Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Prof. Dr. Ulrich Siemeling' _publ_contact_author_address ; Institute of Chemistry and Centre for Interdisciplinary Nanostructure Science and Technology - CINSaT, University of Kassel, Heinrich-Plett-Str. 40, D-34109 Kassel Germany ; _publ_contact_author_phone '+49 561 804 4576' _publ_contact_author_fax '+49 561 804 4777' _publ_contact_author_email siemeling@uni-kassel.de _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; December 16, 2005 The following structures I0034 and I0045 (CCDC Numbers: 269773 and 269774) are accepted for publication in Dalton. I0045 (269774) has been recalculated after a very slight modification. Clemens Bruhn ; #===================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_paper_category ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _iucr_compatibility_tag ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _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 ; Novel Tripod Ligands for Prickly Self-Assembled Monolayers ; loop_ _publ_author_name _publ_author_footnote _publ_author_address T.Weidner ? ; Institute for Physics and Centre for Interdisciplinary Nanostructure Science and Technology - CINSaT, University of Kassel, Heinrich-Plett-Str. 40, 34109 Kassel Germany ; A.Kramer ? ; Institute of Chemistry and Centre for Interdisciplinary Nanostructure Science and Technology - CINSaT, University of Kassel, Heinrich-Plett-Str. 40, 34109 Kassel, Germany ; C.Bruhn ? ; Institute of Chemistry and Centre for Interdisciplinary Nanostructure Science and Technology - CINSaT, University of Kassel, Heinrich-Plett-Str. 40, 34109 Kassel, Germany ; M.Zharnikov ? ; Institute of Physical Chemistry, University of Heidelberg, Im Neuenheimer Feld 253, 69120 Heidelberg, Germany ; A.Shaporenko ? ; Institute of Physical Chemistry, University of Heidelberg, Im Neuenheimer Feld 253, 69120 Heidelberg, Germany ; ; U.Siemeling ; ? ; Institute of Chemistry and Centre for Interdisciplinary Nanostructure Science and Technology - CINSaT, University of Kassel, Heinrich-Plett-Str. 40, 34109 Kassel, Germany ; F.Trager ? ; Institute for Physics and Centre for Interdisciplinary Nanostructure Science and Technology - CINSaT, University of Kassel, Heinrich-Plett-Str. 40, 34109 Kassel Germany ; #============================================================================= data_i0034 _database_code_depnum_ccdc_archive 'CCDC 269773' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H20 O3 S3 Si W' _chemical_formula_sum 'C15 H20 O3 S3 Si W' _chemical_formula_weight 556.43 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' Si Si 0.0817 0.0704 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 13.1471(8) _cell_length_b 23.7606(19) _cell_length_c 12.7676(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.895(5) _cell_angle_gamma 90.00 _cell_volume 3871.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 22112 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 26.10 _exptl_crystal_description blocks _exptl_crystal_colour green _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 6.362 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2361 _exptl_absorpt_correction_T_max 0.5659 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 213(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 130 mm ; _diffrn_measured_fraction_theta_max 0.980 _diffrn_measured_fraction_theta_full 0.977 _diffrn_standards_decay_% none _diffrn_reflns_number 26213 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_full 25.50 _reflns_number_total 7152 _reflns_number_gt 5825 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00066(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7152 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.0395 _refine_ls_wR_factor_gt 0.0382 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _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 C1 C 0.5150(3) 0.69241(13) 0.6582(3) 0.0363(8) Uani 1 1 d . . . H1A H 0.5764 0.6990 0.6291 0.044 Uiso 1 1 calc R . . H1B H 0.4637 0.7220 0.6304 0.044 Uiso 1 1 calc R . . C2 C 0.5280(3) 0.56761(14) 0.7076(3) 0.0410(9) Uani 1 1 d . . . H2A H 0.5232 0.5311 0.6712 0.049 Uiso 1 1 calc R . . H2B H 0.6022 0.5779 0.7298 0.049 Uiso 1 1 calc R . . C3 C 0.3134(3) 0.62196(13) 0.6087(3) 0.0363(8) Uani 1 1 d . . . H3B H 0.2717 0.6333 0.5374 0.044 Uiso 1 1 calc R . . H3A H 0.2917 0.5840 0.6241 0.044 Uiso 1 1 calc R . . C4 C 0.5542(4) 0.77213(14) 0.8232(4) 0.0545(11) Uani 1 1 d . . . H4A H 0.4859 0.7874 0.7890 0.065 Uiso 1 1 calc R . . H4B H 0.6068 0.7891 0.7914 0.065 Uiso 1 1 calc R . . H4C H 0.5704 0.7803 0.8998 0.065 Uiso 1 1 calc R . . C5 C 0.5937(3) 0.53909(16) 0.9233(3) 0.0510(10) Uani 1 1 d . . . H5A H 0.6462 0.5685 0.9314 0.061 Uiso 1 1 calc R . . H5B H 0.6205 0.5049 0.8983 0.061 Uiso 1 1 calc R . . H5C H 0.5774 0.5321 0.9923 0.061 Uiso 1 1 calc R . . C6 C 0.1574(3) 0.65633(15) 0.7118(4) 0.0458(9) Uani 1 1 d . . . H6A H 0.1497 0.6168 0.7273 0.055 Uiso 1 1 calc R . . H6B H 