# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'En-Cui Yang' 'Xiao-Jun Zhao' _publ_contact_author_email xiaojun_zhao15@yahoo.com.cn _publ_contact_author_name 'Xiao-Jun Zhao' data_n110328b _database_code_depnum_ccdc_archive 'CCDC 865357' #TrackingRef 'N110328B.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H18 Co3.50 N12 O10.50 S' _chemical_formula_weight 784.74 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.143(2) _cell_length_b 12.699(2) _cell_length_c 15.039(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.866(3) _cell_angle_gamma 90.00 _cell_volume 2681.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3024 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 27.84 _exptl_crystal_description BLOCK _exptl_crystal_colour PINK _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1570 _exptl_absorpt_coefficient_mu 2.288 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7253 _exptl_absorpt_correction_T_max 0.7552 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13308 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4714 _reflns_number_gt 3534 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0285P)^2^+1.9323P] 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 4714 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 0.43260(3) 0.70126(4) 0.15819(3) 0.00855(13) Uani 1 1 d . . . Co2 Co 0.5000 0.5000 0.0000 0.00684(16) Uani 1 2 d S . . Co3 Co 0.35753(3) 0.88842(4) -0.22328(3) 0.00917(13) Uani 1 1 d . . . Co4 Co 0.31250(3) 0.81014(4) 0.30679(3) 0.00802(13) Uani 1 1 d . . . S1 S 0.73101(6) 0.44082(7) 0.41017(6) 0.0100(2) Uani 1 1 d . . . O1 O 0.39644(16) 0.7693(2) 0.42027(16) 0.0135(6) Uani 1 1 d . . . O2 O 0.42431(16) 0.6799(2) 0.30099(16) 0.0112(6) Uani 1 1 d . . . O3 O 0.60874(17) 0.7603(2) 0.69869(18) 0.0227(7) Uani 1 1 d . . . O4 O 0.75794(16) 0.7142(2) 0.67997(17) 0.0144(6) Uani 1 1 d . . . O5 O 0.80010(16) 0.5078(2) 0.37388(17) 0.0144(6) Uani 1 1 d . . . O6 O 0.67124(16) 0.3857(2) 0.34010(18) 0.0189(6) Uani 1 1 d . . . O7 O 0.77510(18) 0.3736(2) 0.48012(17) 0.0226(7) Uani 1 1 d . . . O8 O 0.22466(16) 0.6798(2) 0.34297(17) 0.0135(6) Uani 1 1 d . . . H8A H 0.2156 0.6617 0.3957 0.020 Uiso 1 1 d R . . H8B H 0.1708 0.6730 0.3118 0.020 Uiso 1 1 d R . . O9 O 0.41695(15) 0.7995(2) -0.31888(16) 0.0131(6) Uani 1 1 d . . . H9A H 0.3845 0.7454 -0.3361 0.020 Uiso 1 1 d R . . H9B H 0.4744 0.7784 -0.3106 0.020 Uiso 1 1 d R . . N1 N 0.57184(19) 0.6499(2) 0.1654(2) 0.0094(7) Uani 1 1 d . . . N2 N 0.59649(19) 0.5713(2) 0.1096(2) 0.0099(7) Uani 1 1 d . . . N3 N 0.72451(19) 0.6137(3) 0.2046(2) 0.0111(7) Uani 1 1 d . . . N4 N 0.36760(19) 0.5596(2) 0.14193(19) 