# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 207/373 #============================================================ data_I #============================================================ # 5. CHEMICAL DATA _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C29 H35 O3 P Si' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H35 O3 P Si' _chemical_formula_weight 490.63 _chemical_melting_point ? _chemical_compound_source 'See manuscript' 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' 'N' 'N' 0.0061 0.0033 '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' #============================================================ # 6.CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21/b 21/c 21/a' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.761(2) _cell_length_b 19.813(3) _cell_length_c 23.024(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5365.1(14) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20 _cell_measurement_theta_max 30 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.215 _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 0.175 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================ # 7. EXPERIMENTAL DATA _exptl_special_details ; ****************ADD for H's ; _diffrn_ambient_temperature 295(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4705 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1466 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4705 _reflns_number_observed 2219 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf Nonius)' _computing_cell_refinement 'CAD4, SETANG (Enraf Nonius)' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' #============================================================ # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _refine_ls_R_factor_obs 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^)+(0.0648P)^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 refU _refine_ls_extinction_method none _refine_ls_number_reflns 4609 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1928 _refine_ls_R_factor_obs 0.0558 _refine_ls_wR_factor_all 0.1692 _refine_ls_wR_factor_obs 0.1123 _refine_ls_goodness_of_fit_all 0.967 _refine_ls_goodness_of_fit_obs 1.084 _refine_ls_restrained_S_all 1.083 _refine_ls_restrained_S_obs 1.084 _refine_ls_shift/esd_max -0.005 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.286 _refine_diff_density_min -0.327 #============================================================ # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1 P 0.10829(9) 0.40957(5) 0.23249(5) 0.0347(3) Uani 1 d . . Si1 Si 0.07333(11) 0.30734(6) 0.07000(6) 0.0468(4) Uani 1 d . . O1 O 0.1607(2) 0.44237(13) 0.07978(12) 0.0445(8) Uani 1 d . . O2 O -0.0113(2) 0.41544(14) 0.21265(12) 0.0453(8) Uani 1 d . . O3 O 0.1521(2) 0.33800(13) 0.12386(11) 0.0415(7) Uani 1 d . . C1 C 0.2143(3) 0.3983(2) 0.1201(2) 0.0377(10) Uani 1 d . . C2 C 0.2153(3) 0.4362(2) 0.1802(2) 0.0328(10) Uani 1 d . . H2 H 0.2906(3) 0.4308(2) 0.1979(2) 0.037(11) Uiso 1 calc R . C3 C 0.2036(4) 0.5098(2) 0.1586(2) 0.0388(11) Uani 1 d . . H3 H 0.2771(4) 0.5218(2) 0.1414(2) 0.048(13) Uiso 1 calc R . C4 C 0.1215(4) 0.5020(2) 0.1085(2) 0.0441(11) Uani 1 d . . H4 H 0.0446(4) 0.4945(2) 0.1236(2) 0.047(13) Uiso 1 calc R . C5 C 0.1217(5) 0.5623(2) 0.0694(2) 0.0621(15) Uani 1 d . . H51 H 0.0662(5) 0.5564(2) 0.0387(2) 0.079(12) Uiso 1 calc R . H52 H 0.1960(5) 0.5678(2) 0.0518(2) 0.079(12) Uiso 1 calc R . C6 C 0.0921(5) 0.6251(2) 0.1056(2) 0.074(2) Uani 1 d . . H61 H 0.0991(5) 0.6650(2) 0.0814(2) 0.074(11) Uiso 1 calc R . H62 H 0.0137(5) 0.6219(2) 0.1184(2) 0.074(11) Uiso 1 calc R . C7 C 0.1685(5) 0.6324(2) 0.1580(2) 0.066(2) Uani 1 d . . H71 H 0.1436(5) 0.6708(2) 0.1808(2) 0.063(10) Uiso 1 calc R . H72 H 0.2456(5) 0.6413(2) 0.1450(2) 0.063(10) Uiso 1 calc R . C8 C 0.1683(4) 0.5694(2) 0.1962(2) 0.0530(13) Uani 1 d . . H81 H 0.0930(4) 0.5619(2) 0.2121(2) 0.041(8) Uiso 1 calc R . H82 H 0.2212(4) 0.5750(2) 0.2282(2) 0.041(8) Uiso 1 calc R . C9 C 0.1342(3) 0.4625(2) 0.2955(2) 