# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Michael Bruce' _publ_contact_author_email MICHAEL.BRUCE@ADELAIDE.EDU.AU _publ_section_title ; Syntheses and molecular structures of some tricobalt carbonyl clusters containing 2,4,6-trimethyl-1,3,5-trithiane ; loop_ _publ_author_name 'M Bruce' 'Mark Fox' 'Paul Low' 'Brian W Skelton' 'Allan H White' 'Natasha N. Zaitseva' #===END data_br1141 _database_code_depnum_ccdc_archive 'CCDC 667572' _audit_creation_date 2007-11-12T14:04:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C16 H18 Co3 N O7 S3' _chemical_formula_moiety 'C16 H18 Co3 N O7 S3' _chemical_formula_weight 609.28 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_c_1 _symmetry_space_group_name_Hall c_-2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.696(2) _cell_length_b 9.7690(10) _cell_length_c 15.877(2) _cell_angle_alpha 90 _cell_angle_beta 108.114(2) _cell_angle_gamma 90 _cell_volume 2166.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 6147 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 32.6 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.598 _exptl_crystal_description prism _exptl_crystal_size_max .35 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .14 _exptl_crystal_size_rad ? _exptl_crystal_colour dark_red _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .77 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents .035 _diffrn_reflns_av_unetI/netI 0.057 _diffrn_reflns_number 7401 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 33.56 _diffrn_reflns_theta_full 33. _diffrn_measured_fraction_theta_full 0.97 _diffrn_measured_fraction_theta_max 0.948 _reflns_number_total 7401 _reflns_number_gt 6460 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0592P)^2^+10.1745P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7401 _refine_ls_number_parameters 276 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1234 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.042(17) _refine_diff_density_max 1.558 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.152 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.49994(4) 0.64308(6) 0.50000(4) 0.01635(13) Uani 1 1 d . . . Co2 Co 0.61718(4) 0.76234(6) 0.44497(4) 0.01580(13) Uani 1 1 d . . . Co3 Co 0.54064(4) 0.55412(7) 0.37015(4) 0.01595(12) Uani 1 1 d . . . C11 C 0.5344(4) 0.7211(6) 0.6080(3) 0.0234(10) Uani 1 1 d . . . O11 O 0.5598(4) 0.7669(5) 0.6765(3) 0.0376(10) Uani 1 1 d . . . C12 C 0.4424(4) 0.4944(6) 0.5234(3) 0.0238(10) Uani 1 1 d . . . O12 O 0.4085(3) 0.3948(5) 0.5389(3) 0.0370(10) Uani 1 1 d . . . C21 C 0.7135(4) 0.7558(5) 0.4002(3) 0.0206(9) Uani 1 1 d . . . O21 O 0.7769(3) 0.7420(4) 0.3740(4) 0.0357(10) Uani 1 1 d . . . C22 C 0.6755(4) 0.8673(5) 0.5384(4) 0.0238(10) Uani 1 1 d . . . O22 O 0.7138(4) 0.9359(5) 0.5964(3) 0.0391(10) Uani 1 1 d . . . C31 C 0.4858(4) 0.3894(6) 0.3524(3) 0.0213(9) Uani 1 1 d . . . O31 O 0.4539(3) 0.2809(4) 0.3350(3) 0.0333(9) Uani 1 1 d . . . C32 C 0.6224(4) 0.5159(6) 0.3110(3) 0.0235(9) Uani 1 1 d . . . O32 O 0.6766(3) 0.4861(5) 0.2756(3) 0.0386(10) Uani 1 1 d . . . S1 S 0.37062(8) 0.77125(13) 0.42353(8) 0.0191(2) Uani 1 1 d . . . C1 C 0.4146(3) 0.9368(5) 0.3994(3) 0.0196(9) Uani 1 1 d . . . H1 H 0.3619 0.9838 0.3529 0.023 Uiso 1 1 calc R . . C101 C 0.4412(4) 1.0236(6) 0.4829(4) 0.0278(10) Uani 1 1 d . . . H10A H 0.4942 0.9802 0.5286 0.042 Uiso 1 1 calc R . . H10B H 0.3857 1.0316 0.5044 0.042 Uiso 1 1 calc R . . H10C H 0.4608 1.1149 0.4697 0.042 Uiso 1 1 calc R . . S2 S 0.51703(8) 0.92026(12) 0.35903(8) 0.0185(2) Uani 1 1 d . . . C2 C 0.4601(3) 0.8374(5) 0.2530(3) 0.0196(9) Uani 1 1 d . . . H2 H 0.4028 0.8924 0.2198 0.024 Uiso 1 1 calc R . . C201 C 0.5303(4) 0.8357(6) 0.1997(3) 0.0253(10) Uani 1 1 d . . . H20A H 0.5865 0.7807 0.231 0.038 Uiso 1 1 calc R . . H20B H 0.5505 0.9295 0.1927 0.038 Uiso 1 1 calc R . . H20C H 0.4992 0.7957 0.1412 0.038 Uiso 1 1 calc R . . S3 S 0.42168(8) 0.66366(12) 0.26491(7) 0.0183(2) Uani 1 1 d . . . C3 C 0.3256(3) 0.7020(6) 0.3116(3) 0.0210(9) Uani 1 1 d . . . H3 H 0.2815 0.7706 0.2728 0.025 Uiso 1 1 calc R . . C301 C 0.2687(4) 0.5713(6) 0.3147(4) 0.0292(11) Uani 1 1 d . . . H30A H 0.3084 0.509 0.3596 0.044 Uiso 1 1 calc R . . H30B H 0.2505 0.5265 0.2566 0.044 Uiso 1 1 calc R . . H30C H 0.211 0.595 0.3299 0.044 Uiso 1 1 calc R . . C10 C 0.6182(4) 0.5822(5) 0.4901(3) 0.0180(8) Uani 1 1 d . . . C20 C 0.7022(3) 0.5234(5) 0.5597(3) 0.0200(9) Uani 1 1 d . . . O20 O 0.7617(3) 0.6039(4) 0.6094(3) 0.0335(10) Uani 1 1 d . . . N30 N 0.7155(3) 0.3871(5) 0.5717(3) 0.0256(9) Uani 1 1 d . . . C40 C 0.6487(5) 0.2843(6) 0.5254(4) 0.0345(13) Uani 1 1 d . . . H40A H 0.584 0.3229 0.5059 0.052 Uiso 1 1 calc R . . H40B H 0.6508 0.2066 0.565 0.052 Uiso 1 1 calc R . . H40C H 0.6659 0.2531 0.4736 0.052 Uiso 1 1 calc R . . C50 C 0.7998(4) 0.3381(6) 0.6406(4) 0.0320(12) Uani 1 1 d . . . H50A H 0.855 0.3952 0.6418 0.048 Uiso 1 1 calc R . . H50B H 0.8126 0.243 0.6282 0.048 Uiso 1 1 calc R . . H50C H 0.7885 0.3432 0.6982 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0156(3) 0.0183(3) 0.0139(3) 0.0016(2) 0.0027(2) 0.0000(2) Co2 0.0142(3) 0.0163(3) 0.0149(3) 0.0011(2) 0.0016(2) -0.0011(2) Co3 0.0150(3) 0.0162(3) 0.0151(3) -0.0004(2) 0.0025(2) -0.0002(2) C11 0.022(2) 0.031(3) 0.016(2) 0.0032(18) 0.0055(17) 0.002(2) O11 0.048(3) 0.042(3) 0.0200(19) -0.0032(17) 0.0070(18) 0.000(2) C12 0.023(2) 0.024(2) 0.025(2) 0.0041(18) 0.0081(18) 0.0017(18) O12 0.037(2) 0.034(2) 0.039(2) 0.0106(18) 0.0092(19) -0.0107(18) C21 0.0162(19) 0.019(2) 0.024(2) 0.0015(16) 0.0023(17) -0.0027(16) O21 0.027(2) 0.034(2) 0.052(3) -0.0017(19) 0.0199(19) -0.0057(17) C22 0.024(2) 0.022(2) 0.023(2) 0.0014(18) 0.0031(18) 0.0034(18) O22 0.041(2) 0.038(2) 0.029(2) -0.0115(18) -0.0019(18) -0.0038(19) C31 0.020(2) 0.028(2) 0.0129(19) 0.0028(17) 0.0014(16) 0.0008(18) O31 0.032(2) 0.0238(19) 0.044(3) -0.0046(17) 0.0122(18) -0.0110(16) C32 0.020(2) 0.024(2) 0.024(2) -0.0013(18) 0.0030(18) -0.0009(18) O32 0.033(2) 0.036(2) 0.054(3) -0.013(2) 0.025(2) -0.0026(18) S1 0.0169(5) 0.0215(5) 0.0181(5) 0.0012(4) 0.0043(4) 0.0018(4) C1 0.0137(19) 0.021(2) 0.020(2) 0.0008(16) 0.0003(16) 0.0052(16) C101 0.032(3) 0.023(2) 0.029(3) -0.002(2) 0.010(2) 0.002(2) S2 0.0190(5) 0.0170(5) 0.0174(5) 0.0025(4) 0.0024(4) 0.0000(4) C2 0.0148(19) 0.021(2) 0.018(2) 0.0057(16) -0.0017(15) -0.0020(16) C201 0.028(2) 0.033(3) 0.015(2) 0.0002(18) 0.0072(18) -0.005(2) S3 0.0179(5) 0.0202(5) 0.0138(5) 0.0003(4) 0.0004(4) -0.0006(4) C3 0.0134(19) 0.026(2) 0.020(2) 0.0039(18) -0.0003(16) -0.0007(17) C301 0.024(2) 0.029(3) 0.034(3) 0.002(2) 0.008(2) -0.011(2) C10 0.022(2) 0.0148(19) 0.018(2) 0.0022(15) 0.0076(16) 0.0012(16) C20 0.0143(19) 0.024(2) 0.019(2) 0.0022(17) 0.0020(16) 0.0018(17) O20 0.030(2) 0.0236(19) 0.036(2) 0.0004(16) -0.0045(18) -0.0029(16) N30 0.0202(19) 0.021(2) 0.031(2) 0.0044(17) 0.0010(17) 0.0034(16) C40 0.030(3) 0.024(3) 0.039(3) 0.000(2) -0.005(2) -0.001(2) C50 0.033(3) 0.029(3) 0.024(3) 0.005(2) -0.006(2) 0.008(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C12 1.777(6) . ? Co1 C11 1.799(5) . ? Co1 C10 1.889(5) . ? Co1 S1 2.2845(13) . ? Co1 Co2 2.4547(9) . ? Co1 Co3 2.4760(9) . ? Co2 C21 1.771(5) . ? Co2 C22 1.787(5) . ? Co2 C10 1.898(5) . ? Co2 S2 2.2714(13) . ? Co2 Co3 2.4461(9) . ? Co3 C32 1.780(5) . ? Co3 C31 1.782(5) . ? Co3 C10 1.911(5) . ? Co3 S3 2.2753(13) . ? C11 O11 1.127(7) . ? C12 O12 1.154(7) . ? C21 O21 1.141(7) . ? C22 O22 1.137(7) . ? C31 O31 1.158(7) . ? C32 O32 1.145(7) . ? S1 C3 1.823(5) . ? S1 C1 1.826(5) . ? C1 C101 1.520(7) . ? C1 S2 1.817(5) . ? S2 C2 1.820(5) . ? C2 C201 1.525(7) . ? C2 S3 1.817(5) . ? S3 C3 1.826(5) . ? C3 C301 1.536(7) . ? C10 C20 1.493(7) . ? C20 O20 1.255(6) . ? C20 N30 1.350(7) . ? N30 C40 1.437(8) . ? N30 C50 1.455(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 C12 Co1 C11 99.1(2) . . ? C12 