001 -0.014 -0.010 C66B 0.073 0.073 0.073 0.001 -0.017 -0.013 C67B 0.084 0.084 0.084 0.001 -0.019 -0.014 C68B 0.078 0.078 0.078 0.001 -0.018 -0.013 C69B 0.084 0.084 0.084 0.001 -0.019 -0.014 C70B 0.074 0.074 0.074 0.001 -0.017 -0.013 N1S 0.093 0.093 0.093 0.001 -0.021 -0.016 C1S 0.137 0.137 0.137 0.001 -0.032 -0.023 C2S 0.154 0.154 0.154 0.001 -0.036 -0.026 C3S 0.111 0.111 0.111 0.001 -0.026 -0.019 C4S 0.100 0.100 0.100 0.001 -0.023 -0.017 C5S 0.148 0.148 0.148 0.001 -0.034 -0.025 _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 O4 1.885(6) . ? Co1 O6 1.904(6) . ? Co1 N5 1.929(7) . ? Co1 N9 1.937(8) . ? Co1 N1 1.947(7) . ? Co1 N10 1.957(7) . ? Co2 N2 1.945(6) . ? Co2 O3 1.946(6) . ? Co2 N6 1.963(7) . ? Co2 O1 1.981(6) . ? Co3 O3 1.925(6) . ? Co3 N7 1.960(6) . ? Co3 O2 1.964(6) . ? Co3 N3 1.967(6) . ? Co4 O7 1.900(6) . ? Co4 N12 1.907(7) . ? Co4 O5 1.921(6) . ? Co4 N8 1.940(8) . ? Co4 N11 1.959(7) . ? Co4 N4 1.963(7) . ? O1 C1 1.232(10) . ? O2 C1 1.252(10) . ? O4 C3 1.328(11) . ? O5 C26 1.352(10) . ? O6 C27 1.310(11) . ? O7 C50 1.297(11) . ? N1 C9 1.343(10) . ? N1 N2 1.394(9) . ? N2 C11 1.367(10) . ? N3 N4 1.359(9) . ? N3 C18 1.365(10) . ? N4 C20 1.336(10) . ? N5 N6 1.350(9) . ? N5 C33 1.367(11) . ? N6 C35 1.353(11) . ? N7 C42 1.363(11) . ? N7 N8 1.371(10) . ? N8 C44 1.381(11) . ? N9 C51 1.312(10) . ? N9 C55 1.372(11) . ? N10 C60 1.304(12) . ? N10 C56 1.322(11) . ? N11 C65 1.330(11) . ? N11 C61 1.358(11) . ? N12 C70 1.317(11) . ? N12 C66 1.346(10) . ? C1 C2 1.524(12) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C8 1.406(12) . ? C3 C4 1.412(13) . ? C4 C5 1.354(14) . ? C4 H4A 0.9500 . ? C5 C6 1.382(15) . ? C5 H5A 0.9500 . ? C6 C7 1.429(14) . ? C6 H6A 0.9500 . ? C7 C8 1.389(12) . ? C7 H7A 0.9500 . ? C8 C9 1.443(11) . ? C9 C10 1.382(12) . ? C10 C11 1.397(12) . ? C10 H10A 0.9500 . ? C11 C12 1.472(12) . ? C12 C13 1.355(12) . ? C12 C17 1.397(11) . ? C13 C14 1.423(13) . ? C13 H13A 0.9500 . ? C14 C15 1.391(13) . ? C14 H14A 0.9500 . ? C15 C16 1.349(11) . ? C15 H15A 0.9500 . ? C16 C17 1.422(11) . ? C16 C18 1.486(11) . ? C17 H17A 0.9500 . ? C18 C19 1.349(12) . ? C19 C20 1.358(11) . ? C19 H19A 0.9500 . ? C20 C21 1.508(11) . ? C21 C26 1.384(11) . ? C21 C22 1.440(12) . ? C22 C23 1.349(13) . ? C22 H22A 0.9500 . ? C23 C24 1.416(13) . ? C23 H23A 0.9500 . ? C24 C25 1.318(13) . ? C24 H24A 0.9500 . ? C25 C26 1.384(12) . ? C25 H25A 0.9500 . ? C27 C28 1.372(13) . ? C27 C32 1.437(13) . ? C28 C29 1.401(15) . ? C28 H28A 0.9500 . ? C29 C30 1.428(14) . ? C29 H29A 0.9500 . ? C30 C31 1.386(14) . ? C30 H30A 0.9500 . ? C31 C32 1.410(14) . ? C31 H31A 0.9500 . ? C32 C33 1.457(14) . ? C33 C34 1.365(13) . ? C34 C35 1.384(13) . ? C34 H34A 0.9500 . ? C35 C36 1.454(12) . ? C36 C37 1.380(12) . ? C36 C41 1.394(11) . ? C37 C38 1.407(14) . ? C37 H37A 0.9500 . ? C38 C39 1.392(13) . ? C38 H38A 0.9500 . ? C39 C40 1.369(12) . ? C39 H39A 0.9500 . ? C40 C41 1.409(12) . ? C40 C42 1.481(12) . ? C41 H41A 0.9500 . ? C42 C43 1.370(12) . ? C43 C44 1.388(12) . ? C43 H43A 0.9500 . ? C44 C45 1.467(12) . ? C45 C50 1.400(13) . ? C45 C46 1.401(13) . ? C46 