0.0339(10) Uani 1 d . . C10 C 0.0416(4) 0.4977(2) 0.3175(2) 0.0465(12) Uani 1 d . . H10 H -0.0301(4) 0.4911(2) 0.3014(2) 0.053(6) Uiso 1 calc R . C11 C 0.0549(5) 0.5423(2) 0.3629(2) 0.0587(14) Uani 1 d . . H11 H -0.0073(5) 0.5662(2) 0.3770(2) 0.053(6) Uiso 1 calc R . C12 C 0.1606(5) 0.5514(3) 0.3874(2) 0.0644(15) Uani 1 d . . H12 H 0.1698(5) 0.5815(3) 0.4180(2) 0.053(6) Uiso 1 calc R . C13 C 0.2515(5) 0.5165(2) 0.3669(2) 0.0541(13) Uani 1 d . . H13 H 0.3223(5) 0.5221(2) 0.3841(2) 0.053(6) Uiso 1 calc R . C14 C 0.2397(4) 0.4726(2) 0.3205(2) 0.0454(11) Uani 1 d . . H14 H 0.3029(4) 0.4499(2) 0.3061(2) 0.053(6) Uiso 1 calc R . C15 C 0.1433(3) 0.3241(2) 0.2541(2) 0.0346(10) Uani 1 d . . C16 C 0.0614(4) 0.2749(2) 0.2431(2) 0.0489(12) Uani 1 d . . H16 H -0.0055(4) 0.2862(2) 0.2239(2) 0.078(7) Uiso 1 calc R . C17 C 0.0798(4) 0.2091(2) 0.2608(2) 0.0594(14) Uani 1 d . . H17 H 0.0260(4) 0.1761(2) 0.2525(2) 0.078(7) Uiso 1 calc R . C18 C 0.1764(5) 0.1921(2) 0.2903(2) 0.0627(14) Uani 1 d . . H18 H 0.1871(5) 0.1480(2) 0.3030(2) 0.078(7) Uiso 1 calc R . C19 C 0.2574(4) 0.2400(2) 0.3012(2) 0.0624(14) Uani 1 d . . H19 H 0.3233(4) 0.2285(2) 0.3212(2) 0.078(7) Uiso 1 calc R . C20 C 0.2412(4) 0.3057(2) 0.2826(2) 0.0515(12) Uani 1 d . . H20 H 0.2974(4) 0.3378(2) 0.2894(2) 0.078(7) Uiso 1 calc R . C21 C 0.3347(4) 0.3833(2) 0.0999(2) 0.0367(10) Uani 1 d . . C22 C 0.3960(4) 0.3313(2) 0.1245(2) 0.0476(12) Uani 1 d . . H22 H 0.3619(4) 0.3045(2) 0.1527(2) 0.057(6) Uiso 1 calc R . C23 C 0.5058(5) 0.3182(3) 0.1085(2) 0.0588(13) Uani 1 d . . H23 H 0.5455(5) 0.2829(3) 0.1257(2) 0.057(6) Uiso 1 calc R . C24 C 0.5575(4) 0.3574(3) 0.0668(2) 0.0628(14) Uani 1 d . . H24 H 0.6326(4) 0.3493(3) 0.0562(2) 0.057(6) Uiso 1 calc R . C25 C 0.4975(5) 0.4085(3) 0.0411(2) 0.0628(14) Uani 1 d . . H25 H 0.5316(5) 0.4345(3) 0.0124(2) 0.057(6) Uiso 1 calc R . C26 C 0.3867(4) 0.4219(2) 0.0575(2) 0.0505(12) Uani 1 d . . H26 H 0.3469(4) 0.4569(2) 0.0399(2) 0.057(6) Uiso 1 calc R . C27 C 0.0578(5) 0.2163(2) 0.0877(2) 0.075(2) Uani 1 d . . H271 H 0.1312(5) 0.1951(2) 0.0875(2) 0.113(12) Uiso 1 calc R . H272 H 0.0099(5) 0.1950(2) 0.0592(2) 0.113(12) Uiso 1 calc R . H273 H 0.0241(5) 0.2115(2) 0.1254(2) 0.113(12) Uiso 1 calc R . C28 C 0.1452(4) 0.3164(3) -0.0011(2) 0.0659(15) Uani 1 d . . H281 H 0.2183(4) 0.2948(3) 0.0004(2) 0.118(13) Uiso 1 calc R . H282 H 0.1550(4) 0.3634(3) -0.0098(2) 0.118(13) Uiso 1 calc R . H283 H 0.0998(4) 0.2957(3) -0.0308(2) 0.118(13) Uiso 1 calc R . C29 C -0.0686(4) 0.3477(3) 0.0704(2) 0.069(2) Uani 1 d . . H291 H -0.1031(4) 0.3418(3) 0.1078(2) 0.131(14) Uiso 1 calc R . H292 H -0.1156(4) 0.3271(3) 0.0412(2) 0.131(14) Uiso 1 calc R . H293 H -0.0606(4) 0.3950(3) 0.0622(2) 0.131(14) 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 P1 0.0285(6) 0.0357(6) 0.0399(6) 0.0002(5) -0.0006(5) 0.0023(5) Si1 0.0515(8) 0.0485(7) 0.0403(7) -0.0029(6) -0.0083(7) -0.0075(7) O1 0.054(2) 0.042(2) 0.038(2) 0.0010(14) -0.010(2) 0.0106(15) O2 0.030(2) 0.049(2) 0.057(2) -0.001(2) -0.0073(14) 0.0048(14) O3 0.046(2) 0.040(2) 0.038(2) -0.0004(14) -0.0056(14) -0.0086(15) C1 0.040(3) 0.041(3) 0.032(2) 0.003(2) 0.000(2) 0.002(2) C2 0.029(2) 0.036(2) 0.033(2) -0.002(2) -0.003(2) 0.001(2) C3 0.040(3) 0.032(2) 0.044(3) 0.002(2) 0.007(2) -0.005(2) C4 0.045(3) 0.043(3) 0.045(3) 0.005(2) -0.003(2) 0.007(2) C5 0.086(4) 0.048(3) 0.052(3) 0.018(3) -0.007(3) 0.016(3) C6 0.096(5) 0.046(3) 0.080(4) 0.019(3) 0.004(4) 0.013(3) C7 0.091(4) 0.038(3) 0.070(4) 0.009(3) 0.013(4) 0.001(3) C8 0.066(3) 0.042(3) 0.051(3) 0.003(2) 0.003(3) -0.006(2) C9 0.033(3) 0.033(2) 0.036(2) 0.001(2) 0.006(2) 0.001(2) C10 0.035(3) 0.047(3) 0.058(3) -0.006(2) 0.006(2) 0.002(2) C11 0.055(3) 0.053(3) 0.069(4) -0.019(3) 0.023(3) 0.005(3) C12 0.072(4) 0.059(3) 0.062(3) -0.021(3) 0.008(3) -0.009(3) C13 0.051(3) 0.059(3) 0.052(3) -0.013(3) -0.011(3) -0.008(3) C14 0.041(3) 0.046(3) 0.049(3) -0.004(2) 0.001(2) 0.006(2) C15 0.035(2) 0.036(2) 0.033(2) 0.004(2) 0.006(2) 0.002(2) C16 0.046(3) 0.048(3) 0.053(3) 0.001(2) 0.000(2) -0.007(2) C17 0.066(4) 