0.1120 0.6655 0.6420 0.055 Uiso 1 1 calc R . . H6C H 0.1382 0.6791 0.7671 0.055 Uiso 1 1 calc R . . C7 C 0.4759(3) 0.60445(13) 0.4735(3) 0.0356(8) Uani 1 1 d . . . C8 C 0.5761(3) 0.59549(16) 0.4593(4) 0.0520(10) Uani 1 1 d . . . H8A H 0.6336 0.5978 0.5194 0.062 Uiso 1 1 calc R . . C9 C 0.5936(4) 0.58319(17) 0.3585(4) 0.0626(13) Uani 1 1 d . . . H9A H 0.6622 0.5779 0.3503 0.075 Uiso 1 1 calc R . . C10 C 0.5088(4) 0.57885(15) 0.2705(4) 0.0611(13) Uani 1 1 d . . . H10A H 0.5197 0.5701 0.2022 0.073 Uiso 1 1 calc R . . C11 C 0.4098(4) 0.58719(16) 0.2823(4) 0.0585(12) Uani 1 1 d . . . H11A H 0.3526 0.5843 0.2221 0.070 Uiso 1 1 calc R . . C12 C 0.3930(3) 0.59987(14) 0.3823(3) 0.0440(9) Uani 1 1 d . . . H12A H 0.3242 0.6056 0.3891 0.053 Uiso 1 1 calc R . . C13 C 0.5233(3) 0.65322(14) 1.0268(3) 0.0371(8) Uani 1 1 d . . . C14 C 0.3609(3) 0.72386(13) 0.9359(3) 0.0355(8) Uani 1 1 d . . . C15 C 0.3249(3) 0.61050(13) 0.9606(3) 0.0354(8) Uani 1 1 d . . . C16 C 0.1160(3) 0.45587(13) 0.9210(3) 0.0348(8) Uani 1 1 d . . . H16A H 0.0526 0.4788 0.8982 0.042 Uiso 1 1 calc R . . H16B H 0.1716 0.4797 0.9638 0.042 Uiso 1 1 calc R . . C17 C 0.1726(3) 0.33303(13) 0.9879(3) 0.0348(8) Uani 1 1 d . . . H17A H 0.2407 0.3463 0.9793 0.042 Uiso 1 1 calc R . . H17B H 0.1849 0.3096 1.0529 0.042 Uiso 1 1 calc R . . C18 C -0.0509(3) 0.37527(14) 0.9598(3) 0.0369(8) Uani 1 1 d . . . H18A H -0.0599 0.3380 0.9891 0.044 Uiso 1 1 calc R . . H18B H -0.0925 0.4019 0.9907 0.044 Uiso 1 1 calc R . . C19 C 0.1428(4) 0.49282(15) 0.7233(4) 0.0534(11) Uani 1 1 d . . . H19A H 0.1922 0.5208 0.7604 0.064 Uiso 1 1 calc R . . H19B H 0.0721 0.5074 0.7122 0.064 Uiso 1 1 calc R . . H19C H 0.1573 0.4842 0.6541 0.064 Uiso 1 1 calc R . . C20 C 0.2211(3) 0.25102(14) 0.8521(3) 0.0428(9) Uani 1 1 d . . . H20A H 0.2476 0.2273 0.9146 0.051 Uiso 1 1 calc R . . H20B H 0.2757 0.2767 0.8430 0.051 Uiso 1 1 calc R . . H20C H 0.1997 0.2276 0.7883 0.051 Uiso 1 1 calc R . . C21 C -0.1875(3) 0.31235(15) 0.8058(3) 0.0485(10) Uani 1 1 d . . . H21A H -0.2403 0.3195 0.8458 0.058 Uiso 1 1 calc R . . H21B H -0.1459 0.2800 0.8363 0.058 Uiso 1 1 calc R . . H21C H -0.2215 0.3049 0.7308 0.058 Uiso 1 1 calc R . . C22 C 0.1154(2) 0.41527(13) 1.1508(3) 0.0316(7) Uani 1 1 d . . . C23 C 0.1572(3) 0.46701(14) 1.1922(3) 0.0399(9) Uani 1 1 d . . . H23A H 0.1763 0.4935 1.1457 0.048 Uiso 1 1 calc R . . C24 C 0.1710(3) 0.48012(16) 1.3005(3) 0.0519(10) Uani 1 1 d . . . H24A H 0.1989 0.5153 1.3264 0.062 Uiso 1 1 calc R . . C25 C 0.1442(3) 0.44190(17) 1.3704(3) 0.0515(10) Uani 1 1 d . . . H25A H 0.1540 0.4508 1.4439 0.062 Uiso 1 1 calc R . . C26 C 0.1025(3) 0.39018(17) 1.3317(3) 0.0493(10) Uani 1 1 d . . . H26A H 0.0839 0.3638 1.3787 0.059 Uiso 1 1 calc R . . C27 C 0.0887(3) 0.37763(15) 1.2232(3) 0.0422(9) Uani 1 1 d . . . H27A H 0.0604 0.3425 1.1976 0.051 Uiso 1 1 calc R . . C28 C 0.1387(3) 0.33357(14) 0.6272(3) 0.0422(9) Uani 1 1 d . . . C29 C -0.0342(3) 0.40083(14) 0.5869(3) 0.0393(8) Uani 1 1 d . . . C30 C -0.0408(3) 0.28774(15) 0.6318(3) 0.0402(8) Uani 1 1 d . . . O1 O 0.5891(2) 0.65400(11) 1.1067(2) 0.0518(7) Uani 1 1 d . . . O2 O 0.3285(2) 0.76589(10) 0.9612(2) 0.0515(7) Uani 1 1 d . . . O3 O 0.2724(2) 0.58288(11) 1.0028(2) 0.0496(7) Uani 1 1 d . . . O4 O 0.1999(2) 0.32043(14) 0.5779(2) 0.0612(8) Uani 1 1 d . . . O5 O -0.0748(2) 0.42930(11) 0.5152(2) 0.0543(7) Uani 1 1 d . . . O6 O -0.0820(2) 0.24847(11) 0.5847(3) 0.0643(9) Uani 1 1 d . . . Si1 Si 0.45615(7) 0.62197(4) 0.60919(8) 0.0310(2) Uani 1 1 d . . . Si2 Si 0.08967(7) 0.39548(3) 1.00545(8) 0.0300(2) Uani 1 1 d . . . S1 S 0.55349(6) 0.69724(3) 0.80325(7) 0.03188(19) Uani 1 1 d . . . S2 S 0.47677(7) 0.56093(3) 0.82659(7) 0.03328(19) Uani 1 1 d . . . S3 S 0.29147(6) 0.67044(3) 0.70977(7) 0.03228(18) Uani 1 1 d . . . S4 S 0.15534(7) 0.42986(3) 0.80362(7) 0.03383(19) Uani 1 1 d . . . S5 S 0.11032(6) 0.29074(3) 0.87137(7) 0.03246(18) Uani 1 1 d . . . S6 S -0.10347(6) 0.37332(3) 0.81398(7) 0.03260(19) Uani 1 1 d . . . W1 W 0.416373(10) 0.653795(5) 0.891581(11) 0.02902(4) Uani 1 1 d . . . W2 W 0.035158(10) 0.352270(5) 0.706549(11) 0.03124(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0362(19) 0.0384(18) 0.033(2) 0.0026(15) 0.0053(16) -0.0090(14) C2 0.042(2) 0.0349(17) 0.048(2) 0.0056(16) 0.0155(18) 0.0073(15) C3 0.0362(19) 0.0357(17) 0.036(2) -0.0065(15) 0.0075(16) -0.0047(14) C4 0.079(3) 0.0354(19) 0.056(3) -0.0119(18) 0.031(2) -0.0157(19) C5 0.056(2) 0.047(2) 0.046(3) 0.0029(18) 0.003(2) 0.0186(18) C6 0.0368(19) 0.045(2) 0.058(3) -0.0071(18) 0.0150(18) 0.0002(16) C7 0.045(2) 0.0287(16) 0.036(2) -0.0030(14) 0.0164(17) -0.0033(14) C8 0.051(2) 0.054(2) 0.057(3) -0.012(2) 0.023(2) -0.0046(18) C9 0.077(3) 0.050(2) 0.079(4) -0.016(2) 0.053(3) -0.009(2) C10 0.117(4) 0.0327(19) 0.047(3) -0.0058(18) 0.046(3) -0.013(2) C11 0.091(4) 0.045(2) 0.038(3) -0.0051(18) 0.012(2) 0.004(2) C12 0.055(2) 0.0403(19) 0.036(2) -0.0066(16) 0.0107(19) 0.0019(16) C13 0.0382(19) 0.0376(18) 0.039(2) 0.0025(15) 0.0152(17) -0.0035(15) C14 0.0333(18) 0.0372(18) 