Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' #========================================================================== # 2. Processing Summary (IUCr Office Use Only) _journal_coden_Cambridge 0222 #============================================================================== _audit_creation_date ? _audit_creation_method SHELXL-97 _audit_update_record ; ? ; #========================================================================== # 1. Submission Details _publ_contact_author_name 'Thomas Baumgartner' _publ_contact_author_address ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; _publ_contact_author_email thomas.baumgartner@ac.rwth-aachen.de _publ_contact_author_fax 0049-241-8092644 _publ_contact_author_phone 0049-241-8099684 _publ_requested_category 'Full paper' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #========================================================================== # 3. Title and Author List _publ_section_title ; Synthesis and optoelectronic properties of transition metal complexes incorporating dithieno[3,2-b:2',3'-d]phosphole ligands ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' Y.Dienes ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; M.Eggenstein ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; T.Neumann ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; U.Englert ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; T.Baumgartner ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; #========================================================================== # Attachment 'CCDC276963.CIF' data_S2PW _database_code_depnum_ccdc_archive 'CCDC 276963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common S2PW _chemical_melting_point ? _chemical_formula_moiety 'C57 H58 O10 P2 S4 Si4 W2' _chemical_formula_sum 'C57 H58 O10 P2 S4 Si4 W2' _chemical_formula_weight 1573.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1535(4) _cell_length_b 11.5231(4) _cell_length_c 14.0934(6) _cell_angle_alpha 85.3590(10) _cell_angle_beta 67.8200(10) _cell_angle_gamma 72.7510(10) _cell_volume 1600.87(11) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8006 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 29.96 _exptl_crystal_description irreg _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 778 _exptl_absorpt_coefficient_mu 3.898 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 00.2137 _exptl_absorpt_correction_T_max 0.5569 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28162 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 30.05 _reflns_number_total 9031 _reflns_number_gt 8604 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+0.5704P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9031 _refine_ls_number_parameters 378 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0236 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.415679(8) 0.741424(7) 0.048994(6) 0.01308(3) Uani 1 1 d . . . S1 S 0.51529(5) 1.05023(5) 0.30605(4) 0.01828(11) Uani 1 1 d . . . S2 S 0.20748(5) 1.22621(5) 0.23972(4) 0.01476(10) Uani 1 1 d . . . P1 P 0.31143(5) 0.84332(5) 0.22327(4) 0.01216(10) Uani 1 1 d . . . Si1 Si 0.76268(6) 0.85946(6) 0.34172(5) 0.02110(13) Uani 1 1 d . . . Si2 Si -0.02445(6) 1.31245(5) 0.15053(5) 0.01775(12) Uani 1 1 d . . . O1 O 0.21157(18) 0.58252(17) 0.09216(14) 0.0274(4) Uani 1 1 d . . . O2 O 0.61808(18) 0.54353(16) 0.13072(15) 0.0268(4) Uani 1 1 d . . . O3 O 0.62324(17) 0.89724(15) 0.00243(14) 0.0236(3) Uani 1 1 d . . . O4 O 0.2185(2) 0.95347(16) -0.02858(15) 0.0291(4) Uani 1 1 d . . . O5 O 0.56229(19) 0.62550(17) -0.17534(13) 0.0296(4) Uani 1 1 d . . . C1 C 0.6063(2) 0.8996(2) 0.31029(18) 0.0192(4) Uani 1 1 d . . . C2 C 0.5473(2) 0.8229(2) 0.28626(17) 0.0177(4) Uani 1 1 d . . . H2A H 0.5822 0.7368 0.2836 0.015(6) Uiso 1 1 d R . . C3 C 0.4293(2) 0.88438(19) 0.26591(16) 0.0141(4) Uani 1 1 d . . . C4 C 0.4002(2) 1.00883(19) 0.27363(16) 0.0141(4) Uani 1 1 d . . . C5 C 0.2812(2) 1.07584(18) 0.25214(15) 0.0136(4) Uani 1 1 d . . . C6 C 0.2162(2) 1.00278(18) 0.22973(15) 0.0130(4) Uani 1 1 d . . . C7 C 0.1062(2) 1.07089(19) 0.20265(16) 0.0148(4) Uani 1 1 d . . . H7A H 0.0510 1.0347 0.1847 0.017(6) Uiso 1 1 d R . . C8 C 0.0869(2) 1.19418(19) 0.20424(16) 0.0149(4) Uani 1 1 d . . . C11 C 0.9133(3) 0.8219(3) 0.2203(2) 0.0328(6) Uani 1 1 d . . . H11D H 0.9105 0.8912 0.1756 0.045(10) Uiso 1 1 d R . . H11E H 0.9135 0.7517 0.1858 0.038(9) Uiso 1 1 d R . . H11F H 0.9953 0.8028 0.2356 0.042(9) Uiso 1 1 d R . . C12 C 0.7628(3) 0.9930(2) 0.4079(2) 0.0305(6) Uani 1 1 d . . . H12D H 0.7629 1.0621 0.3625 0.045(10) Uiso 1 1 d R . . H12E H 0.8437 0.9725 0.4252 0.042(9) Uiso 1 1 d R . . H12F H 0.6820 1.0146 0.4708 0.056(11) Uiso 1 1 d R . . C13 C 0.7603(3) 0.7274(2) 0.4267(2) 0.0328(6) Uani 1 1 d . . . H13D H 0.8413 0.7047 0.4439 0.058(11) Uiso 1 1 d R . . H13E H 0.7587 0.6585 0.3911 0.049(10) Uiso 1 1 d R . . H13F H 0.6795 0.7490 0.4897 0.057(11) Uiso 1 1 d R . . C21 C -0.1035(3) 1.4535(2) 0.2328(2) 0.0260(5) Uani 1 1 d . . . H21D H -0.1609 1.4362 0.3012 0.044(9) Uiso 1 1 d R . . H21E H -0.1586 1.5154 0.2023 0.038(9) Uiso 1 1 d R . . H21F H -0.0327 1.4836 0.2380 0.039(9) Uiso 1 1 d R . . C22 C 0.0860(3) 1.3413(2) 0.01895(19) 0.0309(6) Uani 1 1 d . . . H22D H 0.1271 1.2657 -0.0229 0.057(11) Uiso 1 1 d R . . H22E H 0.1573 1.3714 0.0234 0.043(9) Uiso 1 1 d R . . H22F H 0.0317 1.4024 -0.0126 0.050(10) Uiso 1 1 d R . . C23 C -0.1508(3) 1.2437(2) 0.1418(3) 0.0351(6) Uani 1 1 d . . . H23D H -0.2058 1.2251 0.2106 0.042(9) Uiso 1 1 d R . . H23E H -0.1043 1.1689 0.0992 0.060(11) Uiso 1 1 d R . . H23F H -0.2092 1.3012 0.1112 0.053(10) Uiso 1 1 d R . . C31 C 0.2112(2) 0.77435(19) 0.33430(16) 0.0146(4) Uani 1 1 d . . . C32 C 0.1334(2) 0.8413(2) 0.42626(17) 0.0206(4) Uani 1 1 d . . . H32A H 0.1281 0.9247 0.4305 0.018(7) Uiso 1 1 d R . . C33 C 0.0634(3) 0.7865(2) 0.51197(18) 0.0253(5) Uani 1 1 d . . . H33B H 0.0104 0.8321 0.5745 0.038(9) Uiso 1 1 d R . . C34 C 0.0712(2) 0.6647(2) 0.50636(18) 0.0245(5) Uani 1 1 d . . . H34A H 0.0236 0.6271 0.5652 0.027(7) Uiso 1 1 d R . . C35 C 0.1478(2) 0.5981(2) 0.41558(19) 0.0232(5) Uani 1 1 d . . . H35A H 0.1529 0.5146 0.4119 0.034(8) Uiso 1 1 d R . . C36 C 0.2175(2) 0.6525(2) 0.32948(17) 0.0190(4) Uani 1 1 d . . . H36B H 0.2695 0.6064 0.2670 0.020(7) Uiso 1 1 d R . . C41 C 0.2840(2) 0.6401(2) 0.07856(17) 0.0184(4) Uani 1 1 