# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2011 data_global #TrackingRef '- p1-2-r1.cif' _journal_name_full 'RSC Advances' _journal_coden_cambridge 1500 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email dfsun@sdu.edu.cn _publ_contact_author_name 'Daofeng Sun' loop_ _publ_author_name 'Di Sun' 'Daofeng Sun' data_p1 #TrackingRef '- p1-2-r1.cif' _database_code_depnum_ccdc_archive 'CCDC 838340' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Co N6, 2(C5 H N4), 4(H2 O)' _chemical_formula_sum 'C40 H34 Co N14 O4' _chemical_formula_weight 833.74 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.8648(9) _cell_length_b 29.440(2) _cell_length_c 13.9210(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.890(2) _cell_angle_gamma 90.00 _cell_volume 4028.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5796 _cell_measurement_theta_min 4.453 _cell_measurement_theta_max 48.341 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 0.486 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9530 _exptl_absorpt_correction_T_max 0.9621 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19965 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7084 _reflns_number_gt 5127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+ (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0424P)^2^+0.8052P] 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 7084 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1040 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.04638(3) 0.653968(11) 0.52473(2) 0.02308(11) Uani 1 1 d . . . C1 C 0.3214(3) 0.68772(9) 0.62589(19) 0.0325(7) Uani 1 1 d . . . H1A H 0.3175 0.7099 0.5762 0.039 Uiso 1 1 calc R . . C2 C 0.4317(3) 0.68753(10) 0.6934(2) 0.0401(7) Uani 1 1 d . . . H2A H 0.5030 0.7090 0.6899 0.048 Uiso 1 1 calc R . . C3 C 0.4370(3) 0.65581(10) 0.7656(2) 0.0411(7) Uani 1 1 d . . . H3A H 0.5121 0.6551 0.8130 0.049 Uiso 1 1 calc R . . C4 C 0.3323(3) 0.62487(9) 0.76895(19) 0.0346(7) Uani 1 1 d . . . H4A H 0.3342 0.6029 0.8191 0.042 Uiso 1 1 calc R . . C5 C 0.2240(3) 0.62619(8) 0.69819(18) 0.0256(6) Uani 1 1 d . . . C6 C 0.1109(3) 0.59294(8) 0.69148(18) 0.0263(6) Uani 1 1 d . . . C7 C 0.0935(3) 0.56042(9) 0.7610(2) 0.0375(7) Uani 1 1 d . . . H7A H 0.1527 0.5595 0.8185 0.045 Uiso 1 1 calc R . . C8 C -0.0110(3) 0.52928(10) 0.7459(2) 0.0460(8) Uani 1 1 d . . . H8A H -0.0258 0.5072 0.7937 0.055 Uiso 1 1 calc R . . C9 C -0.0931(3) 0.53060(10) 0.6615(2) 0.0424(8) Uani 1 1 d . . . H9A H -0.1629 0.5087 0.6487 0.051 Uiso 1 1 calc R . . C10 C -0.0726(3) 0.56423(9) 0.5956(2) 0.0337(7) Uani 1 1 d . . . H10A H -0.1308 0.5654 0.5376 0.040 Uiso 1 1 calc R . . C11 C -0.1349(3) 0.68242(9) 0.68903(19) 0.0316(6) Uani 1 1 d . . . H11A H -0.1401 0.6507 0.7012 0.038 Uiso 1 1 calc R . . C12 C -0.1969(3) 0.71198(10) 0.7486(2) 0.0374(7) Uani 1 1 d . . . H12A H -0.2433 0.7009 0.8009 0.045 Uiso 1 1 calc R . . C13 C -0.1898(3) 0.75772(10) 0.7307(2) 0.0472(8) Uani 1 1 d . . . H13A H -0.2313 0.7788 0.7706 0.057 Uiso 1 1 calc R . . C14 C -0.1220(3) 0.77280(10) 0.6542(2) 0.0430(8) Uani 1 1 d . . . H14A H -0.1166 0.8044 0.6411 0.052 Uiso 1 1 calc R . . C15 C -0.0617(3) 0.74166(8) 0.59661(18) 0.0278(6) Uani 1 1 d . . . C16 C 0.0124(3) 0.75488(9) 0.51267(18) 0.0280(6) Uani 1 1 d . . . C17 C 