# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Paul Wood' _publ_contact_author_address ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW UNITED KINGDOM ; _publ_contact_author_email PTW22@CAM.AC.UK _publ_section_title ; A new Co(II) coordination solid with mixed oxygen, carboxylate, pyridine and thiolate donors exhibiting canted antiferromagnetism with TC ? 68 K. ; loop_ _publ_author_name 'Paul Wood' 'Antonio Alberola' 'Carlos J. Gomez Garcia' 'Simon Humphrey' # Attachment 'CCDC287016.cif' data_e:\xtals\smh15\pw0321 _database_code_depnum_ccdc_archive 'CCDC 287016' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetracobalt(ii)tetra-2-mercaptonicotinate hydrate ; _chemical_name_common 'tetracobalt(ii)tetra-2-mercaptonicotinate hydrate' _chemical_melting_point ? _chemical_formula_moiety 'C24 H14 Co4 N4 O9 S4' _chemical_formula_sum 'C24 H14 Co4 N4 O9 S4' _chemical_formula_weight 866.35 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' 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 orthorhombic _symmetry_space_group_name_H-M 'P c a 2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 20.8760(6) _cell_length_b 12.3647(2) _cell_length_c 10.9125(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2816.79(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 26774 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description 'pointed rod' _exptl_crystal_colour purple-red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.043 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 2.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 1.180 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 15465 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4610 _reflns_number_gt 3961 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0271P)^2^+7.3201P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 4610 _refine_ls_number_parameters 412 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 0.26041(4) 0.51708(8) 1.47444(9) 0.0228(2) Uani 1 1 d . . . Co2 Co 0.12708(5) 0.26069(7) 1.70539(10) 0.0220(2) Uani 1 1 d . . . Co3 Co 0.35014(5) 0.77025(7) 1.75414(9) 0.0203(2) Uani 1 1 d . . . Co4 Co 0.02955(5) -0.02208(8) 1.44164(9) 0.0248(2) Uani 1 1 d D . . S1 S 0.32094(11) 0.36679(15) 1.34544(19) 0.0340(5) Uani 1 1 d . . . S2 S 0.29410(10) 0.68472(15) 1.60054(17) 0.0276(4) Uani 1 1 d . . . S3 S 0.18790(10) 0.39066(15) 1.5455(2) 0.0304(5) Uani 1 1 