data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name C.Krempner _publ_contact_author_name 'Krempner, Clemens' _publ_contact_author_email clemens.krempner@ttu.edu # Attachment '- X-ray data.txt' data_w14oh _database_code_depnum_ccdc_archive 'CCDC 778866' #TrackingRef '- X-ray data.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3,6-Dihydroxy-1,1,1,2,7,8,8,8-octamethyl-3,6-bis(1',2',2',2'- tetramethyl-1'-trimethylsilyl-disilanyl)-2,7-bis(trimethylsilyl)- 1,2,3,6,7,8-hexasilaoctane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H90 O2 Si14' _chemical_formula_weight 876.28 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 Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2513(6) _cell_length_b 12.3844(7) _cell_length_c 12.7960(7) _cell_angle_alpha 83.126(2) _cell_angle_beta 73.021(2) _cell_angle_gamma 66.837(3) _cell_volume 1428.45(14) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9349 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 30.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.019 _exptl_crystal_density_method ? _exptl_crystal_F_000 482 _exptl_absorpt_coefficient_mu 0.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8288 _exptl_absorpt_correction_T_max 0.9576 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker X8Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29353 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0385 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6149 _reflns_number_gt 4607 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0421P)^2^+1.6255P] 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_number_reflns 6149 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1256 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.023 _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 0.78272(7) 0.62789(6) 0.10588(6) 0.02589(16) Uani 1 1 d . . . Si2 Si 0.71873(7) 0.50423(6) 0.24947(6) 0.02582(16) Uani 1 1 d . . . Si3 Si 0.59874(8) 0.39834(6) 0.20099(6) 0.03072(18) Uani 1 1 d . . . Si4 Si 0.91060(8) 0.37831(7) 0.32570(7) 0.03449(19) Uani 1 1 d . . . Si5 Si 0.73141(7) 0.81780(6) 0.16458(6) 0.02720(17) Uani 1 1 d . . . Si6 Si 0.84841(8) 0.82801(7) 0.29363(7) 0.03367(19) Uani 1 1 d . . . Si7 Si 0.47666(8) 0.93237(7) 0.22280(7) 0.03410(19) Uani 1 1 d . . . O1 O 0.6862(2) 0.64421(17) 0.01418(17) 0.0400(5) Uani 1 1 d . . . H1 H 0.6398 0.7160 0.0050 0.060 Uiso 1 1 calc R . . C1 C 0.9802(3) 0.5603(2) 0.0245(2) 0.0305(6) Uani 1 1 d . . . H1A H 1.0005 0.6146 -0.0356 0.037 Uiso 1 1 calc R . . H1B H 1.0446 0.5508 0.0722 0.037 Uiso 1 1 calc R . . C2 C 0.5703(3) 0.6047(2) 0.3631(2) 0.0353(6) Uani 1 1 d . . . H2A H 0.4858 0.6544 0.3355 0.053 Uiso 1 1 calc R . . H2B H 0.6100 0.6543 0.3877 0.053 Uiso 1 1 calc R . . H2C H 0.5388 0.5570 0.4245 0.053 Uiso 1 1 calc R . . C3 C 0.4310(3) 0.5056(3) 0.1621(3) 0.0509(8) Uani 1 1 d . . . H3A H 0.4610 0.5500 0.0972 0.076 Uiso 1 1 calc R . . H3B H 0.3681 0.5599 0.2226 0.076 Uiso 1 1 calc R . . H3C H 0.3764 0.4630 0.1461 0.076 Uiso 1 1 calc R . . C4 C 0.5337(4) 0.3159(3) 0.3248(3) 0.0470(8) Uani 1 1 d . . . H4A H 0.4816 0.2724 0.3063 0.071 Uiso 1 1 calc R . . H4B H 0.4670 0.3715 0.3835 0.071 Uiso 1 1 calc R . . H4C H 0.6187 0.2607 0.3490 0.071 Uiso 1 1 calc R . . C5 C 0.7175(4) 0.2930(3) 0.0861(3) 0.0467(8) Uani 1 1 d . . . H5A H 0.6596 0.2549 0.0675 0.070 Uiso 1 1 calc R . . H5B H 0.8012 0.2332 0.1085 0.070 Uiso 1 1 calc R . . H5C H 0.7537 0.3356 0.0221 0.070 Uiso 1 1 calc R . . C6 C 0.8298(4) 0.3765(5) 0.4757(3) 0.0854(16) Uani 1 1 d . . . H6A H 0.9067 0.3269 0.5108 0.128 Uiso 1 1 calc R . . H6B H 0.7520 0.3450 0.4916 0.128 Uiso 1 1 calc R . . H6C H 0.7880 0.4567 0.5040 0.128 Uiso 1 1 calc R . . C7 C 0.9849(4) 0.2253(3) 0.2730(4) 0.0668(11) Uani 1 1 d . . . H7A H 1.0631 0.1749 0.3065 0.100 Uiso 1 1 calc R . . H7B H 1.0250 0.2256 0.1934 0.100 Uiso 1 1 calc R . . H7C H 0.9055 0.1953 0.2913 0.100 Uiso 1 1 calc R . . C8 C 1.0715(4) 0.4232(3) 0.2985(3) 0.0568(9) Uani 1 1 d . . . H8A H 1.0378 0.5030 0.3256 0.085 Uiso 1 1 calc R . . H8B H 1.1179 0.4213 0.2197 0.085 Uiso 1 1 calc R . . H8C H 1.1431 0.3689 0.3359 0.085 Uiso 1 1 calc R . . C9 C 0.8117(3) 0.8939(3) 0.0384(3) 0.0409(7) Uani 1 1 d . . . H9A H 0.7908 0.9747 0.0567 0.061 Uiso 1 1 calc R . . H9B H 0.7671 0.8948 -0.0200 0.061 Uiso 1 1 calc R . . H9C H 0.9185 0.8512 0.0136 0.061 Uiso 1 1 calc R . . C10 C 0.7909(3) 0.7622(3) 0.4306(3) 0.0448(7) Uani 1 1 d . . . H10A H 0.8194 0.6776 0.4228 0.067 Uiso 1 1 calc R . . H10B H 0.6838 0.7991 0.4599 0.067 Uiso 1 1 calc R . . H10C H 0.8393 0.7756 0.4806 0.067 Uiso 1 1 calc R . . C11 C 1.0529(3) 0.7555(3) 0.2363(3) 0.0537(9) Uani 1 1 d . . . H11A H 1.0836 0.7927 0.1665 0.081 Uiso 1 1 calc R . . H11B H 1.0792 0.6719 0.2247 0.081 Uiso 1 1 calc R . . H11C H 1.1027 0.7641 0.2877 0.081 Uiso 1 1 calc R . . C12 C 0.8029(5) 0.9870(3) 0.3148(3) 0.0620(10) Uani 1 1 d . . . H12A H 0.8546 0.9944 0.3653 0.093 Uiso 1 1 calc R . . H12B H 0.6964 1.0264 0.3455 0.093 Uiso 1 1 calc R . . H12C H 0.8337 1.0235 0.2446 0.093 Uiso 1 1 calc R . . C13 C 0.4483(4) 1.0836(3) 0.1632(3) 0.0510(9) Uani 1 1 d . . . H13A H 0.3444 1.1348 0.1890 0.077 Uiso 1 1 calc R . . H13B H 0.4767 1.0792 0.0832 0.077 Uiso 1 1 calc R . . H13C H 0.5092 1.1154 0.1862 0.077 Uiso 1 1 calc R . . C14 C 0.4050(4) 0.9472(3) 0.3747(3) 0.0589(10) Uani 1 1 d . . . H14A H 0.2997 0.9962 0.3940 0.088 Uiso 1 1 calc R . . H14B H 0.4580 0.9839 0.4017 0.088 Uiso 1 1 calc R . . H14C H 0.4200 0.8693 0.4081 0.088 Uiso 1 1 calc R . . C15 C 0.3616(3) 0.8737(3) 0.1744(3) 0.0499(8) Uani 1 1 d . . . H15A H 0.3705 0.7965 0.2077 0.075 Uiso 1 1 calc R . . H15B H 0.3959 0.8661 0.0946 0.075 Uiso 1 1 calc R . . H15C H 0.2584 0.9277 0.1954 0.075 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 0.0264(3) 0.0253(3) 0.0244(4) -0.0054(3) -0.0023(3) -0.0099(3) Si2 0.0250(3) 0.0277(3) 0.0258(4) -0.0030(3) -0.0045(3) -0.0120(3) Si3 0.0303(4) 