0.0097(7) Uani 1 1 d . . . N5 N 0.39054(19) 0.4862(2) 0.08130(19) 0.0091(7) Uani 1 1 d . . . N6 N 0.27617(19) 0.4196(3) 0.1529(2) 0.0105(7) Uani 1 1 d . . . N7 N 0.42261(19) 0.7265(2) 0.0192(2) 0.0094(7) Uani 1 1 d . . . N8 N 0.44480(19) 0.6497(2) -0.0399(2) 0.0094(7) Uani 1 1 d . . . N9 N 0.38963(19) 0.7886(3) -0.1196(2) 0.0108(7) Uani 1 1 d . . . N10 N 0.41760(18) 0.9039(2) 0.2571(2) 0.0106(7) Uani 1 1 d . . . N11 N 0.45744(19) 0.8546(2) 0.1883(2) 0.0104(7) Uani 1 1 d . . . N12 N 0.53903(19) 1.0009(2) 0.2229(2) 0.0104(7) Uani 1 1 d . . . C1 C 0.6878(2) 0.5532(3) 0.1358(2) 0.0116(9) Uani 1 1 d . . . H1 H 0.7232 0.5031 0.1090 0.014 Uiso 1 1 calc R . . C2 C 0.6488(2) 0.6730(3) 0.2198(3) 0.0122(8) Uani 1 1 d . . . H2 H 0.6509 0.7245 0.2640 0.015 Uiso 1 1 calc R . . C3 C 0.3357(2) 0.4050(3) 0.0897(2) 0.0103(8) Uani 1 1 d . . . H3 H 0.3373 0.3438 0.0559 0.012 Uiso 1 1 calc R . . C4 C 0.2993(2) 0.5166(3) 0.1832(3) 0.0135(9) Uani 1 1 d . . . H4 H 0.2707 0.5500 0.2280 0.016 Uiso 1 1 calc R . . C5 C 0.4245(2) 0.6902(3) -0.1200(2) 0.0108(8) Uani 1 1 d . . . H5 H 0.4334 0.6542 -0.1723 0.013 Uiso 1 1 calc R . . C6 C 0.3904(2) 0.8068(3) -0.0309(2) 0.0118(8) Uani 1 1 d . . . H6 H 0.3703 0.8697 -0.0076 0.014 Uiso 1 1 calc R . . C7 C 0.5282(2) 0.9154(3) 0.1705(2) 0.0126(9) Uani 1 1 d . . . H7 H 0.5668 0.9005 0.1262 0.015 Uiso 1 1 calc R . . C8 C 0.4681(2) 0.9887(3) 0.2752(3) 0.0114(8) Uani 1 1 d . . . H8 H 0.4565 1.0363 0.3196 0.014 Uiso 1 1 calc R . . C9 C 0.5243(2) 0.6497(3) 0.4383(2) 0.0118(9) Uani 1 1 d . . . C10 C 0.5526(2) 0.6926(3) 0.5213(3) 0.0163(9) Uani 1 1 d . . . H10 H 0.5158 0.7449 0.5435 0.020 Uiso 1 1 calc R . . C11 C 0.6348(2) 0.6588(3) 0.5721(3) 0.0154(9) Uani 1 1 d . . . C12 C 0.6872(2) 0.5767(3) 0.5403(3) 0.0124(9) Uani 1 1 d . . . H12 H 0.7421 0.5523 0.5742 0.015 Uiso 1 1 calc R . . C13 C 0.6568(2) 0.5319(3) 0.4579(2) 0.0114(8) Uani 1 1 d . . . C14 C 0.5751(2) 0.5685(3) 0.4058(2) 0.0113(8) Uani 1 1 d . . . H14 H 0.5553 0.5386 0.3502 0.014 Uiso 1 1 calc R . . C15 C 0.4437(2) 0.7017(3) 0.3830(3) 0.0115(8) Uani 1 1 d . . . C16 C 0.6679(2) 0.7150(3) 0.6568(3) 0.0157(9) Uani 1 1 d . . . O10 O 0.4610(9) 0.9784(10) 0.4987(7) 0.098(5) Uani 0.50 1 d P . 1 O10' O 0.4039(8) 0.9718(18) 0.5248(9) 0.188(11) Uani 0.50 1 d P A 2 O11 O 0.6622(7) 0.8733(9) 0.4177(8) 0.108(4) Uani 0.50 1 d P . . 