d . . . C42 C 0.5438(2) 0.6125(2) 0.10129(17) 0.0179(4) Uani 1 1 d . . . C43 C 0.5485(2) 0.8422(2) 0.01805(16) 0.0172(4) Uani 1 1 d . . . C44 C 0.2889(2) 0.8777(2) -0.00083(18) 0.0202(4) Uani 1 1 d . . . C45 C 0.5090(2) 0.6669(2) -0.09377(18) 0.0203(4) Uani 1 1 d . . . C3T C 0.5735(9) 0.3378(8) 0.4154(7) 0.046(2) Uiso 0.50 1 d PD A -1 H3TA H 0.6113 0.2671 0.3743 0.055 Uiso 0.50 1 calc PR A -1 C2T C 0.4993(7) 0.4609(6) 0.3838(5) 0.0437(14) Uiso 0.50 1 d PD A -1 H2TA H 0.4843 0.4656 0.3228 0.052 Uiso 0.50 1 calc PR A -1 C1T C 0.4531(8) 0.5684(7) 0.4476(6) 0.0326(19) Uiso 0.50 1 d PD A -1 H1TA H 0.4134 0.6438 0.4269 0.039 Uiso 0.50 1 calc PR A -1 C4T C 0.5773(7) 0.3439(6) 0.5061(5) 0.0459(15) Uiso 0.50 1 d PD A -1 H4TA H 0.6150 0.2711 0.5315 0.055 Uiso 0.50 1 calc PR A -1 C7T C 0.4372(12) 0.6483(10) 0.6094(9) 0.067(3) Uiso 0.50 1 d P A -1 H7TA H 0.3898 0.7240 0.5892 0.101 Uiso 0.50 1 calc PR A -1 H7TB H 0.5190 0.6556 0.6130 0.101 Uiso 0.50 1 calc PR A -1 H7TD H 0.3811 0.6285 0.6755 0.101 Uiso 0.50 1 calc PR A -1 C5T C 0.5297(8) 0.4508(7) 0.5712(6) 0.034(2) Uiso 0.50 1 d PD A -1 H5TA H 0.5403 0.4471 0.6338 0.041 Uiso 0.50 1 calc PR A -1 C6T C 0.4688(6) 0.5569(5) 0.5379(4) 0.0361(12) Uiso 0.50 1 d PD A -1 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 W1 0.01489(5) 0.01138(5) 0.01375(5) -0.00101(3) -0.00501(3) -0.00492(3) S1 0.0170(2) 0.0155(2) 0.0264(3) -0.0031(2) -0.0118(2) -0.00453(19) S2 0.0156(2) 0.0116(2) 0.0178(2) -0.00018(18) -0.00665(19) -0.00426(18) P1 0.0126(2) 0.0110(2) 0.0139(2) -0.00025(18) -0.00588(19) -0.00350(18) Si1 0.0179(3) 0.0202(3) 0.0296(3) -0.0039(3) -0.0147(3) -0.0027(2) Si2 0.0204(3) 0.0125(3) 0.0230(3) 0.0009(2) -0.0125(2) -0.0026(2) O1 0.0247(9) 0.0296(9) 0.0306(9) -0.0025(7) -0.0072(7) -0.0149(8) O2 0.0248(9) 0.0201(8) 0.0374(10) 0.0027(7) -0.0165(8) -0.0030(7) O3 0.0216(8) 0.0208(8) 0.0276(9) -0.0007(7) -0.0041(7) -0.0110(7) O4 0.0385(10) 0.0204(9) 0.0394(11) 0.0028(8) -0.0279(9) -0.0069(8) O5 0.0366(10) 0.0335(10) 0.0195(8) -0.0068(7) -0.0015(7) -0.0208(8) C1 0.0164(10) 0.0184(10) 0.0243(11) -0.0012(8) -0.0102(9) -0.0031(8) C2 0.0170(10) 0.0138(10) 0.0232(11) -0.0026(8) -0.0103(8) -0.0015(8) C3 0.0138(9) 0.0149(9) 0.0146(9) 0.0004(7) -0.0063(7) -0.0043(7) C4 0.0126(9) 0.0155(10) 0.0156(9) -0.0018(7) -0.0060(7) -0.0047(7) C5 0.0154(9) 0.0114(9) 0.0141(9) -0.0003(7) -0.0053(7) -0.0043(7) C6 0.0140(9) 0.0108(9) 0.0144(9) 0.0001(7) -0.0055(7) -0.0037(7) C7 0.0151(9) 0.0153(10) 0.0159(9) 0.0008(8) -0.0065(8) -0.0061(8) C8 0.0142(9) 0.0134(9) 0.0174(10) 0.0004(7) -0.0068(8) -0.0032(7) C11 0.0201(12) 0.0396(15) 0.0402(15) -0.0086(12) -0.0130(11) -0.0057(11) C12 0.0312(14) 0.0266(13) 0.0411(15) -0.0063(11) -0.0213(12) -0.0070(11) C13 0.0311(14) 0.0285(14) 0.0455(16) 0.0039(12) -0.0243(13) -0.0057(11) C21 0.0276(12) 0.0180(11) 0.0316(13) -0.0037(9) -0.0142(10) 0.0000(9) C22 0.0391(15) 0.0257(13) 0.0243(12) 0.0055(10) -0.0127(11) -0.0040(11) C23 0.0357(15) 0.0264(13) 0.0582(19) 0.0047(13) -0.0341(14) -0.0096(11) C31 0.0149(9) 0.0144(9) 0.0165(9) 0.0023(7) -0.0078(8) -0.0048(8) C32 0.0220(11) 0.0190(11) 0.0197(11) -0.0004(8) -0.0057(9) -0.0067(9) C33 0.0266(12) 0.0273(12) 0.0176(11) -0.0003(9) -0.0020(9) -0.0093(10) C34 0.0270(12) 0.0294(13) 0.0202(11) 0.0075(9) -0.0082(9) -0.0150(10) C35 0.0292(12) 0.0186(11) 0.0253(12) 0.0061(9) -0.0113(10) -0.0116(9) C36 0.0254(11) 0.0163(10) 0.0167(10) 0.0004(8) -0.0089(9) -0.0064(9) C41 0.0198(10) 0.0179(10) 0.0172(10) -0.0027(8) -0.0065(8) -0.0047(8) C42 0.0182(10) 0.0135(10) 0.0211(10) -0.0028(8) -0.0034(8) -0.0073(8) C43 0.0200(10) 0.0146(10) 0.0145(9) -0.0026(8) -0.0046(8) -0.0030(8) C44 0.0263(11) 0.0187(11) 0.0200(11) -0.0023(8) -0.0095(9) -0.0110(9) C45 0.0234(11) 0.0165(10) 0.0233(11) 0.0006(8) -0.0069(9) -0.0112(9) _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 W1 C45 2.009(2) . ? W1 C42 2.037(2) . ? W1 C41 2.043(2) . ? W1 C43 2.046(2) . ? W1 C44 2.053(2) . ? W1 P1 2.5028(5) . ? S1 C4 1.710(2) . ? S1 C1 1.741(2) . ? S2 C5 1.710(2) . ? S2 C8 1.740(2) . ? P1 C6 1.819(2) . ? P1 C3 1.824(2) . ? P1 C31 1.826(2) . ? Si1 C11 1.859(3) . ? Si1 C13 1.859(3) . ? Si1 C12 1.863(3) . ? Si1 C1 1.877(2) . ? Si2 C23 1.853(3) . ? Si2 C21 1.856(2) . ? Si2 C22 1.867(3) . ? Si2 C8 1.874(2) . ? O1 C41 1.144(3) . ? O2 C42 1.143(3) . ? O3 C43 1.139(3) . ? O4 C44 1.141(3) . ? O5 C45 1.143(3) . ? C1 C2 1.375(3) . ? C2 C3 1.420(3) . ? C2 H2A 0.9500 . ? C3 C4 1.377(3) . ? C4 C5 1.452(3) . ? C5 C6 1.383(3) . ? C6 C7 1.414(3) . ? C7 C8 1.373(3) . ? C7 H7A 0.9505 . ? C11 H11D 0.9769 . ? C11 H11E 0.9767 . ? C11 H11F 0.9768 . ? C12 H12D 0.9800 . ? C12 H12E 0.9801 . ? C12 H12F 0.9799 . ? C13 H13D 0.9797 . ? C13 H13E 0.9803 . ? C13 H13F 0.9799 . ? C21 H21D 0.9792 . ? C21 H21E 0.9800 . ? C21 H21F 0.9798 . ? C22 H22D 0.9790 . ? C22 H22E 0.9804 . ? C22 H22F 0.9794 . ? C23 H23D 0.9789 . ? C23 H23E 0.9784 . ? C23 H23F 0.9789 . ? C31 C36 1.390(3) . ? C31 C32 1.394(3) . ? C32 C33 1.388(3) . ? C32 H32A 0.9497 . ? C33 C34 1.387(3) . ? C33 H33B 0.9481 . ? C34 C35 1.379(3) . ? C34 H34A 0.9496 . ? C35 C36 1.387(3) . ? C35 H35A 0.9505 . ? C36 H36B 0.9492 . ? C3T C4T 1.302(9) . ? C3T C2T 1.541(9) . ? C3T H3TA 0.9300 . ? C2T C1T 1.435(8) . ? C2T H2TA 0.9300 . ? C1T C6T 1.340(8) . ? C1T H1TA 0.9300 . ? C4T C5T 1.439(9) . ? C4T H4TA 0.9300 . ? C7T C6T 1.391(12) . ? C7T H7TA 0.9600 . ? C7T H7TB 0.9600 . ? C7T H7TD 0.9600 . ? C5T C6T 1.353(8) . ? C5T H5TA 0.9300 . ? 