0.032(2) -0.0012(15) 0.0000(15) -0.0009(14) C15 0.0330(18) 0.0349(17) 0.036(2) -0.0041(15) 0.0032(16) 0.0091(14) C16 0.0344(18) 0.0292(16) 0.039(2) -0.0054(14) 0.0045(15) -0.0006(13) C17 0.0373(18) 0.0329(16) 0.035(2) -0.0008(14) 0.0103(16) 0.0036(14) C18 0.0324(18) 0.0396(18) 0.039(2) -0.0045(15) 0.0094(16) -0.0031(14) C19 0.071(3) 0.041(2) 0.050(3) 0.0107(18) 0.019(2) -0.0068(19) C20 0.046(2) 0.0341(18) 0.051(2) -0.0020(16) 0.0172(19) 0.0085(15) C21 0.047(2) 0.0406(19) 0.056(3) -0.0099(18) 0.008(2) -0.0161(16) C22 0.0273(17) 0.0352(17) 0.031(2) -0.0010(14) 0.0052(15) 0.0052(13) C23 0.043(2) 0.0377(18) 0.039(2) -0.0057(15) 0.0102(18) 0.0023(15) C24 0.058(3) 0.050(2) 0.046(3) -0.0156(19) 0.009(2) -0.0040(19) C25 0.053(2) 0.065(3) 0.033(2) -0.0106(19) 0.0040(19) 0.008(2) C26 0.047(2) 0.062(2) 0.039(2) 0.0053(19) 0.0109(19) 0.0000(18) C27 0.044(2) 0.0437(19) 0.037(2) -0.0012(16) 0.0055(18) -0.0006(16) C28 0.046(2) 0.0415(19) 0.035(2) -0.0033(15) 0.0013(18) -0.0003(16) C29 0.039(2) 0.0378(18) 0.040(2) -0.0040(16) 0.0073(17) 0.0010(15) C30 0.042(2) 0.0429(19) 0.038(2) -0.0020(16) 0.0125(17) 0.0014(16) O1 0.0451(15) 0.0696(18) 0.0346(16) 0.0044(13) -0.0021(13) -0.0088(13) O2 0.0553(16) 0.0423(14) 0.0519(18) -0.0173(12) 0.0034(14) 0.0135(12) O3 0.0403(15) 0.0537(15) 0.0607(19) 0.0146(14) 0.0240(14) -0.0018(12) O4 0.0557(18) 0.087(2) 0.048(2) -0.0112(15) 0.0275(16) 0.0061(15) O5 0.0602(18) 0.0548(16) 0.0386(17) 0.0090(13) -0.0062(14) 0.0059(13) O6 0.071(2) 0.0503(16) 0.071(2) -0.0325(15) 0.0161(17) -0.0191(14) Si1 0.0333(5) 0.0303(4) 0.0297(5) -0.0011(4) 0.0080(4) -0.0021(4) Si2 0.0294(5) 0.0289(4) 0.0312(5) -0.0024(4) 0.0064(4) 0.0002(3) S1 0.0320(4) 0.0307(4) 0.0309(5) -0.0014(3) 0.0035(4) -0.0045(3) S2 0.0374(5) 0.0275(4) 0.0359(5) 0.0029(3) 0.0106(4) 0.0030(3) S3 0.0300(4) 0.0299(4) 0.0359(5) -0.0013(3) 0.0059(4) 0.0017(3) S4 0.0352(4) 0.0304(4) 0.0361(5) 0.0011(3) 0.0089(4) -0.0025(3) S5 0.0333(4) 0.0271(4) 0.0373(5) -0.0004(3) 0.0091(4) 0.0013(3) S6 0.0296(4) 0.0279(4) 0.0385(5) -0.0004(3) 0.0046(4) -0.0007(3) W1 0.03078(7) 0.02692(6) 0.02943(8) 0.00018(5) 0.00736(6) 0.00105(5) W2 0.03364(8) 0.02833(7) 0.03097(8) -0.00207(5) 0.00625(6) -0.00065(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 C1 S1 1.803(4) . ? C1 Si1 1.886(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 S2 1.810(4) . ? C2 Si1 1.889(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 S3 1.804(3) . ? C3 Si1 1.875(4) . ? C3 H3B 0.9800 . ? C3 H3A 0.9800 . ? C4 S1 1.797(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 S2 1.802(4) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 S3 1.801(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 C8 1.389(5) . ? C7 C12 1.394(5) . ? C7 Si1 1.860(4) . ? C8 C9 1.392(6) . ? C8 H8A 0.9400 . ? C9 C10 1.384(7) . ? C9 H9A 0.9400 . ? C10 C11 1.361(7) . ? C10 H10A 0.9400 . ? C11 C12 1.380(6) . ? C11 H11A 0.9400 . ? C12 H12A 0.9400 . ? C13 O1 1.168(4) . ? C13 W1 1.948(4) . ? C14 O2 1.162(4) . ? C14 W1 1.955(3) . ? C15 O3 1.174(4) . ? C15 W1 1.946(4) . ? C16 S4 1.808(4) . ? C16 Si2 1.876(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C17 S5 1.819(3) . ? C17 Si2 1.886(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 S6 1.825(4) . ? C18 Si2 1.862(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C19 S4 1.798(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 S5 1.801(3) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 S6 1.810(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 C27 1.390(5) . ? C22 C23 1.397(5) . ? C22 Si2 1.865(4) . ? C23 C24 1.386(5) . ? C23 H23A 0.9400 . ? C24 C25 1.377(6) . ? C24 H24A 0.9400 . ? C25 C26 1.387(5) . ? C25 H25A 0.9400 . ? C26 C27 1.386(5) . ? C26 H26A 0.9400 . ? C27 H27A 0.9400 . ? C28 O4 1.176(5) . ? C28 W2 1.935(4) . ? C29 O5 1.160(4) . ? C29 W2 1.956(4) . ? C30 O6 1.171(4) . ? C30 W2 1.949(4) . ? S1 W1 2.5619(9) . ? S2 W1 2.5503(8) . ? S3 W1 2.5319(9) . ? S4 W2 2.5477(8) . ? S5 W2 2.5581(9) . ? S6 W2 2.5795(9) . ? 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 S1 C1 Si1 112.88(17) . . ? S1 C1 H1A 109.0 . . ? Si1 C1 H1A 109.0 . . ? S1 C1 H1B 109.0 . . ? Si1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? S2 C2 Si1 113.00(18) . . ? S2 C2 H2A 109.0 . . ? Si1 C2 H2A 109.0 . . ? S2 C2 H2B 109.0 . . ? Si1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? S3 C3 Si1 109.22(17) . . ? S3 C3 H3B 109.8 . . ? Si1 C3 H3B 109.8 . . ? S3 C3 H3A 109.8 . . ? Si1 C3 H3A 109.8 . . ? H3B C3 H3A 108.3 . . ? S1 C4 H4A 109.5 . . ? S1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S2 C5 H5A 109.5 . . ? S2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S3 C6 H6A 109.5 . . ? S3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? S3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 117.1(4) . . ? C8 C7 Si1 120.3(3) . . ? C12 C7 Si1 122.6(3) . . ? C7 C8 C9 121.7(4) . . ? C7 C8 H8A 119.2 . . ? C9 C8 H8A 119.2 . . ? C10 C9 C8 119.1(4) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 120.3(5) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C11 