0.0218(3) 0.79951(9) 0.4823(2) 0.0412(7) Uani 1 1 d . . . H17A H -0.0208 0.8232 0.5150 0.049 Uiso 1 1 calc R . . C18 C 0.0935(3) 0.80918(10) 0.4040(2) 0.0504(8) Uani 1 1 d . . . H18A H 0.1019 0.8396 0.3828 0.061 Uiso 1 1 calc R . . C19 C 0.1530(3) 0.77417(10) 0.3568(2) 0.0425(8) Uani 1 1 d . . . H19A H 0.2023 0.7800 0.3023 0.051 Uiso 1 1 calc R . . C20 C 0.1393(3) 0.73074(9) 0.39049(19) 0.0327(7) Uani 1 1 d . . . H20A H 0.1801 0.7066 0.3578 0.039 Uiso 1 1 calc R . . C21 C 0.2782(3) 0.60517(9) 0.4271(2) 0.0357(7) Uani 1 1 d . . . H21A H 0.3316 0.6112 0.4858 0.043 Uiso 1 1 calc R . . C22 C 0.3387(3) 0.58379(9) 0.3539(2) 0.0391(7) Uani 1 1 d . . . H22A H 0.4310 0.5743 0.3628 0.047 Uiso 1 1 calc R . . C23 C 0.2633(3) 0.57629(9) 0.2674(2) 0.0421(8) Uani 1 1 d . . . H23A H 0.3036 0.5629 0.2147 0.051 Uiso 1 1 calc R . . C24 C 0.1277(3) 0.58869(9) 0.2589(2) 0.0370(7) Uani 1 1 d . . . H24A H 0.0734 0.5835 0.2003 0.044 Uiso 1 1 calc R . . C25 C 0.0712(3) 0.60867(8) 0.33611(18) 0.0266(6) Uani 1 1 d . . . C26 C -0.0759(3) 0.62065(8) 0.33546(18) 0.0262(6) Uani 1 1 d . . . C27 C -0.1708(3) 0.61057(9) 0.2594(2) 0.0386(7) Uani 1 1 d . . . H27A H -0.1435 0.5962 0.2031 0.046 Uiso 1 1 calc R . . C28 C -0.3058(3) 0.62172(10) 0.2662(2) 0.0421(8) Uani 1 1 d . . . H28A H -0.3724 0.6147 0.2150 0.051 Uiso 1 1 calc R . . C29 C -0.3429(3) 0.64309(9) 0.3477(2) 0.0359(7) Uani 1 1 d . . . H29A H -0.4347 0.6516 0.3532 0.043 Uiso 1 1 calc R . . C30 C -0.2436(3) 0.65191(9) 0.42150(19) 0.0297(6) Uani 1 1 d . . . H30A H -0.2694 0.6662 0.4783 0.036 Uiso 1 1 calc R . . C31 C 0.5458(3) 0.51226(10) 0.8411(2) 0.0409(7) Uani 1 1 d . . . H31A H 0.5759 0.5052 0.9060 0.049 Uiso 1 1 calc R . . C32 C 0.4298(3) 0.51183(9) 0.7068(2) 0.0346(7) Uani 1 1 d . . . C33 C 0.5377(3) 0.54188(9) 0.7027(2) 0.0340(7) Uani 1 1 d . . . C34 C 0.5657(3) 0.57055(11) 0.6250(2) 0.0456(8) Uani 1 1 d . . . C35 C 0.3264(3) 0.50222(11) 0.6313(2) 0.0490(8) Uani 1 1 d . . . C36 C 0.5376(3) 0.60908(11) 0.0183(2) 0.0458(8) Uani 1 1 d . . . H36A H 0.5663 0.5795 0.0020 0.055 Uiso 1 1 calc R . . C37 C 0.5277(3) 0.68021(10) 0.0266(2) 0.0357(7) Uani 1 1 d . . . C38 C 0.4265(3) 0.66177(9) 0.07712(19) 0.0334(7) Uani 1 1 d . . . C39 C 0.3314(3) 0.68429(10) 0.1319(2) 0.0406(7) Uani 1 1 d . . . C40 C 0.5540(3) 0.72686(12) 0.0088(2) 0.0541(9) Uani 1 1 d . . . N1 N 0.2190(2) 0.65776(7) 0.62750(15) 0.0261(5) Uani 1 1 d . . . N2 N 0.0261(2) 0.59550(7) 0.60991(15) 0.0260(5) Uani 1 1 d . . . N3 N -0.0677(2) 0.69647(7) 0.61468(14) 0.0256(5) Uani 1 1 d . . . N4 N 0.0714(2) 0.72055(7) 0.46708(14) 0.0266(5) Uani 1 1 d . . . N5 N 0.1468(2) 0.61787(7) 0.41910(15) 0.0282(5) Uani 1 1 d . . . N6 N -0.1123(2) 0.64104(7) 0.41611(14) 0.0245(5) Uani 1 1 d . . . N7 N 0.5834(3) 0.59438(11) 0.5620(2) 0.0699(9) Uani 1 1 d . . . N8 N 0.2452(3) 0.49574(12) 0.5694(2) 0.0830(11) Uani 1 1 d . . . N9 N 0.4345(2) 0.49282(8) 0.79646(18) 0.0408(6) Uani 1 1 d . . . N10 N 0.6119(2) 0.54201(8) 0.78983(17) 0.0388(6) Uani 1 1 d . . . N11 N 0.4330(3) 0.61563(8) 0.07182(17) 0.0409(6) Uani 1 1 d . . . N12 N 0.6001(2) 0.64639(9) -0.01129(17) 0.0441(6) Uani 1 1 d . . . N13 N 0.2560(3) 0.70284(9) 0.1776(2) 0.0608(8) Uani 1 1 d . . . N14 N 0.5703(4) 0.76473(11) -0.0063(3) 0.0893(12) Uani 1 1 d . . . O1W O 0.2031(2) 0.56145(9) 0.0071(2) 