####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_bpsino _database_code_depnum_ccdc_archive 'CCDC 639019' _audit_creation_method 'enCIFer editing of SHELXL97 CIF output' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H54 O7 Si' _chemical_formula_sum 'C33 H54 O7 Si' _chemical_formula_weight 590.85 _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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5372(5) _cell_length_b 11.0197(6) _cell_length_c 16.2672(9) _cell_angle_alpha 90.00 _cell_angle_beta 92.323(2) _cell_angle_gamma 90.00 _cell_volume 1708.23(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10224 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.5 _exptl_crystal_description sphenoid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.86 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.47 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method ? _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.919 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS version 2.05; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15706 _diffrn_reflns_av_R_equivalents 0.011 _diffrn_reflns_av_sigmaI/netI 0.014 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.55 _reflns_number_total 7613 _reflns_number_gt 7366 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97-2 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'enCIFer (Allen et al., 2004); PLATON' _refine_special_details ; ? ; _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^)+(0.058P)^2^+0.254P] 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 0.05(7) _refine_ls_number_reflns 7597 _refine_ls_number_parameters 371 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.46158(14) 0.65154(16) 0.41237(8) 0.0330(3) Uani 1 1 d . . . H1 H 0.5652 0.6608 0.4222 0.040 Uiso 1 1 calc R . . O1A O 0.39417(14) 0.75358(11) 0.44847(7) 0.0422(3) Uani 1 1 d . . . C1A C 0.24586(19) 0.74268(18) 0.45355(11) 0.0449(4) Uani 1 1 d . . . H1AA H 0.2086 0.8156 0.4794 0.067 Uiso 1 1 calc R . . H1AB H 0.2240 0.6714 0.4867 0.067 Uiso 1 1 calc R . . H1AC H 0.2030 0.7335 0.3981 0.067 Uiso 1 1 calc R . . C1B C 0.4749(2) 0.5325(2) 0.53082(10) 0.0560(5) Uani 1 1 d . . . H1BA H 0.4435 0.4557 0.5541 0.084 Uiso 1 1 calc R . . H1BB H 0.4406 0.6002 0.5635 0.084 Uiso 1 1 calc R . . H1BC H 0.5777 0.5343 0.5317 0.084 Uiso 1 1 calc R . . O1B O 0.42103(12) 0.54339(11) 0.44793(6) 0.0377(2) Uani 1 1 d . . . C2 C 0.43095(15) 0.64548(15) 0.32014(8) 0.0306(3) Uani 1 1 d . . . H2A H 0.4676 0.7200 0.2946 0.037 Uiso 1 1 calc R . . H2B H 0.3280 0.6444 0.3096 0.037 Uiso 1 1 calc R . . O3 O 0.63797(11) 0.51866(11) 0.30635(6) 0.0365(2) Uani 1 1 d . . . C3 C 