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 C45 W1 C42 92.08(9) . . ? C45 W1 C41 88.74(9) . . ? C42 W1 C41 92.87(9) . . ? C45 W1 C43 90.73(9) . . ? C42 W1 C43 87.12(9) . . ? C41 W1 C43 179.47(8) . . ? C45 W1 C44 89.59(9) . . ? C42 W1 C44 177.17(8) . . ? C41 W1 C44 89.44(9) . . ? C43 W1 C44 90.58(9) . . ? C45 W1 P1 175.80(6) . . ? C42 W1 P1 87.86(6) . . ? C41 W1 P1 95.46(6) . . ? C43 W1 P1 85.07(6) . . ? C44 W1 P1 90.31(6) . . ? C4 S1 C1 92.47(10) . . ? C5 S2 C8 92.53(10) . . ? C6 P1 C3 90.14(9) . . ? C6 P1 C31 106.21(9) . . ? C3 P1 C31 104.41(10) . . ? C6 P1 W1 115.52(7) . . ? C3 P1 W1 114.66(7) . . ? C31 P1 W1 121.11(7) . . ? C11 Si1 C13 111.10(14) . . ? C11 Si1 C12 109.35(13) . . ? C13 Si1 C12 110.50(13) . . ? C11 Si1 C1 108.73(11) . . ? C13 Si1 C1 108.18(12) . . ? C12 Si1 C1 108.92(11) . . ? C23 Si2 C21 112.64(13) . . ? C23 Si2 C22 109.52(14) . . ? C21 Si2 C22 111.03(12) . . ? C23 Si2 C8 106.41(11) . . ? C21 Si2 C8 110.45(11) . . ? C22 Si2 C8 106.52(11) . . ? C2 C1 S1 109.95(16) . . ? C2 C1 Si1 128.52(17) . . ? S1 C1 Si1 121.52(13) . . ? C1 C2 C3 113.7(2) . . ? C1 C2 H2A 123.1 . . ? C3 C2 H2A 123.2 . . ? C4 C3 C2 112.19(19) . . ? C4 C3 P1 110.63(15) . . ? C2 C3 P1 137.00(17) . . ? C3 C4 C5 114.23(18) . . ? C3 C4 S1 111.70(15) . . ? C5 C4 S1 134.07(16) . . ? C6 C5 C4 113.97(18) . . ? C6 C5 S2 111.38(15) . . ? C4 C5 S2 134.49(16) . . ? C5 C6 C7 112.32(18) . . ? C5 C6 P1 110.64(15) . . ? C7 C6 P1 136.14(16) . . ? C8 C7 C6 113.76(19) . . ? C8 C7 H7A 123.1 . . ? C6 C7 H7A 123.2 . . ? C7 C8 S2 110.01(15) . . ? C7 C8 Si2 126.85(16) . . ? S2 C8 Si2 121.93(12) . . ? Si1 C11 H11D 109.8 . . ? Si1 C11 H11E 109.4 . . ? H11D C11 H11E 109.4 . . ? Si1 C11 H11F 109.5 . . ? H11D C11 H11F 109.4 . . ? H11E C11 H11F 109.4 . . ? Si1 C12 H12D 109.5 . . ? Si1 C12 H12E 109.5 . . ? H12D C12 H12E 109.5 . . ? Si1 C12 H12F 109.5 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.4 . . ? Si1 C13 H13D 109.5 . . ? Si1 C13 H13E 109.3 . . ? H13D C13 H13E 109.5 . . ? Si1 C13 H13F 109.6 . . ? H13D C13 H13F 109.5 . . ? H13E C13 H13F 109.4 . . ? Si2 C21 H21D 109.6 . . ? Si2 C21 H21E 109.4 . . ? H21D C21 H21E 109.5 . . ? Si2 C21 H21F 109.5 . . ? H21D C21 H21F 109.5 . . ? H21E C21 H21F 109.4 . . ? Si2 C22 H22D 109.6 . . ? Si2 C22 H22E 109.3 . . ? H22D C22 H22E 109.5 . . ? Si2 C22 H22F 109.4 . . ? H22D C22 H22F 109.5 . . ? H22E C22 H22F 109.4 . . ? Si2 C23 H23D 109.4 . . ? Si2 C23 H23E 109.6 . . ? H23D C23 H23E 109.5 . . ? Si2 C23 H23F 109.4 . . ? H23D C23 H23F 109.4 . . ? H23E C23 H23F 109.5 . . ? C36 C31 C32 119.4(2) . . ? C36 C31 P1 120.18(16) . . ? C32 C31 P1 120.38(16) . . ? C33 C32 C31 120.1(2) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 120.1 . . ? C34 C33 C32 120.0(2) . . ? C34 C33 H33B 119.9 . . ? C32 C33 H33B 120.1 . . ? C35 C34 C33 120.1(2) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C36 120.1(2) . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 119.9 . . ? C35 C36 C31 120.3(2) . . ? C35 C36 H36B 119.8 . . ? C31 C36 H36B 119.9 . . ? O1 C41 W1 178.0(2) . . ? O2 C42 W1 177.33(19) . . ? O3 C43 W1 178.6(2) . . ? O4 C44 W1 180.0(3) . . ? O5 C45 W1 179.4(2) . . ? C4T C3T C2T 112.5(7) . . ? C4T C3T H3TA 123.8 . . ? C2T C3T H3TA 123.8 . . ? C1T C2T C3T 120.6(6) . . ? C1T C2T H2TA 119.7 . . ? C3T C2T H2TA 119.7 . . ? C6T C1T C2T 118.1(6) . . ? C6T C1T H1TA 121.0 . . ? C2T C1T H1TA 121.0 . . ? C3T C4T C5T 127.2(7) . . ? C3T C4T H4TA 116.4 . . ? C5T C4T H4TA 116.4 . . ? C6T C7T H7TA 109.5 . . ? C6T C7T H7TB 109.5 . . ? H7TA C7T H7TB 109.5 . . ? C6T C7T H7TD 109.5 . . ? H7TA C7T H7TD 109.5 . . ? H7TB C7T H7TD 109.5 . . ? C6T C5T C4T 117.5(7) . . ? C6T C5T H5TA 121.2 . . ? C4T C5T H5TA 121.2 . . ? C1T C6T C5T 124.0(6) . . ? C1T C6T C7T 127.9(7) . . ? C5T C6T C7T 107.9(7) . . ? _diffrn_measured_fraction_theta_max .963 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full .963 _refine_diff_density_max 1.462 _refine_diff_density_min -.789 _refine_diff_density_rms .114 data_s2pau _database_code_depnum_ccdc_archive 'CCDC 276964' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common S2PAu _chemical_melting_point ? _chemical_formula_moiety 'C26 H37 Au Cl P S2 Si2' _chemical_formula_sum 'C26 H37 Au Cl P S2 Si2' _chemical_formula_weight 733.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.279(3) _cell_length_b 13.492(3) _cell_length_c 14.313(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.33(3) _cell_angle_gamma 90.00 _cell_volume 3142.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6172 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 27.82 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 5.040 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4149 _exptl_absorpt_correction_T_max 0.6334 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25336 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.02 _reflns_number_total 7583 _reflns_number_gt 6650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+1.5770P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7583 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.024400(9) 0.524850(13) 0.194270(11) 0.01535(6) Uani 1 1 d . . . Cl1 Cl -0.08787(7) 0.47809(9) 0.27768(8) 0.0239(2) Uani 1 1 d . . . S1 S 0.37559(6) 0.57850(9) 0.20451(8) 0.0194(2) Uani 1 1 d . . . P1 P 0.12928(6) 0.57449(9) 0.10899(7) 0.0147(2) Uani 1 1 d . . . Si1 Si 0.38496(7) 0.74470(10) 0.36126(9) 0.0212(3) Uani 1 1 d . . . C1 C 0.3279(3) 0.6715(3) 0.2672(3) 0.0171(9) Uani 1 1 d . . . S2 S 0.31437(6) 0.38200(8) 0.01841(8) 0.0187(2) Uani 1 1 d . . . Si2 Si 0.22640(8) 0.23639(9) -0.12741(8) 0.0189(3) Uani 1 1 d . . . C2 C 0.2464(3) 0.6781(3) 0.2417(3) 0.0168(9) Uani 1 1 d . . . H2A H 0.2102 0.7229 0.2681 0.020 Uiso 1 1 calc R . . C3 C 0.2232(2) 0.6098(3) 0.1711(3) 0.0144(8) Uani 1 1 d . . . C4 C 0.2864(2) 0.5492(3) 0.1439(3) 0.0159(9) Uani 1 1 d . . . C5 C 0.2638(3) 0.4753(3) 0.0734(3) 0.0165(8) Uani 1 1 d . . . C6 C 0.1823(3) 0.4801(3) 0.0445(3) 0.0174(9) Uani 1 1 d . . . C7 C 0.1614(3) 0.4050(3) -0.0227(3) 0.0189(9) Uani 1 1 d . . . H7A H 0.1088 0.3971 -0.0484 0.023 Uiso 1 1 calc R . . C8 C 0.2265(3) 0.3456(3) -0.0453(3) 0.0182(9) Uani 1 1 d . . . C11 C 0.1014(2) 0.6753(3) 0.0305(3) 0.0151(8) Uani 1 1 d . . . C12 C 0.0884(3) 0.7696(3) 0.0674(3) 0.0217(10) Uani 1 1 d . . . H12A H 0.0973 0.7809 0.1309 0.026 Uiso 1 1 calc R . . C13 C 0.0625(3) 0.8464(4) 0.0100(3) 0.0274(11) Uani 1 1 d . . . H13A H 0.0555 0.9097 0.0344 0.033 Uiso 1 1 calc R . . C14 C 0.0469(3) 0.8285(4) -0.0850(3) 0.0271(11) Uani 1 1 d . . . H14A H 0.0278 0.8795 -0.1234 0.033 Uiso 1 1 calc R . . C15 C 0.0597(3) 0.7355(4) -0.1219(3) 0.0265(11) Uani 1 1 d . . . H15A H 0.0493 0.7243 -0.1852 0.032 Uiso 1 1 calc R . . C16 C 0.0881(3) 0.6582(4) -0.0651(3) 0.0209(9) Uani 1 1 d . . . H16A H 0.0980 0.5960 -0.0905 0.025 Uiso 1 1 calc R . . C21 C 0.3229(3) 0.7385(4) 0.4691(3) 0.0345(12) Uani 1 1 d . . . H21A H 0.3503 0.7749 0.5183 0.052 Uiso 1 1 calc R . . H21B H 0.3169 0.6706 0.4877 0.052 Uiso 1 1 calc R . . H21C H 0.2697 0.7669 0.4567 0.052 Uiso 1 1 calc R . . C22 C 0.4871(3) 0.6828(5) 0.3823(4) 0.0424(15) Uani 1 1 d . . . H22A H 0.5187 0.6864 0.3266 0.064 Uiso 1 1 calc R . . H22B H 0.4786 0.6146 0.3987 0.064 Uiso 1 1 calc R . . H22C H 0.5162 0.7158 0.4325 0.064 Uiso 1 1 calc R . . C23 C 0.3982(3) 0.8774(4) 0.3207(4) 0.0269(11) Uani 1 