d . . . S4 S 0.08284(11) 0.11239(17) 1.5392(2) 0.0376(5) Uani 1 1 d . . . N1 N 0.3266(3) 0.4183(5) 1.5684(6) 0.0311(16) Uani 1 1 d . . . N2 N 0.3192(3) 0.6292(4) 1.3814(5) 0.0194(13) Uani 1 1 d . . . N3 N 0.0726(3) 0.3691(4) 1.6099(5) 0.0235(14) Uani 1 1 d . . . N4 N 0.1896(3) 0.1425(5) 1.6478(6) 0.0255(14) Uani 1 1 d . . . O1 O 0.4302(3) 0.1906(4) 1.3328(4) 0.0299(13) Uani 1 1 d . . . O2 O 0.4860(2) 0.1548(4) 1.4962(5) 0.0311(13) Uani 1 1 d . . . O3 O 0.4033(2) 0.8577(4) 1.6376(4) 0.0246(12) Uani 1 1 d . . . O4 O 0.4421(2) 0.9403(4) 1.4741(5) 0.0341(13) Uani 1 1 d . . . O5 O 0.1830(2) 0.6022(4) 1.4011(4) 0.0258(12) Uani 1 1 d . . . O6 O 0.0909(2) 0.6676(4) 1.3370(5) 0.0260(12) Uani 1 1 d . . . O7 O 0.1129(3) -0.0999(4) 1.4003(5) 0.0284(12) Uani 1 1 d . . . O8 O 0.2117(2) -0.1386(4) 1.3526(5) 0.0265(12) Uani 1 1 d . . . O9 O 0.0124(3) -0.0121(4) 1.2590(4) 0.0340(13) Uani 1 1 d D . . H9A H -0.0241(15) -0.036(6) 1.230(2) 0.041 Uiso 1 1 d D . . H9B H 0.0431(14) -0.021(6) 1.2065(19) 0.041 Uiso 1 1 d D . . C2 C 0.3539(3) 0.3477(5) 1.4870(7) 0.0219(16) Uani 1 1 d . . . C3 C 0.4010(4) 0.2742(6) 1.5271(7) 0.0263(17) Uani 1 1 d . . . C4 C 0.4145(4) 0.2666(6) 1.6539(8) 0.0315(19) Uani 1 1 d . . . H4 H 0.4454 0.2164 1.6830 0.038 Uiso 1 1 calc R . . C5 C 0.3825(4) 0.3321(7) 1.7342(8) 0.039(2) Uani 1 1 d . . . H5 H 0.3896 0.3252 1.8198 0.046 Uiso 1 1 calc R . . C6 C 0.3401(4) 0.4080(7) 1.6908(7) 0.041(2) Uani 1 1 d . . . H6 H 0.3195 0.4548 1.7475 0.050 Uiso 1 1 calc R . . C7 C 0.4398(3) 0.2024(5) 1.4445(8) 0.0277(18) Uani 1 1 d . . . C12 C 0.3367(3) 0.7040(5) 1.4647(7) 0.0213(15) Uani 1 1 d . . . C13 C 0.3825(3) 0.7841(5) 1.4347(7) 0.0201(16) Uani 1 1 d . . . C14 C 0.4050(5) 0.7873(6) 1.3152(7) 0.040(2) Uani 1 1 d . . . H14 H 0.4360 0.8401 1.2931 0.048 Uiso 1 1 calc R . . C15 C 0.3830(4) 0.7134(6) 1.2253(8) 0.040(2) Uani 1 1 d . . . H15 H 0.3950 0.7187 1.1415 0.048 Uiso 1 1 calc R . . C16 C 0.3424(4) 0.6321(6) 1.2687(8) 0.0345(19) Uani 1 1 d . . . H16 H 0.3308 0.5756 1.2140 0.041 Uiso 1 1 calc R . . C17 C 0.4107(4) 0.8657(6) 1.5194(7) 0.0249(17) Uani 1 1 d . . . C22 C 0.1104(3) 0.4349(5) 1.5403(7) 0.0203(15) Uani 1 1 d . . . C23 C 0.0829(3) 0.5196(5) 1.4710(7) 0.0192(14) Uani 1 1 d . . . C24 C 0.0178(4) 0.5273(6) 1.4687(9) 0.0355(19) Uani 1 1 d . . . H24 H -0.0018 0.5804 1.4183 0.043 Uiso 1 1 calc R . . C25 C -0.0202(4) 0.4591(6) 1.5385(9) 0.037(2) Uani 1 1 d . . . H25 H -0.0656 0.4661 1.5373 0.044 Uiso 1 1 calc R . . C26 C 0.0082(4) 0.3822(6) 1.6086(7) 0.0327(19) Uani 1 1 d . . . H26 H -0.0177 0.3365 1.6580 0.039 Uiso 1 1 calc R . . C27 C 0.1226(4) 0.5990(5) 1.3991(6) 0.0181(15) Uani 1 1 d . . . C32 C 0.1618(4) 0.0760(6) 1.5637(7) 0.0301(18) Uani 1 1 d . . . C33 C 0.1984(3) -0.0042(5) 1.5045(6) 0.0236(17) Uani 1 1 d . . . C34 C 0.2634(4) -0.0097(6) 1.5366(8) 0.035(2) Uani 1 1 d . . . H34 H 0.2897 -0.0619 1.4974 0.042 Uiso 1 1 calc R . . C35 C 0.2898(4) 0.0567(6) 1.6211(8) 0.040(2) Uani 1 1 d . . . H35 H 0.3339 0.0513 1.6415 0.048 Uiso 1 1 calc R . . C36 C 0.2509(4) 0.1324(6) 1.6770(8) 0.034(2) Uani 1 1 d . . . H36 H 0.2686 0.1785 1.7379 0.041 Uiso 1 1 calc R . . C37 C 0.1727(4) -0.0846(6) 1.4149(7) 0.0257(17) Uani 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 0.0201(5) 0.0283(5) 0.0200(5) -0.0044(4) 0.0011(5) -0.0048(4) Co2 0.0266(6) 0.0181(5) 0.0214(5) -0.0030(4) -0.0017(5) -0.0015(4) Co3 0.0234(6) 0.0194(5) 0.0182(5) -0.0016(4) -0.0002(4) -0.0012(4) Co4 0.0250(5) 0.0236(5) 0.0257(6) -0.0033(4) -0.0014(5) 0.0022(4) S1 0.0456(13) 0.0307(11) 0.0257(11) -0.0053(8) -0.0030(10) 0.0126(10) S2 0.0298(11) 0.0315(11) 0.0215(10) -0.0091(8) 0.0061(9) -0.0105(8) S3 0.0260(11) 0.0310(11) 0.0343(12) 0.0034(9) 0.0018(9) -0.0005(8) S4 0.0319(12) 0.0348(12) 0.0460(13) -0.0183(10) -0.0075(11) 0.0027(9) N1 0.023(4) 0.033(4) 0.038(5) -0.011(3) 0.001(3) 0.000(3) N2 0.014(3) 0.021(3) 0.024(4) -0.009(2) 0.000(3) -0.003(2) N3 0.030(4) 0.018(3) 0.023(3) 0.001(2) -0.002(3) -0.002(3) N4 0.028(4) 0.023(3) 0.026(4) -0.003(3) -0.004(3) 0.004(3) O1 0.052(4) 0.024(3) 0.014(3) -0.005(2) 0.003(3) 0.003(2) O2 0.032(3) 0.023(3) 0.038(3) 0.001(2) 0.001(3) 0.004(2) O3 0.032(3) 0.024(3) 0.018(3) 0.000(2) 0.001(2) -0.007(2) O4 0.039(3) 0.031(3) 0.032(3) 0.002(2) -0.005(3) -0.017(2) O5 0.025(3) 0.028(3) 0.024(3) 0.004(2) 0.000(2) -0.004(2) O6 0.028(3) 0.021(3) 0.029(3) 0.005(2) -0.002(2) -0.002(2) O7 0.025(3) 0.031(3) 0.029(3) -0.012(2) -0.005(2) 0.006(2) O8 0.028(3) 0.027(3) 0.025(3) -0.010(2) -0.004(2) 0.005(2) O9 0.039(3) 0.043(3) 0.020(3) -0.003(3) -0.002(3) 0.007(3) C2 0.015(4) 0.024(4) 0.026(4) -0.013(3) 0.002(3) 0.002(3) C3 0.024(4) 0.033(4) 0.022(4) 0.003(3) -0.007(3) -0.008(3) C4 0.031(5) 0.029(4) 0.034(5) -0.003(4) -0.008(4) 0.000(4) C5 0.033(5) 0.049(5) 0.034(5) -0.001(4) -0.004(4) 0.003(4) C6 0.046(5) 0.062(6) 0.015(4) -0.014(4) -0.007(4) -0.002(4) C7 