C47 1.360(13) . ? C46 H46A 0.9500 . ? C47 C48 1.440(14) . ? C47 H47A 0.9500 . ? C48 C49 1.354(13) . ? C48 H48A 0.9500 . ? C49 C50 1.445(14) . ? C49 H49A 0.9500 . ? C51 C52 1.419(13) . ? C51 H51A 0.9500 . ? C52 C53 1.371(14) . ? C52 H52A 0.9500 . ? C53 C54 1.381(13) . ? C53 H53A 0.9500 . ? C54 C55 1.375(13) . ? C54 H54A 0.9500 . ? C55 H55A 0.9500 . ? C56 C57 1.391(13) . ? C56 H56A 0.9500 . ? C57 C58 1.349(14) . ? C57 H57A 0.9500 . ? C58 C59 1.363(14) . ? C58 H58A 0.9500 . ? C59 C60 1.393(14) . ? C59 H59A 0.9500 . ? C60 H60A 0.9500 . ? C61 C62 1.415(13) . ? C61 H61A 0.9500 . ? C62 C63 1.353(13) . ? C62 H62A 0.9500 . ? C63 C64 1.399(14) . ? C63 H63A 0.9500 . ? C64 C65 1.396(13) . ? C64 H64A 0.9500 . ? C65 H65A 0.9500 . ? C66 C67 1.383(13) . ? C66 H66A 0.9500 . ? C67 C68 1.374(14) . ? C67 H67A 0.9500 . ? C68 C69 1.332(12) . ? C68 H68A 0.9500 . ? C69 C70 1.423(13) . ? C69 H69A 0.9500 . ? C70 H70A 0.9500 . ? Co1B O4B 1.882(6) . ? Co1B O6B 1.893(7) . ? Co1B N5B 1.928(9) . ? Co1B N9B 1.937(8) . ? Co1B N10B 1.944(8) . ? Co1B N1B 1.954(7) . ? Co2B O3B 1.915(6) . ? Co2B N6B 1.936(7) . ? Co2B N2B 1.943(7) . ? Co2B O1B 1.976(7) . ? Co3B O3B 1.943(6) . ? Co3B N7B 1.954(7) . ? Co3B N3B 1.958(6) . ? Co3B O2B 1.960(6) . ? Co4B O5B 1.887(5) . ? Co4B N11B 1.913(7) . ? Co4B O7B 1.918(5) . ? Co4B N12B 1.938(7) . ? Co4B N8B 1.944(6) . ? Co4B N4B 1.949(7) . ? O1B C1B 1.273(10) . ? O2B C1B 1.264(9) . ? O4B C3B 1.325(10) . ? O5B C26B 1.347(10) . ? O6B C27B 1.362(12) . ? O7B C50B 1.326(9) . ? N1B C9B 1.363(10) . ? N1B N2B 1.365(9) . ? N2B C11B 1.346(10) . ? N3B C18B 1.325(10) . ? N3B N4B 1.380(9) . ? N4B C20B 1.367(10) . ? N5B C33B 1.348(12) . ? N5B N6B 1.389(10) . ? N6B C35B 1.369(11) . ? N7B C42B 1.362(10) . ? N7B N8B 1.415(9) . ? N8B C44B 1.319(10) . ? N9B C55B 1.321(12) . ? N9B C51B 1.349(11) . ? N10B C56B 1.277(13) . ? N10B C60B 1.320(12) . ? N11B C61B 1.336(10) . ? N11B C65B 1.373(10) . ? N12B C70B 1.336(11) . ? N12B C66B 1.343(11) . ? C1B C2B 1.487(13) . ? C2B H2BA 0.9800 . ? C2B H2BB 0.9800 . ? C2B H2BC 0.9800 . ? C3B C8B 1.389(12) . ? C3B C4B 1.428(13) . ? C4B C5B 1.351(14) . ? C4B H4BA 0.9500 . ? C5B C6B 1.410(14) . ? C5B H5BA 0.9500 . ? C6B C7B 1.390(13) . ? C6B H6BA 0.9500 . ? C7B C8B 1.397(12) . ? C7B H7BA 0.9500 . ? C8B C9B 1.478(12) . ? C9B C10B 1.388(11) . ? C10B C11B 1.398(11) . ? C10B H10B 0.9500 . ? C11B C12B 1.480(11) . ? C12B C13B 1.347(12) . ? C12B C17B 1.403(11) . ? C13B C14B 1.428(14) . ? C13B H13B 0.9500 . ? C14B C15B 1.366(13) . ? C14B H14B 0.9500 . ? C15B C16B 1.381(12) . ? C15B H15B 0.9500 . ? C16B C17B 1.379(11) . ? C16B C18B 1.494(12) . ? C17B H17B 0.9500 . ? C18B C19B 1.399(12) . ? C19B C20B 1.373(11) . ? C19B H19B 0.9500 . ? C20B C21B 1.443(12) . ? C21B C26B 1.402(11) . ? C21B C22B 1.416(12) . ? C22B C23B 1.388(12) . ? C22B H22B 0.9500 . ? C23B C24B 1.366(13) . ? C23B H23B 0.9500 . ? C24B C25B 1.354(13) . ? C24B H24B 0.9500 . ? C25B C26B 1.381(12) . ? C25B H25B 0.9500 . ? C27B C28B 1.387(17) . ? C27B C32B 1.408(14) . ? C28B C29B 1.435(17) . ? C28B H28B 0.9500 . ? C29B C30B 1.354(17) . ? C29B H29B 