data_kaw60 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H34 O2 Si' _chemical_formula_weight 358.58 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 P2(1)/n 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 10.6806(13) _cell_length_b 13.2710(16) _cell_length_c 14.7945(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.257(2) _cell_angle_gamma 90.00 _cell_volume 2097.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9475 _exptl_absorpt_correction_T_max 0.9733 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 frames' _diffrn_standards_interval_count 'initial 50 frames recollected' _diffrn_standards_interval_time ? _diffrn_standards_decay_% '< 1.0' _diffrn_reflns_number 21777 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0186 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5028 _reflns_number_gt 4327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART/SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0526P)^2^+0.5790P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5028 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0938 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.33623(3) 0.29563(2) 0.126173(19) 0.01656(9) Uani 1 1 d . . . O1 O 0.28052(7) 0.22484(6) 0.21326(5) 0.02152(17) Uani 1 1 d . . . O2 O 0.13231(8) 0.21845(6) 0.31819(5) 0.02559(18) Uani 1 1 d . . . C1 C 0.17811(9) 0.26166(8) 0.25500(7) 0.0173(2) Uani 1 1 d . . . C2 C 0.13089(9) 0.36404(7) 0.21794(6) 0.01535(19) Uani 1 1 d . . . C3 C 0.20042(9) 0.38722(7) 0.12781(7) 0.01548(19) Uani 1 1 d . . . C4 C 0.22722(11) 0.49861(8) 0.10750(8) 0.0245(2) Uani 1 1 d . . . C5 C 0.16051(10) 0.44078(9) 0.29322(7) 0.0222(2) Uani 1 1 d . . . C6 C -0.01580(9) 0.35615(8) 0.20866(7) 0.0174(2) Uani 1 1 d . . . C7 C -0.07596(10) 0.45802(8) 0.19462(8) 0.0240(2) Uani 1 1 d . . . C8 C -0.16002(11) 0.49699(10) 0.24958(10) 0.0320(3) Uani 1 1 d . . . C9 C -0.05953(9) 0.28076(8) 0.13750(7) 0.0181(2) Uani 1 1 d . . . C10 C -0.09320(11) 0.31012(9) 0.05024(8) 0.0254(2) Uani 1 1 d . . . C11 C -0.13546(13) 0.24074(10) -0.01323(9) 0.0334(3) Uani 1 1 d . . . C12 C -0.14313(13) 0.13972(10) 0.00936(9) 0.0334(3) Uani 1 1 d . . . C13 C -0.11010(12) 0.10881(9) 0.09550(8) 0.0292(3) Uani 1 1 d . . . C14 C -0.06987(10) 0.17860(8) 0.15964(8) 0.0221(2) Uani 1 1 d . . . C15 C 0.33042(11) 0.21766(8) 0.01842(8) 0.0249(2) Uani 1 1 d . . . C16 C 0.44139(13) 0.14506(11) 0.00614(10) 0.0367(3) Uani 1 1 d . . . C17 C 0.20994(13) 0.15406(10) 0.02016(10) 0.0348(3) Uani 1 1 d . . . C18 C 0.32451(13) 0.28915(11) -0.06350(8) 0.0323(3) Uani 1 1 d . . . C19 C 0.49762(10) 0.33980(9) 0.16285(8) 0.0239(2) Uani 1 1 d . . . C20 C 0.57872(13) 0.24873(12) 0.19071(11) 0.0374(3) Uani 1 1 d . . . C21 C 