0.041(3) 0.071(4) -0.004(3) 0.011(3) -0.013(3) C18 0.071(4) 0.042(3) 0.076(4) 0.010(3) 0.029(3) 0.008(3) C19 0.049(3) 0.056(3) 0.082(4) 0.015(3) 0.004(3) 0.013(3) C20 0.040(3) 0.046(3) 0.069(3) 0.009(2) -0.002(3) 0.003(2) C21 0.042(3) 0.036(2) 0.032(2) -0.008(2) 0.004(2) -0.005(2) C22 0.054(3) 0.046(3) 0.042(3) 0.000(2) 0.001(3) 0.008(3) C23 0.060(4) 0.063(3) 0.054(3) -0.007(3) -0.005(3) 0.019(3) C24 0.044(3) 0.076(4) 0.068(4) -0.026(3) 0.012(3) 0.006(3) C25 0.069(4) 0.061(3) 0.059(3) -0.005(3) 0.027(3) -0.001(3) C26 0.059(3) 0.042(3) 0.050(3) -0.002(2) 0.009(3) 0.004(3) C27 0.100(5) 0.054(3) 0.072(4) -0.008(3) -0.017(3) -0.019(3) C28 0.080(4) 0.073(3) 0.045(3) -0.015(3) 0.000(3) -0.012(3) C29 0.053(3) 0.087(4) 0.068(4) 0.006(3) -0.014(3) 0.000(3) #============================================================ # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O2 1.484(3) . ? P1 C15 1.812(4) . ? P1 C9 1.815(4) . ? P1 C2 1.819(4) . ? Si1 O3 1.663(3) . ? Si1 C29 1.850(5) . ? Si1 C28 1.852(5) . ? Si1 C27 1.859(5) . ? O1 C1 1.421(4) . ? O1 C4 1.431(5) . ? O3 C1 1.403(4) . ? C1 C21 1.521(5) . ? C1 C2 1.576(5) . ? C2 C3 1.546(5) . ? C2 H2 0.98 . ? C3 C4 1.511(6) . ? C3 C8 1.523(5) . ? C3 H3 0.98 . ? C4 C5 1.496(6) . ? C4 H4 0.98 . ? C5 C6 1.536(6) . ? C5 H51 0.97 . ? C5 H52 0.97 . ? C6 C7 1.511(7) . ? C6 H61 0.97 . ? C6 H62 0.97 . ? C7 C8 1.526(6) . ? C7 H71 0.97 . ? C7 H72 0.97 . ? C8 H81 0.97 . ? C8 H82 0.97 . ? C9 C14 1.383(5) . ? C9 C10 1.388(5) . ? C10 C11 1.379(6) . ? C10 H10 0.93 . ? C11 C12 1.376(7) . ? C11 H11 0.93 . ? C12 C13 1.358(6) . ? C12 H12 0.93 . ? C13 C14 1.383(6) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 C20 1.374(5) . ? C15 C16 1.394(5) . ? C16 C17 1.382(6) . ? C16 H16 0.93 . ? C17 C18 1.366(7) . ? C17 H17 0.93 . ? C18 C19 1.369(6) . ? C18 H18 0.93 . ? C19 C20 1.383(6) . ? C19 H19 0.93 . ? C20 H20 0.93 . ? C21 C22 1.379(6) . ? C21 C26 1.381(5) . ? C22 C23 1.368(6) . ? C22 H22 0.93 . ? C23 C24 1.377(7) . ? C23 H23 0.93 . ? C24 C25 1.368(7) . ? C24 H24 0.93 . ? C25 C26 1.383(6) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C27 H271 0.96 . ? C27 H272 0.96 . ? C27 H273 0.96 . ? C28 H281 0.96 . ? C28 H282 0.96 . ? C28 H283 0.96 . ? C29 H291 0.96 . ? C29 H292 0.96 . ? C29 H293 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 P1 C15 111.9(2) . . ? O2 P1 C9 111.1(2) . . ? C15 P1 C9 106.4(2) . . ? O2 P1 C2 115.4(2) . . ? C15 P1 C2 107.2(2) . . ? C9 P1 C2 104.1(2) . . ? O3 Si1 C29 110.0(2) . . ? O3 Si1 C28 111.7(2) . . ? C29 Si1 C28 112.0(2) . . ? O3 Si1 C27 104.3(2) . . ? C29 Si1 C27 109.2(3) . . ? C28 Si1 C27 109.4(2) . . ? C1 O1 C4 110.4(3) . . ? C1 O3 Si1 123.7(2) . . ? O3 C1 O1 109.4(3) . . ? O3 C1 C21 109.7(3) . . ? O1 C1 C21 109.5(3) . . ? O3 C1 C2 110.8(3) . . ? O1 C1 C2 106.5(3) . . ? C21 C1 C2 110.8(3) . . ? C3 C2 C1 99.5(3) . . ? C3 C2 P1 115.2(3) . . ? C1 C2 P1 115.9(3) . . ? C3 C2 H2 108.6(2) . . ? C1 C2 H2 108.6(2) . . ? P1 C2 H2 108.57(13) . . ? C4 C3 C8 109.7(4) . . ? C4 C3 C2 102.0(3) . . ? C8 C3 C2 124.9(4) . . ? C4 C3 H3 106.3(2) . . ? C8 C3 H3 106.3(2) . . ? C2 C3 H3 106.3(2) . . ? O1 C4 C5 112.4(4) . . ? O1 C4 C3 103.3(3) . . ? C5 C4 C3 112.1(4) . . ? O1 C4 H4 109.6(2) . . ? C5 C4 H4 109.6(3) . . ? C3 C4 H4 109.6(2) . . ? C4 C5 C6 108.6(4) . . ? C4 C5 H51 110.0(3) . . ? C6 C5 H51 110.0(3) . . ? C4 C5 H52 110.0(3) . . ? C6 C5 H52 110.0(3) . . ? H51 C5 H52 108.3 . . ? C7 C6 C5 112.1(4) . . ? C7 C6 H61 109.2(3) . . ? C5 C6 H61 109.2(2) . . ? C7 C6 H62 109.2(3) . . ? C5 C6 H62 109.2(3) . . ? H61 C6 H62 107.9 . . ? C6 C7 C8 112.3(4) . . ? C6 C7 H71 109.1(3) . . ? C8 C7 H71 109.1(3) . . ? C6 C7 H72 109.1(3) . . ? C8 C7 H72 109.1(3) . . ? H71 C7 H72 107.9 . . ? C7 C8 C3 107.8(4) . . ? C7 C8 H81 110.1(3) . . ? C3 C8 H81 110.1(2) . . ? C7 C8 H82 110.1(3) . . ? C3 C8 H82 110.1(2) . . ? H81 C8 H82 108.4 . . ? C14 C9 C10 118.6(4) . . ? C14 C9 P1 124.6(3) . . ? C10 C9 P1 116.8(3) . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10 119.7(3) . . ? C9 C10 H10 119.7(3) . . ? C12 C11 C10 119.8(5) . . ? C12 C11 H11 120.1(3) . . ? C10 C11 H11 120.1(3) . . ? C13 C12 C11 120.2(5) . . ? C13 C12 H12 119.9(3) . . ? C11 C12 H12 119.9(3) . . ? C12 C13 C14 120.6(5) . . ? C12 C13 H13 119.7(3) . . ? C14 C13 H13 119.7(3) . . ? C9 C14 C13 120.2(4) . . ? C9 C14 H14 119.9(2) . . ? C13 C14 H14 119.9(3) . . ? C20 C15 C16 118.7(4) . . ? C20 C15 P1 124.7(3) . . ? C16 C15 P1 116.6(3) . . ? C17 C16 C15 119.8(4) . . ? C17 C16 H16 120.1(3) . . ? C15 C16 H16 120.1(2) . . ? C18 C17 C16 120.6(4) . . ? C18 C17 H17 119.7(3) . . ? C16 C17 H17 119.7(3) . . ? C17 C18 C19 119.9(4) . . ? C17 C18 H18 120.0(3) . . ? C19 C18 H18 120.0(3) . . ? C18 C19 C20 120.0(5) . . ? C18 C19 H19 120.0(3) . . ? C20 C19 H19 120.0(3) . . ? C15 C20 C19 120.9(4) . . ? C15 C20 H20 119.6(2) . . ? C19 C20 H20 119.6(3) . . ? C22 C21 C26 118.2(4) . . ? C22 C21 C1 120.5(4) . . ? C26 C21 C1 121.3(4) . . ? C23 C22 C21 121.6(4) . . ? C23 C22 H22 119.2(3) . . ? C21 C22 H22 119.2(3) . . ? C22 C23 C24 119.9(5) . . ? C22 C23 H23 120.1(3) . . ? C24 C23 H23 120.1(3) . . ? C25 C24 C23 119.4(5) . . ? C25 C24 H24 120.3(3) . . ? C23 C24 H24 120.3(3) . . ? C24 C25 C26 120.7(5) . . ? C24 C25 H25 119.6(3) . . ? C26 C25 H25 119.6(3) . . ? C25 C26 C21 120.2(5) . . ? C25 C26 H26 119.9(3) . . ? C21 C26 H26 119.9(3) . . ? Si1 C27 H271 109.5(2) . . ? Si1 C27 H272 109.5(2) . . ? H271 C27 H272 109.5 . . ? Si1 C27 H273 109.5(2) . . ? H271 C27 H273 109.5 . . ? H272 C27 H273 109.5 . . ? Si1 C28 H281 109.5(2) . . ? Si1 C28 H282 109.5(2) . . ? H281 C28 H282 109.5 . . ? Si1 C28 H283 109.5(2) . . ? H281 C28 H283 109.5 . . ? H282 C28 H283 109.5 . . ? Si1 C29 H291 109.5(2) . . ? Si1 C29 H292 109.5(2) . . ? H291 C29 H292 109.5 . . ? Si1 C29 H293 109.5(2) . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 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 C29 Si1 O3 C1 -83.6(3) . . . . ? C28 Si1 O3 C1 41.3(4) . . . . ? C27 Si1 O3 C1 159.4(3) . . . . ? Si1 O3 C1 O1 27.8(4) . . . . ? Si1 O3 C1 C21 -92.3(3) . . . . ? Si1 O3 C1 C2 145.0(3) . . . . ? C4 O1 C1 O3 116.2(3) . . . . ? C4 O1 C1 C21 -123.5(3) . . . . ? C4 O1 C1 C2 -3.6(4) . . . . ? O3 C1 C2 C3 -141.1(3) . . . . ? O1 C1 C2 C3 -22.1(4) . . . . ? C21 C1 C2 C3 96.8(4) . . . . ? O3 C1 C2 P1 -16.9(4) . . . . ? O1 C1 C2 P1 102.0(3) . . . . ? C21 C1 C2 P1 -139.0(3) . . . . ? O2 P1 C2 C3 57.4(3) . . . . ? C15 P1 C2 C3 -177.2(3) . . . . ? C9 P1 C2 C3 -64.6(3) . . . . ? O2 P1 C2 C1 -58.2(3) . . . . ? C15 P1 C2 C1 67.3(3) . . . . ? C9 P1 C2 C1 179.8(3) . . . . ? C1 C2 C3 C4 38.3(4) . . . . ? P1 C2 C3 C4 -86.4(3) . . . . ? C1 C2 C3 C8 162.9(4) . . . . ? P1 C2 C3 C8 38.3(5) . . . . ? C1 O1 C4 C5 149.9(4) . . . . ? C1 O1 C4 C3 28.9(4) . . . . ? C8 C3 C4 O1 -176.4(3) . . . . ? C2 C3 C4 O1 -42.2(4) . . . . ? C8 C3 C4 C5 62.3(5) . . . . ? C2 C3 C4 C5 -163.4(4) . . . . ? O1 C4 C5 C6 -173.4(4) . . . . ? C3 C4 C5 C6 -57.6(5) . . . . ? C4 C5 C6 C7 53.5(6) . . . . ? C5 C6 C7 C8 -55.1(6) . . . . ? C6 C7 C8 C3 56.8(6) . . . . ? C4 C3 C8 C7 -59.2(5) . . . . ? C2 C3 C8 C7 179.5(4) . . . . ? O2 P1 C9 C14 -173.7(3) . . . . ? C15 P1 C9 C14 64.3(4) . . . . ? C2 P1 C9 C14 -48.8(4) . . . . ? O2 P1 C9 C10 2.7(4) . . . . ? C15 P1 C9 C10 -119.4(3) . . . . ? C2 P1 C9 C10 127.5(3) . . . . ? C14 C9 C10 C11 0.7(6) . . . . ? P1 C9 C10 C11 -175.9(3) . . . . ? C9 C10 C11 C12 -1.0(7) . . . . ? C10 C11 C12 C13 0.0(8) . . . . ? C11 C12 C13 C14 1.4(7) . . . . ? C10 C9 C14 C13 0.7(6) . . . . ? P1 C9 C14 C13 177.0(3) . . . . ? C12 C13 C14 C9 -1.8(7) . . . . ? O2 P1 C15 C20 -169.4(3) . . . . ? C9 P1 C15 C20 -47.9(4) . . . . ? C2 P1 C15 C20 63.0(4) . . . . ? O2 P1 C15 C16 7.4(4) . . . . ? C9 P1 C15 C16 128.9(3) . . . . ? C2 P1 C15 C16 -120.1(3) . . . . ? C20 C15 C16 C17 0.0(6) . . . . ? P1 C15 C16 C17 -177.1(4) . . . . ? C15 C16 C17 C18 1.7(7) . . . . ? C16 C17 C18 C19 -1.8(7) . . . . ? C17 C18 C19 C20 0.2(7) . . . . ? C16 C15 C20 C19 -1.6(6) . . . . ? P1 C15 C20 C19 175.3(4) . . . . ? C18 C19 C20 C15 1.5(7) . . . . ? O3 C1 C21 C22 -46.4(5) . . . . ? O1 C1 C21 C22 -166.4(4) . . . . ? C2 C1 C21 C22 76.4(5) . . . . ? O3 C1 C21 