Supplementary Material (ESI) for Photochemical & Photobiological Sciences This journal is © The Royal Society of Chemistry and Owner Societies 2005 data_global _journal_coden_Cambridge 171 loop_ _publ_author_name 'Antonios K. Zarkadis' 'V. Georgakilas' 'Gagik Gurzadyan' 'Gerasimos P. Perdikomatis' 'Michael Siskos' 'Stavroula Skoulika' 'Anton Trifonov' _publ_contact_author_name 'Dr Antonios K Zarkadis' _publ_contact_author_address ; Department of Chemistry University of Ioannina IOANNINA 451 10 GREECE ; _publ_contact_author_email AZARKAD@CC.UOI.GR _publ_requested_journal Phys.Chem.Chem.Phys. _publ_section_title ; Triplet- vs. Singlet-State Imposed Photochemistry. The Role of Substituent Effects on the Photo-Fries and Photodissociation Reaction of Triphenylmethyl Silanes ; data_orsi2 _database_code_depnum_ccdc_archive 'CCDC 263099' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 Si' _chemical_formula_weight 316.50 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.986(2) _cell_length_b 12.9990(10) _cell_length_c 18.745(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.350(10) _cell_angle_gamma 90.00 _cell_volume 3718.0(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 9 _cell_measurement_theta_max 12 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type P4 _diffrn_measurement_method scintillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3395 _diffrn_reflns_av_R_equivalents 0.0178 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3269 _reflns_number_gt 2248 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL97 _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 w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+1.3405P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3269 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.066 _refine_ls_shift/su_mean 0.013 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.16769(4) 0.98301(6) 0.39373(4) 0.0508(2) Uani 1 d . . . C1 C 0.29507(14) 0.99788(16) 0.43736(12) 0.0385(5) Uani 1 d . . . C2 C 0.32015(15) 1.00470(17) 0.52296(12) 0.0422(6) Uani 1 d . . . C3 C 0.38276(17) 1.0731(2) 0.56302(14) 0.0517(6) Uani 1 d . . . C4 C 0.4100(2) 1.0737(3) 0.64052(16) 0.0661(8) Uani 1 d . . . C5 C 0.3748(2) 1.0069(3) 0.67944(18) 0.0710(9) Uani 1 d . . . C6 C 0.3117(2) 0.9394(2) 0.64157(17) 0.0672(8) Uani 1 d . . . C7 C 0.28451(19) 0.9379(2) 0.56409(15) 0.0546(7) Uani 1 d . . . C8 C 0.1061(3) 1.0478(4) 0.4515(3) 0.0843(11) Uani 1 d . . . C9 C 0.1311(3) 1.0408(3) 0.2978(2) 0.0753(10) Uani 1 d . . . C10 C 0.1343(3) 0.8450(3) 0.3849(3) 0.0758(10) Uani 1 d . . . C22 C 0.32378(15) 1.09593(17) 0.40555(12) 0.0406(5) Uani 1 d . . . C23 C 0.39253(17) 1.0978(2) 0.37475(14) 0.0494(6) Uani 1 d . . . C24 C 0.4172(2) 1.1882(3) 0.34746(17) 0.0673(8) Uani 1 d . . . C25 C 0.3746(2) 1.2782(2) 0.35093(18) 0.0727(9) Uani 1 d . . . C26 C 0.3072(2) 1.2791(2) 0.38198(19) 0.0693(9) Uani 1 d . . . C27 C 0.28249(18) 1.1894(2) 0.40932(16) 0.0558(7) Uani 1 d . . . C32 C 0.33679(14) 0.90148(17) 0.41407(12) 