0.0337(4) 0.0317(4) -0.0056(3) -0.0053(3) -0.0163(3) Si4 0.0282(4) 0.0400(4) 0.0354(5) 0.0037(3) -0.0097(3) -0.0132(3) Si5 0.0263(3) 0.0251(3) 0.0290(4) -0.0059(3) -0.0045(3) -0.0089(3) Si6 0.0368(4) 0.0321(4) 0.0374(5) -0.0042(3) -0.0122(3) -0.0158(3) Si7 0.0283(4) 0.0308(4) 0.0389(5) -0.0074(3) -0.0059(3) -0.0069(3) O1 0.0494(12) 0.0352(10) 0.0390(13) -0.0047(9) -0.0179(10) -0.0142(9) C1 0.0318(13) 0.0260(13) 0.0295(15) -0.0047(10) 0.0021(10) -0.0127(11) C2 0.0361(14) 0.0357(14) 0.0292(16) -0.0066(11) 0.0017(11) -0.0141(12) C3 0.0407(17) 0.056(2) 0.066(3) -0.0036(16) -0.0242(16) -0.0208(15) C4 0.0553(19) 0.0453(17) 0.045(2) -0.0057(14) -0.0017(15) -0.0308(15) C5 0.0502(18) 0.0532(19) 0.039(2) -0.0164(14) -0.0012(14) -0.0255(15) C6 0.043(2) 0.139(4) 0.043(3) 0.024(2) -0.0137(17) -0.007(2) C7 0.060(2) 0.0352(18) 0.105(4) -0.0004(19) -0.037(2) -0.0066(16) C8 0.0412(18) 0.063(2) 0.078(3) 0.0084(19) -0.0277(18) -0.0265(16) C9 0.0405(16) 0.0396(16) 0.0388(19) 0.0008(12) -0.0054(13) -0.0152(13) C10 0.0457(17) 0.0499(18) 0.043(2) 0.0018(14) -0.0168(14) -0.0198(14) C11 0.0396(17) 0.073(2) 0.056(2) 0.0004(17) -0.0133(15) -0.0289(17) C12 0.090(3) 0.0453(19) 0.067(3) -0.0094(17) -0.027(2) -0.0356(19) C13 0.0425(17) 0.0279(15) 0.079(3) -0.0039(15) -0.0158(16) -0.0089(13) C14 0.0449(19) 0.062(2) 0.045(2) -0.0166(17) 0.0000(15) 0.0006(16) C15 0.0377(16) 0.0461(18) 0.071(3) 0.0006(16) -0.0185(16) -0.0186(14) _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 1.691(2) . ? Si1 C1 1.878(3) . ? Si1 Si2 2.3589(10) . ? Si1 Si5 2.3645(9) . ? Si2 C2 1.905(3) . ? Si2 Si3 2.3510(9) . ? Si2 Si4 2.3654(10) . ? Si3 C5 1.874(3) . ? Si3 C3 1.874(3) . ? Si3 C4 1.878(3) . ? Si4 C6 1.857(4) . ? Si4 C8 1.868(3) . ? Si4 C7 1.869(4) . ? Si5 C9 1.909(3) . ? Si5 Si6 2.3468(10) . ? Si5 Si7 2.3643(10) . ? Si6 C12 1.871(3) . ? Si6 C10 1.875(3) . ? Si6 C11 1.875(3) . ? Si7 C14 1.870(4) . ? Si7 C15 1.874(3) . ? Si7 C13 1.879(3) . ? O1 H1 0.8400 . ? C1 C1 1.546(5) 2_765 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? 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 C1 103.92(12) . . ? O1 Si1 Si2 109.31(8) . . ? C1 Si1 Si2 112.16(9) . . ? O1 Si1 Si5 107.34(7) . . ? C1 Si1 Si5 110.19(8) . . ? Si2 Si1 Si5 113.38(4) . . ? C2 Si2 Si3 103.51(9) . . ? C2 Si2 Si1 106.44(9) . . ? Si3 Si2 Si1 111.57(4) . . ? C2 Si2 Si4 107.34(10) . . ? Si3 Si2 Si4 110.90(4) . . ? Si1 Si2 Si4 116.09(4) . . ? C5 Si3 C3 109.46(16) . . ? C5 Si3 C4 109.46(15) . . ? C3 Si3 C4 107.23(16) . . ? C5 Si3 Si2 113.62(10) . . ? C3 Si3 Si2 108.47(10) . . ? C4 Si3 Si2 108.39(11) . . ? C6 Si4 C8 108.6(2) . . ? C6 Si4 C7 108.8(2) . . ? C8 Si4 C7 106.53(18) . . ? C6 Si4 Si2 106.87(12) . . ? C8 Si4 Si2 114.82(12) . . ? C7 Si4 Si2 111.14(13) . . ? C9 Si5 Si6 103.96(10) . . ? C9 Si5 Si7 106.80(10) . . ? Si6 Si5 Si7 109.92(4) . . ? C9 Si5 Si1 105.36(10) . . ? Si6 Si5 Si1 116.50(4) . . ? Si7 Si5 Si1 113.30(4) . . ? C12 Si6 C10 107.61(17) . . ? C12 Si6 C11 108.14(18) . . ? C10 Si6 C11 109.47(16) . . ? C12 Si6 Si5 107.29(13) . . ? C10 Si6 Si5 115.07(10) . . ? C11 Si6 Si5 109.03(12) . . ? C14 Si7 C15 107.73(18) . . ? C14 Si7 C13 107.73(17) . . ? C15 Si7 C13 108.00(16) . . ? C14 Si7 Si5 113.06(11) . . ? C15 Si7 Si5 112.85(11) . . ? C13 Si7 Si5 107.24(11) . . ? Si1 O1 H1 109.5 . . ? C1 C1 Si1 113.4(2) 2_765 . ? C1 C1 H1A 108.9 2_765 . ? Si1 C1 H1A 108.9 . . ? C1 C1 H1B 108.9 2_765 . ? Si1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? Si2 C2 H2A 109.5 . . ? Si2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si3 C3 H3A 109.5 . . ? Si3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si3 C4 H4A 109.5 . . ? Si3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si3 C5 H5A 109.5 . . ? Si3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si4 C6 H6A 109.5 . . ? Si4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si4 C7 H7A 109.5 . . ? Si4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si4 C8 H8A 109.5 . . ? Si4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si5 C9 H9A 109.5 . . ? Si5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si6 C10 H10A 109.5 . . ? Si6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si6 C11 H11A 109.5 . . ? Si6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si6 C12 H12A 109.5 . . ? Si6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si7 C13 H13A 109.5 . . ? Si7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si7 C14 H14A 109.5 . . ? Si7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si7 C15 H15A 109.5 . . ? Si7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 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 O1 Si1 Si2 C2 -95.73(12) . . . . ? C1 Si1 Si2 C2 149.56(13) . . . . ? Si5 Si1 Si2 C2 23.97(10) . . . . ? O1 Si1 Si2 Si3 16.52(9) . . . . ? C1 Si1 Si2 Si3 -98.19(10) . . . . ? Si5 Si1 Si2 Si3 136.21(4) . . . . ? O1 Si1 Si2 Si4 144.89(8) . . . . ? C1 Si1 Si2 Si4 30.18(10) . . . . ? Si5 Si1 Si2 Si4 -95.41(5) . . . . ? C2 Si2 Si3 C5 178.41(16) . . . . ? Si1 Si2 Si3 C5 64.33(14) . . . . ? Si4 Si2 Si3 C5 -66.76(14) . . . . ? C2 Si2 Si3 C3 56.43(16) . . . . ? Si1 Si2 Si3 C3 -57.65(14) . . . . ? Si4 Si2 Si3 C3 171.26(13) . . . . ? C2 Si2 Si3 C4 -59.68(15) . . . . ? Si1 Si2 Si3 C4 -173.76(11) . . . . ? Si4 Si2 Si3 C4 55.15(12) . . . . ? C2 Si2 Si4 C6 21.1(2) . . . . ? Si3 Si2 Si4 C6 -91.3(2) . . . . ? Si1 Si2 Si4 C6 139.9(2) . . . . ? C2 Si2 Si4 C8 -99.41(17) . . . . ? Si3 Si2 Si4 C8 148.18(15) . . . . ? Si1 Si2 Si4 C8 19.48(15) . . . . ? C2 Si2 Si4 C7 139.59(18) . . . . ? Si3 Si2 Si4 C7 27.19(16) . . . . ? Si1 Si2 Si4 C7 -101.51(16) . . . . ? O1 Si1 Si5 C9 -65.39(13) . . . . ? C1 Si1 Si5 C9 47.14(14) . . . . ? Si2 Si1 Si5 C9 173.79(10) . . . . ? O1 Si1 Si5 Si6 179.99(9) . . . . ? C1 Si1 Si5 Si6 -67.48(11) . . . . ? Si2 Si1 Si5 Si6 59.17(5) . . . . ? O1 Si1 Si5 Si7 51.00(10) . . . . ? C1 Si1 Si5 Si7 163.54(10) . . . . ? Si2 Si1 Si5 Si7 -69.81(5) . . . . ? C9 Si5 Si6 C12 59.28(17) . . . . ? Si7 Si5 Si6 C12 -54.73(15) . . . . ? Si1 Si5 Si6 C12 174.68(14) . . . . ? C9 Si5 Si6 C10 178.97(14) . . . . ? Si7 Si5 Si6 C10 64.96(12) . . . . ? Si1 Si5 Si6 C10 -65.63(12) . . . . ? C9 Si5 Si6 C11 -57.62(16) . . . . ? Si7 Si5 Si6 C11 -171.62(13) . . . . ? Si1 Si5 Si6 C11 57.79(13) . . . . ? C9 Si5 Si7 C14 -139.24(18) . . . . ? Si6 Si5 Si7 C14 -27.06(15) . . . . ? Si1 Si5 Si7 C14 105.21(15) . . . . ? C9 Si5 Si7 C15 98.17(16) . . . . ? Si6 Si5 Si7 C15 -149.65(13) . . . . ? Si1 Si5 Si7 C15 -17.38(14) . . . . ? C9 Si5 Si7 C13 -20.64(17) . . . . ? Si6 Si5 Si7 C13 91.54(13) . . . . ? Si1 Si5 Si7 C13 -136.19(13) . . . . ? O1 Si1 C1 C1 -60.9(3) . . . 