C12 C7 121.5(4) . . ? C11 C12 H12A 119.2 . . ? C7 C12 H12A 119.2 . . ? O1 C13 W1 178.1(3) . . ? O2 C14 W1 179.1(3) . . ? O3 C15 W1 177.6(3) . . ? S4 C16 Si2 110.11(16) . . ? S4 C16 H16A 109.6 . . ? Si2 C16 H16A 109.6 . . ? S4 C16 H16B 109.6 . . ? Si2 C16 H16B 109.6 . . ? H16A C16 H16B 108.2 . . ? S5 C17 Si2 111.87(18) . . ? S5 C17 H17A 109.2 . . ? Si2 C17 H17A 109.2 . . ? S5 C17 H17B 109.2 . . ? Si2 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? S6 C18 Si2 115.5(2) . . ? S6 C18 H18A 108.4 . . ? Si2 C18 H18A 108.4 . . ? S6 C18 H18B 108.4 . . ? Si2 C18 H18B 108.4 . . ? H18A C18 H18B 107.5 . . ? S4 C19 H19A 109.5 . . ? S4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? S4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? S5 C20 H20A 109.5 . . ? S5 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? S5 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? S6 C21 H21A 109.5 . . ? S6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 117.0(3) . . ? C27 C22 Si2 119.0(3) . . ? C23 C22 Si2 124.0(3) . . ? C24 C23 C22 121.4(4) . . ? C24 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C25 C24 C23 120.4(4) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C24 C25 C26 119.6(4) . . ? C24 C25 H25A 120.2 . . ? C26 C25 H25A 120.2 . . ? C27 C26 C25 119.5(4) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C22 122.2(3) . . ? C26 C27 H27A 118.9 . . ? C22 C27 H27A 118.9 . . ? O4 C28 W2 177.6(3) . . ? O5 C29 W2 179.3(4) . . ? O6 C30 W2 176.5(3) . . ? C7 Si1 C3 111.11(16) . . ? C7 Si1 C1 111.70(15) . . ? C3 Si1 C1 109.36(15) . . ? C7 Si1 C2 107.91(16) . . ? C3 Si1 C2 110.02(16) . . ? C1 Si1 C2 106.64(16) . . ? C18 Si2 C22 107.79(16) . . ? C18 Si2 C16 108.88(16) . . ? C22 Si2 C16 111.38(15) . . ? C18 Si2 C17 108.56(15) . . ? C22 Si2 C17 110.15(15) . . ? C16 Si2 C17 110.01(16) . . ? C4 S1 C1 101.48(18) . . ? C4 S1 W1 108.49(14) . . ? C1 S1 W1 111.89(11) . . ? C2 S2 W1 113.88(11) . . ? C3 S3 W1 112.11(12) . . ? C5 S2 C2 99.92(19) . . ? C5 S2 W1 107.89(13) . . ? C6 S3 C3 102.50(17) . . ? C6 S3 W1 112.31(15) . . ? C19 S4 C16 100.53(18) . . ? C19 S4 W2 111.30(15) . . ? C20 S5 C17 100.46(17) . . ? C20 S5 W2 110.63(13) . . ? C16 S4 W2 112.52(11) . . ? C17 S5 W2 111.49(11) . . ? C18 S6 W2 113.87(11) . . ? C21 S6 C18 98.97(18) . . ? C21 S6 W2 108.28(14) . . ? C15 W1 C13 89.32(14) . . ? C15 W1 C14 90.29(14) . . ? C13 W1 C14 89.41(14) . . ? C15 W1 S3 99.35(10) . . ? C13 W1 S3 170.12(10) . . ? C14 W1 S3 85.83(10) . . ? C15 W1 S2 87.96(9) . . ? C13 W1 S2 93.87(10) . . ? C14 W1 S2 176.27(10) . . ? S3 W1 S2 91.20(3) . . ? C15 W1 S1 171.34(9) . . ? C13 W1 S1 87.62(10) . . ? C14 W1 S1 97.77(11) . . ? S3 W1 S1 84.46(3) . . ? S2 W1 S1 84.17(3) . . ? C28 W2 C30 84.55(15) . . ? C28 W2 C29 88.90(15) . . ? C30 W2 C29 89.66(15) . . ? C28 W2 S4 89.35(11) . . ? C30 W2 S4 172.79(11) . . ? C29 W2 S4 94.09(10) . . ? C28 W2 S5 96.80(11) . . ? C30 W2 S5 90.25(11) . . ? C29 W2 S5 174.27(11) . . ? S4 W2 S5 86.64(3) . . ? C28 W2 S6 177.89(11) . . ? C30 W2 S6 93.94(11) . . ? C29 W2 S6 92.57(11) . . ? S4 W2 S6 92.06(3) . . ? S5 W2 S6 81.72(3) . . ? _refine_diff_density_max 0.518 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.076 #====================================================================== data_i0045 _database_code_depnum_ccdc_archive 'CCDC 269774' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C21 H24 O3 S3 Si W); 0.5(C4 H8 O)' _chemical_formula_sum 'C23 H28 O3.50 S3 Si W' _chemical_formula_weight 668.57 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' Si Si 0.0817 0.0704 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8433(4) _cell_length_b 41.729(2) _cell_length_c 13.1267(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.271(3) _cell_angle_gamma 90.00 _cell_volume 5390.4(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 58959 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 25.52 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2640 _exptl_absorpt_coefficient_mu 4.586 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.336 _exptl_absorpt_correction_T_max 0.697 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.0470 0 -1 0 0.0380 -6 -3 4 0.0880 5 3 -4 0.0940 0 1 4 0.1230 0 -1 -4 0.1810 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 173(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 527 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 45135 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9369 _reflns_number_gt 6676 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00066(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9369 _refine_ls_number_parameters 585 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0644 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 C1 C 0.6969(7) 0.22618(19) 0.4426(5) 0.0482(18) Uani 1 1 d . . . H1A H 0.7001 0.2389 0.3791 0.058 Uiso 1 1 calc R . . H1B H 0.6023 0.2187 0.4508 0.058 Uiso 1 1 calc R . . C2 C 0.9564(7) 0.20375(17) 0.3481(5) 0.0441(17) Uani 1 1 d . . . H2A H 1.0376 0.1904 