Co1 C10 105.7(2) . . ? C11 Co1 C10 102.7(2) . . ? C12 Co1 S1 100.82(17) . . ? C11 Co1 S1 102.43(18) . . ? C10 Co1 S1 139.73(14) . . ? C12 Co1 Co2 153.47(18) . . ? C11 Co1 Co2 96.75(17) . . ? C10 Co1 Co2 49.76(14) . . ? S1 Co1 Co2 96.35(4) . . ? C12 Co1 Co3 98.12(18) . . ? C11 Co1 Co3 150.82(17) . . ? C10 Co1 Co3 49.71(15) . . ? S1 Co1 Co3 97.25(4) . . ? Co2 Co1 Co3 59.48(3) . . ? C21 Co2 C22 96.7(2) . . ? C21 Co2 C10 101.8(2) . . ? C22 Co2 C10 105.9(2) . . ? C21 Co2 S2 103.47(17) . . ? C22 Co2 S2 99.36(17) . . ? C10 Co2 S2 141.62(16) . . ? C21 Co2 Co3 94.55(16) . . ? C22 Co2 Co3 155.44(18) . . ? C10 Co2 Co3 50.27(15) . . ? S2 Co2 Co3 99.14(4) . . ? C21 Co2 Co1 149.60(16) . . ? C22 Co2 Co1 100.68(18) . . ? C10 Co2 Co1 49.45(15) . . ? S2 Co2 Co1 98.09(4) . . ? Co3 Co2 Co1 60.69(3) . . ? C32 Co3 C31 94.2(2) . . ? C32 Co3 C10 105.3(2) . . ? C31 Co3 C10 112.8(2) . . ? C32 Co3 S3 101.63(17) . . ? C31 Co3 S3 95.87(16) . . ? C10 Co3 S3 138.46(15) . . ? C32 Co3 Co2 98.43(17) . . ? C31 Co3 Co2 160.82(16) . . ? C10 Co3 Co2 49.82(14) . . ? S3 Co3 Co2 95.62(4) . . ? C32 Co3 Co1 152.95(17) . . ? C31 Co3 Co1 103.53(16) . . ? C10 Co3 Co1 48.97(14) . . ? S3 Co3 Co1 96.72(4) . . ? Co2 Co3 Co1 59.83(3) . . ? O11 C11 Co1 176.8(5) . . ? O12 C12 Co1 177.1(5) . . ? O21 C21 Co2 174.9(5) . . ? O22 C22 Co2 178.1(6) . . ? O31 C31 Co3 173.9(5) . . ? O32 C32 Co3 176.6(5) . . ? C3 S1 C1 99.7(2) . . ? C3 S1 Co1 107.73(17) . . ? C1 S1 Co1 107.84(16) . . ? C101 C1 S2 110.0(4) . . ? C101 C1 S1 108.8(4) . . ? S2 C1 S1 112.4(3) . . ? C1 S2 C2 99.9(2) . . ? C1 S2 Co2 107.55(16) . . ? C2 S2 Co2 106.21(16) . . ? C201 C2 S3 109.5(4) . . ? C201 C2 S2 108.8(3) . . ? S3 C2 S2 112.8(3) . . ? C2 S3 C3 98.9(2) . . ? C2 S3 Co3 108.83(15) . . ? C3 S3 Co3 108.24(16) . . ? C301 C3 S1 108.2(4) . . ? C301 C3 S3 109.9(4) . . ? S1 C3 S3 112.3(2) . . ? C20 C10 Co1 129.1(3) . . ? C20 C10 Co2 122.9(4) . . ? Co1 C10 Co2 80.79(19) . . ? C20 C10 Co3 141.5(4) . . ? Co1 C10 Co3 81.32(19) . . ? Co2 C10 Co3 79.91(18) . . ? O20 C20 N30 119.1(4) . . ? O20 C20 C10 118.6(5) . . ? N30 C20 C10 122.3(4) . . ? C20 N30 C40 124.9(4) . . ? C20 N30 C50 118.8(5) . . ? C40 N30 C50 116.2(5) . . ? #===END # Attachment 'Compound1_2_3_4_8.cif' data_br1162 _database_code_depnum_ccdc_archive 'CCDC 667573' _audit_creation_date 2009-05-16T18:56:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C13 H13 Co3 O6 S3' _chemical_formula_moiety 'C13 H13 Co3 O6 S3' _chemical_formula_weight 538.2 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_n_m_a _symmetry_space_group_name_Hall -p_2ac_2n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 14.181(2) _cell_length_b 14.934(2) _cell_length_c 9.1039(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1928.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7307 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 28.55 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.854 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_size_max .35 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .18 _exptl_crystal_size_rad ? _exptl_crystal_colour dark_red _exptl_crystal_F_000 1072 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .375 _exptl_absorpt_correction_T_max .593 _exptl_absorpt_coefficient_mu 2.9 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_unetI/netI 0.0128 _diffrn_reflns_av_R_equivalents .021 _diffrn_reflns_number 17303 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 28.76 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.96 _reflns_number_total 2498 _reflns_number_gt 2178 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_molecular_graphics OrtepII _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0339P)^2^+0.6672P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2498 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0673 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.306 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.846246(18) 0.332988(17) 0.01739(3) 0.03883(9) Uani 1 1 d . . . Co2 Co 0.81662(3) 0.25 -0.21275(4) 0.04439(11) Uani 1 2 d S . . S1 S 0.69323(4) 0.35184(3) 0.08391(6) 0.04468(13) Uani 1 1 d . . . S2 S 0.65687(5) 0.25 -0.19819(8) 0.04754(17) Uani 1 2 d S . . C11 C 0.90798(15) 0.34802(13) 0.1846(2) 0.0465(4) Uani 1 1 d . . . O11 O 0.95275(13) 0.35741(12) 0.28760(19) 0.0709(5) Uani 1 1 d . . . C12 C 0.87510(18) 0.43974(16) -0.0576(3) 0.0611(6) Uani 1 1 d . . . O12 O 0.89866(18) 0.50751(14) -0.1019(3) 0.1034(8) Uani 1 1 d . . . C21 C 0.8392(2) 0.33983(19) -0.3346(3) 0.0694(7) Uani 1 1 d . . . O21 O 0.8583(2) 0.39617(17) -0.4129(2) 0.1197(9) Uani 1 1 d . . . C10 C 0.9206(2) 0.25 -0.0846(3) 0.0478(6) Uani 1 2 d S . . H10 H 0.9884 0.25 -0.1055 0.057 Uiso 1 2 calc SR . . C1 C 0.6553(2) 0.25 0.1766(3) 0.0478(6) Uani 1 2 d S . . H1 H 0.5862 0.25 0.1791 0.057 Uiso 1 2 calc SR . . C2 C 0.62093(16) 0.34281(14) -0.0813(2) 0.0518(5) Uani 1 1 d . . . H2 H 0.5554 0.3328 -0.0511 0.062 Uiso 1 1 calc R . . C3 C 0.6909(3) 0.25 0.3354(4) 0.0664(9) Uani 1 2 d S . . H3A H 0.7564 0.234 0.337 0.1 Uiso 0.5 1 calc PR . . H3B H 0.6554 0.2074 0.3918 0.1 Uiso 0.5 1 calc PR . . H3C H 0.683 0.3086 0.3768 0.1 Uiso 0.5 1 calc PR . . C4 C 0.6251(2) 0.42981(17) -0.1677(3) 0.0742(7) Uani 1 1 d . . . H4A H 0.6891 0.4418 -0.1956 0.111 Uiso 1 1 calc R . . H4B H 0.6019 0.478 -0.1079 0.111 Uiso 1 1 calc R . . H4C H 0.5868 0.4246 -0.2543 0.111 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.03992(15) 0.03776(15) 0.03882(15) 0.00064(10) -0.00118(10) -0.00480(10) Co2 0.0506(2) 0.0510(2) 0.03164(19) 0 0.00304(15) 0 S1 0.0456(3) 0.0416(2) 0.0468(3) -0.0051(2) 0.0011(2) 0.0061(2) S2 0.0497(4) 0.0481(4) 0.0449(4) 0 -0.0134(3) 0 C11 0.0494(11) 0.0392(10) 0.0508(11) -0.0040(8) -0.0042(9) 0.0038(8) O11 0.0793(12) 0.0672(10) 0.0661(11) -0.0158(8) -0.0312(9) 0.0125(9) C12 0.0689(14) 0.0549(13) 0.0596(13) 0.0109(11) -0.0091(12) -0.0141(11) O12 0.1292(19) 0.0702(13) 0.1109(17) 0.0355(12) -0.0188(15) -0.0400(13) C21 0.091(2) 0.0740(17) 0.0430(12) 0.0089(12) 0.0073(12) -0.0067(14) O21 0.187(3) 0.1016(17) 0.0706(14) 0.0323(14) 0.0263(15) -0.0272(17) C10 0.0424(15) 0.0579(17) 0.0429(15) 0 0.0072(12) 0 C1 0.0411(14) 0.0541(16) 0.0481(16) 0 0.0099(12) 0 C2 0.0470(11) 0.0506(12) 0.0578(13) 0.0007(10) -0.0101(10) 0.0105(9) C3 0.082(2) 0.075(2) 0.0423(17) 0 0.0121(16) 0 C4 0.0929(19) 0.0533(13) 0.0766(17) 0.0081(12) -0.0228(15) 0.0188(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C11 1.770(2) . ? Co1 C12 1.782(2) . ? Co1 C10 1.873(2) . ? Co1 S1 2.2704(6) . ? Co1 Co2 2.4703(4) . ? Co1 Co1 2.4787(6) 8_565 ? Co2 C21 1.770(3) 8_565 ? Co2 C21 1.770(3) . ? Co2 C10 1.880(3) . ? Co2 S2 2.2693(9) . ? Co2 Co1 2.4703(4) 8_565 ? S1 C1 1.8203(17) . ? S1 C2 1.825(2) . ? S2 C2 1.820(2) . ? S2 C2 1.820(2) 8_565 ? C11 O11 1.141(2) . ? C12 O12 1.140(3) . ? C21 O21 1.135(3) . ? C10 Co1 1.873(2) 8_565 ? C10 H10 0.98 . ? C1 C3 1.531(5) . ? C1 S1 1.8203(17) 8_565 ? C1 H1 0.98 . ? C2 C4 1.520(3) . ? C2 H2 0.98 . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? 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 C11 Co1 C12 95.88(10) . . ? C11 Co1 C10 103.39(11) . . ? C12 Co1 C10 105.83(11) . . ? C11 Co1 S1 103.16(7) . . ? C12 Co1 S1 102.16(9) . . ? C10 Co1 S1 138.78(8) . . ? C11 Co1 Co2 151.28(6) . . ? C12 Co1 Co2 99.37(8) . . ? C10 Co1 Co2 48.97(9) . . ? S1 Co1 Co2 97.234(18) . . ? C11 Co1 Co1 97.29(6) . 8_565 ? C12 Co1 Co1 153.46(9) . 8_565 ? C10 Co1 Co1 48.58(6) . 8_565 ? S1 Co1 Co1 97.125(14) . 8_565 ? Co2 Co1 Co1 59.888(8) . 8_565 ? C21 Co2 C21 98.56(18) 8_565 . ? C21 Co2 C10 104.30(11) 8_565 . ? C21 Co2 C10 104.30(11) . . ? C21 Co2 S2 102.55(10) 8_565 . ? C21 Co2 S2 102.55(10) . . ? C10 Co2 S2 138.29(9) . . ? C21 Co2 Co1 151.77(9) 8_565 . ? C21 Co2 Co1 96.93(9) . . ? C10 Co2 Co1 48.72(6) . . ? S2 Co2 Co1 96.90(2) . . ? C21 Co2 Co1 96.93(9) 8_565 8_565 ? C21 Co2 Co1 151.77(9) . 