2_765 ? Si2 Si1 C1 C1 57.1(3) . . . 2_765 ? Si5 Si1 C1 C1 -175.6(2) . . . 2_765 ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.528 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.069 #====================================================================== #===END #====================================================================== data_w313w _database_code_depnum_ccdc_archive 'CCDC 778867' #TrackingRef '- X-ray data.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2-Methyl-4,4,7,7-tetrakis(1',2',2',2'-tetramethyl-1'-trimethylsilyl- disilanyl)-2-alumina-1,3-dioxa-4,7-disilacycloheptane-tetrahydrofuranate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H97 Al O3 Si14' _chemical_formula_weight 986.37 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' Al Al 0.0645 0.0514 '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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5376(4) _cell_length_b 14.6049(4) _cell_length_c 19.3483(5) _cell_angle_alpha 100.673(2) _cell_angle_beta 92.987(2) _cell_angle_gamma 107.5350(10) _cell_volume 3297.72(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8767 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 36.47 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.993 _exptl_crystal_density_method ? _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.311 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7934 _exptl_absorpt_correction_T_max 0.9461 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90530 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15009 _reflns_number_gt 12819 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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. The crystal contains pentane near the centre of inversion. However, the atom positions of the solvent could not be properly refined since there is no centre of inversion in pentane. That's why the hkl was squeezed using the Platon programme facilities. However, even when the solvent atoms were included in the refinement calculation assuming disordered positions for the carbon chain atoms the values for R went down to 0.0327 (gt) and 0.0413 (all), which is not so far from the final results for the refinement without pentane (R1=0.0314 and 0.0377, respectively) . So squeezing is not considered to have caused too many errors here. ; _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^)+(0.0546P)^2^+0.6177P] 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_number_reflns 15009 _refine_ls_number_parameters 507 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0894 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.002 _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 Al1 Al 0.08551(3) 0.29861(3) 0.65120(2) 0.02441(9) Uani 1 1 d . . . Si1 Si 0.23231(3) 0.19922(2) 0.728886(17) 0.02060(8) Uani 1 1 d . . . Si2 Si 0.10160(3) 0.12528(3) 0.803159(19) 0.02452(8) Uani 1 1 d . . . Si3 Si 0.17845(4) 0.11443(3) 0.91412(2) 0.03651(10) Uani 1 1 d . . . Si4 Si -0.03220(3) -0.02806(3) 0.75232(2) 0.03364(9) Uani 1 1 d . . . Si5 Si 0.34623(3) 0.10114(3) 0.687659(19) 0.02412(8) Uani 1 1 d . . . Si6 Si 0.54297(3) 0.17849(3) 0.70456(2) 0.03267(9) Uani 1 1 d . . . Si7 Si 0.29059(3) 0.02951(3) 0.56708(2) 0.03154(9) Uani 1 1 d . . . Si8 Si 0.25094(3) 0.48128(2) 0.760984(17) 0.02072(8) Uani 1 1 d . . . Si9 Si 0.19642(3) 0.60083(3) 0.838345(18) 0.02469(8) Uani 1 1 d . . . Si10 Si 0.00287(3) 0.56784(3) 0.808199(19) 0.02789(8) Uani 1 1 d . . . Si11 Si 0.23298(3) 0.60131(3) 0.95914(2) 0.03448(10) Uani 1 1 d . . . Si12 Si 0.40550(3) 0.54706(3) 0.699591(19) 0.02540(8) Uani 1 1 d . . . Si13 Si 0.58096(3) 0.60790(3) 0.76962(2) 0.03328(9) Uani 1 1 d . . . Si14 Si 0.39061(4) 0.66871(3) 0.63763(2) 0.03827(10) Uani 1 1 d . . . O1 O 0.15932(8) 0.21972(7) 0.66415(5) 0.02625(19) Uani 1 1 d . . . O2 O 0.14499(8) 0.41521(7) 0.70155(5) 0.02660(19) Uani 1 1 d . . . O3 O 0.12110(11) 0.32027(9) 0.56006(5) 0.0436(3) Uani 1 1 d . . . C1 C -0.07872(13) 0.25016(13) 0.63738(10) 0.0471(4) Uani 1 1 d . . . H1A H -0.1041 0.1864 0.6041 0.071 Uiso 1 1 calc R . . H1B H -0.1071 0.2971 0.6183 0.071 Uiso 1 1 calc R . . H1C H -0.1074 0.2426 0.6829 0.071 Uiso 1 1 calc R . . C2 C 0.33498(11) 0.31799(9) 0.78187(7) 0.0241(2) Uani 1 1 d . . . H2A H 0.3771 0.3012 0.8197 0.029 Uiso 1 1 calc R . . H2B H 0.3900 0.3451 0.7501 0.029 Uiso 1 1 calc R . . C3 C 0.29152(11) 0.40156(9) 0.81720(6) 0.0247(3) Uani 1 1 d . . . H3A H 0.3504 0.4453 0.8553 0.030 Uiso 1 1 calc R . . H3B H 0.2249 0.3717 0.8403 0.030 Uiso 1 1 calc R . . C4 C 0.1378(2) 0.25090(15) 0.50267(10) 0.0650(6) Uani 1 1 d . . . H4A H 0.0701 0.1920 0.4896 0.078 Uiso 1 1 calc R . . H4B H 0.2031 0.2302 0.5155 0.078 Uiso 1 1 calc R . . C5 C 0.1580(5) 0.3013(3) 0.44527(14) 0.166(2) Uani 1 1 d . . . H5 H 0.1908 0.2815 0.4043 0.200 Uiso 1 1 calc R . . C6 C 0.1211(4) 0.3856(3) 0.45939(15) 0.1421(17) Uani 1 1 d . . . H6 H 0.1109 0.4241 0.4266 0.171 Uiso 1 1 calc R . . C7 C 0.1020(4) 0.4016(3) 0.53387(13) 0.1184(14) Uani 1 1 d . . . H7A H 0.1550 0.4649 0.5605 0.142 Uiso 1 1 calc R . . H7B H 0.0240 0.4023 0.5387 0.142 Uiso 1 1 calc R . . C8 C 0.00833(14) 0.20692(12) 0.82393(10) 0.0428(4) Uani 1 1 d . . . H8A H -0.0499 0.1771 