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 0.0094(2) 0.0073(3) 0.0092(3) -0.0014(2) 0.0021(2) -0.0012(2) Co2 0.0066(3) 0.0068(4) 0.0074(4) 0.0005(3) 0.0020(3) 0.0001(3) Co3 0.0068(2) 0.0082(3) 0.0121(3) 0.0020(2) -0.0004(2) -0.0012(2) Co4 0.0062(2) 0.0095(3) 0.0084(3) -0.0004(2) 0.00122(19) 0.0008(2) S1 0.0098(4) 0.0087(5) 0.0122(5) -0.0006(4) 0.0041(4) 0.0009(4) O1 0.0107(12) 0.0185(15) 0.0108(14) -0.0047(13) -0.0006(11) 0.0039(12) O2 0.0111(11) 0.0153(15) 0.0068(15) -0.0005(12) -0.0012(10) 0.0017(11) O3 0.0128(12) 0.0356(19) 0.0184(16) -0.0132(15) -0.0033(12) 0.0116(13) O4 0.0121(12) 0.0222(16) 0.0086(14) -0.0013(13) 0.0001(11) 0.0049(12) O5 0.0137(12) 0.0104(14) 0.0205(16) 0.0022(13) 0.0080(11) -0.0007(11) O6 0.0149(12) 0.0165(15) 0.0249(17) -0.0117(14) 0.0002(12) -0.0034(12) O7 0.0296(15) 0.0251(18) 0.0139(16) 0.0094(14) 0.0068(13) 0.0170(14) O8 0.0134(12) 0.0173(16) 0.0099(14) 0.0017(12) 0.0015(11) -0.0009(11) O9 0.0070(11) 0.0130(14) 0.0190(15) -0.0028(13) 0.0007(11) -0.0018(11) N1 0.0095(14) 0.0087(16) 0.0101(18) -0.0020(14) 0.0013(13) -0.0016(13) N2 0.0092(14) 0.0080(16) 0.0131(18) -0.0026(14) 0.0039(13) -0.0020(13) N3 0.0094(14) 0.0126(17) 0.0105(18) -0.0006(15) -0.0019(13) -0.0003(14) N4 0.0100(14) 0.0122(17) 0.0073(17) 0.0000(14) 0.0024(13) -0.0003(13) N5 0.0109(14) 0.0070(16) 0.0097(18) -0.0021(14) 0.0021(13) 0.0000(13) N6 0.0090(13) 0.0124(17) 0.0106(17) -0.0013(15) 0.0035(13) -0.0007(13) N7 0.0099(13) 0.0071(16) 0.0113(18) 0.0007(15) 0.0018(13) 0.0016(13) N8 0.0111(14) 0.0086(16) 0.0092(18) 0.0002(14) 0.0042(13) 0.0017(13) N9 0.0104(14) 0.0134(18) 0.0089(17) -0.0029(15) 0.0020(13) -0.0011(14) N10 0.0085(13) 0.0110(17) 0.0131(18) -0.0006(15) 0.0041(13) 0.0005(14) N11 0.0090(13) 0.0116(17) 0.0107(18) -0.0052(15) 0.0014(13) -0.0018(13) N12 0.0104(13) 0.0087(16) 0.0121(18) -0.0005(15) 0.0013(13) 0.0009(14) C1 0.0110(16) 0.010(2) 0.014(2) -0.0007(18) 0.0029(16) 0.0024(16) C2 0.0146(17) 0.011(2) 0.012(2) -0.0024(18) 0.0031(16) 0.0017(16) C3 0.0106(16) 0.0084(19) 0.012(2) -0.0025(17) 0.0022(16) -0.0022(16) C4 0.0111(17) 0.015(2) 0.016(2) -0.0040(18) 0.0070(16) -0.0012(16) C5 0.0119(17) 0.010(2) 0.011(2) -0.0022(18) 0.0043(15) 0.0017(16) C6 0.0110(16) 0.012(2) 0.013(2) 0.0018(18) 0.0024(16) 0.0012(16) C7 0.0122(17) 0.013(2) 0.013(2) -0.0005(18) 0.0038(16) -0.0006(16) C8 0.0093(16) 0.0081(19) 0.018(2) -0.0020(18) 0.0057(16) 0.0018(16) C9 0.0078(16) 0.018(2) 0.010(2) -0.0021(18) 0.0015(15) -0.0012(16) C10 0.0152(18) 0.016(2) 0.018(2) -0.003(2) 0.0025(17) 0.0059(18) C11 0.0121(17) 0.024(2) 0.010(2) -0.0006(19) -0.0005(16) 0.0027(17) C12 0.0059(15) 0.017(2) 0.014(2) -0.0009(18) 0.0010(15) 0.0031(16) C13 0.0159(17) 0.011(2) 0.008(2) 0.0029(17) 0.0035(16) 0.0053(16) C14 0.0115(16) 0.014(2) 0.008(2) 0.0009(17) 0.0015(16) -0.0012(16) C15 0.0098(16) 0.011(2) 0.014(2) 0.0041(18) 0.0046(16) -0.0028(16) C16 0.0150(18) 0.018(2) 0.013(2) -0.0013(19) -0.0033(17) 0.0094(17) O10 0.153(13) 0.103(10) 