0.0386(5) Uani 1 d . . . C33 C 0.39635(16) 0.84024(19) 0.46487(14) 0.0463(6) Uani 1 d . . . C34 C 0.43142(19) 0.7533(2) 0.44169(17) 0.0574(7) Uani 1 d . . . C35 C 0.4087(2) 0.7257(2) 0.36819(17) 0.0626(8) Uani 1 d . . . C36 C 0.3510(2) 0.7870(2) 0.31681(17) 0.0622(8) Uani 1 d . . . C37 C 0.31573(18) 0.8729(2) 0.33910(14) 0.0522(6) Uani 1 d . . . H1 H 0.4235(17) 1.039(2) 0.3719(14) 0.054(7) Uiso 1 d . . . H2 H 0.4049(17) 1.120(2) 0.5368(14) 0.057(8) Uiso 1 d . . . H3 H 0.4128(16) 0.8556(19) 0.5141(14) 0.050(7) Uiso 1 d . . . H4 H 0.2765(17) 0.9115(19) 0.3021(14) 0.053(7) Uiso 1 d . . . H5 H 0.2412(17) 0.8904(19) 0.5387(13) 0.051(7) Uiso 1 d . . . H6 H 0.2873(18) 0.895(2) 0.6666(15) 0.060(8) Uiso 1 d . . . H7 H 0.048(3) 1.034(2) 0.4282(18) 0.087(10) Uiso 1 d . . . H8 H 0.389(2) 1.009(2) 0.7315(19) 0.088(10) Uiso 1 d . . . H9 H 0.4366(19) 0.670(2) 0.3516(16) 0.077(9) Uiso 1 d . . . H10 H 0.4720(18) 0.714(2) 0.4760(14) 0.063(8) Uiso 1 d . . . H11 H 0.389(2) 1.337(2) 0.3310(16) 0.076(9) Uiso 1 d . . . H12 H 0.2358(18) 1.191(2) 0.4308(15) 0.062(8) Uiso 1 d . . . H13 H 0.3364(18) 0.766(2) 0.2690(16) 0.068(9) Uiso 1 d . . . H14 H 0.4624(19) 1.184(2) 0.3272(16) 0.072(9) Uiso 1 d . . . H15 H 0.4526(19) 1.123(2) 0.6663(16) 0.074(9) Uiso 1 d . . . H16 H 0.112(2) 1.118(3) 0.453(2) 0.106(14) Uiso 1 d . . . H17 H 0.150(3) 0.815(3) 0.348(2) 0.122(17) Uiso 1 d . . . H18 H 0.122(3) 1.011(3) 0.498(3) 0.141(19) Uiso 1 d . . . H19 H 0.279(2) 1.337(2) 0.3862(16) 0.075(9) Uiso 1 d . . . H21 H 0.158(3) 0.809(3) 0.431(2) 0.120(15) Uiso 1 d . . . H22 H 0.077(3) 0.834(3) 0.375(2) 0.122(15) Uiso 1 d . . . H23 H 0.168(3) 1.031(3) 0.270(2) 0.135(18) Uiso 1 d . . . H24 H 0.114(3) 1.107(4) 0.303(3) 0.150(19) Uiso 1 d . . . H25 H 0.083(4) 1.009(4) 0.270(3) 0.17(2) Uiso 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 Si 0.0381(4) 0.0489(4) 0.0624(5) 0.0041(3) 0.0105(3) 0.0008(3) C1 0.0389(11) 0.0353(12) 0.0410(12) 0.0020(9) 0.0118(9) 0.0020(9) C2 0.0428(12) 0.0448(13) 0.0413(13) 0.0039(10) 0.0162(10) 0.0099(10) C3 0.0495(15) 0.0605(17) 0.0451(15) -0.0021(13) 0.0141(12) 0.0002(12) C4 0.0646(18) 0.083(2) 0.0450(16) -0.0108(15) 0.0084(14) -0.0009(16) C5 0.087(2) 0.086(2) 0.0414(16) -0.0008(16) 0.0215(16) 0.0158(19) C6 0.091(2) 0.0638(19) 0.0584(18) 0.0155(16) 0.0396(18) 0.0104(17) C7 0.0644(17) 0.0492(15) 0.0539(16) 0.0028(13) 0.0234(14) 0.0029(13) C8 0.052(2) 0.095(3) 0.111(3) -0.003(3) 0.031(2) 0.018(2) C9 0.059(2) 0.078(2) 0.073(2) 0.0142(18) -0.0062(18) -0.0006(18) C10 0.065(2) 0.066(2) 0.095(3) 0.001(2) 0.022(2) -0.0219(17) C22 0.0407(13) 0.0408(13) 0.0372(12) 0.0007(10) 0.0065(10) -0.0015(10) C23 0.0535(15) 0.0457(15) 0.0491(14) 0.0009(12) 0.0156(12) -0.0042(12) C24 0.072(2) 0.072(2) 0.0625(19) 0.0049(15) 0.0261(16) -0.0208(17) C25 0.087(2) 0.0523(19) 0.068(2) 0.0154(15) 0.0076(17) -0.0220(17) C26 0.074(2) 0.0390(16) 0.084(2) 0.0076(14) 0.0070(18) 0.0014(15) C27 0.0542(16) 0.0432(15) 0.0666(18) 0.0018(13) 0.0128(14) 0.0036(12) C32 0.0361(12) 0.0374(12) 0.0423(13) 0.0025(10) 