0.027(4) 0.015(4) 0.041(5) 0.004(3) -0.005(4) -0.004(3) C12 0.017(4) 0.029(4) 0.018(4) -0.002(3) -0.002(3) 0.006(3) C13 0.020(4) 0.020(4) 0.021(4) -0.001(3) 0.001(3) -0.002(3) C14 0.067(7) 0.028(5) 0.026(5) -0.007(3) 0.002(4) -0.012(4) C15 0.056(6) 0.043(5) 0.020(5) -0.009(4) 0.009(4) -0.021(4) C16 0.037(5) 0.039(5) 0.028(5) -0.014(4) -0.008(4) -0.004(4) C17 0.020(4) 0.026(4) 0.029(5) -0.003(3) -0.004(3) 0.002(3) C22 0.023(4) 0.019(4) 0.018(4) -0.003(3) 0.002(3) 0.001(3) C23 0.016(3) 0.022(3) 0.020(3) 0.000(3) -0.005(3) -0.003(3) C24 0.029(5) 0.030(4) 0.047(5) 0.011(4) -0.001(5) 0.006(3) C25 0.018(4) 0.031(5) 0.062(6) 0.008(4) 0.000(4) 0.005(3) C26 0.022(4) 0.042(5) 0.034(5) -0.001(4) 0.014(4) -0.004(3) C27 0.025(4) 0.023(4) 0.007(3) -0.002(3) 0.004(3) 0.001(3) C32 0.037(5) 0.026(4) 0.027(5) -0.004(3) -0.006(4) 0.000(4) C33 0.023(4) 0.020(4) 0.028(4) -0.007(3) -0.002(3) -0.002(3) C34 0.024(4) 0.038(5) 0.044(5) -0.009(4) -0.008(4) 0.006(3) C35 0.026(5) 0.037(5) 0.056(6) -0.011(4) -0.016(4) 0.009(4) C36 0.039(5) 0.023(4) 0.041(5) -0.012(3) -0.021(4) 0.004(4) C37 0.036(5) 0.024(4) 0.018(4) 0.002(3) -0.004(4) 0.006(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 O5 2.088(5) . ? Co1 N1 2.111(7) . ? Co1 N2 2.112(6) . ? Co1 S3 2.310(2) . ? Co1 S2 2.585(2) . ? Co1 S1 2.652(2) . ? Co2 O1 2.028(5) 4 ? Co2 N3 2.044(6) . ? Co2 N4 2.058(6) . ? Co2 S1 2.288(2) 4 ? Co2 S3 2.691(2) . ? Co2 S4 2.739(2) . ? Co3 O6 1.985(5) 4 ? Co3 O3 2.005(5) . ? Co3 O8 2.023(5) 4_565 ? Co3 S2 2.301(2) . ? Co3 O7 2.391(5) 4_565 ? Co4 O2 1.968(5) 3_455 ? Co4 O9 2.028(5) . ? Co4 O7 2.039(5) . ? Co4 O4 2.117(5) 3_465 ? Co4 S4 2.266(2) . ? S1 C2 1.707(7) . ? S1 Co2 2.288(2) 4_554 ? S2 C12 1.745(7) . ? S3 C22 1.708(7) . ? S4 C32 1.729(8) . ? N1 C2 1.370(9) . ? N1 C6 1.371(10) . ? N2 C16 1.322(10) . ? N2 C12 1.347(9) . ? N3 C26 1.354(10) . ? N3 C22 1.364(9) . ? N4 C36 1.326(10) . ? N4 C32 1.362(9) . ? O1 C7 1.244(9) . ? O1 Co2 2.028(5) 4_554 ? O2 C7 1.263(9) . ? O2 Co4 1.968(5) 3 ? O3 C17 1.302(9) . ? O4 C17 1.235(9) . ? O4 Co4 2.117(5) 3_565 ? O5 C27 1.262(8) . ? O6 C27 1.272(8) . ? O6 Co3 1.985(5) 4_554 ? O7 C37 1.272(9) . ? O7 Co3 2.391(5) 4_544 ? O8 C37 1.254(9) . ? O8 Co3 2.023(5) 4_544 ? O9 H9A 0.878(18) . ? O9 H9B 0.866(18) . ? C2 C3 1.408(10) . ? C3 C4 1.416(11) . ? C3 C7 1.504(11) . ? C4 C5 1.367(11) . ? C4 H4 0.9500 . ? C5 C6 1.373(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C12 