# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email m.schroder@nottingham.ac.uk _publ_contact_author_name M.Schroder loop_ _publ_author_name M.Schroder 'Junhua Jia' 'Harprit Athwal' 'Alexander Blake' 'Neil Champness' P.Hubberstey data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 825859' #TrackingRef '- Cobalt.CIF' # code COPYDB #5240 _refine_special_details ; 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 -0.021 0.127 0.317 2002.3 279 ; _platon_squeeze_details ; 279 electrons/unit cell were assigned as 7DMF molecules/unit cell. They have been included in the formula as 1.75 DMF per asymmetric unit. H atoms on C1NA and C1NB of the coordinated DMF molecule were not located but have been included in the formula. ; _audit_creation_method 'enCIfer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H21 Co2 N3 O9, 1.75(C3 H7 N O)' _chemical_formula_sum 'C34.25 H33.25 Co2 N4.75 O10.75' _chemical_formula_weight 801.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.287(1) _cell_length_b 28.242(3) _cell_length_c 16.667(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.030(2) _cell_angle_gamma 90.00 _cell_volume 4339(1) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3034 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 25.75 _exptl_crystal_description PLATE _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.165 _exptl_crystal_size_mid 0.141 _exptl_crystal_size_min 0.029 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.684 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS version 2.05; Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 27393 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_sigmaI/netI 0.060 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10111 _reflns_number_gt 5280 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer(Allen et al.,2004);PLATON(Spek,2003)' _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^)+(0.087P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom + difmap' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7603 _refine_ls_number_parameters 368 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.148 _refine_ls_wR_factor_gt 0.139 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.01 _refine_ls_shift/su_max 0.005 _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 -0.80722(5) 0.304782(17) 0.28021(3) 0.02258(15) Uani 1 1 d . . . Co2 Co 0.24455(5) 0.424573(17) 0.26939(3) 0.02398(15) Uani 1 1 d . . . O1 O -0.8054(3) 0.31206(9) 0.16126(15) 0.0317(6) Uani 1 1 d . . . O2 O -0.8150(3) 0.39123(9) 0.15894(15) 0.0376(7) Uani 1 1 d . . . O3 O -0.8114(3) 0.22791(9) -0.10105(15) 0.0378(7) Uani 1 1 d . . . O4 O -0.8645(3) 0.26669(9) -0.21439(15) 0.0363(7) Uani 1 1 d . . . O5 O -0.6755(3) 0.35999(8) 0.32608(14) 0.0248(6) Uani 1 1 d . . . O6 O -0.5526(3) 0.29648(9) 0.30084(17) 0.0365(7) Uani 1 1 d . . . O7 O -0.0058(3) 0.33351(9) 0.28716(15) 0.0312(6) Uani 1 1 d . . . O8 O 0.0529(3) 0.41018(9) 0.31224(15) 0.0272(6) Uani 1 1 d . . . N1 N -1.1522(4) 0.51283(11) -0.21107(18) 0.0305(8) Uani 1 1 d . . . N2 N -0.2981(3) 0.53237(11) 0.62427(18) 0.0270(7) Uani 1 1 d . . . C1 C -1.0663(5) 0.48328(14) -0.2461(2) 0.0355(10) Uani 1 1 d . . . H1A H -1.0493 0.4899 -0.3000 0.043 Uiso 1 1 calc R . . C2 C -1.0003(5) 0.44356(14) -0.2090(2) 0.0365(10) Uani 1 1 d . . . H2A H -0.9390 0.4242 -0.2367 0.044 Uiso 1 1 calc R . . C3 C -1.0253(5) 0.43263(13) -0.1310(2) 0.0377(10) Uani 1 1 d . . . C4 C -1.1142(6) 0.46314(15) -0.0945(2) 0.0480(12) Uani 1 1 d . . . H4A H -1.1340 0.4572 -0.0408 0.058 Uiso 1 1 calc R . . C5 C -1.1744(5) 0.50231(14) -0.1361(2) 0.0419(11) Uani 1 1 d . . . H5A H -1.2347 0.5227 -0.1094 0.050 Uiso 1 1 calc R . . C6 C -0.9593(5) 0.39023(14) -0.0885(2) 0.0411(11) Uani 1 1 d . . . C7 C -0.9324(5) 0.34947(14) -0.1312(2) 0.0400(11) Uani 1 1 d . . . H7A H -0.9518 0.3494 -0.1885 0.048 Uiso 1 1 calc R . . C8 C -0.8774(5) 0.30870(14) -0.0912(2) 0.0357(10) Uani 1 1 d . . . C9 C -0.8447(5) 0.30923(13) -0.0082(2) 0.0346(10) Uani 1 1 d . . . H9A H -0.8084 0.2814 0.0191 0.041 Uiso 1 1 calc R . . C10 C -0.8643(5) 0.35037(14) 0.0365(2) 0.0355(10) Uani 1 1 d . . . C11 C -0.9217(5) 0.39040(14) -0.0049(2) 0.0403(11) Uani 1 1 d . . . H11A H -0.9355 0.4185 0.0247 0.048 Uiso 1 1 calc R . . C12 C -0.8489(5) 0.26528(14) -0.1380(2) 0.0333(9) Uani 1 1 d . . . C13 C -0.8251(5) 0.35144(14) 0.1259(2) 0.0338(10) Uani 1 1 d . . . C14 C -0.3699(4) 0.49117(14) 0.6287(2) 0.0315(9) Uani 1 1 d . . . H14A H -0.4179 0.4855 0.6749 0.038 Uiso 1 1 calc R . . C15 C -0.3772(4) 0.45690(14) 0.5693(2) 0.0327(9) Uani 1 1 d . . . H15A H -0.4302 0.4285 0.5748 0.039 Uiso 1 1 calc R . . C16 C -0.3066(4) 0.46410(13) 0.5016(2) 0.0297(9) Uani 1 1 d . . . C17 C -0.2371(4) 0.50755(14) 0.4955(2) 0.0307(9) Uani 1 1 d . . . H17A H -0.1905 0.5146 0.4492 0.037 Uiso 1 1 calc R . . C18 C -0.2366(4) 0.54004(14) 0.5570(2) 0.0282(8) Uani 1 1 d . . . H18A H -0.1900 0.5696 0.5513 0.034 Uiso 1 1 calc R . . C19 C -0.3024(4) 0.42701(14) 0.4390(2) 0.0285(9) Uani 1 1 d . . . C20 C -0.4240(4) 0.39906(14) 0.4144(2) 0.0314(9) Uani 1 1 d . . . H20A H -0.5115 0.4043 0.4373 0.038 Uiso 1 1 calc R . . C21 C -0.4183(4) 0.36378(13) 0.3570(2) 0.0285(9) Uani 1 1 d . . . C22 C -0.2901(4) 0.35449(13) 