0.49455(13) 0.53465(13) 0.27828(8) 0.0250(2) Uani 1 1 d . . . H3 H 0.4398 0.4607 0.2924 0.030 Uiso 1 1 calc R . . C3M C 0.66428(18) 0.40587(19) 0.34653(11) 0.0461(4) Uani 1 1 d . . . H3MA H 0.7636 0.4010 0.3642 0.069 Uiso 1 1 calc R . . H3MB H 0.6413 0.3392 0.3084 0.069 Uiso 1 1 calc R . . H3MC H 0.6061 0.3996 0.3946 0.069 Uiso 1 1 calc R . . C4 C 0.49237(12) 0.54902(12) 0.18390(8) 0.0227(2) Uani 1 1 d . . . H4 H 0.5579 0.6168 0.1716 0.027 Uiso 1 1 calc R . . C4M C 0.54846(14) 0.43501(13) 0.14277(9) 0.0285(3) Uani 1 1 d . . . H4MA H 0.5459 0.4465 0.0830 0.043 Uiso 1 1 calc R . . H4MB H 0.4900 0.3653 0.1563 0.043 Uiso 1 1 calc R . . H4MC H 0.6453 0.4203 0.1626 0.043 Uiso 1 1 calc R . . C5 C 0.34638(12) 0.58494(11) 0.14747(7) 0.0211(2) Uani 1 1 d . . . H5 H 0.3171 0.6629 0.1731 0.025 Uiso 1 1 calc R . . O5A O 0.35255(10) 0.60209(9) 0.05934(5) 0.02469(19) Uani 1 1 d . . . C5A C 0.36659(15) 0.72261(13) 0.03347(8) 0.0284(3) Uani 1 1 d . . . H5AA H 0.3475 0.7264 -0.0267 0.034 Uiso 1 1 calc R . . H5AB H 0.2948 0.7726 0.0599 0.034 Uiso 1 1 calc R . . O5B O 0.49868(11) 0.77298(10) 0.05163(6) 0.0334(2) Uani 1 1 d . . . C5B C 0.60755(18) 0.71669(17) 0.00827(11) 0.0423(4) Uani 1 1 d . . . H5BA H 0.6975 0.7551 0.0238 0.063 Uiso 1 1 calc R . . H5BB H 0.5885 0.7260 -0.0511 0.063 Uiso 1 1 calc R . . H5BC H 0.6117 0.6302 0.0222 0.063 Uiso 1 1 calc R . . C6 C 0.23306(13) 0.49019(12) 0.15962(8) 0.0235(2) Uani 1 1 d . . . H6A H 0.2404 0.4602 0.2170 0.028 Uiso 1 1 calc R . . H6B H 0.2486 0.4205 0.1226 0.028 Uiso 1 1 calc R . . O7 O 0.05941(11) 0.61812(10) 0.21021(8) 0.0409(3) Uani 1 1 d . . . C7 C 0.08590(13) 0.54087(12) 0.14198(9) 0.0275(3) Uani 1 1 d . . . H7 H 0.0882 0.5924 0.0914 0.033 Uiso 1 1 calc R . . C7M C -0.0549(2) 0.6993(2) 0.19632(19) 0.0673(7) Uani 1 1 d . . . H7MA H -0.0663 0.7491 0.2455 0.101 Uiso 1 1 calc R . . H7MB H -0.1409 0.6529 0.1844 0.101 Uiso 1 1 calc R . . H7MC H -0.0361 0.7519 0.1495 0.101 Uiso 1 1 calc R . . C8 C -0.02906(13) 0.44446(13) 0.12812(9) 0.0305(3) Uani 1 1 d . . . H8 H -0.1194 0.4896 0.1192 0.037 Uiso 1 1 calc R . . C8M C -0.00801(19) 0.37137(17) 0.04977(10) 0.0423(4) Uani 1 1 d . . . H8MA H -0.0826 0.3106 0.0431 0.063 Uiso 1 1 calc R . . H8MB H 0.0833 0.3306 0.0537 0.063 Uiso 1 1 calc R . . H8MC H -0.0112 0.4261 0.0022 0.063 Uiso 1 1 calc R . . C9 C -0.04778(14) 0.36233(13) 0.20235(10) 0.0308(3) Uani 1 1 d . . . H9A H -0.0514 0.4124 0.2528 0.037 Uiso 1 1 calc R . . H9B H -0.1376 0.3178 0.1955 0.037 Uiso 1 1 calc R . . O9 O 0.06539(9) 0.27776(9) 0.21088(6) 0.02624(19) Uani 1 1 d . . . Si1 Si 0.06527(3) 0.15225(3) 0.26598(2) 0.02166(8) Uani 1 1 d . . . C10 C 0.22668(14) 0.06869(12) 0.23265(9) 