# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Rockshana Begum' 'Takashi Komuro' 'Hiromi Tobita' _publ_author_address ; Department of Chemistry, Graduate School of Science Tohoku University Sendai 980-8578 JAPAN ; _publ_contact_author_name 'Professor Hiromi Tobita' _publ_contact_author_address ; Department of Chemistry, Graduate School of Science Tohoku University Sendai 980-8578 JAPAN ; _publ_contact_author_email tobita@mail.tains.tohoku.ac.jp _publ_requested_journal 'Chemical Communications' _publ_section_title ; Group 6 metal xantsil complexes with a labile oxygen coordination and insertion of tBuCN into a W-Si bond [xantsil = (9,9-dimethylxantene- 4,5-diyl)bis(dimethylsilyl)] ; data_complex2a _database_code_depnum_ccdc_archive 'CCDC 284200' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H40 O2 Si2 W' _chemical_formula_weight 672.65 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21' _symmetry_int_tables_number 29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 9.5123(3) _cell_length_b 18.0026(6) _cell_length_c 16.9940(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2910.16(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25393 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour 'orange ' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 4.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4961 _exptl_absorpt_correction_T_max 0.6860 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23638 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6401 _reflns_number_gt 5813 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+11.5632P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.024(13) _refine_ls_number_reflns 6401 _refine_ls_number_parameters 327 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.213 _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 W1 W 0.57537(3) 0.812410(13) 0.65166(3) 0.02759(9) Uani 1 1 d . . . Si1 Si 0.4262(2) 0.77986(15) 0.77166(17) 0.0366(5) Uani 1 1 d . . . Si2 Si 0.4533(3) 0.72809(15) 0.54949(16) 0.0368(5) Uani 1 1 d . . . O1 O 0.6341(6) 0.6927(3) 0.6922(3) 0.0287(12) Uani 1 1 d . . . O2 O 0.2931(8) 0.8750(5) 0.5932(7) 0.083(3) Uani 1 1 d . . . C1 C 0.2711(12) 0.7155(8) 0.7551(9) 0.052(3) Uani 1 1 d . . . H1 H 0.2994 0.6748 0.7202 0.078 Uiso 1 1 calc R . . H2 H 0.1939 0.7433 0.7308 0.078 Uiso 1 1 calc R . . H3 H 0.2399 0.6951 0.8056 0.078 Uiso 1 1 calc R . . C2 C 0.3535(13) 0.8513(7) 0.8437(8) 0.065(4) Uani 1 1 d . . . H4 H 0.3044 0.8257 0.8866 0.098 Uiso 1 1 calc R . . H5 H 0.2877 0.8842 0.8163 0.098 Uiso 1 1 calc R . . H6 H 0.4311 0.8807 0.8654 0.098 Uiso 1 1 calc R . . C3 C 0.5494(9) 0.7131(5) 0.8237(5) 0.0326(17) Uani 1 1 d . . . C4 C 0.5573(11) 0.6936(6) 0.9023(6) 0.047(2) Uani 1 1 d . . . H7 H 0.5036 0.7209 0.9395 0.056 Uiso 1 1 calc R . . C5 C 0.6416(12) 0.6353(6) 0.9286(6) 0.051(3) Uani 1 1 d . . . H8 H 0.6455 0.6237 0.9831 0.062 Uiso 1 1 calc R . . C6 C 0.7208(11) 0.5937(6) 0.8742(6) 0.048(2) Uani 1 1 d . . . H9 H 0.7765 0.5531 0.8918 0.058 Uiso 1 1 calc R . . C7 C 0.7174(9) 0.6117(5) 0.7957(5) 0.0318(17) Uani 1 1 d . . . C8 C 0.6367(8) 0.6720(4) 0.7735(5) 0.0280(16) Uani 1 1 d . . . C9 C 0.7999(9) 0.5686(5) 0.7333(6) 0.039(2) Uani 1 1 d . . . C10 C 0.8424(12) 0.4920(5) 0.7604(9) 0.060(3) Uani 1 1 d . . . H10 H 0.7595 0.4653 0.7797 0.090 Uiso 1 1 calc R . . H11 H 0.9118 0.4962 0.8028 0.090 Uiso 1 1 calc R . . H12 H 0.8837 0.4646 0.7162 0.090 Uiso 1 1 calc R . . C11 C 0.9337(11) 0.6123(7) 0.7101(8) 0.057(3) Uani 1 1 d . . . H13 H 0.9921 0.6201 0.7569 0.086 Uiso 1 1 calc R . . H14 H 0.9068 0.6604 0.6878 0.086 Uiso 1 1 calc R . . H15 H 0.9870 0.5839 0.6709 0.086 Uiso 1 1 calc R . . C12 C 0.5377(8) 0.6363(5) 0.5760(5) 0.0294(16) Uani 1 1 d . . . C13 C 0.5286(10) 0.5725(5) 0.5292(6) 0.042(2) Uani 1 1 d . . . H16 H 0.4672 0.5724 0.4851 0.050 Uiso 1 1 calc R . . C14 C 0.6059(10) 0.5100(5) 0.5453(6) 0.042(2) Uani 1 1 d . . . H17 H 0.5998 0.4682 0.5114 0.051 Uiso 1 1 calc R . . C15 C 0.6921(9) 0.5076(4) 0.6100(6) 0.036(2) Uani 1 1 d . . . H18 H 0.7440 0.4635 0.6202 0.044 Uiso 1 1 calc R . . C16 C 0.7058(8) 0.5676(4) 0.6613(8) 0.035(2) Uani 1 1 d . . . C17 C 0.6250(7) 0.6300(4) 0.6393(5) 0.0211(18) Uani 1 1 d . . . C18 C 0.2575(15) 0.7068(9) 0.5445(12) 0.070(5) Uani 1 1 d . . . H19 H 0.2407 0.6684 0.5047 0.105 Uiso 1 1 calc R . . H20 H 0.2060 0.7520 0.5302 0.105 Uiso 1 1 calc R . . H21 H 0.2252 0.6891 0.5959 0.105 Uiso 1 1 calc R . . C19 C 0.5005(14) 0.7484(7) 0.4434(6) 0.059(3) Uani 1 1 d . . . H22 H 0.6013 0.7400 0.4355 0.088 Uiso 1 1 calc R . . H23 H 0.4778 0.8002 0.4312 0.088 Uiso 1 1 calc R . . H24 H 0.4469 0.7155 0.4087 0.088 Uiso 1 1 calc R . . C20 C 0.3962(10) 0.8491(5) 0.6151(7) 0.047(3) Uani 1 1 d . . . C21 C 0.6942(9) 0.8960(5) 0.7377(5) 0.0314(18) Uani 1 1 d . . . C22 C 0.6141(10) 0.9346(5) 0.6782(5) 0.0316(19) Uani 1 1 d . . . C23 C 0.6718(11) 0.9182(5) 0.6030(5) 0.033(2) Uani 1 1 d . . . C24 C 0.7863(12) 0.8715(6) 0.6149(8) 0.040(3) Uani 1 1 d . . . C25 C 0.7985(10) 0.8546(5) 0.6973(6) 0.025(2) Uani 1 1 d . . . C26 C 0.6957(14) 0.9078(7) 0.8223(6) 0.062(3) Uani 1 1 d . . . H25 H 0.6975 0.8597 0.8492 0.093 Uiso 1 1 calc R . . H26 H 0.6113 0.9353 0.8379 0.093 Uiso 1 1 calc R . . H27 H 0.7795 0.9364 0.8367 0.093 Uiso 1 1 calc R . . C27 C 0.5055(13) 0.9941(6) 0.6956(8) 0.063(3) Uani 1 1 d . . . H28 H 0.4621 0.9844 0.7469 0.094 Uiso 1 1 calc R . . H29 H 0.4330 0.9936 0.6547 0.094 Uiso 1 1 calc R . . H30 H 0.5513 1.0429 0.6965 0.094 Uiso 1 1 calc R . . C28 C 0.6314(14) 0.9576(6) 0.5280(6) 0.056(3) Uani 1 1 d . . . H31 H 0.6892 1.0023 0.5219 0.084 Uiso 1 1 calc R . . H32 H 0.5320 0.9717 0.5303 0.084 Uiso 1 1 calc R . . H33 H 0.6468 0.9245 0.4831 0.084 Uiso 1 1 calc R . . C29 C 0.8875(14) 0.8435(8) 0.5520(10) 0.069(4) Uani 1 1 d . . . H34 H 0.8386 0.8407 0.5014 0.104 Uiso 1 1 calc R . . H35 H 0.9217 0.7940 0.5666 0.104 Uiso 1 1 calc R . . H36 H 0.9673 0.8777 0.5477 0.104 Uiso 1 1 calc R . . C30 C 0.9115(12) 0.8104(6) 0.7352(11) 0.060(4) Uani 1 1 d . . . H37 H 0.9712 0.8433 0.7667 0.089 Uiso 1 1 calc R . . H38 H 0.9685 0.7863 0.6945 0.089 Uiso 1 1 calc R . . H39 H 0.8694 0.7726 0.7692 0.089 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 0.02567(14) 0.02344(13) 0.03366(15) 0.0017(2) -0.0047(2) 0.00205(9) Si1 0.0289(12) 0.0336(13) 0.0473(15) -0.0021(11) 