0.3255(2) 0.0273(8) Uani 1 1 d . . . H22A H -0.2843 0.3288 0.2892 0.033 Uiso 1 1 calc R . . C23 C -0.1700(4) 0.38310(14) 0.3474(2) 0.0282(9) Uani 1 1 d . . . C24 C -0.1772(4) 0.41952(13) 0.4026(2) 0.0297(9) Uani 1 1 d . . . H24A H -0.0957 0.4396 0.4157 0.036 Uiso 1 1 calc R . . C25 C -0.5550(4) 0.33765(14) 0.3263(2) 0.0280(9) Uani 1 1 d . . . C26 C -0.0285(4) 0.37499(14) 0.3127(2) 0.0265(8) Uani 1 1 d . . . O1N O 0.4419(3) 0.44233(11) 0.23055(17) 0.0436(7) Uiso 1 1 d . . . N1N N 0.6404(7) 0.4362(2) 0.1657(4) 0.1026(19) Uiso 1 1 d D . . C1NA C 0.7081(10) 0.4774(3) 0.2072(5) 0.132(3) Uiso 1 1 d D . . C1NB C 0.7220(12) 0.4073(4) 0.1108(7) 0.173(4) Uiso 1 1 d D . . C1NC C 0.5108(6) 0.4223(2) 0.1831(3) 0.0719(18) Uani 1 1 d . . . H1NG H 0.4693 0.3949 0.1567 0.086 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 0.0311(3) 0.0168(3) 0.0206(3) 0.0000(2) 0.0059(2) -0.0022(2) Co2 0.0327(3) 0.0183(3) 0.0220(3) -0.0015(2) 0.0077(2) -0.0007(2) O1 0.0514(17) 0.0215(14) 0.0233(13) 0.0027(11) 0.0088(12) 0.0055(13) O2 0.072(2) 0.0176(14) 0.0231(14) -0.0017(11) 0.0077(13) 0.0040(14) O3 0.0587(19) 0.0245(15) 0.0293(15) -0.0028(12) 0.0018(13) 0.0144(14) O4 0.0651(19) 0.0198(14) 0.0250(15) -0.0023(11) 0.0096(13) 0.0060(14) O5 0.0277(14) 0.0178(13) 0.0296(14) 0.0014(11) 0.0064(11) -0.0006(11) O6 0.0338(16) 0.0267(16) 0.0492(18) -0.0096(13) 0.0067(13) -0.0019(13) O7 0.0286(14) 0.0274(15) 0.0386(15) -0.0059(12) 0.0078(12) -0.0007(12) O8 0.0294(14) 0.0225(14) 0.0306(14) -0.0050(11) 0.0071(11) -0.0017(12) N1 0.048(2) 0.0173(16) 0.0264(17) -0.0039(13) 0.0065(15) 0.0014(15) N2 0.0327(18) 0.0214(17) 0.0273(17) 0.0011(13) 0.0052(14) -0.0012(14) C1 0.052(3) 0.031(2) 0.024(2) 0.0044(17) 0.0054(18) 0.005(2) C2 0.058(3) 0.025(2) 0.027(2) 0.0003(17) 0.0067(19) 0.006(2) C3 0.072(3) 0.019(2) 0.021(2) -0.0031(16) 0.0027(19) 0.004(2) C4 0.093(4) 0.029(2) 0.026(2) 0.0025(18) 0.020(2) 0.010(2) C5 0.073(3) 0.024(2) 0.031(2) -0.0018(18) 0.019(2) 0.010(2) C6 0.077(3) 0.021(2) 0.025(2) -0.0038(17) 0.005(2) 0.009(2) C7 0.076(3) 0.024(2) 0.021(2) -0.0011(17) 0.007(2) 0.006(2) C8 0.062(3) 0.021(2) 0.026(2) -0.0037(16) 0.0098(19) 0.002(2) C9 0.060(3) 0.020(2) 0.024(2) 0.0036(16) 0.0099(18) 0.004(2) C10 0.063(3) 0.024(2) 0.021(2) -0.0009(16) 0.0096(19) 0.005(2) C11 0.078(3) 0.022(2) 0.022(2) -0.0001(17) 0.012(2) 0.010(2) C12 0.046(2) 0.026(2) 0.028(2) -0.0033(18) 0.0057(18) 0.0017(19) C13 0.052(3) 0.024(2) 0.027(2) 0.0012(18) 0.0117(19) 0.0060(19) C14 0.035(2) 0.027(2) 0.034(2) -0.0014(17) 0.0089(17) -0.0034(18) C15 0.037(2) 0.022(2) 0.040(2) -0.0017(18) 0.0084(18) -0.0066(18) C16 0.025(2) 0.025(2) 0.037(2) -0.0056(17) -0.0004(16) 0.0061(17) C17 0.033(2) 0.032(2) 0.027(2) -0.0059(17) 0.0046(17) -0.0029(18) C18 0.029(2) 0.027(2) 0.029(2) -0.0006(16) 0.0030(16) -0.0002(17) C19 0.029(2) 0.029(2) 0.027(2) -0.0057(17) 0.0019(16) -0.0002(17) C20 0.032(2) 0.029(2) 0.033(2) -0.0056(18) 0.0042(17) 0.0032(18) C21 0.029(2) 0.027(2) 0.030(2) -0.0034(17) 0.0021(16) -0.0006(17) C22 0.027(2) 0.026(2) 0.029(2) -0.0022(16) 0.0055(16) 0.0007(17) C23 0.028(2) 0.027(2) 0.030(2) -0.0017(17) 0.0048(16) 0.0030(17) C24 0.027(2) 0.026(2) 0.036(2) -0.0035(17) 0.0038(17) -0.0008(17) C25 0.027(2) 0.027(2) 0.031(2) -0.0008(17) 0.0053(16) -0.0007(18) C26 0.028(2) 0.028(2) 0.0225(19) -0.0040(16) 0.0011(15) 0.0042(18) C1NC 0.054(3) 0.116(5) 0.053(3) 0.023(3) 0.035(3) 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 1.995(2) . ? Co1 O3 2.188(3) 4_566 ? Co1 O4 2.092(3) 4_566 ? Co1 O5 2.069(2) . ? Co1 O6 2.359(3) . ? Co1 O7 2.031(3) 1_455 ? Co1 C12 2.460(4) 4_566 ? Co2 O2 2.081(3) 1_655 ? Co2 O5 2.144(2) 1_655 ? Co2 O8 2.038(2) . ? Co2 O1N 2.078(3) . ? Co2 N1 2.145(3) 3_465 ? Co2 N2 2.157(3) 3_566 ? O1 C13 1.262(4) . ? O2 C13 1.250(5) . ? O3 C12 1.250(4) . ? O4 C12 1.264(4) . ? O5 C25 1.285(4) . ? O6 C25 1.239(4) . ? O7 C26 1.273(4) . ? O8 C26 1.250(4) . ? N1 C5 1.325(5) . ? N1 C1 1.338(5) . ? N2 C18 1.337(5) . ? N2 C14 1.348(5) . ? C1 C2 1.387(5) . ? C2 C3 1.383(5) . ? C3 C4 1.385(6) . ? C3 C6 1.485(5) . ? C4 C5 1.386(6) . ? C6 C7 1.393(5) . ? C6 C11 1.394(5) . ? C7 C8 1.396(5) . ? C8 C9 1.379(5) . ? C8 C12 1.494(5) . ? C9 C10 1.404(5) . ? C10 C11 1.396(5) . ? C10 C13 1.491(5) . ? C14 C15 1.380(5) . ? C15 C16 1.389(5) . ? C16 C17 1.396(5) . ? C16 C19 1.482(5) . ? C17 C18 1.375(5) . ? C19 C24 1.392(5) . ? C19 C20 1.397(5) . ? C20 C21 1.387(5) . ? C21 C22 1.384(5) . ? C21 C25 1.503(5) . ? C22 C23 1.390(5) . ? C23 C24 1.386(5) . ? C23 C26 1.516(5) . ? O1N C1NC 1.215(6) . ? N1N C1NC 1.331(8) . ? N1N C1NA 1.455(8) . ? N1N C1NB 1.499(9) . ? 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 O1 Co1 O7 97.69(11) . 1_455 ? O1 Co1 O5 102.29(10) . . ? O7 Co1 O5 100.23(10) 1_455 . ? O1 Co1 O4 100.09(10) . 4_566 ? O7 Co1 O4 98.37(11) 1_455 4_566 ? O5 Co1 O4 148.53(11) . 4_566 ? O1 Co1 O3 160.95(10) . 4_566 ? O7 Co1 O3 90.02(11) 1_455 4_566 ? O5 Co1 O3 93.38(10) . 4_566 ? O4 Co1 O3 61.40(10) 4_566 4_566 ? O1 Co1 O6 91.42(11) . . ? O7 Co1 O6 158.80(10) 1_455 . ? O5 Co1 O6 58.98(9) . . ? O4 Co1 O6 98.82(10) 4_566 . ? O3 Co1 O6 87.40(11) 4_566 . ? O1 Co1 C12 130.87(12) . 4_566 ? O7 Co1 C12 94.83(12) 1_455 4_566 ? O5 Co1 C12 121.83(12) . 4_566 ? O4 Co1 C12 30.91(11) 4_566 4_566 ? O3 Co1 C12 30.49(11) 4_566 4_566 ? O6 Co1 C12 93.56(12) . 