Supplementary Material (ESI) for Journal of Materials Chemistry This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Guionneau, Philippe' 'Bravic, G.' 'Chasseau, D.' 'Letard, Jean-Francois' 'Marchivie, M.' _publ_contact_author_name 'Dr Philippe Guionneau' _publ_contact_author_address ; Institut de Chimie de la Matiere Condensee de Bordeaux 87 Av. dr A. Scwheitzer Pessac 33608 FRANCE ; _publ_contact_author_email 'GUIONNEAU@ICMCB.U-BORDEAUX.FR' _publ_section_title ; Co(II) molecular complexes as a reference to the spin crossover in Fe(II) analogues ; data_[Co(PM-BiA)2(NCS)2]293K _database_code_CSD 181918 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H28 Co N6 S2' _chemical_formula_weight 691.71 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' '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 P21/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 17.664(5) _cell_length_b 12.548(5) _cell_length_c 17.271(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 115.910(5) _cell_angle_gamma 90.000(5) _cell_volume 3443(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.656 _exptl_absorpt_correction_type no _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6038 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.98 _reflns_number_total 6038 _reflns_number_gt 4065 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0507P)^2^+1.1501P] 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_number_reflns 6038 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 S4 S 0.54550(6) 0.15728(8) 0.92040(5) 0.0816(3) Uani 1 1 d . . . S104 S 0.95169(6) 0.38168(7) 1.07042(6) 0.0877(3) Uani 1 1 d . . . Co1 Co 0.75861(2) 0.19808(3) 0.82427(2) 0.05745(13) Uani 1 1 d . . . C3 C 0.6193(2) 0.1521(2) 0.88830(17) 0.0628(7) Uani 1 1 d . . . C10 C 0.8934(6) 0.8183(6) 0.5552(4) 0.177(4) Uani 1 1 d . . . H10 H 0.8983 0.8834 0.5321 0.213 Uiso 1 1 calc R . . C11 C 0.8452(5) 0.8088(4) 0.5973(4) 0.173(3) Uani 1 1 d . . . H11 H 0.8177 0.8685 0.6045 0.207 Uiso 1 1 calc R . . C12 C 0.8358(3) 0.7113(3) 0.6303(3) 0.1232(15) Uani 1 1 d . . . H12 H 0.8034 0.7074 0.6606 0.148 Uiso 1 1 calc R . . C13 C 0.8730(2) 0.6217(3) 0.6192(2) 0.0817(10) Uani 1 1 d . . . C14 C 0.9234(3) 0.6306(4) 0.5759(3) 0.1200(16) Uani 1 1 d . . . H14 H 0.9493 0.5710 0.5662 0.144 Uiso 1 1 calc R . . C15 C 0.9342(4) 0.7321(6) 0.5472(4) 0.166(3) Uani 1 1 d . . . H15 H 0.9709 0.7395 0.5220 0.200 Uiso 1 1 calc R . . C20 C 0.8426(2) 0.4251(3) 0.60689(19) 0.0738(9) Uani 1 1 d . . . H20 H 0.8304 0.4285 0.5488 0.089 Uiso 1 1 calc R . . C22 C 0.83745(19) 0.3293(2) 0.64200(18) 0.0677(8) Uani 1 1 d . . . H22 H 0.8218 0.2684 0.6078 0.081 Uiso 1 1 calc R . . C23 C 0.85547(17) 0.3227(2) 0.72818(17) 0.0556(6) Uani 1 1 d . . . C24 C 0.87822(17) 0.4134(2) 0.77855(17) 0.0613(7) Uani 1 1 d . . . H24 H 0.8904 0.4095 0.8366 0.074 Uiso 1 1 calc R . . C25 C 0.88276(18) 0.5094(2) 0.74232(18) 0.0660(8) Uani 1 1 d . . . H25 H 0.8977 0.5703 0.7764 0.079 Uiso 1 1 calc R . . C26 C 0.86551(18) 0.5175(2) 0.65601(18) 0.0653(7) Uani 1 1 d . . . C27 C 0.8798(2) 0.1413(3) 0.7553(2) 0.0740(9) Uani 1 1 d . . . C33 C 0.7929(3) -0.0444(3) 0.8556(2) 0.1042(13) Uani 1 1 d . . . H33 H 0.7549 -0.0418 0.8796 0.125 Uiso 1 1 calc R . . C35 C 0.8658(2) 0.0407(3) 0.7893(2) 0.0819(10) Uani 1 1 d . . . C42 C 0.8300(5) -0.1403(4) 0.8529(4) 0.144(2) Uani 1 1 d . . . H42 H 0.8157 -0.2023 0.8730 0.173 Uiso 1 1 calc R . . C44 C 0.8890(5) -0.1431(4) 0.8197(4) 0.162(3) Uani 1 1 d . . . H44 H 0.9166 -0.2065 0.8204 0.195 Uiso 1 1 calc R . . C103 C 0.89202(19) 0.2998(2) 0.99670(18) 0.0614(7) Uani 1 1 d . . . C110 C 0.5690(2) -0.3539(3) 0.3662(3) 0.0906(11) Uani 1 1 d . . . H110 H 0.5618 -0.4136 0.3317 0.109 Uiso 1 1 calc R . . C111 C 0.6013(3) -0.3647(3) 0.4533(3) 0.0994(12) Uani 1 1 d . . . H111 H 0.6155 -0.4319 0.4783 0.119 Uiso 1 1 calc R . . C112 C 0.6130(2) -0.2761(3) 0.5045(2) 0.0873(10) Uani 1 1 d . . . H112 H 0.6349 -0.2847 0.5638 0.105 Uiso 1 1 calc R . . C113 C 0.59285(18) -0.1747(2) 0.46983(19) 0.0644(7) Uani 1 1 d . . . C114 C 0.55910(19) -0.1659(3) 0.38092(19) 0.0740(8) Uani 1 1 d . . . H114 H 0.5441 -0.0991 0.3553 0.089 Uiso 1 1 calc R . . C115 C 0.5473(2) -0.2554(3) 0.3296(2) 0.0854(10) Uani 1 1 d . . . H115 H 0.5246 -0.2481 0.2701 0.102 Uiso 1 1 calc R . . C120 C 0.60488(19) -0.0819(2) 0.60412(19) 0.0702(8) Uani 1 1 d . . . H120 H 0.5883 -0.1446 0.6211 0.084 Uiso 1 1 calc R . . C121 C 0.62471(19) 0.0059(2) 0.65725(18) 0.0682(8) Uani 1 1 d . . . H121 H 0.6229 0.0011 0.7101 0.082 Uiso 1 1 calc R . . C122 C 0.64729(17) 0.1009(2) 0.63270(16) 0.0590(7) Uani 1 1 d . . . C123 C 0.65166(19) 0.1055(2) 0.55447(18) 0.0673(8) Uani 1 1 d . . . H123 H 0.6677 0.1686 0.5374 0.081 Uiso 1 1 calc R . . C124 C 0.6324(2) 0.0174(2) 0.50217(19) 0.0698(8) Uani 1 1 d . . . H124 H 0.6350 0.0222 0.4496 0.084 Uiso 1 1 calc R . . C125 C 0.60913(18) -0.0790(2) 0.52573(18) 0.0617(7) Uani 1 1 d . . . C127 C 0.63858(19) 0.2812(2) 0.65704(19) 0.0630(7) Uani 1 1 d . . . C132 C 0.73094(19) 0.4407(2) 0.84958(19) 0.0684(8) Uani 1 1 d . . . H132 H 0.7645 0.4291 0.9079 0.082 Uiso 1 1 calc R . . C133 C 0.7051(2) 0.5426(3) 0.8221(2) 0.0764(9) Uani 1 1 d . . . H133 H 0.7208 0.5987 0.8613 0.092 Uiso 1 1 calc R . . C134 C 0.6561(2) 0.5608(3) 0.7367(2) 0.0856(10) Uani 1 1 d . . . H134 H 0.6389 0.6295 0.7166 0.103 Uiso 1 1 calc R . . C135 C 0.6327(2) 0.4756(2) 0.6809(2) 0.0762(9) Uani 1 1 d . . . H135 H 0.5984 0.4857 0.6225 0.091 Uiso 1 1 calc R . . C137 C 0.66062(17) 0.3757(2) 0.71231(17) 0.0588(7) Uani 1 1 d . . . C333 C 0.9066(3) -0.0522(3) 0.7859(3) 0.1225(16) Uani 1 1 d . . . H333 H 0.9444 -0.0532 0.7618 0.147 Uiso 1 1 calc R . . N2 N 0.67195(19) 0.1475(2) 0.86551(17) 0.0843(8) Uani 1 1 d . . . N26 N 0.84539(14) 0.22530(17) 0.76524(13) 0.0577(6) Uani 1 1 d . . . N31 N 0.81056(18) 0.04495(18) 0.82437(16) 0.0742(7) Uani 1 1 d . . . N102 N 0.84973(16) 0.2425(2) 0.94311(15) 0.0702(7) Uani 1 1 d . . . N126 N 0.66750(14) 0.19049(18) 0.68872(13) 0.0574(5) Uani 1 1 d . . . N131 N 0.70993(14) 0.35728(17) 0.79615(14) 0.0576(5) Uani 1 1 d . . . H27 H 0.9125(18) 0.139(2) 0.7248(18) 0.069 Uiso 1 1 d . . . H127 H 0.6040(18) 0.292(2) 0.6003(18) 0.069 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 S4 0.0906(6) 0.0875(6) 0.0691(5) -0.0094(4) 0.0371(5) -0.0121(5) S104 0.1016(7) 0.0754(6) 0.0792(6) -0.0218(4) 0.0331(5) -0.0164(5) Co1 0.0733(3) 0.0523(2) 0.0440(2) 0.00305(16) 0.02307(17) -0.00305(18) C3 0.083(2) 0.0536(16) 0.0452(15) 0.0000(12) 0.0217(15) -0.0168(15) C10 0.203(8) 0.125(5) 0.114(4) 0.043(4) -0.013(5) -0.085(5) C11 0.236(8) 0.081(3) 0.134(5) 0.019(3) 0.020(5) -0.030(4) C12 0.148(4) 0.083(3) 0.122(4) 0.014(3) 0.044(3) -0.012(3) C13 0.079(2) 0.084(2) 0.066(2) 0.0088(18) 0.0158(17) -0.0262(19) C14 0.098(3) 0.149(4) 0.105(3) 0.032(3) 0.036(3) -0.031(3) C15 0.124(4) 0.210(7) 0.126(4) 0.073(5) 0.018(3) -0.084(5) C20 0.091(2) 0.080(2) 0.0540(16) -0.0011(16) 0.0348(16) -0.0157(18) C22 0.084(2) 0.0694(19) 0.0547(16) -0.0109(14) 0.0347(16) -0.0104(16) C23 0.0577(16) 0.0583(17) 0.0534(15) -0.0016(13) 0.0267(13) -0.0004(13) C24 0.0656(17) 0.0669(18) 0.0485(15) -0.0027(14) 0.0222(14) -0.0029(14) C25 0.0685(18) 0.0641(18) 0.0594(17) -0.0084(14) 0.0223(15) -0.0141(15) C26 0.0596(17) 0.0704(19) 0.0593(17) 0.0018(15) 0.0198(14) -0.0118(14) C27 0.086(2) 0.069(2) 0.068(2) -0.0066(16) 0.0352(18) 0.0104(18) C33 0.153(4) 0.058(2) 0.076(2) 0.0123(18) 0.025(2) -0.009(2) C35 0.104(3) 0.0580(19) 0.068(2) -0.0025(16) 0.023(2) 0.0157(18) C42 0.217(7) 0.058(3) 0.122(4) 0.019(3) 0.040(4) -0.001(3) C44 0.226(7) 0.057(3) 0.157(5) 0.003(3) 0.039(5) 0.038(4) C103 0.0731(18) 0.0614(17) 0.0506(15) 0.0070(14) 0.0278(15) 0.0056(15) C110 0.111(3) 0.074(2) 0.093(3) -0.025(2) 0.050(2) -0.018(2) C111 0.137(3) 0.061(2) 0.096(3) -0.0119(19) 0.048(3) -0.007(2) C112 0.115(3) 0.068(2) 0.074(2) -0.0032(17) 0.037(2) -0.0104(19) C113 0.0688(18) 0.0612(18) 0.0636(17) -0.0085(14) 0.0294(15) -0.0124(14) C114 0.078(2) 0.072(2) 0.0646(19) -0.0049(16) 0.0244(16) -0.0114(16) C115 0.095(2) 0.094(3) 0.066(2) -0.019(2) 0.0335(18) -0.021(2) C120 0.086(2) 0.0628(18) 0.0642(18) -0.0019(15) 0.0354(16) -0.0181(16) C121 0.086(2) 0.0679(19) 0.0523(16) -0.0027(14) 0.0317(16) -0.0153(16) C122 0.0657(17) 0.0557(16) 0.0474(15) -0.0012(13) 0.0171(13) -0.0061(13) C123 0.085(2) 0.0568(17) 0.0599(17) 0.0021(14) 0.0319(16) -0.0122(15) C124 0.092(2) 0.0656(19) 0.0561(17) -0.0044(15) 0.0364(16) -0.0107(16) C125 0.0660(18) 0.0590(17) 0.0577(16) -0.0015(13) 0.0247(14) -0.0090(14) C127 0.0638(18) 0.069(2) 0.0475(15) 0.0012(14) 0.0161(14) -0.0021(15) C132 0.0758(19) 0.0692(19) 0.0596(17) -0.0092(15) 0.0289(16) 0.0070(16) C133 0.087(2) 0.0627(19) 