0.3626 0.053 Uiso 1 1 calc R . . H2B H 0.9292 0.2006 0.2758 0.053 Uiso 1 1 calc R . . C3 C 0.8826(8) 0.18009(19) 0.5653(5) 0.0519(19) Uani 1 1 d . . . H3A H 0.8140 0.1854 0.6168 0.062 Uiso 1 1 calc R . . H3B H 0.9025 0.1569 0.5699 0.062 Uiso 1 1 calc R . . C4 C 0.6527(8) 0.2879(2) 0.5227(7) 0.063(2) Uani 1 1 d . . . H4A H 0.5552 0.2832 0.5186 0.076 Uiso 1 1 calc R . . H4B H 0.6820 0.2967 0.4574 0.076 Uiso 1 1 calc R . . H4C H 0.6705 0.3037 0.5768 0.076 Uiso 1 1 calc R . . C5 C 1.1707(8) 0.2461(2) 0.3286(6) 0.059(2) Uani 1 1 d . . . H5A H 1.1733 0.2396 0.2570 0.070 Uiso 1 1 calc R . . H5B H 1.2242 0.2311 0.3705 0.070 Uiso 1 1 calc R . . H5C H 1.2088 0.2677 0.3360 0.070 Uiso 1 1 calc R . . C6 C 1.0692(9) 0.1942(2) 0.7232(5) 0.064(2) Uani 1 1 d . . . H6C H 1.1520 0.2054 0.7460 0.076 Uiso 1 1 calc R . . H6B H 1.0814 0.1711 0.7324 0.076 Uiso 1 1 calc R . . H6A H 0.9924 0.2015 0.7635 0.076 Uiso 1 1 calc R . . C7 C 1.1916(8) 0.27142(17) 0.5770(5) 0.0477(18) Uani 1 1 d . . . C8 C 0.9776(7) 0.27342(19) 0.7048(6) 0.0492(18) Uani 1 1 d . . . C9 C 0.9688(7) 0.30899(19) 0.5271(5) 0.0433(17) Uani 1 1 d . . . C10 C 0.7212(8) 0.15500(18) 0.3750(5) 0.0480(17) Uani 1 1 d . . . C11 C 0.6853(9) 0.1285(2) 0.4354(6) 0.061(2) Uani 1 1 d . . . H11A H 0.7122 0.1280 0.5053 0.074 Uiso 1 1 calc R . . C12 C 0.6113(9) 0.1031(2) 0.3941(6) 0.061(2) Uani 1 1 d . . . H12A H 0.5873 0.0857 0.4365 0.074 Uiso 1 1 calc R . . C13 C 0.5711(7) 0.10279(18) 0.2902(6) 0.0479(17) Uani 1 1 d . . . C14 C 0.6066(7) 0.12891(18) 0.2300(5) 0.0463(17) Uani 1 1 d . . . H14A H 0.5802 0.1292 0.1600 0.056 Uiso 1 1 calc R . . C15 C 0.6805(7) 0.15463(17) 0.2710(5) 0.0445(17) Uani 1 1 d . . . H15A H 0.7036 0.1721 0.2284 0.053 Uiso 1 1 calc R . . C16 C 0.4898(7) 0.07563(19) 0.2475(6) 0.0516(18) Uani 1 1 d . . . C17 C 0.5092(7) 0.06386(19) 0.1479(6) 0.0537(19) Uani 1 1 d . . . H17A H 0.5738 0.0742 0.1063 0.064 Uiso 1 1 calc R . . C18 C 0.4378(9) 0.0380(2) 0.1086(7) 0.068(2) Uani 1 1 d . . . H18A H 0.4544 0.0304 0.0418 0.081 Uiso 1 1 calc R . . C19 C 0.3413(10) 0.0232(2) 0.1685(7) 0.075(3) Uani 1 1 d . . . H19A H 0.2922 0.0052 0.1433 0.090 Uiso 1 1 calc R . . C20 C 0.3166(10) 0.0350(2) 0.2665(7) 0.074(3) Uani 1 1 d . . . H20A H 0.2476 0.0254 0.3056 0.088 Uiso 1 1 calc R . . C21 C 0.3899(9) 0.0604(2) 0.3077(6) 0.061(2) Uani 1 1 d . . . H21A H 0.3739 0.0675 0.3752 0.074 Uiso 1 1 calc R . . C22 C 0.4385(8) 0.36049(18) 0.5771(6) 0.0509(18) Uani 1 1 d . . . H22A H 0.4945 0.3454 0.5375 0.061 Uiso 1 1 calc R . . H22B H 0.3938 0.3481 0.6312 0.061 Uiso 1 1 calc R . . C23 C 0.4529(9) 0.4297(2) 0.6611(6) 0.060(2) Uani 1 1 d . . . H23A H 0.3592 0.4239 0.6799 0.072 Uiso 1 1 calc R . . H23B H 0.4950 0.4416 0.7190 0.072 Uiso 1 1 calc R . . C24 C 0.6879(8) 0.4007(2) 0.5433(5) 0.057(2) Uani 1 1 d . . . H24A H 0.7277 0.4220 0.5593 0.068 Uiso 1 1 calc R . . H24B H 0.7613 0.3846 0.5511 0.068 Uiso 1 1 calc R . . C25 C 0.2675(10) 0.3441(2) 0.4107(7) 0.071(2) Uani 1 1 d . . . H25A H 0.3458 0.3388 0.3691 0.107 Uiso 0.717(3) 1 calc PR . . H25B H 0.1903 0.3500 0.3662 0.107 Uiso 0.717(3) 1 calc PR . . H25C H 0.2433 0.3255 0.4520 0.107 Uiso 0.717(3) 1 calc PR . . C26 C 0.3150(8) 0.48317(19) 0.5785(6) 0.056(2) Uani 1 1 d . . . H26A H 0.2265 0.4725 0.5733 0.084 Uiso 0.717(3) 1 calc PR . . H26B H 0.3176 0.5008 0.5293 0.084 Uiso 0.717(3) 1 calc PR . . H26C H 0.3288 0.4917 0.6476 0.084 Uiso 0.717(3) 1 calc PR . . C27 C 0.7553(10) 0.4236(3) 0.3498(7) 0.089(3) Uani 1 1 d . . . H27A H 0.7612 0.4449 0.3807 0.134 Uiso 0.717(3) 1 calc PR . . H27B H 0.7316 0.4257 0.2772 0.134 Uiso 0.717(3) 1 calc PR . . H27C H 0.8432 0.4127 0.3576 0.134 Uiso 0.717(3) 1 calc PR . . C28 C 0.4357(8) 0.4631(2) 0.3057(6) 0.056(2) Uani 1 1 d . A . C29 C 0.3878(15) 0.4035(2) 0.2502(8) 0.103(4) Uani 1 1 d . A . C30 C 0.2068(10) 0.4342(3) 0.3639(8) 0.097(4) Uani 1 1 d . A . C31 C 0.6315(7) 0.37701(17) 0.7611(5) 0.0441(17) Uani 1 1 d . . . C32 C 0.5820(8) 0.38606(19) 0.8589(5) 0.0510(18) Uani 1 1 d . . . H32A H 0.5035 0.3992 0.8628 0.061 Uiso 1 1 calc R . . C33 C 0.6483(8) 0.37576(19) 0.9491(5) 0.0516(19) Uani 1 1 d . . . H33A H 0.6140 0.3823 1.0129 0.062 Uiso 1 1 calc R . . C34 C 0.7634(7) 0.35615(18) 0.9470(5) 0.0466(17) Uani 1 1 d . . . C35 C 0.8086(7) 0.34636(19) 0.8511(5) 0.0487(18) Uani 1 1 d . . . H35A H 0.8840 0.3322 0.8477 0.058 Uiso 1 1 calc R . . C36 C 0.7459(7) 0.35676(18) 0.7610(5) 0.0485(18) Uani 1 1 d . . . H36A H 0.7812 0.3500 0.6977 0.058 Uiso 1 1 calc R . . C37 C 0.8349(8) 0.34559(19) 1.0438(5) 0.0509(19) Uani 1 1 d . . . C38 C 0.8595(11) 0.3665(2) 1.1243(7) 0.080(3) Uani 1 1 d . . . H38A H 0.8317 0.3882 1.1187 0.096 Uiso 1 1 calc R . . C39 C 0.9258(14) 0.3556(3) 1.2149(8) 0.104(4) Uani 1 1 d . . . H39A H 0.9430 0.3702 1.2693 0.125 Uiso 1 1 calc R . . C40 C 0.9649(10) 0.3243(2) 1.2245(6) 0.071(3) Uani 1 1 d . . . H40A H 1.0055 0.3170 1.2865 0.085 Uiso 1 1 calc R . . C41 C 0.9455(8) 0.3032(2) 1.1437(6) 0.058(2) Uani 1 1 d . . . H41A H 0.9766 0.2817 1.1494 0.070 Uiso 1 1 calc R . . C42 C 0.8798(7) 0.31369(19) 