C13 1.415(9) . ? C13 C14 1.387(11) . ? C13 C17 1.490(10) . ? C14 C15 1.418(11) . ? C14 H14 0.9500 . ? C15 C16 1.397(11) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C22 C23 1.414(10) . ? C23 C24 1.363(9) . ? C23 C27 1.505(9) . ? C24 C25 1.387(11) . ? C24 H24 0.9500 . ? C25 C26 1.356(11) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C32 C33 1.409(11) . ? C33 C34 1.403(10) . ? C33 C37 1.494(10) . ? C34 C35 1.353(11) . ? C34 H34 0.9500 . ? C35 C36 1.381(11) . ? C35 H35 0.9500 . ? C36 H36 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 O5 Co1 N1 170.0(2) . . ? O5 Co1 N2 86.2(2) . . ? N1 Co1 N2 103.5(2) . . ? O5 Co1 S3 87.87(15) . . ? N1 Co1 S3 82.80(18) . . ? N2 Co1 S3 170.58(17) . . ? O5 Co1 S2 90.60(15) . . ? N1 Co1 S2 91.56(18) . . ? N2 Co1 S2 64.63(16) . . ? S3 Co1 S2 122.83(8) . . ? O5 Co1 S1 121.23(15) . . ? N1 Co1 S1 62.62(18) . . ? N2 Co1 S1 85.86(16) . . ? S3 Co1 S1 90.93(7) . . ? S2 Co1 S1 135.62(8) . . ? O1 Co2 N3 107.6(2) 4 . ? O1 Co2 N4 106.3(2) 4 . ? N3 Co2 N4 131.5(3) . . ? O1 Co2 S1 93.83(16) 4 4 ? N3 Co2 S1 103.22(18) . 4 ? N4 Co2 S1 108.09(19) . 4 ? O1 Co2 S3 167.95(16) 4 . ? N3 Co2 S3 62.63(18) . . ? N4 Co2 S3 85.80(18) . . ? S1 Co2 S3 82.35(7) 4 . ? O1 Co2 S4 88.23(15) 4 . ? N3 Co2 S4 85.05(18) . . ? N4 Co2 S4 62.36(18) . . ? S1 Co2 S4 170.39(9) 4 . ? S3 Co2 S4 97.44(8) . . ? O6 Co3 O3 106.9(2) 4 . ? O6 Co3 O8 120.7(2) 4 4_565 ? O3 Co3 O8 113.0(2) . 4_565 ? O6 Co3 S2 110.67(16) 4 . ? O3 Co3 S2 93.85(15) . . ? O8 Co3 S2 108.56(16) 4_565 . ? O6 Co3 O7 85.7(2) 4 4_565 ? O3 Co3 O7 83.26(19) . 4_565 ? O8 Co3 O7 58.50(19) 4_565 4_565 ? S2 Co3 O7 163.42(15) . 4_565 ? O2 Co4 O9 105.5(2) 3_455 . ? O2 Co4 O7 93.9(2) 3_455 . ? O9 Co4 O7 87.8(2) . . ? O2 Co4 O4 87.1(2) 3_455 3_465 ? O9 Co4 O4 89.1(2) . 3_465 ? O7 Co4 O4 176.9(2) . 3_465 ? O2 Co4 S4 134.13(17) 3_455 . ? O9 Co4 S4 120.22(18) . . ? O7 Co4 S4 91.79(15) . . ? O4 Co4 S4 89.67(16) 3_465 . ? C2 S1 Co2 109.5(2) . 4_554 ? C2 S1 Co1 79.0(2) . . ? Co2 S1 Co1 169.26(10) 4_554 . ? C12 S2 Co3 107.3(2) . . ? C12 S2 Co1 78.2(2) . . ? Co3 S2 Co1 153.42(10) . . ? C22 S3 Co1 113.1(3) . . ? C22 S3 Co2 76.5(3) . . ? Co1 S3 Co2 158.61(10) . . ? C32 S4 Co4 110.5(3) . . ? C32 S4 Co2 75.5(3) . . ? Co4 S4 Co2 165.38(12) . . ? C2 N1 C6 119.1(7) . . ? C2 N1 Co1 109.0(5) . . ? C6 N1 Co1 131.4(5) . . ? C16 N2 C12 120.7(6) . . ? C16 N2 Co1 132.6(5) . . ? C12 N2 Co1 106.5(5) . . ? C26 N3 C22 119.9(6) . . ? C26 N3 Co2 129.5(5) . . ? C22 N3 Co2 110.6(5) . . ? C36 N4 C32 121.2(7) . . ? C36 N4 Co2 127.3(5) . . ? C32 N4 Co2 111.3(5) . . ? C7 O1 Co2 135.8(5) . 