1 d . . . C24 C 0.4496(3) 0.9336(4) 0.3952(4) 0.0383(14) Uani 1 1 d . . . H24A H 0.4569 1.0010 0.3756 0.057 Uiso 1 1 calc R . . H24B H 0.5023 0.9023 0.4030 0.057 Uiso 1 1 calc R . . H24C H 0.4216 0.9326 0.4535 0.057 Uiso 1 1 calc R . . C25 C 0.3137(3) 0.9290(4) 0.3089(5) 0.0403(14) Uani 1 1 d . . . H25A H 0.3214 0.9959 0.2882 0.060 Uiso 1 1 calc R . . H25B H 0.2865 0.9293 0.3677 0.060 Uiso 1 1 calc R . . H25C H 0.2807 0.8937 0.2635 0.060 Uiso 1 1 calc R . . C26 C 0.4431(4) 0.8806(5) 0.2267(4) 0.0461(15) Uani 1 1 d . . . H26A H 0.4493 0.9482 0.2073 0.069 Uiso 1 1 calc R . . H26B H 0.4116 0.8450 0.1802 0.069 Uiso 1 1 calc R . . H26C H 0.4963 0.8506 0.2343 0.069 Uiso 1 1 calc R . . C31 C 0.1275(3) 0.2401(4) -0.1957(4) 0.0311(12) Uani 1 1 d . . . H31A H 0.1254 0.1853 -0.2386 0.047 Uiso 1 1 calc R . . H31B H 0.1239 0.3012 -0.2300 0.047 Uiso 1 1 calc R . . H31C H 0.0825 0.2356 -0.1538 0.047 Uiso 1 1 calc R . . C32 C 0.3149(3) 0.2488(4) -0.2076(4) 0.0389(14) Uani 1 1 d . . . H32A H 0.3155 0.1933 -0.2496 0.058 Uiso 1 1 calc R . . H32B H 0.3654 0.2503 -0.1716 0.058 Uiso 1 1 calc R . . H32C H 0.3094 0.3090 -0.2429 0.058 Uiso 1 1 calc R . . C33 C 0.2354(3) 0.1193(4) -0.0551(3) 0.0254(10) Uani 1 1 d . . . C34 C 0.2125(4) 0.0307(4) -0.1166(4) 0.0352(13) Uani 1 1 d . . . H34A H 0.2166 -0.0291 -0.0805 0.053 Uiso 1 1 calc R . . H34B H 0.2492 0.0271 -0.1680 0.053 Uiso 1 1 calc R . . H34C H 0.1571 0.0384 -0.1401 0.053 Uiso 1 1 calc R . . C35 C 0.3241(4) 0.1043(4) -0.0176(5) 0.0496(17) Uani 1 1 d . . . H35A H 0.3270 0.0448 0.0191 0.074 Uiso 1 1 calc R . . H35B H 0.3400 0.1599 0.0206 0.074 Uiso 1 1 calc R . . H35C H 0.3606 0.0988 -0.0691 0.074 Uiso 1 1 calc R . . C36 C 0.1777(4) 0.1237(5) 0.0278(4) 0.0460(15) Uani 1 1 d . . . H36A H 0.1829 0.0639 0.0637 0.069 Uiso 1 1 calc R . . H36B H 0.1220 0.1306 0.0051 0.069 Uiso 1 1 calc R . . H36C H 0.1919 0.1795 0.0665 0.069 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 0.01770(9) 0.01500(10) 0.01324(9) -0.00078(7) -0.00196(6) -0.00115(6) Cl1 0.0292(5) 0.0254(6) 0.0174(5) -0.0015(5) 0.0054(4) -0.0087(5) S1 0.0152(5) 0.0189(6) 0.0240(6) -0.0068(5) -0.0039(4) 0.0020(4) P1 0.0157(5) 0.0138(6) 0.0143(5) -0.0020(4) -0.0030(4) 0.0006(4) Si1 0.0181(6) 0.0202(7) 0.0248(7) -0.0088(5) -0.0067(5) 0.0010(5) C1 0.021(2) 0.014(2) 0.017(2) -0.0016(17) 0.0002(17) 0.0002(17) S2 0.0182(5) 0.0156(5) 0.0223(6) -0.0057(4) -0.0014(4) 0.0012(4) Si2 0.0240(6) 0.0159(6) 0.0168(6) -0.0055(5) 0.0001(5) -0.0013(5) C2 0.021(2) 0.014(2) 0.015(2) -0.0002(17) 0.0000(16) 0.0001(17) C3 0.0163(19) 0.015(2) 0.0121(19) -0.0009(16) -0.0023(15) 0.0000(16) C4 0.0137(18) 0.016(2) 0.017(2) 0.0003(17) -0.0017(16) -0.0001(16) C5 0.019(2) 0.014(2) 0.016(2) -0.0006(17) -0.0013(16) 0.0003(17) C6 0.020(2) 0.014(2) 0.018(2) -0.0003(18) -0.0009(17) 0.0033(17) C7 0.019(2) 0.020(2) 0.017(2) -0.0019(18) -0.0035(17) 0.0004(17) C8 0.024(2) 0.015(2) 0.016(2) -0.0049(17) -0.0012(17) -0.0009(17) C11 0.0135(18) 0.019(2) 0.013(2) 0.0037(17) -0.0002(15) -0.0024(16) C12 0.032(2) 0.018(2) 0.015(2) 0.0005(18) 0.0003(18) 0.0068(19) C13 0.042(3) 0.019(3) 0.022(2) 0.000(2) 0.000(2) 0.006(2) C14 0.036(3) 0.023(3) 0.022(2) 0.011(2) -0.002(2) 0.004(2) C15 0.030(2) 0.034(3) 0.015(2) 0.004(2) -0.0041(19) -0.001(2) C16 0.024(2) 0.022(2) 0.016(2) 0.0005(19) -0.0020(17) -0.0027(19) C21 0.042(3) 0.038(3) 0.023(3) -0.009(2) -0.003(2) -0.006(2) C22 0.028(3) 0.041(4) 0.057(4) -0.022(3) -0.020(3) 0.011(2) C23 0.023(2) 0.023(3) 0.034(3) -0.011(2) -0.005(2) -0.002(2) C24 0.028(3) 0.034(3) 0.053(4) -0.019(3) -0.004(2) -0.006(2) C25 0.037(3) 0.021(3) 0.062(4) -0.002(3) -0.015(3) -0.001(2) C26 0.054(4) 0.039(4) 0.045(4) -0.007(3) 0.011(3) -0.014(3) C31 0.041(3) 0.022(3) 0.029(3) -0.005(2) -0.015(2) 0.001(2) C32 0.045(3) 0.034(3) 0.039(3) -0.015(3) 0.016(3) -0.007(3) C33 0.030(2) 0.019(2) 0.027(3) 0.001(2) -0.006(2) -0.001(2) C34 0.050(3) 0.018(3) 0.037(3) -0.005(2) -0.010(3) -0.001(2) C35 0.051(4) 0.026(3) 0.071(5) 0.008(3) -0.025(3) 0.003(3) C36 0.070(4) 0.033(3) 0.036(3) 0.004(3) 0.013(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2249(12) . ? Au1 Cl1 2.2946(12) . ? S1 C4 1.719(4) . ? S1 C1 1.737(4) . ? P1 C6 1.803(4) . ? P1 C3 1.814(4) . ? P1 C11 1.815(4) . ? Si1 C21 1.865(5) . ? Si1 C22 1.879(5) . ? Si1 C1 1.896(4) . ? Si1 C23 1.896(6) . ? C1 C2 1.370(6) . ? S2 C5 1.707(4) . ? S2 C8 1.749(4) . ? Si2 C31 1.864(5) . ? Si2 C32 1.871(5) . ? Si2 C8 1.885(4) . ? Si2 C33 1.893(5) . ? C2 C3 1.412(6) . ? C2 H2A 0.9300 . ? C3 C4 1.378(6) . ? C4 C5 1.460(6) . ? C5 C6 1.382(6) . ? C6 C7 1.433(6) . ? C7 C8 1.373(6) . ? C7 H7A 0.9300 . ? C11 C12 1.397(6) . ? C11 C16 1.399(6) . ? C12 C13 1.382(6) . ? C12 H12A 0.9300 . ? C13 C14 1.398(7) . ? C13 H13A 0.9300 . ? C14 C15 1.379(7) . ? C14 H14A 0.9300 . ? C15 C16 1.395(6) . ? C15 H15A 0.9300 . ? C16 H16A 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.539(7) . ? C23 C26 1.547(7) . ? C23 C25 1.548(7) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 C34 1.526(7) . ? C33 C36 1.532(7) . ? C33 C35 1.541(7) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? 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 P1 Au1 Cl1 177.26(4) . . ? C4 S1 C1 92.5(2) . . ? C6 P1 C3 91.6(2) . . ? C6 P1 C11 109.1(2) . . ? C3 P1 C11 107.60(19) . . ? C6 P1 Au1 116.78(15) . . ? C3 P1 Au1 117.31(14) . . ? C11 P1 Au1 112.42(13) . . ? C21 Si1 C22 110.0(3) . . ? C21 Si1 C1 107.4(2) . . ? C22 Si1 C1 107.5(2) . . ? C21 Si1 C23 111.3(2) . . ? C22 Si1 C23 111.2(3) . . ? C1 Si1 C23 109.4(2) . . ? C2 C1 S1 110.6(3) . . ? C2 C1 Si1 127.7(3) . . ? S1 C1 Si1 121.7(2) . . ? C5 S2 C8 92.9(2) . . ? C31 Si2 C32 110.1(3) . . ? C31 Si2 C8 107.1(2) . . ? C32 Si2 C8 108.9(2) . . ? C31 Si2 C33 111.4(2) . . ? C32 Si2 C33 111.0(3) . . ? C8 Si2 C33 108.2(2) . . ? C1 C2 C3 112.9(4) . . ? C1 C2 H2A 123.5 . . ? C3 C2 H2A 123.5 . . ? C4 C3 C2 113.6(4) . . ? C4 C3 P1 109.4(3) . . ? C2 C3 P1 136.9(3) . . ? C3 C4 C5 115.0(4) . . ? C3 C4 S1 110.4(3) . . ? C5 C4 S1 134.6(3) . . ? C6 C5 C4 113.6(4) . . ? C6 C5 S2 111.5(3) . . ? C4 C5 S2 134.9(3) . . ? C5 C6 C7 112.2(4) . . ? C5 C6 P1 110.3(3) . . ? C7 C6 P1 137.2(3) . . ? C8 C7 C6 113.5(4) . . ? C8 C7 H7A 123.3 . . ? C6 C7 H7A 123.3 . . ? C7 C8 S2 109.9(3) . . ? C7 C8 Si2 127.8(3) . . ? S2 C8 Si2 122.2(2) . . ? C12 C11 C16 119.9(4) . . ? C12 C11 P1 119.1(3) . . ? C16 C11 P1 120.9(4) . . ? C13 C12 C11 