1.0537(5) 0.0498(18) Uani 1 1 d . . . H42A H 0.8655 0.2991 0.9990 0.060 Uiso 1 1 calc R . . C46 C 0.6688(18) 0.4646(4) 1.0516(11) 0.129(5) Uani 1 1 d . . . H46A H 0.5926 0.4581 1.0950 0.155 Uiso 1 1 calc R . . H46B H 0.6437 0.4601 0.9796 0.155 Uiso 1 1 calc R . . C47 C 0.700(3) 0.4995(4) 1.0659(18) 0.189(10) Uani 1 1 d . . . H47A H 0.7079 0.5105 0.9995 0.226 Uiso 1 1 calc R . . H47B H 0.6291 0.5102 1.1059 0.226 Uiso 1 1 calc R . . C49 C 0.896(2) 0.4687(5) 1.1127(14) 0.158(7) Uani 1 1 d . . . H49A H 0.9682 0.4696 1.0618 0.190 Uiso 1 1 calc R . . H49B H 0.9359 0.4620 1.1790 0.190 Uiso 1 1 calc R . . C48 C 0.830(3) 0.4993(6) 1.121(3) 0.253(17) Uani 1 1 d . . . H48A H 0.8895 0.5162 1.0940 0.303 Uiso 1 1 calc R . . H48B H 0.8150 0.5040 1.1942 0.303 Uiso 1 1 calc R . . O1 O 1.3067(5) 0.27698(14) 0.5904(4) 0.0600(14) Uani 1 1 d . . . O2 O 0.9646(5) 0.27924(15) 0.7925(3) 0.0597(15) Uani 1 1 d . . . O3 O 0.9492(6) 0.33648(13) 0.5107(4) 0.0614(14) Uani 1 1 d . . . O4 O 0.4558(6) 0.48657(14) 0.2561(4) 0.0704(16) Uani 1 1 d . . . O5 O 0.3852(16) 0.3921(2) 0.1665(6) 0.193(6) Uani 1 1 d . . . O6 O 0.0886(7) 0.4412(3) 0.3551(8) 0.150(4) Uani 1 1 d . . . O7 O 0.7922(15) 0.4477(3) 1.0812(9) 0.154(4) Uani 1 1 d . . . Si1 Si 0.8134(2) 0.19035(5) 0.43188(14) 0.0446(5) Uani 1 1 d . . . Si2 Si 0.5534(2) 0.39170(5) 0.63839(14) 0.0453(5) Uani 1 1 d . . . S1 S 0.74617(18) 0.25141(5) 0.55084(13) 0.0456(4) Uani 1 1 d . . . S2 S 0.99953(19) 0.24615(4) 0.36925(12) 0.0429(4) Uani 1 1 d . . . S3 S 1.03544(18) 0.20279(5) 0.58991(13) 0.0443(4) Uani 1 1 d . . . S4 S 0.3104(3) 0.37759(6) 0.49403(19) 0.0465(7) Uani 0.717(3) 1 d P A . S4F S 0.4199(7) 0.36365(16) 0.4420(5) 0.0475(18) Uiso 0.283(3) 1 d P A 1 S5 S 0.4461(2) 0.45517(6) 0.55179(17) 0.0418(7) Uani 0.717(3) 1 d P A . S5F S 0.3456(7) 0.43753(16) 0.5550(5) 0.0455(17) Uiso 0.283(3) 1 d P A 1 S6 S 0.6277(3) 0.40075(7) 0.41144(19) 0.0481(7) Uani 0.717(3) 1 d P A . S6F S 0.6555(7) 0.42536(18) 0.4407(5) 0.0477(17) Uiso 0.283(3) 1 d P A 1 W2 W 0.39690(3) 0.424130(8) 0.38231(2) 0.04807(10) Uani 1 1 d . . . W1 W 0.99796(3) 0.263052(7) 0.559607(19) 0.03844(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(4) 0.061(5) 0.043(4) -0.003(3) -0.003(3) -0.003(3) C2 0.043(4) 0.048(4) 0.042(4) -0.001(3) 0.003(3) 0.002(3) C3 0.056(5) 0.050(5) 0.049(4) 0.008(3) 0.001(4) -0.007(4) C4 0.042(4) 0.075(6) 0.073(5) -0.011(4) -0.003(4) 0.008(4) C5 0.052(5) 0.078(6) 0.047(4) -0.005(4) 0.018(4) -0.009(4) C6 0.069(5) 0.077(6) 0.045(4) 0.014(4) -0.010(4) -0.005(5) C7 0.056(5) 0.046(4) 0.041(4) 0.001(3) 0.007(4) -0.002(4) C8 0.028(3) 0.058(5) 0.062(5) 0.005(4) 0.000(3) 0.000(3) C9 0.035(4) 0.061(5) 0.034(3) -0.010(3) -0.003(3) 0.005(3) C10 0.049(4) 0.052(5) 0.043(4) -0.001(3) 0.000(3) -0.005(4) C11 0.073(6) 0.060(5) 0.050(4) 0.004(4) -0.017(4) -0.010(4) C12 0.074(6) 0.049(5) 0.060(5) 0.012(4) -0.018(4) -0.014(4) C13 0.042(4) 0.049(4) 0.052(4) -0.005(3) -0.003(3) 0.001(3) C14 0.042(4) 0.052(5) 0.045(4) -0.008(3) 0.002(3) -0.002(3) C15 0.043(4) 0.044(4) 0.047(4) 0.000(3) 0.006(3) -0.004(3) C16 0.045(4) 0.056(5) 0.054(4) -0.003(4) -0.012(3) 0.001(4) C17 0.040(4) 0.052(5) 0.069(5) -0.011(4) -0.005(4) 0.001(4) C18 0.058(5) 0.068(6) 0.077(6) -0.026(5) 0.001(5) 0.001(5) C19 0.085(7) 0.058(6) 0.082(6) -0.014(5) -0.015(5) -0.013(5) C20 0.079(6) 0.061(6) 0.081(6) 0.003(5) -0.010(5) -0.015(5) C21 0.062(5) 0.059(5) 0.063(5) 0.000(4) -0.001(4) -0.013(4) C22 0.052(4) 0.050(5) 0.050(4) 0.003(3) 0.003(4) -0.001(4) C23 0.070(5) 0.058(5) 0.050(4) -0.005(4) -0.010(4) 0.007(4) C24 0.044(4) 0.073(6) 0.052(4) 0.005(4) -0.001(4) -0.009(4) C25 0.074(6) 0.074(6) 0.064(5) -0.002(5) -0.015(5) -0.022(5) C26 0.053(5) 0.046(4) 0.069(5) 0.005(4) -0.002(4) 0.004(4) C27 0.061(6) 0.139(10) 0.067(6) 0.019(6) 0.017(5) -0.016(6) C28 0.052(5) 0.067(6) 0.048(4) -0.008(4) -0.005(4) -0.003(4) C29 0.179(13) 0.052(6) 0.077(7) 0.002(5) -0.030(7) 0.017(7) C30 0.059(6) 0.140(10) 0.091(7) 0.065(7) -0.014(5) -0.028(6) C31 0.040(4) 0.048(4) 0.045(4) 0.005(3) 0.003(3) 0.001(3) C32 0.044(4) 0.061(5) 0.048(4) 0.003(4) -0.006(3) 0.006(4) C33 0.059(5) 0.055(5) 0.041(4) 0.001(3) 0.001(4) 0.009(4) C34 0.048(4) 0.047(4) 0.045(4) 0.004(3) -0.005(3) -0.005(3) C35 0.044(4) 0.055(5) 0.047(4) 0.005(3) 0.001(3) 0.005(3) C36 0.047(4) 0.055(5) 0.044(4) 0.005(3) 0.003(3) 0.002(4) C37 0.056(5) 0.055(5) 0.042(4) 0.005(3) -0.006(4) 0.000(4) C38 0.109(8) 0.052(5) 0.079(6) -0.010(5) -0.032(6) 0.017(5) C39 0.163(12) 0.065(7) 0.082(7) -0.023(5) -0.068(7) 0.009(7) C40 0.094(7) 0.065(6) 0.053(5) 0.002(4) -0.029(5) 0.005(5) C41 0.058(5) 0.063(5) 0.054(4) 0.002(4) -0.007(4) 0.006(4) C42 0.045(4) 0.059(5) 0.045(4) 0.000(3) -0.009(3) 0.007(4) C46 0.177(16) 0.103(11) 0.107(10) 0.010(8) 0.009(10) 0.019(11) C47 0.24(3) 0.105(14) 0.22(2) -0.013(14) 0.11(2) -0.020(16) C49 0.21(2) 0.134(15) 0.129(13) 0.025(11) 0.022(13) -0.055(15) C48 0.17(2) 0.18(2) 0.42(4) -0.15(3) 0.08(3) -0.055(19) O1 0.032(3) 0.067(4) 0.080(4) 0.003(3) -0.003(3) -0.005(3) O2 0.055(3) 0.097(4) 0.027(2) -0.015(3) -0.001(2) 