data_k08220 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H26 O2 Si' _chemical_formula_sum 'C18 H26 O2 Si' _chemical_formula_weight 302.48 _chemical_absolute_configuration 'ad' 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 Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.9876(5) _cell_length_b 7.3491(3) _cell_length_c 19.9858(18) _cell_angle_alpha 90.00 _cell_angle_beta 97.689(3) _cell_angle_gamma 90.00 _cell_volume 871.54(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 5697 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 0.137 # Absorption correction _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5697 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3612 _reflns_number_gt 2986 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.0597P)^2^+0.2455P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.13(17) _refine_ls_number_reflns 3612 _refine_ls_number_parameters 196 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 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 Si1 Si 0.75208(13) 0.38829(11) 0.33639(4) 0.0357(2) Uani 1 1 d . . . O1 O 0.5446(3) 0.5956(3) 0.16393(10) 0.0360(5) Uani 1 1 d . . . O2 O 0.8909(4) 0.5019(3) 0.28348(10) 0.0411(5) Uani 1 1 d . . . C1 C 0.6485(5) 0.8945(5) 0.15519(14) 0.0358(6) Uani 1 1 d . . . H1 H 0.6183 1.0213 0.1560 0.043 Uiso 1 1 calc R . . C2 C 0.5002(5) 0.7479(4) 0.11715(16) 0.0349(7) Uani 1 1 d . . . H2A H 0.3381 0.7806 0.1040 0.042 Uiso 1 1 calc R . . C3 C 0.6255(4) 0.6806(4) 0.06022(15) 0.0313(6) Uani 1 1 d . . . C4 C 0.5927(5) 0.6979(4) -0.00900(15) 0.0352(6) Uani 1 1 d . . . H4A H 0.4644 0.7588 -0.0316 0.042 Uiso 1 1 calc R . . C5 C 0.7552(5) 0.6227(4) -0.04465(15) 0.0381(7) Uani 1 1 d . . . H5A H 0.7363 0.6320 -0.0925 0.046 Uiso 1 1 calc R . . C6 C 0.9439(5) 0.5344(4) -0.01190(16) 0.0386(7) Uani 1 1 d . . . H6A H 1.0515 0.4837 -0.0374 0.046 Uiso 1 1 calc R . . C7 C 0.9763(5) 0.5199(4) 0.05844(15) 0.0332(6) Uani 1 1 d . . . H7A H 1.1068 0.4622 0.0813 0.040 Uiso 1 1 calc R . . C8 C 0.8150(4) 0.5911(4) 0.09388(15) 0.0323(6) Uani 1 1 d . . . C9 C 0.7891(4) 0.6043(4) 0.16879(14) 0.0316(6) Uani 1 1 d . . . C10 C 0.8290(5) 0.8084(4) 0.18694(14) 0.0324(6) Uani 1 1 d . . . C11 C 1.0409(5) 0.8808(5) 0.22563(15) 0.0397(6) Uani 1 1 d . . . H11A H 1.0421 1.0138 0.2223 0.060 Uiso 1 1 calc R . . H11B H 1.1711 0.8309 0.2069 0.060 Uiso 1 1 calc R . . H11C H 1.0486 0.8451 0.2731 0.060 Uiso 1 1 calc R . . C12 C 0.9063(5) 0.4632(4) 0.21514(15) 0.0369(7) Uani 1 1 d . . . H12A H 0.8382 0.3427 0.2035 0.044 Uiso 1 1 calc R . . H12B H 1.0671 0.4575 0.2085 0.044 Uiso 1 1 calc R . . C13 C 0.5024(6) 0.2698(5) 0.28970(19) 0.0538(9) Uani 1 1 d . . . H13A H 0.5522 0.1600 0.2681 0.081 Uiso 1 1 calc R . . H13B H 0.4261 0.3513 0.2551 0.081 Uiso 1 1 calc R . . H13C H 0.3979 0.2359 0.3214 0.081 Uiso 1 1 calc R . . C14 C 0.9394(6) 0.2140(5) 0.38151(17) 0.0460(8) Uani 1 1 d . . . H14A H 0.9960 0.1331 0.3486 0.069 Uiso 1 1 calc R . . H14B H 0.8546 0.1428 0.4110 0.069 Uiso 1 1 calc R . . H14C H 1.0666 0.2741 0.4087 0.069 Uiso 1 1 calc R . . C15 C 0.6726(5) 0.5679(4) 0.39611(16) 0.0398(7) Uani 1 1 d . . . C16 C 0.5755(6) 0.4778(5) 0.45552(19) 0.0530(9) Uani 1 1 d . . . H16A H 0.5228 0.5721 0.4843 0.080 Uiso 1 1 calc R . . H16B H 0.6928 0.4049 0.4820 0.080 Uiso 1 1 calc R . . H16C H 0.4489 0.3990 0.4381 0.080 Uiso 1 1 calc R . . C17 C 0.4951(6) 0.6955(6) 0.3581(2) 0.0599(10) Uani 1 1 d . . . H17A H 0.4632 0.7953 0.3880 0.090 Uiso 1 1 calc