0.9500 . ? C30B C31B 1.438(18) . ? C30B H30B 0.9500 . ? C31B C32B 1.412(15) . ? C31B H31B 0.9500 . ? C32B C33B 1.432(13) . ? C33B C34B 1.414(12) . ? C34B C35B 1.365(13) . ? C34B H34B 0.9500 . ? C35B C36B 1.487(12) . ? C36B C37B 1.372(12) . ? C36B C41B 1.407(12) . ? C37B C38B 1.359(13) . ? C37B H37B 0.9500 . ? C38B C39B 1.433(13) . ? C38B H38B 0.9500 . ? C39B C40B 1.385(12) . ? C39B H39B 0.9500 . ? C40B C41B 1.379(11) . ? C40B C42B 1.463(12) . ? C41B H41B 0.9500 . ? C42B C43B 1.385(12) . ? C43B C44B 1.384(12) . ? C43B H43B 0.9500 . ? C44B C45B 1.474(11) . ? C45B C46B 1.365(11) . ? C45B C50B 1.412(11) . ? C46B C47B 1.360(12) . ? C46B H46B 0.9500 . ? C47B C48B 1.419(13) . ? C47B H47B 0.9500 . ? C48B C49B 1.354(13) . ? C48B H48B 0.9500 . ? C49B C50B 1.404(12) . ? C49B H49B 0.9500 . ? C51B C52B 1.425(12) . ? C51B H51B 0.9500 . ? C52B C53B 1.328(13) . ? C52B H52B 0.9500 . ? C53B C54B 1.398(13) . ? C53B H53B 0.9500 . ? C54B C55B 1.422(14) . ? C54B H54B 0.9500 . ? C55B H55B 0.9500 . ? C56B C57B 1.413(15) . ? C56B H56B 0.9500 . ? C57B C58B 1.398(16) . ? C57B H57B 0.9500 . ? C58B C59B 1.329(15) . ? C58B H58B 0.9500 . ? C59B C60B 1.435(14) . ? C59B H59B 0.9500 . ? C60B H60B 0.9500 . ? C61B C62B 1.379(12) . ? C61B H61B 0.9500 . ? C62B C63B 1.328(13) . ? C62B H62B 0.9500 . ? C63B C64B 1.368(13) . ? C63B H63B 0.9500 . ? C64B C65B 1.385(12) . ? C64B H64B 0.9500 . ? C65B H65B 0.9500 . ? C66B C67B 1.382(13) . ? C66B H66B 0.9500 . ? C67B C68B 1.367(13) . ? C67B H67B 0.9500 . ? C68B C69B 1.376(13) . ? C68B H68B 0.9500 . ? C69B C70B 1.351(13) . ? C69B H69B 0.9500 . ? C70B H70B 0.9500 . ? N1S C1S 1.3900 . ? N1S C5S 1.3900 . ? C1S C2S 1.3900 . ? C1S H1S 0.9500 . ? C2S C3S 1.3900 . ? C2S H2S 0.9500 . ? C3S C4S 1.3900 . ? C3S H3S 0.9500 . ? C4S C5S 1.3900 . ? C4S H4S 0.9500 . ? C5S H5S 0.9500 . ? 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 O4 Co1 O6 85.3(3) . . ? O4 Co1 N5 171.9(3) . . ? O6 Co1 N5 87.0(3) . . ? O4 Co1 N9 92.4(3) . . ? O6 Co1 N9 92.3(3) . . ? N5 Co1 N9 90.0(3) . . ? O4 Co1 N1 87.3(3) . . ? O6 Co1 N1 172.5(3) . . ? N5 Co1 N1 100.5(3) . . ? N9 Co1 N1 87.2(3) . . ? O4 Co1 N10 87.9(3) . . ? O6 Co1 N10 88.9(3) . . ? N5 Co1 N10 89.9(3) . . ? N9 Co1 N10 178.8(3) . . ? N1 Co1 N10 91.6(3) . . ? N2 Co2 O3 115.0(3) . . ? N2 Co2 N6 105.5(3) . . ? O3 Co2 N6 117.2(3) . . ? N2 Co2 O1 103.0(3) . . ? O3 Co2 O1 112.0(3) . . ? N6 Co2 O1 102.4(3) . . ? O3 Co3 N7 112.2(3) . . ? O3 Co3 O2 112.4(3) . . ? N7 Co3 O2 105.6(3) . . ? O3 Co3 N3 117.7(3) . . ? N7 Co3 N3 104.4(3) . . ? O2 Co3 N3 103.4(3) . . ? O7 Co4 N12 91.5(3) . . ? O7 Co4 O5 83.4(3) . . ? N12 Co4 O5 90.7(3) . . ? O7 Co4 N8 86.9(3) . . ? N12 Co4 N8 88.6(3) . . ? O5 Co4 N8 170.3(3) . . ? O7 Co4 N11 91.6(3) . . ? N12 Co4 N11 176.5(3) . . ? O5 Co4 N11 88.0(3) . . ? N8 Co4 N11 93.2(3) . . ? O7 Co4 N4 171.6(3) . . ? N12 Co4 N4 89.4(3) . . ? O5 Co4 N4 88.3(3) . . ? N8 Co4 N4 101.4(3) . . ? N11 Co4 N4 87.2(3) . . ? C1 O1 Co2 130.6(6) . . ? C1 O2 Co3 131.1(6) . . ? Co3 O3 Co2 108.1(3) . . ? C3 O4 Co1 123.7(6) . . ? C26 O5 Co4 122.6(5) . . ? C27 O6 Co1 122.1(5) . . ? C50 O7 