8_565 ? C10 Co2 Co1 48.72(6) . 8_565 ? S2 Co2 Co1 96.90(2) . 8_565 ? Co1 Co2 Co1 60.225(17) . 8_565 ? C1 S1 C2 98.87(12) . . ? C1 S1 Co1 107.58(9) . . ? C2 S1 Co1 107.94(8) . . ? C2 S2 C2 99.17(15) . 8_565 ? C2 S2 Co2 108.28(8) . . ? C2 S2 Co2 108.28(8) 8_565 . ? O11 C11 Co1 175.9(2) . . ? O12 C12 Co1 176.0(2) . . ? O21 C21 Co2 176.6(3) . . ? Co1 C10 Co1 82.84(11) . 8_565 ? Co1 C10 Co2 82.31(11) . . ? Co1 C10 Co2 82.31(11) 8_565 . ? Co1 C10 H10 130.4 . . ? Co1 C10 H10 130.4 8_565 . ? Co2 C10 H10 130.4 . . ? C3 C1 S1 109.90(13) . 8_565 ? C3 C1 S1 109.90(13) . . ? S1 C1 S1 113.35(15) 8_565 . ? C3 C1 H1 107.8 . . ? S1 C1 H1 107.8 8_565 . ? S1 C1 H1 107.8 . . ? C4 C2 S2 109.70(17) . . ? C4 C2 S1 109.98(17) . . ? S2 C2 S1 112.38(11) . . ? C4 C2 H2 108.2 . . ? S2 C2 H2 108.2 . . ? S1 C2 H2 108.2 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? #===END data_br1174 _database_code_depnum_ccdc_archive 'CCDC 667574' _audit_creation_date 2009-05-16T20:31:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C18 H21 Co3 O6 S3 Si' _chemical_formula_moiety 'C18 H21 Co3 O6 S3 Si' _chemical_formula_weight 634.41 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P_42/n:2 _symmetry_space_group_name_Hall -p_4bc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 19.192(4) _cell_length_b 19.192(4) _cell_length_c 14.169(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5218.9(19) _cell_formula_units_Z 8 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 7230 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 28.85 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_crystal_description plate _exptl_crystal_size_max .21 _exptl_crystal_size_mid .21 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour dark_red _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.2 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.37 _exptl_absorpt_correction_T_max 0.84 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_number 40734 _diffrn_reflns_av_R_equivalents .064 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 4616 _reflns_number_gt 3906 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_molecular_graphics OrtepII _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0501P)^2^+12.7054P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4616 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.062 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.113 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.81 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.116 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.30165(3) 0.46690(3) 0.06744(4) 0.02087(17) Uani 1 1 d . . . Co2 Co 0.27388(3) 0.59095(3) 0.03086(4) 0.02080(17) Uani 1 1 d . . . Co3 Co 0.17753(3) 0.50678(3) 0.06622(4) 0.01918(16) Uani 1 1 d . . . S1 S 0.32279(6) 0.48061(6) 0.22567(8) 0.0233(3) Uani 1 1 d . . . S2 S 0.28887(6) 0.63285(6) 0.18116(8) 0.0237(3) Uani 1 1 d . . . S3 S 0.17044(6) 0.53063(6) 0.22462(7) 0.0234(3) Uani 1 1 d . . . C11 C 0.2803(3) 0.3761(3) 0.0600(4) 0.0376(13) Uani 1 1 d . . . O11 O 0.2661(3) 0.3187(2) 0.0516(4) 0.0807(18) Uani 1 1 d . . . C12 C 0.3868(3) 0.4591(3) 0.0126(4) 0.0364(13) Uani 1 1 d . . . O12 O 0.4378(2) 0.4506(3) -0.0278(3) 0.0636(13) Uani 1 1 d . . . C21 C 0.3578(3) 0.6110(3) -0.0204(3) 0.0294(12) Uani 1 1 d . . . O21 O 0.4104(2) 0.6232(2) -0.0567(3) 0.0482(11) Uani 1 1 d . . . C22 C 0.2216(3) 0.6567(3) -0.0266(3) 0.0320(12) Uani 1 1 d . . . O22 O 0.1879(2) 0.6961(2) -0.0673(3) 0.0544(12) Uani 1 1 d . . . C31 C 0.1070(2) 0.5545(3) 0.0124(3) 0.0263(11) Uani 1 1 d . . . O31 O 0.0625(2) 0.5825(2) -0.0282(3) 0.0462(10) Uani 1 1 d . . . C32 C 0.1352(3) 0.4224(3) 0.0648(3) 0.0269(11) Uani 1 1 d . . . O32 O 0.1074(2) 0.3693(2) 0.0609(3) 0.0414(9) Uani 1 1 d . . . C1 C 0.2377(2) 0.4789(3) 0.2865(3) 0.0278(11) Uani 1 1 d . . . H1 H 0.244 0.4988 0.3511 0.033 Uiso 1 1 calc R . . C2 C 0.3461(3) 0.5724(2) 0.2452(3) 0.0255(10) Uani 1 1 d . . . H2 H 0.341 0.5823 0.3142 0.031 Uiso 1 1 calc R . . C3 C 0.2070(2) 0.6182(3) 0.2460(3) 0.0271(11) Uani 1 1 d . . . H3 H 0.2166 0.6231 0.3151 0.033 Uiso 1 1 calc R . . C4 C 0.2131(3) 0.4031(3) 0.2968(4) 0.0406(14) Uani 1 1 d . . . H4A H 0.2079 0.3821 0.2342 0.061 Uiso 1 1 calc R . . H4B H 0.1682 0.4021 0.3297 0.061 Uiso 1 1 calc R . . H4C H 0.2476 0.3767 0.3332 0.061 Uiso 1 1 calc R . . C5 C 0.4227(3) 0.5847(3) 0.2186(4) 0.0345(12) Uani 1 1 d . . . H5A H 0.4285 0.5788 0.1503 0.052 Uiso 1 1 calc R . . H5B H 0.4522 0.5511 0.2519 0.052 Uiso 1 1 calc R . . H5C H 0.4362 0.6322 0.2364 0.052 Uiso 1 1 calc R . . C6 C 0.1531(3) 0.6731(3) 0.2174(4) 0.0398(13) Uani 1 1 d . . . H6A H 0.1714 0.7197 0.2308 0.06 Uiso 1 1 calc R . . H6B H 0.11 0.6657 0.2533 0.06 Uiso 1 1 calc R . . H6C H 0.1432 0.6689 0.1497 0.06 Uiso 1 1 calc R . . C10 C 0.2467(2) 0.5070(2) -0.0315(3) 0.0200(9) Uani 1 1 d . . . C20 C 0.2480(2) 0.4881(2) -0.1291(3) 0.0233(10) Uani 1 1 d . . . C30 C 0.2547(3) 0.4714(3) -0.2120(3) 0.0270(11) Uani 1 1 d . . . Si Si 0.28617(7) 0.44295(7) -0.32994(8) 0.0270(3) Uani 1 1 d . . . C101 C 0.2502(3) 0.5015(3) -0.4243(3) 0.0375(13) Uani 1 1 d . . . H10A H 0.2014 0.4894 -0.4363 0.056 Uiso 1 1 calc R . . H10B H 0.2773 0.4955 -0.4824 0.056 Uiso 1 1 calc R . . H10C H 0.2532 0.5501 -0.4035 0.056 Uiso 1 1 calc R . . C102 C 0.3842(3) 0.4481(3) -0.3224(4) 0.0459(15) Uani 1 1 d . . . H10D H 0.3981 0.4955 -0.3046 0.069 Uiso 1 1 calc R . . H10E H 0.4045 0.4365 -0.3839 0.069 Uiso 1 1 calc R . . H10F H 0.4011 0.4151 -0.2749 0.069 Uiso 1 1 calc R . . C103 C 0.2560(4) 0.3513(3) -0.3545(4) 0.0511(16) Uani 1 1 d . . . H10G H 0.2774 0.3193 -0.3089 0.077 Uiso 1 1 calc R . . H10H H 0.2697 0.3378 -0.4186 0.077 Uiso 1 1 calc R . . H10I H 0.2051 0.3489 -0.3486 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0258(3) 0.0248(3) 0.0120(3) -0.0017(2) -0.0037(2) 0.0009(3) Co2 0.0296(4) 0.0250(3) 0.0077(3) 0.0022(2) -0.0024(2) -0.0033(3) Co3 0.0242(3) 0.0263(3) 0.0070(3) -0.0003(2) -0.0021(2) -0.0018(2) S1 0.0279(6) 0.0286(6) 0.0135(5) 0.0041(4) -0.0063(4) -0.0028(5) S2 0.0330(7) 0.0255(6) 0.0126(5) -0.0030(4) -0.0023(5) -0.0043(5) S3 0.0262(6) 0.0362(7) 0.0078(5) -0.0023(4) 0.0006(4) -0.0037(5) C11 0.039(3) 0.035(3) 0.039(3) 0.001(2) -0.019(2) 0.003(2) O11 0.080(4) 0.020(2) 0.142(5) -0.013(3) -0.044(3) -0.004(2) C12 0.034(3) 0.046(3) 0.030(3) -0.008(2) -0.006(2) 0.004(2) O12 0.039(3) 0.082(3) 0.070(3) -0.016(3) 0.015(2) 0.010(2) C21 0.048(3) 0.034(3) 0.007(2) 0.0032(19) -0.008(2) -0.008(2) O21 0.044(2) 0.075(3) 0.026(2) 0.0108(19) 0.0066(18) -0.020(2) C22 0.047(3) 0.027(3) 0.022(3) 0.002(2) -0.010(2) -0.013(2) O22 0.064(3) 0.043(2) 0.057(3) 0.021(2) -0.032(2) -0.001(2) C31 0.028(3) 0.037(3) 0.013(2) -0.001(2) 0.0044(19) 0.002(2) O31 0.042(2) 0.063(3) 0.034(2) 0.0134(19) -0.0080(18) 0.015(2) C32 0.034(3) 0.040(3) 0.006(2) 0.0022(19) -0.0080(19) -0.001(2) O32 0.056(3) 0.039(2) 0.029(2) 0.0009(16) -0.0084(18) -0.0207(19) C1 0.029(3) 0.044(3) 0.010(2) 0.004(2) 0.0009(19) -0.009(2) C2 0.037(3) 0.030(3) 0.009(2) -0.0013(18) -0.0047(19) -0.005(2) C3 0.030(3) 0.036(3) 0.015(2) -0.009(2) 0.0044(19) -0.003(2) C4 0.044(3) 0.051(4) 0.027(3) 0.019(2) -0.011(2) -0.018(3) C5 0.030(3) 0.044(3) 0.029(3) -0.001(2) -0.007(2) -0.012(2) C6 0.044(3) 0.039(3) 0.036(3) -0.011(2) 0.002(3) 0.007(3) C10 0.023(2) 0.026(2) 0.011(2) -0.0020(18) -0.0022(17) -0.0003(19) C20 0.028(3) 0.034(3) 0.008(2) -0.0019(18) -0.0028(18) 0.000(2) C30 0.032(3) 0.036(3) 0.014(2) -0.001(2) 0.0013(19) -0.002(2) Si 0.0393(8) 0.0360(8) 0.0057(6) -0.0036(5) 0.0000(5) 0.0025(6) C101 0.044(3) 0.054(4) 0.014(2) 0.001(2) -0.003(2) 0.000(3) C102 0.046(3) 0.071(4) 0.021(3) -0.006(3) -0.003(2) 0.013(3) C103 0.081(5) 0.038(3) 0.034(3) -0.010(3) 0.014(3) -0.008(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C11 1.793(6) . ? Co1 C12 1.816(6) . ? Co1 C10 1.916(4) . ? Co1 S1 2.2937(13) . ? Co1 Co2 2.4942(10) . ? Co1 Co3 2.5020(10) . ? Co2 C22 1.806(5) . ? Co2 C21 1.808(5) . ? Co2 C10 1.910(4) . ? Co2 S2 2.2946(13) . ? Co2 Co3 2.5060(10) . ? Co3 C31 1.804(5) . ? Co3 C32 1.812(5) . ? Co3 C10 1.918(4) . ? Co3 S3 2.2947(13) . ? S1 C2 1.838(5) . ? S1 C1 1.848(5) . ? S2 C2 1.837(5) . ? S2 C3 1.842(5) . ? S3 C3 1.846(5) . ? S3 C1 1.849(5) . ? C11 O11 1.142(7) . ? C12 O12 1.145(7) . ? C21 O21 1.158(6) . ? C22 O22 1.149(6) . ? C31 O31 1.161(6) . ? C32 O32 1.151(6) . ? C1 C4 1.536(7) . ? C1 H1 1 . ? C2 C5 1.537(7) . ? C2 H2 1 . ? C3 C6 1.532(7) . ? C3 H3 1 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C10 C20 1.429(6) . ? C20 C30 1.224(6) . ? C30 Si 1.859(5) . ? Si C101 1.879(5) . ? Si C103 1.885(6) . ? Si C102 1.888(6) . ? C101 H10A 0.98 . ? C101 H10B 0.98 . ? C101 H10C 0.98 . ? C102 H10D 0.98 . ? C102 H10E 0.98 . ? C102 H10F 0.98 . ? C103 H10G 0.98 . ? C103 H10H 0.98 . ? C103 H10I 0.98 . ? 