0.007(3) O3 0.070(4) 0.044(3) 0.070(3) 0.000(3) -0.001(3) 0.003(3) O4 0.084(4) 0.062(4) 0.065(3) 0.022(3) -0.006(3) -0.005(3) O5 0.42(2) 0.094(6) 0.064(5) -0.043(5) -0.078(8) 0.078(9) O6 0.046(4) 0.216(11) 0.186(9) 0.110(8) -0.025(5) -0.021(5) O7 0.190(12) 0.116(8) 0.155(9) 0.015(7) -0.029(8) 0.009(9) Si1 0.0468(11) 0.0495(12) 0.0374(9) 0.0011(8) -0.0012(9) -0.0063(9) Si2 0.0422(11) 0.0519(12) 0.0418(10) 0.0051(9) -0.0004(9) 0.0017(9) S1 0.0356(9) 0.0632(12) 0.0381(9) -0.0073(8) 0.0019(7) 0.0003(8) S2 0.0484(10) 0.0493(11) 0.0312(8) -0.0004(7) 0.0046(7) -0.0021(8) S3 0.0420(9) 0.0534(11) 0.0373(8) 0.0036(8) -0.0040(7) -0.0004(8) S4 0.0403(14) 0.0524(16) 0.0467(14) 0.0017(11) -0.0009(11) -0.0006(12) S5 0.0427(13) 0.0433(14) 0.0392(12) 0.0019(10) -0.0011(10) -0.0005(11) S6 0.0455(14) 0.0559(18) 0.0432(13) 0.0041(12) 0.0079(11) 0.0078(12) W2 0.05191(19) 0.04881(19) 0.04310(17) 0.00366(13) -0.00774(13) -0.00535(15) W1 0.03412(15) 0.04853(18) 0.03267(14) -0.00165(12) 0.00095(10) -0.00041(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 C1 S1 1.825(7) . ? C1 Si1 1.892(8) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 S2 1.839(7) . ? C2 Si1 1.889(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 S3 1.801(8) . ? C3 Si1 1.914(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 S1 1.814(9) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 S2 1.778(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 S3 1.810(7) . ? C6 H6C 0.9800 . ? C6 H6B 0.9800 . ? C6 H6A 0.9800 . ? C7 O1 1.166(9) . ? C7 W1 1.946(8) . ? C8 O2 1.186(8) . ? C8 W1 1.969(8) . ? C9 O3 1.182(9) . ? C9 W1 1.984(8) . ? C10 C11 1.410(10) . ? C10 C15 1.415(10) . ? C10 Si1 1.878(8) . ? C11 C12 1.388(11) . ? C11 H11A 0.9500 . ? C12 C13 1.412(11) . ? C12 H12A 0.9500 . ? C13 C14 1.395(10) . ? C13 C16 1.490(10) . ? C14 C15 1.397(10) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.413(10) . ? C16 C21 1.426(11) . ? C17 C18 1.382(11) . ? C17 H17A 0.9500 . ? C18 C19 1.391(12) . ? C18 H18A 0.9500 . ? C19 C20 1.404(12) . ? C19 H19A 0.9500 . ? C20 C21 1.382(12) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 S4 1.796(8) . ? C22 Si2 1.892(8) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 S5 1.785(8) . ? C23 Si2 1.897(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 S6 1.818(8) . ? C24 Si2 1.878(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 S4 1.818(9) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 S5 1.781(8) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 S6 1.785(9) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 O4 1.195(9) . ? C28 W2 1.954(9) . ? C29 O5 1.196(12) . ? C29 W2 1.938(11) . ? C30 O6 1.202(12) . ? C30 W2 1.927(11) . ? C31 C36 1.408(10) . ? C31 C32 1.433(9) . ? C31 Si2 1.873(7) . ? C32 C33 1.407(10) . ? C32 H32A 0.9500 . ? C33 C34 1.399(10) . ? C33 H33A 0.9500 . ? C34 C35 1.405(9) . ? C34 C37 1.505(10) . ? C35 C36 1.391(10) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.387(11) . ? C37 C42 1.408(11) . ? C38 C39 1.417(13) . ? C38 H38A 0.9500 . ? C39 C40 1.367(13) . ? C39 H39A 0.9500 . ? C40 C41 1.388(11) . ? C40 H40A 0.9500 . ? C41 C42 1.404(10) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C46 O7 1.452(17) . ? C46 C47 1.50(2) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.46(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C49 O7 1.401(19) . ? C49 C48 1.43(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? S1 W1 2.5258(18) . ? S2 W1 2.5968(16) . ? S3 W1 2.5713(19) . ? S4 W2 2.589(3) . ? S4F W2 2.651(7) . ? S5 W2 2.610(2) . ? S5F W2 2.399(6) . ? S6 W2 2.494(3) . ? S6F W2 2.642(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 C1 Si1 111.3(4) . . ? S1 C1 H1A 109.4 . . ? Si1 C1 H1A 109.4 . . ? S1 C1 H1B 109.4 . . ? Si1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? S2 C2 Si1 111.7(3) . . ? S2 C2 H2A 109.3 . . ? Si1 C2 H2A 109.3 . . ? S2 C2 H2B 109.3 . . ? Si1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? S3 C3 Si1 109.0(4) . . ? S3 C3 H3A 109.9 . . ? Si1 C3 H3A 109.9 . . ? S3 C3 H3B 109.9 . . ? Si1 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? S1 C4 H4A 109.5 . . ? S1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? S1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? S2 C5 H5A 109.5 . . ? S2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? S3 C6 H6C 109.5 . . ? S3 C6 H6B 109.5 . . ? H6C C6 H6B 109.5 . . ? S3 C6 H6A 109.5 . . ? H6C C6 H6A 109.5 . . ? H6B C6 H6A 109.5 . . ? O1 C7 W1 177.7(7) . . ? O2 C8 W1 179.1(7) . . ? O3 C9 W1 177.8(6) . . ? C11 C10 C15 117.7(7) . . ? C11 C10 Si1 121.2(6) . . ? C15 C10 Si1 121.1(5) . . ? C12 C11 C10 121.0(7) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 121.2(7) . . ? C11 C12 H12A 119.4 . . ? C13 C12 H12A 119.4 . . ? C14 C13 C12 118.1(7) . . ? C14 C13 C16 121.4(7) . . ? C12 C13 C16 120.5(7) . . ? C13 C14 C15 121.2(7) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C14 C15 C10 120.9(7) . . ? C14 C15 H15A 119.6 . . ? C10 C15 H15A 119.6 . . ? C17 C16 C21 