0.0853(9) Uani 1 1 d . . . H1WA H 0.1262 0.5724 0.0178 0.102 Uiso 1 1 d R . . H1WB H 0.2648 0.5797 0.0291 0.102 Uiso 1 1 d R . . O2W O 0.7659(2) 0.52038(7) 0.07221(17) 0.0663(7) Uani 1 1 d . . . H2WA H 0.7286 0.5277 0.1228 0.080 Uiso 1 1 d R . . H2WB H 0.7806 0.4923 0.0638 0.080 Uiso 1 1 d R . . O3W O 0.9439(2) 0.58776(7) 0.02991(15) 0.0500(6) Uani 1 1 d . . . H3WA H 0.9101 0.5926 -0.0274 0.060 Uiso 1 1 d R . . H3WB H 0.9031 0.5631 0.0405 0.060 Uiso 1 1 d R . . O4W O 0.79215(19) 0.61334(6) 0.86169(14) 0.0429(5) Uani 1 1 d . . . H4WA H 0.7356 0.6257 0.8963 0.051 Uiso 1 1 d R . . H4WB H 0.7613 0.5899 0.8317 0.051 Uiso 1 1 d 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 0.02327(19) 0.0233(2) 0.02219(19) -0.00094(15) -0.00070(13) 0.00074(16) C1 0.0316(15) 0.0297(16) 0.0357(16) 0.0027(12) -0.0013(13) -0.0040(13) C2 0.0291(16) 0.0426(18) 0.0468(19) -0.0071(15) -0.0071(14) -0.0055(14) C3 0.0316(16) 0.0496(19) 0.0391(18) -0.0014(15) -0.0137(13) 0.0036(15) C4 0.0370(17) 0.0354(17) 0.0301(16) -0.0009(13) -0.0050(13) 0.0044(14) C5 0.0285(15) 0.0253(15) 0.0224(14) -0.0036(11) -0.0005(11) 0.0081(12) C6 0.0300(15) 0.0218(14) 0.0270(15) -0.0007(11) 0.0023(12) 0.0059(11) C7 0.0434(18) 0.0346(17) 0.0334(17) 0.0056(13) -0.0033(14) 0.0034(14) C8 0.056(2) 0.0342(18) 0.048(2) 0.0150(14) 0.0075(16) -0.0055(15) C9 0.0405(18) 0.0326(17) 0.053(2) 0.0081(14) 0.0002(15) -0.0081(14) C10 0.0349(16) 0.0282(16) 0.0371(17) -0.0002(13) -0.0020(13) -0.0028(13) C11 0.0302(15) 0.0339(16) 0.0312(16) -0.0010(12) 0.0055(12) -0.0009(12) C12 0.0370(17) 0.0451(19) 0.0311(16) -0.0032(13) 0.0090(13) -0.0004(14) C13 0.057(2) 0.0406(19) 0.047(2) -0.0149(15) 0.0194(16) 0.0061(16) C14 0.055(2) 0.0302(17) 0.0449(19) -0.0069(14) 0.0139(16) 0.0037(15) C15 0.0301(15) 0.0253(15) 0.0271(15) -0.0032(11) -0.0028(12) 0.0031(12) C16 0.0302(15) 0.0267(15) 0.0262(15) -0.0001(11) -0.0034(12) 0.0006(12) C17 0.058(2) 0.0271(16) 0.0395(18) 0.0031(13) 0.0079(15) 0.0030(15) C18 0.074(2) 0.0309(18) 0.048(2) 0.0096(15) 0.0100(18) -0.0048(17) C19 0.0508(19) 0.0423(19) 0.0357(17) 0.0098(14) 0.0100(15) -0.0041(16) C20 0.0353(16) 0.0339(16) 0.0292(16) 0.0018(12) 0.0038(13) 0.0013(13) C21 0.0286(16) 0.0350(17) 0.0435(18) -0.0018(13) 0.0034(13) 0.0043(13) C22 0.0327(16) 0.0312(17) 0.055(2) 0.0000(14) 0.0148(15) 0.0037(13) C23 0.052(2) 0.0337(17) 0.0440(19) -0.0058(14) 0.0235(15) 0.0035(15) C24 0.0513(19) 0.0305(16) 0.0296(16) -0.0048(12) 0.0063(14) -0.0019(14) C25 0.0346(15) 0.0221(14) 0.0234(14) 0.0013(11) 0.0038(12) -0.0009(12) C26 0.0346(15) 0.0205(14) 0.0235(14) 0.0006(11) 0.0012(12) -0.0026(12) C27 0.0509(19) 0.0364(17) 0.0274(16) -0.0062(12) -0.0035(14) -0.0033(14) C28 0.0401(18) 0.0442(19) 0.0388(18) -0.0018(14) -0.0155(15) -0.0088(15) C29 0.0253(15) 0.0383(17) 0.0427(18) 0.0068(13) -0.0053(13) -0.0034(13) C30 0.0275(15) 0.0306(15) 0.0310(15) 0.0023(12) 0.0018(12) -0.0008(12) C31 0.0480(19) 0.0414(18) 0.0331(17) 0.0017(14) 0.0020(14) 0.0072(15) C32 0.0345(16) 0.0319(16) 0.0373(17) -0.0086(13) 0.0017(13) 0.0045(13) C33 0.0330(16) 0.0361(17) 0.0329(17) -0.0023(13) 0.0032(13) 0.0064(13) C34 0.0325(17) 0.057(2) 0.048(2) 0.0052(17) 0.0035(15) 0.0046(15) C35 0.049(2) 0.045(2) 0.053(2) -0.0172(16) 0.0028(16) 0.0002(16) C36 0.060(2) 0.0380(18) 0.0385(19) -0.0029(14) -0.0020(16) 