0.079(2) -0.0109(16) 0.0354(19) 0.0097(17) C134 0.096(2) 0.060(2) 0.094(3) 0.0091(18) 0.035(2) 0.0178(18) C135 0.083(2) 0.065(2) 0.0660(19) 0.0072(16) 0.0190(17) 0.0111(16) C137 0.0592(16) 0.0596(17) 0.0541(16) 0.0030(13) 0.0214(14) 0.0036(13) C333 0.148(4) 0.075(3) 0.134(4) -0.014(3) 0.052(3) 0.032(3) N2 0.097(2) 0.091(2) 0.0685(17) 0.0086(15) 0.0395(16) -0.0177(16) N26 0.0681(14) 0.0540(13) 0.0478(12) -0.0041(10) 0.0225(11) 0.0020(11) N31 0.097(2) 0.0496(14) 0.0578(14) 0.0061(12) 0.0165(14) 0.0006(13) N102 0.0838(17) 0.0728(16) 0.0461(13) 0.0011(12) 0.0212(13) -0.0049(14) N126 0.0647(14) 0.0552(14) 0.0483(12) -0.0004(11) 0.0208(11) -0.0054(11) N131 0.0646(14) 0.0577(14) 0.0520(13) -0.0017(11) 0.0271(11) 0.0033(11) _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 S4 C3 1.626(4) . ? S104 C103 1.617(3) . ? Co1 N2 2.051(3) . ? Co1 N102 2.056(3) . ? Co1 N31 2.129(3) . ? Co1 N131 2.145(2) . ? Co1 N126 2.188(2) . ? Co1 N26 2.207(2) . ? C3 N2 1.158(4) . ? C10 C15 1.340(10) . ? C10 C11 1.345(10) . ? C11 C12 1.389(7) . ? C12 C13 1.357(6) . ? C13 C14 1.395(5) . ? C13 C26 1.484(4) . ? C14 C15 1.409(7) . ? C20 C22 1.368(4) . ? C20 C26 1.388(4) . ? C22 C23 1.382(4) . ? C23 C24 1.381(4) . ? C23 N26 1.427(3) . ? C24 C25 1.377(4) . ? C25 C26 1.389(4) . ? C27 N26 1.265(4) . ? C27 C35 1.457(5) . ? C33 N31 1.339(4) . ? C33 C42 1.381(6) . ? C35 N31 1.357(4) . ? C35 C333 1.385(5) . ? C42 C44 1.392(8) . ? C44 C333 1.377(7) . ? C103 N102 1.152(3) . ? C110 C111 1.363(5) . ? C110 C115 1.366(5) . ? C111 C112 1.378(5) . ? C112 C113 1.385(4) . ? C113 C114 1.388(4) . ? C113 C125 1.488(4) . ? C114 C115 1.389(4) . ? C120 C121 1.378(4) . ? C120 C125 1.389(4) . ? C121 C122 1.381(4) . ? C122 C123 1.388(4) . ? C122 N126 1.423(3) . ? C123 C124 1.373(4) . ? C124 C125 1.394(4) . ? C127 N126 1.269(4) . ? C127 C137 1.465(4) . ? C132 N131 1.336(3) . ? C132 C133 1.371(4) . ? C133 C134 1.364(4) . ? C134 C135 1.377(4) . ? C135 C137 1.368(4) . ? C137 N131 1.344(3) . ? 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 N102 96.58(11) . . ? N2 Co1 N31 96.17(12) . . ? N102 Co1 N31 95.43(10) . . ? N2 Co1 N131 94.62(11) . . ? N102 Co1 N131 92.01(9) . . ? N31 Co1 N131 166.10(9) . . ? N2 Co1 N126 92.67(10) . . ? N102 Co1 N126 165.69(9) . . ? N31 Co1 N126 94.40(9) . . ? N131 Co1 N126 76.33(8) . . ? N2 Co1 N26 169.34(10) . . ? N102 Co1 N26 91.17(9) . . ? N31 Co1 N26 75.75(10) . . ? N131 Co1 N26 92.40(8) . . ? N126 Co1 N26 81.21(8) . . ? N2 C3 S4 179.5(3) . . ? C15 C10 C11 118.7(6) . . ? C10 C11 C12 121.1(7) . . ? C13 C12 C11 121.4(6) . . ? C12 C13 C14 118.0(4) . . ? C12 C13 C26 122.1(4) . . ? C14 C13 C26 119.8(4) . . ? C13 C14 C15 118.6(5) . . ? C10 C15 C14 122.1(7) . . ? C22 C20 C26 121.4(3) . . ? C20 C22 C23 120.1(3) . . ? C24 C23 C22 119.8(3) . . ? C24 C23 N26 118.8(2) . . ? C22 C23 N26 121.3(2) . . ? C25 C24 C23 119.6(3) . . ? C24 C25 C26 121.5(3) . . ? C20 C26 C25 117.6(3) . . ? C20 C26 C13 122.1(3) . . ? C25 C26 C13 120.3(3) . . ? N26 C27 C35 119.5(3) . . ? N31 C33 C42 121.2(5) . . ? N31 C35 C333 122.7(4) . . ? N31 C35 C27 115.3(3) . . ? C333 C35 C27 122.0(4) . . ? C33 C42 C44 119.2(5) . . ? C333 C44 C42 120.1(5) . . ? N102 C103 S104 178.8(3) . . ? C111 C110 C115 119.8(3) . . ? C110 C111 C112 120.1(4) . . ? C111 C112 C113 121.7(3) . . ? C112 C113 C114 117.2(3) . . ? C112 C113 C125 121.4(3) . . ? C114 C113 C125 121.4(3) . . ? C113 C114 C115 120.9(3) . . ? C110 C115 C114 120.2(3) . . ? C121 C120 C125 121.4(3) . . ? C120 C121 C122 120.6(3) . . ? C121 C122 C123 118.8(3) . . ? C121 C122 N126 119.6(2) . . ? C123 C122 N126 121.6(2) . . ? C124 C123 C122 120.2(3) . . ? C123 C124 C125 121.8(3) . . ? C120 C125 C124 117.1(3) . . ? C120 C125 C113 122.2(3) . . ? C124 C125 C113 120.6(3) . . ? N126 C127 C137 120.2(3) . . ? N131 C132 C133 122.8(3) . . ? C134 C133 C132 119.2(3) . . ? C133 C134 C135 118.8(3) . . ? C137 C135 C134 119.1(3) . . ? N131 C137 C135 122.5(3) . . ? N131 C137 C127 115.1(2) . . ? C135 C137 C127 122.4(3) . . ? C44 C333 C35 117.5(5) . . ? C3 N2 Co1 159.1(3) . . ? C27 N26 C23 119.5(3) . . ? C27 N26 Co1 113.9(2) . . ? C23 N26 Co1 126.01(17) . . ? C33 N31 C35 119.2(3) . . ? C33 N31 Co1 125.4(3) . . ? C35 N31 Co1 115.4(2) . . ? C103 N102 Co1 157.1(2) . . ? C127 N126 C122 118.8(2) . . ? C127 N126 Co1 113.04(19) . . ? C122 N126 Co1 127.62(17) . . ? C132 N131 C137 117.6(2) . . ? C132 N131 Co1 127.60(19) . . ? C137 N131 Co1 114.29(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.264 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.046 ############################################ # END ############################################ data_[Co(PM-BiA)2(NCS)2]120K _database_code_CSD 181919 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H28 Co N6 S2' _chemical_formula_weight 691.71 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' '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 P21/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 17.1637(2) _cell_length_b 12.5575(2) _cell_length_c 17.2701(2) _cell_angle_alpha 90.000(5) _cell_angle_beta 115.844(5) _cell_angle_gamma 90.000(5) _cell_volume 3349.99(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type no _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24300 _diffrn_reflns_av_R_equivalents 0.0696 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6828 _reflns_number_gt 4784 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0722P)^2^+1.0646P] 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_number_reflns 6828 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _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 S4 S 0.54261(6) 0.15670(7) 0.92187(5) 0.0274(2) Uani 1 1 d . . . S104 S 0.95280(6) 0.38149(7) 1.06837(5) 0.0302(2) Uani 1 1 d . . . Co1 Co 0.75978(3) 0.19149(3) 0.82310(3) 0.02008(14) Uani 1 1 d . . . C3 C 0.6172(2) 0.1458(2) 0.88731(19) 0.0234(7) Uani 1 1 d . . . C10 C 0.8816(3) 0.8279(3) 0.5598(3) 0.0537(13) Uani 1 1 d . . . H10 H 0.8869 0.8962 0.5390 0.064 Uiso 1 1 calc R . . C11 C 0.8309(3) 0.8149(3) 0.6033(3) 0.0515(12) Uani 1 1 d . . . H11 H 0.8001 0.8737 0.6109 0.062 Uiso 1 1 calc R . . C12 C 0.8252(2) 0.7147(3) 0.6359(2) 0.0373(9) Uani 1 1 d . . . H12 H 0.7928 0.7066 0.6683 0.045 Uiso 1 1 calc R . . C13 C 0.8670(2) 0.6259(3) 0.6212(2) 0.0295(8) Uani 1 1 d . . . C14 C 0.9161(2) 0.6396(3) 0.5755(2) 0.0365(9) Uani 1 1 d . . . H14 H 0.9438 0.5804 0.5640 0.044 Uiso 1 1 calc R . . C15 C 0.9244(3) 0.7417(4) 0.5466(2) 0.0510(12) Uani 1 1 d . . . H15 H 0.9598 0.7515 0.5176 0.061 Uiso 1 1 calc R . . C20 C 0.8422(2) 0.4278(3) 0.6076(2) 0.0258(7) Uani 1 1 d . . . H20 H 0.8303 0.4323 0.5486 0.031 Uiso 1 1 calc R . . C22 C 0.8398(2) 0.3299(2) 0.6435(2) 0.0241(7) Uani 1 1 d . . . H22 H 0.8254 0.2677 0.6087 0.029 Uiso 1 1 calc R . . C23 C 0.8584(2) 0.3221(2) 0.7304(2) 0.0209(7) Uani 1 1 d . . . C24 C 0.8789(2) 0.4131(2) 0.78121(19) 0.0229(7) Uani 1 1 d . . . H24 H 0.8921 0.4081 0.8405 0.028 Uiso 1 1 calc R . . C25 C 0.88007(19) 0.5115(2) 0.7447(2) 0.0234(7) Uani 1 1 d . . . H25 H 0.8933 0.5738 0.7793 0.028 Uiso 1 1 calc R . . C26 C 0.8620(2) 0.5199(2) 0.6577(2) 0.0243(7) Uani 1 1 d . . . C27 C 0.8880(2) 0.1406(3) 0.7577(2) 0.0240(7) Uani 1 1 d . . . C33 C 0.7976(2) -0.0513(3) 0.8524(2) 0.0332(9) Uani 1 1 d . . . H33 H 0.7555 -0.0514 0.8743 0.040 Uiso 1 1 calc R . . C35 C 0.8739(2) 0.0387(2) 0.7906(2) 0.0252(7) Uani 1 1 d . . . C42 C 0.8392(3) -0.1465(3) 0.8516(2) 0.0435(10) Uani 1 1 d . . . H42 H 0.8252 -0.2103 0.8724 0.052 Uiso 1 1 calc R . . C44 C 0.9004(3) -0.1472(3) 0.8206(3) 0.0447(11) Uani 1 1 d . . . H44 H 0.9303 -0.2110 0.8209 0.054 Uiso 1 1 calc R . . C103 C 0.8950(2) 0.2935(2) 0.9964(2) 0.0233(7) Uani 1 1 d . . . C110 C 0.5669(2) -0.3561(3) 0.3603(2) 0.0309(8) Uani 1 1 d . . . H110 H 0.5603 -0.4168 0.3252 0.037 Uiso 1 1 calc R . . C111 C 0.5974(2) -0.3667(3) 0.4484(2) 0.0324(8) Uani 1 1 d . . . H111 H 0.6108 -0.4354 0.4739 0.039 Uiso 1 1 calc R . . C112 C 0.6087(2) -0.2779(3) 0.4999(2) 0.0281(8) Uani 1 1 d . . . H112 H 0.6302 -0.2868 0.5604 0.034 Uiso 1 1 calc R . . C113 C 0.5893(2) -0.1759(2) 0.4650(2) 0.0229(7) Uani 1 1 d . . . C114 C 0.5573(2) -0.1662(3) 0.3760(2) 0.0253(7) Uani 1 1 d . . . H114 H 0.5430 -0.0977 0.3502 0.030 Uiso 1 1 calc R . . C115 C 0.5462(2) -0.2555(3) 0.3243(2) 0.0294(8) Uani 1 1 d . . . H115 H 0.5241 -0.2473 0.2638 0.035 Uiso 1 1 calc R . . C120 C 0.6032(2) -0.0859(3) 0.6014(2) 0.0247(7) Uani 1 1 d . . . H120 H 0.5864 -0.1505 0.6185 0.030 Uiso 1 1 calc R . . C121 C 0.6242(2) 0.0018(2) 0.65567(19) 0.0234(7) Uani 1 1 d . . . H121 H 0.6229 -0.0035 0.7100 0.028 Uiso 1 1 calc R . . C122 C 0.64706(19) 0.0979(2) 0.63051(19) 0.0209(7) Uani 1 1 d . . . C123 C 0.6498(2) 0.1046(2) 