C26 135.1(4) . . . . ? O1 C1 C21 C26 15.0(5) . . . . ? C2 C1 C21 C26 -102.2(4) . . . . ? C26 C21 C22 C23 0.9(6) . . . . ? C1 C21 C22 C23 -177.8(4) . . . . ? C21 C22 C23 C24 0.0(7) . . . . ? C22 C23 C24 C25 -1.1(7) . . . . ? C23 C24 C25 C26 1.3(7) . . . . ? C24 C25 C26 C21 -0.4(7) . . . . ? C22 C21 C26 C25 -0.6(6) . . . . ? C1 C21 C26 C25 178.0(4) . . . . ? #============================================================ #2......... #===================================================================== data_II #============================================================ # 5. CHEMICAL DATA _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C27 H33 O3 P Si' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H33 O3 P Si' _chemical_formula_weight 464.59 _chemical_melting_point ? _chemical_compound_source 'See manuscript' 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' 'N' 'N' 0.0061 0.0033 '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' #============================================================ # 6.CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall ? 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 18.753(4) _cell_length_b 8.349(2) _cell_length_c 18.019(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.75(3) _cell_angle_gamma 90.00 _cell_volume 2620.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20 _cell_measurement_theta_max 30 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.178 _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.175 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #============================================================ # 7. EXPERIMENTAL DATA _exptl_special_details ;? ; _diffrn_ambient_temperature 295(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 'Nonius CAD4' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 4747 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4599 _reflns_number_observed 2948 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf Nonius)' _computing_cell_refinement 'CAD4, SETANG (Enraf Nonius)' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' #============================================================ # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _refine_ls_R_factor_obs 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^)+(0.0693P)^2^+0.1143P] 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 refU _refine_ls_extinction_method none _refine_ls_number_reflns 4542 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_obs 0.0449 _refine_ls_wR_factor_all 0.1305 _refine_ls_wR_factor_obs 0.1102 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.133 _refine_ls_restrained_S_all 1.055 _refine_ls_restrained_S_obs 1.133 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.192 _refine_diff_density_min -0.233 #============================================================ # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1 P 0.18924(4) 0.15942(8) 0.44978(4) 0.0458(2) Uani 1 d . . Si1 Si 0.31241(5) 0.52212(9) 0.62403(5) 0.0560(2) Uani 1 d . . O1 O 0.39430(9) 0.2460(2) 0.59299(9) 0.0492(4) Uani 1 d . . O2 O 0.18747(11) 0.3080(2) 0.40478(10) 0.0625(5) Uani 1 d . . O3 O 0.27713(9) 0.3456(2) 0.58538(9) 0.0490(4) Uani 1 d . . C1 C 0.32091(13) 0.2053(3) 0.59356(14) 0.0439(6) Uani 1 d . . C2 C 0.28334(13) 0.0930(3) 0.51931(13) 0.0416(5) Uani 1 d . . H2 H 0.27647(13) -0.0126(3) 0.53946(13) 0.053(7) Uiso 1 calc R . C3 C 0.34718(14) 0.0769(3) 0.48413(15) 0.0503(6) Uani 1 d . . H3 H 0.38116(14) -0.0102(3) 0.51296(15) 0.059(7) Uiso 1 calc R . C4 C 0.39064(15) 0.2321(3) 0.5118(2) 0.0517(6) Uani 1 d . . H4 H 0.36095(15) 0.3214(3) 0.4798(2) 0.046(6) Uiso 1 calc R . C5 C 0.4716(2) 0.2372(4) 0.5134(2) 0.0773(9) Uani 1 d . . H51 H 0.4937(2) 0.3404(4) 0.5317(2) 0.088(6) Uiso 1 calc R . H52 H 0.4709(2) 0.2185(4) 0.4606(2) 0.088(6) Uiso 1 calc R . H53 H 0.5018(2) 0.1558(4) 0.5488(2) 0.088(6) Uiso 1 calc R . C8 C 0.3251(2) 0.0446(4) 0.3957(2) 0.0745(9) Uani 1 d . . H81 H 0.2978(2) -0.0552(4) 0.3822(2) 0.071(5) Uiso 1 calc R . H82 H 0.3706(2) 