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 C11 Co1 C12 95.7(3) . . ? C11 Co1 C10 102.8(2) . . ? C12 Co1 C10 102.4(2) . . ? C11 Co1 S1 102.10(18) . . ? C12 Co1 S1 105.57(17) . . ? C10 Co1 S1 140.05(14) . . ? C11 Co1 Co2 150.07(16) . . ? C12 Co1 Co2 100.49(18) . . ? C10 Co1 Co2 49.22(13) . . ? S1 Co1 Co2 97.55(4) . . ? C11 Co1 Co3 94.57(18) . . ? C12 Co1 Co3 151.54(17) . . ? C10 Co1 Co3 49.30(13) . . ? S1 Co1 Co3 98.05(4) . . ? Co2 Co1 Co3 60.21(2) . . ? C22 Co2 C21 99.5(2) . . ? C22 Co2 C10 103.2(2) . . ? C21 Co2 C10 103.7(2) . . ? C22 Co2 S2 104.06(16) . . ? C21 Co2 S2 100.73(14) . . ? C10 Co2 S2 139.40(14) . . ? C22 Co2 Co1 151.55(16) . . ? C21 Co2 Co1 95.52(16) . . ? C10 Co2 Co1 49.42(13) . . ? S2 Co2 Co1 96.60(4) . . ? C22 Co2 Co3 97.48(16) . . ? C21 Co2 Co3 151.02(16) . . ? C10 Co2 Co3 49.24(13) . . ? S2 Co2 Co3 97.64(4) . . ? Co1 Co2 Co3 60.05(2) . . ? C31 Co3 C32 96.5(2) . . ? C31 Co3 C10 102.31(19) . . ? C32 Co3 C10 107.7(2) . . ? C31 Co3 S3 105.50(15) . . ? C32 Co3 S3 99.34(14) . . ? C10 Co3 S3 138.32(13) . . ? C31 Co3 Co1 150.81(15) . . ? C32 Co3 Co1 98.82(16) . . ? C10 Co3 Co1 49.23(13) . . ? S3 Co3 Co1 96.36(4) . . ? C31 Co3 Co2 98.17(16) . . ? C32 Co3 Co2 154.79(16) . . ? C10 Co3 Co2 48.98(13) . . ? S3 Co3 Co2 96.36(4) . . ? Co1 Co3 Co2 59.74(2) . . ? C2 S1 C1 99.3(2) . . ? C2 S1 Co1 107.47(14) . . ? C1 S1 Co1 107.30(15) . . ? C2 S2 C3 99.6(2) . . ? C2 S2 Co2 108.19(15) . . ? C3 S2 Co2 107.62(15) . . ? C3 S3 C1 98.4(2) . . ? C3 S3 Co3 108.65(15) . . ? C1 S3 Co3 108.36(16) . . ? O11 C11 Co1 177.4(5) . . ? O12 C12 Co1 174.1(5) . . ? O21 C21 Co2 177.2(4) . . ? O22 C22 Co2 176.2(5) . . ? O31 C31 Co3 175.0(4) . . ? O32 C32 Co3 177.6(4) . . ? C4 C1 S1 109.4(4) . . ? C4 C1 S3 109.9(3) . . ? S1 C1 S3 112.7(2) . . ? C4 C1 H1 108.2 . . ? S1 C1 H1 108.2 . . ? S3 C1 H1 108.2 . . ? C5 C2 S2 110.7(3) . . ? C5 C2 S1 110.1(3) . . ? S2 C2 S1 112.7(2) . . ? C5 C2 H2 107.7 . . ? S2 C2 H2 107.7 . . ? S1 C2 H2 107.7 . . ? C6 C3 S2 109.8(4) . . ? C6 C3 S3 109.0(3) . . ? S2 C3 S3 112.4(2) . . ? C6 C3 H3 108.5 . . ? S2 C3 H3 108.5 . . ? S3 C3 H3 108.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C20 C10 Co2 131.1(3) . . ? C20 C10 Co1 126.6(3) . . ? Co2 C10 Co1 81.36(17) . . ? C20 C10 Co3 135.2(3) . . ? Co2 C10 Co3 81.77(17) . . ? Co1 C10 Co3 81.47(17) . . ? C30 C20 C10 174.9(5) . . ? C20 C30 Si 166.8(4) . . ? C30 Si C101 110.2(2) . . ? C30 Si C103 109.9(2) . . ? C101 Si C103 108.3(3) . . ? C30 Si C102 104.9(2) . . ? C101 Si C102 112.0(3) . . ? C103 Si C102 111.5(3) . . ? Si C101 H10A 109.5 . . ? Si C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? Si C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? Si C102 H10D 109.5 . . ? Si C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? Si C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? Si C103 H10G 109.5 . . ? Si C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? Si C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? #===END data_br1179 _database_code_depnum_ccdc_archive 'CCDC 667575' _audit_creation_date 2009-05-17T10:52:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C34 H28 Au Cl3 Co3 O6 P S3' _chemical_formula_moiety 'C33 H27 Au Co3 O6 P S3, C H Cl3' _chemical_formula_weight 1139.82 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.634(3) _cell_length_b 15.125(2) _cell_length_c 25.670(3) _cell_angle_alpha 90 _cell_angle_beta 109.336(2) _cell_angle_gamma 90 _cell_volume 7925.8(18) _cell_formula_units_Z 8 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 5791 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 28.89 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.91 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4432 _exptl_crystal_description spear _exptl_crystal_size_max .45 _exptl_crystal_size_mid .23 _exptl_crystal_size_min .18 _exptl_crystal_size_rad ? _exptl_crystal_colour dark_red _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .204 _exptl_absorpt_correction_T_max .381 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_unetI/netI 0.0312 _diffrn_reflns_number 36320 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.96 _diffrn_reflns_theta_full 28.0 _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.939 _reflns_number_total 9864 _reflns_number_gt 8590 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction xtal _computing_structure_solution xtal _computing_molecular_graphics OrtepII _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0187P)^2^+40.7608P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9864 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0668 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.622 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.124 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 Au1 Au 0.627067(7) 0.423051(9) 0.559628(5) 0.01974(4) Uani 1 1 d . . . Co1 Co 0.60787(2) 0.14878(3) 0.724793(19) 0.02027(10) Uani 1 1 d . . . Co2 Co 0.67731(2) 0.07874(3) 0.676934(19) 0.01973(10) Uani 1 1 d . . . Co3 Co 0.72689(2) 0.17555(3) 0.757746(19) 0.02052(10) Uani 1 1 d . . . S1 S 0.60768(4) 0.03343(6) 0.78176(4) 0.02383(19) Uani 1 1 d . . . S2 S 0.69332(4) -0.05139(6) 0.72302(4) 0.02343(19) Uani 1 1 d . . . S3 S 0.75382(4) 0.06595(6) 0.82149(4) 0.02466(19) Uani 1 1 d . . . C11 C 0.5863(2) 0.2399(3) 0.75936(18) 0.0323(9) Uani 1 1 d . . . O11 O 0.57351(18) 0.3011(2) 0.77940(17) 0.0562(10) Uani 1 1 d . . . C12 C 0.53175(19) 0.1380(3) 0.67096(17) 0.0305(9) Uani 1 1 d . . . O12 O 0.48361(15) 0.1362(3) 0.63513(14) 0.0551(10) Uani 1 1 d . . . C21 C 0.6146(2) 0.0533(3) 0.61378(16) 0.0288(8) Uani 1 1 d . . . O21 O 0.57504(16) 0.0412(2) 0.57226(13) 0.0489(9) Uani 1 1 d . . . C22 C 0.7451(2) 0.0766(3) 0.65173(16) 0.0277(8) Uani 1 1 d . . . O22 O 0.78779(16) 0.0763(2) 0.63519(14) 0.0436(8) Uani 1 1 d . . . C31 C 0.8029(2) 0.1971(3) 0.74791(15) 0.0271(8) Uani 1 1 d . . . O31 O 0.85155(15) 0.2123(2) 0.74137(14) 0.0422(8) Uani 1 1 d . . . C32 C 0.72713(19) 0.2628(3) 0.80426(15) 0.0277(8) Uani 1 1 d . . . O32 O 0.72703(17) 0.3177(2) 0.83495(12) 0.0435(8) Uani 1 1 d . . . C1 C 0.68262(18) 0.0414(3) 0.84127(15) 0.0266(8) Uani 1 1 d . . . H1 H 0.69 -0.0166 0.8611 0.032 Uiso 1 1 calc R . . C2 C 0.62698(18) -0.0664(2) 0.75091(16) 0.0248(8) Uani 1 1 d . . . H2 H 0.64 -0.1134 0.7799 0.03 Uiso 1 1 calc R . . C3 C 0.76101(18) -0.0357(3) 0.78660(16) 0.0259(8) Uani 1 1 d . . . H3 H 0.7619 -0.0865 0.8118 0.031 Uiso 1 1 calc R . . C4 C 0.5662(2) -0.0974(3) 0.70489(18) 0.0334(9) Uani 1 1 d . . . H4A H 0.5532 -0.0524 0.6758 0.05 Uiso 1 1 calc R . . H4B H 0.5305 -0.1069 0.7198 0.05 Uiso 1 1 calc R . . H4C H 0.5759 -0.1529 0.6894 0.05 Uiso 1 1 calc R . . C5 C 0.82563(18) -0.0337(3) 0.77505(17) 0.0305(9) Uani 1 1 d . . . H5A H 0.8324 -0.0906 0.7595 0.046 Uiso 1 1 calc R . . H5B H 0.8616 -0.0228 0.8095 0.046 Uiso 1 1 calc R . . H5C H 0.8244 0.0137 0.7487 0.046 Uiso 1 1 calc R . . C6 C 0.6737(2) 0.1120(3) 