0.0273(3) Uani 1 1 d . . . C11 C 0.35339(14) 0.15262(16) 0.24805(10) 0.0369(3) Uani 1 1 d . . . H11A H 0.4388 0.1115 0.2313 0.055 Uiso 1 1 calc R . . H11B H 0.3625 0.1728 0.3067 0.055 Uiso 1 1 calc R . . H11C H 0.3399 0.2273 0.2159 0.055 Uiso 1 1 calc R . . C12 C 0.21304(18) 0.03592(17) 0.14090(10) 0.0405(3) Uani 1 1 d . . . H12A H 0.2974 -0.0075 0.1250 0.061 Uiso 1 1 calc R . . H12B H 0.2023 0.1103 0.1082 0.061 Uiso 1 1 calc R . . H12C H 0.1307 -0.0160 0.1310 0.061 Uiso 1 1 calc R . . C13 C 0.24971(17) -0.04845(14) 0.28239(11) 0.0385(3) Uani 1 1 d . . . H13A H 0.3337 -0.0900 0.2640 0.058 Uiso 1 1 calc R . . H13B H 0.1680 -0.1016 0.2740 0.058 Uiso 1 1 calc R . . H13C H 0.2622 -0.0285 0.3409 0.058 Uiso 1 1 calc R . . C14 C 0.08595(14) 0.19037(13) 0.37820(8) 0.0276(3) Uani 1 1 d . . . C15 C 0.07687(15) 0.10410(15) 0.44092(9) 0.0325(3) Uani 1 1 d . . . H15 H 0.0538 0.0226 0.4271 0.039 Uiso 1 1 calc R . . C16 C 0.10113(17) 0.13551(19) 0.52360(10) 0.0421(4) Uani 1 1 d . . . H16 H 0.0928 0.0759 0.5653 0.051 Uiso 1 1 calc R . . C17 C 0.13718(19) 0.2532(2) 0.54452(10) 0.0470(4) Uani 1 1 d . . . H17 H 0.1542 0.2745 0.6006 0.056 Uiso 1 1 calc R . . C18 C 0.1484(2) 0.33951(18) 0.48409(12) 0.0460(4) Uani 1 1 d . . . H18 H 0.1739 0.4203 0.4986 0.055 Uiso 1 1 calc R . . C19 C 0.12259(17) 0.30924(14) 0.40152(10) 0.0356(3) Uani 1 1 d . . . H19 H 0.1299 0.3700 0.3605 0.043 Uiso 1 1 calc R . . C20 C -0.10088(13) 0.06688(12) 0.24043(8) 0.0240(2) Uani 1 1 d . . . C21 C -0.14664(15) 0.05472(13) 0.15749(8) 0.0294(3) Uani 1 1 d . . . H21 H -0.0946 0.0929 0.1162 0.035 Uiso 1 1 calc R . . C22 C -0.26540(16) -0.01134(14) 0.13430(9) 0.0318(3) Uani 1 1 d . . . H22 H -0.2941 -0.0177 0.0779 0.038 Uiso 1 1 calc R . . C23 C -0.34221(14) -0.06821(14) 0.19383(9) 0.0312(3) Uani 1 1 d . . . H23 H -0.4221 -0.1155 0.1781 0.037 Uiso 1 1 calc R . . C24 C -0.30235(15) -0.05590(14) 0.27577(9) 0.0325(3) Uani 1 1 d . . . H24 H -0.3559 -0.0936 0.3166 0.039 Uiso 1 1 calc R . . C25 C -0.18349(15) 0.01174(13) 0.29897(8) 0.0283(3) Uani 1 1 d . . . H25 H -0.1581 0.0205 0.3557 0.034 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 C1 0.0316(6) 0.0407(7) 0.0266(6) -0.0022(6) 0.0002(5) -0.0050(7) O1A 0.0533(7) 0.0364(6) 0.0370(6) -0.0071(5) 0.0042(5) -0.0009(5) C1A 0.0474(9) 0.0499(10) 0.0379(8) 0.0008(7) 0.0078(7) 0.0138(8) C1B 0.0668(12) 0.0706(13) 0.0306(8) 0.0098(9) 0.0020(8) 0.0223(11) O1B 0.0487(6) 0.0370(6) 0.0278(5) 0.0055(4) 0.0053(4) 0.0034(5) C2 0.0384(7) 0.0293(6) 0.0240(6) 0.0013(6) 0.0006(5) -0.0032(6) O3 0.0248(5) 0.0508(7) 0.0333(5) 0.0068(5) -0.0066(4) -0.0023(4) C3 0.0219(6) 0.0295(6) 0.0234(6) 0.0036(5) -0.0016(4) -0.0039(5) C3M 0.0373(8) 