0.8522 0.064 Uiso 1 1 calc R . . H8B H -0.0273 0.2134 0.7796 0.064 Uiso 1 1 calc R . . H8C H 0.0545 0.2720 0.8506 0.064 Uiso 1 1 calc R . . C9 C 0.32788(14) 0.00131(12) 0.74083(9) 0.0398(3) Uani 1 1 d . . . H9A H 0.2478 -0.0361 0.7375 0.060 Uiso 1 1 calc R . . H9B H 0.3568 0.0315 0.7905 0.060 Uiso 1 1 calc R . . H9C H 0.3696 -0.0429 0.7219 0.060 Uiso 1 1 calc R . . C10 C 0.32434(18) 0.20182(17) 0.94102(10) 0.0663(6) Uani 1 1 d . . . H10A H 0.3510 0.1978 0.9886 0.099 Uiso 1 1 calc R . . H10B H 0.3240 0.2689 0.9412 0.099 Uiso 1 1 calc R . . H10C H 0.3745 0.1846 0.9074 0.099 Uiso 1 1 calc R . . C11 C 0.0873(2) 0.14730(19) 0.98165(10) 0.0710(6) Uani 1 1 d . . . H11A H 0.0103 0.1020 0.9690 0.107 Uiso 1 1 calc R . . H11B H 0.0872 0.2147 0.9831 0.107 Uiso 1 1 calc R . . H11C H 0.1167 0.1424 1.0283 0.107 Uiso 1 1 calc R . . C12 C 0.18229(18) -0.01218(15) 0.91746(10) 0.0545(5) Uani 1 1 d . . . H12A H 0.2322 -0.0304 0.8840 0.082 Uiso 1 1 calc R . . H12B H 0.1062 -0.0592 0.9047 0.082 Uiso 1 1 calc R . . H12C H 0.2104 -0.0131 0.9655 0.082 Uiso 1 1 calc R . . C13 C -0.13271(18) -0.05957(17) 0.81917(12) 0.0678(6) Uani 1 1 d . . . H13A H -0.1627 -0.0053 0.8342 0.102 Uiso 1 1 calc R . . H13B H -0.0932 -0.0706 0.8603 0.102 Uiso 1 1 calc R . . H13C H -0.1948 -0.1193 0.7980 0.102 Uiso 1 1 calc R . . C14 C 0.02414(16) -0.13386(12) 0.72788(11) 0.0508(4) Uani 1 1 d . . . H14A H -0.0388 -0.1952 0.7135 0.076 Uiso 1 1 calc R . . H14B H 0.0709 -0.1375 0.7688 0.076 Uiso 1 1 calc R . . H14C H 0.0696 -0.1241 0.6886 0.076 Uiso 1 1 calc R . . C15 C -0.11520(15) -0.02049(14) 0.67134(10) 0.0524(4) Uani 1 1 d . . . H15A H -0.0647 -0.0039 0.6353 0.079 Uiso 1 1 calc R . . H15B H -0.1512 0.0304 0.6837 0.079 Uiso 1 1 calc R . . H15C H -0.1731 -0.0840 0.6527 0.079 Uiso 1 1 calc R . . C16 C 0.59396(15) 0.23324(14) 0.80068(10) 0.0481(4) Uani 1 1 d . . . H16A H 0.6763 0.2523 0.8077 0.072 Uiso 1 1 calc R . . H16B H 0.5620 0.1847 0.8290 0.072 Uiso 1 1 calc R . . H16C H 0.5702 0.2913 0.8155 0.072 Uiso 1 1 calc R . . C17 C 0.59740(15) 0.27606(14) 0.65313(11) 0.0522(4) Uani 1 1 d . . . H17A H 0.6787 0.3069 0.6664 0.078 Uiso 1 1 calc R . . H17B H 0.5594 0.3258 0.6637 0.078 Uiso 1 1 calc R . . H17C H 0.5826 0.2466 0.6024 0.078 Uiso 1 1 calc R . . C18 C 0.60939(15) 0.08033(14) 0.67658(13) 0.0580(5) Uani 1 1 d . . . H18A H 0.5865 0.0513 0.6261 0.087 Uiso 1 1 calc R . . H18B H 0.5848 0.0293 0.7041 0.087 Uiso 1 1 calc R . . H18C H 0.6915 0.1092 0.6849 0.087 Uiso 1 1 calc R . . C19 C 0.13365(14) -0.00928(14) 0.54748(9) 0.0454(4) Uani 1 1 d . . . H19A H 0.1073 0.0468 0.5640 0.068 Uiso 1 1 calc R . . H19B H 0.0992 -0.0622 0.5718 0.068 Uiso 1 1 calc R . . H19C H 0.1123 -0.0328 0.4963 0.068 Uiso 1 1 calc R . . C20 C 0.35582(17) 0.11875(16) 0.51117(10) 0.0563(5) Uani 1 1 d . . . H20A H 0.3187 0.0942 0.4625 0.084 Uiso 1 1 calc R . . H20B H 0.4362 0.1261 0.5115 0.084 Uiso 1 1 calc R . . H20C H 0.3467 0.1826 0.5303 0.084 Uiso 1 1 calc R . . C21 C 0.33489(19) -0.08230(15) 0.54026(10) 0.0604(5) Uani 1 1 d . . . H21A H 0.3072 -0.1123 0.4904 0.091 Uiso 1 1 calc R . . H21B H 0.3034 -0.1295 0.5697 0.091 Uiso 1 1 calc R . . H21C H 0.4173 -0.0635 0.5467 0.091 Uiso 1 1 calc R . . C22 C 0.27062(15) 0.73143(11) 0.82851(10) 0.0438(4) Uani 1 1 d . . . H22A H 0.2506 0.7382 0.7805 0.066 Uiso 1 1 calc R . . H22B H 0.3523 0.7457 0.8371 0.066 Uiso 1 1 calc R . . H22C H 0.2471 0.7777 0.8629 0.066 Uiso 1 1 calc R . . C23 C 0.41167(14) 0.44140(12) 0.62620(8) 0.0381(3) Uani 1 1 d . . . H23A H 0.4829 0.4610 0.6058 0.057 Uiso 1 1 calc R . . H23B H 0.3486 0.4257 0.5892 0.057 Uiso 1 1 calc R . . H23C H 0.4066 0.3834 0.6461 0.057 Uiso 1 1 calc R . . C24 C -0.02753(15) 0.56649(14) 0.71191(8) 0.0442(4) Uani 1 1 d . . . H24A H -0.0001 0.5175 0.6831 0.066 Uiso 1 1 calc R . . H24B H 0.0106 0.6315 0.7027 0.066 Uiso 1 1 calc R . . H24C H -0.1089 0.5497 0.6996 0.066 Uiso 1 1 calc R . . C25 C -0.08011(14) 0.44504(12) 0.82371(9) 0.0424(4) Uani 1 1 d . . . H25A H -0.0654 0.4431 0.8736 0.064 Uiso 1 1 calc R . . H25B H -0.0579 0.3936 0.7937 0.064 Uiso 1 1 calc R . . H25C H -0.1606 0.4341 0.8120 0.064 Uiso 1 1 calc R . . C26 C -0.04482(14) 0.66678(12) 0.86132(9) 0.0419(4) Uani 1 1 d . . . H26A H -0.1221 0.6592 0.8431 0.063 Uiso 1 1 calc R . . H26B H 0.0050 0.7313 0.8575 0.063 Uiso 1 1 calc R . . H26C H -0.0422 0.6614 0.9111 0.063 Uiso 1 1 calc R . . C27 C 0.16367(17) 0.48035(14) 0.98262(9) 0.0521(4) Uani 1 1 d . . . H27A H 0.1780 0.4865 1.0338 0.078 Uiso 1 1 calc R . . H27B H 0.1944 0.4309 0.9577 0.078 Uiso 1 1 calc R . . H27C H 0.0823 0.4602 0.9686 0.078 Uiso 1 1 calc R . . C28 C 0.18081(18) 0.69671(15) 1.01313(9) 0.0547(5) Uani 1 1 d . . . H28A H 0.0983 0.6754 1.0058 0.082 Uiso 1 1 calc R . . H28B H 0.2110 0.7593 0.9983 0.082 Uiso 1 1 calc R . . H28C H 0.2059 0.7051 1.0634 0.082 Uiso 1 1 calc R . . C29 C 0.38735(16) 0.63609(19) 0.98663(10) 0.0642(6) Uani 1 1 d . . . H29A H 0.4255 0.7006 0.9765 0.096 Uiso 1 1 calc R . . H29B H 0.4172 0.5870 0.9603 0.096 Uiso 1 1 calc R . . H29C H 0.4003 0.6389 1.0375 0.096 Uiso 1 1 calc R . . C30 C 0.59351(16) 0.71885(14) 0.83939(10) 0.0518(4) Uani 1 1 d . . . H30A H 0.5354 0.7023 0.8710 0.078 Uiso 1 1 calc R . . H30B H 0.5837 0.7712 0.8170 0.078 Uiso 1 1 calc R . . H30C H 0.6681 0.7413 0.8667 0.078 Uiso 1 1 calc R . . C31 C 0.69153(14) 0.64274(16) 0.70889(10) 0.0529(5) Uani 1 1 d . . . H31A H 0.6785 0.6934 0.6859 0.079 Uiso 1 1 calc R . . H31B H 0.6877 0.5848 0.6728 0.079 Uiso 1 1 calc R . . H31C H 0.7661 0.6682 0.7363 0.079 Uiso 1 1 calc R . . C32 C 0.61233(15) 0.51436(14) 0.81503(12) 0.0566(5) Uani 1 1 d . . . H32A H 0.6844 0.5443 0.8452 0.085 Uiso 1 1 calc R . . H32B H 0.6167 0.4588 0.7794 0.085 Uiso 1 1 calc R . . H32C H 0.5523 0.4912 0.8442 0.085 Uiso 1 1 calc R . . C33 C 0.24202(17) 0.67068(17) 0.62186(13) 0.0635(5) Uani 1 1 d . . . H33A H 0.2341 0.7295 0.6520 0.095 Uiso 1 1 calc R . . H33B H 0.1897 0.6120 