4_566 ? O8 Co2 O1N 176.73(11) . . ? O8 Co2 O2 94.06(11) . 1_655 ? O1N Co2 O2 89.00(12) . 1_655 ? O8 Co2 O5 86.90(10) . 1_655 ? O1N Co2 O5 94.11(11) . 1_655 ? O2 Co2 O5 92.58(10) 1_655 1_655 ? O8 Co2 N1 90.30(11) . 3_465 ? O1N Co2 N1 88.79(12) . 3_465 ? O2 Co2 N1 85.64(11) 1_655 3_465 ? O5 Co2 N1 176.57(11) 1_655 3_465 ? O8 Co2 N2 87.00(11) . 3_566 ? O1N Co2 N2 89.81(12) . 3_566 ? O2 Co2 N2 172.51(11) 1_655 3_566 ? O5 Co2 N2 94.87(10) 1_655 3_566 ? N1 Co2 N2 86.95(11) 3_465 3_566 ? C13 O1 Co1 122.5(2) . . ? C13 O2 Co2 142.6(3) . 1_455 ? C12 O3 Co1 86.8(2) . 4_565 ? C12 O4 Co1 90.8(2) . 4_565 ? C25 O5 Co1 96.1(2) . . ? C25 O5 Co2 132.3(2) . 1_455 ? Co1 O5 Co2 108.73(11) . 1_455 ? C25 O6 Co1 84.1(2) . . ? C26 O7 Co1 125.1(2) . 1_655 ? C26 O8 Co2 135.7(2) . . ? C5 N1 C1 116.2(3) . . ? C5 N1 Co2 120.8(3) . 3_465 ? C1 N1 Co2 122.9(3) . 3_465 ? C18 N2 C14 116.8(3) . . ? C18 N2 Co2 121.3(3) . 3_566 ? C14 N2 Co2 120.5(2) . 3_566 ? N1 C1 C2 124.3(4) . . ? C3 C2 C1 119.0(4) . . ? C2 C3 C4 116.8(4) . . ? C2 C3 C6 121.5(4) . . ? C4 C3 C6 121.7(4) . . ? C3 C4 C5 120.2(4) . . ? N1 C5 C4 123.4(4) . . ? C7 C6 C11 118.4(4) . . ? C7 C6 C3 120.8(4) . . ? C11 C6 C3 120.8(3) . . ? C6 C7 C8 121.0(4) . . ? C9 C8 C7 119.5(4) . . ? C9 C8 C12 120.1(4) . . ? C7 C8 C12 120.4(3) . . ? C8 C9 C10 120.9(4) . . ? C11 C10 C9 118.3(3) . . ? C11 C10 C13 120.6(3) . . ? C9 C10 C13 121.1(4) . . ? C6 C11 C10 121.6(4) . . ? O3 C12 O4 120.9(3) . . ? O3 C12 C8 119.5(3) . . ? O4 C12 C8 119.6(3) . . ? O3 C12 Co1 62.7(2) . 4_565 ? O4 C12 Co1 58.25(19) . 4_565 ? C8 C12 Co1 177.8(3) . 4_565 ? O2 C13 O1 126.0(4) . . ? O2 C13 C10 117.1(3) . . ? O1 C13 C10 116.9(3) . . ? N2 C14 C15 123.2(3) . . ? C14 C15 C16 119.6(4) . . ? C15 C16 C17 117.2(3) . . ? C15 C16 C19 121.6(4) . . ? C17 C16 C19 121.2(3) . . ? C18 C17 C16 119.4(4) . . ? N2 C18 C17 123.7(4) . . ? C24 C19 C20 118.3(3) . . ? C24 C19 C16 120.6(3) . . ? C20 C19 C16 121.1(3) . . ? C21 C20 C19 120.7(4) . . ? C22 C21 C20 120.3(4) . . ? C22 C21 C25 120.5(3) . . ? C20 C21 C25 119.1(3) . . ? C21 C22 C23 119.4(3) . . ? C24 C23 C22 120.2(3) . . ? C24 C23 C26 118.7(3) . . ? C22 C23 C26 121.1(3) . . ? C23 C24 C19 120.9(4) . . ? O6 C25 O5 120.8(3) . . ? O6 C25 C21 121.9(3) . . ? O5 C25 C21 117.3(3) . . ? O8 C26 O7 127.2(3) . . ? O8 C26 C23 115.8(3) . . ? O7 C26 C23 117.0(3) . . ? C1NC O1N Co2 130.2(4) . . ? C1NC N1N C1NA 118.8(7) . . ? C1NC N1N C1NB 120.7(7) . . ? C1NA N1N C1NB 120.2(8) . . ? O1N C1NC N1N 124.5(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.03 _refine_diff_density_min -0.70 _refine_diff_density_rms 0.09 #===END data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 825860' #TrackingRef '- Cobalt.CIF' # code COPMCN #5311 _refine_special_details ; Large displacement ellipsoids was observed for atoms C1NA, C1NB and C1NC in one solvent dmf molecule: because no satisfactory disorder model could be developed, these atoms were refined isotropically. AFIX 137 and AFIX 43 instructions were used to place H atoms on solvent dmf molecules. The occupancies of the DMF solvent molecules refined to 0.9, so both were subsequently treated as fully occupied. ; _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H7 N O4 Co, 2(C3 H7 N O)' _chemical_formula_sum 'C19 H21 Co N3 O6' _chemical_formula_weight 446.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.850(2) _cell_length_b 13.853(2) _cell_length_c 13.944(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.793(3) _cell_angle_gamma 90.00 _cell_volume 2078.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1190 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 20.6 _exptl_crystal_description NEEDLE _exptl_crystal_colour RED _exptl_crystal_size_max 0.608 _exptl_crystal_size_mid 0.063 _exptl_crystal_size_min 0.039 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.697 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS V2.10; Sheldrick, 1996)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 0 _diffrn_reflns_number 11203 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_sigmaI/netI 0.078 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4644 _reflns_number_gt 3461 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)' _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^)+(0.083P)^2^+8.342P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed+difmap' _refine_ls_hydrogen_treatment 'riding model+rigid rotor for Me groups' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4644 _refine_ls_number_parameters 251 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.104 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.197 _refine_ls_wR_factor_gt 0.181 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.005 _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 0.10650(5) 0.55813(4) 0.04996(5) 0.01397(19) Uani 1 1 d . . . N1 N -0.7138(3) 0.6062(3) 0.0970(3) 0.0182(8) Uani 1 1 d . . . O1 O 0.0393(3) 0.6333(3) 0.1386(3) 0.0234(8) Uani 1 1 d . . . O2 O -0.1264(3) 0.5385(2) 0.0573(3) 0.0239(8) Uani 1 1 d . . . O3 O 0.0159(3) 0.8546(2) 0.4247(3) 0.0220(8) Uani 1 1 d . . . O4 O -0.1583(3) 0.9437(3) 0.3504(3) 0.0232(8) Uani 1 1 d . . . C1 C -0.6242(5) 0.5404(4) 0.1120(4) 0.0248(11) Uani 1 1 