0.0167(17) C37 0.0371(17) 0.0360(17) 0.0332(16) -0.0028(13) -0.0022(13) 0.0027(14) C38 0.0369(16) 0.0349(17) 0.0280(15) -0.0039(12) -0.0007(12) 0.0042(13) C39 0.0444(19) 0.0353(18) 0.0423(19) 0.0033(14) 0.0049(15) -0.0023(15) C40 0.053(2) 0.052(2) 0.060(2) -0.0028(18) 0.0194(18) -0.0027(19) N1 0.0249(12) 0.0255(12) 0.0276(12) -0.0043(10) -0.0003(9) 0.0020(10) N2 0.0252(12) 0.0240(12) 0.0283(12) -0.0009(9) -0.0008(10) 0.0031(10) N3 0.0254(12) 0.0263(12) 0.0248(12) -0.0014(9) 0.0002(9) -0.0005(10) N4 0.0284(12) 0.0275(12) 0.0232(12) 0.0008(9) -0.0016(10) -0.0004(10) N5 0.0297(13) 0.0282(13) 0.0267(12) 0.0008(10) 0.0021(10) 0.0017(10) N6 0.0266(12) 0.0245(12) 0.0221(11) 0.0025(9) 0.0003(9) -0.0011(9) N7 0.0554(19) 0.091(2) 0.065(2) 0.0292(19) 0.0123(16) 0.0058(17) N8 0.069(2) 0.096(3) 0.079(2) -0.038(2) -0.0215(19) -0.0007(19) N9 0.0437(15) 0.0344(14) 0.0450(16) -0.0005(12) 0.0070(12) 0.0005(12) N10 0.0346(14) 0.0423(15) 0.0390(15) 0.0006(12) 0.0000(11) 0.0019(12) N11 0.0519(16) 0.0329(14) 0.0374(15) -0.0016(11) 0.0016(12) 0.0050(12) N12 0.0455(15) 0.0481(17) 0.0385(15) -0.0010(12) 0.0024(12) 0.0120(13) N13 0.068(2) 0.0527(18) 0.065(2) -0.0001(15) 0.0252(17) 0.0084(16) N14 0.104(3) 0.052(2) 0.120(3) 0.004(2) 0.054(2) -0.016(2) O1W 0.0482(15) 0.0836(19) 0.119(2) -0.0376(17) -0.0211(15) 0.0026(14) O2W 0.0789(17) 0.0518(14) 0.0728(17) 0.0186(12) 0.0336(14) 0.0155(13) O3W 0.0524(13) 0.0493(13) 0.0456(13) 0.0019(10) -0.0109(10) -0.0087(11) O4W 0.0414(12) 0.0470(13) 0.0407(12) -0.0012(9) 0.0064(10) -0.0029(10) _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 N2 2.109(2) . y Co1 N6 2.1164(19) . y Co1 N5 2.126(2) . y Co1 N1 2.132(2) . y Co1 N4 2.140(2) . y Co1 N3 2.154(2) . y C1 N1 1.343(3) . ? C1 C2 1.375(4) . ? C1 H1A 0.9500 . ? C2 C3 1.370(4) . ? C2 H2A 0.9500 . ? C3 C4 1.381(4) . ? C3 H3A 0.9500 . ? C4 C5 1.390(3) . ? C4 H4A 0.9500 . ? C5 N1 1.351(3) . ? C5 C6 1.481(4) . ? C6 N2 1.354(3) . ? C6 C7 1.382(4) . ? C7 C8 1.382(4) . ? C7 H7A 0.9500 . ? C8 C9 1.370(4) . ? C8 H8A 0.9500 . ? C9 C10 1.376(4) . ? C9 H9A 0.9500 . ? C10 N2 1.343(3) . ? C10 H10A 0.9500 . ? C11 N3 1.341(3) . ? C11 C12 1.381(4) . ? C11 H11A 0.9500 . ? C12 C13 1.372(4) . ? C12 H12A 0.9500 . ? C13 C14 1.378(4) . ? C13 H13A 0.9500 . ? C14 C15 1.385(4) . ? C14 H14A 0.9500 . ? C15 N3 1.356(3) . ? C15 C16 1.482(4) . ? C16 N4 1.352(3) . ? C16 C17 1.386(4) . ? C17 C18 1.378(4) . ? C17 H17A 0.9500 . ? C18 C19 1.380(4) . ? C18 H18A 0.9500 . ? C19 C20 1.373(4) . ? C19 H19A 0.9500 . ? C20 N4 1.341(3) . ? C20 H20A 0.9500 . ? C21 N5 1.345(3) . ? C21 C22 1.376(4) . ? C21 H21A 0.9500 . ? C22 C23 1.378(4) . ? C22 H22A 0.9500 . ? C23 C24 1.382(4) . ? C23 H23A 0.9500 . ? C24 C25 1.383(4) . ? C24 H24A 0.9500 . ? C25 N5 1.348(3) . ? C25 C26 1.493(4) . ? C26 N6 1.349(3) . ? C26 C27 1.385(3) . ? C27 C28 1.383(4) . ? C27 H27A 0.9500 . ? C28 C29 1.374(4) . ? C28 H28A 0.9500 . ? C29 C30 1.382(3) . ? C29 H29A 0.9500 . ? C30 N6 1.342(3) . ? C30 H30A 0.9500 . ? C31 N10 1.335(4) . ? C31 N9 1.342(3) . ? C31 H31A 0.9500 . ? C32 N9 1.365(3) . ? C32 C33 1.389(4) . ? C32 C35 1.429(4) . ? C33 N10 1.362(3) . ? C33 C34 1.418(4) . ? C34 N7 1.149(4) . ? C35 N8 1.142(4) . ? C36 N11 1.337(4) . ? C36 N12 1.341(4) . ? C36 H36A 0.9500 . ? C37 N12 1.358(4) . ? C37 C38 