0.6333 0.095 Uiso 1 1 calc R . . H33C H 0.2248 0.6716 0.5720 0.095 Uiso 1 1 calc R . . C34 C 0.47971(17) 0.79602(13) 0.68228(12) 0.0551(5) Uani 1 1 d . . . H34A H 0.5588 0.7988 0.6877 0.083 Uiso 1 1 calc R . . H34B H 0.4559 0.8135 0.7290 0.083 Uiso 1 1 calc R . . H34C H 0.4710 0.8425 0.6535 0.083 Uiso 1 1 calc R . . C35 C 0.4411(2) 0.64072(18) 0.54899(11) 0.0730(7) Uani 1 1 d . . . H35A H 0.4338 0.6889 0.5215 0.109 Uiso 1 1 calc R . . H35B H 0.3957 0.5747 0.5236 0.109 Uiso 1 1 calc R . . H35C H 0.5203 0.6439 0.5556 0.109 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 Al1 0.0246(2) 0.02451(19) 0.02293(18) 0.00278(15) -0.00201(14) 0.00803(15) Si1 0.02038(17) 0.01952(16) 0.02247(16) 0.00542(13) 0.00406(12) 0.00631(13) Si2 0.02363(18) 0.02386(18) 0.02633(17) 0.00695(14) 0.00734(13) 0.00617(14) Si3 0.0410(2) 0.0412(2) 0.02506(18) 0.01043(17) 0.00571(16) 0.00744(18) Si4 0.0280(2) 0.0292(2) 0.0385(2) 0.00836(17) 0.00444(16) 0.00052(15) Si5 0.02201(17) 0.02551(18) 0.02640(17) 0.00539(14) 0.00553(13) 0.00943(14) Si6 0.02231(19) 0.0331(2) 0.0438(2) 0.00885(17) 0.00556(16) 0.00974(15) Si7 0.0318(2) 0.0370(2) 0.02717(18) 0.00231(16) 0.00436(15) 0.01536(16) Si8 0.02084(17) 0.01958(16) 0.02151(16) 0.00411(13) 0.00386(12) 0.00599(13) Si9 0.02464(18) 0.02381(17) 0.02429(17) 0.00162(13) 0.00526(13) 0.00736(14) Si10 0.02636(19) 0.0310(2) 0.02816(18) 0.00373(15) 0.00504(14) 0.01303(15) Si11 0.0317(2) 0.0433(2) 0.02304(18) -0.00013(16) 0.00274(15) 0.00826(17) Si12 0.02448(18) 0.02547(18) 0.02796(18) 0.00850(14) 0.00828(14) 0.00786(14) Si13 0.02359(19) 0.0345(2) 0.0398(2) 0.00951(17) 0.00536(16) 0.00505(15) Si14 0.0410(2) 0.0357(2) 0.0436(2) 0.02171(19) 0.01212(18) 0.01112(18) O1 0.0289(5) 0.0265(5) 0.0246(4) 0.0059(4) 0.0008(4) 0.0107(4) O2 0.0261(5) 0.0251(5) 0.0268(4) 0.0017(4) -0.0002(4) 0.0084(4) O3 0.0719(8) 0.0478(7) 0.0224(5) 0.0090(4) 0.0047(5) 0.0344(6) C1 0.0288(8) 0.0448(9) 0.0598(11) 0.0030(8) -0.0105(7) 0.0075(7) C2 0.0222(6) 0.0229(6) 0.0267(6) 0.0070(5) 0.0002(5) 0.0058(5) C3 0.0278(7) 0.0227(6) 0.0213(6) 0.0039(5) 0.0011(5) 0.0053(5) C4 0.0957(17) 0.0528(11) 0.0385(9) -0.0051(8) 0.0225(10) 0.0181(11) C5 0.356(7) 0.095(2) 0.0468(15) 0.0220(15) 0.083(3) 0.056(3) C6 0.260(5) 0.173(4) 0.0505(15) 0.064(2) 0.036(2) 0.126(4) C7 0.234(4) 0.133(3) 0.0631(15) 0.0648(17) 0.052(2) 0.135(3) C8 0.0369(8) 0.0404(9) 0.0576(10) 0.0114(7) 0.0192(7) 0.0186(7) C9 0.0402(9) 0.0399(8) 0.0491(9) 0.0205(7) 0.0137(7) 0.0189(7) C10 0.0613(13) 0.0749(14) 0.0429(10) 0.0208(10) -0.0150(9) -0.0088(10) C11 0.0976(18) 0.0917(17) 0.0355(9) 0.0175(10) 0.0309(10) 0.0409(14) C12 0.0687(13) 0.0565(11) 0.0478(10) 0.0268(9) 0.0085(9) 0.0239(10) C13 0.0511(12) 0.0649(13) 0.0723(13) 0.0210(11) 0.0263(10) -0.0108(10) C14 0.0509(10) 0.0281(8) 0.0668(12) 0.0070(8) -0.0025(9) 0.0063(7) C15 0.0402(9) 0.0563(11) 0.0539(10) 0.0049(9) -0.0103(8) 0.0119(8) C16 0.0370(9) 0.0487(10) 0.0535(10) 0.0100(8) -0.0093(7) 0.0089(7) C17 0.0379(9) 0.0550(11) 0.0664(12) 0.0278(9) 0.0128(8) 0.0085(8) C18 0.0324(9) 0.0465(10) 0.0972(16) 0.0073(10) 0.0182(9) 0.0186(8) C19 0.0368(9) 0.0531(10) 0.0388(8) 0.0013(7) -0.0022(7) 0.0092(7) C20 0.0533(11) 0.0772(14) 0.0418(9) 0.0234(9) 0.0119(8) 0.0180(10) C21 0.0759(14) 0.0586(12) 0.0505(10) -0.0103(9) -0.0032(9) 0.0418(11) C22 0.0475(10) 0.0279(7) 0.0528(9) 0.0050(7) 0.0138(8) 0.0081(7) C23 0.0480(9) 0.0386(8) 0.0338(7) 0.0079(6) 0.0143(7) 0.0209(7) C24 0.0436(9) 0.0634(11) 0.0338(8) 0.0089(7) 0.0022(7) 0.0300(8) C25 0.0336(8) 0.0380(8) 0.0538(10) 0.0084(7) 0.0080(7) 0.0091(6) C26 0.0389(9) 0.0434(9) 0.0468(9) 0.0023(7) 0.0097(7) 0.0217(7) C27 0.0659(12) 0.0587(11) 0.0335(8) 0.0136(8) 0.0162(8) 0.0183(9) C28 0.0665(12) 0.0592(11) 0.0334(8) -0.0051(8) 0.0098(8) 0.0209(9) C29 0.0404(10) 0.1001(17) 0.0369(9) -0.0046(10) -0.0057(7) 0.0133(10) C30 0.0445(10) 0.0480(10) 0.0514(10) -0.0001(8) 0.0043(8) 0.0041(8) C31 0.0287(8) 0.0706(12) 0.0594(11) 0.0186(9) 0.0158(8) 0.0111(8) C32 0.0352(9) 0.0505(10) 0.0811(14) 0.0248(10) -0.0121(9) 0.0055(8) C33 0.0520(12) 0.0653(13) 0.0828(15) 0.0382(11) 0.0016(10) 0.0201(10) C34 0.0560(11) 0.0332(9) 0.0795(13) 0.0259(9) 0.0076(10) 0.0109(8) C35 0.1039(18) 0.0751(15) 0.0520(11) 0.0364(11) 0.0349(12) 0.0281(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 Al1 O2 1.7175(10) . ? Al1 O1 1.7240(10) . ? Al1 O3 1.9006(11) . ? Al1 C1 1.9510(16) . ? Si1 O1 1.6373(9) . ? Si1 C2 1.8908(13) . ? Si1 Si5 2.3784(5) . ? Si1 Si2 2.3813(5) . ? Si2 C8 1.9136(15) . ? Si2 Si4 2.3549(5) . ? Si2 Si3 2.3591(5) . ? Si3 C10 1.869(2) . ? Si3 C11 1.8702(19) . ? Si3 C12 1.8770(19) . ? Si4 C15 1.8744(18) . ? Si4 C13 1.8745(18) . ? Si4 C14 1.8795(18) . ? Si5 C9 1.9014(15) . ? Si5 Si7 2.3475(5) . ? Si5 Si6 2.3596(5) . ? Si6 C17 1.8699(18) . ? Si6 C18 1.8763(17) . ? Si6 C16 1.8772(18) . ? Si7 C21 1.8727(18) . ? Si7 C19 1.8727(17) . ? Si7 C20 1.8734(19) . ? Si8 O2 1.6356(9) . ? Si8 C3 1.8883(13) . ? Si8 Si9 2.3694(5) . ? Si8 Si12 2.3728(5) . ? Si9 C22 1.9036(16) . ? Si9 Si10 2.3462(5) . ? Si9 Si11 2.3564(5) . ? Si10 C25 1.8700(17) . ? Si10 C24 1.8774(16) . ? Si10 C26 1.8805(15) . ? Si11 C29 1.8674(19) . ? Si11 C27 1.8698(19) . ? Si11 C28 1.8819(18) . ? Si12 C23 1.9172(15) . ? Si12 Si13 2.3516(6) . ? Si12 Si14 2.3652(6) . ? Si13 C30 1.8674(18) . ? Si13 C32 1.8776(19) . ? Si13 C31 1.8780(17) . ? Si14 C34 1.8719(19) . ? Si14 C35 1.876(2) . ? Si14 C33 1.882(2) . ? O3 C4 1.428(2) . ? O3 C7 1.451(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.5442(17) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.435(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.428(5) . ? C5 H5 0.9500 . ? C6 C7 1.460(4) . ? C6 H6 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? 