0.88012(16) 0.0339(9) Uani 1 1 d . . . H6A H 0.7142 0.118 0.9116 0.051 Uiso 1 1 calc R . . H6B H 0.6378 0.095 0.8934 0.051 Uiso 1 1 calc R . . H6C H 0.6633 0.1685 0.8605 0.051 Uiso 1 1 calc R . . C10 C 0.66245(17) 0.1995(2) 0.68822(14) 0.0196(7) Uani 1 1 d . . . C20 C 0.65101(17) 0.2695(2) 0.65054(14) 0.0201(7) Uani 1 1 d . . . C30 C 0.64014(18) 0.3289(2) 0.61684(14) 0.0224(7) Uani 1 1 d . . . P1 P 0.61827(5) 0.52576(6) 0.49271(4) 0.02029(19) Uani 1 1 d . . . C111 C 0.58572(18) 0.6322(2) 0.50416(15) 0.0229(8) Uani 1 1 d . . . C112 C 0.61482(19) 0.6730(3) 0.55514(16) 0.0296(9) Uani 1 1 d . . . H112 H 0.6513 0.6459 0.5819 0.036 Uiso 1 1 calc R . . C113 C 0.5910(2) 0.7523(3) 0.56698(18) 0.0342(9) Uani 1 1 d . . . H113 H 0.6117 0.7804 0.6015 0.041 Uiso 1 1 calc R . . C114 C 0.5368(2) 0.7912(3) 0.5286(2) 0.0365(10) Uani 1 1 d . . . H114 H 0.5198 0.8452 0.5371 0.044 Uiso 1 1 calc R . . C115 C 0.5077(2) 0.7512(3) 0.47823(19) 0.0358(10) Uani 1 1 d . . . H115 H 0.4706 0.7779 0.4519 0.043 Uiso 1 1 calc R . . C116 C 0.53206(19) 0.6722(3) 0.46561(16) 0.0283(8) Uani 1 1 d . . . H116 H 0.5121 0.6453 0.4306 0.034 Uiso 1 1 calc R . . C121 C 0.56932(18) 0.4906(3) 0.42390(14) 0.0240(8) Uani 1 1 d . . . C122 C 0.5236(2) 0.4246(3) 0.41749(16) 0.0323(9) Uani 1 1 d . . . H122 H 0.5175 0.3985 0.4491 0.039 Uiso 1 1 calc R . . C123 C 0.4862(2) 0.3960(3) 0.36509(17) 0.0401(11) Uani 1 1 d . . . H123 H 0.4551 0.35 0.361 0.048 Uiso 1 1 calc R . . C124 C 0.4942(2) 0.4341(3) 0.31934(17) 0.0363(10) Uani 1 1 d . . . H124 H 0.4686 0.4146 0.2835 0.044 Uiso 1 1 calc R . . C125 C 0.5393(2) 0.5006(3) 0.32529(16) 0.0413(11) Uani 1 1 d . . . H125 H 0.5443 0.5276 0.2935 0.05 Uiso 1 1 calc R . . C126 C 0.5772(2) 0.5282(3) 0.37707(17) 0.0385(11) Uani 1 1 d . . . H126 H 0.609 0.5733 0.3809 0.046 Uiso 1 1 calc R . . C131 C 0.69811(18) 0.5496(3) 0.48744(14) 0.0221(7) Uani 1 1 d . . . C132 C 0.7444(2) 0.4818(3) 0.49859(16) 0.0284(8) Uani 1 1 d . . . H132 H 0.734 0.4253 0.5097 0.034 Uiso 1 1 calc R . . C133 C 0.8052(2) 0.4963(3) 0.49352(18) 0.0355(10) Uani 1 1 d . . . H133 H 0.8365 0.4498 0.501 0.043 Uiso 1 1 calc R . . C134 C 0.8207(2) 0.5782(3) 0.47770(18) 0.0352(10) Uani 1 1 d . . . H134 H 0.8627 0.5883 0.4748 0.042 Uiso 1 1 calc R . . C135 C 0.7750(2) 0.6455(3) 0.46608(17) 0.0333(9) Uani 1 1 d . . . H135 H 0.7856 0.7015 0.4545 0.04 Uiso 1 1 calc R . . C136 C 0.71388(19) 0.6322(3) 0.47108(15) 0.0258(8) Uani 1 1 d . . . H136 H 0.6829 0.679 0.4634 0.031 Uiso 1 1 calc R . . Cl1 Cl 0.91826(7) 0.33207(14) 0.63086(7) 0.0858(6) Uani 1 1 d . . . Cl2 Cl 0.78204(5) 0.28836(8) 0.60414(5) 0.0398(2) Uani 1 1 d . . . Cl3 Cl 0.85066(6) 0.24742(9) 0.52770(5) 0.0492(3) Uani 1 1 d . . . C01 C 0.8567(2) 0.2557(3) 0.59715(19) 0.0404(11) Uani 1 1 d . . . H01 H 0.869 0.1965 0.6149 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02308(7) 0.02085(7) 0.01404(6) 0.00383(5) 0.00447(5) -0.00076(6) Co1 0.0206(2) 0.0225(3) 0.0169(2) 0.00347(18) 0.00517(19) 0.00264(19) Co2 0.0210(2) 0.0193(2) 0.0175(2) 0.00040(19) 0.00448(18) 0.00104(19) Co3 0.0219(2) 0.0206(2) 0.0157(2) 0.00173(18) 0.00178(18) -0.00076(19) S1 0.0227(4) 0.0274(5) 0.0203(4) 0.0055(4) 0.0057(4) 0.0000(4) S2 0.0221(4) 0.0196(4) 0.0265(5) 0.0024(3) 0.0052(4) 0.0011(3) S3 0.0232(4) 0.0269(5) 0.0187(4) 0.0053(4) 0.0000(3) -0.0004(4) C11 0.028(2) 0.035(2) 0.035(2) -0.0023(18) 0.0122(18) 0.0028(17) O11 0.053(2) 0.045(2) 0.075(3) -0.0201(19) 0.027(2) 0.0071(17) C12 0.026(2) 0.041(2) 0.026(2) 0.0064(17) 0.0109(17) 0.0021(17) O12 0.0266(17) 0.097(3) 0.0336(18) 0.0094(19) -0.0004(14) 0.0012(18) C21 0.030(2) 0.030(2) 0.025(2) -0.0020(16) 0.0066(17) 0.0044(16) O21 0.0398(18) 0.065(2) 0.0303(17) -0.0165(16) -0.0039(14) 0.0104(17) C22 0.031(2) 0.028(2) 0.0235(19) -0.0020(16) 0.0088(16) -0.0004(17) O22 0.0409(18) 0.053(2) 0.0452(19) -0.0067(16) 0.0257(16) -0.0039(15) C31 0.030(2) 0.026(2) 0.0206(18) -0.0005(15) 0.0020(16) -0.0009(16) O31 0.0323(17) 0.0442(19) 0.051(2) -0.0014(15) 0.0154(15) -0.0095(14) C32 0.030(2) 0.032(2) 0.0188(18) 0.0021(16) 0.0047(15) -0.0037(16) O32 0.061(2) 0.0427(19) 0.0292(16) -0.0126(14) 0.0173(15) -0.0100(16) C1 0.0241(19) 0.032(2) 0.0212(18) 0.0103(16) 0.0040(15) 0.0005(16) C2 0.0249(18) 0.0228(19) 0.0276(19) 0.0047(15) 0.0096(15) -0.0026(15) C3 0.0239(19) 0.0221(19) 0.030(2) 0.0051(15) 0.0061(16) 0.0021(15) C4 0.025(2) 0.035(2) 0.037(2) -0.0009(18) 0.0068(17) -0.0056(17) C5 0.0222(19) 0.029(2) 0.035(2) 0.0064(17) 0.0034(17) 0.0026(16) C6 0.039(2) 0.044(3) 0.0171(18) 0.0024(17) 0.0067(17) 0.003(2) C10 0.0214(17) 0.0190(17) 0.0179(16) -0.0014(13) 0.0058(14) 0.0004(13) C20 0.0183(16) 0.0222(18) 0.0189(17) -0.0030(14) 0.0051(13) -0.0004(14) C30 0.0232(18) 0.0236(19) 0.0174(17) -0.0004(14) 0.0026(14) -0.0021(14) P1 0.0228(4) 0.0231(5) 0.0140(4) 0.0040(3) 0.0048(3) -0.0019(4) C111 0.0250(18) 0.0228(19) 0.0222(18) 0.0065(14) 0.0094(15) -0.0026(14) C112 0.026(2) 0.037(2) 0.026(2) 0.0020(17) 0.0083(16) -0.0007(16) C113 0.041(2) 0.033(2) 0.033(2) -0.0053(18) 0.0178(19) -0.0116(19) C114 0.036(2) 0.027(2) 0.053(3) 0.0003(19) 0.023(2) 0.0008(18) C115 0.030(2) 0.034(2) 0.043(3) 0.0116(19) 0.0113(19) 0.0041(18) C116 0.0262(19) 0.033(2) 0.0213(18) 0.0065(16) 0.0023(15) -0.0018(16) C121 0.0280(19) 0.028(2) 0.0154(16) 0.0023(14) 0.0057(14) -0.0027(15) C122 0.034(2) 0.045(2) 0.0176(18) 0.0039(17) 0.0080(16) -0.0134(19) C123 0.040(2) 0.052(3) 0.026(2) -0.0045(19) 0.0065(18) -0.023(2) C124 0.040(2) 0.048(3) 0.0181(19) -0.0031(17) 0.0058(17) -0.011(2) C125 0.053(3) 0.052(3) 0.0156(19) 0.0047(18) 0.0075(19) -0.019(2) C126 0.047(3) 0.043(3) 0.022(2) 0.0019(18) 0.0072(19) -0.021(2) C131 0.0235(18) 0.0285(19) 0.0142(16) -0.0015(14) 0.0059(14) -0.0029(15) C132 0.033(2) 0.028(2) 0.0242(19) -0.0015(15) 0.0095(16) -0.0033(16) C133 0.033(2) 0.039(3) 0.039(2) -0.0051(19) 0.0181(19) 0.0010(18) C134 0.032(2) 0.043(3) 0.037(2) -0.009(2) 0.0207(19) -0.0092(19) C135 0.045(2) 0.033(2) 0.028(2) -0.0025(17) 0.0196(19) -0.0125(19) C136 0.030(2) 0.026(2) 0.0234(19) 0.0011(15) 0.0111(16) -0.0036(16) Cl1 0.0405(7) 0.1322(16) 0.0832(11) -0.0687(11) 0.0185(7) -0.0319(9) Cl2 0.0311(5) 0.0467(7) 0.0399(6) -0.0037(5) 0.0097(5) 0.0027(5) Cl3 0.0515(7) 0.0541(8) 0.0435(7) -0.0193(6) 0.0176(6) -0.0026(6) C01 0.030(2) 0.051(3) 0.037(2) -0.010(2) 0.0068(19) 0.000(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Au1 C30 1.997(4) . ? Au1 P1 2.2768(9) . ? Co1 C12 1.772(4) . ? Co1 C11 1.783(4) . ? Co1 C10 1.897(4) . ? Co1 S1 2.2772(10) . ? Co1 Co3 2.4632(8) . ? Co1 Co2 2.4719(7) . ? Co2 C21 1.778(4) . ? Co2 C22 1.789(4) . ? Co2 C10 1.894(4) . ? Co2 S2 2.2632(11) . ? Co2 Co3 2.4747(7) . ? Co3 C31 1.774(4) . ? Co3 C32 1.778(4) . ? Co3 C10 1.901(3) . ? Co3 S3 2.2658(10) . ? S1 C2 1.816(4) . ? S1 C1 1.827(4) . ? S2 C3 1.812(4) . ? S2 C2 1.818(4) . ? S3 C3 1.811(4) . ? S3 C1 1.813(4) . ? C11 O11 1.136(5) . ? C12 O12 1.139(5) . ? C21 O21 1.139(5) . ? C22 O22 1.137(5) . ? C31 O31 1.143(5) . ? C32 O32 1.145(5) . ? C1 C6 1.516(6) . ? C1 H1 1 . ? C2 C4 1.522(5) . ? C2 H2 1 . ? C3 C5 1.522(5) . ? C3 H3 1 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C10 C20 1.399(5) . ? C20 C30 1.215(5) . ? P1 C131 1.813(4) . ? P1 C121 1.813(4) . ? P1 C111 1.820(4) . ? C111 C116 1.389(5) . ? C111 C112 1.394(5) . ? C112 C113 1.379(6) . ? C112 H112 0.95 . ? C113 C114 1.388(6) . ? C113 H113 0.95 . ? C114 C115 1.377(6) . ? C114 H114 0.95 . ? C115 C116 1.388(6) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.376(5) . ? C121 C126 1.391(5) . ? C122 C123 1.389(6) . ? C122 H122 0.95 . ? C123 C124 1.369(6) . ? C123 H123 0.95 . ? C124 C125 1.374(6) . ? C124 H124 0.95 . ? C125 C126 1.376(6) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C132 1.395(5) . ? C131 C136 1.396(5) . ? C132 C133 1.383(6) . ? C132 H132 0.95 . ? C133 C134 1.378(6) . ? C133 H133 0.95 . ? C134 C135 1.381(6) . ? C134 H134 0.95 . ? C135 C136 1.384(6) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? Cl1 C01 1.758(5) . ? Cl2 C01 1.755(5) . ? Cl3 C01 1.748(5) . ? C01 H01 1 . ? 