0.0117(10) -0.0003(9) C33 0.0485(14) 0.0479(14) 0.0422(14) 0.0016(11) 0.0128(11) 0.0076(11) C34 0.0602(17) 0.0521(16) 0.0597(18) 0.0074(13) 0.0177(14) 0.0189(13) C35 0.0717(19) 0.0498(16) 0.070(2) -0.0075(14) 0.0264(16) 0.0144(14) C36 0.0733(19) 0.0645(18) 0.0473(16) -0.0155(14) 0.0158(15) 0.0078(15) C37 0.0574(16) 0.0502(15) 0.0441(14) 0.0004(12) 0.0077(12) 0.0102(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 Si C10 1.865(3) . ? Si C8 1.867(4) . ? Si C9 1.873(4) . ? Si C1 1.965(2) . ? C1 C22 1.534(3) . ? C1 C2 1.536(3) . ? C1 C32 1.542(3) . ? C2 C3 1.381(3) . ? C2 C7 1.391(3) . ? C3 C4 1.387(4) . ? C3 H2 0.92(3) . ? C4 C5 1.360(4) . ? C4 H15 0.95(3) . ? C5 C6 1.365(5) . ? C5 H8 0.93(3) . ? C6 C7 1.387(4) . ? C6 H6 0.90(3) . ? C7 H5 0.94(3) . ? C8 H7 0.92(4) . ? C8 H16 0.92(4) . ? C8 H18 0.95(4) . ? C9 H23 0.90(4) . ? C9 H24 0.92(5) . ? C9 H25 0.89(6) . ? C10 H17 0.89(4) . ? C10 H21 0.96(4) . ? C10 H22 0.90(4) . ? C22 C23 1.386(3) . ? C22 C27 1.395(3) . ? C23 C24 1.385(4) . ? C23 H1 0.92(3) . ? C24 C25 1.366(5) . ? C24 H14 0.91(3) . ? C25 C26 1.368(5) . ? C25 H11 0.91(3) . ? C26 C27 1.378(4) . ? C26 H19 0.90(3) . ? C27 H12 0.95(3) . ? C32 C33 1.381(3) . ? C32 C37 1.394(3) . ? C33 C34 1.388(4) . ? C33 H3 0.90(2) . ? C34 C35 1.364(4) . ? C34 H10 0.92(3) . ? C35 C36 1.373(4) . ? C35 H9 0.95(3) . ? C36 C37 1.371(4) . ? C36 H13 0.90(3) . ? C37 H4 0.93(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Si C8 107.4(2) . . ? C10 Si C9 107.5(2) . . ? C8 Si C9 107.9(2) . . ? C10 Si C1 111.45(15) . . ? C8 Si C1 112.00(16) . . ? C9 Si C1 110.40(15) . . ? C22 C1 C2 110.05(18) . . ? C22 C1 C32 111.11(17) . . ? C2 C1 C32 110.02(17) . . ? C22 C1 Si 108.24(14) . . ? C2 C1 Si 110.84(14) . . ? C32 C1 Si 106.51(14) . . ? C3 C2 C7 116.8(2) . . ? C3 C2 C1 121.7(2) . . ? C7 C2 C1 121.4(2) . . ? C2 C3 C4 121.6(3) . . ? C2 C3 H2 117.9(16) . . ? C4 C3 H2 120.5(16) . . ? C5 C4 C3 120.5(3) . . ? C5 C4 H15 120.3(17) . . ? C3 C4 H15 119.2(17) . . ? C4 C5 C6 119.4(3) . . ? C4 C5 H8 122(2) . . ? C6 C5 H8 118(2) . . ? C5 C6 C7 120.4(3) . . ? C5 C6 H6 120.3(17) . . ? C7 C6 H6 119.3(18) . . ? C6 C7 C2 121.3(3) . . ? C6 C7 H5 119.5(15) . . ? C2 C7 H5 119.3(15) . . ? Si C8 H7 106(2) . . ? Si C8 H16 113(2) . . ? H7 C8 H16 107(3) . . ? Si C8 H18 105(3) . . ? H7 C8 H18 107(3) . . ? H16 C8 H18 118(4) . . ? Si C9 H23 115(3) . . ? Si C9 H24 107(3) . . ? H23 C9 H24 117(4) . . ? Si C9 H25 110(3) . . ? H23 C9 H25 102(4) . . ? H24 C9 H25 105(4) . . ? Si C10 H17 110(3) . . ? Si C10 H21 111(2) . . ? H17 C10 H21 111(4) . . ? Si C10 H22 115(3) . . ? H17 C10 H22 107(4) . . ? H21 C10 H22 102(3) . . ? C23 C22 C27 116.9(2) . . ? C23 C22 C1 122.9(2) . . ? C27 C22 C1 120.2(2) . . ? C24 C23 C22 121.2(3) . . ? C24 C23 H1 117.6(16) . . ? C22 C23 H1 121.2(16) . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H14 122.4(19) . . ? C23 C24 H14 117.1(19) . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H11 120.4(19) . . ? C26 C25 H11 119.8(19) . . ? C25 C26 C27 120.0(3) . . ? C25 C26 H19 122.2(19) . . ? C27 C26 H19 118(2) . . ? C26 C27 C22 121.7(3) . . ? C26 C27 H12 119.1(17) . . ? C22 C27 H12 119.2(17) . . ? C33 C32 C37 116.8(2) . . ? C33 C32 C1 122.7(2) . . ? C37 C32 C1 120.5(2) . . ? C32 C33 C34 120.9(2) . . ? C32 C33 H3 120.5(16) . . ? C34 C33 H3 118.6(16) . . ? C35 C34 C33 121.3(3) . . ? C35 C34 H10 118.6(16) . . ? C33 C34 H10 120.0(17) . . ? C34 C35 C36 118.5(3) . . ? C34 C35 H9 121.4(18) . . ? C36 C35 H9 119.8(18) . . ? C35 C36 C37 120.7(3) . . ? C35 C36 H13 116.6(18) . . ? C37 C36 H13 122.6(18) . . ? C36 C37 C32 121.8(2) . . ? C36 C37 H4 117.3(15) . . ? C32 C37 H4 120.9(15) . . ? 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 C10 Si C1 C22 149.4(2) . . . . ? C8 Si C1 C22 -90.3(2) . . . . ? C9 Si C1 C22 30.0(2) . . . . ? C10 Si C1 C2 -89.8(2) . . . . ? C8 Si C1 C2 30.5(2) . . . . ? C9 Si C1 C2 150.8(2) . . . . ? C10 Si C1 C32 29.9(2) . . . . ? C8 Si C1 C32 150.2(2) . . . . ? C9 Si C1 C32 -89.5(2) . . . . ? C22 C1 C2 C3 -18.8(3) . . . . ? C32 C1 C2 C3 103.9(2) . . . . ? Si C1 C2 C3 -138.5(2) . . . . ? C22 C1 C2 C7 165.0(2) . . . . ? C32 C1 C2 C7 -72.2(3) . . . . ? Si C1 C2 C7 45.3(3) . . . . ? C7 C2 C3 C4 1.2(4) . . . . ? C1 C2 C3 C4 -175.1(2) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C3 C4 C5 C6 -0.5(5) . . . . ? C4 C5 C6 C7 0.9(5) . . . . ? C5 C6 C7 C2 -0.2(4) . . . . ? C3 C2 C7 C6 -0.8(4) . . . . ? C1 C2 C7 C6 175.5(2) . . . . ? C2 C1 C22 C23 108.9(2) . . . . ? C32 C1 C22 C23 -13.2(3) . . . . ? Si C1 C22 C23 -129.8(2) . . . . ? C2 C1 C22 C27 -68.6(3) . . . . ? C32 C1 C22 C27 169.3(2) . . . . ? Si C1 C22 C27 52.6(2) . . . . ? C27 C22 C23 C24 -1.5(4) . . . . ? C1 C22 C23 C24 -179.2(2) . . . . ? C22 C23 C24 C25 0.6(4) . . . . ? C23 C24 C25 C26 0.4(5) . . . . ? C24 C25 C26 C27 -0.3(5) . . . . ? C25 C26 C27 C22 -0.8(5) . . . . ? C23 C22 C27 C26 1.6(4) . . . . ? C1 C22 C27 C26 179.3(2) . . . . ? C22 C1 C32 C33 114.7(2) . . . . ? C2 C1 C32 C33 -7.5(3) . . . . ? Si C1 C32 C33 -127.6(2) . . . . ? C22 C1 C32 C37 -64.8(3) . . . . ? C2 C1 C32 C37 173.1(2) . . . . ? Si C1 C32 C37 52.9(2) . . . . ? C37 C32 C33 C34 -1.4(4) . . . . ? C1 C32 C33 C34 179.1(2) . . . . ? C32 C33 C34 C35 0.4(4) . . . . ? C33 C34 C35 C36 1.0(4) . . . . ? C34 C35 C36 C37 -1.2(5) . . . . ? C35 C36 C37 C32 0.1(4) . . . . ? C33 C32 C37 C36 1.2(4) . . . . ? C1 C32 C37 C36 -179.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.475 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.475 _refine_diff_density_max 0.219 _refine_diff_density_min -0.196 _refine_diff_density_rms 0.037 data_orsi1 _database_code_depnum_ccdc_archive 'CCDC 263100' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H28 O Si' _chemical_formula_weight 420.60 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' _symmetry_cell_setting Orthorombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.088(2) _cell_length_b 10.053(3) _cell_length_c 13.654(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2345.