Co4 123.3(6) . . ? C9 N1 N2 108.0(7) . . ? C9 N1 Co1 125.6(5) . . ? N2 N1 Co1 126.4(5) . . ? C11 N2 N1 108.3(6) . . ? C11 N2 Co2 127.0(6) . . ? N1 N2 Co2 124.5(5) . . ? N4 N3 C18 108.6(7) . . ? N4 N3 Co3 124.0(5) . . ? C18 N3 Co3 126.4(5) . . ? C20 N4 N3 106.7(6) . . ? C20 N4 Co4 126.0(5) . . ? N3 N4 Co4 124.9(5) . . ? N6 N5 C33 105.9(7) . . ? N6 N5 Co1 128.6(5) . . ? C33 N5 Co1 125.4(6) . . ? N5 N6 C35 109.8(7) . . ? N5 N6 Co2 122.5(5) . . ? C35 N6 Co2 125.7(6) . . ? C42 N7 N8 109.4(7) . . ? C42 N7 Co3 125.1(6) . . ? N8 N7 Co3 125.5(5) . . ? N7 N8 C44 106.0(7) . . ? N7 N8 Co4 126.2(5) . . ? C44 N8 Co4 127.7(6) . . ? C51 N9 C55 118.6(8) . . ? C51 N9 Co1 121.3(6) . . ? C55 N9 Co1 120.0(6) . . ? C60 N10 C56 116.0(8) . . ? C60 N10 Co1 123.4(7) . . ? C56 N10 Co1 120.1(6) . . ? C65 N11 C61 118.0(8) . . ? C65 N11 Co4 122.6(6) . . ? C61 N11 Co4 119.4(6) . . ? C70 N12 C66 117.0(8) . . ? C70 N12 Co4 122.2(6) . . ? C66 N12 Co4 120.7(6) . . ? O1 C1 O2 125.1(8) . . ? O1 C1 C2 117.4(8) . . ? O2 C1 C2 117.5(8) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O4 C3 C8 123.2(8) . . ? O4 C3 C4 119.2(9) . . ? C8 C3 C4 117.6(9) . . ? C5 C4 C3 121.8(10) . . ? C5 C4 H4A 119.1 . . ? C3 C4 H4A 119.1 . . ? C4 C5 C6 121.5(11) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C5 C6 C7 118.4(11) . . ? C5 C6 H6A 120.8 . . ? C7 C6 H6A 120.8 . . ? C8 C7 C6 119.9(9) . . ? C8 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? C7 C8 C3 120.8(8) . . ? C7 C8 C9 119.4(8) . . ? C3 C8 C9 119.7(8) . . ? N1 C9 C10 109.2(7) . . ? N1 C9 C8 122.8(8) . . ? C10 C9 C8 127.8(8) . . ? C9 C10 C11 107.2(8) . . ? C9 C10 H10A 126.4 . . ? C11 C10 H10A 126.4 . . ? N2 C11 C10 107.4(7) . . ? N2 C11 C12 123.0(7) . . ? C10 C11 C12 129.5(8) . . ? C13 C12 C17 118.9(8) . . ? C13 C12 C11 120.0(8) . . ? C17 C12 C11 121.0(7) . . ? C12 C13 C14 121.8(9) . . ? C12 C13 H13A 119.1 . . ? C14 C13 H13A 119.1 . . ? C15 C14 C13 118.4(9) . . ? C15 C14 H14A 120.8 . . ? C13 C14 H14A 120.8 . . ? C16 C15 C14 120.4(9) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C17 120.7(8) . . ? C15 C16 C18 119.0(8) . . ? C17 C16 C18 120.3(7) . . ? C12 C17 C16 119.5(7) . . ? C12 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C19 C18 N3 107.5(8) . . ? C19 C18 C16 129.4(8) . . ? N3 C18 C16 123.1(8) . . ? C18 C19 C20 107.3(8) . . ? C18 C19 H19A 126.4 . . ? C20 C19 H19A 126.4 . . ? N4 C20 C19 109.8(7) . . ? N4 C20 C21 121.6(7) . . ? C19 C20 C21 128.4(8) . . ? C26 C21 C22 120.4(8) . . ? C26 C21 C20 120.7(7) . . ? C22 C21 C20 118.9(7) . . ? C23 C22 C21 119.2(9) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? C22 C23 C24 119.2(9) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? C25 C24 C23 120.6(9) . . ? C25 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? C24 C25 C26 123.3(9) . . ? C24 C25 H25A 118.3 . . ? C26 C25 H25A 118.3 . . ? O5 C26 C25 121.1(7) . . ? O5 C26 C21 121.5(7) . . ? C25 C26 C21 117.2(8) . . ? O6 C27 C28 119.2(9) . . ? O6 C27 C32 122.4(8) . . ? C28 C27 C32 118.4(9) . . ? C27 C28 C29 124.2(10) . . ? C27 C28 H28A 117.9 . . ? C29 C28 H28A 117.9 . . ? C28 