0.0388(4) 0.3833(2) 0.071(5) Uiso 1 calc R . H83 H 0.2928(2) 0.1296(4) 0.3655(2) 0.071(5) Uiso 1 calc R . C9 C 0.15221(14) -0.0100(3) 0.38348(15) 0.0502(6) Uani 1 d . . C10 C 0.1052(2) 0.0222(4) 0.3052(2) 0.0777(9) Uani 1 d . . H10 H 0.0943(2) 0.1276(4) 0.2882(2) 0.103(5) Uiso 1 calc R . C11 C 0.07435(13) -0.1016(3) 0.25259(13) 0.1082(13) Uani 1 d . . H11 H 0.04219(13) -0.0790(3) 0.20033(13) 0.103(5) Uiso 1 calc R . C12 C 0.09059(13) -0.2581(3) 0.27641(13) 0.0963(12) Uani 1 d R . H12 H 0.06951(13) -0.3405(3) 0.24018(13) 0.103(5) Uiso 1 calc R . C13 C 0.13720(13) -0.2930(3) 0.35248(13) 0.0789(9) Uani 1 d R . H13 H 0.14870(13) -0.3989(3) 0.36841(13) 0.103(5) Uiso 1 calc R . C14 C 0.1673(2) -0.1701(3) 0.4058(2) 0.0615(7) Uani 1 d . . H14 H 0.1985(2) -0.1944(3) 0.4582(2) 0.103(5) Uiso 1 calc R . C15 C 0.12875(14) 0.1654(3) 0.50796(15) 0.0522(6) Uani 1 d . . C16 C 0.0944(2) 0.3091(4) 0.5136(2) 0.0803(9) Uani 1 d . . H16 H 0.1010(2) 0.3993(4) 0.4866(2) 0.115(6) Uiso 1 calc R . C17 C 0.0499(2) 0.3169(6) 0.5602(3) 0.1102(14) Uani 1 d . . H17 H 0.0271(2) 0.4135(6) 0.5648(3) 0.115(6) Uiso 1 calc R . C18 C 0.0389(2) 0.1851(7) 0.5996(2) 0.1076(15) Uani 1 d . . H18 H 0.0091(2) 0.1921(7) 0.6308(2) 0.115(6) Uiso 1 calc R . C19 C 0.0716(2) 0.0441(6) 0.5927(2) 0.0944(11) Uani 1 d . . H19 H 0.0639(2) -0.0462(6) 0.6191(2) 0.115(6) Uiso 1 calc R . C20 C 0.1162(2) 0.0335(4) 0.5469(2) 0.0719(8) Uani 1 d . . H20 H 0.1380(2) -0.0642(4) 0.5423(2) 0.115(6) Uiso 1 calc R . C21 C 0.33188(14) 0.1223(3) 0.67222(14) 0.0460(6) Uani 1 d . . C22 C 0.2776(2) 0.1369(3) 0.7067(2) 0.0591(7) Uani 1 d . . H22 H 0.2347(2) 0.2010(3) 0.6827(2) 0.086(5) Uiso 1 calc R . C23 C 0.2868(2) 0.0567(4) 0.7770(2) 0.0736(9) Uani 1 d . . H23 H 0.2498(2) 0.0665(4) 0.7997(2) 0.086(5) Uiso 1 calc R . C24 C 0.3502(2) -0.0370(4) 0.8132(2) 0.0811(10) Uani 1 d . . H24 H 0.3563(2) -0.0903(4) 0.8604(2) 0.086(5) Uiso 1 calc R . C25 C 0.4047(2) -0.0523(4) 0.7797(2) 0.0744(9) Uani 1 d . . H25 H 0.4477(2) -0.1159(4) 0.8042(2) 0.086(5) Uiso 1 calc R . C26 C 0.3955(2) 0.0271(3) 0.7095(2) 0.0592(7) Uani 1 d . . H26 H 0.4325(2) 0.0163(3) 0.6869(2) 0.086(5) Uiso 1 calc R . C27 C 0.3520(2) 0.6284(3) 0.5578(2) 0.0839(10) Uani 1 d . . H271 H 0.3952(2) 0.5702(3) 0.5555(2) 0.119(8) Uiso 1 calc R . H272 H 0.3680(2) 0.7339(3) 0.5784(2) 0.119(8) Uiso 1 calc R . H273 H 0.3132(2) 0.6362(3) 0.5051(2) 0.119(8) Uiso 1 calc R . C28 C 0.3883(2) 0.5020(4) 0.7244(2) 0.0846(10) Uani 1 d . . H281 H 0.4313(2) 0.4456(4) 0.7203(2) 0.158(10) Uiso 1 calc R . H282 H 0.3686(2) 0.4435(4) 0.7585(2) 0.158(10) Uiso 1 calc R . H283 H 0.4044(2) 0.6065(4) 0.7465(2) 0.158(10) Uiso 1 calc R . C29 C 0.2290(2) 0.6301(4) 0.6302(2) 0.0889(11) Uani 1 d . . H291 H 0.1901(2) 0.6397(4) 0.5777(2) 0.121(8) Uiso 1 calc R . H292 H 0.2447(2) 0.7349(4) 0.6521(2) 0.121(8) Uiso 1 calc R . H293 H 0.2088(2) 0.5719(4) 0.6640(2) 0.121(8) 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 P1 0.0525(4) 0.0431(4) 0.0454(3) 0.0056(3) 0.0223(3) 0.0088(3) Si1 0.0736(5) 0.0390(4) 0.0653(5) -0.0025(3) 0.0373(4) 0.0018(4) O1 0.0512(10) 0.0493(10) 0.0534(10) -0.0004(8) 0.0266(8) -0.0025(8) O2 0.0819(13) 0.0499(11) 0.0600(11) 0.0167(9) 0.0313(10) 0.0139(9) O3 0.0532(10) 0.0391(9) 0.0578(10) -0.0006(8) 0.0241(8) 0.0067(8) C1 0.0451(14) 0.0371(13) 0.0527(14) 0.0005(11) 0.0221(11) 0.0027(11) C2 0.0493(13) 0.0350(12) 0.0452(13) 0.0046(10) 0.0228(11) 0.0053(11) C3 0.0565(15) 0.0475(15) 0.058(2) 0.0006(12) 0.0336(13) 0.0095(12) C4 0.057(2) 0.052(2) 0.0575(15) 0.0045(13) 0.0340(13) 0.0030(13) C5 0.072(2) 0.090(2) 0.088(2) -0.012(2) 0.052(2) -0.013(2) C8 0.078(2) 0.091(2) 0.070(2) -0.016(2) 0.046(2) 0.000(2) C9 0.0476(14) 0.060(2) 0.0458(14) 0.0005(12) 0.0199(11) 0.0055(12) C10 0.092(2) 0.081(2) 0.053(2) 0.004(2) 0.019(2) 0.003(2) C11 0.126(3) 0.138(4) 0.042(2) -0.015(2) 0.010(2) -0.017(3) C12 0.124(3) 0.092(3) 0.080(3) -0.042(2) 0.047(2) -0.026(2) C13 0.085(2) 0.070(2) 0.089(2) -0.021(2) 0.040(2) -0.004(2) C14 0.063(2) 0.054(2) 0.066(2) -0.0091(14) 0.0226(14) 0.0022(14) C15 0.0469(14) 