0.5516(2) 0.0236(7) Uani 1 1 d . . . H123 H 0.6654 0.1699 0.5343 0.028 Uiso 1 1 calc R . . C124 C 0.6301(2) 0.0165(2) 0.4978(2) 0.0251(7) Uani 1 1 d . . . H124 H 0.6327 0.0221 0.4441 0.030 Uiso 1 1 calc R . . C125 C 0.60634(19) -0.0810(2) 0.52167(19) 0.0209(7) Uani 1 1 d . . . C127 C 0.6387(2) 0.2790(2) 0.6562(2) 0.0221(7) Uani 1 1 d . . . C132 C 0.7312(2) 0.4334(3) 0.8529(2) 0.0261(7) Uani 1 1 d . . . H132 H 0.7643 0.4197 0.9125 0.031 Uiso 1 1 calc R . . C133 C 0.7070(2) 0.5375(3) 0.8267(2) 0.0266(7) Uani 1 1 d . . . H133 H 0.7236 0.5938 0.8674 0.032 Uiso 1 1 calc R . . C134 C 0.6583(2) 0.5575(3) 0.7403(2) 0.0294(8) Uani 1 1 d . . . H134 H 0.6413 0.6282 0.7205 0.035 Uiso 1 1 calc R . . C135 C 0.6342(2) 0.4731(2) 0.6824(2) 0.0258(7) Uani 1 1 d . . . H135 H 0.5998 0.4849 0.6227 0.031 Uiso 1 1 calc R . . C137 C 0.66145(19) 0.3714(2) 0.71351(19) 0.0211(7) Uani 1 1 d . . . C333 C 0.9184(2) -0.0533(3) 0.7887(2) 0.0376(9) Uani 1 1 d . . . H333 H 0.9600 -0.0520 0.7662 0.045 Uiso 1 1 calc R . . N2 N 0.66983(19) 0.1379(2) 0.86225(18) 0.0308(7) Uani 1 1 d . . . N26 N 0.85020(16) 0.22314(19) 0.76700(15) 0.0203(6) Uani 1 1 d . . . N31 N 0.81507(17) 0.0405(2) 0.82304(16) 0.0239(6) Uani 1 1 d . . . N102 N 0.85266(18) 0.2328(2) 0.94371(16) 0.0270(6) Uani 1 1 d . . . N126 N 0.66788(16) 0.18721(19) 0.68751(16) 0.0203(6) Uani 1 1 d . . . N131 N 0.70995(16) 0.3509(2) 0.79786(16) 0.0208(6) Uani 1 1 d . . . H27 H 0.928(2) 0.141(2) 0.734(2) 0.025 Uiso 1 1 d . . . H127 H 0.601(2) 0.289(2) 0.597(2) 0.025 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 S4 0.0283(5) 0.0293(4) 0.0260(4) -0.0036(3) 0.0130(4) -0.0031(4) S104 0.0353(5) 0.0235(4) 0.0280(5) -0.0054(3) 0.0102(4) -0.0021(4) Co1 0.0233(2) 0.0194(2) 0.0171(2) 0.00052(17) 0.00841(18) -0.00105(17) C3 0.0308(19) 0.0198(16) 0.0160(16) 0.0003(12) 0.0068(14) -0.0044(14) C10 0.058(3) 0.038(2) 0.037(2) 0.0111(18) -0.006(2) -0.025(2) C11 0.061(3) 0.026(2) 0.039(2) 0.0041(17) -0.004(2) -0.0059(19) C12 0.038(2) 0.031(2) 0.034(2) 0.0002(16) 0.0074(17) -0.0037(16) C13 0.0266(18) 0.0303(19) 0.0210(17) 0.0029(14) 0.0005(14) -0.0104(15) C14 0.031(2) 0.046(2) 0.0278(19) 0.0092(16) 0.0083(16) -0.0069(17) C15 0.041(2) 0.069(3) 0.031(2) 0.015(2) 0.0040(18) -0.028(2) C20 0.0283(18) 0.0290(18) 0.0201(16) 0.0010(14) 0.0106(14) -0.0034(14) C22 0.0256(18) 0.0250(18) 0.0220(17) -0.0043(13) 0.0107(14) -0.0031(13) C23 0.0195(16) 0.0199(16) 0.0232(16) -0.0003(12) 0.0092(13) 0.0002(12) C24 0.0218(16) 0.0285(18) 0.0181(16) 0.0009(13) 0.0083(13) -0.0011(13) C25 0.0196(17) 0.0248(17) 0.0252(17) -0.0047(13) 0.0091(14) -0.0051(13) C26 0.0221(17) 0.0238(17) 0.0259(17) 0.0033(13) 0.0094(14) -0.0031(13) C27 0.0215(17) 0.0289(19) 0.0214(17) -0.0035(13) 0.0090(14) -0.0010(14) C33 0.042(2) 0.0270(19) 0.0238(17) 0.0046(14) 0.0077(16) -0.0041(16) C35 0.0255(18) 0.0214(17) 0.0219(17) -0.0028(13) 0.0042(14) 0.0023(13) C42 0.060(3) 0.0193(18) 0.039(2) 0.0051(16) 0.010(2) 0.0001(18) C44 0.050(3) 0.0227(19) 0.045(2) -0.0017(17) 0.006(2) 0.0121(17) C103 0.0275(18) 0.0224(17) 0.0223(17) 0.0075(14) 0.0131(15) 0.0049(14) C110 0.032(2) 0.0262(18) 0.037(2) -0.0101(15) 0.0181(17) -0.0054(15) C111 0.037(2) 0.0233(18) 0.038(2) -0.0020(15) 0.0174(17) -0.0037(15) C112 0.0292(19) 0.0275(18) 0.0272(18) 0.0004(14) 0.0120(15) -0.0007(14) C113 0.0206(17) 0.0234(17) 0.0270(17) -0.0027(13) 0.0126(14) -0.0021(13) C114 0.0217(17) 0.0240(17) 0.0291(18) -0.0008(14) 0.0101(15) -0.0029(13) C115 0.0282(19) 0.037(2) 0.0238(18) -0.0059(15) 0.0120(15) -0.0034(15) C120 0.0243(17) 0.0240(17) 0.0242(17) 0.0000(13) 0.0092(14) -0.0032(14) C121 0.0245(17) 0.0255(17) 0.0181(16) 0.0003(13) 0.0074(14) 0.0004(13) C122 0.0192(16) 0.0213(16) 0.0190(16) -0.0032(12) 0.0053(13) -0.0023(13) C123 0.0240(17) 0.0210(16) 0.0260(17) 0.0029(13) 0.0109(14) -0.0012(13) C124 0.0269(18) 0.0272(17) 0.0229(17) 0.0005(14) 0.0123(14) 0.0011(14) C125 0.0155(15) 0.0223(16) 0.0226(16) -0.0001(13) 0.0061(13) 0.0008(13) C127 0.0199(17) 0.0238(17) 0.0216(17) -0.0008(13) 0.0079(14) -0.0018(13) C132 0.0257(18) 0.0299(18) 0.0236(17) -0.0020(14) 0.0116(14) 0.0020(14) C133 0.0246(17) 0.0253(17) 0.0312(18) -0.0076(14) 0.0135(15) 0.0005(14) C134 0.0296(19) 0.0221(17) 0.034(2) 0.0023(14) 0.0119(16) 0.0062(14) C135 0.0254(18) 0.0238(17) 0.0239(17) 0.0020(13) 0.0069(14) 0.0038(14) C137 0.0172(16) 0.0247(17) 0.0209(16) 0.0004(13) 0.0079(13) 0.0008(13) C333 0.036(2) 0.030(2) 0.040(2) -0.0054(16) 0.0103(17) 0.0078(16) N2 0.0347(17) 0.0315(17) 0.0293(16) 0.0038(13) 0.0167(14) -0.0044(13) N26 0.0189(13) 0.0213(14) 0.0191(13) -0.0002(11) 0.0069(11) -0.0018(11) N31 0.0276(15) 0.0202(14) 0.0177(13) 0.0005(11) 0.0042(12) -0.0008(11) N102 0.0321(16) 0.0274(15) 0.0182(14) 0.0006(12) 0.0080(12) -0.0020(13) N126 0.0179(13) 0.0233(14) 0.0198(13) -0.0009(11) 0.0084(11) -0.0014(11) N131 0.0196(14) 0.0233(14) 0.0209(14) -0.0004(11) 0.0102(11) 0.0006(11) _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 S4 C3 1.637(4) . ? S104 C103 1.636(3) . ? Co1 N2 2.050(3) . ? Co1 N102 2.063(3) . ? Co1 N31 2.120(3) . ? Co1 N131 2.145(3) . ? Co1 N126 2.180(2) . ? Co1 N26 2.195(3) . ? C3 N2 1.163(4) . ? C10 C15 1.382(6) . ? C10 C11 1.384(7) . ? C11 C12 1.399(5) . ? C12 C13 1.409(5) . ? C13 C14 1.393(5) . ? C13 C26 1.491(4) . ? C14 C15 1.405(5) . ? C20 C22 1.386(4) . ? C20 C26 1.395(4) . ? C22 C23 1.396(4) . ? C23 C24 1.389(4) . ? C23 N26 1.428(4) . ? C24 C25 1.391(4) . ? C25 C26 1.400(4) . ? C27 N26 1.269(4) . ? C27 C35 1.463(4) . ? C33 N31 1.345(4) . ? C33 C42 1.395(5) . ? C35 N31 1.353(4) . ? C35 C333 1.392(5) . ? C42 C44 1.372(6) . ? C44 C333 1.392(5) . ? C103 N102 1.166(4) . ? C110 C111 1.382(5) . ? C110 C115 1.384(5) . ? C111 C112 1.386(5) . ? C112 C113 1.392(4) . ? C113 C114 1.395(4) . ? C113 C125 1.488(4) . ? C114 C115 1.394(4) . ? C120 C121 1.389(4) . ? C120 C125 1.402(4) . ? C121 C122 1.395(4) . ? C122 C123 1.386(4) . ? C122 N126 1.431(4) . ? C123 C124 1.389(4) . ? C124 C125 1.407(4) . ? C127 N126 1.280(4) . ? C127 C137 1.463(4) . ? C132 N131 1.344(4) . ? C132 C133 1.387(4) . ? C133 C134 1.378(4) . ? C134 C135 1.391(4) . ? C135 C137 1.385(4) . ? C137 N131 1.351(4) . ? 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 N102 96.38(11) . . ? N2 Co1 N31 96.23(11) . . ? N102 Co1 N31 94.38(10) . . ? N2 Co1 N131 94.72(11) . . ? N102 Co1 N131 91.98(10) . . ? N31 Co1 N131 166.65(10) . . ? N2 Co1 N126 92.86(10) . . ? N102 Co1 N126 165.83(10) . . ? N31 Co1 N126 95.27(9) . . ? N131 Co1 N126 76.53(9) . . ? N2 Co1 N26 169.79(10) . . ? N102 Co1 N26 90.93(10) . . ? N31 Co1 N26 76.05(10) . . ? N131 Co1 N26 92.14(10) . . ? N126 Co1 N26 81.38(9) . . ? N2 C3 S4 179.6(3) . . ? C15 C10 C11 120.1(4) . . ? C10 C11 C12 119.7(4) . . ? C11 C12 C13 120.6(4) . . ? C14 C13 C12 119.0(3) . . ? C14 C13 C26 120.7(3) . . ? C12 C13 C26 120.2(3) . . ? C13 C14 C15 119.6(4) . . ? C10 C15 C14 120.8(4) . . ? C22 C20 C26 120.3(3) . . ? C20 C22 C23 120.4(3) . . ? C24 C23 C22 119.8(3) . . ? C24 C23 N26 118.9(3) . . ? C22 C23 N26 121.1(3) . . ? C23 C24 C25 119.6(3) . . ? C24 C25 C26 120.9(3) . . ? C20 C26 C25 118.9(3) . . ? C20 C26 C13 121.4(3) . . ? C25 C26 C13 119.7(3) . . ? N26 C27 C35 119.0(3) . . ? N31 C33 C42 122.1(4) . . ? N31 C35 C333 122.7(3) . . ? N31 C35 C27 115.2(3) . . ? C333 C35 C27 122.2(3) . . ? C44 C42 C33 119.4(4) . . ? C42 C44 C333 119.3(3) . . ? N102 C103 S104 178.3(3) . . ? C111 C110 C115 118.8(3) . . ? C110 C111 C112 120.6(3) . . ? C111 C112 C113 121.5(3) . . ? C112 C113 C114 117.5(3) . . ? C112 C113 C125 120.7(3) . . ? C114 C113 C125 121.7(3) . . ? C115 C114 C113 120.9(3) . . ? C110 C115 C114 120.7(3) . . ? C121 C120 C125 121.2(3) . . ? C120 C121 C122 120.1(3) . . ? C123 C122 C121 119.6(3) . . ? C123 C122 N126 121.5(3) . . ? C121 C122 N126 118.9(3) . . ? C122 C123 C124 120.5(3) . . ? C123 C124 C125 120.9(3) . . ? C120 C125 C124 117.8(3) . . ? C120 C125 C113 121.9(3) . . ? C124 C125 C113 120.2(3) . . ? N126 C127 C137 119.2(3) . . ? N131 C132 C133 123.1(3) . . ? C134 C133 C132 118.6(3) . . ? C133 C134 C135 119.3(3) . . ? C137 C135 C134 118.6(3) . . ? N131 C137 C135 122.6(3) . . ? N131 C137 C127 115.9(3) . . ? C135 C137 C127 121.5(3) . . ? C35 C333 C44 118.4(4) . . ? C3 N2 Co1 156.0(3) . . ? C27 N26 C23 120.0(3) . . ? C27 N26 Co1 114.0(2) . . ? C23 N26 Co1 125.3(2) . . ? C33 N31 C35 118.1(3) . . ? C33 N31 Co1 126.4(2) . . ? C35 N31 Co1 115.5(2) . . ? C103 N102 Co1 153.7(2) . . ? C127 N126 C122 118.8(3) . . ? C127 N126 Co1 113.5(2) . . ? C122 N126 Co1 127.22(19) . . ? C132 N131 C137 117.7(3) . . ? C132 N131 Co1 127.9(2) . . ? C137 N131 Co1 113.62(19) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.498 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.135 ############################################ # END ############################################ data__[Co(PM-PeA)2(NCS)2](CH3OH)1/2 #293K _database_code_CSD 181920 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.50 H30 Co N6 O0.50 S2' _chemical_formula_weight 755.78 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' 'N' 'N' 0.0061 0.0033 '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' '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' '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 P21/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 15.599(5) _cell_length_b 14.727(5) _cell_length_c 16.870(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.65(5) _cell_angle_gamma 90.00 _cell_volume 3868(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6230 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.10 _reflns_number_total 4924 _reflns_number_gt 2967 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0768P)^2^+1.3383P] 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_number_reflns 4924 _refine_ls_number_parameters 481 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1407 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.019 _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 -0.20628(4) -0.21125(4) 0.54873(3) 0.0546(3) Uani 1 1 d . . . S4 S -0.06294(9) -0.42195(10) 0.38890(8) 0.0794(5) Uani 1 1 d . . . S104 S -0.30604(10) -0.00325(10) 0.34451(7) 0.0761(5) Uani 1 1 d . . . N26 N -0.2233(3) -0.1208(2) 0.65258(19) 0.0489(10) Uani 1 1 d . . . N126 N -0.1740(3) -0.3082(3) 0.6450(2) 0.0527(10) Uani 1 1 d . . . C21 C -0.4484(3) -0.1007(3) 0.7005(3) 0.0627(14) Uani 1 1 d . . . H121 H -0.5014 -0.0920 0.6730 0.075 Uiso 1 1 calc R . . N131 N -0.3226(2) -0.2829(3) 0.5647(2) 0.0549(10) Uani 1 1 d . . . C23 C -0.2971(3) -0.1158(3) 0.6975(2) 0.0484(12) Uani 1 1 d . . . C20 C -0.4444(3) -0.1091(3) 0.7827(3) 0.0620(13) Uani 1 1 d . . . C124 C -0.0767(3) -0.2964(3) 0.7638(3) 0.0684(15) Uani 1 1 d . . . H224 H -0.1217 -0.2785 0.7939 0.082 Uiso 1 1 calc R . . N102 N -0.2597(3) -0.1209(3) 0.4692(2) 0.0711(12) Uani 1 1 d . . . C22 C -0.3753(3) -0.1048(3) 0.6592(3) 0.0572(13) Uani 1 1 d . . . H122 H -0.3796 -0.1000 0.6041 0.069 Uiso 1 1 calc R . . N31 N -0.0862(3) -0.1403(3) 0.5667(2) 0.0624(11) Uani 1 1 d . . . C123 C -0.0921(3) -0.3185(3) 0.6845(3) 0.0518(12) Uani 1 1 d . . . C24 C -0.2905(3) -0.1246(4) 0.7795(3) 0.0686(15) Uani 1 1 d . . . H124 H -0.2373 -0.1331 0.8064 0.082 Uiso 1 1 calc R . . C25 C -0.3645(4) -0.1205(4) 0.8206(3) 0.0778(16) Uani 1 1 d . . . H125 H -0.3600 -0.1257 0.8756 0.093 Uiso 1 1 calc R . . C122 C -0.0246(3) -0.3463(4) 0.6410(3) 0.0681(14) Uani 1 1 d . . . H222 H -0.0342 -0.3607 0.5875 0.082 Uiso 1 1 calc R . . C17 C -0.5238(4) -0.1048(3) 0.8265(3) 0.0640(15) Uani 1 1 d . . . C120 C 0.0731(3) -0.3308(3) 0.7558(3) 0.0627(14) Uani 1 1 d . . . C116 C 0.2244(4) -0.3493(4) 0.8227(3) 0.0668(15) Uani 1 1 d . . . C117 C 0.1594(4) -0.3395(4) 0.7942(3) 0.0696(16) Uani 1 1 d . . . C3 C -0.1201(3) -0.3485(4) 0.4345(3) 0.0547(13) Uani 1 1 d . . . C127 C -0.2391(4) -0.3460(4) 0.6720(3) 0.0578(13) Uani 1 1 d D . . H227 H -0.227(3) -0.384(3) 0.719(2) 0.105(19) Uiso 1 1 d D . . C113 C 0.3122(4) -0.3622(3) 0.8575(3) 0.0686(14) Uani 1 1 d . . . C130 C -0.3227(3) -0.3333(3) 0.6311(3) 0.0527(12) Uani 1 1 d . . . C125 C 0.0051(4) -0.3010(4) 0.7975(3) 0.0771(16) Uani 1 1 d . . . H225 H 0.0154 -0.2835 0.8502 0.093 Uiso 1 1 calc R . . C27 C -0.1551(4) -0.0805(4) 0.6769(3) 0.0585(13) Uani 1 1 d D . . H127 H -0.147(3) -0.042(3) 0.7249(18) 0.072(15) Uiso 1 1 d D . . C114 C 0.3843(4) -0.3470(4) 0.8151(4) 0.0903(18) Uani 1 1 d . . . H214 H 0.3775 -0.3260 0.7630 0.108 Uiso 1 1 calc R . . C132 C -0.3960(4) -0.2735(3) 0.5225(3) 0.0671(14) Uani 1 1 d . . . H232 H -0.3962 -0.2413 0.4750 0.081 Uiso 1 1 calc R . . N2 N -0.1605(3) -0.2964(3) 0.4662(2) 0.0714(13) Uani 1 1 d . . . C134 C -0.4727(4) -0.3588(4) 0.6145(4) 0.0788(16) Uani 1 1 d . . . H234 H -0.5233 -0.3831 0.6318 0.095 Uiso 1 1 calc R . . C13 C -0.6657(4) -0.0858(4) 0.8932(3) 0.0710(15) Uani 1 1 d . . . C103 C -0.2785(3) -0.0716(3) 0.4178(3) 0.0555(12) Uiso 1 1 d . . . C121 C 0.0569(3) -0.3526(4) 0.6770(3) 0.0684(15) Uani 1 1 d . . . H221 H 0.1018 -0.3720 0.6475 0.082 Uiso 1 1 calc R . . C135 C -0.3963(4) -0.3716(4) 0.6574(3) 0.0709(15) Uani 1 1 d . . . H235 H -0.3940 -0.4058 0.7038 0.085 Uiso 1 1 calc R . . C115 C 0.4651(4) -0.3624(4) 0.8485(4) 0.0913(19) Uani 1 1 d . . . H215 H 0.5127 -0.3513 0.8195 0.110 Uiso 1 1 calc R . . C30 C -0.0778(3) -0.0880(3) 0.6324(3) 0.0589(13) Uani 1 1 d . . . C133 C -0.4734(4) -0.3092(4) 0.5452(4) 0.0827(17) Uani 1 1 d . . . H233 H -0.5242 -0.2998 0.5143 0.099 Uiso 1 1 calc R . . C35 C -0.0023(4) -0.0464(4) 0.6567(4) 0.0837(17) Uani 1 1 d . . . H135 H 0.0019 -0.0122 0.7031 0.100 Uiso 1 1 calc R . . C16 C -0.5838(4) -0.0990(4) 0.8563(3) 0.0674(15) Uani 1 1 d . . . C12 C -0.7411(4) -0.1111(4) 0.8505(3) 0.0823(17) Uani 1 1 d . . . H112 H -0.7382 -0.1380 0.8009 0.099 Uiso 1 1 calc R . . C33 C 0.0593(5) -0.1067(5) 0.5436(5) 0.110(2) Uani 1 1 d . . . H133 H 0.1052 -0.1134 0.5116 0.132 Uiso 1 1 calc R . . C14 C -0.6717(4) -0.0465(4) 0.9674(3) 0.0839(17) Uani 1 1 d . . . H114 H -0.6220 -0.0289 0.9968 0.101 Uiso 1 1 calc R . . C112 C 0.3267(4) -0.3922(4) 0.9355(3) 0.0800(16) Uani 1 1 d . . . H212 H 0.2803 -0.4022 0.9663 0.096 Uiso 1 1 calc R . . C110 C 0.4756(4) -0.3940(4) 0.9239(4) 0.0873(18) Uani 1 1 d . . . H210 H 0.5306 -0.4068 0.9458 0.105 Uiso 1 1 calc R . . C34 C 0.0673(4) -0.0559(5) 0.6112(5) 0.107(2) Uani 1 1 d . . . H134 H 0.1193 -0.0280 0.6264 0.128 Uiso 1 1 calc R . . C11 C -0.8204(4) -0.0968(4) 0.8809(4) 0.098(2) Uani 1 1 d . . . H111 H -0.8706 -0.1133 0.8518 0.118 Uiso 1 1 calc R . . C111 C 0.4078(5) -0.4069(4) 0.9671(4) 0.0883(18) Uani 1 1 d . . . H211 H 0.4162 -0.4263 1.0195 0.106 Uiso 1 1 calc R . . C32 C -0.0183(5) -0.1477(4) 0.5238(4) 0.0921(19) Uani 1 1 d . . . H132 H -0.0234 -0.1825 0.4777 0.111 Uiso 1 1 calc R . . C15 C -0.7501(5) -0.0334(4) 0.9977(4) 0.098(2) Uani 1 1 d . . . H115 H -0.7530 -0.0077 1.0479 0.117 Uiso 1 1 calc R . . C10 C -0.8241(4) -0.0574(5) 0.9553(4) 0.097(2) Uani 1 1 d . . . H100 H -0.8770 -0.0474 0.9763 0.116 Uiso 1 1 calc R . . O40 C 0.3368(11) -0.2245(11) 0.6327(10) 0.123(5) Uani 0.50 1 d P . . C41 C 0.2695(12) -0.2587(13) 0.6045(10) 0.146(7) 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 0.0594(5) 0.0658(4) 0.0391(3) 0.0016(3) 0.0071(3) 0.0081(4) S4 0.0793(10) 0.0879(11) 0.0730(9) -0.0031(8) 0.0210(8) 0.0191(9) S104 0.0868(11) 0.0880(10) 0.0527(7) 0.0167(7) -0.0029(7) 0.0025(8) N26 0.050(3) 0.055(2) 0.042(2) 0.0040(18) 0.007(2) 0.006(2) N126 0.049(3) 0.062(3) 0.047(2) -0.0066(19) 0.003(2) 0.010(2) C21 0.056(3) 0.071(3) 0.060(3) 0.001(3) -0.004(3) 0.008(3) N131 0.054(3) 0.063(3) 0.046(2) -0.005(2) -0.007(2) 0.010(2) C23 0.046(3) 0.054(3) 0.045(3) -0.001(2) 0.007(3) 0.008(2) C20 0.059(4) 0.066(3) 0.061(3) -0.002(3) 0.006(3) 0.001(3) C124 0.072(4) 0.088(4) 0.045(3) -0.003(3) 0.005(3) 0.022(3) N102 0.080(3) 0.079(3) 0.054(2) 0.008(2) 0.001(2) 0.008(2) C22 0.056(4) 0.071(3) 0.046(3) -0.002(2) 0.010(3) 0.007(3) N31 0.059(3) 0.074(3) 0.056(2) 0.003(2) 0.021(2) 0.007(2) C123 0.053(3) 0.055(3) 0.047(3) -0.001(2) 0.002(3) 0.009(3) C24 0.055(3) 0.110(4) 0.042(3) 0.001(3) 0.006(3) 0.005(3) C25 0.077(4) 0.114(5) 0.043(3) 0.001(3) 0.012(3) 0.006(4) C122 0.065(4) 0.085(4) 0.054(3) -0.017(3) -0.002(3) 0.011(3) C17 0.064(4) 0.063(3) 0.067(3) -0.002(3) 0.016(3) 0.013(3) C120 0.066(4) 0.059(3) 0.062(3) -0.001(3) -0.007(3) 0.008(3) C116 0.071(4) 0.059(3) 0.066(3) 0.002(3) -0.022(3) 0.006(3) C117 0.078(5) 0.059(4) 0.070(4) -0.001(3) -0.007(3) 0.004(3) C3 0.059(3) 0.067(3) 0.038(2) 0.009(2) -0.003(2) -0.005(3) C127 0.058(4) 0.065(3) 0.049(3) 0.002(3) -0.004(3) 0.013(3) C113 0.074(4) 0.061(3) 0.070(3) -0.001(3) -0.001(4) 0.001(3) C130 0.053(4) 0.052(3) 0.053(3) 0.002(2) 0.009(3) 0.004(3) C125 0.080(4) 0.103(5) 0.046(3) -0.010(3) -0.012(3) 0.020(4) C27 0.058(4) 0.067(4) 0.052(3) -0.001(3) 0.006(3) 0.001(3) C114 0.088(5) 0.106(5) 0.076(4) 0.013(4) -0.003(4) 0.004(4) C132 0.077(4) 0.067(4) 0.057(3) -0.003(3) 0.000(3) 0.000(3) N2 0.082(3) 0.082(3) 0.051(2) -0.009(2) 0.009(2) 0.017(3) C134 0.062(4) 0.087(4) 0.088(4) 0.004(4) 0.008(4) -0.007(3) C13 0.071(4) 0.067(4) 0.077(4) 0.010(3) 0.023(4) 0.005(3) C121 0.052(4) 0.084(4) 0.069(3) -0.012(3) 0.003(3) 0.011(3) C135 0.072(4) 0.073(4) 0.068(3) 0.003(3) 0.003(3) -0.003(3) C115 0.063(5) 0.106(5) 0.106(5) 0.008(4) 0.010(4) -0.002(4) C30 0.054(4) 0.059(3) 0.064(3) 0.010(3) 0.010(3) 0.001(3) C133 0.075(4) 0.083(4) 0.088(4) -0.005(3) -0.016(4) 0.001(4) C35 0.059(4) 0.096(5) 0.097(4) -0.005(4) 