C29 C30 117.0(11) . . ? C28 C29 H29A 121.5 . . ? C30 C29 H29A 121.5 . . ? C31 C30 C29 120.1(10) . . ? C31 C30 H30A 119.9 . . ? C29 C30 H30A 119.9 . . ? C30 C31 C32 121.7(9) . . ? C30 C31 H31A 119.2 . . ? C32 C31 H31A 119.2 . . ? C31 C32 C27 118.5(9) . . ? C31 C32 C33 121.6(9) . . ? C27 C32 C33 119.0(9) . . ? C34 C33 N5 110.7(8) . . ? C34 C33 C32 127.4(9) . . ? N5 C33 C32 121.2(8) . . ? C33 C34 C35 105.2(8) . . ? C33 C34 H34A 127.4 . . ? C35 C34 H34A 127.4 . . ? N6 C35 C34 108.4(8) . . ? N6 C35 C36 122.8(8) . . ? C34 C35 C36 128.8(8) . . ? C37 C36 C41 119.0(8) . . ? C37 C36 C35 120.0(8) . . ? C41 C36 C35 121.0(7) . . ? C36 C37 C38 119.0(9) . . ? C36 C37 H37A 120.5 . . ? C38 C37 H37A 120.5 . . ? C39 C38 C37 122.3(10) . . ? C39 C38 H38A 118.8 . . ? C37 C38 H38A 118.8 . . ? C40 C39 C38 118.2(9) . . ? C40 C39 H39A 120.9 . . ? C38 C39 H39A 120.9 . . ? C39 C40 C41 120.2(8) . . ? C39 C40 C42 118.6(8) . . ? C41 C40 C42 121.1(8) . . ? C36 C41 C40 121.2(8) . . ? C36 C41 H41A 119.4 . . ? C40 C41 H41A 119.4 . . ? N7 C42 C43 108.6(8) . . ? N7 C42 C40 121.4(8) . . ? C43 C42 C40 129.9(8) . . ? C42 C43 C44 106.4(8) . . ? C42 C43 H43A 126.8 . . ? C44 C43 H43A 126.8 . . ? N8 C44 C43 109.3(8) . . ? N8 C44 C45 121.1(8) . . ? C43 C44 C45 129.6(8) . . ? C50 C45 C46 119.4(9) . . ? C50 C45 C44 119.0(8) . . ? C46 C45 C44 121.6(8) . . ? C47 C46 C45 123.8(10) . . ? C47 C46 H46A 118.1 . . ? C45 C46 H46A 118.1 . . ? C46 C47 C48 117.6(10) . . ? C46 C47 H47A 121.2 . . ? C48 C47 H47A 121.2 . . ? C49 C48 C47 119.4(10) . . ? C49 C48 H48A 120.3 . . ? C47 C48 H48A 120.3 . . ? C48 C49 C50 123.0(10) . . ? C48 C49 H49A 118.5 . . ? C50 C49 H49A 118.5 . . ? O7 C50 C45 124.2(9) . . ? O7 C50 C49 119.5(9) . . ? C45 C50 C49 116.3(9) . . ? N9 C51 C52 122.5(8) . . ? N9 C51 H51A 118.7 . . ? C52 C51 H51A 118.7 . . ? C53 C52 C51 116.2(9) . . ? C53 C52 H52A 121.9 . . ? C51 C52 H52A 121.9 . . ? C52 C53 C54 123.4(10) . . ? C52 C53 H53A 118.3 . . ? C54 C53 H53A 118.3 . . ? C55 C54 C53 115.6(10) . . ? C55 C54 H54A 122.2 . . ? C53 C54 H54A 122.2 . . ? N9 C55 C54 123.7(8) . . ? N9 C55 H55A 118.2 . . ? C54 C55 H55A 118.2 . . ? N10 C56 C57 123.5(9) . . ? N10 C56 H56A 118.3 . . ? C57 C56 H56A 118.3 . . ? C58 C57 C56 119.1(10) . . ? C58 C57 H57A 120.5 . . ? C56 C57 H57A 120.5 . . ? C57 C58 C59 118.7(10) . . ? C57 C58 H58A 120.7 . . ? C59 C58 H58A 120.7 . . ? C58 C59 C60 117.7(10) . . ? C58 C59 H59A 121.2 . . ? C60 C59 H59A 121.2 . . ? N10 C60 C59 124.8(10) . . ? N10 C60 H60A 117.6 . . ? C59 C60 H60A 117.6 . . ? N11 C61 C62 120.8(9) . . ? N11 C61 H61A 119.6 . . ? C62 C61 H61A 119.6 . . ? C63 C62 C61 119.8(9) . . ? C63 C62 H62A 120.1 . . ? C61 C62 H62A 120.1 . . ? C62 C63 C64 120.1(10) . . ? C62 C63 H63A 119.9 . . ? C64 C63 H63A 119.9 . . ? C65 C64 C63 116.8(10) . . ? C65 C64 H64A 121.6 . . ? C63 C64 H64A 121.6 . . ? N11 C65 C64 124.5(9) . . ? N11 C65 H65A 117.8 . . ? C64 C65 H65A 117.8 . . ? N12 C66 C67 120.5(9) . . ? N12 C66 H66A 119.7 . . ? C67 C66 H66A 119.7 . . ? C68 C67 C66 120.9(9) . . ? C68 C67 H67A 119.6 . . ? C66 C67 H67A 119.6 . . ? C69 C68 C67 119.9(9) . . ? C69 