0.039(6) 0.008(6) 0.015(8) -0.062(9) O10' 0.073(8) 0.39(3) 0.088(10) -0.118(14) -0.037(6) 0.103(13) O11 0.088(7) 0.101(9) 0.141(10) 0.035(8) 0.043(7) -0.047(7) _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 N11 2.021(3) . ? Co1 N4 2.021(3) . ? Co1 N1 2.065(3) . ? Co1 N7 2.103(3) . ? Co1 O2 2.182(2) . ? Co2 N5 2.092(2) 3_665 ? Co2 N5 2.092(2) . ? Co2 N8 2.114(3) 3_665 ? Co2 N8 2.114(3) . ? Co2 N2 2.204(3) . ? Co2 N2 2.204(3) 3_665 ? Co3 N9 2.019(3) . ? Co3 N12 2.029(3) 3_675 ? Co3 N3 2.057(3) 4_575 ? Co3 O9 2.082(2) . ? Co3 O5 2.195(2) 4_575 ? Co4 O4 1.994(3) 4_575 ? Co4 N6 2.013(3) 2 ? Co4 O1 2.026(3) . ? Co4 N10 2.109(3) . ? Co4 O8 2.177(2) . ? Co4 O2 2.297(2) . ? Co4 C15 2.479(4) . ? S1 O7 1.438(3) . ? S1 O6 1.450(3) . ? S1 O5 1.450(2) . ? S1 C13 1.770(3) . ? O1 C15 1.260(4) . ? O2 C15 1.262(4) . ? O3 C16 1.247(4) . ? O4 C16 1.279(4) . ? O4 Co4 1.994(3) 4_676 ? O5 Co3 2.195(2) 4_676 ? O8 H8A 0.8499 . ? O8 H8B 0.8499 . ? O9 H9A 0.8500 . ? O9 H9B 0.8500 . ? N1 C2 1.315(5) . ? N1 N2 1.375(4) . ? N2 C1 1.324(4) . ? N3 C1 1.343(5) . ? N3 C2 1.351(4) . ? N3 Co3 2.056(3) 4_676 ? N4 C4 1.326(4) . ? N4 N5 1.370(4) . ? N5 C3 1.305(5) . ? N6 C4 1.340(5) . ? N6 C3 1.356(4) . ? N6 Co4 2.013(3) 2_545 ? N7 C6 1.316(5) . ? N7 N8 1.380(4) . ? N8 C5 1.311(5) . ? N9 C5 1.344(5) . ? N9 C6 1.352(4) . ? N10 C8 1.303(5) . ? N10 N11 1.386(4) . ? N11 C7 1.316(4) . ? N12 C7 1.339(5) . ? N12 C8 1.355(4) . ? N12 Co3 2.029(3) 3_675 ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C9 C10 1.378(5) . ? C9 C14 1.379(5) . ? C9 C15 1.483(5) . ? C10 C11 1.381(5) . ? C10 H10 0.9300 . ? C11 C12 1.395(5) . ? C11 C16 1.486(6) . ? C12 C13 1.385(5) . ? C12 H12 0.9300 . ? C13 C14 1.395(5) . ? C14 H14 0.9300 . ? O10 O10 1.23(2) 3_676 ? 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 N11 Co1 N4 161.62(10) . . ? N11 Co1 N1 98.84(12) . . ? N4 Co1 N1 98.18(12) . . ? N11 Co1 N7 93.74(12) . . ? N4 Co1 N7 92.27(12) . . ? N1 Co1 N7 92.88(11) . . ? N11 Co1 O2 85.87(11) . . ? N4 Co1 O2 86.05(10) . . ? N1 Co1 O2 94.15(10) . . ? N7 Co1 O2 172.93(10) . . ? N5 Co2 N5 180.00(12) 3_665 . ? N5 Co2 N8 88.11(11) 3_665 3_665 ? N5 Co2 N8 91.89(11) . 3_665 ? N5 Co2 N8 91.89(11) 3_665 . ? N5 Co2 N8 88.11(11) . . ? N8 Co2 N8 180.0 3_665 . ? N5 Co2 N2 88.13(10) 3_665 . ? N5 Co2 N2 91.87(10) . . ? N8 Co2 N2 88.99(12) 3_665 . ? N8 Co2 N2 91.01(12) . . ? N5 Co2 N2 91.87(10) 3_665 3_665 ? N5 Co2 N2 88.13(10) . 3_665 ? N8 Co2 N2 91.01(12) 3_665 3_665 ? N8 Co2 N2 88.99(12) . 3_665 ? N2 Co2 N2 180.0 . 3_665 ? N9 Co3 N12 109.74(12) . 3_675 ? N9 Co3 N3 120.43(12) . 4_575 ? N12 Co3 N3 128.62(13) 3_675 4_575 ? N9 Co3 O9 96.94(11) . . ? N12 Co3 O9 91.55(10) 3_675 . ? N3 Co3 O9 92.76(11) 4_575 . ? N9 Co3 O5 85.98(11) . 