0.059(2) 0.0528(15) -0.0046(13) 0.0206(12) 0.0040(13) C16 0.075(2) 0.083(2) 0.096(2) -0.004(2) 0.048(2) 0.021(2) C17 0.095(3) 0.125(4) 0.136(4) -0.023(3) 0.073(3) 0.025(3) C18 0.082(3) 0.170(5) 0.093(3) -0.032(3) 0.058(2) -0.015(3) C19 0.088(2) 0.130(3) 0.082(2) 0.002(2) 0.052(2) -0.014(2) C20 0.073(2) 0.084(2) 0.070(2) 0.008(2) 0.038(2) 0.001(2) C21 0.058(2) 0.0367(13) 0.0462(13) -0.0028(11) 0.0224(12) -0.0044(11) C22 0.068(2) 0.061(2) 0.058(2) -0.0012(14) 0.0354(14) -0.0055(14) C23 0.099(2) 0.075(2) 0.063(2) -0.007(2) 0.049(2) -0.017(2) C24 0.122(3) 0.071(2) 0.054(2) 0.010(2) 0.037(2) -0.012(2) C25 0.092(2) 0.069(2) 0.056(2) 0.010(2) 0.020(2) 0.007(2) C26 0.072(2) 0.056(2) 0.0509(15) 0.0054(13) 0.0242(14) 0.0063(14) C27 0.117(3) 0.049(2) 0.105(3) 0.012(2) 0.064(2) 0.003(2) C28 0.101(2) 0.083(2) 0.069(2) -0.018(2) 0.031(2) -0.016(2) C29 0.106(3) 0.054(2) 0.125(3) -0.013(2) 0.064(2) 0.011(2) #============================================================ # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 O2 1.475(2) . ? P1 C15 1.808(3) . ? P1 C9 1.816(3) . ? P1 C2 1.831(2) . ? Si1 O3 1.659(2) . ? Si1 C29 1.844(3) . ? Si1 C28 1.848(3) . ? Si1 C27 1.849(3) . ? O1 C1 1.421(3) . ? O1 C4 1.443(3) . ? O3 C1 1.407(3) . ? C1 C21 1.521(3) . ? C1 C2 1.570(3) . ? C2 C3 1.554(3) . ? C2 H2 0.98 . ? C3 C4 1.513(3) . ? C3 C8 1.516(4) . ? C3 H3 0.98 . ? C4 C5 1.509(4) . ? C4 H4 0.98 . ? C5 H51 0.96 . ? C5 H52 0.96 . ? C5 H53 0.96 . ? C8 H81 0.96 . ? C8 H82 0.96 . ? C8 H83 0.96 . ? C9 C10 1.385(4) . ? C9 C14 1.394(4) . ? C10 C11 1.376(4) . ? C10 H10 0.93 . ? C11 C12 1.37 . ? C11 H11 0.93 . ? C12 C13 1.36 . ? C12 H12 0.93 . ? C13 C14 1.376(3) . ? C13 H13 0.93 . ? C14 H14 0.93 . ? C15 C20 1.372(4) . ? C15 C16 1.384(4) . ? C16 C17 1.388(5) . ? C16 H16 0.93 . ? C17 C18 1.365(6) . ? C17 H17 0.93 . ? C18 C19 1.354(6) . ? C18 H18 0.93 . ? C19 C20 1.379(4) . ? C19 H19 0.93 . ? C20 H20 0.93 . ? C21 C22 1.380(3) . ? C21 C26 1.383(3) . ? C22 C23 1.386(4) . ? C22 H22 0.93 . ? C23 C24 1.370(5) . ? C23 H23 0.93 . ? C24 C25 1.371(4) . ? C24 H24 0.93 . ? C25 C26 1.382(4) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C27 H271 0.96 . ? C27 H272 0.96 . ? C27 H273 0.96 . ? C28 H281 0.96 . ? C28 H282 0.96 . ? C28 H283 0.96 . ? C29 H291 0.96 . ? C29 H292 0.96 . ? C29 H293 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 P1 C15 113.84(12) . . ? O2 P1 C9 111.61(11) . . ? C15 P1 C9 103.52(12) . . ? O2 P1 C2 116.76(11) . . ? C15 P1 C2 105.32(11) . . ? C9 P1 C2 104.54(11) . . ? O3 Si1 C29 104.14(13) . . ? O3 Si1 C28 111.88(12) . . ? C29 Si1 C28 110.4(2) . . ? O3 Si1 C27 110.37(12) . . ? C29 Si1 C27 110.9(2) . . ? C28 Si1 C27 109.1(2) . . ? C1 O1 C4 107.8(2) . . ? C1 O3 Si1 124.71(14) . . ? O3 C1 O1 109.2(2) . . ? O3 C1 C21 110.4(2) . . ? O1 C1 C21 108.6(2) . . ? O3 C1 C2 110.3(2) . . ? O1 C1 C2 105.5(2) . . ? C21 C1 C2 112.7(2) . . ? C3 C2 C1 103.2(2) . . ? C3 C2 P1 116.1(2) . . ? C1 C2 P1 114.6(2) . . ? C3 C2 H2 107.47(13) . . ? C1 C2 H2 107.47(12) . . ? P1 C2 H2 107.47(7) . . ? C4 C3 C8 113.8(2) . . ? C4 C3 C2 101.2(2) . . ? C8 C3 C2 119.5(2) . . ? C4 C3 H3 107.21(14) . . ? C8 C3 H3 107.2(2) . . ? C2 C3 H3 107.21(13) . . ? O1 C4 C5 108.0(2) . . ? O1 C4 C3 102.8(2) . . ? C5 C4 C3 116.5(2) . . ? O1 C4 H4 109.76(12) . . ? C5 C4 H4 109.8(2) . . ? C3 C4 H4 109.76(14) . . ? C4 C5 H51 109.5(2) . . ? C4 C5 H52 109.5(2) . . ? H51 C5 H52 109.5 . . ? C4 C5 H53 109.5(2) . . ? H51 C5 H53 109.5 . . ? H52 C5 H53 109.5 . . ? C3 C8 H81 109.5(2) . . ? C3 C8 H82 109.47(15) . . ? H81 C8 H82 109.5 . . ? C3 C8 H83 109.5(2) . . ? H81 C8 H83 109.5 . . ? H82 C8 H83 109.5 . . ? C10 C9 C14 117.7(3) . . ? C10 C9 P1 117.6(2) . . ? C14 C9 P1 124.7(2) . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H10 119.9(2) . . ? C9 C10 H10 119.9(2) . . ? C12 C11 C10 120.7(2) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6(2) . . ? C13 C12 C11 120.4 . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.3(2) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4(2) . . ? C13 C14 C9 121.8(3) . . ? C13 C14 H14 119.1(2) . . ? C9 C14 H14 119.1(2) . . ? C20 C15 C16 119.0(3) . . ? C20 C15 P1 122.5(2) . . ? C16 C15 P1 118.4(2) . . ? C15 C16 C17 119.1(3) . . ? C15 C16 H16 120.5(2) . . ? C17 C16 H16 120.5(2) . . ? C18 C17 C16 121.1(4) . . ? C18 C17 H17 119.4(2) . . ? C16 C17 H17 119.4(2) . . ? C19 C18 C17 119.6(3) . . ? C19 C18 H18 120.2(2) . . ? C17 C18 H18 120.2(2) . . ? C18 C19 C20 120.4(4) . . ? C18 C19 H19 119.8(2) . . ? C20 C19 H19 119.8(2) . . ? C15 C20 C19 120.8(3) . . ? C15 C20 H20 119.6(2) . . ? C19 C20 H20 119.6(2) . . ? C22 C21 C26 118.6(2) . . ? C22 C21 C1 120.8(2) . . ? C26 C21 C1 120.6(2) . . ? C21 C22 C23 120.5(3) . . ? C21 C22 H22 119.8(2) . . ? C23 C22 H22 119.8(2) . . ? C24 C23 C22 120.1(3) . . ? C24 C23 H23 119.9(2) . . ? C22 C23 H23 119.9(2) . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 120.0(2) . . ? C25 C24 H24 120.0(2) . . ? C24 C25 C26 119.8(3) . . ? C24 C25 H25 120.1(2) . . ? C26 C25 H25 120.1(2) . . ? C25 C26 C21 120.9(3) . . ? C25 C26 H26 119.6(2) . . ? C21 C26 H26 119.57(15) . . ? Si1 C27 H271 109.47(11) . . ? Si1 C27 H272 109.47(10) . . ? H271 C27 H272 109.5 . . ? Si1 C27 H273 109.47(12) . . ? H271 C27 H273 109.5 . . ? H272 C27 H273 109.5 . . ? Si1 C28 H281 109.47(11) . . ? Si1 C28 H282 109.47(11) . . ? H281 C28 H282 109.5 . . ? Si1 C28 H283 109.47(11) . . ? H281 C28 H283 109.5 . . ? H282 C28 H283 109.5 . . ? Si1 C29 H291 109.47(12) . . ? Si1 C29 H292 109.47(11) . . ? H291 C29 H292 109.5 . . ? Si1 C29 H293 109.47(11) . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 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 C29 Si1 O3 C1 -157.6(2) . . . . ? C28 Si1 O3 C1 -38.4(2) . . . . ? C27 Si1 O3 C1 83.4(2) . . . . ? Si1 O3 C1 O1 -35.3(2) . . . . ? Si1 O3 C1 C21 84.0(2) . . . . ? Si1 O3 C1 C2 -150.81(15) . . . . ? C4 O1 C1 O3 -93.4(2) . . . . ? C4 O1 C1 C21 146.1(2) . . . . ? C4 O1 C1 C2 25.1(2) . . . . ? O3 C1 C2 C3 120.1(2) . . . . ? O1 C1 C2 C3 2.3(2) . . . . ? C21 C1 C2 C3 -116.0(2) . . . . ? O3 C1 C2 P1 -7.1(2) . . . . ? O1 C1 C2 P1 -124.9(2) . . . . ? C21 C1 C2 P1 116.8(2) . . . . ? O2 P1 C2 C3 -52.7(2) . . . . ? C15 P1 C2 C3 179.9(2) . . . . ? C9 P1 C2 C3 71.1(2) . . . . ? O2 P1 C2 C1 67.6(2) . . . . ? C15 P1 C2 C1 -59.8(2) . . . . ? C9 P1 C2 C1 -168.6(2) . . . . ? C1 C2 C3 C4 -26.7(2) . . . . ? P1 C2 C3 C4 99.6(2) . . . . ? C1 C2 C3 C8 -152.5(2) . . . . ? P1 C2 C3 C8 -26.2(3) . . . . ? C1 O1 C4 C5 -167.1(2) . . . . ? C1 O1 C4 C3 -43.4(2) . . . . ? C8 C3 C4 O1 171.7(2) . . . . ? C2 C3 C4 O1 42.2(2) . . . . ? C8 C3 C4 C5 -70.4(3) . . . . ? C2 C3 C4 C5 160.1(2) . . . . ? O2 P1 C9 C10 -21.0(3) . . . . ? C15 P1 C9 C10 101.9(2) . . . . ? C2 P1 C9 C10 -148.1(2) . . . . ? O2 P1 C9 C14 159.5(2) . . . . ? C15 P1 C9 C14 -77.7(2) . . . . ? C2 P1 C9 C14 32.4(3) . . . . ? C14 C9 C10 C11 0.6(4) . . . . ? P1 C9 C10 C11 -178.9(2) . . . . ? C9 C10 C11 C12 -1.0(3) . . . . ? C10 C11 C12 C13 0.2(2) . . . . ? C11 C12 C13 C14 0.8(2) . . . . ? C12 C13 C14 C9 -1.1(3) . . . . ? C10 C9 C14 C13 0.4(4) . . . . ? P1 C9 C14 C13 179.9(2) . . . . ? O2 P1 C15 C20 172.8(2) . . . . ? C9 P1 C15 C20 51.4(3) . . . . ? C2 P1 C15 C20 -58.1(3) . . . . ? O2 P1 C15 C16 -7.6(3) . . . . ? C9 P1 C15 C16 -129.0(2) . . . . ? C2 P1 C15 C16 121.5(2) . . . . ? C20 C15 C16 C17 1.7(5) . . . . ? P1 C15 C16 C17 -177.9(3) . . . . ? C15 C16 C17 C18 -0.8(6) . . . . ? C16 C17 C18 C19 -0.3(6) . . . . ? C17 C18 C19 C20 0.5(6) . . . . ? C16 C15 C20 C19 -1.6(5) . . . . ? P1 C15 C20 C19 177.9(2) . . . . ? C18 C19 C20 C15 0.5(5) . . . . ? O3 C1 C21 C22 29.1(3) . . . . ? O1 C1 C21 C22 148.8(2) . . . . ? C2 C1 C21 C22 -94.8(3) . . . . ? O3 C1 C21 C26 -152.8(2) . . . . ? O1 C1 C21 C26 -33.1(3) . . . . ? C2 C1 C21 C26 83.4(3) . . . . ? C26 C21 C22 C23 -0.4(4) . . . . ? C1 C21 C22 C23 177.8(2) . . . . ? C21 C22 C23 C24 0.5(4) . . . . ? C22 C23 C24 C25 -0.3(5) . . . . ? C23 C24 C25 C26 0.0(5) . . . . ? C24 C25 C26 C21 0.1(4) . . . . ? C22 C21 C26 C25 0.1(4) . . . . ? C1 C21 C26 C25 -178.1(2) . . . . ? #============================================================