d . . . H1A H -0.6458 0.4739 0.1037 0.030 Uiso 1 1 calc R . . C2 C -0.5017(5) 0.5665(4) 0.1391(4) 0.0248(11) Uani 1 1 d . . . H2A H -0.4410 0.5182 0.1486 0.030 Uiso 1 1 calc R . . C3 C -0.4675(4) 0.6637(4) 0.1524(4) 0.0205(10) Uani 1 1 d . . . C4 C -0.5608(4) 0.7307(4) 0.1392(4) 0.0229(11) Uani 1 1 d . . . H4A H -0.5416 0.7975 0.1494 0.028 Uiso 1 1 calc R . . C5 C -0.6808(4) 0.6995(4) 0.1112(4) 0.0223(11) Uani 1 1 d . . . H5A H -0.7432 0.7464 0.1016 0.027 Uiso 1 1 calc R . . C6 C -0.0854(4) 0.7351(4) 0.2401(4) 0.0179(10) Uani 1 1 d . . . H6A H 0.0008 0.7478 0.2628 0.021 Uiso 1 1 calc R . . C7 C -0.1551(4) 0.7901(3) 0.2796(4) 0.0173(9) Uani 1 1 d . . . C8 C -0.2814(4) 0.7693(4) 0.2486(4) 0.0202(10) Uani 1 1 d . . . H8A H -0.3296 0.8076 0.2738 0.024 Uiso 1 1 calc R . . C9 C -0.3361(4) 0.6920(4) 0.1803(4) 0.0199(10) Uani 1 1 d . . . C10 C -0.2662(4) 0.6402(4) 0.1396(4) 0.0200(10) Uani 1 1 d . . . H10A H -0.3039 0.5889 0.0916 0.024 Uiso 1 1 calc R . . C11 C -0.1410(4) 0.6622(3) 0.1680(4) 0.0176(10) Uani 1 1 d . . . C12 C -0.0947(4) 0.8694(3) 0.3574(4) 0.0177(10) Uani 1 1 d . . . C13 C -0.0708(4) 0.6065(4) 0.1181(4) 0.0196(10) Uani 1 1 d . . . O1N O -0.4708(5) 0.6750(4) -0.1154(4) 0.0633(15) Uani 1 1 d . . . N1N N -0.6243(7) 0.7740(6) -0.1241(5) 0.071(2) Uani 1 1 d D . . C1NA C -0.7137(13) 0.6953(9) -0.1552(12) 0.140(5) Uiso 1 1 d D . . H1NA H -0.7668 0.6997 -0.2310 0.210 Uiso 1 1 calc R . . H1NB H -0.7652 0.6998 -0.1157 0.210 Uiso 1 1 calc R . . H1NC H -0.6694 0.6335 -0.1397 0.210 Uiso 1 1 calc R . . C1NB C -0.6844(11) 0.8624(7) -0.1219(10) 0.108(4) Uiso 1 1 d D . . H1ND H -0.7158 0.8591 -0.0673 0.130 Uiso 1 1 calc R . . H1NE H -0.7538 0.8733 -0.1909 0.130 Uiso 1 1 calc R . . H1NF H -0.6248 0.9156 -0.1062 0.130 Uiso 1 1 calc R . . C1NC C -0.5140(8) 0.7530(7) -0.1086(7) 0.074(3) Uiso 1 1 d D . . H1NG H -0.4570 0.8054 -0.0888 0.089 Uiso 1 1 calc R . . O2N O -0.1452(6) 1.1124(5) -0.0970(7) 0.093(2) Uani 1 1 d . . . N2N N 0.0549(6) 1.0888(4) -0.0710(5) 0.0513(15) Uani 1 1 d D . . C2NA C 0.1843(8) 1.1098(8) -0.0096(7) 0.088(3) Uani 1 1 d D . . H1NH H 0.2215 1.1322 -0.0565 0.106 Uiso 1 1 calc R . . H1NI H 0.2271 1.0513 0.0274 0.106 Uiso 1 1 calc R . . H1NJ H 0.1924 1.1602 0.0422 0.106 Uiso 1 1 calc R . . C2NB C 0.0330(10) 1.0157(6) -0.1482(7) 0.081(3) Uani 1 1 d D . . H1NK H -0.0508 0.9894 -0.1693 0.097 Uiso 1 1 calc R . . H1NL H 0.0943 0.9640 -0.1186 0.097 Uiso 1 1 calc R . . H1NM H 0.0402 1.0434 -0.2101 0.097 Uiso 1 1 calc R . . C2NC C -0.0245(11) 1.1326(6) -0.0471(9) 0.082(3) Uani 1 1 d D . . H1NN H 0.0027 1.1803 0.0068 0.099 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 0.0097(3) 0.0142(3) 0.0190(3) 0.0003(3) 0.0070(2) 0.0000(2) N1 0.0129(19) 0.021(2) 0.023(2) -0.0017(17) 0.0091(16) -0.0007(16) O1 0.0180(17) 0.0266(19) 0.0313(19) -0.0023(16) 0.0161(15) 0.0008(14) O2 0.0232(18) 0.0211(19) 0.0293(19) -0.0082(15) 0.0129(15) 0.0024(14) O3 0.0179(17) 0.0223(18) 0.0251(18) -0.0065(15) 0.0084(14) -0.0052(14) O4 0.0163(16) 0.0226(18) 0.0321(19) -0.0068(16) 0.0116(14) 0.0006(14) C1 0.019(2) 0.022(3) 0.034(3) -0.003(2) 0.011(2) -0.002(2) C2 0.017(2) 0.020(3) 0.038(3) -0.002(2) 0.012(2) 0.000(2) C3 0.015(2) 0.024(3) 0.023(2) -0.006(2) 0.0093(19) -0.0034(19) C4 0.017(2) 0.021(3) 0.032(3) -0.005(2) 0.012(2) -0.004(2) C5 0.017(2) 0.021(3) 0.032(3) -0.002(2) 0.013(2) -0.0003(19) C6 0.013(2) 0.022(2) 0.020(2) 0.0015(19) 0.0086(18) -0.0006(18) C7 0.018(2) 0.017(2) 0.021(2) -0.0012(19) 0.0114(18) 0.0008(18) C8 0.014(2) 0.022(2) 0.027(3) -0.006(2) 0.0104(19) -0.0004(19) C9 0.015(2) 0.022(3) 0.024(2) -0.003(2) 0.0095(19) -0.0041(19) C10 0.014(2) 0.022(3) 0.024(2) -0.005(2) 0.0086(19) -0.0025(19) C11 0.016(2) 0.019(2) 0.022(2) 0.0017(19) 0.0116(18) 0.0027(18) C12 0.017(2) 0.021(2) 0.021(2) -0.004(2) 0.0131(19) -0.0059(19) C13 0.017(2) 0.022(3) 0.021(2) 0.002(2) 0.0083(19) 0.0033(19) O1N 0.074(4) 0.059(3) 0.067(3) 0.014(3) 0.038(3) 0.033(3) N1N 0.072(5) 0.097(6) 0.043(3) 0.011(4) 0.024(3) 0.048(4) O2N 0.070(4) 0.062(4) 0.149(7) 0.005(4) 0.048(4) 0.026(4) N2N 0.062(4) 0.045(3) 0.054(4) 0.004(3) 0.032(3) 0.010(3) C2NA 0.089(7) 0.098(8) 0.061(6) 0.016(5) 0.016(5) 0.004(6) C2NB 0.149(10) 0.046(5) 0.078(6) -0.019(5) 0.079(7) -0.008(6) C2NC 0.122(9) 0.048(5) 0.099(8) 0.003(5) 0.067(7) 0.026(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 O1 2.019(3) . ? Co1 O2 2.093(3) 3_565 ? Co1 O3 2.023(3) 4_575 ? Co1 O4 2.026(3) 2_545 ? Co1 N1 2.058(4) 1_655 ? N1 C5 1.342(6) . ? N1 C1 1.347(6) . ? O1 C13 1.268(6) . ? O2 C13 1.254(6) . ? O3 C12 1.268(6) . ? O4 C12 1.255(6) . ? O4 Co1 2.026(3) 2 ? C1 C2 1.386(7) . ? C2 C3 1.396(7) . ? C3 C4 1.395(7) . ? C3 C9 1.491(6) . ? C4 C5 1.378(7) . ? C6 C11 1.381(7) . ? C6 C7 1.396(6) . ? C7 C8 1.402(6) . ? C7 C12 1.498(6) . ? C8 C9 1.399(7) . ? C9 C10 1.384(7) . ? C10 C11 1.399(6) . ? C11 C13 1.503(6) . ? O1N C1NC 1.216(10) . ? N1N C1NC 1.266(9) . ? N1N C1NB 1.423(8) . ? N1N C1NA 1.454(9) . ? O2N C2NC 1.332(12) . ? N2N C2NC 1.276(9) . ? N2N C2NB 1.420(7) . ? N2N C2NA 1.438(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 O1 Co1 O3 91.02(15) . 4_575 ? O1 Co1 O4 93.89(15) . 2_545 ? O3 Co1 O4 163.35(14) 4_575 2_545 ? O1 Co1 N1 105.02(15) . 1_655 ? O3 Co1 N1 100.67(15) 4_575 1_655 ? O4 Co1 N1 93.40(15) 2_545 1_655 ? O1 Co1 O2 163.64(14) . 