C68 H68A 120.1 . . ? C67 C68 H68A 120.1 . . ? C68 C69 C70 116.3(9) . . ? C68 C69 H69A 121.8 . . ? C70 C69 H69A 121.8 . . ? N12 C70 C69 125.1(9) . . ? N12 C70 H70A 117.4 . . ? C69 C70 H70A 117.4 . . ? O4B Co1B O6B 84.7(3) . . ? O4B Co1B N5B 171.0(3) . . ? O6B Co1B N5B 86.6(3) . . ? O4B Co1B N9B 91.0(3) . . ? O6B Co1B N9B 92.8(3) . . ? N5B Co1B N9B 91.4(3) . . ? O4B Co1B N10B 88.0(3) . . ? O6B Co1B N10B 87.3(3) . . ? N5B Co1B N10B 89.6(3) . . ? N9B Co1B N10B 179.0(3) . . ? O4B Co1B N1B 87.6(3) . . ? O6B Co1B N1B 172.1(3) . . ? N5B Co1B N1B 101.2(3) . . ? N9B Co1B N1B 88.4(3) . . ? N10B Co1B N1B 91.4(3) . . ? O3B Co2B N6B 118.3(3) . . ? O3B Co2B N2B 114.4(3) . . ? N6B Co2B N2B 105.1(3) . . ? O3B Co2B O1B 112.3(3) . . ? N6B Co2B O1B 102.0(3) . . ? N2B Co2B O1B 102.9(3) . . ? O3B Co3B N7B 114.9(3) . . ? O3B Co3B N3B 117.4(3) . . ? N7B Co3B N3B 105.7(3) . . ? O3B Co3B O2B 111.7(2) . . ? N7B Co3B O2B 103.4(3) . . ? N3B Co3B O2B 102.1(3) . . ? O5B Co4B N11B 91.5(3) . . ? O5B Co4B O7B 83.2(2) . . ? N11B Co4B O7B 93.3(3) . . ? O5B Co4B N12B 88.7(2) . . ? N11B Co4B N12B 176.7(3) . . ? O7B Co4B N12B 90.1(3) . . ? O5B Co4B N8B 169.2(2) . . ? N11B Co4B N8B 87.3(3) . . ? O7B Co4B N8B 86.2(2) . . ? N12B Co4B N8B 93.1(3) . . ? O5B Co4B N4B 88.8(3) . . ? N11B Co4B N4B 89.8(3) . . ? O7B Co4B N4B 171.6(3) . . ? N12B Co4B N4B 86.9(3) . . ? N8B Co4B N4B 101.8(3) . . ? C1B O1B Co2B 131.1(5) . . ? C1B O2B Co3B 132.1(5) . . ? Co2B O3B Co3B 109.1(3) . . ? C3B O4B Co1B 124.8(6) . . ? C26B O5B Co4B 124.0(5) . . ? C27B O6B Co1B 122.7(6) . . ? C50B O7B Co4B 122.1(5) . . ? C9B N1B N2B 107.2(7) . . ? C9B N1B Co1B 125.7(6) . . ? N2B N1B Co1B 127.0(5) . . ? C11B N2B N1B 108.5(6) . . ? C11B N2B Co2B 126.6(5) . . ? N1B N2B Co2B 124.6(5) . . ? C18B N3B N4B 109.0(7) . . ? C18B N3B Co3B 127.0(6) . . ? N4B N3B Co3B 123.3(5) . . ? C20B N4B N3B 107.3(6) . . ? C20B N4B Co4B 125.1(6) . . ? N3B N4B Co4B 126.3(5) . . ? C33B N5B N6B 108.9(8) . . ? C33B N5B Co1B 125.0(6) . . ? N6B N5B Co1B 126.0(6) . . ? C35B N6B N5B 107.2(7) . . ? C35B N6B Co2B 127.6(6) . . ? N5B N6B Co2B 124.6(5) . . ? C42B N7B N8B 107.8(6) . . ? C42B N7B Co3B 128.0(6) . . ? N8B N7B Co3B 124.2(5) . . ? C44B N8B N7B 107.0(6) . . ? C44B N8B Co4B 126.9(5) . . ? N7B N8B Co4B 126.1(5) . . ? C55B N9B C51B 120.1(8) . . ? C55B N9B Co1B 119.5(8) . . ? C51B N9B Co1B 120.5(6) . . ? C56B N10B C60B 117.4(10) . . ? C56B N10B Co1B 122.2(8) . . ? C60B N10B Co1B 120.4(7) . . ? C61B N11B C65B 116.8(7) . . ? C61B N11B Co4B 122.1(6) . . ? C65B N11B Co4B 121.1(5) . . ? C70B N12B C66B 116.0(8) . . ? C70B N12B Co4B 121.6(6) . . ? C66B N12B Co4B 122.4(5) . . ? O2B C1B O1B 123.3(7) . . ? O2B C1B C2B 119.0(8) . . ? O1B C1B C2B 117.7(8) . . ? C1B C2B H2BA 109.5 . . ? C1B C2B H2BB 109.5 . . ? H2BA C2B H2BB 109.5 . . ? C1B C2B H2BC 109.5 . . ? H2BA C2B H2BC 109.5 . . ? H2BB C2B H2BC 109.5 . . ? O4B C3B C8B 122.9(8) . . ? O4B C3B C4B 118.3(8) . . ? C8B C3B C4B 118.8(9) . . ? C5B C4B C3B 121.8(10) . . ? C5B C4B H4BA 119.1 . . ? C3B C4B H4BA 119.1 . . ? C4B C5B C6B 120.3(11) . . ? C4B C5B H5BA 119.9 . . ? C6B