4_575 ? N12 Co3 O5 84.61(10) 3_675 4_575 ? N3 Co3 O5 88.33(11) 4_575 4_575 ? O9 Co3 O5 175.80(10) . 4_575 ? O4 Co4 N6 102.22(12) 4_575 2 ? O4 Co4 O1 152.42(11) 4_575 . ? N6 Co4 O1 104.26(11) 2 . ? O4 Co4 N10 87.57(11) 4_575 . ? N6 Co4 N10 101.98(12) 2 . ? O1 Co4 N10 94.36(11) . . ? O4 Co4 O8 87.36(10) 4_575 . ? N6 Co4 O8 93.14(10) 2 . ? O1 Co4 O8 83.64(10) . . ? N10 Co4 O8 164.75(10) . . ? O4 Co4 O2 92.37(10) 4_575 . ? N6 Co4 O2 164.75(11) 2 . ? O1 Co4 O2 60.73(9) . . ? N10 Co4 O2 82.86(10) . . ? O8 Co4 O2 83.00(9) . . ? O4 Co4 C15 122.59(12) 4_575 . ? N6 Co4 C15 134.66(13) 2 . ? O1 Co4 C15 30.41(11) . . ? N10 Co4 C15 87.53(11) . . ? O8 Co4 C15 83.13(10) . . ? O2 Co4 C15 30.34(10) . . ? O7 S1 O6 114.14(18) . . ? O7 S1 O5 111.76(16) . . ? O6 S1 O5 111.72(16) . . ? O7 S1 C13 108.54(16) . . ? O6 S1 C13 106.69(17) . . ? O5 S1 C13 103.22(16) . . ? C15 O1 Co4 95.1(2) . . ? C15 O2 Co1 154.6(2) . . ? C15 O2 Co4 82.8(2) . . ? Co1 O2 Co4 93.78(10) . . ? C16 O4 Co4 121.4(2) . 4_676 ? S1 O5 Co3 157.28(17) . 4_676 ? Co4 O8 H8A 126.4 . . ? Co4 O8 H8B 116.1 . . ? H8A O8 H8B 105.2 . . ? Co3 O9 H9A 113.6 . . ? Co3 O9 H9B 121.8 . . ? H9A O9 H9B 105.2 . . ? C2 N1 N2 106.9(3) . . ? C2 N1 Co1 132.5(2) . . ? N2 N1 Co1 120.5(2) . . ? C1 N2 N1 104.7(3) . . ? C1 N2 Co2 130.2(2) . . ? N1 N2 Co2 125.1(2) . . ? C1 N3 C2 102.0(3) . . ? C1 N3 Co3 130.1(2) . 4_676 ? C2 N3 Co3 127.7(3) . 4_676 ? C4 N4 N5 105.9(3) . . ? C4 N4 Co1 131.0(2) . . ? N5 N4 Co1 123.07(19) . . ? C3 N5 N4 106.4(2) . . ? C3 N5 Co2 127.8(2) . . ? N4 N5 Co2 125.6(2) . . ? C4 N6 C3 102.5(3) . . ? C4 N6 Co4 131.9(2) . 2_545 ? C3 N6 Co4 125.3(3) . 2_545 ? C6 N7 N8 105.7(3) . . ? C6 N7 Co1 131.6(2) . . ? N8 N7 Co1 122.6(2) . . ? C5 N8 N7 105.8(3) . . ? C5 N8 Co2 130.3(2) . . ? N7 N8 Co2 123.9(2) . . ? C5 N9 C6 101.8(3) . . ? C5 N9 Co3 129.0(2) . . ? C6 N9 Co3 129.0(3) . . ? C8 N10 N11 105.5(3) . . ? C8 N10 Co4 141.7(2) . . ? N11 N10 Co4 112.1(2) . . ? C7 N11 N10 105.9(3) . . ? C7 N11 Co1 129.5(2) . . ? N10 N11 Co1 121.8(2) . . ? C7 N12 C8 102.0(3) . . ? C7 N12 Co3 126.5(2) . 3_675 ? C8 N12 Co3 131.4(3) . 3_675 ? N2 C1 N3 113.8(3) . . ? N2 C1 H1 123.1 . . ? N3 C1 H1 123.1 . . ? N1 C2 N3 112.5(3) . . ? N1 C2 H2 123.7 . . ? N3 C2 H2 123.7 . . ? N5 C3 N6 112.7(3) . . ? N5 C3 H3 123.7 . . ? N6 C3 H3 123.7 . . ? N4 C4 N6 112.4(3) . . ? N4 C4 H4 123.8 . . ? N6 C4 H4 123.8 . . ? N8 C5 N9 113.6(3) . . ? N8 C5 H5 123.2 . . ? N9 C5 H5 123.2 . . ? N7 C6 N9 113.1(3) . . ? N7 C6 H6 123.4 . . ? N9 C6 H6 123.4 . . ? N11 C7 N12 113.1(3) . . ? N11 C7 H7 123.5 . . ? N12 C7 H7 123.5 . . ? N10 C8 N12 