3_565 ? O3 Co1 O2 86.72(14) 4_575 3_565 ? O4 Co1 O2 84.10(14) 2_545 3_565 ? N1 Co1 O2 91.31(15) 1_655 3_565 ? O1 Co1 Co1 95.51(10) . 3_565 ? O3 Co1 Co1 82.75(10) 4_575 3_565 ? O4 Co1 Co1 80.95(10) 2_545 3_565 ? N1 Co1 Co1 159.06(12) 1_655 3_565 ? O2 Co1 Co1 68.14(10) 3_565 3_565 ? C5 N1 C1 117.8(4) . . ? C5 N1 Co1 123.9(3) . 1_455 ? C1 N1 Co1 118.3(3) . 1_455 ? C13 O1 Co1 110.1(3) . . ? C13 O2 Co1 141.2(3) . 3_565 ? C12 O3 Co1 123.5(3) . 4_576 ? C12 O4 Co1 126.1(3) . 2 ? N1 C1 C2 122.3(5) . . ? C1 C2 C3 120.0(5) . . ? C4 C3 C2 117.1(4) . . ? C4 C3 C9 122.8(5) . . ? C2 C3 C9 120.1(4) . . ? C5 C4 C3 119.7(5) . . ? N1 C5 C4 123.1(5) . . ? C11 C6 C7 120.3(4) . . ? C6 C7 C8 119.8(4) . . ? C6 C7 C12 120.3(4) . . ? C8 C7 C12 119.9(4) . . ? C9 C8 C7 119.8(4) . . ? C10 C9 C8 119.3(4) . . ? C10 C9 C3 119.7(4) . . ? C8 C9 C3 121.0(4) . . ? C9 C10 C11 121.1(4) . . ? C6 C11 C10 119.5(4) . . ? C6 C11 C13 121.6(4) . . ? C10 C11 C13 119.0(4) . . ? O4 C12 O3 126.2(4) . . ? O4 C12 C7 117.1(4) . . ? O3 C12 C7 116.7(4) . . ? O2 C13 O1 124.9(4) . . ? O2 C13 C11 117.6(4) . . ? O1 C13 C11 117.5(4) . . ? C1NC N1N C1NB 133.1(10) . . ? C1NC N1N C1NA 116.8(9) . . ? C1NB N1N C1NA 110.0(9) . . ? O1N C1NC N1N 128.9(10) . . ? C2NC N2N C2NB 128.0(8) . . ? C2NC N2N C2NA 117.9(8) . . ? C2NB N2N C2NA 114.0(8) . . ? N2N C2NC O2N 120.8(9) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.91 _refine_diff_density_min -0.88 _refine_diff_density_rms 0.12 #=== END data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 825861' #TrackingRef '- Cobalt.CIF' # code CODBPY #5443 _refine_special_details ? # 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 0.016 0.467 0.683 1299.1 541.4 _platon_squeeze_details ; The results above correspond to 271 electrons/Co3 or 6.75 lattice DMF/Co3 in unit cell. These molecules have been included in the formula. Coordinated DMF molecule was treated as half-occupancy, sharing an O atoms with a half-occupied water molecule. The H atoms of these molecules cannot be located, but have been included in the formula. The C-O11, C-O11 and C-O12 distances were restrained. ; _audit_creation_method SHELXL97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40.5 H27.5 Co3 N3.5 O14, 6.75(C3 H7 N O)' _chemical_formula_sum 'C60.75 H74.75 Co3 N10.25 O20.75' _chemical_formula_weight 1457.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.164(6) _cell_length_b 13.363(8) _cell_length_c 22.395(13) _cell_angle_alpha 86.833(9) _cell_angle_beta 80.346(8) _cell_angle_gamma 83.224(9) _cell_volume 2975(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2206 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 22.9 _exptl_crystal_description LATH _exptl_crystal_colour PURPLE _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1516 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.465 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS v2.03' _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6902 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury Laboratory Station 9.8' _diffrn_radiation_monochromator 'silicon (111)' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22034 _diffrn_reflns_av_R_equivalents 0.101 _diffrn_reflns_av_sigmaI/netI 0.173 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 24.71 _reflns_number_total 10100 _reflns_number_gt 4437 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1204P)^2^] 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 SHELXL _refine_ls_extinction_coef 0.0097(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10100 _refine_ls_number_parameters 543 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.138 _refine_ls_R_factor_gt 0.0799 _refine_ls_wR_factor_ref 0.224 _refine_ls_wR_factor_gt 0.203 _refine_ls_goodness_of_fit_ref 0.84 _refine_ls_restrained_S_all 0.84 _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 -0.07110(8) 0.20973(9) 0.27646(4) 0.0474(4) Uani 1 1 d . . . Co2 Co -0.32323(9) -0.00179(10) 0.27860(5) 0.0555(4) Uani 1 1 d . . . Co3 Co -0.43475(9) 0.04840(9) -0.16438(4) 0.0494(4) Uani 1 1 d . . . N1 N 0.0979(5) -0.1999(5) 0.6251(2) 0.0459(16) Uani 1 1 d . . . N2 N -0.5603(5) 0.7991(6) 0.1929(3) 0.064(2) Uani 1 1 d . . . N3 N -0.0447(5) 0.2122(5) 0.1781(2) 0.0474(17) Uani 1 1 d . . . O1 O -0.1938(4) -0.0539(4) 0.3388(2) 0.0555(15) Uani 1 1 d . . . O2 O -0.0878(4) 0.0562(5) 0.2743(2) 0.0608(17) Uani 1 1 d . . . O3 O 0.5154(4) -0.0528(4) 0.3320(2) 0.0566(15) Uani 1 1 d . . . O4 O 0.4243(4) -0.0013(4) 0.2502(2) 0.0477(13) Uani 1 1 d . . . O5 O -0.3889(5) 0.1452(5) 0.2902(2) 0.0568(15) Uani 1 1 d . . . O6 O -0.2626(4) 0.2755(4) 0.2792(2) 0.0542(15) Uani 1 1 d . . . O7 O -0.9735(5) 0.3586(4) 0.2720(2) 0.0587(15) Uani 1 1 d . . . O8 O -0.8655(4) 0.2039(5) 0.2737(2) 0.0461(13) Uani 1 1 d . . . O9 O -0.3486(5) 0.0814(5) -0.0815(2) 0.074(2) Uani 1 1 d . . . O10 O -0.2242(4) 0.0451(5) -0.1702(2) 0.0613(16) Uani 1 1 d . . . O11 O 0.2572(10) 0.0527(9) -0.2032(4) 0.067(3) Uiso 0.60 1 d PD . 1 O11' O 0.2762(13) -0.0113(9) -0.1867(6) 0.050(3) Uiso 0.40 1 d PD . 