120.4(4) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C14 119.6(5) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C15 C14 C13 120.3(4) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 120.5(4) . . ? C14 C15 H15A 119.7 . . ? C16 C15 H15A 119.7 . . ? C15 C16 C11 119.2(4) . . ? C15 C16 H16A 120.4 . . ? C11 C16 H16A 120.4 . . ? Si1 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C26 109.2(4) . . ? C24 C23 C25 108.8(4) . . ? C26 C23 C25 109.2(5) . . ? C24 C23 Si1 108.5(4) . . ? C26 C23 Si1 110.6(4) . . ? C25 C23 Si1 110.5(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C31 H31A 109.5 . . ? Si2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si2 C32 H32A 109.5 . . ? Si2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C36 109.3(5) . . ? C34 C33 C35 108.3(4) . . ? C36 C33 C35 108.8(5) . . ? C34 C33 Si2 108.9(3) . . ? C36 C33 Si2 110.4(4) . . ? C35 C33 Si2 111.1(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.473 _refine_diff_density_min -1.376 _refine_diff_density_rms 0.203 # Attachment 'CCDC276965.CIF' #========================================================================== data_s2p2w _database_code_depnum_ccdc_archive 'CCDC 276965' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common S2P2W _chemical_melting_point ? _chemical_formula_moiety 'C32 H18 O4 P2 S4 W' _chemical_formula_sum 'C32 H18 O4 P2 S4 W' _chemical_formula_weight 840.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.179(2) _cell_length_b 14.844(3) _cell_length_c 18.518(4) _cell_angle_alpha 94.93(3) _cell_angle_beta 95.76(3) _cell_angle_gamma 94.64(3) _cell_volume 3033.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 986 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 28.36 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 4.227 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1879 _exptl_absorpt_correction_T_max 0.3470 _exptl_absorpt_process_details 'SADABS (1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47437 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 28.47 _reflns_number_total 15170 _reflns_number_gt 13222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+0.0163P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15170 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0811 _refine_ls_wR_factor_gt 0.0781 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.103594(11) 0.304133(8) 0.458100(7) 0.01266(4) Uani 1 1 d . . . W2 W 0.907549(11) 0.167546(8) 1.106392(7) 0.01237(4) Uani 1 1 d . . . P1 P 0.14586(7) 0.29943(5) 0.59278(5) 0.01348(16) Uani 1 1 d . . . P2 P 0.26802(8) 0.20716(5) 0.42821(5) 0.01428(17) Uani 1 1 d . . . P3 P 0.74593(8) 0.25407(5) 1.15222(5) 0.01335(16) Uani 1 1 d . . . P4 P 0.85773(7) 0.21337(5) 0.98257(5) 0.01271(16) Uani 1 1 d . . . S1 S 0.48233(8) 0.35852(6) 0.72172(5) 0.02223(19) Uani 1 1 d . . . S2 S 0.35110(7) 0.10855(5) 0.69373(5) 0.01705(17) Uani 1 1 d . . . S3 S 0.31484(9) 0.15948(7) 0.20509(5) 0.0271(2) Uani 1 1 d . . . S4 S 0.20538(8) -0.04507(6) 0.29956(5) 0.02462(19) Uani 1 1 d . . . S5 S 0.52608(8) 0.19147(6) 0.84797(5) 0.02317(19) Uani 1 1 d . . . S6 S 0.66907(8) 0.43143(5) 0.91008(5) 0.01912(17) Uani 1 1 d . . . S7 S 0.66615(8) 0.52371(6) 1.12690(5) 0.02162(18) Uani 1 1 d . . . S8 S 0.43101(8) 0.33344(6) 1.03710(5) 0.02069(18) Uani 1 1 d . . . O1 O 0.2966(2) 0.47379(17) 0.45985(16) 0.0291(6) Uani 1 1 d . . . O2 O -0.0732(2) 0.12452(17) 0.45251(15) 0.0284(6) Uani 1 1 d . . . O3 O -0.1121(2) 0.42596(16) 0.46752(15) 0.0265(6) Uani 1 1 d . . . O4 O 0.0411(2) 0.31980(16) 0.29122(14) 0.0252(6) Uani 1 1 d . . . O5 O 1.0990(2) 0.34089(17) 1.13260(14) 0.0281(6) Uani 1 1 d . . . O6 O 0.7116(2) -0.00262(16) 1.07252(15) 0.0257(6) Uani 1 1 d . . . O7 O 1.1156(2) 0.05980(17) 1.04809(14) 0.0255(6) Uani 1 1 d . . . O8 O 0.9726(2) 0.11021(16) 1.26514(13) 0.0249(6) Uani 1 1 d . . . C1 C 0.2264(3) 0.4143(2) 0.46090(19) 0.0180(7) Uani 1 1 d . . . C2 C -0.0108(3) 0.1888(2) 0.45444(19) 0.0179(7) Uani 1 1 d . . . C3 C -0.0317(3) 0.3816(2) 0.46779(19) 0.0183(7) Uani 1 1 d . . . C4 C 0.0651(3) 0.3111(2) 0.35105(19) 0.0163(7) Uani 1 1 d . . . C5 C 1.0296(3) 0.2794(2) 1.12502(18) 0.0168(7) Uani 1 1 d . . . C6 C 0.7831(3) 0.0578(2) 1.08410(18) 0.0160(7) Uani 1 1 d . . . C7 C 1.0377(3) 0.0979(2) 1.06945(18) 0.0186(7) Uani 1 1 d . . . C8 C 0.9502(3) 0.1318(2) 1.20761(19) 0.0179(7) Uani 1 1 d . . . C11 C 0.4407(3) 0.4607(2) 0.6939(2) 0.0247(8) Uani 1 1 d . . . H11 H 0.4869 0.5157 0.7066 0.030 Uiso 1 1 calc R . . C12 C 0.3335(3) 0.4522(2) 0.65142(19) 0.0217(7) Uani 1 1 d . . . H12A H 0.2983 0.5002 0.6312 0.026 Uiso 1 1 calc R . . C13 C 0.2819(3) 0.3610(2) 0.64184(18) 0.0161(6) Uani 1 1 d . . . C14 C 0.3529(3) 0.3029(2) 0.67635(17) 0.0154(6) Uani 1 1 d . . . C15 C 0.3027(3) 0.2084(2) 0.66647(17) 0.0144(6) Uani 1 1 d . . . C16 C 0.1464(3) 0.1017(2) 0.61630(18) 0.0173(7) Uani 1 1 d . . . H16A H 0.0730 0.0802 0.5899 0.021 Uiso 1 1 calc R . . C17 C 0.1925(3) 0.1944(2) 0.62514(17) 0.0146(6) Uani 1 1 d . . . C18 C 0.2214(3) 0.0480(2) 0.65069(18) 0.0183(7) Uani 1 1 d . . . H18 H 0.2050 -0.0143 0.6511 0.022 Uiso 1 1 calc R . . C21 C 0.3622(3) 0.2724(3) 0.2300(2) 0.0296(9) Uani 1 1 d . . . H21 H 0.3890 0.3120 0.1975 0.036 Uiso 1 1 calc R . . C22 C 0.3565(3) 0.2977(3) 0.3016(2) 0.0243(8) Uani 1 1 d . . . H22A H 0.3775 0.3562 0.3238 0.029 Uiso 1 1 calc R . . C23 C 0.3142(3) 0.2232(2) 0.33841(18) 0.0175(7) Uani 1 1 d . . . C24 C 0.2893(3) 0.1445(2) 0.29298(18) 0.0190(7) Uani 1 1 d . . . C25 C 0.2445(3) 0.0675(2) 0.32875(18) 0.0185(7) Uani 1 1 d . . . C26 C 0.2310(3) 0.0872(2) 0.40104(19) 0.0172(7) Uani 1 1 d . . . C27 C 0.1859(3) 0.0097(2) 0.4337(2) 0.0192(7) Uani 1 1 d . . . H27A H 0.1702 0.0106 0.4821 0.023 Uiso 1 1 calc R . . C28 C 0.1685(3) -0.0665(2) 0.3849(2) 0.0226(8) Uani 1 1 d . . . H28 H 0.1399 -0.1234 0.3966 0.027 Uiso 1 1 calc R . . C31 C 0.4154(3) 0.2164(2) 1.0293(2) 0.0229(8) Uani 1 1 d . . . H31 H 0.3484 0.1815 1.0048 0.027 Uiso 1 1 calc R . . C32 C 0.5126(3) 0.1809(2) 1.06293(18) 0.0187(7) Uani 1 1 d . . . H32A H 0.5204 0.1190 1.0629 0.022 Uiso 1 1 calc R . . C33 C 0.6001(3) 0.2493(2) 1.09802(17) 0.0157(6) Uani 1 1 d . . . C34 C 0.5682(3) 0.3358(2) 1.08823(17) 0.0146(6) Uani 1 1 d . . . C35 C 0.6562(3) 0.4076(2) 1.12259(17) 0.0158(6) Uani 1 1 d . . . C36 C 0.7569(3) 0.3776(2) 1.15896(18) 0.0167(7) Uani 1 1 d . . . C37 C 0.8427(3) 0.4488(2) 1.19017(18) 0.0191(7) Uani 1 1 d . . . H37A H 0.9157 0.4402 1.2163 0.023 Uiso 1 1 calc R . . C38 C 0.8057(3) 0.5319(2) 1.1773(2) 0.0235(8) Uani 1 1 d . . . H38 H 0.8505 0.5866 1.1938 0.028 Uiso 1 1 calc R . . C41 C 0.5596(3) 0.0815(2) 0.8587(2) 0.0248(8) Uani 1 1 d . . . H41 H 0.5105 0.0305 0.8378 0.030 Uiso 1 1 calc R . . C42 C 0.6649(3) 0.0776(2) 0.90065(19) 0.0194(7) Uani 1 1 d . . . H42A H 0.6962 0.0239 0.9125 0.023 Uiso 1 1 calc R . . C43 C 0.7220(3) 0.1660(2) 0.92456(17) 0.0147(6) Uani 1 1 d . . . C44 C 0.6573(3) 0.2343(2) 0.90014(18) 0.0154(6) Uani 1 1 d . . . C45 C 0.7102(3) 0.3249(2) 0.92453(17) 0.0150(6) Uani 1 1 d . . . C46 C 0.8173(3) 0.3279(2) 0.96860(17) 0.0142(6) Uani 1 1 d . . . C47 C 0.8668(3) 0.4177(2) 0.99161(18) 0.0171(7) Uani 1 1 d . . . H47A H 0.9382 0.4323 1.0221 0.021 Uiso 1 1 calc R . . C48 C 0.7970(3) 0.4805(2) 0.96359(18) 0.0195(7) Uani 1 1 d . . . H48 H 0.8163 0.5428 0.9724 0.023 Uiso 1 1 calc R . . C101 C 0.0284(3) 0.3299(2) 0.65041(17) 0.0144(6) Uani 1 1 d . . . C102 C -0.0204(3) 0.4125(2) 0.64382(18) 0.0190(7) Uani 1 1 d . . . H10B H 0.0052 0.4503 0.6098 0.023 Uiso 1 1 calc R . . C103 C -0.1077(3) 0.4386(2) 0.6882(2) 0.0238(8) Uani 1 1 d . . . H10E H -0.1394 0.4942 0.6840 0.029 Uiso 1 1 calc R . . C104 C -0.1477(3) 0.3827(2) 0.73855(19) 0.0238(8) Uani 1 1 d . . . H10A H -0.2067 0.4000 0.7676 0.029 Uiso 1 1 calc R . . C105 C -0.0989(3) 0.3005(2) 0.74531(19) 0.0222(7) Uani 1 1 d . . . H10D H -0.1251 0.2626 0.7791 0.027 Uiso 1 1 calc R . . C106 C -0.0116(3) 0.2744(2) 0.70217(17) 0.0166(7) Uani 1 1 d . . . H10C H 0.0210 0.2194 0.7076 0.020 Uiso 1 1 calc R . . C201 C 0.4083(3) 0.2129(2) 0.48882(18) 0.0171(7) Uani 1 1 d . . . C202 C 0.4474(3) 0.1375(2) 0.52079(19) 0.0198(7) Uani 1 1 d . . . H20B H 0.4010 0.0820 0.5119 0.024 Uiso 1 1 calc R . . C203 C 0.5555(3) 0.1449(2) 0.56601(19) 0.0218(7) Uani 1 1 d . . . H20C H 0.5817 0.0942 0.5870 0.026 Uiso 1 1 calc R . . C204 C 0.6244(3) 0.2278(2) 0.57985(19) 0.0227(7) Uani 1 1 d . . . H20D H 0.6963 0.2326 0.6104 0.027 Uiso 1 1 calc R . . C205 C 0.5862(3) 0.3039(2) 0.5481(2) 0.0260(8) Uani 1 1 d . . . H20E H 0.6325 0.3594 0.5573 0.031 Uiso 1 1 calc R . . C206 C 0.4788(3) 0.2961(2) 0.5029(2) 0.0213(7) Uani 1 1 d . . . H20A H 0.4532 0.3468 0.4816 0.026 Uiso 1 1 calc R . . C301 C 0.7012(3) 0.2271(2) 1.24087(18) 0.0155(6) Uani 1 1 d . . . C302 C 0.7376(3) 0.2830(3) 1.30471(19) 0.0245(8) Uani 1 1 d . . . H30E H 0.7839 0.3376 1.3031 0.029 Uiso 1 1 calc R . . C303 C 0.7050(3) 0.2576(3) 1.3707(2) 0.0312(9) Uani 1 1 d . . . H30C H 0.7311 0.2947 1.4133 0.037 Uiso 1 1 calc R . . C304 C 0.6345(3) 0.1779(2) 1.37387(19) 0.0225(7) Uani 1 1 d . . . H30D H 0.6124 0.1614 1.4183 0.027 Uiso 1 1 calc R . . C305 C 0.5965(3) 0.1223(2) 1.3100(2) 0.0228(8) Uani 1 1 d . . . H30B H 0.5483 0.0685 1.3116 0.027 Uiso 1 1 calc R . . C306 C 0.6304(3) 0.1468(2) 1.24436(19) 0.0219(7) Uani 1 1 d . . . H30A H 0.6055 0.1091 1.2019 0.026 Uiso 1 1 calc R . . C401 C 0.9789(3) 0.2013(2) 0.92389(16) 0.0127(6) Uani 1 1 d . . . C402 C 0.9768(3) 0.1269(2) 0.87220(18) 0.0170(7) Uani 1 1 d . . . H40A H 0.9098 0.0845 0.8642 0.020 Uiso 1 1 calc R . . C403 C 1.0745(3) 0.1162(2) 0.83291(19) 0.0217(7) Uani 1 1 d . . . H40E H 1.0727 0.0667 0.7983 0.026 Uiso 1 1 calc R . . C404 C 1.1749(3) 0.1788(2) 0.84478(19) 0.0220(7) Uani 1 1 d . . . H40D H 1.2405 0.1713 0.8183 0.026 Uiso 1 1 calc R . . C405 C 1.1773(3) 0.2526(2) 0.89629(18) 0.0197(7) Uani 1 1 d . . . H40C H 1.2447 0.2947 0.9043 0.024 Uiso 1 1 calc R . . C406 C 1.0803(3) 0.2641(2) 0.93579(18) 0.0190(7) Uani 1 1 d . . . H40B H 1.0826 0.3137 0.9704 0.023 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 W1 0.01591(7) 0.00750(7) 0.01509(7) 0.00270(5) 0.00403(5) -0.00044(5) W2 0.01415(7) 0.00881(7) 0.01454(7) 0.00258(5) 0.00307(5) -0.00004(5) P1 0.0161(4) 0.0094(4) 0.0152(4) 0.0023(3) 0.0037(3) -0.0008(3) P2 0.0169(4) 0.0102(4) 0.0163(4) 0.0018(3) 0.0049(3) -0.0002(3) P3 0.0156(4) 0.0093(4) 0.0155(4) 0.0021(3) 0.0031(3) 0.0006(3) P4 0.0138(4) 0.0089(4) 0.0155(4) 0.0026(3) 0.0025(3) -0.0012(3) S1 0.0204(4) 0.0203(4) 0.0237(5) 0.0005(3) -0.0005(4) -0.0065(3) S2 0.0193(4) 0.0131(4) 0.0189(4) 0.0031(3) 0.0010(3) 0.0018(3) S3 0.0289(5) 0.0359(5) 0.0173(4) 0.0022(4) 0.0070(4) 0.0018(4) S4 0.0257(5) 0.0179(4) 0.0280(5) -0.0066(4) 0.0008(4) 0.0005(4) S5 0.0204(4) 0.0185(4) 0.0283(5) 0.0060(4) -0.0068(4) -0.0049(3) S6 0.0203(4) 0.0123(4) 0.0255(4) 0.0062(3) 0.0027(3) 0.0013(3) S7 0.0300(5) 0.0108(4) 0.0246(4) 0.0027(3) 0.0032(4) 0.0043(3) S8 0.0186(4) 0.0203(4) 0.0239(4) 0.0074(3) 0.0005(3) 0.0025(3) O1 0.0272(14) 0.0148(12) 0.0469(17) 0.0065(11) 0.0121(12) -0.0025(11) O2 0.0291(14) 0.0175(13) 0.0368(16) 0.0068(11) 0.0007(12) -0.0090(11) O3 0.0228(13) 0.0170(12) 0.0390(16) -0.0015(11) 0.0021(12) 0.0037(11) O4 0.0344(15) 0.0189(13) 0.0229(14) 0.0049(10) 0.0044(11) 0.0017(11) O5 0.0317(15) 0.0227(14) 0.0290(15) 0.0062(11) 0.0032(12) -0.0078(11) O6 0.0236(13) 0.0164(12) 0.0368(16) 0.0034(11) 0.0042(11) -0.0030(10) O7 0.0247(13) 0.0252(14) 0.0283(14) 0.0032(11) 0.0066(11) 0.0071(11) O8 0.0338(15) 0.0193(13) 0.0222(13) 0.0106(10) 0.0018(11) -0.0012(11) C1 0.0192(17) 0.0111(15) 0.0245(18) 0.0024(13) 0.0052(14) 0.0008(13) C2 0.0189(17) 0.0150(16) 0.0204(17) 0.0045(13) 0.0027(13) 0.0009(13) C3 0.0226(17) 0.0114(15) 0.0202(17) 0.0029(13) 0.0029(14) -0.0063(13) C4 0.0189(16) 0.0076(14) 0.0229(18) 0.0019(12) 0.0050(13) 0.0010(12) C5 0.0162(16) 0.0177(16) 0.0161(16) 0.0031(13) 0.0029(13) -0.0033(13) C6 0.0165(16) 0.0146(16) 0.0179(16) 0.0048(13) 0.0033(13) 0.0026(13) C7 0.0211(17) 0.0167(16) 0.0176(17) 0.0030(13) 0.0014(14) -0.0012(14) C8 0.0165(16) 0.0132(15) 0.0235(18) -0.0012(13) 0.0040(14) -0.0002(13) C11 0.032(2) 0.0138(16) 0.0262(19) 0.0009(14) 0.0038(16) -0.0089(15) C12 0.0292(19) 0.0120(16) 0.0243(18) 0.0027(13) 0.0079(15) -0.0030(14) C13 0.0173(16) 0.0125(15) 0.0183(16) 0.0003(12) 0.0061(13) -0.0041(12) C14 0.0171(16) 0.0137(15) 0.0147(16) -0.0007(12) 0.0030(13) -0.0034(12) C15 0.0174(16) 0.0112(15) 0.0152(15) 0.0022(12) 0.0046(13) 0.0001(12) C16 0.0173(16) 0.0149(16) 0.0197(17) 0.0010(13) 0.0049(13) -0.0008(13) C17 0.0174(16) 0.0115(15) 0.0154(16) 0.0023(12) 0.0043(13) 0.0006(12) C18 0.0226(17) 0.0105(15) 0.0215(17) 0.0003(13) 0.0053(14) -0.0031(13) C21 0.030(2) 0.032(2) 0.030(2) 0.0134(17) 0.0131(17) 0.0009(17) C22 0.0255(19) 0.0233(18) 0.0260(19) 0.0079(15) 0.0111(15) -0.0030(15) C23 