0.0632(11) 0.0378(8) 0.0122(8) 0.0011(6) 0.0173(8) C4 0.0188(5) 0.0264(6) 0.0227(6) 0.0018(5) -0.0003(4) -0.0037(5) C4M 0.0227(6) 0.0325(7) 0.0304(7) 0.0000(5) 0.0027(5) 0.0027(5) C5 0.0216(5) 0.0227(6) 0.0189(5) 0.0008(4) 0.0011(4) -0.0012(5) O5A 0.0285(4) 0.0259(4) 0.0196(4) 0.0008(3) -0.0012(3) -0.0044(4) C5A 0.0323(7) 0.0281(6) 0.0245(6) 0.0052(5) -0.0016(5) -0.0013(5) O5B 0.0373(5) 0.0334(5) 0.0297(5) 0.0012(4) 0.0024(4) -0.0113(4) C5B 0.0358(8) 0.0499(9) 0.0419(8) 0.0103(7) 0.0098(6) -0.0075(7) C6 0.0192(5) 0.0233(6) 0.0279(6) 0.0043(5) -0.0005(4) -0.0014(4) O7 0.0275(5) 0.0342(6) 0.0615(7) -0.0079(5) 0.0085(5) 0.0037(4) C7 0.0211(6) 0.0253(6) 0.0358(7) 0.0080(5) -0.0003(5) -0.0003(5) C7M 0.0373(10) 0.0400(10) 0.125(2) -0.0143(12) 0.0111(11) 0.0109(8) C8 0.0183(5) 0.0289(7) 0.0438(8) 0.0113(6) -0.0050(5) -0.0014(5) C8M 0.0415(8) 0.0480(9) 0.0361(8) 0.0063(7) -0.0141(6) -0.0138(7) C9 0.0222(6) 0.0265(6) 0.0443(8) 0.0093(6) 0.0069(5) 0.0013(5) O9 0.0217(4) 0.0231(4) 0.0341(5) 0.0070(4) 0.0041(3) 0.0010(4) Si1 0.02207(15) 0.01970(14) 0.02319(16) 0.00138(13) 0.00062(11) -0.00165(13) C10 0.0267(6) 0.0220(6) 0.0334(7) 0.0013(5) 0.0026(5) 0.0025(5) C11 0.0248(6) 0.0310(6) 0.0553(9) 0.0007(7) 0.0053(6) 0.0019(6) C12 0.0422(8) 0.0430(8) 0.0368(8) -0.0046(7) 0.0081(6) 0.0081(7) C13 0.0380(8) 0.0256(7) 0.0518(10) 0.0091(6) 0.0014(7) 0.0068(6) C14 0.0249(6) 0.0296(6) 0.0281(6) -0.0030(5) 0.0003(5) -0.0013(5) C15 0.0308(7) 0.0362(7) 0.0302(7) 0.0007(6) -0.0036(5) -0.0028(6) C16 0.0370(7) 0.0584(11) 0.0305(7) 0.0043(7) -0.0030(6) 0.0004(7) C17 0.0422(9) 0.0687(12) 0.0297(8) -0.0152(8) -0.0027(6) -0.0022(8) C18 0.0476(9) 0.0454(9) 0.0452(9) -0.0199(7) 0.0026(7) -0.0073(7) C19 0.0389(8) 0.0325(7) 0.0356(8) -0.0052(6) 0.0037(6) -0.0059(6) C20 0.0244(6) 0.0211(5) 0.0262(6) 0.0009(5) -0.0008(4) -0.0007(5) C21 0.0332(7) 0.0292(7) 0.0257(6) 0.0036(5) 0.0008(5) -0.0028(6) C22 0.0349(7) 0.0322(7) 0.0277(7) -0.0020(5) -0.0072(5) -0.0005(6) C23 0.0256(6) 0.0309(7) 0.0365(7) -0.0039(6) -0.0045(5) -0.0034(5) C24 0.0282(6) 0.0360(7) 0.0333(7) 0.0022(6) 0.0031(5) -0.0081(6) C25 0.0284(6) 0.0321(7) 0.0243(6) 0.0011(5) -0.0004(5) -0.0050(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1A 1.433(2) . ? C1 O1B 1.3867(19) . ? C1 C2 1.5182(18) . ? C1 H1 1.0000 . ? O1A C1A 1.425(2) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C1B O1B 1.429(2) . ? C1B H1BA 0.9800 . ? C1B H1BB 0.9800 . ? C1B H1BC 0.9800 . ? C2 C3 1.535(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 C3M 1.422(2) . ? O3 C3 1.4352(15) . ? C3 C4 1.5427(17) . ? C3 H3 1.0000 . ? C3M H3MA 0.9800 . ? C3M H3MB 0.9800 . ? C3M H3MC 0.9800 . ? C4 C4M 1.5302(19) . ? C4 