C5B H5BA 119.9 . . ? C7B C6B C5B 117.5(10) . . ? C7B C6B H6BA 121.2 . . ? C5B C6B H6BA 121.2 . . ? C6B C7B C8B 123.3(9) . . ? C6B C7B H7BA 118.3 . . ? C8B C7B H7BA 118.3 . . ? C3B C8B C7B 118.1(8) . . ? C3B C8B C9B 120.3(8) . . ? C7B C8B C9B 121.2(8) . . ? N1B C9B C10B 110.2(7) . . ? N1B C9B C8B 121.1(8) . . ? C10B C9B C8B 128.7(8) . . ? C9B C10B C11B 104.0(7) . . ? C9B C10B H10B 128.0 . . ? C11B C10B H10B 128.0 . . ? N2B C11B C10B 109.9(7) . . ? N2B C11B C12B 122.3(7) . . ? C10B C11B C12B 127.7(7) . . ? C13B C12B C17B 120.8(8) . . ? C13B C12B C11B 117.4(8) . . ? C17B C12B C11B 121.7(7) . . ? C12B C13B C14B 118.1(9) . . ? C12B C13B H13B 120.9 . . ? C14B C13B H13B 120.9 . . ? C15B C14B C13B 121.0(9) . . ? C15B C14B H14B 119.5 . . ? C13B C14B H14B 119.5 . . ? C14B C15B C16B 120.0(9) . . ? C14B C15B H15B 120.0 . . ? C16B C15B H15B 120.0 . . ? C17B C16B C15B 119.3(8) . . ? C17B C16B C18B 120.9(7) . . ? C15B C16B C18B 119.8(8) . . ? C16B C17B C12B 120.5(7) . . ? C16B C17B H17B 119.8 . . ? C12B C17B H17B 119.8 . . ? N3B C18B C19B 108.7(7) . . ? N3B C18B C16B 122.9(8) . . ? C19B C18B C16B 128.2(8) . . ? C20B C19B C18B 106.4(7) . . ? C20B C19B H19B 126.8 . . ? C18B C19B H19B 126.8 . . ? N4B C20B C19B 108.5(7) . . ? N4B C20B C21B 122.7(7) . . ? C19B C20B C21B 128.3(8) . . ? C26B C21B C22B 118.6(8) . . ? C26B C21B C20B 121.3(8) . . ? C22B C21B C20B 120.1(8) . . ? C23B C22B C21B 122.2(8) . . ? C23B C22B H22B 118.9 . . ? C21B C22B H22B 118.9 . . ? C24B C23B C22B 116.5(9) . . ? C24B C23B H23B 121.7 . . ? C22B C23B H23B 121.7 . . ? C25B C24B C23B 122.9(10) . . ? C25B C24B H24B 118.6 . . ? C23B C24B H24B 118.6 . . ? C24B C25B C26B 121.9(9) . . ? C24B C25B H25B 119.0 . . ? C26B C25B H25B 119.0 . . ? O5B C26B C25B 120.3(8) . . ? O5B C26B C21B 121.7(7) . . ? C25B C26B C21B 117.8(8) . . ? O6B C27B C28B 118.8(10) . . ? O6B C27B C32B 121.0(9) . . ? C28B C27B C32B 120.2(11) . . ? C27B C28B C29B 117.4(13) . . ? C27B C28B H28B 121.3 . . ? C29B C28B H28B 121.3 . . ? C30B C29B C28B 125.7(13) . . ? C30B C29B H29B 117.1 . . ? C28B C29B H29B 117.1 . . ? C29B C30B C31B 115.2(13) . . ? C29B C30B H30B 122.4 . . ? C31B C30B H30B 122.4 . . ? C32B C31B C30B 121.6(12) . . ? C32B C31B H31B 119.2 . . ? C30B C31B H31B 119.2 . . ? C27B C32B C31B 119.8(10) . . ? C27B C32B C33B 119.1(9) . . ? C31B C32B C33B 121.0(9) . . ? N5B C33B C34B 107.7(8) . . ? N5B C33B C32B 123.7(9) . . ? C34B C33B C32B 128.1(9) . . ? C35B C34B C33B 106.8(8) . . ? C35B C34B H34B 126.6 . . ? C33B C34B H34B 126.6 . . ? C34B C35B N6B 109.2(8) . . ? C34B C35B C36B 128.6(8) . . ? N6B C35B C36B 122.1(8) . . ? C37B C36B C41B 119.6(8) . . ? C37B C36B C35B 119.3(8) . . ? C41B C36B C35B 121.1(7) . . ? C38B C37B C36B 119.3(9) . . ? C38B C37B H37B 120.3 . . ? C36B C37B H37B 120.3 . . ? C37B C38B C39B 122.3(9) . . ? C37B C38B H38B 118.9 . . ? C39B C38B H38B 118.9 . . ? C40B C39B C38B 117.6(8) . . ? C40B C39B H39B 121.2 . . ? C38B C39B H39B 121.2 . . ? C41B C40B C39B 119.8(8) . . ? C41B C40B C42B 122.1(7) . . ? C39B C40B C42B 118.1(8) . . ? C40B C41B C36B 121.3(8) . . ? C40B C41B H41B 