0.0137(16) 0.0195(17) 0.0204(17) 0.0054(13) 0.0048(13) 0.0015(13) C24 0.0166(16) 0.0240(18) 0.0174(17) 0.0035(14) 0.0037(13) 0.0039(14) C25 0.0145(16) 0.0172(16) 0.0226(17) -0.0025(13) 0.0000(13) 0.0022(13) C26 0.0156(16) 0.0136(15) 0.0226(17) 0.0006(13) 0.0039(13) 0.0007(13) C27 0.0154(16) 0.0139(16) 0.0289(19) 0.0002(14) 0.0052(14) 0.0030(13) C28 0.0158(17) 0.0163(17) 0.036(2) -0.0003(15) 0.0055(15) 0.0015(13) C31 0.0158(17) 0.0264(19) 0.0258(19) 0.0047(15) 0.0018(14) -0.0043(14) C32 0.0213(17) 0.0151(16) 0.0201(17) 0.0026(13) 0.0055(14) 0.0000(13) C33 0.0156(16) 0.0159(16) 0.0158(16) 0.0022(12) 0.0038(13) 0.0001(13) C34 0.0144(15) 0.0153(15) 0.0149(15) 0.0033(12) 0.0033(12) 0.0010(12) C35 0.0221(17) 0.0098(15) 0.0172(16) 0.0050(12) 0.0069(13) 0.0019(12) C36 0.0206(17) 0.0123(15) 0.0178(16) 0.0042(12) 0.0037(13) -0.0002(13) C37 0.0241(18) 0.0128(16) 0.0197(17) 0.0026(13) 0.0007(14) -0.0017(13) C38 0.0285(19) 0.0169(17) 0.0234(18) -0.0010(14) 0.0018(15) -0.0048(15) C41 0.029(2) 0.0152(17) 0.0277(19) 0.0025(14) -0.0033(16) -0.0073(14) C42 0.0208(17) 0.0108(15) 0.0267(19) 0.0039(13) 0.0052(14) -0.0031(13) C43 0.0135(15) 0.0133(15) 0.0171(16) 0.0041(12) 0.0027(12) -0.0042(12) C44 0.0148(15) 0.0137(15) 0.0171(16) 0.0026(12) 0.0020(13) -0.0034(12) C45 0.0184(16) 0.0094(14) 0.0182(16) 0.0031(12) 0.0062(13) 0.0004(12) C46 0.0182(16) 0.0090(14) 0.0162(15) 0.0037(12) 0.0046(13) -0.0009(12) C47 0.0171(16) 0.0133(15) 0.0199(17) 0.0006(13) 0.0014(13) -0.0032(13) C48 0.0233(18) 0.0116(15) 0.0235(18) 0.0007(13) 0.0062(14) -0.0028(13) C101 0.0176(16) 0.0106(14) 0.0149(15) 0.0001(12) 0.0021(13) 0.0003(12) C102 0.0241(18) 0.0158(16) 0.0185(17) 0.0047(13) 0.0069(14) 0.0012(14) C103 0.030(2) 0.0147(17) 0.029(2) 0.0035(14) 0.0084(16) 0.0072(15) C104 0.0237(18) 0.0251(19) 0.0242(19) -0.0007(15) 0.0104(15) 0.0053(15) C105 0.0264(19) 0.0198(17) 0.0205(18) 0.0033(14) 0.0060(15) -0.0026(15) C106 0.0227(17) 0.0118(15) 0.0158(15) 0.0053(12) 0.0032(13) -0.0003(13) C201 0.0192(16) 0.0157(16) 0.0175(16) 0.0006(13) 0.0077(13) 0.0023(13) C202 0.0195(17) 0.0189(17) 0.0224(18) 0.0061(14) 0.0076(14) -0.0009(14) C203 0.0223(18) 0.0218(18) 0.0228(18) 0.0071(14) 0.0046(14) 0.0029(14) C204 0.0192(17) 0.0266(19) 0.0211(18) -0.0020(14) 0.0003(14) 0.0021(15) C205 0.0218(18) 0.0188(18) 0.035(2) -0.0062(15) 0.0010(16) -0.0026(14) C206 0.0230(18) 0.0127(16) 0.0285(19) 0.0001(14) 0.0043(15) 0.0036(14) C301 0.0143(15) 0.0139(15) 0.0194(16) 0.0042(13) 0.0034(13) 0.0032(12) C302 0.0236(18) 0.0283(19) 0.0201(18) 0.0000(15) 0.0065(15) -0.0102(15) C303 0.027(2) 0.043(2) 0.0211(19) -0.0031(17) 0.0083(16) -0.0119(18) C304 0.0193(17) 0.031(2) 0.0200(17) 0.0092(15) 0.0084(14) 0.0036(15) C305 0.0245(18) 0.0168(17) 0.031(2) 0.0110(15) 0.0124(15) 0.0039(14) C306 0.0299(19) 0.0129(16) 0.0230(18) 0.0019(13) 0.0044(15) 0.0004(14) C401 0.0133(15) 0.0121(15) 0.0132(15) 0.0055(12) 0.0016(12) -0.0005(12) C402 0.0208(17) 0.0126(15) 0.0174(16) 0.0018(12) 0.0011(13) 0.0005(13) C403 0.0286(19) 0.0195(17) 0.0187(17) 0.0023(14) 0.0074(15) 0.0053(15) C404 0.0234(18) 0.0228(18) 0.0238(18) 0.0111(14) 0.0121(15) 0.0052(14) C405 0.0189(17) 0.0194(17) 0.0222(17) 0.0094(14) 0.0046(14) -0.0008(13) C406 0.0206(17) 0.0148(16) 0.0203(17) 0.0000(13) 0.0020(14) -0.0045(13) _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 W1 C3 1.986(4) . ? W1 C4 1.999(3) . ? W1 C1 2.042(3) . ? W1 C2 2.045(3) . ? W1 P1 2.4995(10) . ? W1 P2 2.5006(11) . ? W2 C7 1.994(4) . ? W2 C8 2.014(4) . ? W2 C6 2.040(3) . ? W2 C5 2.044(3) . ? W2 P4 2.4707(10) . ? W2 P3 2.4760(11) . ? P1 C17 1.814(3) . ? P1 C13 1.825(3) . ? P1 C101 1.833(3) . ? P2 C26 1.811(3) . ? P2 C23 1.819(3) . ? P2 C201 1.826(3) . ? P3 C33 1.819(3) . ? P3 C36 1.820(3) . ? P3 C301 1.830(3) . ? P4 C43 1.822(3) . ? P4 C46 1.827(3) . ? P4 C401 1.830(3) . ? S1 C14 1.710(3) . ? S1 C11 1.727(4) . ? S2 C15 1.717(3) . ? S2 C18 1.726(3) . ? S3 C24 1.711(4) . ? S3 C21 1.725(4) . ? S4 C25 1.719(3) . ? S4 C28 1.722(4) . ? S5 C44 1.717(3) . ? S5 C41 1.727(4) . ? S6 C45 1.717(3) . ? S6 C48 1.726(4) . ? S7 C35 1.713(3) . ? S7 C38 1.725(4) . ? S8 C34 1.716(3) . ? S8 C31 1.724(4) . ? O1 C1 1.136(4) . ? O2 C2 1.131(4) . ? O3 C3 1.156(4) . ? O4 C4 1.134(4) . ? O5 C5 1.138(4) . ? O6 C6 1.143(4) . ? O7 C7 1.160(4) . ? O8 C8 1.148(4) . ? C11 C12 1.356(5) . ? C11 H11 0.9300 . ? C12 C13 1.417(4) . ? C12 H12A 0.9300 . ? C13 C14 1.374(4) . ? C14 C15 1.457(4) . ? C15 C17 1.375(4) . ? C16 C18 1.353(4) . ? C16 C17 1.420(4) . ? C16 H16A 0.9300 . ? C18 H18 0.9300 . ? C21 C22 1.356(5) . ? C21 H21 0.9300 . ? C22 C23 1.422(5) . ? C22 H22A 0.9300 . ? C23 C24 1.372(5) . ? C24 C25 1.449(5) . ? C25 C26 1.372(5) . ? C26 C27 1.425(5) . ? C27 C28 1.374(5) . ? C27 H27A 0.9300 . ? C28 H28 0.9300 . ? C31 C32 1.364(5) . ? C31 H31 0.9300 . ? C32 C33 1.418(4) . ? C32 H32A 0.9300 . ? C33 C34 1.382(4) . ? C34 C35 1.448(4) . ? C35 C36 1.378(4) . ? C36 C37 1.411(4) . ? C37 C38 1.365(5) . ? C37 H37A 0.9300 . ? C38 H38 0.9300 . ? C41 C42 1.353(5) . ? C41 H41 0.9300 . ? C42 C43 1.427(4) . ? C42 H42A 0.9300 . ? C43 C44 1.374(4) . ? C44 C45 1.441(4) . ? C45 C46 1.374(4) . ? C46 C47 1.415(4) . ? C47 C48 1.365(4) . ? C47 H47A 0.9300 . ? C48 H48 0.9300 . ? C101 C102 1.392(4) . ? C101 C106 1.400(4) . ? C102 C103 1.396(5) . ? C102 H10B 0.9300 . ? C103 C104 1.384(5) . ? C103 H10E 0.9300 . ? C104 C105 1.387(5) . ? C104 H10A 0.9300 . ? C105 C106 1.380(5) . ? C105 H10D 0.9300 . ? C106 H10C 0.9300 . ? C201 C202 1.391(5) . ? C201 C206 1.401(5) . ? C202 C203 1.391(5) . ? C202 H20B 0.9300 . ? C203 C204 1.387(5) . ? C203 H20C 0.9300 . ? C204 C205 1.395(5) . ? C204 H20D 0.9300 . ? C205 C206 1.384(5) . ? C205 H20E 0.9300 . ? C206 H20A 0.9300 . ? C301 C306 1.386(4) . ? C301 C302 1.390(5) . ? C302 C303 1.383(5) . ? C302 H30E 0.9300 . ? C303 C304 1.376(5) . ? C303 H30C 0.9300 . ? C304 C305 1.391(5) . ? C304 H30D 0.9300 . ? C305 C306 1.379(5) . ? C305 H30B 0.9300 . ? C306 H30A 0.9300 . ? C401 C406 1.395(4) . ? C401 C402 1.395(4) . ? C402 C403 1.384(5) . ? C402 H40A 0.9300 . ? C403 C404 1.385(5) . ? C403 H40E 0.9300 . ? C404 C405 1.387(5) . ? C404 H40D 0.9300 . ? C405 C406 1.381(5) . ? C405 H40C 0.9300 . ? C406 H40B 0.9300 . ? 