C5 1.5426(17) . ? C4 H4 1.0000 . ? C4M H4MA 0.9800 . ? C4M H4MB 0.9800 . ? C4M H4MC 0.9800 . ? C5 O5A 1.4495(15) . ? C5 C6 1.5214(17) . ? C5 H5 1.0000 . ? O5A C5A 1.4012(16) . ? C5A O5B 1.3972(17) . ? C5A H5AA 0.9900 . ? C5A H5AB 0.9900 . ? O5B C5B 1.421(2) . ? C5B H5BA 0.9800 . ? C5B H5BB 0.9800 . ? C5B H5BC 0.9800 . ? C6 C7 1.5268(17) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O7 C7M 1.421(2) . ? O7 C7 1.4294(18) . ? C7 C8 1.5368(18) . ? C7 H7 1.0000 . ? C7M H7MA 0.9800 . ? C7M H7MB 0.9800 . ? C7M H7MC 0.9800 . ? C8 C9 1.5252(19) . ? C8 C8M 1.528(2) . ? C8 H8 1.0000 . ? C8M H8MA 0.9800 . ? C8M H8MB 0.9800 . ? C8M H8MC 0.9800 . ? C9 O9 1.4285(16) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? O9 Si1 1.6480(10) . ? Si1 C20 1.8750(13) . ? Si1 C14 1.8758(14) . ? Si1 C10 1.8919(14) . ? C10 C11 1.534(2) . ? C10 C13 1.5344(19) . ? C10 C12 1.536(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.400(2) . ? C14 C19 1.404(2) . ? C15 C16 1.399(2) . ? C15 H15 0.9500 . ? C16 C17 1.381(3) . ? C16 H16 0.9500 . ? C17 C18 1.375(3) . ? C17 H17 0.9500 . ? C18 C19 1.396(2) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.3993(18) . ? C20 C21 1.4074(19) . ? C21 C22 1.386(2) . ? C21 H21 0.9500 . ? C22 C23 1.387(2) . ? C22 H22 0.9500 . ? C23 C24 1.378(2) . ? C23 H23 0.9500 . ? C24 C25 1.3958(19) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? 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 O1B C1 O1A 111.47(11) . . ? O1B C1 C2 109.19(12) . . ? O1A C1 C2 111.59(13) . . ? O1B C1 H1 108.2 . . ? O1A C1 H1 108.2 . . ? C2 C1 H1 108.2 . . ? C1A O1A C1 114.86(13) . . ? O1A C1A H1AA 109.5 . . ? O1A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? O1A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? O1B C1B H1BA 109.5 . . ? O1B C1B H1BB 109.5 . . ? H1BA C1B H1BB 109.5 . . ? O1B C1B H1BC 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? C1 O1B C1B 111.71(15) . . ? C1 C2 C3 114.18(12) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C3M O3 C3 113.68(12) . . ? O3 C3 C2 110.19(11) . . ? O3 C3 C4 107.67(10) . . ? C2 C3 C4 111.72(11) . . ? O3 C3 H3 109.1 . . ? C2 C3 H3 109.1 . . ? C4 C3 H3 109.1 . . ? O3 C3M H3MA 109.5 . . ? O3 C3M H3MB 109.5 . . ? H3MA C3M H3MB 109.5 . . ? O3 C3M H3MC 109.5 . . ? H3MA C3M H3MC 109.5 . . ? H3MB C3M H3MC 109.5 . . ? C4M C4 C5 111.64(10) . . ? C4M C4 C3 111.10(11) . . ? C5 C4 C3 112.60(10) . . ? C4M C4 H4 107.0 . . ? C5 C4 H4 107.0 . . ? C3 C4 H4 107.0 . . ? C4 C4M H4MA 109.5 . . ? C4 C4M H4MB 109.5 . . ? H4MA C4M H4MB 109.5 . . ? C4 C4M H4MC 109.5 . . ? H4MA C4M H4MC 109.5 . . ? H4MB C4M H4MC 109.5 . . ? O5A C5 C6 105.99(10) . . ? O5A C5 C4 109.95(9) . . ? C6 