0.48973(12) 0.40882(12) 0.24575(9) 0.0352(3) Uani 1 1 d . . . C22 C 0.56306(12) 0.39756(11) 0.08634(9) 0.0332(3) Uani 1 1 d . . . H3 H 0.1461(12) 0.3612(10) 0.0795(9) 0.019(3) Uiso 1 1 d . . . H4A H 0.1514(15) 0.5383(12) 0.1078(10) 0.035(4) Uiso 1 1 d . . . H4B H 0.2647(15) 0.5047(11) 0.0468(11) 0.034(4) Uiso 1 1 d . . . H4C H 0.2851(14) 0.5293(11) 0.1507(10) 0.032(4) Uiso 1 1 d . . . H5A H 0.2507(14) 0.4430(11) 0.3066(10) 0.030(4) Uiso 1 1 d . . . H5B H 0.1139(14) 0.4199(11) 0.3473(11) 0.033(4) Uiso 1 1 d . . . H5C H 0.1347(13) 0.5095(11) 0.2750(10) 0.029(4) Uiso 1 1 d . . . H6 H -0.0452(12) 0.3319(10) 0.2676(9) 0.019(3) Uiso 1 1 d . . . H7 H -0.0532(14) 0.4950(11) 0.1411(11) 0.036(4) Uiso 1 1 d . . . H8A H -0.1958(15) 0.5599(13) 0.2374(11) 0.041(4) Uiso 1 1 d . . . H8B H -0.1853(15) 0.4590(12) 0.3044(11) 0.041(4) Uiso 1 1 d . . . H10 H -0.0900(14) 0.3808(12) 0.0335(10) 0.035(4) Uiso 1 1 d . . . H11 H -0.1599(16) 0.2639(13) -0.0722(12) 0.046(5) Uiso 1 1 d . . . H12 H -0.1723(16) 0.0923(13) -0.0346(12) 0.048(5) Uiso 1 1 d . . . H13 H -0.1141(14) 0.0376(12) 0.1109(10) 0.035(4) Uiso 1 1 d . . . H14 H -0.0498(13) 0.1571(10) 0.2195(9) 0.023(3) Uiso 1 1 d . . . H16A H 0.5202(16) 0.1798(13) -0.0042(11) 0.042(4) Uiso 1 1 d . . . H16B H 0.4513(16) 0.0981(13) 0.0583(12) 0.048(5) Uiso 1 1 d . . . H16C H 0.4257(16) 0.1041(14) -0.0487(13) 0.052(5) Uiso 1 1 d . . . H17A H 0.1327(16) 0.1956(12) 0.0252(11) 0.040(4) Uiso 1 1 d . . . H17B H 0.2026(15) 0.1162(13) -0.0351(12) 0.045(4) Uiso 1 1 d . . . H17C H 0.2074(18) 0.1050(15) 0.0712(13) 0.058(5) Uiso 1 1 d . . . H18A H 0.3122(17) 0.2484(14) -0.1174(13) 0.050(5) Uiso 1 1 d . . . H18B H 0.2522(16) 0.3360(13) -0.0580(11) 0.043(4) Uiso 1 1 d . . . H18C H 0.4020(16) 0.3285(13) -0.0720(11) 0.043(4) Uiso 1 1 d . . . H20A H 0.5980(18) 0.2027(13) 0.1430(13) 0.050(5) Uiso 1 1 d . . . H20B H 0.5354(17) 0.2074(12) 0.2349(12) 0.045(5) Uiso 1 1 d . . . H20C H 0.6592(18) 0.2737(13) 0.2167(13) 0.052(5) Uiso 1 1 d . . . H21A H 0.4401(16) 0.4723(13) 0.2324(11) 0.042(4) Uiso 1 1 d . . . H21B H 0.4516(15) 0.3748(12) 0.2984(11) 0.040(4) Uiso 1 1 d . . . H21C H 0.5758(17) 0.4282(13) 0.2642(12) 0.053(5) Uiso 1 1 d . . . H22A H 0.5151(16) 0.4571(13) 0.0692(12) 0.046(4) Uiso 1 1 d . . . H22B H 0.5743(15) 0.3554(12) 0.0305(12) 0.040(4) Uiso 1 1 d . . . H22C H 0.6463(16) 0.4180(13) 0.1070(11) 0.045(4) Uiso 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 Si1 0.01509(14) 0.01622(14) 0.01840(15) 0.00157(10) 0.00253(10) 0.00073(9) O1 0.0208(4) 0.0192(4) 0.0246(4) 0.0065(3) 0.0051(3) 0.0048(3) O2 0.0241(4) 0.0310(4) 0.0216(4) 0.0105(3) 0.0029(3) 0.0020(3) C1 0.0163(4) 0.0197(5) 0.0158(5) 0.0010(4) -0.0019(4) -0.0008(4) C2 0.0152(4) 0.0161(4) 0.0148(4) 