2 O12 O 0.3706(5) 0.0722(4) -0.1252(2) 0.0564(15) Uani 1 1 d D . . C1 C 0.2087(7) -0.1697(7) 0.5925(3) 0.064(3) Uani 1 1 d . . . H1A H 0.2829 -0.1685 0.6131 0.077 Uiso 1 1 calc R . . O1N O -0.4315(5) -0.1070(5) -0.1332(3) 0.082(2) Uani 1 1 d . . . N1N N -0.4577(13) -0.2316(10) -0.0634(6) 0.052(3) Uiso 0.50 1 d P . . C1NC C -0.4577(13) -0.1381(11) -0.0770(6) 0.037(3) Uiso 0.50 1 d P . . C1NB C -0.484(3) -0.261(2) -0.0025(13) 0.129(9) Uiso 0.50 1 d P . . C1NA C -0.427(2) -0.3097(17) -0.1068(10) 0.097(7) Uiso 0.50 1 d P . . C2 C 0.2281(7) -0.1397(8) 0.5315(3) 0.079(3) Uani 1 1 d . . . H2A H 0.3111 -0.1180 0.5123 0.095 Uiso 1 1 calc R . . C3 C 0.1229(6) -0.1424(6) 0.4993(3) 0.050(2) Uani 1 1 d . . . C4 C 0.0073(8) -0.1741(8) 0.5329(3) 0.074(3) Uani 1 1 d . . . H4A H -0.0680 -0.1776 0.5134 0.089 Uiso 1 1 calc R . . C5 C -0.0022(7) -0.1999(8) 0.5914(3) 0.076(3) Uani 1 1 d . . . H5A H -0.0855 -0.2200 0.6115 0.091 Uiso 1 1 calc R . . C6 C 0.1366(6) -0.1050(7) 0.4344(3) 0.052(2) Uani 1 1 d . . . C7 C 0.0233(7) -0.0786(7) 0.4046(3) 0.056(2) Uani 1 1 d . . . H7A H -0.0635 -0.0891 0.4256 0.067 Uiso 1 1 calc R . . C8 C 0.0356(6) -0.0388(6) 0.3469(3) 0.044(2) Uani 1 1 d . . . C9 C 0.1612(6) -0.0213(6) 0.3138(3) 0.046(2) Uani 1 1 d . . . H9A H 0.1692 0.0085 0.2740 0.055 Uiso 1 1 calc R . . C10 C 0.2743(6) -0.0495(6) 0.3414(3) 0.0410(19) Uani 1 1 d . . . C11 C 0.2625(6) -0.0886(6) 0.4000(3) 0.050(2) Uani 1 1 d . . . H11A H 0.3412 -0.1051 0.4177 0.060 Uiso 1 1 calc R . . C12 C -0.0884(6) -0.0085(6) 0.3163(3) 0.0417(19) Uani 1 1 d . . . C13 C 0.4137(6) -0.0349(6) 0.3053(3) 0.0415(19) Uani 1 1 d . . . C14 C -0.6697(9) 0.7643(8) 0.2328(4) 0.075(3) Uani 1 1 d . . . H14A H -0.7410 0.8132 0.2484 0.091 Uiso 1 1 calc R . . C15 C -0.6813(9) 0.6621(9) 0.2512(4) 0.074(3) Uani 1 1 d . . . H15A H -0.7577 0.6450 0.2788 0.089 Uiso 1 1 calc R . . C16 C -0.5799(8) 0.5858(7) 0.2288(4) 0.061(2) Uani 1 1 d . . . C17 C -0.4709(8) 0.6214(8) 0.1902(4) 0.073(3) Uani 1 1 d . . . H17A H -0.3977 0.5742 0.1743 0.088 Uiso 1 1 calc R . . C18 C -0.4655(9) 0.7210(8) 0.1745(4) 0.072(3) Uani 1 1 d . . . H18A H -0.3876 0.7379 0.1479 0.087 Uiso 1 1 calc R . . C19 C -0.5921(7) 0.4804(7) 0.2466(4) 0.055(2) Uani 1 1 d . . . C20 C -0.4860(7) 0.4130(7) 0.2572(4) 0.061(2) Uani 1 1 d . . . H20A H -0.4015 0.4377 0.2554 0.073 Uiso 1 1 calc R . . C21 C -0.4930(6) 0.3099(7) 0.2705(3) 0.052(2) Uani 1 1 d . . . C22 C -0.6221(7) 0.2738(7) 0.2752(3) 0.058(2) Uani 1 1 d . . . H22A H -0.6323 0.2044 0.2836 0.069 Uiso 1 1 calc R . . C23 C -0.7300(6) 0.3415(6) 0.2673(3) 0.0412(19) Uani 1 1 d . . . C24 C -0.7214(7) 0.4415(7) 0.2544(4) 0.055(2) Uani 1 1 d . . . H24A H -0.8000 0.4858 0.2505 0.066 Uiso 1 1 calc R . . C25 C -0.3734(7) 0.2375(7) 0.2808(3) 0.0443(19) Uani 1 1 d . . . C26 C -0.8655(6) 0.2968(7) 0.2713(3) 0.043(2) Uani 1 1 d . . . C27 C -0.1433(7) 0.2327(8) 0.1464(3) 0.076(3) Uani 1 1 d . . . H27A H -0.2272 0.2623 0.1668 0.091 Uiso 1 1 calc R . . C28 C -0.1335(7) 0.2140(8) 0.0853(3) 0.079(3) Uani 1 1 d . . . H28A H -0.2090 0.2308 0.0653 0.095 Uiso 1 1 calc R . . C29 C -0.0128(6) 0.1708(6) 0.0536(3) 0.050(2) Uani 1 1 d . . . C30 C 0.0935(7) 0.1588(7) 0.0856(3) 0.055(2) Uani 1 1 d . . . H30A H 0.1809 0.1372 0.0650 0.066 Uiso 1 1 calc R . . C31 C 0.0764(7) 0.1772(6) 0.1460(3) 0.051(2) Uani 1 1 d . . . H31A H 0.1519 0.1651 0.1664 0.061 Uiso 1 1 calc R . . C32 C -0.0018(7) 0.1409(6) -0.0114(3) 0.051(2) Uani 1 1 d . . . C33 C -0.1173(6) 0.1268(7) -0.0337(3) 0.058(2) Uani 1 1 d . . . H33A H -0.2026 0.1414 -0.0092 0.070 Uiso 1 1 calc R . . C34 C -0.1094(7) 0.0911(6) -0.0922(3) 0.051(2) Uani 1 1 d . . . C35 C 0.0120(7) 0.0704(7) -0.1283(3) 0.058(2) Uani 1 1 d . . . H35A H 0.0161 0.0471 -0.1679 0.069 Uiso 1 1 calc R . . C36 C 0.1343(7) 0.0839(8) -0.1064(3) 0.065(3) Uani 1 1 d . . . C37 C 0.1209(7) 0.1207(7) -0.0476(3) 0.056(2) Uani 1 1 d . . . H37A H 0.1995 0.1319 -0.0324 0.067 Uiso 1 1 calc R . . C38 C -0.2368(7) 0.0695(7) -0.1153(4) 0.060(2) Uani 1 1 d . . . C39 C 0.2666(7) 0.0553(7) -0.1459(3) 0.066(3) Uani 1 1 d D . . O1W O -0.2638(15) -0.1737(10) 0.2558(6) 0.223(6) 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 Co1 0.0148(5) 0.0919(9) 0.0385(6) -0.0016(5) -0.0092(4) -0.0114(5) Co2 0.0223(5) 0.0963(10) 0.0514(7) 0.0021(6) -0.0125(4) -0.0143(5) Co3 0.0156(5) 0.0944(10) 0.0413(6) -0.0109(6) -0.0079(4) -0.0107(5) N1 0.032(3) 0.074(5) 0.036(3) 0.009(3) -0.016(3) -0.014(3) N2 0.014(3) 0.109(6) 0.068(4) -0.044(4) -0.007(3) 0.013(3) N3 0.025(3) 0.091(5) 0.027(3) -0.003(3) -0.007(2) -0.009(3) O1 0.017(2) 0.102(5) 0.054(3) -0.001(3) -0.017(2) -0.016(3) O2 0.016(2) 0.134(6) 0.030(3) 0.017(3) -0.009(2) 0.002(3) O3 0.023(3) 0.099(5) 0.050(3) 0.001(3) -0.009(2) -0.016(3) O4 0.032(3) 0.072(4) 0.041(3) 0.002(3) -0.004(2) -0.017(3) O5 0.033(3) 0.073(5) 0.071(4) 0.003(3) -0.022(3) -0.016(3) O6 0.013(2) 0.111(5) 0.042(3) -0.001(3) -0.0079(19) -0.015(3) O7 0.021(3) 0.088(4) 0.068(4) 0.006(3) -0.008(2) -0.010(3) O8 0.019(2) 0.060(4) 0.059(3) 0.001(3) -0.006(2) -0.004(2) O9 0.020(3) 0.161(6) 0.048(3) -0.026(3) -0.007(2) -0.025(3) O10 0.021(3) 0.128(5) 0.041(3) -0.010(3) -0.014(2) -0.018(3) O12 0.032(3) 0.085(4) 0.056(3) -0.011(3) -0.011(2) -0.013(3) C1 0.028(4) 0.120(8) 0.051(5) 0.006(5) -0.021(4) -0.018(5) O1N 0.029(3) 0.116(6) 0.098(5) 0.003(4) -0.014(3) 0.007(3) C2 0.025(4) 0.179(11) 0.035(4) 0.007(5) -0.010(3) -0.020(5) C3 0.014(3) 0.089(7) 