113.5(3) . . ? N10 C8 H8 123.3 . . ? N12 C8 H8 123.3 . . ? C10 C9 C14 120.7(4) . . ? C10 C9 C15 116.9(3) . . ? C14 C9 C15 122.2(3) . . ? C9 C10 C11 120.8(3) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 119.3(4) . . ? C10 C11 C16 118.8(3) . . ? C12 C11 C16 121.8(3) . . ? C13 C12 C11 119.5(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 120.9(3) . . ? C12 C13 S1 119.7(3) . . ? C14 C13 S1 118.8(3) . . ? C9 C14 C13 118.8(4) . . ? C9 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? O1 C15 O2 121.3(3) . . ? O1 C15 C9 117.9(3) . . ? O2 C15 C9 120.8(3) . . ? O1 C15 Co4 54.52(19) . . ? O2 C15 Co4 66.9(2) . . ? C9 C15 Co4 171.6(3) . . ? O3 C16 O4 124.9(4) . . ? O3 C16 C11 119.6(3) . . ? O4 C16 C11 115.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Co4 O1 C15 15.5(3) 4_575 . . . ? N6 Co4 O1 C15 178.9(2) 2 . . . ? N10 Co4 O1 C15 -77.6(2) . . . . ? O8 Co4 O1 C15 87.3(2) . . . . ? O2 Co4 O1 C15 1.73(19) . . . . ? N11 Co1 O2 C15 -27.9(5) . . . . ? N4 Co1 O2 C15 168.6(5) . . . . ? N1 Co1 O2 C15 70.6(5) . . . . ? N7 Co1 O2 C15 -115.0(9) . . . . ? N11 Co1 O2 Co4 53.23(10) . . . . ? N4 Co1 O2 Co4 -110.25(10) . . . . ? N1 Co1 O2 Co4 151.81(11) . . . . ? N7 Co1 O2 Co4 -33.8(9) . . . . ? O4 Co4 O2 C15 -175.39(19) 4_575 . . . ? N6 Co4 O2 C15 -12.3(5) 2 . . . ? O1 Co4 O2 C15 -1.74(18) . . . . ? N10 Co4 O2 C15 97.4(2) . . . . ? O8 Co4 O2 C15 -88.4(2) . . . . ? O4 Co4 O2 Co1 29.86(10) 4_575 . . . ? N6 Co4 O2 Co1 -167.0(4) 2 . . . ? O1 Co4 O2 Co1 -156.49(13) . . . . ? N10 Co4 O2 Co1 -57.39(11) . . . . ? O8 Co4 O2 Co1 116.90(10) . . . . ? C15 Co4 O2 Co1 -154.7(2) . . . . ? O7 S1 O5 Co3 161.0(4) . . . 4_676 ? O6 S1 O5 Co3 31.8(5) . . . 4_676 ? C13 S1 O5 Co3 -82.5(4) . . . 4_676 ? N11 Co1 N1 C2 38.9(3) . . . . ? N4 Co1 N1 C2 -134.2(3) . . . . ? N7 Co1 N1 C2 133.1(3) . . . . ? O2 Co1 N1 C2 -47.6(3) . . . . ? N11 Co1 N1 N2 -146.3(2) . . . . ? N4 Co1 N1 N2 40.7(3) . . . . ? N7 Co1 N1 N2 -52.0(3) . . . . ? O2 Co1 N1 N2 127.3(2) . . . . ? C2 N1 N2 C1 0.1(4) . . . . ? Co1 N1 N2 C1 -175.9(2) . . . . ? C2 N1 N2 Co2 -178.3(2) . . . . ? Co1 N1 N2 Co2 5.7(3) . . . . ? N5 Co2 N2 C1 -43.5(3) 3_665 . . . ? N5 Co2 N2 C1 136.5(3) . . . . ? N8 Co2 N2 C1 44.7(3) 3_665 . . . ? N8 Co2 N2 C1 -135.3(3) . . . . ? N2 Co2 N2 C1 27(10) 3_665 . . . ? N5 Co2 N2 N1 134.5(3) 3_665 . . . ? N5 Co2 N2 N1 -45.5(3) . . . . ? N8 Co2 N2 N1 -137.3(3) 3_665 . . . ? N8 Co2 N2 N1 42.7(3) . . . . ? N2 Co2 N2 N1 -155(10) 3_665 . . . ? N11 Co1 N4 C4 -26.2(6) . . . . ? N1 Co1 N4 C4 131.5(3) . . . . ? N7 Co1 N4 C4 -135.2(3) . . . . ? O2 Co1 N4 C4 37.9(3) . . . . ? N11 Co1 N4 N5 154.6(3) . . . . ? N1 Co1 N4 N5 -47.7(3) . . . . ? N7 Co1 N4 N5 