1.381(4) . ? C37 C40 1.423(4) . ? C38 N11 1.362(3) . ? C38 C39 1.423(4) . ? C39 N13 1.156(4) . ? C40 N14 1.148(4) . ? O1W H1WA 0.8499 . ? O1W H1WB 0.8499 . ? O2W H2WA 0.8500 . ? O2W H2WB 0.8502 . ? O3W H3WA 0.8500 . ? O3W H3WB 0.8500 . ? O4W H4WA 0.8500 . ? O4W H4WB 0.8499 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co1 N6 98.92(8) . . y N2 Co1 N5 93.04(8) . . y N6 Co1 N5 77.05(8) . . y N2 Co1 N1 76.94(8) . . y N6 Co1 N1 171.48(8) . . y N5 Co1 N1 95.61(8) . . y N2 Co1 N4 167.86(8) . . y N6 Co1 N4 89.93(7) . . y N5 Co1 N4 97.05(8) . . y N1 Co1 N4 95.31(8) . . y N2 Co1 N3 93.90(8) . . y N6 Co1 N3 97.38(8) . . y N5 Co1 N3 171.71(8) . . y N1 Co1 N3 90.37(7) . . y N4 Co1 N3 76.63(8) . . y N1 C1 C2 122.6(3) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C3 C2 C1 118.8(3) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C2 C3 C4 119.5(3) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C3 C4 C5 119.3(3) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? N1 C5 C4 120.9(2) . . ? N1 C5 C6 115.3(2) . . ? C4 C5 C6 123.7(2) . . ? N2 C6 C7 121.4(2) . . ? N2 C6 C5 115.1(2) . . ? C7 C6 C5 123.5(2) . . ? C8 C7 C6 119.2(3) . . ? C8 C7 H7A 120.4 . . ? C6 C7 H7A 120.4 . . ? C9 C8 C7 119.3(3) . . ? C9 C8 H8A 120.3 . . ? C7 C8 H8A 120.3 . . ? C8 C9 C10 118.9(3) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? N2 C10 C9 122.7(2) . . ? N2 C10 H10A 118.7 . . ? C9 C10 H10A 118.7 . . ? N3 C11 C12 122.9(3) . . ? N3 C11 H11A 118.6 . . ? C12 C11 H11A 118.6 . . ? C13 C12 C11 118.5(3) . . ? C13 C12 H12A 120.8 . . ? C11 C12 H12A 120.8 . . ? C12 C13 C14 119.5(3) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C13 C14 C15 119.6(3) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? N3 C15 C14 121.0(3) . . ? N3 C15 C16 115.8(2) . . ? C14 C15 C16 123.2(2) . . ? N4 C16 C17 121.5(3) . . ? N4 C16 C15 115.8(2) . . ? C17 C16 C15 122.7(2) . . ? C18 C17 C16 119.3(3) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 119.3(3) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? C20 C19 C18 118.3(3) . . ? C20 C19 H19A 120.8 . . ? C18 C19 H19A 120.8 . . ? N4 C20 C19 123.4(3) . . ? N4 C20 H20A 118.3 . . ? C19 C20 H20A 118.3 . . ? N5 C21 C22 122.8(3) . . ? N5 C21 H21A 118.6 . . ? C22 C21 H21A 118.6 . . ? C21 C22 C23 119.0(3) . . ? C21 C22 H22A 120.5 . . ? C23 C22 H22A 120.5 . . ? C22 C23 C24 118.6(3) . . ? C22 C23 H23A 120.7 . . ? C24 C23 H23A 120.7 . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? N5 C25 C24 121.4(2) . . ? N5 C25 C26 115.1(2) . . ? C24 C25 C26 123.5(2) . . ? N6 C26 C27 121.4(2) . . ? N6 C26 C25 115.3(2) . . ? C27 C26 C25 123.2(2) . . ? C28 C27 C26 119.3(3) . . ? C28 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? C29 C28 C27 119.4(2) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C28 C29 C30 118.6(3) . . ? C28 C29 H29A 120.7 . . ? C30 C29 H29A 120.7 . . ? N6 C30 C29 122.6(3) . . ? N6 C30 H30A 118.7 . . ? C29 C30 H30A 118.7 . . ? N10 C31 N9 116.8(3) . . ? N10 C31 H31A 121.6 . . ? N9 C31 H31A 121.6 . . ? N9 C32 C33 109.4(2) . . ? N9 C32 C35 123.9(3) . . ? C33 C32 C35 126.7(3) . . ? N10 C33 C32 108.7(3) . . ? N10 C33 C34 123.5(3) . . ? C32 C33 C34 127.6(3) . . ? N7 C34 C33 177.4(3) . . ? N8 C35 C32 177.7(4) . . ? N11 C36 N12 116.7(3) . . ? N11 C36 H36A 121.6 . . ? N12 C36 H36A 121.6 . . ? N12 C37 C38 109.7(3) . . ? N12 C37 C40 122.0(3) . . ? C38 C37 C40 128.2(3) . . ? N11 C38 C37 109.0(2) . . ? N11 C38 C39 122.0(3) . . ? C37 C38 C39 129.0(3) . . ? N13 C39 C38 178.7(3) . . ? N14 C40 C37 177.6(4) . . ? C1 N1 C5 118.9(2) . . ? C1 N1 Co1 125.62(17) . . ? C5 N1 Co1 115.48(16) . . ? C10 N2 C6 118.3(2) . . ? C10 N2 Co1 125.34(17) . . ? C6 N2 Co1 115.82(16) . . ? C11 N3 C15 118.5(2) . . ? C11 N3 Co1 125.91(17) . . ? C15 N3 Co1 115.40(17) . . ? C20 N4 C16 118.1(2) . . ? C20 N4 Co1 125.79(18) . . ? C16 N4 Co1 116.14(17) . . ? C21 N5 C25 118.3(2) . . ? C21 N5 Co1 125.75(18) . . ? C25 N5 Co1 115.91(16) . . ? C30 N6 C26 118.7(2) . . ? C30 N6 Co1 125.15(17) . . ? C26 N6 Co1 116.19(16) . . ? C31 N9 C32 102.2(2) . . ? C31 N10 C33 102.9(2) . . ? C36 N11 C38 102.5(2) . . ? C36 N12 C37 102.2(3) . . ? H1WA O1W H1WB 108.6 . . ? H2WA O2W H2WB 116.9 . . ? H3WA O3W H3WB 98.9 . . ? H4WA O4W H4WB 113.7 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O3W 0.85 1.88 2.717(3) 170.1 1_455 O1W H1WB N11 0.85 2.01 2.855(3) 170.3 . O2W H2WA N9 0.85 2.13 2.831(3) 140.0 3_666 O2W H2WB O1W 0.85 1.88 2.678(3) 156.2 3_665 O3W H3WA O4W 0.85 1.95 2.774(3) 162.9 1_554 O3W H3WB O2W 0.85 1.93 2.746(3) 161.9 . O4W H4WA N12 0.85 2.03 2.870(3) 171.6 1_556 O4W H4WB N10 0.85 2.09 2.875(3) 154.3 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.275 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.052 data_p2 #TrackingRef '- p1-2-r1.cif' _database_code_depnum_ccdc_archive 'CCDC 838341' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 Co N4 O2, 2(C5 H N4), 2(H2 O) ' _chemical_formula_sum 'C30 H26 Co N12 O4' _chemical_formula_weight 677.56 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 tetragonal _symmetry_space_group_name_H-M 'I 41 c d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-y, x+1/2, z+1/4' 'y+1/2, -x, z+3/4' 'x, -y, z+1/2' '-x+1/2, y+1/2, z' '-y, -x+1/2, z+3/4' 'y+1/2, x, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1, z+1' '-y+1/2, x+1, z+3/4' 'y+1, -x+1/2, z+5/4' 'x+1/2, -y+1/2, z+1' '-x+1, y+1, z+1/2' '-y+1/2, -x+1, z+5/4' 'y+1, x+1/2, z+3/4' _cell_length_a 16.2028(3) _cell_length_b 16.2028(3) _cell_length_c 24.4818(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6427.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4796 _cell_measurement_theta_min 4.213 _cell_measurement_theta_max 54.022 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9711 _exptl_absorpt_correction_T_max 0.9711 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12005 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 27.54 _reflns_number_total 3147 _reflns_number_gt 1930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT+ (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0347P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.30(3) _refine_ls_number_reflns 3147 _refine_ls_number_parameters 215 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.5000 0.0000 0.49615(7) 0.02262(13) Uani 1 2 d S . . C1 C 0.3824(2) -0.1362(2) 0.54117(19) 0.0406(11) Uani 1 1 d . . . H1B H 0.4130 -0.1268 0.5727 0.049 Uiso 1 1 calc R . . C2 C 0.3208(2) -0.1952(2) 0.54229(17) 0.0392(11) Uani 1 1 d . . . H2C H 0.3114 -0.2249 0.5742 0.047 Uiso 1 1 calc R . . C3 C 0.27349(18) -0.21056(19) 0.4969(2) 0.0302(8) Uani 1 1 d . . . C4 C 0.2908(2) -0.1639(2) 0.45094(18) 0.0387(10) Uani 1 1 d . . . H4A H 0.2605 -0.1714 0.4191 0.046 Uiso 1 1 calc R . . C5 C 0.3533(2) -0.1062(3) 0.45279(18) 0.0406(10) Uani 1 1 d . . . H5A H 0.3633 -0.0754 0.4214 0.049 Uiso 1 1 calc R . . C6 C 0.1555(2) -0.4048(2) 0.52864(16) 0.0321(10) Uani 1 1 d . . . H6A H 0.1611 -0.4504 0.5514 0.039 Uiso 1 1 calc R . . C7 C 0.2156(2) -0.3446(2) 0.52987(17) 0.0338(10) Uani 1 1 d . . . H7A H 0.2606 -0.3500 0.5531 0.041 Uiso 1 1 calc R . . C8 C 0.20883(19) -0.27565(17) 0.4963(2) 0.0295(8) Uani 1 1 d . . . C9 C 0.1400(2) -0.2708(2) 0.46285(16) 0.0366(10) Uani 1 1 d . . . H9A H 0.1326 -0.2260 0.4396 0.044 Uiso 1 1 calc R . . C10 C 0.0822(2) -0.3339(2) 0.46460(16) 0.0342(10) Uani 1 1 d . . . H10A H 0.0358 -0.3293 0.4425 0.041 Uiso 1 1 calc R . . C11 C 0.3609(3) -0.5059(3) 0.5395(2) 0.0559(12) Uani 1 1 d . . . H11A H 0.3322 -0.5533 0.5495 0.067 Uiso 1 1 calc R . . C12 C 0.4345(2) -0.3978(3) 0.54426(18) 0.0460(11) Uani 1 1 d . . . C13 C 0.4126(2) -0.4111(2) 0.49028(19) 0.0471(10) Uani 1 1 d . . . C14 C 0.4323(3) -0.3609(3) 0.4448(2) 0.0557(12) Uani 1 1 d . . . C15 C 0.4857(3) -0.3343(3) 0.56541(19) 0.0563(12) Uani 1 1 d . . . N1 N 0.39967(15) -0.09169(14) 0.4960(2) 0.0273(6) Uani 1 1 d . . . N2 N 0.08913(15) -0.40041(15) 0.4959(2) 0.0281(6) Uani 1 1 d . . . N3 N 0.4007(2) -0.4582(2) 0.57671(15) 0.0529(9) Uani 1 1 d . . . N4 N 0.3653(2) -0.4808(2) 0.48782(16) 0.0541(9) Uani 1 1 d . . . N5 N 0.5284(3) -0.2841(3) 0.58163(18) 0.0751(13) Uani 1 1 d . . . N6 N 0.4468(3) -0.3182(3) 0.40901(18) 0.0805(14) Uani 1 1 d . . . O1W O 0.5000 0.0000 0.4118(2) 0.0291(14) Uani 1 2 d S . . H1WA H 0.5087 -0.0397 0.3898 0.035 Uiso 1 1 d R . . O2W O 0.5000 0.0000 0.5796(2) 0.0355(15) Uani 1 2 d S . . H2WA H 0.5208 -0.0379 0.5993 0.043 Uiso 1 1 d R . . O3W O 0.56235(17) -0.12781(16) 0.63811(11) 0.0534(8) Uani 1 1 d . . . H3WA H 0.5437 -0.1275 0.6706 0.064 Uiso 1 1 d R . . H3WB H 0.5496 -0.1721 0.6215 0.064 Uiso 1 1 d 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 0.0185(3) 0.0191(3) 0.0303(3) 0.000 0.000 -0.0003(2) C1 0.041(2) 0.040(2) 0.041(3) 0.005(2) -0.011(2) -0.0157(18) C2 0.046(3) 0.037(2) 0.035(2) 0.008(2) 0.001(2) -0.0153(18) C3 0.0231(18) 0.0244(18) 0.043(2) 0.003(2) -0.003(3) -0.0032(14) C4 0.037(2) 0.040(2) 0.040(3) 0.009(2) -0.014(2) -0.0149(19) C5 0.036(2) 0.046(3) 0.040(3) 0.014(2) -0.007(2) -0.0127(18) C6 0.028(2) 0.028(2) 0.041(3) 0.0072(19) -0.0016(19) -0.0045(16) C7 0.024(2) 0.034(2) 0.043(3) 0.0025(19) -0.0086(19) -0.0047(16) C8 0.0278(19) 0.0234(18) 0.0373(19) 0.001(2) 0.001(2) -0.0076(14) C9 0.035(2) 0.028(2) 0.047(3) 0.0111(18) -0.007(2) -0.0072(17) C10 0.029(2) 0.027(2) 0.047(3) 0.0062(18) -0.0050(19) -0.0034(16) C11 0.057(3) 0.051(3) 0.059(3) 0.006(3) -0.012(3) 0.000(2) C12 0.045(2) 0.048(3) 0.044(3) -0.004(2) -0.014(2) 0.010(2) C13 0.047(2) 0.055(3) 0.039(3) -0.007(2) -0.001(2) 0.0074(17) C14 0.062(3) 0.064(3) 0.042(3) -0.008(3) -0.012(3) 0.007(3) C15 0.072(3) 0.051(3) 0.045(3) 0.004(2) -0.011(2) 0.008(2) N1 0.0244(15) 0.0207(15) 0.0368(15) 0.008(2) 0.002(2) -0.0032(10) N2 0.0221(15) 0.0246(16) 0.0377(16) -0.003(2) -0.004(2) -0.0047(10) N3 0.054(2) 0.057(2) 0.048(2) 0.004(2) -0.013(2) 0.0030(18) N4 0.050(2) 0.058(2) 0.054(3) -0.006(2) -0.009(2) 0.0004(17) N5 