4_554 ? C7 O2 Co4 127.3(5) . 3 ? C17 O3 Co3 137.3(5) . . ? C17 O4 Co4 151.9(5) . 3_565 ? C27 O5 Co1 139.8(5) . . ? C27 O6 Co3 110.3(5) . 4_554 ? C37 O7 Co4 137.7(5) . . ? C37 O7 Co3 82.4(4) . 4_544 ? Co4 O7 Co3 137.7(2) . 4_544 ? C37 O8 Co3 99.8(5) . 4_544 ? Co4 O9 H9A 119(2) . . ? Co4 O9 H9B 121(2) . . ? H9A O9 H9B 111(3) . . ? N1 C2 C3 120.0(7) . . ? N1 C2 S1 109.3(5) . . ? C3 C2 S1 130.7(5) . . ? C2 C3 C4 119.1(7) . . ? C2 C3 C7 124.8(7) . . ? C4 C3 C7 116.1(7) . . ? C5 C4 C3 119.3(8) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 119.9(8) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? N1 C6 C5 122.1(8) . . ? N1 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? O1 C7 O2 120.5(7) . . ? O1 C7 C3 124.7(7) . . ? O2 C7 C3 114.8(7) . . ? N2 C12 C13 120.4(6) . . ? N2 C12 S2 110.0(5) . . ? C13 C12 S2 129.6(5) . . ? C14 C13 C12 117.9(7) . . ? C14 C13 C17 115.5(6) . . ? C12 C13 C17 126.7(6) . . ? C13 C14 C15 121.5(8) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 115.2(8) . . ? C16 C15 H15 122.4 . . ? C14 C15 H15 122.4 . . ? N2 C16 C15 123.8(7) . . ? N2 C16 H16 118.1 . . ? C15 C16 H16 118.1 . . ? O4 C17 O3 121.1(7) . . ? O4 C17 C13 117.9(7) . . ? O3 C17 C13 121.0(7) . . ? N3 C22 C23 120.3(6) . . ? N3 C22 S3 109.8(5) . . ? C23 C22 S3 129.7(6) . . ? C24 C23 C22 117.8(7) . . ? C24 C23 C27 119.6(7) . . ? C22 C23 C27 122.6(6) . . ? C23 C24 C25 121.3(7) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C26 C25 C24 119.0(7) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? N3 C26 C25 121.6(7) . . ? N3 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? O5 C27 O6 120.5(6) . . ? O5 C27 C23 124.2(6) . . ? O6 C27 C23 115.3(6) . . ? N4 C32 C33 120.2(7) . . ? N4 C32 S4 110.7(6) . . ? C33 C32 S4 129.0(6) . . ? C34 C33 C32 116.4(7) . . ? C34 C33 C37 118.6(7) . . ? C32 C33 C37 125.0(7) . . ? C35 C34 C33 122.4(8) . . ? C35 C34 H34 118.8 . . ? C33 C34 H34 118.8 . . ? C34 C35 C36 118.2(8) . . ? C34 C35 H35 120.9 . . ? C36 C35 H35 120.9 . . ? N4 C36 C35 121.7(7) . . ? N4 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? O8 C37 O7 119.4(7) . . ? O8 C37 C33 118.4(7) . . ? O7 C37 C33 122.2(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.697 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.109