C5 C4 114.13(10) . . ? O5A C5 H5 108.9 . . ? C6 C5 H5 108.9 . . ? C4 C5 H5 108.9 . . ? C5A O5A C5 115.39(10) . . ? O5B C5A O5A 114.17(11) . . ? O5B C5A H5AA 108.7 . . ? O5A C5A H5AA 108.7 . . ? O5B C5A H5AB 108.7 . . ? O5A C5A H5AB 108.7 . . ? H5AA C5A H5AB 107.6 . . ? C5A O5B C5B 113.10(12) . . ? O5B C5B H5BA 109.5 . . ? O5B C5B H5BB 109.5 . . ? H5BA C5B H5BB 109.5 . . ? O5B C5B H5BC 109.5 . . ? H5BA C5B H5BC 109.5 . . ? H5BB C5B H5BC 109.5 . . ? C5 C6 C7 112.15(10) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C7M O7 C7 114.21(15) . . ? O7 C7 C6 105.19(11) . . ? O7 C7 C8 112.22(11) . . ? C6 C7 C8 114.81(11) . . ? O7 C7 H7 108.1 . . ? C6 C7 H7 108.1 . . ? C8 C7 H7 108.1 . . ? O7 C7M H7MA 109.5 . . ? O7 C7M H7MB 109.5 . . ? H7MA C7M H7MB 109.5 . . ? O7 C7M H7MC 109.5 . . ? H7MA C7M H7MC 109.5 . . ? H7MB C7M H7MC 109.5 . . ? C9 C8 C8M 111.79(13) . . ? C9 C8 C7 113.56(12) . . ? C8M C8 C7 111.70(12) . . ? C9 C8 H8 106.4 . . ? C8M C8 H8 106.4 . . ? C7 C8 H8 106.4 . . ? C8 C8M H8MA 109.5 . . ? C8 C8M H8MB 109.5 . . ? H8MA C8M H8MB 109.5 . . ? C8 C8M H8MC 109.5 . . ? H8MA C8M H8MC 109.5 . . ? H8MB C8M H8MC 109.5 . . ? O9 C9 C8 110.60(11) . . ? O9 C9 H9A 109.5 . . ? C8 C9 H9A 109.5 . . ? O9 C9 H9B 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C9 O9 Si1 125.67(8) . . ? O9 Si1 C20 108.65(5) . . ? O9 Si1 C14 109.82(6) . . ? C20 Si1 C14 112.50(6) . . ? O9 Si1 C10 103.54(5) . . ? C20 Si1 C10 112.48(6) . . ? C14 Si1 C10 109.46(6) . . ? C11 C10 C13 109.03(12) . . ? C11 C10 C12 109.60(12) . . ? C13 C10 C12 108.62(13) . . ? C11 C10 Si1 107.73(9) . . ? C13 C10 Si1 111.05(10) . . ? C12 C10 Si1 110.79(10) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 117.31(13) . . ? C15 C14 Si1 123.38(11) . . ? C19 C14 Si1 119.15(11) . . ? C16 C15 C14 121.34(16) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C15 119.95(16) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 119.95(15) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.44(17) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C14 121.01(15) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? C25 C20 C21 116.73(12) . . ? C25 C20 Si1 124.13(10) . . ? C21 C20 Si1 119.13(10) . . ? C22 C21 C20 121.95(13) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 119.75(13) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 119.86(13) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 120.22(13) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C20 121.42(13) . . ? C24 C25 H25 119.3 . . ? C20 C25 H25 119.3 . . ? 