R . . H17B H 0.3563 0.6272 0.3439 0.090 Uiso 1 1 calc R . . H17C H 0.5527 0.7454 0.3183 0.090 Uiso 1 1 calc R . . C18 C 0.8801(6) 0.6796(5) 0.42431(18) 0.0495(8) Uani 1 1 d . . . H18A H 0.8370 0.7706 0.4561 0.074 Uiso 1 1 calc R . . H18B H 0.9409 0.7411 0.3871 0.074 Uiso 1 1 calc R . . H18C H 0.9950 0.5987 0.4477 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0361(4) 0.0336(4) 0.0364(4) 0.0012(4) 0.0008(3) -0.0011(4) O1 0.0318(10) 0.0340(11) 0.0417(12) 0.0037(9) 0.0033(9) 0.0013(8) O2 0.0476(12) 0.0386(12) 0.0356(12) 0.0027(9) 0.0001(9) -0.0046(9) C1 0.0395(15) 0.0296(14) 0.0385(15) -0.0022(14) 0.0064(12) 0.0036(14) C2 0.0324(15) 0.0302(15) 0.0409(16) 0.0038(12) 0.0007(12) 0.0039(11) C3 0.0294(14) 0.0246(14) 0.0383(15) -0.0014(11) -0.0009(11) -0.0033(11) C4 0.0381(16) 0.0257(14) 0.0392(16) -0.0001(12) -0.0042(13) -0.0049(12) C5 0.0492(18) 0.0347(16) 0.0299(15) -0.0027(12) 0.0036(13) -0.0106(13) C6 0.0396(16) 0.0304(15) 0.0474(19) -0.0074(13) 0.0114(14) -0.0037(12) C7 0.0331(15) 0.0278(14) 0.0388(16) -0.0046(12) 0.0051(12) -0.0003(11) C8 0.0317(14) 0.0226(14) 0.0406(16) -0.0004(12) -0.0020(12) -0.0013(11) C9 0.0300(14) 0.0284(14) 0.0359(15) 0.0018(12) 0.0026(11) 0.0028(11) C10 0.0319(15) 0.0345(14) 0.0310(15) -0.0043(12) 0.0042(12) 0.0032(12) C11 0.0409(15) 0.0379(16) 0.0392(15) -0.0014(15) 0.0016(12) -0.0043(15) C12 0.0425(17) 0.0345(15) 0.0331(16) 0.0039(12) 0.0037(13) 0.0052(12) C13 0.045(2) 0.056(2) 0.058(2) -0.0069(17) 0.0006(17) -0.0098(16) C14 0.054(2) 0.0379(18) 0.0460(19) 0.0065(15) 0.0055(15) 0.0035(15) C15 0.0409(16) 0.0361(17) 0.0426(18) -0.0013(14) 0.0058(13) 0.0041(13) C16 0.056(2) 0.052(2) 0.054(2) -0.0049(18) 0.0155(17) -0.0042(16) C17 0.064(2) 0.053(2) 0.063(2) 0.0018(19) 0.0092(19) 0.0211(19) C18 0.055(2) 0.047(2) 0.0464(19) -0.0088(16) 0.0089(16) -0.0091(16) _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 Si1 O2 1.656(2) . ? Si1 C14 1.855(3) . ? Si1 C13 1.869(3) . ? Si1 C15 1.883(3) . ? O1 C9 1.456(3) . ? O1 C2 1.460(3) . ? O2 C12 1.410(4) . ? C1 C10 1.337(4) . ? C1 C2 1.532(4) . ? C2 C3 1.527(4) . ? C3 C4 1.377(4) . ? C3 C8 1.403(4) . ? C4 C5 1.395(4) . ? C5 C6 1.388(4) . ? C6 C7 1.397(4) . ? C7 C8 1.376(4) . ? C8 C9 1.529(4) . ? C9 C12 1.500(4) . ? C9 C10 1.554(4) . ? C10 C11 1.493(4) . ? C15 C18 1.532(4) . ? C15 C16 1.540(5) . ? C15 C17 1.540(4) . ? 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 Si1 C14 109.65(14) . . ? O2 Si1 C13 110.65(15) . . ? C14 Si1 C13 108.21(17) . . ? O2 Si1 C15 104.01(13) . . ? C14 Si1 C15 111.31(15) . . ? C13 Si1 C15 112.96(16) . . ? C9 O1 C2 96.0(2) . . ? C12 O2 Si1 128.34(19) . . ? C10 C1 C2 106.3(3) . . ? O1 C2 C3 99.4(2) . . ? O1 C2 C1 100.2(2) . . ? C3 C2 C1 106.7(2) . . ? C4 C3 C8 121.5(3) . . ? C4 C3 C2 134.5(3) . . ? C8 C3 C2 104.0(2) . . ? C3 C4 C5 117.5(3) . . ? C6 C5 C4 121.6(3) . . ? C5 C6 C7 120.3(3) . . ? C8 C7 C6 118.5(3) . . ? C7 C8 C3 120.7(3) . . ? C7 C8 C9 134.3(3) . . ? C3 C8 C9 105.0(2) . . ? O1 C9 C12 113.2(2) . . ? O1 C9 C8 99.5(2) . . ? C12 C9 C8 117.4(2) . . ? O1 C9 C10 100.3(2) . . ? C12 C9 C10 118.6(2) . . ? C8 C9 C10 104.9(2) . . ? C1 C10 C11 130.9(3) . . ? C1 C10 C9 104.9(2) . . ? C11 C10 C9 123.9(3) . . ? O2 C12 C9 111.9(2) . . ? C18 C15 C16 108.6(3) . . ? C18 C15 C17 109.1(3) . . ? C16 C15 C17 109.6(3) . . ? C18 C15 Si1 110.4(2) . . ? C16 C15 Si1 109.9(2) . . ? C17 C15 Si1 109.3(2) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.378 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.053