0.052(5) -0.012(4) -0.013(3) -0.009(4) C4 0.039(5) 0.149(10) 0.042(5) 0.007(5) -0.017(4) -0.033(5) C5 0.031(4) 0.165(10) 0.041(5) 0.018(5) -0.016(3) -0.043(5) C6 0.019(4) 0.094(7) 0.040(4) -0.007(4) -0.003(3) -0.002(4) C7 0.022(4) 0.105(7) 0.043(5) -0.010(4) -0.010(3) -0.011(4) C8 0.020(3) 0.086(6) 0.030(4) -0.007(4) -0.005(3) -0.017(4) C9 0.022(4) 0.073(6) 0.044(4) -0.012(4) -0.009(3) -0.003(4) C10 0.021(3) 0.072(6) 0.034(4) 0.005(4) -0.015(3) -0.012(3) C11 0.012(3) 0.090(6) 0.049(5) 0.001(4) -0.016(3) -0.003(4) C12 0.022(4) 0.060(6) 0.045(4) -0.019(4) -0.010(3) 0.006(3) C13 0.020(3) 0.059(6) 0.046(5) -0.011(4) -0.005(3) -0.003(3) C14 0.043(5) 0.082(8) 0.094(7) -0.002(6) 0.006(5) 0.000(5) C15 0.044(5) 0.101(9) 0.079(7) -0.007(6) -0.003(5) -0.018(5) C16 0.034(5) 0.053(6) 0.098(7) -0.006(5) -0.020(4) -0.004(4) C17 0.022(4) 0.084(8) 0.111(8) -0.010(6) 0.001(4) -0.005(4) C18 0.053(6) 0.083(8) 0.085(7) 0.002(6) -0.010(5) -0.024(6) C19 0.020(4) 0.066(6) 0.083(6) -0.010(5) -0.020(4) -0.002(4) C20 0.025(4) 0.079(7) 0.082(6) -0.007(5) -0.014(4) -0.012(4) C21 0.018(4) 0.089(7) 0.051(5) -0.009(5) -0.009(3) -0.008(4) C22 0.027(4) 0.093(7) 0.056(5) 0.003(5) -0.011(3) -0.019(4) C23 0.010(3) 0.060(6) 0.053(4) -0.005(4) -0.005(3) 0.001(3) C24 0.018(4) 0.066(7) 0.081(6) 0.003(5) -0.012(4) -0.006(4) C25 0.029(4) 0.061(6) 0.040(4) -0.004(4) -0.003(3) 0.002(4) C26 0.017(4) 0.075(7) 0.044(4) -0.004(4) -0.016(3) -0.010(4) C27 0.015(4) 0.171(10) 0.039(5) -0.022(5) -0.002(3) 0.001(5) C28 0.019(4) 0.176(10) 0.041(5) -0.028(5) -0.007(3) 0.006(5) C29 0.022(4) 0.090(7) 0.042(4) -0.006(4) -0.008(3) -0.012(4) C30 0.025(4) 0.097(7) 0.045(5) -0.005(4) -0.009(3) -0.009(4) C31 0.028(4) 0.091(7) 0.034(4) -0.008(4) -0.005(3) -0.004(4) C32 0.022(4) 0.085(6) 0.046(4) -0.016(4) -0.002(3) -0.006(4) C33 0.016(3) 0.120(8) 0.040(4) -0.020(5) -0.002(3) -0.011(4) C34 0.026(4) 0.086(7) 0.046(4) 0.000(4) -0.020(3) -0.011(4) C35 0.030(4) 0.111(8) 0.035(4) -0.014(4) -0.005(3) -0.013(4) C36 0.022(4) 0.138(9) 0.038(4) -0.018(5) -0.002(3) -0.022(4) C37 0.018(4) 0.098(7) 0.058(5) -0.017(5) -0.009(3) -0.014(4) C38 0.015(4) 0.111(8) 0.062(5) -0.006(5) -0.024(4) -0.016(4) C39 0.035(5) 0.111(8) 0.056(5) -0.013(5) -0.013(4) -0.015(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 O6 2.032(5) . ? Co1 O8 2.073(4) 1_655 ? Co1 O2 2.083(7) . ? Co1 N3 2.173(5) . ? Co1 N1 2.175(6) 2_556 ? Co1 O7 2.316(6) 1_655 ? Co1 C26 2.492(7) 1_655 ? Co2 O11 1.845(9) 2 ? Co2 O5 2.015(7) . ? Co2 O3 2.025(5) 1_455 ? Co2 O11' 2.036(13) 2 ? Co2 O1 2.075(5) . ? Co2 O1W 2.367(14) . ? Co3 O12 2.021(5) 1_455 ? Co3 O4 2.038(5) 2 ? Co3 N2 2.099(8) 2_465 ? Co3 O10 2.118(5) . ? Co3 O1N 2.153(7) . ? Co3 O9 2.267(5) . ? Co3 C38 2.499(6) . ? N1 C1 1.328(9) . ? N1 C5 1.364(8) . ? N1 Co1 2.175(6) 2_556 ? N2 C18 1.365(11) . ? N2 C14 1.412(11) . ? N2 Co3 2.099(8) 2_465 ? N3 C27 1.318(8) . ? N3 C31 1.362(9) . ? O1 C12 1.308(8) . ? O2 C12 1.242(9) . ? O3 C13 1.272(8) . ? O3 Co2 2.025(5) 1_655 ? O4 C13 1.280(8) . ? O4 Co3 2.038(5) 2 ? O5 C25 1.263(9) . ? O6 C25 1.283(9) . ? O7 C26 1.292(9) . ? O7 Co1 2.316(6) 1_455 ? O8 C26 1.240(9) . ? O8 Co1 2.073(4) 1_455 ? O9 C38 1.254(9) . ? O10 C38 1.271(9) . ? O11 C39 1.306(8) . ? O11 Co2 1.845(9) 2 ? O11' C39 1.294(8) . ? O11' Co2 2.036(13) 2 ? O12 C39 1.271(6) . ? O12 Co3 2.021(5) 1_655 ? C1 C2 1.391(10) . ? C1 H1A 0.9500 . ? O1N C1NC 1.298(14) . ? N1N C1NC 1.269(17) . ? N1N C1NB 1.39(3) . ? N1N C1NA 1.44(2) . ? C2 C3 1.391(9) . ? C2 H2A 0.9500 . ? C3 C4 1.383(10) . ? C3 C6 1.500(10) . ? C4 C5 1.326(10) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C11 1.412(9) . ? C6 C7 1.426(9) . ? C7 C8 1.360(10) . ? C7 H7A 0.9500 . ? C8 C9 1.403(9) . ? C8 C12 1.536(9) . ? C9 C10 1.398(9) . ? C9 H9A 0.9500 . ? C10 C11 1.377(9) . ? C10 C13 1.538(9) . ? C11 H11A 0.9500 . ? C14 C15 1.417(12) . ? C14 H14A 0.9500 . ? C15 C16 1.411(12) . ? C15 H15A 0.9500 . ? C16 C17 1.399(12) . ? C16 C19 1.456(11) . ? C17 C18 1.364(12) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.365(11) . ? C19 C24 1.450(10) . ? C20 C21 1.401(11) . ? C20 H20A 0.9500 . ? C21 C22 1.437(10) . ? C21 C25 1.503(10) . ? C22 C23 1.366(10) . ? C22 H22A 0.9500 . ? C23 C24 1.361(10) . ? C23 C26 1.553(9) . ? C24 H24A 0.9500 . ? C26 Co1 2.492(7) 1_455 ? C27 C28 1.389(10) . ? C27 H27A 0.9500 . ? C28 C29 1.389(10) . ? C28 H28A 0.9500 . ? C29 C30 1.383(9) . ? C29 C32 1.513(10) . ? C30 C31 1.368(9) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C37 1.375(9) . ? C32 C33 1.386(9) . ? C33 C34 1.406(10) . ? C33 H33A 0.9500 . ? C34 C35 1.364(10) . ? C34 C38 1.535(8) . ? C35 C36 1.445(9) . ? C35 H35A 0.9500 . ? C36 C37 1.411(10) . ? C36 C39 1.501(11) . ? C37 H37A 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 O6 Co1 O8 156.7(2) . 1_655 ? O6 Co1 O2 103.9(2) . . ? O8 Co1 O2 99.4(2) 1_655 . ? O6 Co1 N3 89.9(2) . . ? O8 Co1 N3 90.9(2) 1_655 . ? O2 Co1 N3 87.0(2) . . ? O6 Co1 N1 90.8(2) . 2_556 ? O8 Co1 N1 89.5(2) 1_655 2_556 ? O2 Co1 N1 90.5(2) . 2_556 ? N3 Co1 N1 177.4(3) . 2_556 ? O6 Co1 O7 96.1(2) . 1_655 ? O8 Co1 O7 60.6(2) 1_655 1_655 ? O2 Co1 O7 159.76(18) . 1_655 ? N3 Co1 O7 90.0(2) . 1_655 ? N1 Co1 O7 92.4(2) 2_556 1_655 ? O6 Co1 C26 127.0(3) . 1_655 ? O8 Co1 C26 29.8(2) 1_655 1_655 ? O2 Co1 C26 129.0(2) . 