0.0001(3) -0.0002(3) 0.0006(3) C3 0.0160(4) 0.0158(4) 0.0147(4) 0.0011(3) -0.0001(3) -0.0007(3) C4 0.0264(5) 0.0174(5) 0.0297(6) 0.0056(4) 0.0035(5) -0.0001(4) C5 0.0221(5) 0.0255(5) 0.0189(5) -0.0055(4) -0.0009(4) -0.0015(4) C6 0.0153(4) 0.0188(5) 0.0180(5) 0.0001(4) 0.0011(4) 0.0005(4) C7 0.0193(5) 0.0212(5) 0.0316(6) -0.0009(4) -0.0025(4) 0.0016(4) C8 0.0225(5) 0.0284(6) 0.0452(7) -0.0102(5) -0.0021(5) 0.0059(5) C9 0.0128(4) 0.0212(5) 0.0203(5) 0.0004(4) -0.0002(4) -0.0003(4) C10 0.0262(5) 0.0245(5) 0.0255(6) 0.0031(4) -0.0073(4) 0.0003(4) C11 0.0368(7) 0.0380(7) 0.0253(6) 0.0012(5) -0.0134(5) -0.0043(5) C12 0.0353(6) 0.0354(7) 0.0293(6) -0.0062(5) -0.0083(5) -0.0114(5) C13 0.0320(6) 0.0243(6) 0.0314(6) -0.0005(5) -0.0006(5) -0.0102(5) C14 0.0223(5) 0.0226(5) 0.0213(5) 0.0028(4) 0.0002(4) -0.0050(4) C15 0.0254(6) 0.0233(5) 0.0259(6) -0.0054(4) 0.0075(4) -0.0003(4) C16 0.0346(7) 0.0327(7) 0.0430(8) -0.0093(6) 0.0127(6) 0.0070(5) C17 0.0326(7) 0.0298(6) 0.0420(7) -0.0173(6) 0.0100(6) -0.0082(5) C18 0.0363(7) 0.0398(7) 0.0208(6) -0.0035(5) 0.0041(5) 0.0001(6) C19 0.0151(5) 0.0309(6) 0.0256(5) 0.0046(4) -0.0007(4) 0.0000(4) C20 0.0236(6) 0.0467(8) 0.0419(8) 0.0118(7) -0.0019(5) 0.0102(6) C21 0.0219(6) 0.0512(8) 0.0324(7) -0.0066(6) -0.0062(5) -0.0042(6) C22 0.0214(6) 0.0432(7) 0.0351(7) 0.0091(6) 0.0004(5) -0.0096(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 Si1 O1 1.7040(8) . ? Si1 C3 1.8928(10) . ? Si1 C19 1.8976(11) . ? Si1 C15 1.9013(12) . ? O1 C1 1.3500(12) . ? O2 C1 1.2027(13) . ? C1 C2 1.5487(14) . ? C2 C5 1.5409(14) . ? C2 C3 1.5598(13) . ? C2 C6 1.5756(14) . ? C3 C4 1.5356(14) . ? C6 C7 1.5108(14) . ? C6 C9 1.5242(14) . ? C7 C8 1.3195(17) . ? C9 C10 1.3941(15) . ? C9 C14 1.3993(15) . ? C10 C11 1.3890(17) . ? C11 C12 1.3842(19) . ? C12 C13 1.3831(18) . ? C13 C14 1.3926(16) . ? C15 C16 1.5388(17) . ? C15 C17 1.5392(17) . ? C15 C18 1.5403(17) . ? C19 C21 1.5334(18) . ? C19 C22 1.5376(16) . ? C19 C20 1.5419(17) . ? 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 O1 Si1 C3 94.25(4) . . ? O1 Si1 C19 105.90(5) . . ? C3 Si1 C19 119.55(5) . . ? O1 Si1 C15 108.89(5) . . ? C3 Si1 C15 109.76(5) . . ? C19 Si1 C15 115.73(5) . . ? C1 O1 Si1 115.64(6) . . ? O2 C1 O1 121.08(9) . . ? O2 C1 C2 124.10(9) . . ? O1 C1 C2 114.76(8) . . ? C5 C2 C1 104.98(8) . . ? C5 C2 C3 112.99(8) . . ? C1 C2 C3 108.67(8) . . ? C5 C2 C6 107.93(8) . . ? C1 C2 C6 107.13(8) . . ? C3 C2 C6 114.56(8) . . ? C4 C3 C2 116.55(8) . . ? C4 C3 Si1 118.17(7) . . ? C2 C3 Si1 104.60(6) . . ? C7 C6 C9 111.32(9) . . ? C7 C6 C2 112.00(8) . . ? C9 C6 C2 113.91(8) . . ? C8 C7 C6 123.79(12) . . ? C10 C9 C14 117.86(10) . . ? C10 C9 C6 122.21(9) . . ? C14 C9 C6 119.90(9) . . ? C11 C10 C9 