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.3 _cell_measurement_theta_max 12.5 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.118 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type P4 _diffrn_measurement_method scintillation _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2512 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2352 _reflns_number_gt 1619 _reflns_threshold_expression >2sigma(I) _computing_data_collection XSCANS _computing_cell_refinement XSCANS _computing_data_reduction XSCANS _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL _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 w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+0.3079P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.3(3) _refine_ls_number_reflns 2352 _refine_ls_number_parameters 280 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1616 _refine_ls_wR_factor_gt 0.1316 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si Si 0.10789(9) 0.89931(16) 0.12469(16) 0.0514(5) Uani 1 d . . . C1 C 0.1889(3) 0.7608(5) 0.1086(4) 0.0392(13) Uani 1 d . . . C2 C 0.1417(3) 0.6333(5) 0.1245(5) 0.0398(12) Uani 1 d . . . C3 C 0.1120(3) 0.6060(6) 0.2187(5) 0.0420(14) Uani 1 d . . . H3 H 0.1269 0.6595 0.2711 0.050 Uiso 1 calc R . . C4 C 0.0614(3) 0.5018(6) 0.2348(5) 0.0460(14) Uani 1 d . . . H4 H 0.0424 0.4858 0.2976 0.055 Uiso 1 calc R . . C5 C 0.0383(3) 0.4201(5) 0.1576(4) 0.0403(14) Uani 1 d . . . C6 C 0.0712(4) 0.4413(6) 0.0663(5) 0.0494(15) Uani 1 d . . . H6 H 0.0576 0.3858 0.0146 0.059 Uiso 1 calc R . . C7 C 0.1237(3) 0.5430(6) 0.0505(5) 0.0489(16) Uani 1 d . . . H7 H 0.1475 0.5514 -0.0105 0.059 Uiso 1 calc R . . C8 C 0.0890(5) 0.9386(7) 0.2555(6) 0.071(2) Uani 1 d . . . H8A H 0.0582 0.8688 0.2842 0.107 Uiso 1 calc R . . H8B H 0.0611 1.0212 0.2601 0.107 Uiso 1 calc R . . H8C H 0.1378 0.9459 0.2897 0.107 Uiso 1 calc R . . C9 C 0.1346(5) 1.0554(7) 0.0619(6) 0.076(2) Uani 1 d . . . H9A H 0.1564 1.0353 -0.0012 0.113 Uiso 1 calc R . . H9B H 0.1726 1.1025 0.1004 0.113 Uiso 1 calc R . . H9C H 0.0888 1.1096 0.0539 0.113 Uiso 1 calc R . . C10 C 0.0139(4) 0.8396(7) 0.0709(7) 0.072(2) Uani 1 d . . . H10A H 0.0242 0.7687 0.0256 0.108 Uiso 1 calc R . . H10B H -0.0114 0.9115 0.0373 0.108 Uiso 1 calc R . . H10C H -0.0196 0.8077 0.1223 0.108 Uiso 1 calc R . . C11 C -0.0196(3) 0.3124(6) 0.1759(5) 0.0509(16) Uani 1 d . . . O11 O -0.0197(3) 0.2520(5) 0.2541(4) 0.0663(14) Uani 1 d . . . C12 C -0.0789(3) 0.2824(5) 0.0994(4) 0.0431(14) Uani 1 d . . . C13 C -0.1095(3) 0.1542(6) 0.0928(5) 0.0522(16) Uani 1 d . . . H13 H -0.0906 0.0870 0.1331 0.063 Uiso 1 calc R . . C14 C -0.1684(4) 0.1276(8) 0.0259(6) 0.069(2) Uani 1 d . . . H14 H -0.1880 0.0415 0.0206 0.083 Uiso 1 calc R . . C15 C -0.1983(5) 0.2259(7) -0.0327(6) 0.067(2) Uani 1 d . . . H15 H -0.2384 0.2072 -0.0766 0.081 Uiso 1 calc R . . C16 C -0.1683(4) 0.3526(7) -0.0260(5) 0.0608(18) Uani 1 d . . . H16 H -0.1886 0.4196 -0.0655 0.073 Uiso 1 calc R . . C17 C -0.1089(3) 0.3815(6) 0.0384(5) 0.0496(15) Uani 1 d . . . H17 H -0.0887 0.4672 0.0414 0.060 Uiso 1 calc R . . C22 C 0.2543(3) 0.7734(6) 0.1854(4) 0.0417(14) Uani 1 d . . . C23 C 0.2902(3) 0.6607(7) 0.2240(4) 0.0486(15) Uani 1 d . . . H23 H 0.2700 0.5771 0.2093 0.058 Uiso 1 calc R . . C24 C 0.3559(4) 0.6710(8) 0.2846(5) 0.0580(17) Uani 1 d . . . H24 H 0.3793 0.5945 0.3093 0.070 Uiso 1 calc R . . C25 C 0.3861(4) 0.7942(9) 0.3078(5) 0.065(2) Uani 1 d . . . H25 H 0.4300 0.8013 0.3478 0.078 Uiso 1 calc R . . C26 C 0.3506(4) 0.9062(8) 0.2714(5) 0.0654(19) Uani 1 d . . . H26 H 0.3703 0.9896 0.2875 0.078 Uiso 1 calc R . . C27 C 0.2852(3) 0.8964(6) 0.2102(5) 0.0516(16) Uani 1 d . . . H27 H 0.2622 0.9734 0.1858 0.062 Uiso 1 calc R . . C32 C 0.2253(3) 0.7694(5) 0.0063(5) 0.0400(13) Uani 1 d . . . C33 C 0.3060(4) 0.7575(6) -0.0097(5) 0.0463(15) Uani 1 d . . . H33 H 0.3393 0.7455 0.0435 0.056 Uiso 1 calc R . . C34 C 0.3370(4) 0.7633(7) -0.1028(5) 0.0580(18) Uani 1 d . . . H34 H 0.3908 0.7554 -0.1113 0.070 Uiso 1 calc R . . C35 C 0.2901(4) 0.7805(7) -0.1829(6) 0.0635(19) Uani 1 d . . . H35 H 0.3116 0.7843 -0.2454 0.076 Uiso 1 calc R . . C36 C 0.2113(4) 0.7919(7) -0.1698(5) 0.0614(19) Uani 1 d . . . H36 H 0.1788 0.8030 -0.2239 0.074 Uiso 1 calc R . . C37 C 0.1791(4) 0.7870(7) -0.0770(5) 0.0534(17) Uani 1 d . . . H37 H 0.1253 0.7957 -0.0699 0.064 Uiso 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 Si 0.0501(8) 0.0469(9) 0.0573(11) 0.0007(10) 0.0038(10) 0.0050(8) C1 0.039(3) 0.041(3) 0.038(3) 0.001(3) -0.003(3) -0.008(2) C2 0.038(3) 0.040(3) 0.041(3) -0.001(3) -0.001(3) 0.000(2) C3 0.045(3) 0.038(3) 0.044(3) -0.001(3) 0.001(3) -0.008(3) C4 0.047(3) 0.049(3) 0.041(3) 0.002(3) 0.004(3) 0.001(3) C5 0.042(3) 0.036(3) 0.043(3) 0.000(3) -0.002(3) -0.004(2) C6 0.059(4) 0.049(4) 0.040(3) -0.010(3) 0.003(3) -0.011(3) C7 0.056(4) 0.051(4) 0.041(3) -0.005(3) 0.005(3) -0.008(3) C8 0.078(5) 0.056(4) 0.080(6) -0.003(4) 0.019(4) 0.009(4) C9 0.088(5) 0.057(4) 0.081(5) 0.009(4) 0.011(5) 0.016(4) C10 0.060(4) 0.074(4) 0.082(6) -0.005(5) -0.002(4) 0.014(4) C11 0.045(3) 0.048(3) 0.060(4) 0.006(3) -0.001(3) -0.005(3) O11 0.064(3) 0.069(3) 0.066(3) 0.027(3) -0.014(3) -0.017(2) C12 0.048(3) 0.041(3) 0.041(3) -0.005(3) -0.001(3) -0.002(2) C13 0.062(4) 0.040(3) 0.055(4) 0.001(3) -0.004(3) -0.011(3) C14 0.078(5) 0.064(5) 0.065(5) -0.012(4) 0.001(4) -0.023(4) C15 0.072(5) 0.074(5) 0.055(4) -0.008(4) -0.013(4) -0.011(4) C16 0.057(4) 0.068(4) 0.057(4) 0.005(4) -0.004(4) 0.001(3) C17 0.057(3) 0.045(3) 0.047(4) 0.003(3) 0.000(3) -0.006(3) C22 0.037(3) 0.047(4) 0.041(3) 0.002(3) 0.002(3) -0.005(2) C23 0.048(3) 0.055(4) 0.044(3) 0.002(3) -0.007(3) -0.002(3) C24 0.050(3) 0.077(5) 0.048(4) 0.008(4) -0.005(3) -0.001(4) C25 0.047(4) 0.102(6) 0.046(4) -0.002(4) 0.000(3) -0.014(4) C26 0.061(4) 0.080(5) 0.055(4) -0.013(4) 0.006(4) -0.027(4) C27 0.052(3) 0.045(3) 0.058(4) -0.007(3) -0.003(3) -0.005(3) C32 0.044(3) 0.037(3) 0.039(3) 0.004(3) 0.003(3) -0.003(3) C33 0.041(3) 0.055(4) 0.043(4) 0.004(3) 0.003(3) 0.000(3) C34 0.055(4) 0.068(5) 0.051(4) 0.000(4) 0.010(3) -0.005(3) C35 0.077(5) 0.061(5) 