1_655 ? N3 Co1 C26 90.2(2) . 1_655 ? N1 Co1 C26 91.3(2) 2_556 1_655 ? O7 Co1 C26 30.9(2) 1_655 1_655 ? O11 Co2 O5 122.3(4) 2 . ? O11 Co2 O3 121.7(4) 2 1_455 ? O5 Co2 O3 94.9(2) . 1_455 ? O11 Co2 O11' 27.0(4) 2 2 ? O5 Co2 O11' 95.3(4) . 2 ? O3 Co2 O11' 130.7(4) 1_455 2 ? O11 Co2 O1 109.7(4) 2 . ? O5 Co2 O1 110.9(2) . . ? O3 Co2 O1 93.3(2) 1_455 . ? O11' Co2 O1 126.8(4) 2 . ? O11 Co2 O1W 53.4(5) 2 . ? O5 Co2 O1W 172.9(4) . . ? O3 Co2 O1W 84.1(4) 1_455 . ? O11' Co2 O1W 80.1(5) 2 . ? O1 Co2 O1W 76.2(4) . . ? O12 Co3 O4 109.25(19) 1_455 2 ? O12 Co3 N2 90.0(2) 1_455 2_465 ? O4 Co3 N2 92.9(2) 2 2_465 ? O12 Co3 O10 156.2(2) 1_455 . ? O4 Co3 O10 94.49(19) 2 . ? N2 Co3 O10 87.9(2) 2_465 . ? O12 Co3 O1N 89.2(2) 1_455 . ? O4 Co3 O1N 88.2(2) 2 . ? N2 Co3 O1N 178.8(3) 2_465 . ? O10 Co3 O1N 92.4(2) . . ? O12 Co3 O9 95.82(19) 1_455 . ? O4 Co3 O9 154.68(19) 2 . ? N2 Co3 O9 90.5(2) 2_465 . ? O10 Co3 O9 60.55(18) . . ? O1N Co3 O9 88.7(2) . . ? O12 Co3 C38 125.7(2) 1_455 . ? O4 Co3 C38 125.0(2) 2 . ? N2 Co3 C38 88.5(3) 2_465 . ? O10 Co3 C38 30.6(2) . . ? O1N Co3 C38 91.2(3) . . ? O9 Co3 C38 30.0(2) . . ? C1 N1 C5 112.0(6) . . ? C1 N1 Co1 121.2(5) . 2_556 ? C5 N1 Co1 125.1(5) . 2_556 ? C18 N2 C14 111.0(8) . . ? C18 N2 Co3 128.4(6) . 2_465 ? C14 N2 Co3 120.4(6) . 2_465 ? C27 N3 C31 115.6(6) . . ? C27 N3 Co1 124.3(5) . . ? C31 N3 Co1 119.4(4) . . ? C12 O1 Co2 100.8(4) . . ? C12 O2 Co1 128.6(5) . . ? C13 O3 Co2 109.2(4) . 1_655 ? C13 O4 Co3 141.3(5) . 2 ? C25 O5 Co2 151.0(5) . . ? C25 O6 Co1 131.4(6) . . ? C26 O7 Co1 82.1(5) . 1_455 ? C26 O8 Co1 94.2(4) . 1_455 ? C38 O9 Co3 85.3(4) . . ? C38 O10 Co3 91.5(4) . . ? C39 O11 Co2 149.1(9) . 2 ? C39 O11' Co2 130.5(10) . 2 ? C39 O12 Co3 128.6(5) . 1_655 ? N1 C1 C2 127.1(6) . . ? N1 C1 H1A 116.4 . . ? C2 C1 H1A 116.4 . . ? C1NC O1N Co3 125.3(8) . . ? C1NC N1N C1NB 118.4(17) . . ? C1NC N1N C1NA 124.3(15) . . ? C1NB N1N C1NA 117.3(18) . . ? N1N C1NC O1N 120.4(13) . . ? C3 C2 C1 118.3(7) . . ? C3 C2 H2A 120.9 . . ? C1 C2 H2A 120.9 . . ? C4 C3 C2 114.8(7) . . ? C4 C3 C6 125.0(6) . . ? C2 C3 C6 120.0(6) . . ? C5 C4 C3 122.5(7) . . ? C5 C4 H4A 118.8 . . ? C3 C4 H4A 118.8 . . ? C4 C5 N1 125.2(7) . . ? C4 C5 H5A 117.4 . . ? N1 C5 H5A 117.4 . . ? C11 C6 C7 115.7(6) . . ? C11 C6 C3 121.9(6) . . ? C7 C6 C3 122.3(6) . . ? C8 C7 C6 122.0(6) . . ? C8 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? C7 C8 C9 121.4(6) . . ? C7 C8 C12 121.1(6) . . ? C9 C8 C12 117.5(6) . . ? C10 C9 C8 117.6(7) . . ? C10 C9 H9A 121.2 . . ? C8 C9 H9A 121.2 . . ? C11 C10 C9 121.3(6) . . ? C11 C10 C13 120.0(6) . . ? C9 C10 C13 118.7(6) . . ? C10 C11 C6 121.9(6) . . ? C10 C11 H11A 119.1 . . ? C6 C11 H11A 119.1 . . ? O2 C12 O1 123.2(6) . . ? O2 C12 C8 121.8(6) . . ? O1 C12 C8 115.0(7) . . ? O3 C13 O4 121.7(6) . . ? O3 C13 C10 118.6(6) . . ? O4 C13 C10 119.7(6) . . ? N2 C14 C15 125.0(9) . . ? N2 C14 H14A 117.5 . . ? C15 C14 H14A 117.5 . . ? C16 C15 C14 120.2(8) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C17 C16 C15 114.2(9) . . ? C17 C16 C19 125.1(8) . . ? C15 C16 C19 120.7(8) . . ? C18 C17 C16 122.6(9) . . ? C18 C17 H17A 118.7 . . ? C16 C17 H17A 118.7 . . ? C17 C18 N2 126.9(9) . . ? C17 C18 H18A 116.6 . . ? N2 C18 H18A 116.6 . . ? C20 C19 C24 116.1(8) . . ? C20 C19 C16 123.4(7) . . ? C24 C19 C16 120.6(7) . . ? C19 C20 C21 124.6(7) . . ? C19 C20 H20A 117.7 . . ? C21 C20 H20A 117.7 . . ? C20 C21 C22 117.3(7) . . ? C20 C21 C25 123.1(7) . . ? C22 C21 C25 119.6(8) . . ? C23 C22 C21 118.5(8) . . ? C23 C22 H22A 120.7 . . ? C21 C22 H22A 120.7 . . ? C24 C23 C22 123.4(7) . . ? C24 C23 C26 120.9(6) . . ? C22 C23 C26 115.7(8) . . ? C23 C24 C19 119.9(7) . . ? C23 C24 H24A 120.0 . . ? C19 C24 H24A 120.0 . . ? O5 C25 O6 125.3(7) . . ? O5 C25 C21 118.3(7) . . ? O6 C25 C21 116.4(8) . . ? O8 C26 O7 123.0(6) . . ? O8 C26 C23 118.8(7) . . ? O7 C26 C23 118.2(8) . . ? O8 C26 Co1 56.0(3) . 1_455 ? O7 C26 Co1 67.0(4) . 1_455 ? C23 C26 Co1 174.8(6) . 1_455 ? N3 C27 C28 124.8(7) . . ? N3 C27 H27A 117.6 . . ? C28 C27 H27A 117.6 . . ? C27 C28 C29 119.6(7) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? C30 C29 C28 115.1(7) . . ? C30 C29 C32 123.8(6) . . ? C28 C29 C32 121.0(6) . . ? C31 C30 C29 121.9(7) . . ? C31 C30 H30A 119.1 . . ? C29 C30 H30A 119.1 . . ? N3 C31 C30 122.5(6) . . ? N3 C31 H31A 118.8 . . ? C30 C31 H31A 118.8 . . ? C37 C32 C33 119.1(7) . . ? C37 C32 C29 121.4(6) . . ? C33 C32 C29 119.3(6) . . ? C32 C33 C34 120.6(6) . . ? C32 C33 H33A 119.7 . . ? C34 C33 H33A 119.7 . . ? C35 C34 C33 120.6(6) . . ? C35 C34 C38 118.9(7) . . ? C33 C34 C38 120.4(6) . . ? C34 C35 C36 120.2(7) . . ? C34 C35 H35A 119.9 . . ? C36 C35 H35A 119.9 . . ? C37 C36 C35 116.9(6) . . ? C37 C36 C39 124.1(6) . . ? C35 C36 C39 118.9(6) . . ? C32 C37 C36 122.5(6) . . ? C32 C37 H37A 118.8 . . ? C36 C37 H37A 118.8 . . ? O9 C38 O10 122.6(6) . . ? O9 C38 C34 120.1(7) . . ? O10 C38 C34 117.2(6) . . ? O9 C38 Co3 64.7(3) . . ? O10 C38 Co3 57.9(3) . . ? C34 C38 Co3 172.6(6) . . ? O12 C39 O11' 119.9(9) . . ? O12 C39 O11 125.5(8) . . ? O11' C39 O11 41.6(6) . . ? O12 C39 C36 116.1(6) . . ? O11' C39 C36 120.1(8) . . ? O11 C39 C36 113.2(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.02 _refine_diff_density_min -0.70 _refine_diff_density_rms 0.13 #=== END of CIF