45.5(3) . . . . ? O2 Co1 N4 N5 -141.3(3) . . . . ? C4 N4 N5 C3 0.0(4) . . . . ? Co1 N4 N5 C3 179.4(2) . . . . ? C4 N4 N5 Co2 -175.6(3) . . . . ? Co1 N4 N5 Co2 3.8(4) . . . . ? N5 Co2 N5 C3 -19(12) 3_665 . . . ? N8 Co2 N5 C3 -45.5(3) 3_665 . . . ? N8 Co2 N5 C3 134.5(3) . . . . ? N2 Co2 N5 C3 -134.5(3) . . . . ? N2 Co2 N5 C3 45.5(3) 3_665 . . . ? N5 Co2 N5 N4 156(12) 3_665 . . . ? N8 Co2 N5 N4 129.2(3) 3_665 . . . ? N8 Co2 N5 N4 -50.8(3) . . . . ? N2 Co2 N5 N4 40.1(3) . . . . ? N2 Co2 N5 N4 -139.9(3) 3_665 . . . ? N11 Co1 N7 C6 -33.3(3) . . . . ? N4 Co1 N7 C6 129.3(3) . . . . ? N1 Co1 N7 C6 -132.4(3) . . . . ? O2 Co1 N7 C6 53.2(11) . . . . ? N11 Co1 N7 N8 152.1(2) . . . . ? N4 Co1 N7 N8 -45.2(2) . . . . ? N1 Co1 N7 N8 53.1(2) . . . . ? O2 Co1 N7 N8 -121.3(8) . . . . ? C6 N7 N8 C5 0.2(3) . . . . ? Co1 N7 N8 C5 175.9(2) . . . . ? C6 N7 N8 Co2 -179.8(2) . . . . ? Co1 N7 N8 Co2 -4.1(3) . . . . ? N5 Co2 N8 C5 49.4(3) 3_665 . . . ? N5 Co2 N8 C5 -130.6(3) . . . . ? N8 Co2 N8 C5 -34(12) 3_665 . . . ? N2 Co2 N8 C5 137.6(3) . . . . ? N2 Co2 N8 C5 -42.4(3) 3_665 . . . ? N5 Co2 N8 N7 -130.6(2) 3_665 . . . ? N5 Co2 N8 N7 49.4(2) . . . . ? N8 Co2 N8 N7 146(12) 3_665 . . . ? N2 Co2 N8 N7 -42.4(2) . . . . ? N2 Co2 N8 N7 137.6(2) 3_665 . . . ? N12 Co3 N9 C5 -103.2(3) 3_675 . . . ? N3 Co3 N9 C5 88.3(3) 4_575 . . . ? O9 Co3 N9 C5 -9.0(3) . . . . ? O5 Co3 N9 C5 174.0(3) 4_575 . . . ? N12 Co3 N9 C6 69.6(3) 3_675 . . . ? N3 Co3 N9 C6 -98.9(3) 4_575 . . . ? O9 Co3 N9 C6 163.8(3) . . . . ? O5 Co3 N9 C6 -13.2(3) 4_575 . . . ? O4 Co4 N10 C8 143.9(4) 4_575 . . . ? N6 Co4 N10 C8 42.0(4) 2 . . . ? O1 Co4 N10 C8 -63.6(4) . . . . ? O8 Co4 N10 C8 -145.4(4) . . . . ? O2 Co4 N10 C8 -123.4(4) . . . . ? C15 Co4 N10 C8 -93.3(4) . . . . ? O4 Co4 N10 N11 -47.7(2) 4_575 . . . ? N6 Co4 N10 N11 -149.6(2) 2 . . . ? O1 Co4 N10 N11 104.8(2) . . . . ? O8 Co4 N10 N11 23.0(6) . . . . ? O2 Co4 N10 N11 45.0(2) . . . . ? C15 Co4 N10 N11 75.1(2) . . . . ? C8 N10 N11 C7 -0.6(4) . . . . ? Co4 N10 N11 C7 -173.1(2) . . . . ? C8 N10 N11 Co1 162.0(3) . . . . ? Co4 N10 N11 Co1 -10.5(3) . . . . ? N4 Co1 N11 C7 -170.1(4) . . . . ? N1 Co1 N11 C7 32.2(4) . . . . ? N7 Co1 N11 C7 -61.3(3) . . . . ? O2 Co1 N11 C7 125.8(3) . . . . ? N4 Co1 N11 N10 31.7(6) . . . . ? N1 Co1 N11 N10 -126.0(3) . . . . ? N7 Co1 N11 N10 140.5(3) . . . . ? O2 Co1 N11 N10 -32.4(3) . . . . ? N1 N2 C1 N3 0.2(4) . . . . ? Co2 N2 C1 N3 178.5(2) . . . . ? C2 N3 C1 N2 -0.5(4) . . . . ? Co3 N3 C1 N2 175.1(2) 4_676 . . . ? N2 N1 C2 N3 -0.5(4) . . . . ? Co1 N1 C2 N3 174.8(2) . . . . ? C1 N3 C2 N1 0.6(4) . . . . ? Co3 N3 C2 N1 -175.2(2) 4_676 . . . ? N4 N5 C3 N6 0.2(4) . . . . ? Co2 N5 C3 N6 