0.053(4) -0.005(4) 0.014(4) -0.002(4) C36 0.074(5) 0.075(5) 0.035(3) 0.009(4) 0.000(3) -0.009(4) C37 0.049(4) 0.067(4) 0.043(4) 0.003(3) -0.003(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si C9 1.845(7) . ? Si C8 1.857(8) . ? Si C10 1.866(7) . ? Si C1 1.976(6) . ? C1 C2 1.529(7) . ? C1 C32 1.531(8) . ? C1 C22 1.537(8) . ? C2 C7 1.393(8) . ? C2 C3 1.410(9) . ? C3 C4 1.376(8) . ? C3 H3 0.9300 . ? C4 C5 1.393(8) . ? C4 H4 0.9300 . ? C5 C6 1.384(8) . ? C5 C11 1.487(8) . ? C6 C7 1.377(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O11 1.228(8) . ? C11 C12 1.486(9) . ? C12 C13 1.393(8) . ? C12 C17 1.396(8) . ? C13 C14 1.386(9) . ? C13 H13 0.9300 . ? C14 C15 1.370(10) . ? C14 H14 0.9300 . ? C15 C16 1.376(9) . ? C15 H15 0.9300 . ? C16 C17 1.374(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C22 C27 1.387(8) . ? C22 C23 1.392(8) . ? C23 C24 1.399(8) . ? C23 H23 0.9300 . ? C24 C25 1.379(10) . ? C24 H24 0.9300 . ? C25 C26 1.372(10) . ? C25 H25 0.9300 . ? C26 C27 1.399(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C32 C37 1.395(8) . ? C32 C33 1.402(8) . ? C33 C34 1.379(9) . ? C33 H33 0.9300 . ? C34 C35 1.367(10) . ? C34 H34 0.9300 . ? C35 C36 1.363(10) . ? C35 H35 0.9300 . ? C36 C37 1.383(9) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Si C8 108.0(4) . . ? C9 Si C10 107.7(4) . . ? C8 Si C10 107.3(4) . . ? C9 Si C1 112.0(3) . . ? C8 Si C1 112.2(3) . . ? C10 Si C1 109.4(3) . . ? C2 C1 C32 113.0(5) . . ? C2 C1 C22 110.9(5) . . ? C32 C1 C22 108.8(4) . . ? C2 C1 Si 101.8(3) . . ? C32 C1 Si 110.2(4) . . ? C22 C1 Si 112.1(4) . . ? C7 C2 C3 117.1(5) . . ? C7 C2 C1 124.0(6) . . ? C3 C2 C1 118.9(5) . . ? C4 C3 C2 121.4(5) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 120.4(6) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 118.4(5) . . ? C6 C5 C11 122.3(5) . . ? C4 C5 C11 119.4(5) . . ? C7 C6 C5 121.4(6) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C2 120.9(6) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? Si C8 H8A 109.5 . . ? Si C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si C9 H9A 109.5 . . ? Si C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si C10 H10A 109.5 . . ? Si C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O11 C11 C5 120.5(6) . . ? O11 C11 C12 120.6(5) . . ? C5 C11 C12 118.9(6) . . ? C13 C12 C17 118.9(5) . . ? C13 C12 C11 119.3(5) . . ? C17 C12 C11 121.6(5) . . ? C12 C13 C14 119.6(6) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 121.0(7) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 119.4(7) . . ? C16 C15 H15 120.3 . . ? C14 C15 H15 120.3 . . ? C15 C16 C17 120.8(7) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 120.2(6) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C27 C22 C23 117.8(5) . . ? C27 C22 C1 121.1(5) . . ? C23 C22 C1 120.7(5) . . ? C22 C23 C24 121.2(6) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C23 120.2(7) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 119.3(6) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C25 C26 C27 