0.103(3) 0.062(3) 0.060(3) 0.001(2) -0.027(3) -0.014(2) N6 0.107(4) 0.084(3) 0.051(3) -0.010(2) -0.011(3) -0.013(3) O1W 0.042(3) 0.028(3) 0.017(3) 0.000 0.000 -0.0006(15) O2W 0.039(3) 0.020(2) 0.048(4) 0.000 0.000 0.0020(15) O3W 0.074(2) 0.0455(17) 0.0401(16) 0.0027(14) 0.0027(15) 0.0101(14) _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 O2W 2.043(6) . y Co1 O1W 2.065(5) . y Co1 N2 2.166(2) 6 y Co1 N2 2.166(2) 13_544 y Co1 N1 2.202(2) 10_544 y Co1 N1 2.202(2) . y C1 N1 1.350(6) . ? C1 C2 1.381(5) . ? C1 H1B 0.9300 . ? C2 C3 1.374(6) . ? C2 H2C 0.9300 . ? C3 C4 1.383(6) . ? C3 C8 1.487(3) . ? C4 C5 1.380(5) . ? C4 H4A 0.9300 . ? C5 N1 1.319(6) . ? C5 H5A 0.9300 . ? C6 N2 1.344(5) . ? C6 C7 1.379(5) . ? C6 H6A 0.9300 . ? C7 C8 1.391(5) . ? C7 H7A 0.9300 . ? C8 C9 1.386(5) . ? C9 C10 1.387(5) . ? C9 H9A 0.9300 . ? C10 N2 1.327(5) . ? C10 H10A 0.9300 . ? C11 N4 1.330(5) . ? C11 N3 1.358(5) . ? C11 H11A 0.9300 . ? C12 N3 1.375(5) . ? C12 C13 1.385(6) . ? C12 C15 1.419(6) . ? C13 N4 1.366(4) . ? C13 C14 1.414(7) . ? C14 N6 1.141(6) . ? C15 N5 1.139(5) . ? N2 Co1 2.166(2) 13_444 ? O1W H1WA 0.8499 . ? O2W H2WA 0.8499 . ? O3W H3WA 0.8501 . ? O3W H3WB 0.8500 . ? 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 O2W Co1 O1W 180.000(1) . . y O2W Co1 N2 90.19(13) . 6 y O1W Co1 N2 89.81(13) . 6 y O2W Co1 N2 90.19(13) . 13_544 y O1W Co1 N2 89.81(13) . 13_544 y N2 Co1 N2 179.6(3) 6 13_544 y O2W Co1 N1 90.11(13) . 10_544 y O1W Co1 N1 89.89(13) . 10_544 y N2 Co1 N1 89.40(9) 6 10_544 y N2 Co1 N1 90.60(9) 13_544 10_544 y O2W Co1 N1 90.11(13) . . y O1W Co1 N1 89.89(13) . . y N2 Co1 N1 90.60(9) 6 . y N2 Co1 N1 89.40(9) 13_544 . y N1 Co1 N1 179.8(3) 10_544 . y N1 C1 C2 122.4(4) . . ? N1 C1 H1B 118.8 . . ? C2 C1 H1B 118.8 . . ? C3 C2 C1 120.8(4) . . ? C3 C2 H2C 119.6 . . ? C1 C2 H2C 119.6 . . ? C2 C3 C4 116.5(3) . . ? C2 C3 C8 122.0(4) . . ? C4 C3 C8 121.5(4) . . ? C5 C4 C3 119.5(4) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? N1 C5 C4 124.5(4) . . ? N1 C5 H5A 117.8 . . ? C4 C5 H5A 117.8 . . ? N2 C6 C7 122.7(4) . . ? N2 C6 H6A 118.6 . . ? C7 C6 H6A 118.6 . . ? C6 C7 C8 120.0(4) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 117.3(3) . . ? C9 C8 C3 122.2(3) . . ? C7 C8 C3 120.6(3) . . ? C8 C9 C10 118.9(3) . . ? C8 C9 H9A 120.6 . . ? C10 C9 H9A 120.6 . . ? N2 C10 C9 124.0(3) . . ? N2 C10 H10A 118.0 . . ? C9 C10 H10A 118.0 . . ? N4 C11 N3 116.0(4) . . ? N4 C11 H11A 122.0 . . ? N3 C11 H11A 122.0 . . ? N3 C12 C13 109.8(4) . . ? N3 C12 C15 122.6(4) . . ? C13 C12 C15 127.6(4) . . ? N4 C13 C12 108.3(4) . . ? N4 C13 C14 124.5(4) . . ? C12 C13 C14 127.2(4) . . ? N6 C14 C13 177.6(6) . . ? N5 C15 C12 178.2(6) . . ? C5 N1 C1 116.3(3) . . ? C5 N1 Co1 122.9(3) . . ? C1 N1 Co1 120.8(3) . . ? C10 N2 C6 117.1(3) . . ? C10 N2 Co1 123.4(3) . 13_444 ? C6 N2 Co1 119.5(3) . 13_444 ? C11 N3 C12 101.9(4) . . ? C11 N4 C13 104.0(4) . . ? Co1 O1W H1WA 129.2 . . ? Co1 O2W H2WA 124.6 . . ? H3WA O3W H3WB 111.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA N3 0.85 1.90 2.718(5) 161.0 16_544 O2W H2WA O3W 0.85 1.87 2.713(4) 174.8 . O3W H3WA N4 0.85 1.94 2.778(5) 168.4 3_545 O3W H3WB N5 0.85 2.09 2.938(5) 175.2 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.250 _refine_diff_density_min -0.363 _refine_diff_density_rms 0.050