119.3 . . ? C36B C41B H41B 119.3 . . ? N7B C42B C43B 108.1(8) . . ? N7B C42B C40B 121.9(8) . . ? C43B C42B C40B 130.0(8) . . ? C44B C43B C42B 106.3(8) . . ? C44B C43B H43B 126.8 . . ? C42B C43B H43B 126.8 . . ? N8B C44B C43B 110.7(7) . . ? N8B C44B C45B 123.3(7) . . ? C43B C44B C45B 125.9(8) . . ? C46B C45B C50B 119.0(8) . . ? C46B C45B C44B 123.3(8) . . ? C50B C45B C44B 117.6(7) . . ? C47B C46B C45B 124.8(8) . . ? C47B C46B H46B 117.6 . . ? C45B C46B H46B 117.6 . . ? C46B C47B C48B 115.8(9) . . ? C46B C47B H47B 122.1 . . ? C48B C47B H47B 122.1 . . ? C49B C48B C47B 121.5(9) . . ? C49B C48B H48B 119.2 . . ? C47B C48B H48B 119.2 . . ? C48B C49B C50B 121.4(9) . . ? C48B C49B H49B 119.3 . . ? C50B C49B H49B 119.3 . . ? O7B C50B C49B 118.7(7) . . ? O7B C50B C45B 123.9(7) . . ? C49B C50B C45B 117.4(8) . . ? N9B C51B C52B 120.4(8) . . ? N9B C51B H51B 119.8 . . ? C52B C51B H51B 119.8 . . ? C53B C52B C51B 120.3(9) . . ? C53B C52B H52B 119.9 . . ? C51B C52B H52B 119.9 . . ? C52B C53B C54B 119.4(10) . . ? C52B C53B H53B 120.3 . . ? C54B C53B H53B 120.3 . . ? C53B C54B C55B 118.6(10) . . ? C53B C54B H54B 120.7 . . ? C55B C54B H54B 120.7 . . ? N9B C55B C54B 121.1(9) . . ? N9B C55B H55B 119.4 . . ? C54B C55B H55B 119.4 . . ? N10B C56B C57B 124.4(12) . . ? N10B C56B H56B 117.8 . . ? C57B C56B H56B 117.8 . . ? C58B C57B C56B 116.9(11) . . ? C58B C57B H57B 121.5 . . ? C56B C57B H57B 121.5 . . ? C59B C58B C57B 120.2(12) . . ? C59B C58B H58B 119.9 . . ? C57B C58B H58B 119.9 . . ? C58B C59B C60B 116.9(12) . . ? C58B C59B H59B 121.5 . . ? C60B C59B H59B 121.5 . . ? N10B C60B C59B 123.9(10) . . ? N10B C60B H60B 118.0 . . ? C59B C60B H60B 118.0 . . ? N11B C61B C62B 121.3(8) . . ? N11B C61B H61B 119.3 . . ? C62B C61B H61B 119.3 . . ? C63B C62B C61B 121.3(9) . . ? C63B C62B H62B 119.4 . . ? C61B C62B H62B 119.4 . . ? C62B C63B C64B 120.2(10) . . ? C62B C63B H63B 119.9 . . ? C64B C63B H63B 119.9 . . ? C63B C64B C65B 117.3(9) . . ? C63B C64B H64B 121.3 . . ? C65B C64B H64B 121.3 . . ? N11B C65B C64B 123.1(8) . . ? N11B C65B H65B 118.4 . . ? C64B C65B H65B 118.4 . . ? N12B C66B C67B 122.2(9) . . ? N12B C66B H66B 118.9 . . ? C67B C66B H66B 118.9 . . ? C68B C67B C66B 118.9(10) . . ? C68B C67B H67B 120.6 . . ? C66B C67B H67B 120.6 . . ? C67B C68B C69B 120.3(10) . . ? C67B C68B H68B 119.9 . . ? C69B C68B H68B 119.9 . . ? C70B C69B C68B 116.3(10) . . ? C70B C69B H69B 121.9 . . ? C68B C69B H69B 121.9 . . ? N12B C70B C69B 126.4(10) . . ? N12B C70B H70B 116.8 . . ? C69B C70B H70B 116.8 . . ? C1S N1S C5S 120.0 . . ? N1S C1S C2S 120.0 . . ? N1S C1S H1S 120.0 . . ? C2S C1S H1S 120.0 . . ? C1S C2S C3S 120.0 . . ? C1S C2S H2S 120.0 . . ? C3S C2S H2S 120.0 . . ? C4S C3S C2S 120.0 . . ? C4S C3S H3S 120.0 . . ? C2S C3S H3S 120.0 . . ? C3S C4S C5S 120.0 . . ? C3S C4S H4S 120.0 . . ? C5S C4S H4S 120.0 . . ? C4S C5S N1S 120.0 . . ? C4S C5S H5S 120.0 . . ? N1S C5S H5S 120.0 . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.74 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 2.491 _refine_diff_density_min -1.436 _refine_diff_density_rms 0.157