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 C30 Au1 P1 175.79(11) . . ? C12 Co1 C11 97.5(2) . . ? C12 Co1 C10 102.78(17) . . ? C11 Co1 C10 104.01(18) . . ? C12 Co1 S1 103.40(14) . . ? C11 Co1 S1 102.48(15) . . ? C10 Co1 S1 139.59(11) . . ? C12 Co1 Co3 151.48(13) . . ? C11 Co1 Co3 96.79(14) . . ? C10 Co1 Co3 49.63(11) . . ? S1 Co1 Co3 97.43(3) . . ? C12 Co1 Co2 97.70(13) . . ? C11 Co1 Co2 151.76(14) . . ? C10 Co1 Co2 49.24(11) . . ? S1 Co1 Co2 96.98(3) . . ? Co3 Co1 Co2 60.19(2) . . ? C21 Co2 C22 97.80(18) . . ? C21 Co2 C10 103.40(17) . . ? C22 Co2 C10 105.90(17) . . ? C21 Co2 S2 103.11(14) . . ? C22 Co2 S2 99.86(13) . . ? C10 Co2 S2 139.76(11) . . ? C21 Co2 Co1 98.07(13) . . ? C22 Co2 Co1 153.33(13) . . ? C10 Co2 Co1 49.36(11) . . ? S2 Co2 Co1 97.23(3) . . ? C21 Co2 Co3 151.73(13) . . ? C22 Co2 Co3 97.70(13) . . ? C10 Co2 Co3 49.41(11) . . ? S2 Co2 Co3 97.33(3) . . ? Co1 Co2 Co3 59.73(2) . . ? C31 Co3 C32 99.34(18) . . ? C31 Co3 C10 104.92(16) . . ? C32 Co3 C10 109.10(16) . . ? C31 Co3 S3 102.03(13) . . ? C32 Co3 S3 96.59(13) . . ? C10 Co3 S3 138.68(11) . . ? C31 Co3 Co1 153.37(12) . . ? C32 Co3 Co1 97.05(13) . . ? C10 Co3 Co1 49.50(11) . . ? S3 Co3 Co1 96.74(3) . . ? C31 Co3 Co2 98.88(13) . . ? C32 Co3 Co2 154.94(13) . . ? C10 Co3 Co2 49.17(11) . . ? S3 Co3 Co2 96.26(3) . . ? Co1 Co3 Co2 60.078(19) . . ? C2 S1 C1 98.66(18) . . ? C2 S1 Co1 107.89(13) . . ? C1 S1 Co1 107.28(13) . . ? C3 S2 C2 99.77(18) . . ? C3 S2 Co2 107.15(13) . . ? C2 S2 Co2 108.07(13) . . ? C3 S3 C1 100.63(19) . . ? C3 S3 Co3 107.90(13) . . ? C1 S3 Co3 108.26(13) . . ? O11 C11 Co1 176.1(4) . . ? O12 C12 Co1 175.6(4) . . ? O21 C21 Co2 176.4(4) . . ? O22 C22 Co2 178.9(4) . . ? O31 C31 Co3 179.0(4) . . ? O32 C32 Co3 178.6(4) . . ? C6 C1 S3 110.2(3) . . ? C6 C1 S1 109.0(3) . . ? S3 C1 S1 112.4(2) . . ? C6 C1 H1 108.4 . . ? S3 C1 H1 108.4 . . ? S1 C1 H1 108.4 . . ? C4 C2 S1 109.3(3) . . ? C4 C2 S2 108.9(3) . . ? S1 C2 S2 113.2(2) . . ? C4 C2 H2 108.4 . . ? S1 C2 H2 108.4 . . ? S2 C2 H2 108.4 . . ? C5 C3 S2 110.3(3) . . ? C5 C3 S3 108.3(3) . . ? S2 C3 S3 112.4(2) . . ? C5 C3 H3 108.6 . . ? S2 C3 H3 108.6 . . ? S3 C3 H3 108.6 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C20 C10 Co2 128.6(3) . . ? C20 C10 Co1 130.6(3) . . ? Co2 C10 Co1 81.40(14) . . ? C20 C10 Co3 134.4(3) . . ? Co2 C10 Co3 81.42(14) . . ? Co1 C10 Co3 80.87(14) . . ? C30 C20 C10 178.4(4) . . ? C20 C30 Au1 176.0(3) . . ? C131 P1 C121 104.45(17) . . ? C131 P1 C111 105.37(17) . . ? C121 P1 C111 106.55(17) . . ? C131 P1 Au1 110.39(12) . . ? C121 P1 Au1 114.24(13) . . ? C111 P1 Au1 114.97(12) . . ? C116 C111 C112 119.2(4) . . ? C116 C111 P1 123.1(3) . . ? C112 C111 P1 117.6(3) . . ? C113 C112 C111 120.4(4) . . ? C113 C112 H112 119.8 . . ? C111 C112 H112 119.8 . . ? C112 C113 C114 120.1(4) . . ? C112 C113 H113 119.9 . . ? C114 C113 H113 119.9 . . ? C115 C114 C113 119.8(4) . . ? C115 C114 H114 120.1 . . ? C113 C114 H114 120.1 . . ? C114 C115 C116 120.5(4) . . ? C114 C115 H115 119.8 . . ? C116 C115 H115 119.8 . . ? C115 C116 C111 120.0(4) . . ? C115 C116 H116 120 . . ? C111 C116 H116 120 . . ? C122 C121 C126 118.9(3) . . ? C122 C121 P1 119.6(3) . . ? C126 C121 P1 121.5(3) . . ? C121 C122 C123 120.4(4) . . ? C121 C122 H122 119.8 . . ? C123 C122 H122 119.8 . . ? C124 C123 C122 120.1(4) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C123 C124 C125 119.9(4) . . ? C123 C124 H124 120 . . ? C125 C124 H124 120 . . ? C124 C125 C126 120.3(4) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C125 C126 C121 120.4(4) . . ? C125 C126 H126 119.8 . . ? C121 C126 H126 119.8 . . ? C132 C131 C136 119.3(3) . . ? C132 C131 P1 118.3(3) . . ? C136 C131 P1 122.3(3) . . ? C133 C132 C131 120.3(4) . . ? C133 C132 H132 119.9 . . ? C131 C132 H132 119.9 . . ? C134 C133 C132 120.1(4) . . ? C134 C133 H133 119.9 . . ? C132 C133 H133 119.9 . . ? C133 C134 C135 120.0(4) . . ? C133 C134 H134 120 . . ? C135 C134 H134 120 . . ? C134 C135 C136 120.7(4) . . ? C134 C135 H135 119.7 . . ? C136 C135 H135 119.7 . . ? C135 C136 C131 119.6(4) . . ? C135 C136 H136 120.2 . . ? C131 C136 H136 120.2 . . ? Cl3 C01 Cl2 111.3(2) . . ? Cl3 C01 Cl1 109.8(3) . . ? Cl2 C01 Cl1 109.7(3) . . ? Cl3 C01 H01 108.7 . . ? Cl2 C01 H01 108.7 . . ? Cl1 C01 H01 108.7 . . ? #===END data_br1178 _database_code_depnum_ccdc_archive 'CCDC 667576' _audit_creation_date 2009-05-17T10:12:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C28 H30 Co4 O10 S3 Si2' _chemical_formula_moiety 'C28 H30 Co4 O10 S3 Si2' _chemical_formula_weight 914.6 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.338(2) _cell_length_b 13.998(2) _cell_length_c 23.252(4) _cell_angle_alpha 90 _cell_angle_beta 101.824(3) _cell_angle_gamma 90 _cell_volume 3930.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 5108 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.46 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_crystal_description plate _exptl_crystal_size_max .48 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .1 _exptl_crystal_size_rad ? _exptl_crystal_colour dark_red _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.926 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.561 _exptl_absorpt_correction_T_max 0.825 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_av_unetI/netI 0.0484 _diffrn_reflns_number 34418 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 8955 _reflns_number_gt 6807 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_molecular_graphics OrtepII _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0531P)^2^+5.2113P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8955 _refine_ls_number_parameters 491 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1253 _refine_ls_wR_factor_gt 0.1165 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.957 _refine_diff_density_min -0.47 _refine_diff_density_rms 0.096 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.57591(4) 0.85491(3) 0.12567(2) 0.02865(12) Uani 1 1 d . A . Co2 Co 0.48885(4) 0.84278(3) 0.21164(2) 0.02642(12) Uani 1 1 d . A . Co3 Co 0.21895(4) 0.73880(4) 0.04186(2) 0.03512(14) Uani 1 1 d . . . Co4 Co 0.36266(18) 0.61563(15) 0.05703(10) 0.0288(4) Uani 0.681(5) 1 d P A 1 Co4' Co 0.3802(4) 0.6234(4) 0.04070(18) 0.0274(7) Uani 0.319(5) 1 d P A 2 S1 S 0.69968(8) 0.97364(7) 0.16189(5) 0.0397(2) Uani 1 1 d . . . S2 S 0.58193(8) 0.96749(7) 0.26344(4) 0.0359(2) Uani 1 1 d . . . S3 S 0.79262(9) 0.84860(8) 0.26972(5) 0.0466(3) Uani 1 1 d . . . C11 C 0.6603(4) 0.7485(3) 0.13407(19) 0.0462(10) Uani 1 1 d . . . O11 O 0.7056(3) 0.6770(3) 0.13837(19) 0.0779(12) Uani 1 1 d . . . C12 C 0.5616(3) 0.8827(3) 0.04836(19) 0.0444(10) Uani 1 1 d . . . O12 O 0.5481(3) 0.8980(3) -0.00032(15) 0.0718(11) Uani 1 1 d . . . C21 C 0.3656(4) 0.8457(3) 0.24039(19) 0.0446(10) Uani 1 1 d . . . O21 O 0.2830(3) 0.8461(3) 0.25587(19) 0.0760(12) Uani 1 1 d . . . C22 C 0.5537(3) 0.7354(3) 0.24380(17) 0.0385(9) Uani 1 1 d . . . O22 O 0.5884(3) 0.6623(2) 0.25997(16) 0.0666(10) Uani 1 1 d . . . C31 C 0.1009(4) 0.6688(3) 0.0047(2) 0.0491(11) Uani 1 1 d . A . O31 O 0.0262(3) 0.6262(3) -0.01793(18) 0.0748(11) Uani 1 1 d . . . C32 C 0.2584(5) 0.8154(4) -0.0128(3) 0.0708(17) Uani 1 1 d . A . O32 O 0.2832(5) 0.8638(4) -0.0464(2) 0.133(2) Uani 1 1 d . . . C33 C 0.1414(6) 0.8317(6) 0.0690(5) 0.058(2) Uani 0.681(5) 1 d P A 1 O33 O 0.0929(5) 0.8853(5) 0.0899(5) 0.105(3) Uani 0.681(5) 1 d P A 1 C33' C 0.1532(12) 0.8046(10) 0.0928(6) 0.029(3) Uiso 0.319(5) 1 d P A 2 O33' O 0.1102(11) 0.8472(10) 0.1234(5) 0.060(3) Uiso 0.319(5) 1 d P A 2 C41 C 0.2856(4) 0.5200(3) 0.0129(2) 0.0551(13) Uani 1 1 d . . . O41 O 0.2355(3) 0.4600(3) -0.01237(17) 0.0774(12) Uani 1 1 d . A . C42 C 0.4610(6) 0.5456(5) 