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 Al1 O1 113.31(5) . . ? O2 Al1 O3 100.62(5) . . ? O1 Al1 O3 101.24(5) . . ? O2 Al1 C1 115.81(6) . . ? O1 Al1 C1 119.55(7) . . ? O3 Al1 C1 102.12(7) . . ? O1 Si1 C2 110.85(5) . . ? O1 Si1 Si5 112.55(4) . . ? C2 Si1 Si5 104.81(4) . . ? O1 Si1 Si2 107.04(4) . . ? C2 Si1 Si2 109.46(4) . . ? Si5 Si1 Si2 112.157(18) . . ? C8 Si2 Si4 101.92(6) . . ? C8 Si2 Si3 105.50(6) . . ? Si4 Si2 Si3 107.87(2) . . ? C8 Si2 Si1 106.57(5) . . ? Si4 Si2 Si1 116.970(19) . . ? Si3 Si2 Si1 116.37(2) . . ? C10 Si3 C11 107.84(11) . . ? C10 Si3 C12 107.97(11) . . ? C11 Si3 C12 107.56(10) . . ? C10 Si3 Si2 112.28(6) . . ? C11 Si3 Si2 107.74(8) . . ? C12 Si3 Si2 113.22(6) . . ? C15 Si4 C13 107.58(10) . . ? C15 Si4 C14 107.85(9) . . ? C13 Si4 C14 106.97(10) . . ? C15 Si4 Si2 110.88(6) . . ? C13 Si4 Si2 107.00(7) . . ? C14 Si4 Si2 116.19(6) . . ? C9 Si5 Si7 109.84(6) . . ? C9 Si5 Si6 102.51(5) . . ? Si7 Si5 Si6 108.83(2) . . ? C9 Si5 Si1 108.55(5) . . ? Si7 Si5 Si1 109.712(19) . . ? Si6 Si5 Si1 117.07(2) . . ? C17 Si6 C18 107.54(9) . . ? C17 Si6 C16 108.09(9) . . ? C18 Si6 C16 107.07(10) . . ? C17 Si6 Si5 115.72(6) . . ? C18 Si6 Si5 107.01(6) . . ? C16 Si6 Si5 111.02(6) . . ? C21 Si7 C19 107.52(9) . . ? C21 Si7 C20 107.87(10) . . ? C19 Si7 C20 109.00(9) . . ? C21 Si7 Si5 111.42(6) . . ? C19 Si7 Si5 110.50(5) . . ? C20 Si7 Si5 110.43(7) . . ? O2 Si8 C3 110.25(5) . . ? O2 Si8 Si9 109.54(4) . . ? C3 Si8 Si9 106.76(4) . . ? O2 Si8 Si12 107.41(4) . . ? C3 Si8 Si12 108.48(4) . . ? Si9 Si8 Si12 114.399(18) . . ? C22 Si9 Si10 107.49(6) . . ? C22 Si9 Si11 105.57(6) . . ? Si10 Si9 Si11 109.97(2) . . ? C22 Si9 Si8 113.06(5) . . ? Si10 Si9 Si8 106.860(18) . . ? Si11 Si9 Si8 113.74(2) . . ? C25 Si10 C24 107.44(9) . . ? C25 Si10 C26 110.04(8) . . ? C24 Si10 C26 107.95(8) . . ? C25 Si10 Si9 111.26(6) . . ? C24 Si10 Si9 110.41(6) . . ? C26 Si10 Si9 109.66(6) . . ? C29 Si11 C27 107.75(11) . . ? C29 Si11 C28 107.17(10) . . ? C27 Si11 C28 108.47(9) . . ? C29 Si11 Si9 111.19(6) . . ? C27 Si11 Si9 113.49(6) . . ? C28 Si11 Si9 108.55(6) . . ? C23 Si12 Si13 107.35(5) . . ? C23 Si12 Si14 103.60(5) . . ? Si13 Si12 Si14 107.60(2) . . ? C23 Si12 Si8 106.53(5) . . ? Si13 Si12 Si8 114.41(2) . . ? Si14 Si12 Si8 116.45(2) . . ? C30 Si13 C32 107.43(10) . . ? C30 Si13 C31 108.40(9) . . ? C32 Si13 C31 108.03(10) . . ? C30 Si13 Si12 112.84(6) . . ? C32 Si13 Si12 112.81(6) . . ? C31 Si13 Si12 107.17(6) . . ? C34 Si14 C35 106.96(11) . . ? C34 Si14 C33 107.43(10) . . ? C35 Si14 C33 107.71(12) . . ? C34 Si14 Si12 113.60(6) . . ? C35 Si14 Si12 107.66(8) . . ? C33 Si14 Si12 113.17(7) . . ? Si1 O1 Al1 138.55(6) . . ? Si8 O2 Al1 141.78(6) . . ? C4 O3 C7 109.68(15) . . ? C4 O3 Al1 126.82(11) . . ? C7 O3 Al1 121.31(12) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 Si1 120.00(9) . . ? C3 C2 H2A 107.3 . . ? Si1 C2 H2A 107.3 . . ? C3 C2 H2B 107.3 . . ? Si1 C2 H2B 107.3 . . ? H2A C2 H2B 106.9 . . ? C2 C3 Si8 119.12(9) . . ? C2 C3 H3A 107.5 . . ? Si8 C3 H3A 107.5 . . ? C2 C3 H3B 107.5 . . ? Si8 C3 H3B 107.5 . . ? H3A C3 H3B 107.0 . . ? O3 C4 C5 105.3(2) . . ? O3 C4 H4A 110.7 . . ? C5 C4 H4A 110.7 . . ? O3 C4 H4B 110.7 . . ? C5 C4 H4B 110.7 . . ? H4A C4 H4B 108.8 . . ? C6 C5 C4 109.4(3) . . ? C6 C5 H5 125.3 . . ? C4 C5 H5 125.3 . . ? C5 C6 C7 107.0(2) . . ? C5 C6 H6 126.5 . . ? C7 C6 H6 126.5 . . ? O3 C7 C6 105.8(2) . . ? O3 C7 H7A 110.6 . . ? C6 C7 H7A 110.6 . . ? O3 C7 H7B 110.6 . . ? C6 C7 H7B 110.6 . . ? H7A C7 H7B 108.7 . . ? Si2 C8 H8A 109.5 . . ? Si2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si5 C9 H9A 109.5 . . ? Si5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si3 C10 H10A 109.5 . . ? Si3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si3 C11 H11A 109.5 . . ? Si3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si3 C12 H12A 109.5 . . ? Si3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si4 C13 H13A 109.5 . . ? Si4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si4 C14 H14A 109.5 . . ? Si4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si4 C15 H15A 109.5 . . ? Si4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si6 C16 H16A 109.5 . . ? Si6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si6 C17 H17A 109.5 . . ? Si6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si6 C18 H18A 109.5 . . ? Si6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si7 C19 H19A 109.5 . . ? Si7 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si7 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si7 C20 H20A 109.5 . . ? Si7 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si7 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si7 C21 H21A 109.5 . . ? Si7 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si7 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si9 C22 H22A 109.5 . . ? Si9 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si9 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si12 C23 H23A 109.5 . . ? Si12 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si12 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si10 C24 H24A 109.5 . . ? Si10 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si10 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si10 C25 H25A 109.5 . . ? Si10 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si10 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si10 C26 H26A 109.5 . . ? Si10 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si10 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si11 C27 H27A 109.5 . . ? Si11 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si11 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si11 C28 H28A 109.5 . . ? Si11 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si11 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si11 C29 H29A 109.5 . . ? Si11 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si11 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si13 C30 H30A 109.5 . . ? Si13 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si13 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si13 C31 H31A 