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 O1B C1 O1A C1A -49.81(16) . . . . ? C2 C1 O1A C1A 72.57(16) . . . . ? O1A C1 O1B C1B -69.25(16) . . . . ? C2 C1 O1B C1B 167.00(13) . . . . ? O1B C1 C2 C3 -53.59(15) . . . . ? O1A C1 C2 C3 -177.27(12) . . . . ? C3M O3 C3 C2 119.14(14) . . . . ? C3M O3 C3 C4 -118.79(13) . . . . ? C1 C2 C3 O3 -46.15(15) . . . . ? C1 C2 C3 C4 -165.79(11) . . . . ? O3 C3 C4 C4M 62.06(14) . . . . ? C2 C3 C4 C4M -176.82(11) . . . . ? O3 C3 C4 C5 -171.87(11) . . . . ? C2 C3 C4 C5 -50.75(14) . . . . ? C4M C4 C5 O5A -56.66(13) . . . . ? C3 C4 C5 O5A 177.56(10) . . . . ? C4M C4 C5 C6 62.27(13) . . . . ? C3 C4 C5 C6 -63.50(14) . . . . ? C6 C5 O5A C5A 138.30(11) . . . . ? C4 C5 O5A C5A -97.89(12) . . . . ? C5 O5A C5A O5B 71.58(14) . . . . ? O5A C5A O5B C5B 65.75(15) . . . . ? O5A C5 C6 C7 -72.78(13) . . . . ? C4 C5 C6 C7 166.06(11) . . . . ? C7M O7 C7 C6 163.96(14) . . . . ? C7M O7 C7 C8 -70.55(17) . . . . ? C5 C6 C7 O7 -73.24(13) . . . . ? C5 C6 C7 C8 162.90(11) . . . . ? O7 C7 C8 C9 -58.57(15) . . . . ? C6 C7 C8 C9 61.47(16) . . . . ? O7 C7 C8 C8M 173.89(12) . . . . ? C6 C7 C8 C8M -66.07(16) . . . . ? C8M C8 C9 O9 53.44(16) . . . . ? C7 C8 C9 O9 -74.06(16) . . . . ? C8 C9 O9 Si1 -162.69(9) . . . . ? C9 O9 Si1 C20 48.60(13) . . . . ? C9 O9 Si1 C14 -74.83(12) . . . . ? C9 O9 Si1 C10 168.36(11) . . . . ? O9 Si1 C10 C11 56.85(11) . . . . ? C20 Si1 C10 C11 173.96(9) . . . . ? C14 Si1 C10 C11 -60.20(11) . . . . ? O9 Si1 C10 C13 176.18(10) . . . . ? C20 Si1 C10 C13 -66.72(12) . . . . ? C14 Si1 C10 C13 59.12(12) . . . . ? O9 Si1 C10 C12 -63.01(11) . . . . ? C20 Si1 C10 C12 54.09(12) . . . . ? C14 Si1 C10 C12 179.93(11) . . . . ? O9 Si1 C14 C15 173.94(11) . . . . ? C20 Si1 C14 C15 52.80(13) . . . . ? C10 Si1 C14 C15 -73.02(13) . . . . ? O9 Si1 C14 C19 -10.92(13) . . . . ? C20 Si1 C14 C19 -132.06(12) . . . . ? C10 Si1 C14 C19 102.11(12) . . . . ? C19 C14 C15 C16 1.0(2) . . . . ? Si1 C14 C15 C16 176.21(12) . . . . ? C14 C15 C16 C17 -1.1(2) . . . . ? C15 C16 C17 C18 0.4(3) . . . . ? C16 C17 C18 C19 0.5(3) . . . . ? C17 C18 C19 C14 -0.6(3) . . . . ? C15 C14 C19 C18 -0.2(2) . . . . ? Si1 C14 C19 C18 -175.58(13) . . . . ? O9 Si1 C20 C25 -136.41(12) . . . . ? C14 Si1 C20 C25 -14.60(14) . . . . ? C10 Si1 C20 C25 109.57(13) . . . . ? O9 Si1 C20 C21 44.53(12) . . . . ? C14 Si1 C20 C21 166.34(11) . . . . ? C10 Si1 C20 C21 -69.49(12) . . . . ? C25 C20 C21 C22 -1.8(2) . . . . ? Si1 C20 C21 C22 177.37(11) . . . . ? C20 C21 C22 C23 -0.3(2) . . . . ? C21 C22 C23 C24 1.8(2) . . . . ? C22 C23 C24 C25 -1.2(2) . . . . ? C23 C24 C25 C20 -1.0(2) . . . . ? C21 C20 C25 C24 2.4(2) . . . . ? Si1 C20 C25 C24 -176.67(11) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.38 _refine_diff_density_min -0.16 _refine_diff_density_rms 0.04 #===END of CIF