0.011(4) -0.015(4) C16 0.061(4) 0.072(4) 0.071(3) 0.007(3) 0.018(3) 0.000(3) C12 0.081(5) 0.092(4) 0.077(4) -0.005(3) 0.027(4) 0.000(4) C33 0.070(5) 0.131(6) 0.133(7) 0.004(5) 0.045(5) -0.008(5) C14 0.074(4) 0.102(5) 0.076(4) -0.008(4) 0.013(3) 0.006(4) C112 0.069(4) 0.102(4) 0.068(4) 0.001(3) 0.000(3) 0.004(3) C110 0.068(5) 0.087(4) 0.103(5) -0.013(4) -0.022(4) 0.004(3) C34 0.065(5) 0.114(6) 0.143(7) 0.008(5) 0.015(5) -0.022(4) C11 0.076(5) 0.108(5) 0.112(5) -0.014(4) 0.021(4) -0.006(4) C111 0.083(5) 0.106(5) 0.073(4) 0.005(4) -0.015(4) 0.013(4) C32 0.091(5) 0.109(5) 0.081(4) -0.001(4) 0.037(4) -0.005(4) C15 0.095(5) 0.117(5) 0.086(4) -0.008(4) 0.040(4) 0.022(4) C10 0.065(4) 0.119(5) 0.111(5) -0.014(4) 0.031(4) 0.002(4) O40 0.129(13) 0.117(12) 0.123(12) 0.034(10) 0.005(11) 0.013(10) C41 0.146(16) 0.177(17) 0.118(13) -0.027(12) 0.019(11) -0.057(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 N102 2.031(4) . ? Co1 N2 2.036(5) . ? Co1 N131 2.130(4) . ? Co1 N31 2.150(4) . ? Co1 N126 2.196(4) . ? Co1 N26 2.230(4) . ? S4 C3 1.627(6) . ? S104 C103 1.630(5) . ? N26 C27 1.264(6) . ? N26 C23 1.421(5) . ? N126 C127 1.268(6) . ? N126 C123 1.411(6) . ? C21 C22 1.375(6) . ? C21 C20 1.390(6) . ? C21 H121 0.9300 . ? N131 C132 1.318(6) . ? N131 C130 1.344(5) . ? C23 C22 1.353(6) . ? C23 C24 1.386(6) . ? C20 C25 1.373(7) . ? C20 C17 1.484(8) . ? C124 C125 1.367(7) . ? C124 C123 1.383(6) . ? C124 H224 0.9300 . ? N102 C103 1.155(5) . ? C22 H122 0.9300 . ? N31 C32 1.325(7) . ? N31 C30 1.349(6) . ? C123 C122 1.383(6) . ? C24 C25 1.385(7) . ? C24 H124 0.9300 . ? C25 H125 0.9300 . ? C122 C121 1.376(6) . ? C122 H222 0.9300 . ? C17 C16 1.094(7) . ? C120 C121 1.376(6) . ? C120 C125 1.380(7) . ? C120 C117 1.462(8) . ? C116 C117 1.104(7) . ? C116 C113 1.467(8) . ? C3 N2 1.147(6) . ? C127 C130 1.447(7) . ? C127 H227 0.98(2) . ? C113 C114 1.390(7) . ? C113 C112 1.393(7) . ? C130 C135 1.377(6) . ? C125 H225 0.9300 . ? C27 C30 1.465(7) . ? C27 H127 0.987(19) . ? C114 C115 1.366(7) . ? C114 H214 0.9300 . ? C132 C133 1.392(7) . ? C132 H232 0.9300 . ? C134 C135 1.368(7) . ? C134 C133 1.379(7) . ? C134 H234 0.9300 . ? C13 C14 1.389(7) . ? C13 C12 1.389(7) . ? C13 C16 1.469(8) . ? C121 H221 0.9300 . ? C135 H235 0.9300 . ? C115 C110 1.355(8) . ? C115 H215 0.9300 . ? C30 C35 1.366(7) . ? C133 H233 0.9300 . ? C35 C34 1.377(8) . ? C35 H135 0.9300 . ? C12 C11 1.385(8) . ? C12 H112 0.9300 . ? C33 C34 1.361(9) . ? C33 C32 1.374(8) . ? C33 H133 0.9300 . ? C14 C15 1.369(7) . ? C14 H114 0.9300 . ? C112 C111 1.358(7) . ? C112 H212 0.9300 . ? C110 C111 1.336(8) . ? C110 H210 0.9300 . ? C34 H134 0.9300 . ? C11 C10 1.387(8) . ? C11 H111 0.9300 . ? C111 H211 0.9300 . ? C32 H132 0.9300 . ? C15 C10 1.366(8) . ? C15 H115 0.9300 . ? C10 H100 0.9300 . ? O40 C41 1.232(19) . ? 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 N102 Co1 N2 95.65(16) . . ? N102 Co1 N131 95.23(16) . . ? N2 Co1 N131 96.90(16) . . ? N102 Co1 N31 95.28(16) . . ? N2 Co1 N31 93.17(17) . . ? N131 Co1 N31 164.65(14) . . ? N102 Co1 N126 168.39(17) . . ? N2 Co1 N126 91.81(15) . . ? N131 Co1 N126 75.00(16) . . ? N31 Co1 N126 93.17(16) . . ? N102 Co1 N26 93.64(15) . . ? N2 Co1 N26 165.78(16) . . ? N131 Co1 N26 92.95(15) . . ? N31 Co1 N26 75.24(16) . . ? N126 Co1 N26 80.84(12) . . ? C27 N26 C23 119.8(4) . . ? C27 N26 Co1 113.3(3) . . ? C23 N26 Co1 126.2(3) . . ? C127 N126 C123 120.3(4) . . ? C127 N126 Co1 113.6(3) . . ? C123 N126 Co1 125.3(3) . . ? C22 C21 C20 121.0(5) . . ? C22 C21 H121 119.5 . . ? C20 C21 H121 119.5 . . ? C132 N131 C130 117.5(4) . . ? C132 N131 Co1 126.7(3) . . ? C130 N131 Co1 115.2(3) . . ? C22 C23 C24 119.7(4) . . ? C22 C23 N26 119.2(4) . . ? C24 C23 N26 121.1(4) . . ? C25 C20 C21 117.2(5) . . ? C25 C20 C17 122.4(5) . . ? C21 C20 C17 120.4(5) . . ? C125 C124 C123 119.4(5) . . ? C125 C124 H224 120.3 . . ? C123 C124 H224 120.3 . . ? C103 N102 Co1 169.2(4) . . ? C23 C22 C21 121.0(4) . . ? C23 C22 H122 119.5 . . ? C21 C22 H122 119.5 . . ? C32 N31 C30 117.1(5) . . ? C32 N31 Co1 127.1(4) . . ? C30 N31 Co1 115.6(3) . . ? C124 C123 C122 119.4(5) . . ? C124 C123 N126 121.8(4) . . ? C122 C123 N126 118.6(4) . . ? C25 C24 C23 119.0(5) . . ? C25 C24 H124 120.5 . . ? C23 C24 H124 120.5 . . ? C20 C25 C24 122.2(5) . . ? C20 C25 H125 118.9 . . ? C24 C25 H125 118.9 . . ? C121 C122 C123 119.9(4) . . ? C121 C122 H222 120.0 . . ? C123 C122 H222 120.0 . . ? C16 C17 C20 176.9(6) . . ? C121 C120 C125 117.8(5) . . ? C121 C120 C117 120.9(5) . . ? C125 C120 C117 121.2(5) . . ? C117 C116 C113 177.7(6) . . ? C116 C117 C120 177.5(6) . . ? N2 C3 S4 179.5(5) . . ? N126 C127 C130 119.3(5) . . ? N126 C127 H227 115(3) . . ? C130 C127 H227 126(3) . . ? C114 C113 C112 116.7(5) . . ? C114 C113 C116 122.6(5) . . ? C112 C113 C116 120.7(5) . . ? N131 C130 C135 122.6(5) . . ? N131 C130 C127 114.8(5) . . ? C135 C130 C127 122.5(5) . . ? C124 C125 C120 122.1(5) . . ? C124 C125 H225 119.0 . . ? C120 C125 H225 119.0 . . ? N26 C27 C30 120.1(5) . . ? N26 C27 H127 127(3) . . ? C30 C27 H127 113(3) . . ? C115 C114 C113 121.1(6) . . ? C115 C114 H214 119.5 . . ? C113 C114 H214 119.5 . . ? N131 C132 C133 123.4(5) . . ? N131 C132 H232 118.3 . . ? C133 C132 H232 118.3 . . ? C3 N2 Co1 163.3(4) . . ? C135 C134 C133 118.7(5) . . ? C135 C134 H234 120.6 . . ? C133 C134 H234 120.6 . . ? C14 C13 C12 118.4(5) . . ? C14 C13 C16 123.2(6) . . ? C12 C13 C16 118.4(5) . . ? N102 C103 S104 179.0(5) . . ? C120 C121 C122 121.2(5) . . ? C120 C121 H221 119.4 . . ? C122 C121 H221 119.4 . . ? C134 C135 C130 119.4(5) . . ? C134 C135 H235 120.3 . . ? C130 C135 H235 120.3 . . ? C110 C115 C114 119.9(6) . . ? C110 C115 H215 120.0 . . ? C114 C115 H215 120.0 . . ? N31 C30 C35 122.6(5) . . ? N31 C30 C27 115.1(5) . . ? C35 C30 C27 122.3(5) . . ? C134 C133 C132 118.3(5) . . ? C134 C133 H233 120.9 . . ? C132 C133 H233 120.9 . . ? C30 C35 C34 118.8(6) . . ? C30 C35 H135 120.6 . . ? C34 C35 H135 120.6 . . ? C17 C16 C13 176.2(6) . . ? C11 C12 C13 120.9(6) . . ? C11 C12 H112 119.5 . . ? C13 C12 H112 119.5 . . ? C34 C33 C32 118.6(6) . . ? C34 C33 H133 120.7 . . ? C32 C33 H133 120.7 . . ? C15 C14 C13 120.6(6) . . ? C15 C14 H114 119.7 . . ? C13 C14 H114 119.7 . . ? C111 C112 C113 120.9(6) . . ? C111 C112 H212 119.5 . . ? C113 C112 H212 119.5 . . ? C111 C110 C115 120.5(6) . . ? C111 C110 H210 119.7 . . ? C115 C110 H210 119.8 . . ? C33 C34 C35 119.2(6) . . ? C33 C34 H134 120.4 . . ? C35 C34 H134 120.4 . . ? C12 C11 C10 119.2(6) . . ? C12 C11 H111 120.4 . . ? C10 C11 H111 120.4 . . ? C110 C111 C112 120.8(6) . . ? C110 C111 H211 119.6 . . ? C112 C111 H211 119.6 . . ? N31 C32 C33 123.6(6) . . ? N31 C32 H132 118.2 . . ? C33 C32 H132 118.2 . . ? C10 C15 C14 120.9(6) . . ? C10 C15 H115 119.5 . . ? C14 C15 H115 119.5 . . ? C15 C10 C11 120.0(6) . . ? C15 C10 H100 120.0 . . ? C11 C10 H100 120.0 . . ? _diffrn_measured_fraction_theta_max 0.714 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.714 _refine_diff_density_max 0.300 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.051 ############################################ # END ############################################ data__[Co(PM-PeA)2(NCS)2]293K _database_code_CSD 181921 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H28 Co N6 S2' _chemical_formula_weight 751.76 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' '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 P21/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 15.674(3) _cell_length_b 14.599(3) _cell_length_c 16.844(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.105(4) _cell_angle_gamma 90.00 _cell_volume 3848.