0.0113(10) 0.0050(10) Si2 0.0364(13) 0.0352(14) 0.0389(14) 0.0031(10) -0.0149(10) -0.0036(10) O1 0.037(3) 0.025(3) 0.024(3) -0.001(2) -0.001(2) 0.001(2) O2 0.047(5) 0.065(5) 0.136(9) -0.005(5) -0.045(5) 0.029(4) C1 0.030(6) 0.048(7) 0.079(10) 0.007(7) 0.000(5) -0.009(5) C2 0.055(7) 0.057(7) 0.084(9) -0.016(6) 0.040(6) 0.000(6) C3 0.029(4) 0.036(4) 0.033(5) 0.000(4) 0.003(3) -0.007(3) C4 0.048(6) 0.055(6) 0.038(5) -0.007(5) 0.015(4) -0.011(5) C5 0.058(6) 0.058(7) 0.038(6) 0.013(5) -0.007(5) -0.001(5) C6 0.052(6) 0.044(5) 0.048(6) 0.007(4) -0.016(4) -0.004(5) C7 0.030(4) 0.028(4) 0.037(5) 0.005(3) -0.003(3) -0.006(3) C8 0.023(4) 0.024(4) 0.037(4) 0.001(3) -0.001(3) -0.005(3) C9 0.034(5) 0.032(4) 0.051(6) -0.001(4) -0.004(4) 0.009(4) C10 0.048(6) 0.033(5) 0.099(10) 0.001(5) -0.015(6) 0.019(5) C11 0.040(6) 0.048(6) 0.084(9) -0.010(6) 0.006(5) -0.005(4) C12 0.026(4) 0.031(4) 0.031(4) -0.003(3) 0.003(3) -0.005(3) C13 0.038(5) 0.040(5) 0.048(6) -0.009(4) 0.004(4) -0.020(4) C14 0.047(5) 0.035(5) 0.045(6) -0.005(4) 0.009(4) -0.015(4) C15 0.035(5) 0.018(4) 0.056(6) -0.001(4) 0.016(4) -0.003(3) C16 0.033(4) 0.027(3) 0.044(7) -0.003(4) 0.018(4) -0.002(3) C17 0.022(3) 0.023(3) 0.018(5) -0.002(3) 0.006(3) -0.004(2) C18 0.051(8) 0.063(9) 0.097(13) 0.013(8) -0.041(8) -0.013(6) C19 0.084(8) 0.059(7) 0.034(6) 0.000(5) -0.016(5) -0.005(6) C20 0.028(5) 0.032(5) 0.082(7) -0.003(5) -0.009(4) -0.002(4) C21 0.038(5) 0.025(4) 0.032(5) 0.002(3) -0.003(4) -0.015(3) C22 0.037(5) 0.029(4) 0.030(5) 0.001(3) -0.004(3) -0.001(4) C23 0.055(6) 0.027(5) 0.017(4) 0.002(3) -0.002(4) -0.006(4) C24 0.042(6) 0.023(5) 0.054(6) -0.017(4) 0.006(4) -0.002(4) C25 0.028(4) 0.009(4) 0.038(5) 0.004(3) -0.008(3) 0.001(3) C26 0.084(9) 0.062(7) 0.039(6) -0.001(5) 0.001(5) -0.029(6) C27 0.051(6) 0.039(6) 0.097(9) -0.012(6) -0.007(6) 0.018(5) C28 0.088(8) 0.043(6) 0.038(6) 0.014(4) -0.016(5) -0.010(5) C29 0.062(7) 0.056(9) 0.090(10) -0.022(8) 0.039(7) -0.033(7) C30 0.041(6) 0.028(6) 0.110(12) 0.005(6) -0.033(6) -0.011(4) _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 C20 1.930(10) . ? W1 C23 2.270(9) . ? W1 C22 2.275(9) . ? W1 O1 2.330(5) . ? W1 C24 2.355(12) . ? W1 C21 2.383(8) . ? W1 C25 2.384(9) . ? W1 Si1 2.553(3) . ? W1 Si2 2.582(3) . ? Si1 C1 1.897(12) . ? Si1 C3 1.898(10) . ? Si1 C2 1.906(11) . ? Si2 C12 1.892(9) . ? Si2 C19 1.893(11) . ? Si2 C18 1.903(14) . ? O1 C8 1.432(10) . ? O1 C17 1.445(9) . ? O2 C20 1.148(12) . ? C1 H1 0.9800 . ? C1 H2 0.9800 . ? C1 H3 0.9800 . ? C2 H4 0.9800 . ? C2 H5 0.9800 . ? C2 H6 0.9800 . ? C3 C4 1.382(14) . ? C3 C8 1.401(12) . ? C4 C5 1.395(15) . ? C4 H7 0.9500 . ? C5 C6 1.409(15) . ? C5 H8 0.9500 . ? C6 C7 1.373(13) . ? C6 H9 0.9500 . ? C7 C8 1.381(11) . ? C7 C9 1.532(12) . ? C9 C10 1.509(13) . ? C9 C16 1.517(15) . ? C9 C11 1.547(14) . ? C10 H10 0.9800 . ? C10 H11 0.9800 . ? C10 H12 0.9800 . ? C11 H13 0.9800 . ? C11 H14 0.9800 . ? C11 H15 0.9800 . ? C12 C17 1.365(12) . ? C12 C13 1.400(12) . ? C13 C14 1.370(15) . ? C13 H16 0.9500 . ? C14 C15 1.372(14) . ? C14 H17 0.9500 . ? C15 C16 1.394(13) . ? C15 H18 0.9500 . ? C16 C17 1.411(11) . ? C18 H19 0.9800 . ? C18 H20 0.9800 . ? C18 H21 0.9800 . ? C19 H22 0.9800 . ? C19 H23 0.9800 . ? C19 H24 0.9800 . ? C21 C25 1.418(14) . ? C21 C22 1.443(12) . ? C21 C26 1.453(14) . ? C22 C23 1.423(13) . ? C22 C27 1.518(14) . ? C23 C24 1.390(15) . ? C23 C28 1.509(13) . ? C24 C25 1.438(13) . ? C24 C29 1.525(16) . ? C25 C30 1.484(14) . ? C26 H25 0.9800 . ? C26 H26 0.9800 . ? C26 H27 0.9800 . ? C27 H28 0.9800 . ? C27 H29 0.9800 . ? C27 H30 0.9800 . ? C28 H31 0.9800 . ? C28 H32 0.9800 . ? C28 H33 0.9800 . ? C29 H34 0.9800 . ? C29 H35 0.9800 . ? C29 H36 0.9800 . ? C30 H37 0.9800 . ? C30 H38 0.9800 . ? C30 H39 0.9800 . ? 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 C20 W1 C23 87.3(4) . . ? C20 W1 C22 82.9(4) . . ? C23 W1 C22 36.5(3) . . ? C20 W1 O1 128.5(3) . . ? C23 W1 O1 141.9(3) . . ? C22 W1 O1 142.8(3) . . ? C20 W1 C24 120.8(5) . . ? C23 W1 C24 34.9(4) . . ? C22 W1 C24 58.5(3) . . ? O1 W1 C24 107.0(3) . . ? C20 W1 C21 113.6(4) . . ? C23 W1 C21 60.2(3) . . ? C22 W1 C21 36.0(3) . . ? O1 W1 C21 106.8(3) . . ? C24 W1 C21 58.2(4) . . ? C20 W1 C25 141.4(3) . . ? C23 W1 C25 59.4(3) . . ? C22 W1 C25 58.9(3) . . ? O1 W1 C25 89.1(3) . . ? C24 W1 C25 35.3(3) . . ? C21 W1 C25 34.6(3) . . ? C20 W1 Si1 81.1(4) . . ? C23 W1 Si1 135.1(3) . . ? C22 W1 Si1 98.8(2) . . ? O1 W1 Si1 71.63(15) . . ? C24 W1 Si1 142.1(3) . . ? C21 W1 Si1 85.3(2) . . ? C25 W1 Si1 107.9(3) . . ? C20 W1 Si2 65.6(3) . . ? C23 W1 Si2 115.5(2) . . ? C22 W1 Si2 140.8(2) . . ? O1 W1 Si2 76.29(15) . . ? C24 W1 Si2 118.1(3) . . ? C21 W1 Si2 175.6(2) . . ? C25 W1 Si2 143.8(3) . . ? Si1 W1 Si2 98.76(9) . . ? C1 Si1 C3 99.3(5) . . ? C1 Si1 C2 103.1(6) . . ? C3 Si1 C2 110.6(5) . . ? C1 Si1 W1 117.0(5) . . ? C3 Si1 W1 100.0(3) . . ? C2 Si1 W1 124.1(4) . . ? C12 Si2 C19 107.1(5) . . ? C12 Si2 C18 104.5(6) . . ? C19 Si2 C18 103.2(7) . . ? C12 Si2 W1 99.4(3) . . ? C19 Si2 W1 114.8(4) . . ? C18 Si2 W1 126.1(6) . . ? C8 O1 C17 113.4(6) . . ? C8 O1 W1 122.0(4) . . ? C17 O1 W1 121.6(4) . . ? Si1 C1 H1 109.5 . . ? Si1 C1 H2 109.5 . . ? H1 C1 H2 109.5 . . ? Si1 C1 H3 109.5 . . ? H1 C1 H3 109.5 . . ? H2 C1 H3 109.5 . . ? Si1 C2 H4 109.5 . . ? Si1 C2 H5 109.5 . . ? H4 C2 H5 109.5 . . ? Si1 C2 H6 109.5 . . ? H4 C2 H6 109.5 . . ? H5 C2 H6 109.5 . . ? C4 C3 C8 115.0(9) . . ? C4 C3 Si1 130.1(8) . . ? C8 C3 Si1 114.6(7) . . ? C3 C4 C5 122.1(10) . . ? C3 C4 H7 118.9 . . ? C5 C4 H7 118.9 . . ? C4 C5 C6 119.8(9) . . ? C4 C5 H8 120.1 . . ? C6 C5 H8 120.1 . . ? C7 C6 C5 119.9(9) . . ? C7 C6 H9 120.0 . . ? C5 C6 H9 120.0 . . ? C6 C7 C8 117.7(9) . . ? C6 C7 C9 122.7(8) . . ? C8 C7 C9 119.6(8) . . ? C7 C8 C3 125.3(8) . . ? C7 C8 O1 118.5(7) . . ? C3 C8 O1 116.1(7) . . ? C10 C9 C16 113.2(8) . . ? C10 C9 C7 112.9(9) . . ? C16 C9 C7 105.2(7) . . ? C10 C9 C11 108.8(8) . . ? C16 C9 C11 106.6(9) . . ? C7 C9 C11 109.9(8) . . ? C9 C10 H10 109.5 . . ? C9 C10 H11 109.5 . . ? H10 C10 H11 109.5 . . ? C9 C10 H12 109.5 . . ? H10 C10 H12 109.5 . . ? H11 C10 H12 109.5 . . ? C9 C11 H13 109.5 . . ? C9 C11 H14 109.5 . . ? H13 C11 H14 109.5 . . ? C9 C11 H15 109.5 . . ? H13 C11 H15 109.5 . . ? H14 C11 H15 109.5 . . ? C17 C12 C13 114.7(8) . . ? C17 C12 Si2 121.2(6) . . ? C13 C12 Si2 123.8(7) . . ? C14 C13 C12 