175.7(2) . . . . ? C4 N6 C3 N5 -0.3(4) . . . . ? Co4 N6 C3 N5 -175.1(2) 2_545 . . . ? N5 N4 C4 N6 -0.2(4) . . . . ? Co1 N4 C4 N6 -179.5(2) . . . . ? C3 N6 C4 N4 0.3(4) . . . . ? Co4 N6 C4 N4 174.5(2) 2_545 . . . ? N7 N8 C5 N9 -0.4(4) . . . . ? Co2 N8 C5 N9 179.6(2) . . . . ? C6 N9 C5 N8 0.4(4) . . . . ? Co3 N9 C5 N8 174.7(2) . . . . ? N8 N7 C6 N9 0.1(4) . . . . ? Co1 N7 C6 N9 -175.1(2) . . . . ? C5 N9 C6 N7 -0.3(4) . . . . ? Co3 N9 C6 N7 -174.6(2) . . . . ? N10 N11 C7 N12 0.6(4) . . . . ? Co1 N11 C7 N12 -160.2(3) . . . . ? C8 N12 C7 N11 -0.3(4) . . . . ? Co3 N12 C7 N11 176.7(2) 3_675 . . . ? N11 N10 C8 N12 0.4(4) . . . . ? Co4 N10 C8 N12 169.3(3) . . . . ? C7 N12 C8 N10 -0.1(4) . . . . ? Co3 N12 C8 N10 -176.9(3) 3_675 . . . ? C14 C9 C10 C11 3.2(6) . . . . ? C15 C9 C10 C11 -170.9(3) . . . . ? C9 C10 C11 C12 -3.1(6) . . . . ? C9 C10 C11 C16 173.6(3) . . . . ? C10 C11 C12 C13 1.2(5) . . . . ? C16 C11 C12 C13 -175.4(3) . . . . ? C11 C12 C13 C14 0.7(5) . . . . ? C11 C12 C13 S1 171.3(3) . . . . ? O7 S1 C13 C12 40.2(3) . . . . ? O6 S1 C13 C12 163.6(3) . . . . ? O5 S1 C13 C12 -78.5(3) . . . . ? O7 S1 C13 C14 -149.0(3) . . . . ? O6 S1 C13 C14 -25.6(3) . . . . ? O5 S1 C13 C14 92.2(3) . . . . ? C10 C9 C14 C13 -1.3(5) . . . . ? C15 C9 C14 C13 172.5(3) . . . . ? C12 C13 C14 C9 -0.6(5) . . . . ? S1 C13 C14 C9 -171.3(3) . . . . ? Co4 O1 C15 O2 -3.2(3) . . . . ? Co4 O1 C15 C9 175.8(3) . . . . ? Co1 O2 C15 O1 86.5(6) . . . . ? Co4 O2 C15 O1 2.9(3) . . . . ? Co1 O2 C15 C9 -92.5(6) . . . . ? Co4 O2 C15 C9 -176.1(3) . . . . ? Co1 O2 C15 Co4 83.6(5) . . . . ? C10 C9 C15 O1 -11.7(5) . . . . ? C14 C9 C15 O1 174.3(3) . . . . ? C10 C9 C15 O2 167.3(3) . . . . ? C14 C9 C15 O2 -6.7(5) . . . . ? C10 C9 C15 Co4 12.5(17) . . . . ? C14 C9 C15 Co4 -161.5(14) . . . . ? O4 Co4 C15 O1 -171.54(18) 4_575 . . . ? N6 Co4 C15 O1 -1.5(3) 2 . . . ? N10 Co4 C15 O1 102.9(2) . . . . ? O8 Co4 C15 O1 -89.1(2) . . . . ? O2 Co4 C15 O1 -177.0(3) . . . . ? O4 Co4 C15 O2 5.5(2) 4_575 . . . ? N6 Co4 C15 O2 175.50(17) 2 . . . ? O1 Co4 C15 O2 177.0(3) . . . . ? N10 Co4 C15 O2 -80.06(19) . . . . ? O8 Co4 C15 O2 87.87(19) . . . . ? O4 Co4 C15 C9 162.1(15) 4_575 . . . ? N6 Co4 C15 C9 -27.9(16) 2 . . . ? O1 Co4 C15 C9 -26.4(15) . . . . ? N10 Co4 C15 C9 76.5(16) . . . . ? O8 Co4 C15 C9 -115.5(16) . . . . ? O2 Co4 C15 C9 156.6(17) . . . . ? Co4 O4 C16 O3 44.1(5) 4_676 . . . ? Co4 O4 C16 C11 -137.4(3) 4_676 . . . ? C10 C11 C16 O3 27.8(6) . . . . ? C12 C11 C16 O3 -155.6(4) . . . . ? C10 C11 C16 O4 -150.8(4) . . . . ? C12 C11 C16 O4 25.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.906 _refine_diff_density_min -0.662 _refine_diff_density_rms 0.115