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12611 _diffrn_reflns_av_R_equivalents 0.1182 _diffrn_reflns_av_sigmaI/netI 0.1212 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.24 _reflns_number_total 7746 _reflns_number_gt 3364 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0496P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7746 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1656 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.29517(3) 0.70955(3) 0.04804(2) 0.05091(14) Uani 1 1 d . . . S4 S 0.43845(6) 0.92375(7) -0.11187(6) 0.0738(3) Uani 1 1 d . . . S104 S 0.19362(6) 0.49769(7) -0.15402(5) 0.0735(3) Uani 1 1 d . . . N31 N 0.17899(15) 0.78250(18) 0.06471(15) 0.0525(6) Uani 1 1 d . . . C127 C 0.3460(2) 0.5781(2) 0.1771(2) 0.0525(8) Uani 1 1 d . . . N126 N 0.27751(15) 0.61927(16) 0.15188(13) 0.0449(6) Uani 1 1 d . . . N26 N 0.32831(16) 0.80745(17) 0.14456(14) 0.0498(6) Uani 1 1 d . . . N2 N 0.34084(19) 0.7960(2) -0.03492(16) 0.0707(8) Uani 1 1 d . . . C103 C 0.22131(18) 0.5687(2) -0.08189(19) 0.0532(8) Uani 1 1 d . . . C122 C 0.12445(19) 0.6041(2) 0.1595(2) 0.0526(8) Uani 1 1 d . . . C123 C 0.20381(17) 0.61429(19) 0.19819(16) 0.0444(7) Uani 1 1 d . . . C23 C 0.41041(18) 0.8175(2) 0.18393(18) 0.0478(7) Uani 1 1 d . . . C24 C 0.4261(2) 0.7952(3) 0.26307(19) 0.0648(10) Uani 1 1 d . . . C120 C 0.05683(19) 0.6093(2) 0.2843(2) 0.0564(8) Uani 1 1 d . . . N131 N 0.41478(15) 0.63764(19) 0.06604(15) 0.0581(7) Uani 1 1 d . . . C121 C 0.0522(2) 0.6004(2) 0.2020(2) 0.0567(9) Uani 1 1 d . . . C25 C 0.5076(2) 0.8000(3) 0.2969(2) 0.0712(11) Uani 1 1 d . . . N102 N 0.24083(18) 0.6176(2) -0.03075(17) 0.0690(8) Uani 1 1 d . . . C13 C 0.8143(2) 0.8592(2) 0.3565(2) 0.0654(9) Uani 1 1 d . . . C32 C 0.1047(2) 0.7733(3) 0.0231(2) 0.0642(10) Uani 1 1 d . . . C125 C 0.1369(2) 0.6206(3) 0.3222(2) 0.0700(11) Uani 1 1 d . . . C3 C 0.38187(19) 0.8488(2) -0.06668(18) 0.0514(8) Uani 1 1 d . . . C116 C -0.0833(2) 0.6006(2) 0.3590(2) 0.0647(10) Uani 1 1 d . . . C16 C 0.7277(2) 0.8455(2) 0.3201(2) 0.0633(9) Uani 1 1 d . . . C35 C 0.1063(2) 0.8748(3) 0.1576(2) 0.0672(10) Uani 1 1 d . . . C20 C 0.5754(2) 0.8275(2) 0.2538(2) 0.0588(9) Uani 1 1 d . . . C27 C 0.2636(2) 0.8469(3) 0.1714(2) 0.0556(9) Uani 1 1 d . . . C136 C 0.42313(19) 0.5860(2) 0.1319(2) 0.0562(8) Uani 1 1 d . . . C117 C -0.0218(2) 0.6059(2) 0.3282(2) 0.0633(9) Uani 1 1 d . . . C36 C 0.17916(19) 0.8348(2) 0.13087(19) 0.0534(8) Uani 1 1 d . . . C21 C 0.5594(2) 0.8481(3) 0.1745(2) 0.0655(10) Uani 1 1 d . . . C22 C 0.4783(2) 0.8429(3) 0.1392(2) 0.0658(10) Uani 1 1 d . . . C34 C 0.0297(3) 0.8613(3) 0.1149(3) 0.0795(12) Uani 1 1 d . . . C113 C -0.1656(2) 0.5882(2) 0.3963(2) 0.0632(9) Uani 1 1 d . . . C124 C 0.2096(2) 0.6236(3) 0.28035(19) 0.0618(10) Uani 1 1 d . . . C33 C 0.0288(2) 0.8113(3) 0.0468(3) 0.0773(12) Uani 1 1 d . . . C17 C 0.6619(2) 0.8360(3) 0.2917(2) 0.0669(10) Uani 1 1 d . . . C11 C 0.9074(3) 0.9021(3) 0.4683(3) 0.0843(12) Uani 1 1 d . . . C10 C 0.9768(3) 0.8927(3) 0.4242(3) 0.0850(13) Uani 1 1 d . . . C12 C 0.8263(3) 0.8858(3) 0.4358(3) 0.0770(12) Uani 1 1 d . . . C112 C -0.2402(2) 0.6099(3) 0.3523(3) 0.0765(11) Uani 1 1 d . . . C135 C 0.4992(2) 0.5449(3) 0.1578(3) 0.0807(12) Uani 1 1 d . . . C114 C -0.1713(3) 0.5547(3) 0.4723(2) 0.0807(12) Uani 1 1 d . . . C132 C 0.4837(3) 0.6466(3) 0.0228(3) 0.0854(13) Uani 1 1 d . . . C110 C -0.3238(3) 0.5629(3) 0.4597(3) 0.0923(14) Uani 1 1 d . . . C14 C 0.8854(3) 0.8485(3) 0.3118(3) 0.0870(13) Uani 1 1 d . . . C115 C -0.2504(3) 0.5419(4) 0.5035(3) 0.0924(15) Uani 1 1 d . . . C111 C -0.3191(3) 0.5965(3) 0.3843(3) 0.0897(13) Uani 1 1 d . . . C134 C 0.5687(3) 0.5553(4) 0.1124(4) 0.1055(17) Uani 1 1 d . . . C15 C 0.9667(3) 0.8649(3) 0.3460(3) 0.0904(14) Uani 1 1 d . . . C133 C 0.5612(3) 0.6046(4) 0.0447(4) 0.1056(17) Uani 1 1 d . . . H111 H -0.243(2) 0.640(2) 0.292(2) 0.087(11) Uiso 1 1 d . . . H421 H 0.1228(16) 0.5952(18) 0.1088(16) 0.042(8) Uiso 1 1 d . . . H321 H 0.1083(19) 0.737(2) -0.0196(18) 0.057(10) Uiso 1 1 d . . . H201 H 0.4663(19) 0.858(2) 0.0844(19) 0.070(10) Uiso 1 1 d . . . H361 H -0.0012(18) 0.5898(19) 0.1764(17) 0.057(9) Uiso 1 1 d . . . H211 H 0.6038(19) 0.867(2) 0.1481(18) 0.066(10) Uiso 1 1 d . . . H171 H 0.2615(18) 0.6354(19) 0.3052(16) 0.052(9) Uiso 1 1 d . . . H102 H 0.500(2) 0.508(3) 0.206(2) 0.103(15) Uiso 1 1 d . . . H351 H 0.519(2) 0.777(3) 0.350(2) 0.108(14) Uiso 1 1 d . . . H252 H -0.021(2) 0.891(3) 0.134(2) 0.106(14) Uiso 1 1 d . . . H251 H 0.2684(19) 0.884(2) 0.2132(19) 0.065(11) Uiso 1 1 d . . . H311 H 0.1447(18) 0.630(2) 0.3784(19) 0.063(9) Uiso 1 1 d . . . H481 H 0.3482(19) 0.536(2) 0.223(2) 0.077(11) Uiso 1 1 d . . . H101 H -0.381(3) 0.556(3) 0.482(3) 0.128(15) Uiso 1 1 d . . . H161 H -0.0202(19) 0.799(2) 0.0151(18) 0.058(9) Uiso 1 1 d . . . H41 H -0.376(3) 0.617(3) 0.351(2) 0.111(14) Uiso 1 1 d . . . H81 H 0.467(2) 0.684(2) -0.028(2) 0.094(13) Uiso 1 1 d . . . H131 H 0.111(2) 0.913(2) 0.199(2) 0.073(12) Uiso 1 1 d . . . H91 H -0.117(2) 0.532(2) 0.504(2) 0.093(13) Uiso 1 1 d . . . H132 H 1.044(3) 0.911(3) 0.444(3) 0.137(16) Uiso 1 1 d . . . H391 H 0.376(2) 0.782(2) 0.290(2) 0.085(12) Uiso 1 1 d . . . H71 H 0.779(3) 0.881(3) 0.464(3) 0.113(16) Uiso 1 1 d . . . H21 H 1.015(3) 0.856(3) 0.308(2) 0.120(15) Uiso 1 1 d . . . H92 H 0.874(3) 0.827(3) 0.256(3) 0.132(17) Uiso 1 1 d . . . H31 H 0.617(2) 0.528(3) 0.128(2) 0.098(15) Uiso 1 1 d . . . H141 H 0.912(3) 0.913(3) 0.527(3) 0.15(2) Uiso 1 1 d . . . H11 H 0.603(3) 0.614(3) -0.003(3) 0.156(19) Uiso 1 1 d . . . H51 H -0.255(3) 0.514(3) 0.551(3) 0.110(15) 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 0.0499(2) 0.0619(3) 0.0412(2) -0.0010(2) 0.00582(17) -0.0076(2) S4 0.0658(6) 0.0837(7) 0.0736(6) 0.0020(6) 0.0184(5) -0.0191(5) S104 0.0720(6) 0.0906(7) 0.0570(5) -0.0197(5) -0.0050(5) -0.0005(5) N31 0.0491(15) 0.0562(17) 0.0516(15) 0.0044(14) -0.0023(12) -0.0068(13) C127 0.0508(19) 0.055(2) 0.0516(19) 0.0005(18) 0.0082(15) -0.0011(17) N126 0.0423(14) 0.0490(16) 0.0440(14) -0.0055(12) 0.0073(11) -0.0021(12) N26 0.0475(15) 0.0540(18) 0.0477(15) 0.0015(13) 0.0016(12) -0.0112(13) N2 0.081(2) 0.084(2) 0.0478(16) 0.0021(17) 0.0085(15) -0.0186(17) C103 0.0443(17) 0.070(2) 0.0458(18) -0.0016(18) 0.0041(15) 0.0066(17) C122 0.0481(18) 0.066(2) 0.0438(18) 0.0019(17) 0.0010(15) -0.0096(16) C123 0.0406(16) 0.0486(18) 0.0446(16) 0.0004(15) 0.0069(13) -0.0031(14) C23 0.0454(17) 0.0480(19) 0.0497(18) -0.0009(15) -0.0001(14) -0.0080(14) C24 0.063(2) 0.085(3) 0.0470(19) 0.004(2) 0.0021(17) -0.018(2) C120 0.0473(18) 0.060(2) 0.063(2) 0.0030(17) 0.0165(16) -0.0066(16) N131 0.0500(15) 0.071(2) 0.0549(16) -0.0051(15) 0.0174(13) -0.0054(14) C121 0.0436(18) 0.063(2) 0.063(2) -0.0015(18) 0.0004(17) -0.0112(17) C25 0.068(2) 0.096(3) 0.048(2) 0.008(2) -0.0127(18) -0.019(2) N102 0.076(2) 0.077(2) 0.0536(17) -0.0113(17) 0.0012(15) -0.0076(17) C13 0.056(2) 0.061(2) 0.077(3) -0.002(2) -0.0083(19) -0.0027(18) C32 0.064(2) 0.070(3) 0.057(2) 0.001(2) -0.0072(18) -0.003(2) C125 0.059(2) 0.106(3) 0.046(2) -0.001(2) 0.0121(17) -0.004(2) C3 0.0450(17) 0.066(2) 0.0429(17) -0.0079(17) -0.0016(14) 0.0011(17) C116 0.055(2) 0.064(2) 0.075(2) -0.0096(19) 0.0127(19) -0.0009(18) C16 0.054(2) 0.056(2) 0.078(2) -0.0004(19) -0.0115(18) -0.0093(18) C35 0.063(2) 0.067(3) 0.072(3) -0.008(2) 0.005(2) 0.006(2) C20 0.058(2) 0.058(2) 0.059(2) -0.0011(18) -0.0090(17) -0.0110(17) C27 0.058(2) 0.058(2) 0.051(2) -0.0063(18) -0.0033(17) -0.0062(18) C136 0.0451(18) 0.061(2) 0.064(2) -0.0080(18) 0.0090(16) 0.0017(17) C117 0.063(2) 0.061(2) 0.066(2) 0.0012(18) 0.0126(18) -0.0128(18) C36 0.0528(19) 0.052(2) 0.056(2) -0.0006(17) 0.0023(16) -0.0029(16) C21 0.048(2) 0.078(3) 0.070(3) 0.008(2) 0.0033(18) -0.0146(19) C22 0.060(2) 0.087(3) 0.050(2) 0.012(2) -0.0055(18) -0.015(2) C34 0.056(2) 0.086(3) 0.097(3) 0.000(3) 0.008(2) 0.011(2) C113 0.056(2) 0.063(2) 0.073(2) -0.0057(19) 0.0247(19) -0.0074(18) C124 0.0452(19) 0.097(3) 0.0423(18) -0.0052(19) -0.0005(15) -0.0045(19) C33 0.057(2) 0.084(3) 0.089(3) 0.005(3) -0.016(2) 0.003(2) C17 0.074(2) 0.055(2) 0.070(2) 0.0017(19) -0.005(2) -0.006(2) C11 0.069(3) 0.097(3) 0.085(3) -0.003(3) -0.014(2) 0.000(2) C10 0.062(3) 0.076(3) 0.113(4) 0.010(3) -0.024(3) 0.000(2) C12 0.058(2) 0.092(3) 0.080(3) -0.008(2) -0.005(2) -0.002(2) C112 0.064(2) 0.085(3) 0.083(3) 0.009(2) 0.023(2) 0.007(2) C135 0.053(2) 0.090(3) 0.099(3) 0.002(3) 0.011(2) 0.018(2) C114 0.061(2) 0.104(3) 0.078(3) 0.007(2) 0.013(2) -0.012(2) C132 0.066(3) 0.108(4) 0.086(3) 0.005(3) 0.036(2) 0.008(2) C110 0.060(3) 0.117(4) 0.103(3) 0.011(3) 0.033(3) -0.002(3) C14 0.077(3) 0.098(3) 0.085(3) -0.010(3) 0.000(2) -0.009(3) C115 0.087(3) 0.121(4) 0.073(3) 0.012(3) 0.031(3) -0.016(3) C111 0.058(2) 0.110(4) 0.102(3) 0.016(3) 0.015(2) 0.006(2) C134 0.054(3) 0.129(4) 0.134(5) 0.003(4) 0.013(3) 0.022(3) C15 0.058(3) 0.093(3) 0.122(4) 0.005(3) 0.017(3) -0.004(2) C133 0.066(3) 0.131(4) 0.124(4) -0.014(4) 0.047(3) 0.002(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 N102 2.041(3) . ? Co1 N2 2.041(3) . ? Co1 N31 2.141(3) . ? Co1 N131 2.156(3) . ? Co1 N26 2.206(2) . ? Co1 N126 2.219(2) . ? S4 C3 1.624(4) . ? S104 C103 1.638(4) . ? N31 C32 1.332(4) . ? N31 C36 1.351(4) . ? C127 N126 1.282(4) . ? C127 C136 1.468(4) . ? N126 C123 1.430(3) . ? N26 C27 1.270(4) . ? N26 C23 1.423(3) . ? N2 C3 1.154(4) . ? C103 N102 1.148(4) . ? C122 C121 1.374(4) . ? C122 C123 1.381(4) . ? C123 C124 1.389(4) . ? C23 C24 1.381(4) . ? C23 C22 1.388(4) . ? C24 C25 1.371(5) . ? C120 C125 1.387(4) . ? C120 C121 1.389(4) . ? C120 C117 1.472(4) . ? N131 C136 1.341(4) . ? N131 C132 1.342(4) . ? C25 C20 1.380(5) . ? C13 C14 1.388(5) . ? C13 C12 1.395(5) . ? C13 C16 1.472(4) . ? C32 C33 1.391(5) . ? C125 C124 1.373(4) . ? C116 C117 1.122(4) . ? C116 C113 1.476(4) . ? C16 C17 1.122(4) . ? C35 C36 1.379(4) . ? C35 C34 1.381(5) . ? C20 C21 1.378(5) . ? C20 C17 1.473(5) . ? C27 C36 1.467(4) . ? C136 C135 1.384(5) . ? C21 C22 1.376(4) . ? C34 C33 1.358(5) . ? C113 C114 1.378(5) . ? C113 C112 1.387(5) . ? C11 C10 1.358(6) . ? C11 C12 1.377(5) . ? C10 C15 1.378(6) . ? C112 C111 1.390(5) . ? C135 C134 1.372(6) . ? C114 C115 1.385(5) . ? C132 C133 1.392(6) . ? C110 C111 1.367(6) . ? C110 C115 1.367(6) . ? C14 C15 1.390(6) . ? C134 C133 1.349(7) . ? 