121.7(9) . . ? C14 C13 H16 119.1 . . ? C12 C13 H16 119.1 . . ? C13 C14 C15 120.5(9) . . ? C13 C14 H17 119.8 . . ? C15 C14 H17 119.8 . . ? C14 C15 C16 122.1(9) . . ? C14 C15 H18 119.0 . . ? C16 C15 H18 119.0 . . ? C15 C16 C17 113.7(10) . . ? C15 C16 C9 124.6(8) . . ? C17 C16 C9 121.7(8) . . ? C12 C17 C16 127.3(8) . . ? C12 C17 O1 117.5(6) . . ? C16 C17 O1 115.2(8) . . ? Si2 C18 H19 109.5 . . ? Si2 C18 H20 109.5 . . ? H19 C18 H20 109.5 . . ? Si2 C18 H21 109.5 . . ? H19 C18 H21 109.5 . . ? H20 C18 H21 109.5 . . ? Si2 C19 H22 109.5 . . ? Si2 C19 H23 109.5 . . ? H22 C19 H23 109.5 . . ? Si2 C19 H24 109.5 . . ? H22 C19 H24 109.5 . . ? H23 C19 H24 109.5 . . ? O2 C20 W1 176.0(9) . . ? C25 C21 C22 106.5(8) . . ? C25 C21 C26 123.2(10) . . ? C22 C21 C26 128.9(10) . . ? C25 C21 W1 72.8(5) . . ? C22 C21 W1 67.9(5) . . ? C26 C21 W1 134.8(7) . . ? C23 C22 C21 109.0(8) . . ? C23 C22 C27 125.7(8) . . ? C21 C22 C27 124.2(9) . . ? C23 C22 W1 71.6(5) . . ? C21 C22 W1 76.1(5) . . ? C27 C22 W1 127.7(7) . . ? C24 C23 C22 107.2(9) . . ? C24 C23 C28 127.4(11) . . ? C22 C23 C28 124.3(9) . . ? C24 C23 W1 75.9(6) . . ? C22 C23 W1 72.0(5) . . ? C28 C23 W1 126.9(7) . . ? C23 C24 C25 109.5(9) . . ? C23 C24 C29 126.3(13) . . ? C25 C24 C29 124.2(12) . . ? C23 C24 W1 69.2(6) . . ? C25 C24 W1 73.5(7) . . ? C29 C24 W1 125.0(7) . . ? C21 C25 C24 107.7(9) . . ? C21 C25 C30 125.4(11) . . ? C24 C25 C30 126.4(12) . . ? C21 C25 W1 72.6(5) . . ? C24 C25 W1 71.2(7) . . ? C30 C25 W1 128.0(6) . . ? C21 C26 H25 109.5 . . ? C21 C26 H26 109.5 . . ? H25 C26 H26 109.5 . . ? C21 C26 H27 109.5 . . ? H25 C26 H27 109.5 . . ? H26 C26 H27 109.5 . . ? C22 C27 H28 109.5 . . ? C22 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? C22 C27 H30 109.5 . . ? H28 C27 H30 109.5 . . ? H29 C27 H30 109.5 . . ? C23 C28 H31 109.5 . . ? C23 C28 H32 109.5 . . ? H31 C28 H32 109.5 . . ? C23 C28 H33 109.5 . . ? H31 C28 H33 109.5 . . ? H32 C28 H33 109.5 . . ? C24 C29 H34 109.5 . . ? C24 C29 H35 109.5 . . ? H34 C29 H35 109.5 . . ? C24 C29 H36 109.5 . . ? H34 C29 H36 109.5 . . ? H35 C29 H36 109.5 . . ? C25 C30 H37 109.5 . . ? C25 C30 H38 109.5 . . ? H37 C30 H38 109.5 . . ? C25 C30 H39 109.5 . . ? H37 C30 H39 109.5 . . ? H38 C30 H39 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 W1 Si1 C1 58.9(6) . . . . ? C23 W1 Si1 C1 135.8(6) . . . . ? C22 W1 Si1 C1 140.2(5) . . . . ? O1 W1 Si1 C1 -76.9(5) . . . . ? C24 W1 Si1 C1 -171.2(7) . . . . ? C21 W1 Si1 C1 173.7(5) . . . . ? C25 W1 Si1 C1 -159.8(5) . . . . ? Si2 W1 Si1 C1 -4.6(5) . . . . ? C20 W1 Si1 C3 164.8(4) . . . . ? C23 W1 Si1 C3 -118.2(4) . . . . ? C22 W1 Si1 C3 -113.8(4) . . . . ? O1 W1 Si1 C3 29.1(3) . . . . ? C24 W1 Si1 C3 -65.2(5) . . . . ? C21 W1 Si1 C3 -80.4(4) . . . . ? C25 W1 Si1 C3 -53.8(4) . . . . ? Si2 W1 Si1 C3 101.4(3) . . . . ? C20 W1 Si1 C2 -71.7(6) . . . . ? C23 W1 Si1 C2 5.3(7) . . . . ? C22 W1 Si1 C2 9.6(6) . . . . ? O1 W1 Si1 C2 152.5(6) . . . . ? C24 W1 Si1 C2 58.3(7) . . . . ? C21 W1 Si1 C2 43.1(6) . . . . ? C25 W1 Si1 C2 69.6(6) . . . . ? Si2 W1 Si1 C2 -135.2(6) . . . . ? C20 W1 Si2 C12 -155.4(5) . . . . ? C23 W1 Si2 C12 130.5(4) . . . . ? C22 W1 Si2 C12 164.9(4) . . . . ? O1 W1 Si2 C12 -10.9(3) . . . . ? C24 W1 Si2 C12 91.3(4) . . . . ? C21 W1 Si2 C12 124(3) . . . . ? C25 W1 Si2 C12 58.1(5) . . . . ? Si1 W1 Si2 C12 -79.4(3) . . . . ? C20 W1 Si2 C19 90.7(6) . . . . ? C23 W1 Si2 C19 16.6(6) . . . . ? C22 W1 Si2 C19 51.0(6) . . . . ? O1 W1 Si2 C19 -124.8(5) . . . . ? C24 W1 Si2 C19 -22.6(6) . . . . ? C21 W1 Si2 C19 10(3) . . . . ? C25 W1 Si2 C19 -55.8(6) . . . . ? Si1 W1 Si2 C19 166.7(5) . . . . ? C20 W1 Si2 C18 -39.7(7) . . . . ? C23 W1 Si2 C18 -113.9(7) . . . . ? C22 W1 Si2 C18 -79.4(7) . . . . ? O1 W1 Si2 C18 104.8(6) . . . . ? C24 W1 Si2 C18 -153.0(7) . . . . ? C21 W1 Si2 C18 -121(3) . . . . ? C25 W1 Si2 C18 173.8(7) . . . . ? Si1 W1 Si2 C18 36.3(6) . . . . ? C20 W1 O1 C8 -97.3(7) . . . . ? C23 W1 O1 C8 106.2(6) . . . . ? C22 W1 O1 C8 44.6(8) . . . . ? C24 W1 O1 C8 104.6(6) . . . . ? C21 W1 O1 C8 43.5(6) . . . . ? C25 W1 O1 C8 73.7(6) . . . . ? Si1 W1 O1 C8 -35.6(5) . . . . ? Si2 W1 O1 C8 -139.8(6) . . . . ? C20 W1 O1 C17 62.0(7) . . . . ? C23 W1 O1 C17 -94.4(6) . . . . ? C22 W1 O1 C17 -156.0(5) . . . . ? C24 W1 O1 C17 -96.1(6) . . . . ? C21 W1 O1 C17 -157.2(5) . . . . ? C25 W1 O1 C17 -127.0(6) . . . . ? Si1 W1 O1 C17 123.8(5) . . . . ? Si2 W1 O1 C17 19.5(5) . . . . ? C1 Si1 C3 C4 -84.4(10) . . . . ? C2 Si1 C3 C4 23.4(10) . . . . ? W1 Si1 C3 C4 155.8(8) . . . . ? C1 Si1 C3 C8 88.7(8) . . . . ? C2 Si1 C3 C8 -163.4(7) . . . . ? W1 Si1 C3 C8 -31.0(6) . . . . ? C8 C3 C4 C5 -2.7(14) . . . . ? Si1 C3 C4 C5 170.5(8) . . . . ? C3 C4 C5 C6 -0.7(16) . . . . ? C4 C5 C6 C7 1.5(16) . . . . ? C5 C6 C7 C8 1.1(14) . . . . ? C5 C6 C7 C9 -179.5(9) . . . . ? C6 C7 C8 C3 -5.0(13) . . . . ? C9 C7 C8 C3 175.7(8) . . . . ? C6 C7 C8 O1 178.7(8) . . . . ? C9 C7 C8 O1 -0.6(11) . . . . ? C4 C3 C8 C7 5.7(13) . . . . ? Si1 C3 C8 C7 -168.5(7) . . . . ? C4 C3 C8 O1 -177.9(7) . . . . ? Si1 C3 C8 O1 7.8(9) . . . . ? C17 O1 C8 C7 41.9(9) . . . . ? W1 O1 C8 C7 -157.2(6) . . . . ? C17 O1 C8 C3 -134.8(7) . . . . ? W1 O1 C8 C3 26.1(9) . . . . ? C6 C7 C9 C10 19.7(13) . . . . ? C8 C7 C9 C10 -161.0(8) . . . . ? C6 C7 C9 C16 143.6(9) . . . . ? C8 C7 C9 C16 -37.1(10) . . . . ? C6 C7 C9 C11 -102.0(11) . . . . ? C8 C7 C9 C11 77.3(10) . . . . ? C19 Si2 C12 C17 125.1(7) . . . . ? C18 Si2 C12 C17 -125.8(9) . . . . ? W1 Si2 C12 C17 5.4(7) . . . . ? C19 Si2 C12 C13 -48.1(8) . . . . ? C18 Si2 C12 C13 61.0(10) . . . . ? W1 Si2 C12 C13 -167.8(7) . . . . ? C17 C12 C13 C14 -2.1(12) . . . . ? Si2 C12 C13 C14 171.5(7) . . . . ? C12 C13 C14 C15 2.1(14) . . . . ? C13 C14 C15 C16 -0.5(14) . . . . ? C14 C15 C16 C17 -0.8(12) . . . . ? C14 C15 C16 C9 -179.5(9) . . . . ? C10 C9 C16 C15 -18.7(13) . . . . ? C7 C9 C16 C15 -142.4(9) . . . . ? C11 C9 C16 C15 100.9(10) . . . . ? C10 C9 C16 C17 162.8(9) . . . . ? C7 C9 C16 C17 39.1(11) . . . . ? C11 C9 C16 C17 -77.6(10) . . . . ? C13 C12 C17 C16 0.7(12) . . . . ? Si2 C12 C17 C16 -173.1(7) . . . . ? C13 C12 C17 O1 -177.1(7) . . . . ? Si2 C12 C17 O1 9.1(10) . . . . ? C15 C16 C17 C12 0.7(12) . . . . ? C9 C16 C17 C12 179.4(8) . . . . ? C15 C16 C17 O1 178.6(7) . . . . ? C9 C16 C17 O1 -2.7(11) . . . . ? C8 O1 C17 C12 138.6(7) . . . . ? W1 O1 C17 C12 -22.4(9) . . . . ? C8 