109.5 . . ? Si13 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si13 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si13 C32 H32A 109.5 . . ? Si13 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si13 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si14 C33 H33A 109.5 . . ? Si14 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si14 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si14 C34 H34A 109.5 . . ? Si14 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si14 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si14 C35 H35A 109.5 . . ? Si14 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si14 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 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 O1 Si1 Si2 C8 -50.74(7) . . . . ? C2 Si1 Si2 C8 69.46(7) . . . . ? Si5 Si1 Si2 C8 -174.65(6) . . . . ? O1 Si1 Si2 Si4 62.41(4) . . . . ? C2 Si1 Si2 Si4 -177.38(4) . . . . ? Si5 Si1 Si2 Si4 -61.50(3) . . . . ? O1 Si1 Si2 Si3 -168.05(4) . . . . ? C2 Si1 Si2 Si3 -47.85(5) . . . . ? Si5 Si1 Si2 Si3 68.04(3) . . . . ? C8 Si2 Si3 C10 -98.46(11) . . . . ? Si4 Si2 Si3 C10 153.19(9) . . . . ? Si1 Si2 Si3 C10 19.43(10) . . . . ? C8 Si2 Si3 C11 20.14(10) . . . . ? Si4 Si2 Si3 C11 -88.21(9) . . . . ? Si1 Si2 Si3 C11 138.03(9) . . . . ? C8 Si2 Si3 C12 138.95(9) . . . . ? Si4 Si2 Si3 C12 30.61(8) . . . . ? Si1 Si2 Si3 C12 -103.16(8) . . . . ? C8 Si2 Si4 C15 59.59(9) . . . . ? Si3 Si2 Si4 C15 170.39(7) . . . . ? Si1 Si2 Si4 C15 -56.16(7) . . . . ? C8 Si2 Si4 C13 -57.46(11) . . . . ? Si3 Si2 Si4 C13 53.34(9) . . . . ? Si1 Si2 Si4 C13 -173.21(9) . . . . ? C8 Si2 Si4 C14 -176.83(9) . . . . ? Si3 Si2 Si4 C14 -66.03(8) . . . . ? Si1 Si2 Si4 C14 67.42(8) . . . . ? O1 Si1 Si5 C9 -133.53(7) . . . . ? C2 Si1 Si5 C9 105.91(7) . . . . ? Si2 Si1 Si5 C9 -12.76(6) . . . . ? O1 Si1 Si5 Si7 -13.50(4) . . . . ? C2 Si1 Si5 Si7 -134.06(4) . . . . ? Si2 Si1 Si5 Si7 107.27(2) . . . . ? O1 Si1 Si5 Si6 111.12(4) . . . . ? C2 Si1 Si5 Si6 -9.44(5) . . . . ? Si2 Si1 Si5 Si6 -128.10(2) . . . . ? C9 Si5 Si6 C17 174.82(9) . . . . ? Si7 Si5 Si6 C17 58.54(8) . . . . ? Si1 Si5 Si6 C17 -66.53(8) . . . . ? C9 Si5 Si6 C18 55.01(10) . . . . ? Si7 Si5 Si6 C18 -61.28(8) . . . . ? Si1 Si5 Si6 C18 173.66(8) . . . . ? C9 Si5 Si6 C16 -61.51(8) . . . . ? Si7 Si5 Si6 C16 -177.79(6) . . . . ? Si1 Si5 Si6 C16 57.14(7) . . . . ? C9 Si5 Si7 C21 -38.91(10) . . . . ? Si6 Si5 Si7 C21 72.58(9) . . . . ? Si1 Si5 Si7 C21 -158.15(8) . . . . ? C9 Si5 Si7 C19 80.56(8) . . . . ? Si6 Si5 Si7 C19 -167.96(7) . . . . ? Si1 Si5 Si7 C19 -38.69(7) . . . . ? C9 Si5 Si7 C20 -158.77(9) . . . . ? Si6 Si5 Si7 C20 -47.29(7) . . . . ? Si1 Si5 Si7 C20 81.98(7) . . . . ? O2 Si8 Si9 C22 -111.76(7) . . . . ? C3 Si8 Si9 C22 128.87(8) . . . . ? Si12 Si8 Si9 C22 8.87(7) . . . . ? O2 Si8 Si9 Si10 6.30(4) . . . . ? C3 Si8 Si9 Si10 -113.07(5) . . . . ? Si12 Si8 Si9 Si10 126.93(2) . . . . ? O2 Si8 Si9 Si11 127.84(4) . . . . ? C3 Si8 Si9 Si11 8.48(5) . . . . ? Si12 Si8 Si9 Si11 -111.52(2) . . . . ? C22 Si9 Si10 C25 -174.92(8) . . . . ? Si11 Si9 Si10 C25 -60.46(6) . . . . ? Si8 Si9 Si10 C25 63.44(6) . . . . ? C22 Si9 Si10 C24 65.88(8) . . . . ? Si11 Si9 Si10 C24 -179.66(6) . . . . ? Si8 Si9 Si10 C24 -55.77(7) . . . . ? C22 Si9 Si10 C26 -52.94(8) . . . . ? Si11 Si9 Si10 C26 61.51(6) . . . . ? Si8 Si9 Si10 C26 -174.59(6) . . . . ? C22 Si9 Si11 C29 -60.30(10) . . . . ? Si10 Si9 Si11 C29 -175.98(9) . . . . ? Si8 Si9 Si11 C29 64.22(9) . . . . ? C22 Si9 Si11 C27 178.03(9) . . . . ? Si10 Si9 Si11 C27 62.35(7) . . . . ? Si8 Si9 Si11 C27 -57.45(7) . . . . ? C22 Si9 Si11 C28 57.35(9) . . . . ? Si10 Si9 Si11 C28 -58.32(7) . . . . ? Si8 Si9 Si11 C28 -178.12(7) . . . . ? O2 Si8 Si12 C23 -45.38(7) . . . . ? C3 Si8 Si12 C23 73.78(7) . . . . ? Si9 Si8 Si12 C23 -167.19(5) . . . . ? O2 Si8 Si12 Si13 -163.82(4) . . . . ? C3 Si8 Si12 Si13 -44.66(5) . . . . ? Si9 Si8 Si12 Si13 74.37(3) . . . . ? O2 Si8 Si12 Si14 69.56(4) . . . . ? C3 Si8 Si12 Si14 -171.29(4) . . . . ? Si9 Si8 Si12 Si14 -52.25(3) . . . . ? C23 Si12 Si13 C30 175.05(9) . . . . ? Si14 Si12 Si13 C30 64.10(7) . . . . ? Si8 Si12 Si13 C30 -66.98(7) . . . . ? C23 Si12 Si13 C32 -62.97(10) . . . . ? Si14 Si12 Si13 C32 -173.92(8) . . . . ? Si8 Si12 Si13 C32 55.00(8) . . . . ? C23 Si12 Si13 C31 55.80(9) . . . . ? Si14 Si12 Si13 C31 -55.15(7) . . . . ? Si8 Si12 Si13 C31 173.78(7) . . . . ? C23 Si12 Si14 C34 -138.14(9) . . . . ? Si13 Si12 Si14 C34 -24.65(8) . . . . ? Si8 Si12 Si14 C34 105.29(8) . . . . ? C23 Si12 Si14 C35 -19.91(11) . . . . ? Si13 Si12 Si14 C35 93.59(9) . . . . ? Si8 Si12 Si14 C35 -136.47(9) . . . . ? C23 Si12 Si14 C33 99.00(10) . . . . ? Si13 Si12 Si14 C33 -147.50(9) . . . . ? Si8 Si12 Si14 C33 -17.56(9) . . . . ? C2 Si1 O1 Al1 -46.61(11) . . . . ? Si5 Si1 O1 Al1 -163.64(7) . . . . ? Si2 Si1 O1 Al1 72.70(9) . . . . ? O2 Al1 O1 Si1 35.68(11) . . . . ? O3 Al1 O1 Si1 142.55(9) . . . . ? C1 Al1 O1 Si1 -106.43(11) . . . . ? C3 Si8 O2 Al1 -30.28(11) . . . . ? Si9 Si8 O2 Al1 -147.47(9) . . . . ? Si12 Si8 O2 Al1 87.74(10) . . . . ? O1 Al1 O2 Si8 -1.02(12) . . . . ? O3 Al1 O2 Si8 -108.28(10) . . . . ? C1 Al1 O2 Si8 142.58(10) . . . . ? O2 Al1 O3 C4 151.45(16) . . . . ? O1 Al1 O3 C4 34.85(17) . . . . ? C1 Al1 O3 C4 -89.00(17) . . . . ? O2 Al1 O3 C7 -47.2(2) . . . . ? O1 Al1 O3 C7 -163.8(2) . . . . ? C1 Al1 O3 C7 72.4(2) . . . . ? O1 Si1 C2 C3 57.95(11) . . . . ? Si5 Si1 C2 C3 179.63(9) . . . . ? Si2 Si1 C2 C3 -59.90(10) . . . . ? Si1 C2 C3 Si8 -77.69(12) . . . . ? O2 Si8 C3 C2 63.04(11) . . . . ? Si9 Si8 C3 C2 -178.05(8) . . . . ? Si12 Si8 C3 C2 -54.31(10) . . . . ? C7 O3 C4 C5 14.6(4) . . . . ? Al1 O3 C4 C5 177.8(3) . . . . ? O3 C4 C5 C6 -17.3(5) . . . . ? C4 C5 C6 C7 13.4(6) . . . . ? C4 O3 C7 C6 -6.7(4) . . . . ? Al1 O3 C7 C6 -170.9(3) . . . . ? C5 C6 C7 O3 -4.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.686 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.048 data_w313 _database_code_depnum_ccdc_archive 'CCDC 778868' #TrackingRef '- X-ray compound 4.