120.8(7) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C22 C27 C26 120.8(6) . . ? C22 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C37 C32 C33 116.1(6) . . ? C37 C32 C1 121.5(5) . . ? C33 C32 C1 122.4(5) . . ? C34 C33 C32 121.2(6) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C35 C34 C33 121.2(6) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 119.1(7) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C37 C36 C35 120.6(7) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C32 121.9(6) . . ? C36 C37 H37 119.1 . . ? C32 C37 H37 119.1 . . ? 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 C9 Si C1 C2 -156.4(4) . . . . ? C8 Si C1 C2 81.9(5) . . . . ? C10 Si C1 C2 -37.1(5) . . . . ? C9 Si C1 C32 -36.3(5) . . . . ? C8 Si C1 C32 -158.0(4) . . . . ? C10 Si C1 C32 83.1(4) . . . . ? C9 Si C1 C22 85.0(5) . . . . ? C8 Si C1 C22 -36.6(5) . . . . ? C10 Si C1 C22 -155.6(4) . . . . ? C32 C1 C2 C7 -8.7(7) . . . . ? C22 C1 C2 C7 -131.2(6) . . . . ? Si C1 C2 C7 109.5(5) . . . . ? C32 C1 C2 C3 173.4(5) . . . . ? C22 C1 C2 C3 51.0(6) . . . . ? Si C1 C2 C3 -68.4(5) . . . . ? C7 C2 C3 C4 -6.0(8) . . . . ? C1 C2 C3 C4 172.0(5) . . . . ? C2 C3 C4 C5 0.1(9) . . . . ? C3 C4 C5 C6 3.9(9) . . . . ? C3 C4 C5 C11 -176.9(5) . . . . ? C4 C5 C6 C7 -2.0(9) . . . . ? C11 C5 C6 C7 178.9(6) . . . . ? C5 C6 C7 C2 -4.1(10) . . . . ? C3 C2 C7 C6 8.0(9) . . . . ? C1 C2 C7 C6 -169.9(5) . . . . ? C6 C5 C11 O11 143.9(7) . . . . ? C4 C5 C11 O11 -35.2(9) . . . . ? C6 C5 C11 C12 -38.1(8) . . . . ? C4 C5 C11 C12 142.8(6) . . . . ? O11 C11 C12 C13 -29.8(9) . . . . ? C5 C11 C12 C13 152.2(6) . . . . ? O11 C11 C12 C17 145.4(6) . . . . ? C5 C11 C12 C17 -32.5(9) . . . . ? C17 C12 C13 C14 0.5(9) . . . . ? C11 C12 C13 C14 175.9(6) . . . . ? C12 C13 C14 C15 -1.4(10) . . . . ? C13 C14 C15 C16 1.1(12) . . . . ? C14 C15 C16 C17 0.1(12) . . . . ? C15 C16 C17 C12 -1.1(10) . . . . ? C13 C12 C17 C16 0.7(9) . . . . ? C11 C12 C17 C16 -174.6(6) . . . . ? C2 C1 C22 C27 -155.8(5) . . . . ? C32 C1 C22 C27 79.4(7) . . . . ? Si C1 C22 C27 -42.7(7) . . . . ? C2 C1 C22 C23 31.4(7) . . . . ? C32 C1 C22 C23 -93.4(6) . . . . ? Si C1 C22 C23 144.4(5) . . . . ? C27 C22 C23 C24 -1.0(9) . . . . ? C1 C22 C23 C24 172.1(6) . . . . ? C22 C23 C24 C25 0.5(10) . . . . ? C23 C24 C25 C26 0.4(10) . . . . ? C24 C25 C26 C27 -0.9(10) . . . . ? C23 C22 C27 C26 0.5(9) . . . . ? C1 C22 C27 C26 -172.5(6) . . . . ? C25 C26 C27 C22 0.4(10) . . . . ? C2 C1 C32 C37 69.1(7) . . . . ? C22 C1 C32 C37 -167.3(5) . . . . ? Si C1 C32 C37 -44.1(6) . . . . ? C2 C1 C32 C33 -109.6(6) . . . . ? C22 C1 C32 C33 14.0(7) . . . . ? Si C1 C32 C33 137.3(5) . . . . ? C37 C32 C33 C34 0.1(9) . . . . ? C1 C32 C33 C34 178.8(6) . . . . ? C32 C33 C34 C35 -0.2(10) . . . . ? C33 C34 C35 C36 0.0(11) . . . . ? C34 C35 C36 C37 0.4(11) . . . . ? C35 C36 C37 C32 -0.5(11) . . . . ? C33 C32 C37 C36 0.3(10) . . . . ? C1 C32 C37 C36 -178.5(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.226 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.049