117.8(7) . . ? C17 C16 C13 122.0(7) . . ? C21 C16 C13 120.2(7) . . ? C18 C17 C16 122.6(8) . . ? C18 C17 H17A 118.7 . . ? C16 C17 H17A 118.7 . . ? C17 C18 C19 118.9(8) . . ? C17 C18 H18A 120.5 . . ? C19 C18 H18A 120.5 . . ? C18 C19 C20 119.7(8) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C21 C20 C19 121.9(9) . . ? C21 C20 H20A 119.1 . . ? C19 C20 H20A 119.1 . . ? C20 C21 C16 119.0(8) . . ? C20 C21 H21A 120.5 . . ? C16 C21 H21A 120.5 . . ? S4 C22 Si2 112.9(4) . . ? S4 C22 H22A 109.0 . . ? Si2 C22 H22A 109.0 . . ? S4 C22 H22B 109.0 . . ? Si2 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? S5 C23 Si2 112.4(4) . . ? S5 C23 H23A 109.1 . . ? Si2 C23 H23A 109.1 . . ? S5 C23 H23B 109.1 . . ? Si2 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? S6 C24 Si2 114.4(4) . . ? S6 C24 H24A 108.7 . . ? Si2 C24 H24A 108.7 . . ? S6 C24 H24B 108.7 . . ? Si2 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? S4 C25 H25A 109.5 . . ? S4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S5 C26 H26A 109.5 . . ? S5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? S6 C27 H27A 109.5 . . ? S6 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S6 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O4 C28 W2 177.5(7) . . ? O5 C29 W2 176.6(11) . . ? O6 C30 W2 177.8(13) . . ? C36 C31 C32 116.5(7) . . ? C36 C31 Si2 120.6(5) . . ? C32 C31 Si2 122.9(5) . . ? C33 C32 C31 120.9(7) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C34 C33 C32 121.6(6) . . ? C34 C33 H33A 119.2 . . ? C32 C33 H33A 119.2 . . ? C33 C34 C35 117.4(7) . . ? C33 C34 C37 121.3(6) . . ? C35 C34 C37 121.3(7) . . ? C36 C35 C34 121.9(7) . . ? C36 C35 H35A 119.1 . . ? C34 C35 H35A 119.1 . . ? C35 C36 C31 121.7(6) . . ? C35 C36 H36A 119.1 . . ? C31 C36 H36A 119.1 . . ? C38 C37 C42 118.3(7) . . ? C38 C37 C34 122.0(7) . . ? C42 C37 C34 119.7(7) . . ? C37 C38 C39 120.6(9) . . ? C37 C38 H38A 119.7 . . ? C39 C38 H38A 119.7 . . ? C40 C39 C38 120.4(9) . . ? C40 C39 H39A 119.8 . . ? C38 C39 H39A 119.8 . . ? C39 C40 C41 120.1(8) . . ? C39 C40 H40A 119.9 . . ? C41 C40 H40A 119.9 . . ? C40 C41 C42 120.0(8) . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C41 C42 C37 120.6(7) . . ? C41 C42 H42A 119.7 . . ? C37 C42 H42A 119.7 . . ? O7 C46 C47 105.7(16) . . ? O7 C46 H46A 110.6 . . ? C47 C46 H46A 110.6 . . ? O7 C46 H46B 110.6 . . ? C47 C46 H46B 110.6 . . ? H46A C46 H46B 108.7 . . ? C48 C47 C46 103(2) . . ? C48 C47 H47A 111.1 . . ? C46 C47 H47A 111.1 . . ? C48 C47 H47B 111.1 . . ? C46 C47 H47B 111.1 . . ? H47A C47 H47B 109.0 . . ? O7 C49 C48 104.8(18) . . ? O7 C49 H49A 110.8 . . ? C48 C49 H49A 110.8 . . ? O7 C49 H49B 110.8 . . ? C48 C49 H49B 110.8 . . ? H49A C49 H49B 108.9 . . ? C49 C48 C47 110.9(19) . . ? C49 C48 H48A 109.5 . . ? C47 C48 H48A 109.5 . . ? C49 C48 H48B 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 108.0 . . ? C49 O7 C46 111.8(14) . . ? C10 Si1 C2 111.2(3) . . ? C10 Si1 C1 111.2(3) . . ? C2 Si1 C1 105.7(3) . . ? C10 Si1 C3 110.3(3) . . ? C2 Si1 C3 110.1(3) . . ? C1 Si1 C3 108.2(3) . . ? C31 Si2 C24 110.8(3) . . ? C31 Si2 C22 111.8(3) . . ? C24 Si2 C22 106.2(3) . . ? C31 Si2 C23 110.1(3) . . ? C24 Si2 C23 108.4(4) . . ? C22 Si2 C23 109.5(4) . . ? C4 S1 C1 101.6(4) . . ? C4 S1 W1 109.9(3) . . ? C1 S1 W1 113.0(2) . . ? C5 S2 C2 99.9(4) . . ? C5 S2 W1 108.3(3) . . ? C2 S2 W1 113.6(2) . . ? C3 S3 C6 101.8(4) . . ? C3 S3 W1 111.7(3) . . ? C6 S3 W1 111.4(3) . . ? C22 S4 C25 102.1(4) . . ? C22 S4 W2 114.0(3) . . ? C25 S4 W2 108.1(3) . . ? C26 S5 C23 104.3(4) . . ? C26 S5 W2 111.8(3) . . ? C23 S5 W2 113.1(3) . . ? C27 S6 C24 102.4(4) . . ? C27 S6 W2 111.7(4) . . ? C24 S6 W2 115.0(3) . . ? C30 W2 C29 87.7(6) . . ? C30 W2 C28 87.4(4) . . ? C29 W2 C28 85.2(4) . . ? C30 W2 S5F 81.0(4) . . ? C29 W2 S5F 160.6(4) . . ? C28 W2 S5F 109.9(3) . . ? C30 W2 S6 169.4(3) . . ? C29 W2 S6 89.3(4) . . ? C28 W2 S6 102.5(2) . . ? S5F W2 S6 99.01(17) . . ? C30 W2 S4 84.5(3) . . ? C29 W2 S4 99.4(3) . . ? C28 W2 S4 170.5(2) . . ? S5F W2 S4 63.95(17) . . ? S6 W2 S4 85.96(8) . . ? C30 W2 S5 99.2(4) . . ? C29 W2 S5 171.1(4) . . ? C28 W2 S5 89.5(2) . . ? S5F W2 S5 28.14(16) . . ? S6 W2 S5 84.97(8) . . ? S4 W2 S5 86.94(8) . . ? C30 W2 S6F 163.4(4) . . ? C29 W2 S6F 107.1(5) . . ? C28 W2 S6F 86.3(3) . . ? S5F W2 S6F 86.7(2) . . ? S6 W2 S6F 25.16(16) . . ? S4 W2 S6F 100.19(16) . . ? S5 W2 S6F 65.40(16) . . ? C30 W2 S4F 108.7(4) . . ? C29 W2 S4F 81.0(3) . . ? C28 W2 S4F 158.1(3) . . ? S5F W2 S4F 87.8(2) . . ? S6 W2 S4F 60.70(16) . . ? S4 W2 S4F 31.28(14) . . ? S5 W2 S4F 101.96(15) . . ? S6F W2 S4F 81.8(2) . . ? C7 W1 C8 88.1(3) . . ? C7 W1 C9 89.4(3) . . ? C8 W1 C9 88.8(3) . . ? C7 W1 S1 175.8(2) . . ? C8 W1 S1 88.0(2) . . ? C9 W1 S1 92.2(2) . . ? C7 W1 S3 91.2(2) . . ? C8 W1 S3 94.7(2) . . ? C9 W1 S3 176.47(18) . . ? S1 W1 S3 87.49(6) . . ? C7 W1 S2 97.8(2) . . ? C8 W1 S2 173.7(2) . . ? C9 W1 S2 93.41(18) . . ? S1 W1 S2 86.03(6) . . ? S3 W1 S2 83.06(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.935 _refine_diff_density_min -1.345 _refine_diff_density_rms 0.118