O1 C17 C16 -39.5(9) . . . . ? W1 O1 C17 C16 159.5(5) . . . . ? C23 W1 C20 O2 -20(16) . . . . ? C22 W1 C20 O2 16(16) . . . . ? O1 W1 C20 O2 174(16) . . . . ? C24 W1 C20 O2 -30(16) . . . . ? C21 W1 C20 O2 36(16) . . . . ? C25 W1 C20 O2 9(16) . . . . ? Si1 W1 C20 O2 117(16) . . . . ? Si2 W1 C20 O2 -140(16) . . . . ? C20 W1 C21 C25 -150.3(6) . . . . ? C23 W1 C21 C25 -78.4(6) . . . . ? C22 W1 C21 C25 -116.5(8) . . . . ? O1 W1 C21 C25 62.3(5) . . . . ? C24 W1 C21 C25 -37.6(5) . . . . ? Si1 W1 C21 C25 131.5(5) . . . . ? Si2 W1 C21 C25 -71(3) . . . . ? C20 W1 C21 C22 -33.8(7) . . . . ? C23 W1 C21 C22 38.1(5) . . . . ? O1 W1 C21 C22 178.8(5) . . . . ? C24 W1 C21 C22 78.9(6) . . . . ? C25 W1 C21 C22 116.5(8) . . . . ? Si1 W1 C21 C22 -112.0(5) . . . . ? Si2 W1 C21 C22 45(3) . . . . ? C20 W1 C21 C26 89.6(12) . . . . ? C23 W1 C21 C26 161.5(12) . . . . ? C22 W1 C21 C26 123.5(13) . . . . ? O1 W1 C21 C26 -57.7(12) . . . . ? C24 W1 C21 C26 -157.6(13) . . . . ? C25 W1 C21 C26 -120.0(13) . . . . ? Si1 W1 C21 C26 11.5(11) . . . . ? Si2 W1 C21 C26 169(2) . . . . ? C25 C21 C22 C23 -1.5(10) . . . . ? C26 C21 C22 C23 165.0(9) . . . . ? W1 C21 C22 C23 -64.5(6) . . . . ? C25 C21 C22 C27 -170.6(9) . . . . ? C26 C21 C22 C27 -4.1(15) . . . . ? W1 C21 C22 C27 126.4(10) . . . . ? C25 C21 C22 W1 63.0(6) . . . . ? C26 C21 C22 W1 -130.5(9) . . . . ? C20 W1 C22 C23 -95.0(6) . . . . ? O1 W1 C22 C23 114.0(5) . . . . ? C24 W1 C22 C23 37.9(6) . . . . ? C21 W1 C22 C23 115.9(8) . . . . ? C25 W1 C22 C23 79.5(6) . . . . ? Si1 W1 C22 C23 -174.8(5) . . . . ? Si2 W1 C22 C23 -59.1(7) . . . . ? C20 W1 C22 C21 149.1(6) . . . . ? C23 W1 C22 C21 -115.9(8) . . . . ? O1 W1 C22 C21 -1.9(8) . . . . ? C24 W1 C22 C21 -78.0(6) . . . . ? C25 W1 C22 C21 -36.4(5) . . . . ? Si1 W1 C22 C21 69.3(5) . . . . ? Si2 W1 C22 C21 -175.0(4) . . . . ? C20 W1 C22 C27 26.3(9) . . . . ? C23 W1 C22 C27 121.4(10) . . . . ? O1 W1 C22 C27 -124.6(9) . . . . ? C24 W1 C22 C27 159.3(10) . . . . ? C21 W1 C22 C27 -122.7(11) . . . . ? C25 W1 C22 C27 -159.2(10) . . . . ? Si1 W1 C22 C27 -53.5(9) . . . . ? Si2 W1 C22 C27 62.2(10) . . . . ? C21 C22 C23 C24 -0.9(11) . . . . ? C27 C22 C23 C24 168.0(10) . . . . ? W1 C22 C23 C24 -68.4(7) . . . . ? C21 C22 C23 C28 -169.7(9) . . . . ? C27 C22 C23 C28 -0.8(16) . . . . ? W1 C22 C23 C28 122.8(10) . . . . ? C21 C22 C23 W1 67.5(6) . . . . ? C27 C22 C23 W1 -123.6(10) . . . . ? C20 W1 C23 C24 -164.5(7) . . . . ? C22 W1 C23 C24 113.7(8) . . . . ? O1 W1 C23 C24 -2.8(8) . . . . ? C21 W1 C23 C24 76.2(7) . . . . ? C25 W1 C23 C24 35.9(5) . . . . ? Si1 W1 C23 C24 121.0(6) . . . . ? Si2 W1 C23 C24 -103.2(6) . . . . ? C20 W1 C23 C22 81.7(6) . . . . ? O1 W1 C23 C22 -116.5(5) . . . . ? C24 W1 C23 C22 -113.7(8) . . . . ? C21 W1 C23 C22 -37.6(5) . . . . ? C25 W1 C23 C22 -77.8(6) . . . . ? Si1 W1 C23 C22 7.2(6) . . . . ? Si2 W1 C23 C22 143.0(4) . . . . ? C20 W1 C23 C28 -38.0(10) . . . . ? C22 W1 C23 C28 -119.7(11) . . . . ? O1 W1 C23 C28 123.7(9) . . . . ? C24 W1 C23 C28 126.5(13) . . . . ? C21 W1 C23 C28 -157.3(11) . . . . ? C25 W1 C23 C28 162.4(11) . . . . ? Si1 W1 C23 C28 -112.5(9) . . . . ? Si2 W1 C23 C28 23.3(11) . . . . ? C22 C23 C24 C25 2.9(12) . . . . ? C28 C23 C24 C25 171.3(10) . . . . ? W1 C23 C24 C25 -62.7(8) . . . . ? C22 C23 C24 C29 -175.5(10) . . . . ? C28 C23 C24 C29 -7.1(17) . . . . ? W1 C23 C24 C29 118.8(11) . . . . ? C22 C23 C24 W1 65.7(6) . . . . ? C28 C23 C24 W1 -126.0(10) . . . . ? C20 W1 C24 C23 18.1(8) . . . . ? C22 W1 C24 C23 -39.7(6) . . . . ? O1 W1 C24 C23 178.2(5) . . . . ? C21 W1 C24 C23 -82.2(6) . . . . ? C25 W1 C24 C23 -119.1(8) . . . . ? Si1 W1 C24 C23 -100.1(7) . . . . ? Si2 W1 C24 C23 95.0(6) . . . . ? C20 W1 C24 C25 137.1(6) . . . . ? C23 W1 C24 C25 119.1(8) . . . . ? C22 W1 C24 C25 79.4(6) . . . . ? O1 W1 C24 C25 -62.7(6) . . . . ? C21 W1 C24 C25 36.8(5) . . . . ? Si1 W1 C24 C25 19.0(8) . . . . ? Si2 W1 C24 C25 -146.0(5) . . . . ? C20 W1 C24 C29 -102.4(12) . . . . ? C23 W1 C24 C29 -120.5(15) . . . . ? C22 W1 C24 C29 -160.1(14) . . . . ? O1 W1 C24 C29 57.7(13) . . . . ? C21 W1 C24 C29 157.3(14) . . . . ? C25 W1 C24 C29 120.5(15) . . . . ? Si1 W1 C24 C29 139.4(11) . . . . ? Si2 W1 C24 C29 -25.5(13) . . . . ? C22 C21 C25 C24 3.2(11) . . . . ? C26 C21 C25 C24 -164.2(9) . . . . ? W1 C21 C25 C24 63.1(8) . . . . ? C22 C21 C25 C30 175.5(9) . . . . ? C26 C21 C25 C30 8.1(14) . . . . ? W1 C21 C25 C30 -124.6(9) . . . . ? C22 C21 C25 W1 -59.9(6) . . . . ? C26 C21 C25 W1 132.7(9) . . . . ? C23 C24 C25 C21 -3.9(12) . . . . ? C29 C24 C25 C21 174.6(9) . . . . ? W1 C24 C25 C21 -64.0(6) . . . . ? C23 C24 C25 C30 -176.1(8) . . . . ? C29 C24 C25 C30 2.4(18) . . . . ? W1 C24 C25 C30 123.8(10) . . . . ? C23 C24 C25 W1 60.1(8) . . . . ? C29 C24 C25 W1 -121.5(11) . . . . ? C20 W1 C25 C21 46.7(9) . . . . ? C23 W1 C25 C21 80.7(6) . . . . ? C22 W1 C25 C21 37.9(5) . . . . ? O1 W1 C25 C21 -122.0(5) . . . . ? C24 W1 C25 C21 116.2(8) . . . . ? Si1 W1 C25 C21 -51.7(5) . . . . ? Si2 W1 C25 C21 172.9(4) . . . . ? C20 W1 C25 C24 -69.6(9) . . . . ? C23 W1 C25 C24 -35.5(6) . . . . ? C22 W1 C25 C24 -78.3(6) . . . . ? O1 W1 C25 C24 121.7(6) . . . . ? C21 W1 C25 C24 -116.2(8) . . . . ? Si1 W1 C25 C24 -167.9(5) . . . . ? Si2 W1 C25 C24 56.7(7) . . . . ? C20 W1 C25 C30 168.4(11) . . . . ? C23 W1 C25 C30 -157.6(13) . . . . ? C22 W1 C25 C30 159.6(13) . . . . ? O1 W1 C25 C30 -0.3(11) . . . . ? C24 W1 C25 C30 -122.1(14) . . . . ? C21 W1 C25 C30 121.7(14) . . . . ? Si1 W1 C25 C30 70.0(12) . . . . ? Si2 W1 C25 C30 -65.4(13) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.210 _refine_diff_density_min -2.194 _refine_diff_density_rms 0.172 #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 284201' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H49 N O2 Si2 W' _chemical_formula_weight 755.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_int_tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.3139(5) _cell_length_b 14.8370(5) _cell_length_c 20.5961(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3457.