0.1061(4) 0.062(2) Uani 0.681(5) 1 d P A 1 O42 O 0.5216(6) 0.5030(4) 0.1405(4) 0.119(4) Uani 0.681(5) 1 d P A 1 C43 C 0.4489(7) 0.6528(6) 0.0061(4) 0.0506(18) Uani 0.681(5) 1 d P A 1 O43 O 0.5066(7) 0.6758(6) -0.0253(4) 0.098(3) Uani 0.681(5) 1 d P A 1 C42' C 0.4996(15) 0.5609(12) 0.0753(8) 0.054(4) Uiso 0.319(5) 1 d P A 2 O42' O 0.5758(11) 0.5186(10) 0.0989(6) 0.076(4) Uiso 0.319(5) 1 d P A 2 C43' C 0.4381(16) 0.6815(12) -0.0165(8) 0.042(4) Uiso 0.319(5) 1 d P A 2 O43' O 0.4650(13) 0.7164(11) -0.0509(7) 0.075(4) Uiso 0.319(5) 1 d P A 2 C1 C 0.8215(3) 0.9296(3) 0.2146(2) 0.0468(10) Uani 1 1 d . . . H1 H 0.8602 0.9863 0.2355 0.056 Uiso 1 1 calc R . . C2 C 0.6406(3) 1.0435(3) 0.21349(19) 0.0411(10) Uani 1 1 d . . . H2 H 0.7024 1.0808 0.238 0.049 Uiso 1 1 calc R . . C3 C 0.7133(3) 0.9243(3) 0.30809(18) 0.0452(10) Uani 1 1 d . . . H3 H 0.7597 0.9814 0.3226 0.054 Uiso 1 1 calc R . . C4 C 0.9011(4) 0.8823(5) 0.1808(3) 0.0775(18) Uani 1 1 d . . . H4A H 0.9691 0.8639 0.2084 0.116 Uiso 1 1 calc R . . H4B H 0.9191 0.9274 0.152 0.116 Uiso 1 1 calc R . . H4C H 0.8661 0.8254 0.1606 0.116 Uiso 1 1 calc R . . C5 C 0.5569(4) 1.1151(3) 0.1817(2) 0.0586(14) Uani 1 1 d . . . H5A H 0.5925 1.1566 0.1571 0.088 Uiso 1 1 calc R . . H5B H 0.5289 1.154 0.2105 0.088 Uiso 1 1 calc R . . H5C H 0.4952 1.0809 0.1569 0.088 Uiso 1 1 calc R . . C6 C 0.6889(5) 0.8721(4) 0.3614(2) 0.0680(15) Uani 1 1 d . . . H6A H 0.6438 0.8154 0.3484 0.102 Uiso 1 1 calc R . . H6B H 0.6484 0.9146 0.383 0.102 Uiso 1 1 calc R . . H6C H 0.7586 0.8526 0.387 0.102 Uiso 1 1 calc R . . C101 C 0.1632(7) 1.1462(7) -0.0079(3) 0.146(4) Uani 1 1 d . . . H10A H 0.2319 1.1536 -0.0224 0.218 Uiso 1 1 calc R . . H10B H 0.1148 1.2012 -0.0202 0.218 Uiso 1 1 calc R . . H10C H 0.1254 1.0875 -0.024 0.218 Uiso 1 1 calc R . . C102 C 0.2745(6) 1.2465(4) 0.1036(4) 0.115(3) Uani 1 1 d . . . H10D H 0.2807 1.2485 0.1462 0.173 Uiso 1 1 calc R . . H10E H 0.2357 1.3037 0.0858 0.173 Uiso 1 1 calc R . . H10F H 0.3487 1.2443 0.0946 0.173 Uiso 1 1 calc R . . C103 C 0.0695(5) 1.1290(5) 0.1034(3) 0.092(2) Uani 1 1 d . . . H10G H 0.0283 1.0717 0.0874 0.138 Uiso 1 1 calc R . . H10H H 0.0231 1.1856 0.0924 0.138 Uiso 1 1 calc R . . H10I H 0.0895 1.1242 0.1463 0.138 Uiso 1 1 calc R . . Si1 Si 0.19618(12) 1.13918(10) 0.07351(6) 0.0551(4) Uani 1 1 d . . . C10 C 0.2873(3) 1.0363(3) 0.09619(18) 0.0402(9) Uani 1 1 d . . . C20 C 0.3524(3) 0.9728(3) 0.11319(17) 0.0330(8) Uani 1 1 d . . . C30 C 0.4303(3) 0.9007(2) 0.13470(15) 0.0263(7) Uani 1 1 d . A . C40 C 0.4317(3) 0.8026(2) 0.13034(14) 0.0265(7) Uani 1 1 d . . . C50 C 0.3569(3) 0.7299(2) 0.10281(15) 0.0297(8) Uani 1 1 d . A . C60 C 0.2842(4) 0.6626(3) 0.11119(18) 0.0498(12) Uani 1 1 d . A . Si2 Si 0.1994(3) 0.60629(19) 0.16295(9) 0.0516(8) Uani 0.681(5) 1 d P A 1 Si2' Si 0.2610(4) 0.5629(3) 0.16081(16) 0.0367(14) Uani 0.319(5) 1 d P A 2 C201 C 0.1342(17) 0.4945(12) 0.1220(9) 0.054(5) Uani 0.681(5) 1 d P A 1 H20A H 0.1929 0.4521 0.1143 0.082 Uiso 0.681(5) 1 calc PR A 1 H20B H 0.0867 0.5134 0.0846 0.082 Uiso 0.681(5) 1 calc PR A 1 H20C H 0.0898 0.4609 0.1461 0.082 Uiso 0.681(5) 1 calc PR A 1 C202 C 0.2956(11) 0.5783(8) 0.2313(3) 0.109(5) Uani 0.681(5) 1 d P A 1 H20D H 0.3329 0.6369 0.2479 0.164 Uiso 0.681(5) 1 calc PR A 1 H20E H 0.3509 0.5325 0.2235 0.164 Uiso 0.681(5) 1 calc PR A 1 H20F H 0.255 0.5504 0.2593 0.164 Uiso 0.681(5) 1 calc PR A 1 C203 C 0.0886(9) 0.6874(7) 0.1790(5) 0.109(4) Uani 0.681(5) 1 d P A 1 H20G H 0.049 0.6556 0.2061 0.163 Uiso 0.681(5) 1 calc PR A 1 H20H H 0.0366 0.7026 0.1423 0.163 Uiso 0.681(5) 1 calc PR A 1 H20I H 0.1224 0.7465 0.1969 0.163 Uiso 0.681(5) 1 calc PR A 1 C204 C 0.209(2) 0.6282(17) 0.2227(11) 0.097(7) Uiso 0.319(5) 1 d P A 2 H20J H 0.1789 0.5816 0.2466 0.145 Uiso 0.319(5) 1 calc PR A 2 H20K H 0.1517 0.674 0.2057 0.145 Uiso 0.319(5) 1 calc PR A 2 H20L H 0.2713 0.6622 0.2475 0.145 Uiso 0.319(5) 1 calc PR A 2 C205 C 0.3784(15) 0.4879(13) 0.1921(8) 0.075(5) Uiso 0.319(5) 1 d P A 2 H20M H 0.3991 0.4488 0.1611 0.112 Uiso 0.319(5) 1 calc PR A 2 H20N H 0.3584 0.4461 0.2222 0.112 Uiso 0.319(5) 1 calc PR A 2 H20O H 0.4412 0.5282 0.2101 0.112 Uiso 0.319(5) 1 calc PR A 2 C206 C 0.134(3) 0.504(3) 0.129(2) 0.048(9) Uiso 0.319(5) 1 d P A 2 H20P H 0.1462 0.4628 0.0968 0.072 Uiso 0.319(5) 1 calc PR A 2 H20Q H 0.0777 0.5519 0.1137 0.072 Uiso 0.319(5) 1 calc PR A 2 H20R H 0.1097 0.4653 0.159 0.072 Uiso 0.319(5) 1 calc PR A 2 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 0.0249(2) 0.0311(2) 0.0304(3) 0.0002(2) 0.00671(19) 0.00165(19) Co2 0.0295(3) 0.0239(2) 0.0255(2) -0.00233(18) 0.00483(19) -0.00195(19) Co3 0.0251(3) 0.0326(3) 0.0450(3) -0.0029(2) 0.0010(2) -0.0001(2) Co4 0.0285(7) 0.0294(5) 0.0273(10) -0.0081(6) 0.0027(6) 0.0042(4) Co4' 0.0286(14) 0.0394(13) 0.0163(16) -0.0090(12) 0.0092(10) 0.0065(10) S1 0.0301(5) 0.0414(5) 0.0467(6) 0.0045(4) 0.0062(4) -0.0080(4) S2 0.0340(5) 0.0323(5) 0.0400(5) -0.0118(4) 0.0045(4) -0.0029(4) S3 0.0364(5) 0.0408(5) 0.0545(7) -0.0017(5) -0.0095(5) 0.0063(4) C11 0.041(2) 0.050(2) 0.048(3) -0.005(2) 0.0107(19) 0.011(2) O11 0.073(3) 0.059(2) 0.100(3) -0.008(2) 0.012(2) 0.034(2) C12 0.037(2) 0.056(3) 0.042(2) 0.006(2) 0.0140(18) -0.0051(19) O12 0.076(3) 0.101(3) 0.0411(19) 0.0137(19) 0.0186(18) -0.011(2) C21 0.055(3) 0.036(2) 0.046(2) -0.0139(18) 0.019(2) -0.0090(19) O21 0.068(2) 0.077(2) 0.100(3) -0.034(2) 0.057(2) -0.021(2) C22 0.044(2) 0.036(2) 0.032(2) 0.0047(16) 0.0006(17) -0.0048(18) O22 0.076(2) 0.0390(17) 0.077(2) 0.0193(16) -0.003(2) 0.0048(16) C31 0.038(2) 0.046(2) 0.054(3) -0.004(2) -0.010(2) -0.0014(19) O31 0.051(2) 0.073(2) 0.088(3) -0.015(2) -0.017(2) -0.0190(18) C32 0.063(3) 0.067(3) 0.067(3) 0.026(3) -0.023(3) -0.010(3) O32 0.134(5) 0.138(5) 0.107(4) 0.085(4) -0.023(3) -0.045(4) C33 0.029(4) 0.044(4) 0.097(7) 0.003(5) 0.004(4) -0.004(3) O33 0.050(4) 0.055(4) 0.226(10) -0.045(5) 0.067(5) 0.000(3) C41 0.062(3) 0.039(2) 0.054(3) -0.015(2) -0.012(2) 0.004(2) O41 0.092(3) 0.054(2) 0.075(2) -0.0266(19) -0.009(2) -0.014(2) C42 0.050(4) 0.037(3) 0.083(6) -0.007(4) -0.022(4) 0.010(3) O42 0.097(5) 0.062(4) 0.158(7) 0.014(4) -0.072(6) 0.025(4) C43 0.054(5) 0.057(5) 0.046(5) -0.015(4) 0.024(4) -0.007(4) O43 0.084(5) 0.112(6) 0.118(7) -0.037(5) 0.065(5) -0.020(5) C1 0.024(2) 0.055(3) 0.059(3) -0.008(2) 0.0006(18) -0.0023(18) C2 0.033(2) 0.0262(18) 0.060(3) -0.0025(17) -0.0006(18) -0.0053(15) C3 0.043(2) 0.049(2) 0.037(2) -0.0092(18) -0.0082(18) -0.0055(19) C4 0.032(3) 0.112(5) 0.088(4) -0.025(4) 0.011(3) 0.007(3) C5 0.051(3) 0.029(2) 0.087(4) 0.001(2) -0.007(3) -0.0032(19) C6 0.079(4) 0.085(4) 0.033(2) 0.003(2) -0.004(2) -0.009(3) C101 0.124(6) 0.247(11) 0.066(4) 0.047(5) 0.020(4) 0.132(7) C102 0.112(6) 0.041(3) 0.200(9) 0.002(4) 0.049(6) 0.026(3) C103 0.058(4) 0.110(5) 0.118(5) 0.039(4) 0.039(4) 0.042(4) Si1 0.0537(8) 0.0590(8) 0.0549(8) 0.0149(6) 0.0165(6) 0.0342(6) C10 0.033(2) 0.039(2) 0.046(2) 0.0018(18) 0.0041(18) 0.0060(17) C20 0.0278(19) 0.0313(18) 0.039(2) -0.0002(15) 0.0053(15) -0.0039(15) C30 0.0236(17) 0.0261(16) 0.0287(18) -0.0003(13) 0.0043(13) -0.0021(13) C40 0.0263(17) 0.0292(17) 0.0236(17) -0.0009(13) 0.0043(13) -0.0017(14) C50 0.0346(19) 0.0287(17) 0.0233(17) 0.0006(14) -0.0002(14) 0.0024(15) C60 0.068(3) 0.043(2) 0.032(2) 0.0009(17) -0.005(2) -0.026(2) Si2 0.0720(19) 0.0444(13) 0.0414(11) -0.0063(9) 0.0186(10) -0.0282(13) Si2' 0.040(3) 0.032(2) 0.0318(19) 0.0050(15) -0.0059(16) -0.0180(19) C201 0.068(7) 0.042(6) 0.049(7) -0.006(5) 0.002(5) -0.036(5) C202 0.157(11) 0.119(8) 0.037(4) 0.022(5) -0.013(5) -0.096(8) C203 0.132(9) 0.067(6) 0.163(11) -0.029(6) 0.114(9) -0.034(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C11 1.804(4) . ? Co1 C12 1.812(4) . ? Co1 C40 1.948(3) . ? Co1 C30 1.959(4) . ? Co1 S1 2.2970(11) . ? Co1 Co2 2.4612(8) . ? Co2 C21 1.783(5) . ? Co2 C22 1.793(4) . ? Co2 C40 1.960(3) . ? Co2 C30 