121.49(11) . . ? C12 C11 C10 119.89(12) . . ? C13 C12 C11 119.64(11) . . ? C12 C13 C14 120.48(11) . . ? C13 C14 C9 120.62(10) . . ? C16 C15 C17 107.64(10) . . ? C16 C15 C18 108.76(10) . . ? C17 C15 C18 108.64(11) . . ? C16 C15 Si1 114.68(9) . . ? C17 C15 Si1 107.97(8) . . ? C18 C15 Si1 109.00(8) . . ? C21 C19 C22 108.53(11) . . ? C21 C19 C20 106.69(11) . . ? C22 C19 C20 109.32(10) . . ? C21 C19 Si1 111.11(8) . . ? C22 C19 Si1 111.03(8) . . ? C20 C19 Si1 110.05(9) . . ? 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 C3 Si1 O1 C1 -6.69(8) . . . . ? C19 Si1 O1 C1 115.68(8) . . . . ? C15 Si1 O1 C1 -119.26(8) . . . . ? Si1 O1 C1 O2 -178.84(8) . . . . ? Si1 O1 C1 C2 -1.63(11) . . . . ? O2 C1 C2 C5 67.30(12) . . . . ? O1 C1 C2 C5 -109.82(10) . . . . ? O2 C1 C2 C3 -171.56(10) . . . . ? O1 C1 C2 C3 11.32(11) . . . . ? O2 C1 C2 C6 -47.27(13) . . . . ? O1 C1 C2 C6 135.61(9) . . . . ? C5 C2 C3 C4 -30.82(12) . . . . ? C1 C2 C3 C4 -146.91(9) . . . . ? C6 C2 C3 C4 93.33(10) . . . . ? C5 C2 C3 Si1 101.68(8) . . . . ? C1 C2 C3 Si1 -14.41(9) . . . . ? C6 C2 C3 Si1 -134.17(7) . . . . ? O1 Si1 C3 C4 143.83(8) . . . . ? C19 Si1 C3 C4 32.86(10) . . . . ? C15 Si1 C3 C4 -104.35(9) . . . . ? O1 Si1 C3 C2 12.26(7) . . . . ? C19 Si1 C3 C2 -98.71(7) . . . . ? C15 Si1 C3 C2 124.08(7) . . . . ? C5 C2 C6 C7 53.76(11) . . . . ? C1 C2 C6 C7 166.34(9) . . . . ? C3 C2 C6 C7 -73.05(11) . . . . ? C5 C2 C6 C9 -178.78(8) . . . . ? C1 C2 C6 C9 -66.20(10) . . . . ? C3 C2 C6 C9 54.41(11) . . . . ? C9 C6 C7 C8 110.68(13) . . . . ? C2 C6 C7 C8 -120.49(12) . . . . ? C7 C6 C9 C10 30.50(14) . . . . ? C2 C6 C9 C10 -97.30(11) . . . . ? C7 C6 C9 C14 -147.89(10) . . . . ? C2 C6 C9 C14 84.31(12) . . . . ? C14 C9 C10 C11 -0.16(17) . . . . ? C6 C9 C10 C11 -178.58(11) . . . . ? C9 C10 C11 C12 -0.9(2) . . . . ? C10 C11 C12 C13 0.8(2) . . . . ? C11 C12 C13 C14 0.3(2) . . . . ? C12 C13 C14 C9 -1.42(18) . . . . ? C10 C9 C14 C13 1.32(16) . . . . ? C6 C9 C14 C13 179.77(10) . . . . ? O1 Si1 C15 C16 -82.03(9) . . . . ? C3 Si1 C15 C16 176.07(9) . . . . ? C19 Si1 C15 C16 37.07(11) . . . . ? O1 Si1 C15 C17 37.95(10) . . . . ? C3 Si1 C15 C17 -63.95(10) . . . . ? C19 Si1 C15 C17 157.05(9) . . . . ? O1 Si1 C15 C18 155.80(8) . . . . ? C3 Si1 C15 C18 53.90(9) . . . . ? C19 Si1 C15 C18 -85.10(9) . . . . ? O1 Si1 C19 C21 -63.89(10) . . . . ? C3 Si1 C19 C21 40.59(10) . . . . ? C15 Si1 C19 C21 175.38(9) . . . . ? O1 Si1 C19 C22 175.22(8) . . . . ? C3 Si1 C19 C22 -80.30(10) . . . . ? C15 Si1 C19 C22 54.49(10) . . . . ? O1 Si1 C19 C20 54.05(9) . . . . ? C3 Si1 C19 C20 158.53(8) . . . . ? C15 Si1 C19 C20 -66.68(10) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.376 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.040