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 39058 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 3.441 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5461 _exptl_absorpt_correction_T_max 0.5461 _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32360 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0461 _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 -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7893 _reflns_number_gt 7677 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+3.4298P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 7893 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.133624(18) 0.765662(15) 0.330290(10) 0.02733(8) Uani 1 1 d . . . Si1 Si 0.08734(14) 0.75397(11) 0.20440(8) 0.0302(3) Uani 1 1 d . . . Si2 Si 0.38126(16) 0.59661(12) 0.29752(9) 0.0361(4) Uani 1 1 d . . . O1 O 0.3392(3) 0.6881(3) 0.1695(2) 0.0365(9) Uani 1 1 d . . . O2 O 0.1261(7) 0.9489(3) 0.2595(3) 0.0572(14) Uani 1 1 d . . . N1 N 0.3065(4) 0.6938(4) 0.3217(3) 0.0355(11) Uani 1 1 d . . . C1 C 0.3149(5) 0.7750(4) 0.3386(3) 0.0332(12) Uani 1 1 d . . . C2 C 0.4216(6) 0.8364(5) 0.3453(4) 0.0440(16) Uani 1 1 d . . . C3 C 0.3906(9) 0.9195(6) 0.3849(5) 0.063(2) Uani 1 1 d . . . H1 H 0.3691 0.9014 0.4291 0.095 Uiso 1 1 calc R . . H2 H 0.3237 0.9507 0.3646 0.095 Uiso 1 1 calc R . . H3 H 0.4589 0.9600 0.3864 0.095 Uiso 1 1 calc R . . C4 C 0.4506(8) 0.8661(6) 0.2750(4) 0.059(2) Uani 1 1 d . . . H4 H 0.5186 0.9071 0.2755 0.088 Uiso 1 1 calc R . . H5 H 0.3821 0.8971 0.2563 0.088 Uiso 1 1 calc R . . H6 H 0.4695 0.8130 0.2487 0.088 Uiso 1 1 calc R . . C5 C 0.5258(7) 0.7879(8) 0.3759(6) 0.076(3) Uani 1 1 d . . . H7 H 0.5918 0.8301 0.3810 0.114 Uiso 1 1 calc R . . H8 H 0.5501 0.7378 0.3480 0.114 Uiso 1 1 calc R . . H9 H 0.5027 0.7646 0.4186 0.114 Uiso 1 1 calc R . . C6 C -0.0573(6) 0.8138(6) 0.1867(4) 0.0470(17) Uani 1 1 d . . . H10 H -0.0504 0.8774 0.1990 0.071 Uiso 1 1 calc R . . H11 H -0.1209 0.7857 0.2118 0.071 Uiso 1 1 calc R . . H12 H -0.0751 0.8093 0.1403 0.071 Uiso 1 1 calc R . . C7 C 0.0620(7) 0.6392(5) 0.1665(4) 0.0471(15) Uani 1 1 d . . . H13 H 0.0229 0.6465 0.1244 0.071 Uiso 1 1 calc R . . H14 H 0.0119 0.6029 0.1952 0.071 Uiso 1 1 calc R . . H15 H 0.1381 0.6088 0.1604 0.071 Uiso 1 1 calc R . . C8 C 0.2017(5) 0.8044(4) 0.1474(3) 0.0324(12) Uani 1 1 d . . . C9 C 0.1765(6) 0.8828(5) 0.1125(3) 0.0402(14) Uani 1 1 d . . . H16 H 0.1056 0.9147 0.1217 0.048 Uiso 1 1 calc R . . C10 C 0.2510(8) 0.9155(5) 0.0651(4) 0.0514(18) Uani 1 1 d . . . H17 H 0.2311 0.9693 0.0426 0.062 Uiso 1 1 calc R . . C11 C 0.3555(7) 0.8701(5) 0.0501(4) 0.0442(15) Uani 1 1 d . . . H18 H 0.4061 0.8928 0.0171 0.053 Uiso 1 1 calc R . . C12 C 0.3856(6) 0.7922(5) 0.0832(3) 0.0380(13) Uani 1 1 d . . . C13 C 0.3098(5) 0.7627(5) 0.1324(3) 0.0327(11) Uani 1 1 d . . . C14 C 0.4902(6) 0.7335(6) 0.0652(3) 0.0474(16) Uani 1 1 d . . . C15 C 0.5849(8) 0.7855(7) 0.0276(5) 0.069(3) Uani 1 1 d . . . H19 H 0.6150 0.8349 0.0546 0.104 Uiso 1 1 calc R . . H20 H 0.5504 0.8102 -0.0122 0.104 Uiso 1 1 calc R . . H21 H 0.6500 0.7448 0.0165 0.104 Uiso 1 1 calc R . . C16 C 0.4434(9) 0.6545(7) 0.0208(4) 0.066(2) Uani 1 1 d . . . H22 H 0.5070 0.6108 0.0136 0.099 Uiso 1 1 calc R . . H23 H 0.4173 0.6791 -0.0209 0.099 Uiso 1 1 calc R . . H24 H 0.3768 0.6246 0.0423 0.099 Uiso 1 1 calc R . . C17 C 0.4920(6) 0.6243(4) 0.2328(3) 0.0372(13) Uani 1 1 d . . . C18 C 0.6120(6) 0.6038(5) 0.2399(4) 0.0470(17) Uani 1 1 d . . . H25 H 0.6381 0.5727 0.2776 0.056 Uiso 1 1 calc R . . C19 C 0.6932(6) 0.6281(6) 0.1928(5) 0.056(2) Uani 1 1 d . . . H26 H 0.7746 0.6149 0.1989 0.067 Uiso 1 1 calc R . . C20 C 0.6565(6) 0.6717(6) 0.1367(4) 0.0514(18) Uani 1 1 d . . . H27 H 0.7130 0.6879 0.1046 0.062 Uiso 1 1 calc R . . C21 C 0.5377(6) 0.6921(5) 0.1270(4) 0.0404(14) Uani 1 1 d . . . C22 C 0.4584(5) 0.6678(4) 0.1758(3) 0.0351(12) Uani 1 1 d . . . C23 C 0.2692(7) 0.5136(5) 0.2688(5) 0.056(2) Uani 1 1 d . . . H28 H 0.2864 0.4543 0.2876 0.084 Uiso 1 1 calc R . . H29 H 0.2720 0.5097 0.2214 0.084 Uiso 1 1 calc R . . H30 H 0.1903 0.5331 0.2825 0.084 Uiso 1 1 calc R . . C24 C 0.4584(9) 0.5478(7) 0.3697(4) 0.066(3) Uani 1 1 d . . . H31 H 0.5299 0.5830 0.3789 0.099 Uiso 1 1 calc R . . H32 H 0.4803 0.4852 0.3606 0.099 Uiso 1 1 calc R . . H33 H 0.4056 0.5498 0.4073 0.099 Uiso 1 1 calc R . . C25 C 0.1311(7) 0.8771(4) 0.2833(3) 0.0374(12) Uani 1 1 d . . . C26 C -0.0358(6) 0.7086(5) 0.3844(3) 0.0429(15) Uani 1 1 d . . . C27 C -0.0369(6) 0.8058(5) 0.3862(3) 0.0378(13) Uani 1 1 d . . . C28 C 0.0615(7) 0.8342(5) 0.4226(3) 0.0430(16) Uani 1 1 d . . . C29 C 0.1244(6) 0.7562(6) 0.4451(3) 0.0489(17) Uani 1 1 d . . . C30 C 0.0639(7) 0.6791(5) 0.4207(4) 0.0451(16) Uani 1 1 d . . . C31 C -0.1284(10) 0.6499(7) 0.3547(5) 0.067(3) Uani 1 1 d . . . H34 H -0.0914 0.5954 0.3371 0.101 Uiso 1 1 calc R . . H35 H -0.1680 0.6828 0.3196 0.101 Uiso 1 1 calc R . . H36 H -0.1864 0.6331 0.3879 0.101 Uiso 1 1 calc R . . C32 C -0.1329(8) 0.8657(7) 0.3616(4) 0.058(2) Uani 1 1 d . . . H37 H -0.1894 0.8778 0.3966 0.087 Uiso 1 1 calc R . . H38 H -0.1737 0.8360 0.3255 0.087 Uiso 1 1 calc R . . H39 H -0.0986 0.9226 0.3465 0.087 Uiso 1 1 calc R . . C33 C 0.0827(10) 0.9304(7) 0.4430(5) 0.071(3) Uani 1 1 d . . . H40 H 0.0712 0.9704 0.4056 0.106 Uiso 1 1 calc R . . H41 H 0.1638 0.9367 0.4591 0.106 Uiso 1 1 calc R . . H42 H 0.0270 0.9467 0.4774 0.106 Uiso 1 1 calc R . . C34 C 0.2291(8) 0.7530(11) 0.4893(4) 0.084(4) Uani 1 1 d . . . H43 H 0.2091 0.7819 0.5307 0.126 Uiso 1 1 calc R . . H44 H 0.2955 0.7850 0.4692 0.126 Uiso 1 1 calc R . . H45 H 0.2514 0.6901 0.4971 0.126 Uiso 1 1 calc R . . C35 C 0.0947(12) 0.5812(7) 0.4343(5) 0.079(3) Uani 1 1 d . . . H46 H 0.1787 0.5712 0.4254 0.118 Uiso 1 1 calc R . . H47 H 0.0470 0.5420 0.4064 0.118 Uiso 1 1 calc R . . H48 H 0.0781 0.5674 0.4799 0.118 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 0.02888(11) 0.03000(11) 0.02311(11) 0.00022(8) 0.00048(8) -0.00205(7) Si1 0.0288(7) 0.0368(9) 0.0250(7) 0.0001(6) -0.0024(6) -0.0015(6) Si2 0.0335(8) 0.0344(8) 0.0404(9) 0.0081(7) 0.0012(8) 0.0042(7) O1 0.0303(19) 0.038(2) 0.041(2) 0.010(2) 0.0033(18) 0.0028(15) O2 0.086(4) 0.034(2) 0.052(3) 0.005(2) -0.007(3) 0.000(3) N1 0.029(2) 0.040(3) 0.037(3) 0.000(2) -0.004(2) 0.002(2) C1 0.032(3) 0.039(3) 0.029(3) 0.004(3) -0.003(2) -0.002(2) C2 0.033(3) 0.051(4) 0.048(4) -0.003(3) -0.007(3) -0.011(3) C3 0.066(5) 0.056(5) 0.068(5) -0.013(4) -0.005(5) -0.024(4) C4 0.062(5) 0.055(5) 0.060(5) -0.007(4) 0.015(4) -0.023(4) C5 0.045(4) 0.078(7) 0.106(8) -0.001(6) -0.025(5) -0.012(4) C6 0.036(3) 0.066(5) 0.040(3) 0.003(3) -0.008(3) 