1.962(3) . ? Co2 S2 2.2913(10) . ? Co3 C33 1.803(8) . ? Co3 C32 1.805(6) . ? Co3 C33' 1.818(14) . ? Co3 C31 1.820(4) . ? Co3 C60 1.963(4) . ? Co3 C50 1.983(3) . ? Co3 Co4 2.446(2) . ? Co3 Co4' 2.567(5) . ? Co4 C42 1.780(7) . ? Co4 C43 1.822(8) . ? Co4 C41 1.830(5) . ? Co4 C60 1.859(6) . ? Co4 C50 1.931(4) . ? Co4' C42' 1.759(18) . ? Co4' C43' 1.82(2) . ? Co4' C41 1.888(7) . ? Co4' C50 2.136(5) . ? Co4' C60 2.277(6) . ? S1 C2 1.812(4) . ? S1 C1 1.841(4) . ? S2 C2 1.830(4) . ? S2 C3 1.839(4) . ? S3 C3 1.798(5) . ? S3 C1 1.800(5) . ? C11 O11 1.142(5) . ? C12 O12 1.130(5) . ? C21 O21 1.148(5) . ? C22 O22 1.143(5) . ? C31 O31 1.133(5) . ? C32 O32 1.123(7) . ? C33 O33 1.130(10) . ? C33' O33' 1.140(19) . ? C41 O41 1.133(5) . ? C42 O42 1.144(8) . ? C43 O43 1.165(10) . ? C42' O42' 1.152(19) . ? C43' O43' 1.05(2) . ? C1 C4 1.527(7) . ? C1 H1 1 . ? C2 C5 1.519(6) . ? C2 H2 1 . ? C3 C6 1.521(7) . ? C3 H3 1 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C101 Si1 1.855(7) . ? C101 H10A 0.98 . ? C101 H10B 0.98 . ? C101 H10C 0.98 . ? C102 Si1 1.844(7) . ? C102 H10D 0.98 . ? C102 H10E 0.98 . ? C102 H10F 0.98 . ? C103 Si1 1.842(6) . ? C103 H10G 0.98 . ? C103 H10H 0.98 . ? C103 H10I 0.98 . ? Si1 C10 1.837(4) . ? C10 C20 1.208(5) . ? C20 C30 1.413(5) . ? C30 C40 1.377(5) . ? C40 C50 1.434(5) . ? C50 C60 1.343(5) . ? C60 Si2' 1.870(5) . ? C60 Si2 1.918(5) . ? Si2 C202 1.821(10) . ? Si2 C203 1.871(10) . ? Si2 C201 1.921(15) . ? Si2' C206 1.79(4) . ? Si2' C205 1.817(19) . ? Si2' C204 1.92(2) . ? C201 H20A 0.98 . ? C201 H20B 0.98 . ? C201 H20C 0.98 . ? C202 H20D 0.98 . ? C202 H20E 0.98 . ? C202 H20F 0.98 . ? C203 H20G 0.98 . ? C203 H20H 0.98 . ? C203 H20I 0.98 . ? C204 H20J 0.98 . ? C204 H20K 0.98 . ? C204 H20L 0.98 . ? C205 H20M 0.98 . ? C205 H20N 0.98 . ? C205 H20O 0.98 . ? C206 H20P 0.98 . ? C206 H20Q 0.98 . ? C206 H20R 0.98 . ? 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 C11 Co1 C12 102.8(2) . . ? C11 Co1 C40 101.39(18) . . ? C12 Co1 C40 103.39(17) . . ? C11 Co1 C30 141.25(18) . . ? C12 Co1 C30 97.54(17) . . ? C40 Co1 C30 41.27(14) . . ? C11 Co1 S1 103.41(15) . . ? C12 Co1 S1 97.51(14) . . ? C40 Co1 S1 142.92(11) . . ? C30 Co1 S1 106.23(10) . . ? C11 Co1 Co2 101.14(15) . . ? C12 Co1 Co2 148.27(14) . . ? C40 Co1 Co2 51.17(10) . . ? C30 Co1 Co2 51.18(10) . . ? S1 Co1 Co2 96.90(3) . . ? C21 Co2 C22 101.8(2) . . ? C21 Co2 C40 101.67(17) . . ? C22 Co2 C40 101.74(16) . . ? C21 Co2 C30 98.59(18) . . ? C22 Co2 C30 140.92(16) . . ? C40 Co2 C30 41.10(14) . . ? C21 Co2 S2 99.17(13) . . ? C22 Co2 S2 106.68(12) . . ? C40 Co2 S2 140.19(11) . . ? C30 Co2 S2 102.46(10) . . ? C21 Co2 Co1 148.30(15) . . ? C22 Co2 Co1 99.50(14) . . ? C40 Co2 Co1 50.74(10) . . ? C30 Co2 Co1 51.06(10) . . ? S2 Co2 Co1 96.85(3) . . ? C33 Co3 C32 93.3(4) . . ? C33 Co3 C33' 21.0(4) . . ? C32 Co3 C33' 112.3(5) . . ? C33 Co3 C31 97.2(3) . . ? C32 Co3 C31 106.9(2) . . ? C33' Co3 C31 99.3(5) . . ? C33 Co3 C60 105.2(4) . . ? C32 Co3 C60 141.0(2) . . ? C33' Co3 C60 84.4(5) . . ? C31 Co3 C60 104.53(19) . . ? C33 Co3 C50 103.5(3) . . ? C32 Co3 C50 103.01(19) . . ? C33' Co3 C50 89.9(4) . . ? C31 Co3 C50 142.34(17) . . ? C60 Co3 C50 39.78(16) . . ? C33 Co3 Co4 151.5(3) . . ? C32 Co3 Co4 103.2(2) . . ? C33' Co3 Co4 132.1(4) . . ? C31 Co3 Co4 100.06(15) . . ? C60 Co3 Co4 48.35(16) . . ? C50 Co3 Co4 50.37(11) . . ? C33 Co3 Co4' 157.7(3) . . ? C32 Co3 Co4' 92.6(2) . . ? C33' Co3 Co4' 140.9(4) . . ? C31 Co3 Co4' 101.67(18) . . ? C60 Co3 Co4' 58.56(18) . . ? C50 Co3 Co4' 54.17(14) . . ? Co4 Co3 Co4' 10.78(8) . . ? C42 Co4 C43 99.3(5) . . ? C42 Co4 C41 99.5(3) . . ? C43 Co4 C41 98.6(3) . . ? C42 Co4 C60 98.2(4) . . ? C43 Co4 C60 142.5(3) . . ? C41 Co4 C60 110.8(2) . . ? C42 Co4 C50 101.6(3) . . ? C43 Co4 C50 102.4(3) . . ? C41 Co4 C50 147.3(2) . . ? C60 Co4 C50 41.45(17) . . ? C42 Co4 Co3 149.3(3) . . ? C43 Co4 Co3 102.0(3) . . ? C41 Co4 Co3 99.01(17) . . ? C60 Co4 Co3 52.10(15) . . ? C50 Co4 Co3 52.27(11) . . ? C42' Co4' C43' 97.9(8) . . ? C42' Co4' C41 100.2(6) . . ? C43' Co4' C41 113.5(6) . . ? C42' Co4' C50 104.7(6) . . ? C43' Co4' C50 108.0(6) . . ? C41 Co4' C50 127.4(3) . . ? C42' Co4' C60 107.5(6) . . ? C43' Co4' C60 139.1(6) . . ? C41 Co4' C60 93.2(3) . . ? C50 Co4' C60 35.24(15) . . ? C42' Co4' Co3 152.4(6) . . ? C43' Co4' Co3 98.5(6) . . ? C41 Co4' Co3 93.4(2) . . ? C50 Co4' Co3 48.82(13) . . ? C60 Co4' Co3 47.34(14) . . ? C2 S1 C1 97.13(19) . . ? C2 S1 Co1 107.81(13) . . ? C1 S1 Co1 113.10(15) . . ? C2 S2 C3 97.6(2) . . ? C2 S2 Co2 109.28(13) . . ? C3 S2 Co2 109.59(14) . . ? C3 S3 C1 100.9(2) . . ? O11 C11 Co1 174.3(4) . . ? O12 C12 Co1 176.8(4) . . ? O21 C21 Co2 176.2(4) . . ? O22 C22 Co2 173.4(4) . . ? O31 C31 Co3 178.7(5) . . ? O32 C32 Co3 179.2(6) . . ? O33 C33 Co3 174.4(10) . . ? O33' C33' Co3 178.1(13) . . ? O41 C41 Co4 176.8(5) . . ? O41 C41 Co4' 168.3(5) . . ? O42 C42 Co4 175.7(10) . . ? O43 C43 Co4 178.0(11) . . ? O42' C42' Co4' 177.9(18) . . ? O43' C43' Co4' 175.5(19) . . ? C4 C1 S3 109.6(4) . . ? C4 C1 S1 109.0(3) . . ? S3 C1 S1 115.6(2) . . ? C4 C1 H1 107.4 . . ? S3 C1 H1 107.4 . . ? S1 C1 H1 107.4 . . ? C5 C2 S1 111.0(3) . . ? C5 C2 S2 112.0(3) . . ? S1 C2 S2 111.81(19) . . ? C5 C2 H2 107.2 . . ? S1 C2 H2 107.2 . . ? S2 C2 H2 107.2 . . ? C6 C3 S3 109.9(3) . . ? C6 C3 S2 108.6(3) . . ? S3 C3 S2 114.8(2) . . ? C6 C3 H3 107.8 . . ? S3 C3 H3 107.8 . . ? S2 C3 H3 107.8 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C101 H10A 109.5 . . ? Si1 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? Si1 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? Si1 C102 H10D 109.5 . . ? Si1 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? Si1 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? Si1 C103 H10G 109.5 . . ? Si1 C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? Si1 C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? C10 Si1 C103 110.4(2) . . ? C10 Si1 C102 106.7(3) . . ? C103 Si1 C102 109.8(4) . . ? C10 Si1 C101 109.1(3) . . ? C103 Si1 C101 111.3(4) . . ? C102 Si1 C101 109.4(5) . . ? C20 C10 Si1 175.6(4) . . ? C10 C20 C30 178.0(4) . . ? C40 C30 C20 134.7(3) . . ? C40 C30 Co1 68.9(2) . . ? C20 C30 Co1 140.2(3) . . ? C40 C30 Co2 69.35(19) . . ? C20 C30 Co2 135.6(3) . . ? Co1 C30 Co2 77.76(12) . . ? C30 C40 C50 136.4(3) . . ? C30 C40 Co1 69.8(2) . . ? C50 C40 Co1 138.9(3) . . ? C30 C40 Co2 69.6(2) . . ? C50 C40 Co2 134.9(3) . . ? Co1 C40 Co2 78.08(12) . . ? C60 C50 C40 145.3(4) . . ? C60 C50 Co4 66.4(3) . . ? C40 C50 Co4 137.9(3) . . ? C60 C50 Co3 69.3(2) . . ? C40 C50 Co3 130.8(2) . . ? Co4 C50 Co3 77.36(14) . . ? C60 C50 Co4' 78.1(3) . . ? C40 C50 Co4' 129.4(3) . . ? Co3 C50 Co4' 77.01(17) . . ? C50 C60 Co4 72.2(3) . . ? C50 C60 Si2' 143.6(4) . . ? Co4 C60 Si2' 108.7(3) . . ? C50 C60 Si2 147.8(3) . . ? Co4 C60 Si2 135.0(3) . . ? C50 C60 Co3 70.9(2) . . ? Co4 C60 Co3 79.55(18) . . ? Si2' C60 Co3 145.5(3) . . ? Si2 C60 Co3 123.6(3) . . ? C50 C60 Co4' 66.6(3) . . ? Si2' C60 Co4' 115.6(3) . . ? Si2 C60 Co4' 141.6(3) . . ? Co3 C60 Co4' 74.10(19) . . ? C202 Si2 C203 109.2(6) . . ? C202 Si2 C201 112.9(7) . . ? C203 Si2 C201 110.2(8) . . ? C202 Si2 C60 107.1(4) . . ? C203 Si2 C60 113.0(4) . . ? C201 Si2 C60 104.5(7) . . ? C206 Si2' C205 117.2(15) . . ? C206 Si2' C60 108.7(16) . . ? C205 Si2' C60 117.9(7) . . ? C206 Si2' C204 97.7(17) . . ? C205 Si2' C204 109.5(10) . . ? C60 Si2' C204 102.9(8) . . ? Si2' C204 H20J 109.5 . . ? Si2' C204 H20K 109.5 . . ? H20J C204 H20K 109.5 . . ? Si2' C204 H20L 109.5 . . ? H20J C204 H20L 109.5 . . ? H20K C204 H20L 109.5 . . ? Si2' C205 H20M 109.5 . . ? Si2' C205 H20N 109.5 . . ? H20M C205 H20N 109.5 . . ? Si2' C205 H20O 109.5 . . ? H20M C205 H20O 109.5 . . ? H20N C205 H20O 109.5 . . ? Si2' C206 H20P 109.4 . . ? Si2' C206 H20Q 109.5 . . ? H20P C206 H20Q 109.5 . . ? Si2' C206 H20R 109.5 . . ? H20P C206 H20R 109.5 . . ? H20Q C206 H20R 109.5 . . ?