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 C3 W1 C4 84.68(14) . . ? C3 W1 C1 92.28(13) . . ? C4 W1 C1 88.93(14) . . ? C3 W1 C2 91.29(13) . . ? C4 W1 C2 91.28(13) . . ? C1 W1 C2 176.43(13) . . ? C3 W1 P1 93.18(10) . . ? C4 W1 P1 177.85(9) . . ? C1 W1 P1 90.98(10) . . ? C2 W1 P1 88.94(10) . . ? C3 W1 P2 172.46(10) . . ? C4 W1 P2 87.79(10) . . ? C1 W1 P2 87.67(10) . . ? C2 W1 P2 88.78(10) . . ? P1 W1 P2 94.35(4) . . ? C7 W2 C8 90.61(13) . . ? C7 W2 C6 92.11(13) . . ? C8 W2 C6 90.62(13) . . ? C7 W2 C5 88.27(14) . . ? C8 W2 C5 91.59(13) . . ? C6 W2 C5 177.75(12) . . ? C7 W2 P4 89.28(10) . . ? C8 W2 P4 179.11(10) . . ? C6 W2 P4 90.27(10) . . ? C5 W2 P4 87.52(10) . . ? C7 W2 P3 179.97(12) . . ? C8 W2 P3 89.42(10) . . ? C6 W2 P3 87.90(10) . . ? C5 W2 P3 91.72(10) . . ? P4 W2 P3 90.69(4) . . ? C17 P1 C13 89.99(15) . . ? C17 P1 C101 103.77(15) . . ? C13 P1 C101 102.68(15) . . ? C17 P1 W1 117.47(11) . . ? C13 P1 W1 120.00(11) . . ? C101 P1 W1 118.30(11) . . ? C26 P2 C23 90.08(16) . . ? C26 P2 C201 104.61(15) . . ? C23 P2 C201 105.33(15) . . ? C26 P2 W1 119.36(11) . . ? C23 P2 W1 111.84(11) . . ? C201 P2 W1 120.72(11) . . ? C33 P3 C36 90.33(15) . . ? C33 P3 C301 101.54(15) . . ? C36 P3 C301 103.52(15) . . ? C33 P3 W2 119.75(11) . . ? C36 P3 W2 121.58(12) . . ? C301 P3 W2 115.70(11) . . ? C43 P4 C46 89.90(15) . . ? C43 P4 C401 104.03(15) . . ? C46 P4 C401 101.87(14) . . ? C43 P4 W2 122.17(11) . . ? C46 P4 W2 121.15(11) . . ? C401 P4 W2 113.64(10) . . ? C14 S1 C11 90.76(17) . . ? C15 S2 C18 91.24(16) . . ? C24 S3 C21 90.49(18) . . ? C25 S4 C28 90.97(17) . . ? C44 S5 C41 91.22(17) . . ? C45 S6 C48 90.72(16) . . ? C35 S7 C38 91.47(17) . . ? C34 S8 C31 91.34(16) . . ? O1 C1 W1 177.0(3) . . ? O2 C2 W1 179.4(3) . . ? O3 C3 W1 174.6(3) . . ? O4 C4 W1 176.1(3) . . ? O5 C5 W2 177.2(3) . . ? O6 C6 W2 178.4(3) . . ? O7 C7 W2 178.0(3) . . ? O8 C8 W2 178.7(3) . . ? C12 C11 S1 113.0(3) . . ? C12 C11 H11 123.5 . . ? S1 C11 H11 123.5 . . ? C11 C12 C13 111.5(3) . . ? C11 C12 H12A 124.3 . . ? C13 C12 H12A 124.3 . . ? C14 C13 C12 112.8(3) . . ? C14 C13 P1 110.9(2) . . ? C12 C13 P1 136.3(3) . . ? C13 C14 C15 114.0(3) . . ? C13 C14 S1 111.9(2) . . ? C15 C14 S1 134.1(3) . . ? C17 C15 C14 113.9(3) . . ? C17 C15 S2 111.6(2) . . ? C14 C15 S2 134.5(2) . . ? C18 C16 C17 112.4(3) . . ? C18 C16 H16A 123.8 . . ? C17 C16 H16A 123.8 . . ? C15 C17 C16 112.5(3) . . ? C15 C17 P1 111.2(2) . . ? C16 C17 P1 136.3(2) . . ? C16 C18 S2 112.3(2) . . ? C16 C18 H18 123.8 . . ? S2 C18 H18 123.8 . . ? C22 C21 S3 113.3(3) . . ? C22 C21 H21 123.3 . . ? S3 C21 H21 123.3 . . ? C21 C22 C23 111.2(3) . . ? C21 C22 H22A 124.4 . . ? C23 C22 H22A 124.4 . . ? C24 C23 C22 112.6(3) . . ? C24 C23 P2 110.6(2) . . ? C22 C23 P2 136.4(3) . . ? C23 C24 C25 113.9(3) . . ? C23 C24 S3 112.4(3) . . ? C25 C24 S3 133.7(3) . . ? C26 C25 C24 114.3(3) . . ? C26 C25 S4 112.4(3) . . ? C24 C25 S4 133.2(3) . . ? C25 C26 C27 112.3(3) . . ? C25 C26 P2 110.7(2) . . ? C27 C26 P2 136.9(3) . . ? C28 C27 C26 111.7(3) . . ? C28 C27 H27A 124.1 . . ? C26 C27 H27A 124.1 . . ? C27 C28 S4 112.6(3) . . ? C27 C28 H28 123.7 . . ? S4 C28 H28 123.7 . . ? C32 C31 S8 112.4(3) . . ? C32 C31 H31 123.8 . . ? S8 C31 H31 123.8 . . ? C31 C32 C33 112.1(3) . . ? C31 C32 H32A 124.0 . . ? C33 C32 H32A 124.0 . . ? C34 C33 C32 112.5(3) . . ? C34 C33 P3 110.6(2) . . ? C32 C33 P3 136.9(3) . . ? C33 C34 C35 114.1(3) . . ? C33 C34 S8 111.6(2) . . ? C35 C34 S8 134.3(2) . . ? C36 C35 C34 114.4(3) . . ? C36 C35 S7 111.2(2) . . ? C34 C35 S7 134.3(3) . . ? C35 C36 C37 113.3(3) . . ? C35 C36 P3 110.6(2) . . ? C37 C36 P3 136.2(3) . . ? C38 C37 C36 111.8(3) . . ? C38 C37 H37A 124.1 . . ? C36 C37 H37A 124.1 . . ? C37 C38 S7 112.2(3) . . ? C37 C38 H38 123.9 . . ? S7 C38 H38 123.9 . . ? C42 C41 S5 112.8(3) . . ? C42 C41 H41 123.6 . . ? S5 C41 H41 123.6 . . ? C41 C42 C43 111.5(3) . . ? C41 C42 H42A 124.2 . . ? C43 C42 H42A 124.2 . . ? C44 C43 C42 113.0(3) . . ? C44 C43 P4 110.4(2) . . ? C42 C43 P4 136.5(3) . . ? C43 C44 C45 114.9(3) . . ? C43 C44 S5 111.4(2) . . ? C45 C44 S5 133.7(3) . . ? C46 C45 C44 114.0(3) . . ? C46 C45 S6 112.2(2) . . ? C44 C45 S6 133.8(3) . . ? C45 C46 C47 112.6(3) . . ? C45 C46 P4 110.8(2) . . ? C47 C46 P4 136.7(2) . . ? C48 C47 C46 111.8(3) . . ? C48 C47 H47A 124.1 . . ? C46 C47 H47A 124.1 . . ? C47 C48 S6 112.7(2) . . ? C47 C48 H48 123.7 . . ? S6 C48 H48 123.7 . . ? C102 C101 C106 118.8(3) . . ? C102 C101 P1 118.7(2) . . ? C106 C101 P1 122.5(2) . . ? C101 C102 C103 120.1(3) . . ? C101 C102 H10B 120.0 . . ? C103 C102 H10B 120.0 . . ? C104 C103 C102 120.6(3) . . ? C104 C103 H10E 119.7 . . ? C102 C103 H10E 119.7 . . ? C103 C104 C105 119.3(3) . . ? C103 C104 H10A 120.3 . . ? C105 C104 H10A 120.3 . . ? C106 C105 C104 120.5(3) . . ? C106 C105 H10D 119.8 . . ? C104 C105 H10D 119.8 . . ? C105 C106 C101 120.7(3) . . ? C105 C106 H10C 119.6 . . ? C101 C106 H10C 119.6 . . ? C202 C201 C206 119.3(3) . . ? C202 C201 P2 122.2(3) . . ? C206 C201 P2 118.5(2) . . ? C201 C202 C203 120.2(3) . . ? C201 C202 H20B 119.9 . . ? C203 C202 H20B 119.9 . . ? C204 C203 C202 120.1(3) . . ? C204 C203 H20C 120.0 . . ? C202 C203 H20C 120.0 . . ? C203 C204 C205 120.3(3) . . ? C203 C204 H20D 119.8 . . ? C205 C204 H20D 119.8 . . ? C206 C205 C204 119.4(3) . . ? C206 C205 H20E 120.3 . . ? C204 C205 H20E 120.3 . . ? C205 C206 C201 120.7(3) . . ? C205 C206 H20A 119.6 . . ? C201 C206 H20A 119.6 . . ? C306 C301 C302 119.0(3) . . ? C306 C301 P3 118.4(3) . . ? C302 C301 P3 122.5(3) . . ? C303 C302 C301 120.1(3) . . ? C303 C302 H30E 120.0 . . ? C301 C302 H30E 120.0 . . ? C304 C303 C302 120.7(4) . . ? C304 C303 H30C 119.6 . . ? C302 C303 H30C 119.6 . . ? C303 C304 C305 119.4(3) . . ? C303 C304 H30D 120.3 . . ? C305 C304 H30D 120.3 . . ? C306 C305 C304 120.0(3) . . ? C306 C305 H30B 120.0 . . ? C304 C305 H30B 120.0 . . ? C305 C306 C301 120.8(3) . . ? C305 C306 H30A 119.6 . . ? C301 C306 H30A 119.6 . . ? C406 C401 C402 119.4(3) . . ? C406 C401 P4 118.8(2) . . ? C402 C401 P4 121.6(2) . . ? C403 C402 C401 120.0(3) . . ? C403 C402 H40A 120.0 . . ? C401 C402 H40A 120.0 . . ? C402 C403 C404 120.4(3) . . ? C402 C403 H40E 119.8 . . ? C404 C403 H40E 119.8 . . ? C403 C404 C405 119.7(3) . . ? C403 C404 H40D 120.2 . . ? C405 C404 H40D 120.2 . . ? C406 C405 C404 120.4(3) . . ? C406 C405 H40C 119.8 . . ? C404 C405 H40C 119.8 . . ? C405 C406 C401 120.1(3) . . ? C405 C406 H40B 120.0 . . ? C401 C406 H40B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.47 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 3.047 _refine_diff_density_min -1.908 _refine_diff_density_rms 0.152