0.005(3) C7 0.057(4) 0.048(4) 0.036(3) -0.010(3) -0.006(3) -0.013(3) C8 0.036(3) 0.036(3) 0.026(3) 0.002(2) -0.004(2) -0.002(2) C9 0.044(3) 0.041(3) 0.036(3) 0.003(3) -0.001(3) 0.003(3) C10 0.067(5) 0.039(4) 0.048(4) 0.012(3) 0.004(4) 0.008(3) C11 0.048(4) 0.044(3) 0.040(3) 0.010(3) 0.012(3) -0.008(3) C12 0.040(3) 0.044(3) 0.030(3) 0.002(2) 0.005(2) -0.006(2) C13 0.036(3) 0.037(3) 0.025(2) 0.006(2) -0.003(2) -0.008(2) C14 0.047(3) 0.055(4) 0.040(3) -0.002(3) 0.020(3) -0.002(4) C15 0.057(4) 0.084(7) 0.067(5) 0.016(5) 0.034(4) -0.007(5) C16 0.078(6) 0.081(6) 0.039(4) -0.019(4) 0.006(4) 0.002(5) C17 0.030(3) 0.033(3) 0.048(4) 0.001(3) 0.002(3) 0.002(2) C18 0.038(4) 0.043(4) 0.059(4) 0.004(3) 0.000(3) 0.010(3) C19 0.027(3) 0.065(5) 0.074(6) -0.002(4) 0.001(3) 0.001(3) C20 0.030(3) 0.058(4) 0.066(5) 0.002(4) 0.012(3) 0.000(3) C21 0.036(3) 0.042(3) 0.043(4) 0.000(3) 0.005(3) -0.001(3) C22 0.028(3) 0.037(3) 0.040(3) -0.001(3) 0.005(3) 0.001(2) C23 0.041(4) 0.034(3) 0.093(7) 0.003(4) 0.010(4) -0.004(3) C24 0.067(5) 0.077(6) 0.056(5) 0.030(5) -0.001(4) 0.016(5) C25 0.050(3) 0.037(3) 0.026(2) -0.001(2) -0.002(3) -0.001(3) C26 0.042(3) 0.050(4) 0.037(3) 0.000(3) 0.011(3) -0.011(3) C27 0.034(3) 0.045(3) 0.035(3) -0.006(3) 0.007(3) 0.001(3) C28 0.046(4) 0.051(4) 0.032(3) -0.012(3) 0.012(3) -0.006(3) C29 0.045(3) 0.073(5) 0.029(3) 0.008(3) 0.006(3) -0.003(4) C30 0.049(4) 0.043(4) 0.044(4) 0.015(3) 0.010(3) 0.000(3) C31 0.069(5) 0.071(6) 0.061(5) -0.018(4) 0.019(5) -0.035(5) C32 0.043(4) 0.070(5) 0.061(5) 0.005(4) 0.014(4) 0.013(4) C33 0.080(6) 0.061(5) 0.071(6) -0.031(5) 0.020(5) -0.019(5) C34 0.063(5) 0.156(11) 0.034(3) 0.027(6) -0.015(4) -0.015(7) C35 0.098(8) 0.059(6) 0.079(7) 0.034(5) 0.021(6) 0.016(5) _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 C25 1.916(6) . ? W1 C1 2.063(6) . ? W1 N1 2.235(5) . ? W1 C28 2.306(7) . ? W1 C27 2.324(6) . ? W1 C29 2.370(7) . ? W1 C26 2.374(6) . ? W1 C30 2.395(7) . ? W1 Si1 2.6509(16) . ? Si1 C7 1.896(7) . ? Si1 C6 1.897(7) . ? Si1 C8 1.901(6) . ? Si2 N1 1.744(6) . ? Si2 C23 1.864(8) . ? Si2 C24 1.869(8) . ? Si2 C17 1.875(7) . ? O1 C13 1.387(7) . ? O1 C22 1.388(7) . ? O2 C25 1.173(8) . ? N1 C1 1.257(9) . ? C1 C2 1.519(9) . ? C2 C5 1.518(12) . ? C2 C3 1.519(12) . ? C2 C4 1.548(11) . ? C3 H1 0.9800 . ? C3 H2 0.9800 . ? C3 H3 0.9800 . ? C4 H4 0.9800 . ? C4 H5 0.9800 . ? C4 H6 0.9800 . ? C5 H7 0.9800 . ? C5 H8 0.9800 . ? C5 H9 0.9800 . ? C6 H10 0.9800 . ? C6 H11 0.9800 . ? C6 H12 0.9800 . ? C7 H13 0.9800 . ? C7 H14 0.9800 . ? C7 H15 0.9800 . ? C8 C9 1.397(9) . ? C8 C13 1.405(9) . ? C9 C10 1.377(10) . ? C9 H16 0.9500 . ? C10 C11 1.396(11) . ? C10 H17 0.9500 . ? C11 C12 1.385(10) . ? C11 H18 0.9500 . ? C12 C13 1.398(8) . ? C12 C14 1.515(10) . ? C14 C21 1.513(11) . ? C14 C15 1.531(10) . ? C14 C16 1.577(12) . ? C15 H19 0.9800 . ? C15 H20 0.9800 . ? C15 H21 0.9800 . ? C16 H22 0.9800 . ? C16 H23 0.9800 . ? C16 H24 0.9800 . ? C17 C22 1.392(10) . ? C17 C18 1.399(9) . ? C18 C19 1.385(11) . ? C18 H25 0.9500 . ? C19 C20 1.387(13) . ? C19 H26 0.9500 . ? C20 C21 1.391(9) . ? C20 H27 0.9500 . ? C21 C22 1.394(9) . ? C23 H28 0.9800 . ? C23 H29 0.9800 . ? C23 H30 0.9800 . ? C24 H31 0.9800 . ? C24 H32 0.9800 . ? C24 H33 0.9800 . ? C26 C30 1.422(11) . ? C26 C27 1.443(11) . ? C26 C31 1.492(11) . ? C27 C28 1.406(10) . ? C27 C32 1.493(11) . ? C28 C29 1.436(11) . ? C28 C33 1.506(11) . ? C29 C30 1.425(11) . ? C29 C34 1.496(10) . ? C30 C35 1.520(11) . ? C31 H34 0.9800 . ? C31 H35 0.9800 . ? C31 H36 0.9800 . ? C32 H37 0.9800 . ? C32 H38 0.9800 . ? C32 H39 0.9800 . ? C33 H40 0.9800 . ? C33 H41 0.9800 . ? C33 H42 0.9800 . ? C34 H43 0.9800 . ? C34 H44 0.9800 . ? C34 H45 0.9800 . ? C35 H46 0.9800 . ? C35 H47 0.9800 . ? C35 H48 0.9800 . ? 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 C25 W1 C1 89.9(3) . . ? C25 W1 N1 112.6(3) . . ? C1 W1 N1 33.7(2) . . ? C25 W1 C28 91.7(3) . . ? C1 W1 C28 104.7(3) . . ? N1 W1 C28 125.9(2) . . ? C25 W1 C27 91.0(3) . . ? C1 W1 C27 140.1(2) . . ? N1 W1 C27 152.6(2) . . ? C28 W1 C27 35.4(2) . . ? C25 W1 C29 123.6(3) . . ? C1 W1 C29 88.0(2) . . ? N1 W1 C29 95.1(2) . . ? C28 W1 C29 35.7(3) . . ? C27 W1 C29 59.0(2) . . ? C25 W1 C26 122.2(3) . . ? C1 W1 C26 142.0(2) . . ? N1 W1 C26 125.0(2) . . ? C28 W1 C26 59.0(3) . . ? C27 W1 C26 35.7(3) . . ? C29 W1 C26 58.4(2) . . ? C25 W1 C30 148.2(3) . . ? C1 W1 C30 107.4(2) . . ? N1 W1 C30 95.4(2) . . ? C28 W1 C30 58.6(3) . . ? C27 W1 C30 58.6(3) . . ? C29 W1 C30 34.8(3) . . ? C26 W1 C30 34.7(3) . . ? C25 W1 Si1 63.89(18) . . ? C1 W1 Si1 106.37(17) . . ? N1 W1 Si1 93.68(15) . . ? C28 W1 Si1 139.9(2) . . ? C27 W1 Si1 109.74(17) . . ? C29 W1 Si1 164.35(18) . . ? C26 W1 Si1 106.04(18) . . ? C30 W1 Si1 131.3(2) . . ? C7 Si1 C6 102.2(4) . . ? C7 Si1 C8 101.7(3) . . ? C6 Si1 C8 106.5(3) . . ? C7 Si1 W1 119.4(3) . . ? C6 Si1 W1 109.1(2) . . ? C8 Si1 W1 116.37(18) . . ? N1 Si2 C23 107.9(3) . . ? N1 Si2 C24 108.6(4) . . ? C23 Si2 C24 108.3(5) . . ? N1 Si2 C17 110.2(3) . . ? C23 Si2 C17 112.0(4) . . ? C24 Si2 C17 109.8(4) . . ? C13 O1 C22 117.2(5) . . ? C1 N1 Si2 146.5(5) . . ? C1 N1 W1 65.6(3) . . ? Si2 N1 W1 147.3(3) . . ? N1 C1 C2 131.3(6) . . ? N1 C1 W1 80.6(4) . . ? C2 C1 W1 146.9(5) . . ? C5 C2 C1 111.7(7) . . ? C5 C2 C3 109.9(8) . . ? C1 C2 C3 110.6(6) . . ? C5 C2 C4 111.0(8) . . ? C1 C2 C4 104.7(6) . . ? C3 C2 C4 108.6(7) . . ? C2 C3 H1 109.5 . . ? C2 C3 H2 109.5 . . ? H1 C3 H2 109.5 . . ? C2 C3 H3 109.5 . . ? H1 C3 H3 109.5 . . ? H2 C3 H3 109.5 . . ? C2 C4 H4 109.5 . . ? C2 C4 H5 109.5 . . ? H4 C4 H5 109.5 . . ? C2 C4 H6 109.5 . . ? H4 C4 H6 109.5 . . ? H5 C4 H6 109.5 . . ? C2 C5 H7 109.5 . . ? C2 C5 H8 109.5 . . ? H7 C5 H8 109.5 . . ? C2 C5 H9 109.5 . . ? H7 C5 H9 109.5 . . ? H8 C5 H9 109.5 . . ? Si1 C6 H10 109.5 . . ? Si1 C6 H11 109.5 . . ? H10 C6 H11 109.5 . . ? Si1 C6 H12 109.5 . . ? H10 C6 H12 109.5 . . ? H11 C6 H12 109.5 . . ? Si1 C7 H13 109.5 . . ? Si1 C7 H14 109.5 . . ? H13 C7 H14 109.5 . . ? Si1 C7 H15 109.5 . . ? H13 C7 H15 109.5 . . ? H14 C7 H15 109.5 . . ? C9 C8 C13 115.6(6) . . ? C9 C8 Si1 120.4(5) . . ? C13 C8 Si1 123.7(5) . . ? C10 C9 C8 122.2(7) . . ? C10 C9 H16 118.9 . . ? C8 C9 H16 118.9 . . ? C9 C10 C11 120.4(7) . . ? C9 C10 H17 119.8 . . ? C11 C10 H17 119.8 . . ? C12 C11 C10 120.1(6) . . ? C12 C11 H18 119.9 . . ? C10 C11 H18 119.9 . . ? C11 C12 C13 