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 N102 Co1 N2 96.37(11) . . ? N102 Co1 N31 94.84(11) . . ? N2 Co1 N31 96.56(11) . . ? N102 Co1 N131 95.76(11) . . ? N2 Co1 N131 93.61(11) . . ? N31 Co1 N131 164.39(10) . . ? N102 Co1 N26 168.18(10) . . ? N2 Co1 N26 91.51(10) . . ? N31 Co1 N26 75.47(10) . . ? N131 Co1 N26 92.50(10) . . ? N102 Co1 N126 93.25(10) . . ? N2 Co1 N126 165.95(10) . . ? N31 Co1 N126 92.80(9) . . ? N131 Co1 N126 75.20(9) . . ? N26 Co1 N126 80.70(8) . . ? C32 N31 C36 116.9(3) . . ? C32 N31 Co1 127.3(3) . . ? C36 N31 Co1 115.2(2) . . ? N126 C127 C136 119.3(3) . . ? C127 N126 C123 118.8(3) . . ? C127 N126 Co1 113.7(2) . . ? C123 N126 Co1 126.78(18) . . ? C27 N26 C23 120.4(3) . . ? C27 N26 Co1 113.3(2) . . ? C23 N26 Co1 125.5(2) . . ? C3 N2 Co1 162.8(3) . . ? N102 C103 S104 179.2(3) . . ? C121 C122 C123 120.4(3) . . ? C122 C123 C124 119.3(3) . . ? C122 C123 N126 118.8(3) . . ? C124 C123 N126 121.8(3) . . ? C24 C23 C22 119.1(3) . . ? C24 C23 N26 122.3(3) . . ? C22 C23 N26 118.4(3) . . ? C25 C24 C23 120.2(3) . . ? C125 C120 C121 117.9(3) . . ? C125 C120 C117 122.2(3) . . ? C121 C120 C117 119.8(3) . . ? C136 N131 C132 117.3(3) . . ? C136 N131 Co1 115.78(19) . . ? C132 N131 Co1 126.6(3) . . ? C122 C121 C120 121.0(3) . . ? C24 C25 C20 121.5(3) . . ? C103 N102 Co1 169.2(3) . . ? C14 C13 C12 118.7(4) . . ? C14 C13 C16 120.5(4) . . ? C12 C13 C16 120.7(3) . . ? N31 C32 C33 123.1(4) . . ? C124 C125 C120 121.4(3) . . ? N2 C3 S4 179.2(3) . . ? C117 C116 C113 176.2(4) . . ? C17 C16 C13 179.1(4) . . ? C36 C35 C34 118.8(4) . . ? C21 C20 C25 118.0(3) . . ? C21 C20 C17 121.1(3) . . ? C25 C20 C17 120.9(3) . . ? N26 C27 C36 119.8(3) . . ? N131 C136 C135 123.2(3) . . ? N131 C136 C127 115.3(3) . . ? C135 C136 C127 121.4(4) . . ? C116 C117 C120 176.7(4) . . ? N31 C36 C35 122.9(3) . . ? N31 C36 C27 114.4(3) . . ? C35 C36 C27 122.6(3) . . ? C22 C21 C20 121.5(3) . . ? C21 C22 C23 119.8(3) . . ? C33 C34 C35 119.1(4) . . ? C114 C113 C112 118.8(3) . . ? C114 C113 C116 122.8(3) . . ? C112 C113 C116 118.4(3) . . ? C125 C124 C123 119.9(3) . . ? C34 C33 C32 119.1(4) . . ? C16 C17 C20 177.7(4) . . ? C10 C11 C12 121.0(5) . . ? C11 C10 C15 119.9(4) . . ? C11 C12 C13 120.2(4) . . ? C113 C112 C111 120.2(4) . . ? C134 C135 C136 118.2(5) . . ? C113 C114 C115 120.3(4) . . ? N131 C132 C133 122.0(5) . . ? C111 C110 C115 119.7(4) . . ? C13 C14 C15 120.0(4) . . ? C110 C115 C114 120.7(4) . . ? C110 C111 C112 120.3(4) . . ? C133 C134 C135 119.6(5) . . ? C10 C15 C14 120.2(4) . . ? C134 C133 C132 119.6(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.24 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.219 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.048 ############################################ # END ############################################ data__[Co(PM-PeA)2(NCS)2] #140K _database_code_CSD 181922 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H28 Co N6 S2' _chemical_formula_weight 751.76 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' '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 ? _symmetry_space_group_name_H-M ? 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 15.6741(7) _cell_length_b 14.3226(6) _cell_length_c 16.7829(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.3640(10) _cell_angle_gamma 90.00 _cell_volume 3761.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36473 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 30.37 _reflns_number_total 10487 _reflns_number_gt 7441 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0426P)^2^+2.1229P] 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_number_reflns 10487 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.294396(16) 0.707355(18) 0.048545(14) 0.02618(7) Uani 1 1 d . . . S4 S 0.44103(3) 0.92520(4) -0.11060(3) 0.03587(12) Uani 1 1 d . . . S104 S 0.19164(3) 0.49084(4) -0.15542(3) 0.03644(12) Uani 1 1 d . . . N31 N 0.17863(10) 0.78297(11) 0.06512(9) 0.0279(3) Uani 1 1 d . . . C127 C 0.34654(12) 0.57531(13) 0.17929(11) 0.0275(4) Uani 1 1 d . . . N126 N 0.27814(9) 0.61645(10) 0.15344(9) 0.0239(3) Uani 1 1 d . . . N26 N 0.32853(10) 0.80690(11) 0.14490(9) 0.0268(3) Uani 1 1 d . . . N2 N 0.34056(12) 0.79492(13) -0.03545(10) 0.0372(4) Uani 1 1 d . . . C103 C 0.21921(11) 0.56290(13) -0.08249(11) 0.0277(4) Uani 1 1 d . . . C122 C 0.12453(12) 0.60240(13) 0.16033(11) 0.0268(4) Uani 1 1 d . . . C123 C 0.20472(11) 0.61254(12) 0.19991(10) 0.0239(3) Uani 1 1 d . . . C23 C 0.41164(12) 0.81593(13) 0.18400(11) 0.0274(4) Uani 1 1 d . . . C24 C 0.42701(13) 0.79382(15) 0.26427(11) 0.0326(4) Uani 1 1 d . . . C120 C 0.05803(12) 0.60920(13) 0.28679(12) 0.0292(4) Uani 1 1 d . . . N131 N 0.41417(10) 0.63394(11) 0.06591(10) 0.0316(4) Uani 1 1 d . . . C121 C 0.05189(12) 0.60021(13) 0.20337(12) 0.0291(4) Uani 1 1 d . . . C25 C 0.50943(14) 0.79722(15) 0.29839(12) 0.0359(4) Uani 1 1 d . . . N102 N 0.23893(11) 0.61336(12) -0.03055(10) 0.0356(4) Uani 1 1 d . . . C13 C 0.81721(13) 0.85806(14) 0.35679(13) 0.0333(4) Uani 1 1 d . . . C32 C 0.10404(13) 0.77293(14) 0.02344(12) 0.0333(4) Uani 1 1 d . . . C125 C 0.13884(13) 0.62028(16) 0.32593(12) 0.0346(4) Uani 1 1 d . . . C3 C 0.38238(12) 0.84922(13) -0.06674(10) 0.0276(4) Uani 1 1 d . . . C116 C -0.08167(13) 0.60014(14) 0.36197(13) 0.0342(4) Uani 1 1 d . . . C16 C 0.72974(13) 0.84396(13) 0.31930(13) 0.0319(4) Uani 1 1 d . . . C35 C 0.10707(13) 0.87512(15) 0.16054(13) 0.0347(4) Uani 1 1 d . . . C20 C 0.57748(13) 0.82454(13) 0.25360(12) 0.0313(4) Uani 1 1 d . . . C27 C 0.26463(13) 0.84774(13) 0.17340(11) 0.0292(4) Uani 1 1 d . . . C136 C 0.42354(12) 0.58337(13) 0.13385(12) 0.0301(4) Uani 1 1 d . . . C117 C -0.02045(14) 0.60582(14) 0.33103(12) 0.0347(4) Uani 1 1 d . . . C36 C 0.17993(12) 0.83515(13) 0.13236(11) 0.0287(4) Uani 1 1 d . . . C21 C 0.56129(13) 0.84627(15) 0.17295(13) 0.0349(4) Uani 1 1 d . . . C22 C 0.47946(13) 0.84116(15) 0.13799(12) 0.0341(4) Uani 1 1 d . . . C34 C 0.02982(14) 0.86229(16) 0.11723(14) 0.0396(5) Uani 1 1 d . . . C113 C -0.16487(13) 0.58778(14) 0.39814(12) 0.0327(4) Uani 1 1 d . . . C124 C 0.21165(12) 0.62235(15) 0.28284(11) 0.0315(4) Uani 1 1 d . . . C33 C 0.02800(14) 0.81145(16) 0.04737(14) 0.0395(5) Uani 1 1 d . . . C17 C 0.66345(15) 0.83341(14) 0.29126(13) 0.0376(5) Uani 1 1 d . . . C11 C 0.91133(15) 0.90211(16) 0.46958(15) 0.0429(5) Uani 1 1 d . . . C10 C 0.98094(14) 0.89349(16) 0.42352(16) 0.0429(5) Uani 1 1 d . . . C12 C 0.82959(14) 0.88433(15) 0.43673(13) 0.0382(5) Uani 1 1 d . . . C112 C -0.23979(14) 0.60957(15) 0.35290(14) 0.0377(5) Uani 1 1 d . . . C135 C 0.50038(14) 0.54278(16) 0.16026(15) 0.0407(5) Uani 1 1 d . . . C114 C -0.17050(14) 0.55205(16) 0.47547(14) 0.0390(5) Uani 1 1 d . . . C132 C 0.48220(15) 0.64233(18) 0.02184(15) 0.0452(5) Uani 1 1 d . . . C110 C -0.32381(15) 0.56034(17) 0.46068(15) 0.0435(5) Uani 1 1 d . . . C14 C 0.88827(15) 0.84708(16) 0.31113(15) 0.0423(5) Uani 1 1 d . . . C115 C -0.24941(15) 0.53848(17) 0.50625(14) 0.0439(5) Uani 1 1 d . . . C111 C -0.31885(14) 0.59540(17) 0.38424(15) 0.0429(5) Uani 1 1 d . . . C134 C 0.57048(16) 0.5528(2) 0.11390(18) 0.0534(7) Uani 1 1 d . . . C15 C 0.96970(15) 0.86504(17) 0.34505(16) 0.0465(6) Uani 1 1 d . . . C133 C 0.56056(16) 0.6025(2) 0.04383(18) 0.0555(7) Uani 1 1 d . . . H111 H -0.2390(14) 0.6370(16) 0.3005(14) 0.040(6) Uiso 1 1 d . . . H421 H 0.1216(14) 0.5955(15) 0.1040(14) 0.035(6) Uiso 1 1 d . . . H321 H 0.1052(13) 0.7368(15) -0.0235(13) 0.028(5) Uiso 1 1 d . . . H201 H 0.4672(14) 0.8573(16) 0.0847(14) 0.041(6) Uiso 1 1 d . . . H361 H -0.0006(14) 0.5906(15) 0.1786(13) 0.030(6) Uiso 1 1 d . . . H211 H 0.6071(15) 0.8652(17) 0.1450(14) 0.043(6) Uiso 1 1 d . . . H171 H 0.2667(15) 0.6322(16) 0.3080(13) 0.039(6) Uiso 1 1 d . . . H101 H 0.5045(16) 0.5086(18) 0.2106(16) 0.051(7) Uiso 1 1 d . . . H351 H 0.5228(16) 0.7766(17) 0.3541(15) 0.049(7) Uiso 1 1 d . . . H252 H -0.0221(17) 0.8891(18) 0.1345(15) 0.053(7) Uiso 1 1 d . . . H251 H 0.2713(13) 0.8878(15) 0.2208(13) 0.032(6) Uiso 1 1 d . . . H311 H 0.1447(14) 0.6286(16) 0.3844(14) 0.040(6) Uiso 1 1 d . . . H481 H 0.3514(13) 0.5393(15) 0.2280(13) 0.030(5) Uiso 1 1 d . . . H102 H -0.3775(16) 0.5511(17) 0.4814(15) 0.047(7) Uiso 1 1 d . . . H161 H -0.0228(15) 0.8048(16) 0.0156(14) 0.041(6) Uiso 1 1 d . . . H41 H -0.3691(17) 0.6122(18) 0.3528(16) 0.055(8) Uiso 1 1 d . . . H81 H 0.4712(15) 0.6800(17) -0.0279(15) 0.043(6) Uiso 1 1 d . . . H131 H 0.1135(14) 0.9112(16) 0.2102(14) 0.040(6) Uiso 1 1 d . . . H91 H -0.1176(16) 0.5354(17) 0.5081(14) 0.045(7) Uiso 1 1 d . . . H132 H 1.0401(16) 0.9080(17) 0.4464(15) 0.051(7) Uiso 1 1 d . . . H391 H 0.3812(16) 0.7759(16) 0.2917(14) 0.043(6) Uiso 1 1 d . . . H71 H 0.7796(15) 0.8877(16) 0.4690(14) 0.043(6) Uiso 1 1 d . . . H21 H 1.0195(19) 0.858(2) 0.3110(18) 0.071(9) Uiso 1 1 d . . . H92 H 0.8791(15) 0.8250(18) 0.2540(15) 0.050(7) Uiso 1 1 d . . . H31 H 0.6218(19) 0.526(2) 0.1310(17) 0.066(9) Uiso 1 1 d . . . H141 H 0.9188(17) 0.9198(19) 0.5263(17) 0.063(8) Uiso 1 1 d . . . H11 H 0.607(2) 0.612(2) 0.0075(19) 0.080(10) Uiso 1 1 d . . . H51 H -0.2531(16) 0.5131(18) 0.5592(16) 0.056(8) 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 0.02682(13) 0.02943(13) 0.02247(12) -0.00041(10) 0.00287(9) -0.00448(10) S4 0.0321(3) 0.0395(3) 0.0368(3) 0.0006(2) 0.0081(2) -0.0084(2) S104 0.0351(3) 0.0434(3) 0.0303(2) -0.0103(2) -0.0025(2) 0.0002(2) N31 0.0289(8) 0.0274(8) 0.0270(8) 0.0025(6) -0.0019(6) -0.0035(6) C127 0.0278(9) 0.0270(9) 0.0277(9) -0.0014(7) 0.0020(7) 0.0000(7) N126 0.0228(7) 0.0243(7) 0.0247(7) -0.0028(6) 0.0034(6) -0.0035(6) N26 0.0272(8) 0.0266(8) 0.0265(7) 0.0024(6) -0.0007(6) -0.0065(6) N2 0.0424(10) 0.0422(10) 0.0272(8) 0.0027(7) 0.0030(7) -0.0077(8) C103 0.0225(9) 0.0343(10) 0.0262(9) 0.0013(8) 0.0019(7) 0.0021(7) C122 0.0267(9) 0.0273(9) 0.0262(9) 0.0003(7) 0.0003(7) -0.0038(7) C123 0.0227(8) 0.0238(8) 0.0253(8) 0.0014(7) 0.0032(7) -0.0019(7) C23 0.0291(9) 0.0249(9) 0.0280(9) -0.0014(7) -0.0008(7) -0.0049(7) C24 0.0323(10) 0.0381(10) 0.0273(9) 0.0009(8) 0.0018(8) -0.0083(9) C120 0.0269(9) 0.0282(9) 0.0333(10) 0.0019(8) 0.0087(8) -0.0010(7) N131 0.0294(8) 0.0338(9) 0.0326(8) -0.0030(7) 0.0092(7) -0.0037(7) C121 0.0232(9) 0.0292(9) 0.0345(10) 0.0008(8) -0.0001(8) -0.0051(7) C25 0.0363(11) 0.0428(11) 0.0279(9) 0.0011(9) -0.0033(8) -0.0054(9) N102 0.0365(9) 0.0398(9) 0.0304(8) -0.0036(7) 0.0014(7) -0.0046(8) C13 0.0286(10) 0.0283(10) 0.0424(11) -0.0002(8) -0.0036(8) -0.0018(8) C32 0.0351(11) 0.0330(10) 0.0311(10) 0.0011(8) -0.0045(8) -0.0027(8) C125 0.0310(10) 0.0489(12) 0.0242(9) 0.0011(9) 0.0044(8) 0.0010(9) C3 0.0270(9) 0.0334(10) 0.0224(8) -0.0023(7) 0.0002(7) 0.0004(8) C116 0.0350(11) 0.0298(10) 0.0374(11) -0.0065(8) -0.0010(9) 0.0072(8) C16 0.0329(11) 0.0199(8) 0.0429(11) 0.0008(8) 0.0019(9) -0.0025(7) C35 0.0344(11) 0.0335(10) 0.0362(11) -0.0001(9) 0.0025(8) 0.0024(8) C20 0.0306(10) 0.0270(9) 0.0358(10) -0.0021(8) -0.0037(8) -0.0044(8) C27 0.0347(10) 0.0260(9) 0.0268(9) -0.0004(7) 0.0003(8) -0.0036(8) C136 0.0276(9) 0.0291(9) 0.0338(10) -0.0064(8) 0.0043(8) 0.0005(7) C117 0.0429(12) 0.0277(10) 0.0334(10) 0.0035(8) 0.0024(9) -0.0087(8) C36 0.0310(10) 0.0260(9) 0.0290(9) 0.0026(7) 0.0013(7) -0.0018(7) C21 0.0287(10) 0.0388(11) 0.0371(11) 0.0051(9) 0.0015(8) -0.0065(8) C22 0.0327(10) 0.0395(11) 0.0299(10) 0.0061(9) -0.0003(8) -0.0064(8) C34 0.0300(11) 0.0410(12) 0.0478(13) 0.0008(10) 0.0026(9) 0.0055(9) C113 0.0316(10) 0.0298(9) 0.0378(10) -0.0013(8) 0.0107(8) -0.0023(8) C124 0.0241(9) 0.0443(11) 0.0260(9) -0.0007(8) -0.0002(7) -0.0004(8) C33 0.0316(11) 0.0400(12) 0.0458(12) 0.0053(9) -0.0091(9) -0.0004(9) C17 0.0448(13) 0.0286(10) 0.0393(11) 0.0016(8) 0.0011(10) -0.0002(9) C11 0.0415(13) 0.0449(12) 0.0413(12) -0.0003(10) -0.0074(10) -0.0004(10) C10 0.0296(11) 0.0366(11) 0.0610(15) 0.0064(10) -0.0100(10) -0.0004(9) C12 0.0333(11) 0.0408(11) 0.0402(11) -0.0004(9) -0.0002(9) -0.0012(9) C112 0.0377(11) 0.0370(11) 0.0395(11) 0.0051(9) 0.0110(9) 0.0031(9) C135 0.0298(11) 0.0427(12) 0.0495(13) -0.0018(10) 0.0010(9) 0.0070(9) C114 0.0321(11) 0.0452(12) 0.0400(12) 0.0029(9) 0.0063(9) -0.0028(9) C132 0.0395(12) 0.0504(13) 0.0475(13) -0.0008(11) 0.0195(10) -0.0003(10) C110 0.0310(11) 0.0490(13) 0.0523(14) 0.0057(11) 0.0161(10) -0.0013(10) C14 0.0418(13) 0.0417(12) 0.0433(12) -0.0044(10) 0.0021(10) -0.0035(10) C115 0.0396(12) 0.0521(14) 0.0411(12) 0.0070(11) 0.0115(10) -0.0043(10) C111 0.0285(11) 0.0482(13) 0.0523(14) 0.0071(11) 0.0057(10) 0.0038(9) C134 0.0286(12) 0.0605(16) 0.0717(18) -0.0060(14) 0.0084(12) 0.0095(11) C15 0.0339(12) 0.0441(13) 0.0621(15) -0.0004(11) 0.0091(11) 0.0006(10) C133 0.0355(13) 0.0636(16) 0.0700(18) -0.0072(14) 0.0251(12) -0.0006(11) _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 N102 2.0482(17) . ? Co1 N2 2.0502(17) . ? Co1 N31 2.1453(16) . ? Co1 N131 2.1566(17) . ? Co1 N26 2.1983(15) . ? Co1 N126 2.2163(15) . ? S4 C3 1.6280(19) . ? S104 C103 1.640(2) . ? N31 C32 1.334(3) . ? N31 C36 1.353(2) . ? C127 N126 1.277(2) . ? C127 C136 1.470(3) . ? N126 C123 1.429(2) . ? N26 C27 1.277(2) . ? N26 C23 1.430(2) . ? N2 C3 1.162(2) . ? C103 N102 1.160(2) . ? C122 C121 1.384(3) . ? C122 C123 1.394(3) . ? C123 C124 1.397(3) . ? C23 C24 1.391(3) . ? C23 C22 1.398(3) . ? C24 C25 1.383(3) . ? C120 C125 1.401(3) . ? C120 C121 1.404(3) . ? C120 C117 1.474(3) . ? N131 C132 1.338(3) . ? N131 C136 1.352(3) . ? C25 C20 1.396(3) . ? C13 C12 1.396(3) . ? C13 C14 1.397(3) . ? C13 C16 1.488(3) . ? C32 C33 1.394(3) . ? C125 C124 1.387(3) . ? C116 C117 1.121(3) . ? C116 C113 1.481(3) . ? C16 C17 1.125(3) . ? C35 C36 1.385(3) . ? C35 C34 1.387(3) . ? C20 C21 1.398(3) . ? C20 C17 1.460(3) . ? C27 C36 1.470(3) . ? C136 C135 1.387(3) . ? C21 C22 1.381(3) . ? C34 C33 1.379(3) . ? C113 C112 1.396(3) . ? C113 C114 1.403(3) . ? C11 C10 1.379(3) . ? C11 C12 1.388(3) . ? C10 C15 1.380(4) . ? C112 C111 1.389(3) . ? C135 C134 1.390(3) . ? C114 C115 1.382(3) . ? C132 C133 1.384(4) . ? C110 C111 1.384(3) . ? C110 C115 1.392(3) . ? C14 C15 1.391(3) . ? C134 C133 1.376(4) . ? 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 N102 Co1 N2 96.31(7) . . ? N102 Co1 N31 94.92(7) . . ? N2 Co1 N31 96.64(7) . . ? N102 Co1 N131 95.75(7) . . ? N2 Co1 N131 92.96(7) . . ? N31 Co1 N131 164.77(6) . . ? N102 Co1 N26 168.18(6) . . ? N2 Co1 N26 91.64(6) . . ? N31 Co1 N26 75.43(6) . . ? N131 Co1 N26 92.55(6) . . ? N102 Co1 N126 93.70(6) . . ? N2 Co1 N126 165.28(6) . . ? N31 Co1 N126 93.21(6) . . ? N131 Co1 N126 75.28(6) . . ? N26 Co1 N126 80.28(5) . . ? C32 N31 C36 117.82(17) . . ? C32 N31 Co1 126.82(14) . . ? C36 N31 Co1 114.56(12) . . ? N126 C127 C136 119.09(17) . . ? C127 N126 C123 118.92(15) . . ? C127 N126 Co1 114.06(12) . . ? C123 N126 Co1 126.19(11) . . ? C27 N26 C23 120.02(16) . . ? C27 N26 Co1 114.22(13) . . ? C23 N26 Co1 124.90(12) . . ? C3 N2 Co1 162.03(16) . . ? N102 C103 S104 179.5(2) . . ? C121 C122 C123 119.99(17) . . ? C122 C123 C124 120.03(16) . . ? C122 C123 N126 118.45(15) . . ? C124 C123 N126 121.47(16) . . ? C24 C23 C22 119.99(18) . . ? C24 C23 N26 121.68(17) . . ? C22 C23 N26 118.16(17) . . ? C25 C24 C23 119.84(18) . . ? C125 C120 C121 119.02(17) . . ? C125 C120 C117 121.71(18) . . ? C121 C120 C117 119.26(18) . . ? C132 N131 C136 117.63(19) . . ? C132 N131 Co1 126.66(16) . . ? C136 N131 Co1 115.20(12) . . ? C122 C121 C120 120.54(18) . . ? C24 C25 C20 120.75(19) . . ? C103 N102 Co1 168.70(16) . . ? C12 C13 C14 119.14(19) . . ? C12 C13 C16 121.04(19) . . ? C14 C13 C16 119.80(19) . . ? N31 C32 C33 123.0(2) . . ? C124 C125 C120 120.46(18) . . ? N2 C3 S4 179.9(2) . . ? C117 C116 C113 175.8(2) . . ? C17 C16 C13 179.7(3) . . ? C36 C35 C34 118.6(2) . . ? C25 C20 C21 118.87(18) . . ? C25 C20 C17 120.40(18) . . ? C21 C20 C17 120.69(18) . . ? N26 C27 C36 118.35(17) . . ? N131 C136 C135 122.93(19) . . ? N131 C136 C127 115.35(17) . . ? C135 C136 C127 121.71(19) . . ? C116 C117 C120 176.6(2) . . ? N31 C36 C35 122.73(18) . . ? N31 C36 C27 115.32(17) . . ? C35 C36 C27 121.95(18) . . ? C22 C21 C20 120.73(19) . . ? C21 C22 C23 119.78(19) . . ? C33 C34 C35 119.3(2) . . ? C112 C113 C114 119.23(19) . . ? C112 C113 C116 118.90(18) . . ? C114 C113 C116 121.84(19) . . ? C125 C124 C123 119.95(18) . . ? C34 C33 C32 118.6(2) . . ? C16 C17 C20 177.2(2) . . ? C10 C11 C12 120.2(2) . . ? C11 C10 C15 120.0(2) . . ? C11 C12 C13 120.3(2) . . ? C111 C112 C113 120.1(2) . . ? C136 C135 C134 118.6(2) . . ? C115 C114 C113 120.2(2) . . ? N131 C132 C133 122.6(2) . . ? C111 C110 C115 120.0(2) . . ? C15 C14 C13 119.8(2) . . ? C114 C115 C110 120.2(2) . . ? C110 C111 C112 120.3(2) . . ? C133 C134 C135 118.6(2) . . ? C10 C15 C14 120.5(2) . . ? C134 C133 C132 119.7(2) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 30.37 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.794 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.057