117.9(6) . . ? C11 C12 C14 123.5(6) . . ? C13 C12 C14 118.5(6) . . ? O1 C13 C12 120.2(6) . . ? O1 C13 C8 116.1(5) . . ? C12 C13 C8 123.8(6) . . ? C21 C14 C12 107.8(5) . . ? C21 C14 C15 112.4(7) . . ? C12 C14 C15 112.4(7) . . ? C21 C14 C16 107.7(7) . . ? C12 C14 C16 107.9(6) . . ? C15 C14 C16 108.5(7) . . ? C14 C15 H19 109.5 . . ? C14 C15 H20 109.5 . . ? H19 C15 H20 109.5 . . ? C14 C15 H21 109.5 . . ? H19 C15 H21 109.5 . . ? H20 C15 H21 109.5 . . ? C14 C16 H22 109.5 . . ? C14 C16 H23 109.5 . . ? H22 C16 H23 109.5 . . ? C14 C16 H24 109.5 . . ? H22 C16 H24 109.5 . . ? H23 C16 H24 109.5 . . ? C22 C17 C18 117.0(6) . . ? C22 C17 Si2 121.3(5) . . ? C18 C17 Si2 121.7(6) . . ? C19 C18 C17 120.8(7) . . ? C19 C18 H25 119.6 . . ? C17 C18 H25 119.6 . . ? C18 C19 C20 120.5(7) . . ? C18 C19 H26 119.8 . . ? C20 C19 H26 119.8 . . ? C19 C20 C21 120.6(7) . . ? C19 C20 H27 119.7 . . ? C21 C20 H27 119.7 . . ? C20 C21 C22 117.5(7) . . ? C20 C21 C14 123.5(7) . . ? C22 C21 C14 118.9(6) . . ? O1 C22 C17 116.4(6) . . ? O1 C22 C21 120.2(6) . . ? C17 C22 C21 123.5(6) . . ? Si2 C23 H28 109.5 . . ? Si2 C23 H29 109.5 . . ? H28 C23 H29 109.5 . . ? Si2 C23 H30 109.5 . . ? H28 C23 H30 109.5 . . ? H29 C23 H30 109.5 . . ? Si2 C24 H31 109.5 . . ? Si2 C24 H32 109.5 . . ? H31 C24 H32 109.5 . . ? Si2 C24 H33 109.5 . . ? H31 C24 H33 109.5 . . ? H32 C24 H33 109.5 . . ? O2 C25 W1 174.1(6) . . ? C30 C26 C27 107.4(6) . . ? C30 C26 C31 126.4(8) . . ? C27 C26 C31 126.0(8) . . ? C30 C26 W1 73.5(4) . . ? C27 C26 W1 70.3(4) . . ? C31 C26 W1 125.6(5) . . ? C28 C27 C26 107.9(7) . . ? C28 C27 C32 125.3(7) . . ? C26 C27 C32 126.3(7) . . ? C28 C27 W1 71.6(4) . . ? C26 C27 W1 74.0(4) . . ? C32 C27 W1 126.0(5) . . ? C27 C28 C29 108.8(7) . . ? C27 C28 C33 124.0(8) . . ? C29 C28 C33 126.5(8) . . ? C27 C28 W1 73.0(4) . . ? C29 C28 W1 74.6(4) . . ? C33 C28 W1 126.2(6) . . ? C30 C29 C28 107.2(6) . . ? C30 C29 C34 124.8(9) . . ? C28 C29 C34 127.9(9) . . ? C30 C29 W1 73.6(4) . . ? C28 C29 W1 69.7(4) . . ? C34 C29 W1 125.1(5) . . ? C26 C30 C29 108.7(6) . . ? C26 C30 C35 124.9(9) . . ? C29 C30 C35 126.3(8) . . ? C26 C30 W1 71.8(4) . . ? C29 C30 W1 71.6(4) . . ? C35 C30 W1 125.5(6) . . ? C26 C31 H34 109.5 . . ? C26 C31 H35 109.5 . . ? H34 C31 H35 109.5 . . ? C26 C31 H36 109.5 . . ? H34 C31 H36 109.5 . . ? H35 C31 H36 109.5 . . ? C27 C32 H37 109.5 . . ? C27 C32 H38 109.5 . . ? H37 C32 H38 109.5 . . ? C27 C32 H39 109.5 . . ? H37 C32 H39 109.5 . . ? H38 C32 H39 109.5 . . ? C28 C33 H40 109.5 . . ? C28 C33 H41 109.5 . . ? H40 C33 H41 109.5 . . ? C28 C33 H42 109.5 . . ? H40 C33 H42 109.5 . . ? H41 C33 H42 109.5 . . ? C29 C34 H43 109.5 . . ? C29 C34 H44 109.5 . . ? H43 C34 H44 109.5 . . ? C29 C34 H45 109.5 . . ? H43 C34 H45 109.5 . . ? H44 C34 H45 109.5 . . ? C30 C35 H46 109.5 . . ? C30 C35 H47 109.5 . . ? H46 C35 H47 109.5 . . ? C30 C35 H48 109.5 . . ? H46 C35 H48 109.5 . . ? H47 C35 H48 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C25 W1 Si1 C7 178.9(4) . . . . ? C1 W1 Si1 C7 97.3(3) . . . . ? N1 W1 Si1 C7 65.5(3) . . . . ? C28 W1 Si1 C7 -123.1(4) . . . . ? C27 W1 Si1 C7 -100.0(3) . . . . ? C29 W1 Si1 C7 -58.6(8) . . . . ? C26 W1 Si1 C7 -62.6(4) . . . . ? C30 W1 Si1 C7 -35.0(4) . . . . ? C25 W1 Si1 C6 -64.2(4) . . . . ? C1 W1 Si1 C6 -145.8(3) . . . . ? N1 W1 Si1 C6 -177.6(3) . . . . ? C28 W1 Si1 C6 -6.2(4) . . . . ? C27 W1 Si1 C6 16.9(3) . . . . ? C29 W1 Si1 C6 58.3(8) . . . . ? C26 W1 Si1 C6 54.3(3) . . . . ? C30 W1 Si1 C6 81.9(4) . . . . ? C25 W1 Si1 C8 56.3(3) . . . . ? C1 W1 Si1 C8 -25.3(3) . . . . ? N1 W1 Si1 C8 -57.1(3) . . . . ? C28 W1 Si1 C8 114.2(4) . . . . ? C27 W1 Si1 C8 137.4(3) . . . . ? C29 W1 Si1 C8 178.7(8) . . . . ? C26 W1 Si1 C8 174.8(3) . . . . ? C30 W1 Si1 C8 -157.6(3) . . . . ? C23 Si2 N1 C1 -169.6(9) . . . . ? C24 Si2 N1 C1 73.2(10) . . . . ? C17 Si2 N1 C1 -47.1(10) . . . . ? C23 Si2 N1 W1 -3.6(7) . . . . ? C24 Si2 N1 W1 -120.7(6) . . . . ? C17 Si2 N1 W1 119.0(6) . . . . ? C25 W1 N1 C1 51.2(5) . . . . ? C28 W1 N1 C1 -58.8(5) . . . . ? C27 W1 N1 C1 -96.4(6) . . . . ? C29 W1 N1 C1 -78.6(4) . . . . ? C26 W1 N1 C1 -133.1(4) . . . . ? C30 W1 N1 C1 -113.5(4) . . . . ? Si1 W1 N1 C1 114.4(4) . . . . ? C25 W1 N1 Si2 -120.4(6) . . . . ? C1 W1 N1 Si2 -171.6(9) . . . . ? C28 W1 N1 Si2 129.6(6) . . . . ? C27 W1 N1 Si2 92.0(8) . . . . ? C29 W1 N1 Si2 109.8(6) . . . . ? C26 W1 N1 Si2 55.3(7) . . . . ? C30 W1 N1 Si2 74.8(6) . . . . ? Si1 W1 N1 Si2 -57.3(6) . . . . ? Si2 N1 C1 C2 1.4(14) . . . . ? W1 N1 C1 C2 -170.4(8) . . . . ? Si2 N1 C1 W1 171.8(9) . . . . ? C25 W1 C1 N1 -134.0(4) . . . . ? C28 W1 C1 N1 134.2(4) . . . . ? C27 W1 C1 N1 134.5(4) . . . . ? C29 W1 C1 N1 102.3(4) . . . . ? C26 W1 C1 N1 76.2(6) . . . . ? C30 W1 C1 N1 73.0(4) . . . . ? Si1 W1 C1 N1 -71.4(4) . . . . ? C25 W1 C1 C2 32.7(9) . . . . ? N1 W1 C1 C2 166.7(11) . . . . ? C28 W1 C1 C2 -59.1(9) . . . . ? C27 W1 C1 C2 -58.8(10) . . . . ? C29 W1 C1 C2 -91.0(9) . . . . ? C26 W1 C1 C2 -117.1(8) . . . . ? C30 W1 C1 C2 -120.3(8) . . . . ? Si1 W1 C1 C2 95.4(8) . . . . ? N1 C1 C2 C5 -41.3(11) . . . . ? W1 C1 C2 C5 156.3(8) . . . . ? N1 C1 C2 C3 -164.1(8) . . . . ? W1 C1 C2 C3 33.5(12) . . . . ? N1 C1 C2 C4 79.0(9) . . . . ? W1 C1 C2 C4 -83.4(10) . . . . ? C7 Si1 C8 C9 118.5(6) . . . . ? C6 Si1 C8 C9 11.9(6) . . . . ? W1 Si1 C8 C9 -110.0(5) . . . . ? C7 Si1 C8 C13 -55.0(6) . . . . ? C6 Si1 C8 C13 -161.7(5) . . . . ? W1 Si1 C8 C13 76.5(5) . . . . ? C13 C8 C9 C10 1.9(10) . . . . ? Si1 C8 C9 C10 -172.2(6) . . . . ? C8 C9 C10 C11 0.4(12) . . . . ? C9 C10 C11 C12 -0.6(12) . . . . ? C10 C11 C12 C13 -1.4(11) . . . . ? C10 C11 C12 C14 173.2(7) . . . . ? C22 O1 C13 C12 25.9(8) . . . . ? C22 O1 C13 C8 -154.3(6) . . . . ? C11 C12 C13 O1 -176.3(6) . . . . ? C14 C12 C13 O1 8.8(9) . . . . ? C11 C12 C13 C8 3.9(10) . . . . ? C14 C12 C13 C8 -171.0(6) . . . . ? C9 C8 C13 O1 176.1(6) . . . . ? Si1 C8 C13 O1 -10.1(8) . . . . ? C9 C8 C13 C12 -4.1(9) . . . . ? Si1 C8 C13 C12 169.7(5) . . . . ? C11 C12 C14 C21 147.9(7) . . . . ? C13 C12 C14 C21 -37.5(9) . . . . ? C11 C12 C14 C15 23.5(10) . . . . ? C13 C12 C14 C15 -161.9(7) . . . . ? C11 C12 C14 C16 -96.0(8) . . . . ? C13 C12 C14 C16 78.6(8) . . . . ? N1 Si2 C17 C22 -55.5(6) . . . . ? C23 Si2 C17 C22 64.6(6) . . . . ? C24 Si2 C17 C22 -175.1(6) . . . . ? N1 Si2 C17 C18 123.4(6) . . . . ? C23 Si2 C17 C18 -116.5(7) . . . . ? C24 Si2 C17 C18 3.7(8) . . . . ? C22 C17 C18 C19 1.7(11) . . . . ? Si2 C17 C18 C19 -177.3(6) . . . . ? C17 C18 C19 C20 -1.5(13) . . . . ? C18 C19 C20 C21 0.3(14) . . . . ? C19 C20 C21 C22 0.6(12) . . . . ? C19 C20 C21 C14 -175.5(8) . . . . ? C12 C14 C21 C20 -148.2(7) . . . . ? C15 C14 C21 C20 -23.9(11) . . . . ? C16 C14 C21 C20 95.6(9) . . . . ? C12 C14 C21 C22 35.7(9) . . . . ? C15 C14 C21 C22 160.0(7) . . . . ? C16 C14 C21 C22 -80.5(8) . . . . ? C13 O1 C22 C17 151.1(6) . . . . ? C13 O1 C22 C21 -27.9(9) . . . . ? C18 C17 C22 O1 -179.8(6) . . . . ? Si2 C17 C22 O1 -0.8(8) . . . . ? C18 C17 C22 C21 -0.7(10) . . . . ? Si2 C17 C22 C21 178.2(5) . . . . ? C20 C21 C22 O1 178.6(7) . . . . ? C14 C21 C22 O1 -5.0(10) . . . . ? C20 C21 C22 C17 -0.4(11) . . . . ? C14 C21 C22 C17 176.0(7) . . . . ? C1 W1 C25 O2 -103(7) . . . . ? N1 W1 C25 O2 -129(7) . . . . ? C28 W1 C25 O2 2(7) . . . . ? C27 W1 C25 O2 37(7) . . . . ? C29 W1 C25 O2 -15(7) . . . . ? C26 W1 C25 O2 56(7) . . . . ? C30 W1 C25 O2 22(7) . . . . ? Si1 W1 C25 O2 149(7) . . . . ? C25 W1 C26 C30 -148.8(4) . . . . ? C1 W1 C26 C30 -5.3(7) . . . . ? N1 W1 C26 C30 35.9(5) . . . . ? C28 W1 C26 C30 -78.5(5) . . . . ? C27 W1 C26 C30 -116.0(6) . . . . ? C29 W1 C26 C30 -36.4(4) . . . . ? Si1 W1 C26 C30 142.3(4) . . . . ? C25 W1 C26 C27 -32.8(5) . . . . ? C1 W1 C26 C27 110.7(5) . . . . ? N1 W1 C26 C27 151.9(4) . . . . ? C28 W1 C26 C27 37.5(4) . . . . ? C29 W1 C26 C27 79.6(5) . . . . ? C30 W1 C26 C27 116.0(6) . . . . ? Si1 W1 C26 C27 -101.7(4) . . . . ? C25 W1 C26 C31 88.0(8) . . . . ? C1 W1 C26 C31 -128.5(8) . . . . ? N1 W1 C26 C31 -87.3(8) . . . . ? C28 W1 C26 C31 158.2(9) . . . . ? C27 W1 C26 C31 120.7(10) . . . . ? C29 W1 C26 C31 -159.7(9) . . . . ? C30 W1 C26 C31 -123.3(10) . . . . ? Si1 W1 C26 C31 19.1(8) . . . . ? C30 C26 C27 C28 0.5(8) . . . . ? C31 C26 C27 C28 175.7(7) . . . . ? W1 C26 C27 C28 -64.0(5) . . . . ? C30 C26 C27 C32 -172.2(7) . . . . ? C31 C26 C27 C32 3.0(12) . . . . ? W1 C26 C27 C32 123.2(7) . . . . ? C30 C26 C27 W1 64.6(5) . . . . ? C31 C26 C27 W1 -120.2(7) . . . . ? C25 W1 C27 C28 -91.6(5) . . . . ? C1 W1 C27 C28 -0.5(7) . . . . ? N1 W1 C27 C28 58.8(7) . . . . ? C29 W1 C27 C28 37.9(5) . . . . ? C26 W1 C27 C28 115.7(7) . . . . ? C30 W1 C27 C28 78.8(5) . . . . ? Si1 W1 C27 C28 -154.1(4) . . . . ? C25 W1 C27 C26 152.7(5) . . . . ? C1 W1 C27 C26 -116.2(5) . . . . ? N1 W1 C27 C26 -56.9(7) . . . . ? C28 W1 C27 C26 -115.7(7) . . . . ? C29 W1 C27 C26 -77.8(5) . . . . ? C30 W1 C27 C26 -36.8(4) . . . . ? Si1 W1 C27 C26 90.2(4) . . . . ? C25 W1 C27 C32 29.2(7) . . . . ? C1 W1 C27 C32 120.2(7) . . . . ? N1 W1 C27 C32 179.5(6) . . . . ? C28 W1 C27 C32 120.8(9) . . . . ? C29 W1 C27 C32 158.7(8) . . . . ? C26 W1 C27 C32 -123.6(9) . . . . ? C30 W1 C27 C32 -160.4(8) . . . . ? Si1 W1 C27 C32 -33.4(7) . . . . ? C26 C27 C28 C29 -1.0(8) . . . . ? C32 C27 C28 C29 171.9(7) . . . . ? W1 C27 C28 C29 -66.6(5) . . . . ? C26 C27 C28 C33 -171.7(7) . . . . ? C32 C27 C28 C33 1.1(11) . . . . ? W1 C27 C28 C33 122.6(8) . . . . ? C26 C27 C28 W1 65.6(5) . . . . ? C32 C27 C28 W1 -121.5(7) . . . . ? C25 W1 C28 C27 89.3(5) . . . . ? C1 W1 C28 C27 179.6(4) . . . . ? N1 W1 C28 C27 -150.9(4) . . . . ? C29 W1 C28 C27 -115.7(6) . . . . ? C26 W1 C28 C27 -37.9(5) . . . . ? C30 W1 C28 C27 -78.7(5) . . . . ? Si1 W1 C28 C27 39.7(6) . . . . ? C25 W1 C28 C29 -155.1(4) . . . . ? C1 W1 C28 C29 -64.7(4) . . . . ? N1 W1 C28 C29 -35.3(5) . . . . ? C27 W1 C28 C29 115.7(6) . . . . ? C26 W1 C28 C29 77.8(5) . . . . ? C30 W1 C28 C29 37.0(4) . . . . ? Si1 W1 C28 C29 155.4(3) . . . . ? C25 W1 C28 C33 -30.8(9) . . . . ? C1 W1 C28 C33 59.6(9) . . . . ? N1 W1 C28 C33 89.0(9) . . . . ? C27 W1 C28 C33 -120.1(10) . . . . ? C29 W1 C28 C33 124.2(10) . . . . ? C26 W1 C28 C33 -158.0(10) . . . . ? C30 W1 C28 C33 161.2(10) . . . . ? Si1 W1 C28 C33 -80.4(9) . . . . ? C27 C28 C29 C30 1.0(7) . . . . ? C33 C28 C29 C30 171.5(8) . . . . ? W1 C28 C29 C30 -64.5(5) . . . . ? C27 C28 C29 C34 -175.1(7) . . . . ? C33 C28 C29 C34 -4.6(12) . . . . ? W1 C28 C29 C34 119.3(7) . . . . ? C27 C28 C29 W1 65.6(5) . . . . ? C33 C28 C29 W1 -123.9(8) . . . . ? C25 W1 C29 C30 146.3(5) . . . . ? C1 W1 C29 C30 -125.1(5) . . . . ? N1 W1 C29 C30 -92.1(4) . . . . ? C28 W1 C29 C30 115.9(6) . . . . ? C27 W1 C29 C30 78.4(4) . . . . ? C26 W1 C29 C30 36.3(4) . . . . ? Si1 W1 C29 C30 31.8(10) . . . . ? C25 W1 C29 C28 30.4(5) . . . . ? C1 W1 C29 C28 119.0(4) . . . . ? N1 W1 C29 C28 152.0(4) . . . . ? C27 W1 C29 C28 -37.5(4) . . . . ? C26 W1 C29 C28 -79.6(5) . . . . ? C30 W1 C29 C28 -115.9(6) . . . . ? Si1 W1 C29 C28 -84.1(9) . . . . ? C25 W1 C29 C34 -92.4(10) . . . . ? C1 W1 C29 C34 -3.8(10) . . . . ? N1 W1 C29 C34 29.2(10) . . . . ? C28 W1 C29 C34 -122.8(11) . . . . ? C27 W1 C29 C34 -160.3(10) . . . . ? C26 W1 C29 C34 157.6(10) . . . . ? C30 W1 C29 C34 121.3(11) . . . . ? Si1 W1 C29 C34 153.1(8) . . . . ? C27 C26 C30 C29 0.1(8) . . . . ? C31 C26 C30 C29 -175.1(7) . . . . ? W1 C26 C30 C29 62.6(5) . . . . ? C27 C26 C30 C35 176.5(8) . . . . ? C31 C26 C30 C35 1.4(12) . . . . ? W1 C26 C30 C35 -121.0(8) . . . . ? C27 C26 C30 W1 -62.4(5) . . . . ? C31 C26 C30 W1 122.4(7) . . . . ? C28 C29 C30 C26 -0.7(7) . . . . ? C34 C29 C30 C26 175.6(7) . . . . ? W1 C29 C30 C26 -62.7(5) . . . . ? C28 C29 C30 C35 -177.0(8) . . . . ? C34 C29 C30 C35 -0.7(12) . . . . ? W1 C29 C30 C35 121.0(8) . . . . ? C28 C29 C30 W1 62.0(4) . . . . ? C34 C29 C30 W1 -121.7(7) . . . . ? C25 W1 C30 C26 56.4(7) . . . . ? C1 W1 C30 C26 176.6(4) . . . . ? N1 W1 C30 C26 -151.2(4) . . . . ? C28 W1 C30 C26 79.7(5) . . . . ? C27 W1 C30 C26 38.0(4) . . . . ? C29 W1 C30 C26 117.7(6) . . . . ? Si1 W1 C30 C26 -51.4(5) . . . . ? C25 W1 C30 C29 -61.3(7) . . . . ? C1 W1 C30 C29 59.0(5) . . . . ? N1 W1 C30 C29 91.2(4) . . . . ? C28 W1 C30 C29 -38.0(4) . . . . ? C27 W1 C30 C29 -79.7(5) . . . . ? C26 W1 C30 C29 -117.7(6) . . . . ? Si1 W1 C30 C29 -169.1(3) . . . . ? C25 W1 C30 C35 176.8(8) . . . . ? C1 W1 C30 C35 -63.0(9) . . . . ? N1 W1 C30 C35 -30.7(9) . . . . ? C28 W1 C30 C35 -159.9(10) . . . . ? C27 W1 C30 C35 158.4(10) . . . . ? C29 W1 C30 C35 -121.9(10) . . . . ? C26 W1 C30 C35 120.4(11) . . . . ? Si1 W1 C30 C35 69.0(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.062 _refine_diff_density_min -1.402 _refine_diff_density_rms 0.279 #===END