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2-Hydroxy-4,4,7,7-tetrakis(1',2',2',2'-tetramethyl-1'-trimethylsilyl- disilyl)-2-alumina-1,3-dioxa-4,7-disilacycloheptane ; _chemical_name_common ; 2-Hydroxy-4,4,7,7-tetrakis(1',2',2',2'-tetramethyl-1'- trimethylsilyl-disilyl)-2-alumina-1,3-dioxa-4,7-disilacycloheptane ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H176 Al2 O6 Si28' _chemical_formula_weight 1834.49 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' Al Al 0.0645 0.0514 '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 ' _symmetry_space_group_name_Hall '-P 2yn' 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 12.5114(9) _cell_length_b 18.1996(10) _cell_length_c 25.6540(16) _cell_angle_alpha 90.00 _cell_angle_beta 95.602(2) _cell_angle_gamma 90.00 _cell_volume 5813.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5723 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 21.92 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.048 _exptl_crystal_density_method ? _exptl_crystal_F_000 2004 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9179 _exptl_absorpt_correction_T_max 0.9660 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker X8Apex CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 77499 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.74 _reflns_number_total 11059 _reflns_number_gt 7045 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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. There is quite a high residual electron density. However, attempts to allocate the peaks found in the difference e.g. to disordered atoms failed. ; _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^)+(0.1070P)^2^+9.2025P] 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_number_reflns 11059 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.2100 _refine_ls_wR_factor_gt 0.1814 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Al1 Al 0.53799(10) 0.44786(7) 0.03799(5) 0.0266(3) Uani 1 1 d . . . Si1 Si 0.85527(11) 0.53229(8) 0.15844(5) 0.0442(4) Uani 1 1 d . . . Si2 Si 0.74257(10) 0.46356(7) 0.20806(5) 0.0313(3) Uani 1 1 d . . . Si3 Si 0.57770(9) 0.42863(6) 0.16051(4) 0.0237(3) Uani 1 1 d . . . Si4 Si 0.42510(10) 0.45766(7) 0.20429(5) 0.0309(3) Uani 1 1 d . . . Si5 Si 0.39726(14) 0.39041(9) 0.28001(6) 0.0566(4) Uani 1 1 d . . . Si6 Si 0.84014(16) 0.36678(10) 0.25072(9) 0.0875(8) Uani 1 1 d . . . Si7 Si 0.40209(11) 0.58384(8) 0.21978(6) 0.0437(4) Uani 1 1 d . . . Si8 Si 0.87677(12) 0.33268(9) -0.01644(6) 0.0494(4) Uani 1 1 d . . . Si9 Si 0.75266(11) 0.24016(7) -0.00256(5) 0.0390(3) Uani 1 1 d . . . Si10 Si 0.61090(9) 0.28112(6) 0.04491(5) 0.0277(3) Uani 1 1 d . . . Si11 Si 0.47515(11) 0.18959(7) 0.03674(5) 0.0403(3) Uani 1 1 d . . . Si12 Si 0.41329(12) 0.13943(8) 0.11277(6) 0.0448(4) Uani 1 1 d . . . Si13 Si 0.84859(12) 0.13804(8) 0.03708(6) 0.0490(4) Uani 1 1 d . . . Si14 Si 0.32763(13) 0.23800(9) -0.01511(6) 0.0550(4) Uani 1 1 d . . . O1 O 0.5883(2) 0.51834(16) -0.00453(11) 0.0309(7) Uani 1 1 d . . . O2 O 0.5589(2) 0.46810(15) 0.10275(10) 0.0273(6) Uani 1 1 d . . . O3 O 0.5650(2) 0.35984(15) 0.02123(11) 0.0302(7) Uani 1 1 d . . . C1 C 0.5764(3) 0.3259(2) 0.15033(16) 0.0280(9) Uani 1 1 d . . . H1A H 0.5872 0.3019 0.1851 0.034 Uiso 1 1 calc R . . H1B H 0.5042 0.3116 0.1343 0.034 Uiso 1 1 calc R . . C2 C 0.6608(3) 0.2947(2) 0.11586(16) 0.0292(9) Uani 1 1 d . . . H2A H 0.6865 0.2469 0.1306 0.035 Uiso 1 1 calc R . . H2B H 0.7230 0.3285 0.1179 0.035 Uiso 1 1 calc R . . C3 C 0.8058(5) 0.5309(3) 0.0866(2) 0.0575(15) Uani 1 1 d . . . H3A H 0.8543 0.5599 0.0670 0.086 Uiso 1 1 calc R . . H3B H 0.7334 0.5519 0.0816 0.086 Uiso 1 1 calc R . . H3C H 0.8039 0.4801 0.0739 0.086 Uiso 1 1 calc R . . C4 C 0.8532(7) 0.6299(4) 0.1814(3) 0.089(2) Uani 1 1 d . . . H4A H 0.8997 0.6598 0.1613 0.133 Uiso 1 1 calc R . . H4B H 0.8792 0.6322 0.2187 0.133 Uiso 1 1 calc R . . H4C H 0.7796 0.6488 0.1763 0.133 Uiso 1 1 calc R . . C5 C 0.9968(5) 0.5009(6) 0.1658(3) 0.110(3) Uani 1 1 d . . . H5A H 1.0394 0.5317 0.1442 0.166 Uiso 1 1 calc R . . H5B H 1.0003 0.4496 0.1545 0.166 Uiso 1 1 calc R . . H5C H 1.0256 0.5049 0.2026 0.166 Uiso 1 1 calc R . . C6 C 0.7090(5) 0.5268(4) 0.2627(2) 0.0590(16) Uani 1 1 d . . . H6A H 0.7755 0.5423 0.2832 0.089 Uiso 1 1 calc R . . H6B H 0.6633 0.5007 0.2856 0.089 Uiso 1 1 calc R . . H6C H 0.6709 0.5701 0.2478 0.089 Uiso 1 1 calc R . . C7 C 0.3090(4) 0.4315(3) 0.1540(2) 0.0461(12) Uani 1 1 d . . . H7A H 0.2407 0.4415 0.1685 0.069 Uiso 1 1 calc R . . H7B H 0.3135 0.3791 0.1458 0.069 Uiso 1 1 calc R . . H7C H 0.3130 0.4604 0.1221 0.069 Uiso 1 1 calc R . . C8 C 0.4145(7) 0.2899(4) 0.2711(3) 0.084(2) Uani 1 1 d . . . H8A H 0.4021 0.2643 0.3036 0.127 Uiso 1 1 calc R . . H8B H 0.4876 0.2798 0.2624 0.127 Uiso 1 1 calc R . . H8C H 0.3628 0.2725 0.2426 0.127 Uiso 1 1 calc R . . C9 C 0.2562(8) 0.4075(6) 0.2927(4) 0.153(5) Uani 1 1 d . . . H9A H 0.2402 0.3805 0.3241 0.230 Uiso 1 1 calc R . . H9B H 0.2080 0.3908 0.2626 0.230 Uiso 1 1 calc R . . H9C H 0.2456 0.4602 0.2980 0.230 Uiso 1 1 calc R . . C10 C 0.4856(10) 0.4181(5) 0.3393(3) 0.139(4) Uani 1 1 d . . . H10A H 0.4694 0.3878 0.3691 0.208 Uiso 1 1 calc R . . H10B H 0.4731 0.4699 0.3471 0.208 Uiso 1 1 calc R . . H10C H 0.5609 0.4111 0.3329 0.208 Uiso 1 1 calc R . . C11 C 0.9372(5) 0.4064(4) 0.3029(3) 0.082(2) Uani 1 1 d . . . H11A H 0.9785 0.3666 0.3210 0.123 Uiso 1 1 calc R . . H11B H 0.8980 0.4335 0.3279 0.123 Uiso 1 1 calc R . . H11C H 0.9862 0.4398 0.2870 0.123 Uiso 1 1 calc R . . C12 C 0.7557(9) 0.2986(8) 0.2798(6) 0.274(12) Uani 1 1 d . . . H12A H 0.8012 0.2600 0.2968 0.411 Uiso 1 1 calc R . . H12B H 0.7057 0.2768 0.2522 0.411 Uiso 1 1 calc R . . H12C H 0.7149 0.3226 0.3057 0.411 Uiso 1 1 calc R . . C13 C 0.9229(11) 0.3125(6) 0.2050(5) 0.207(8) Uani 1 1 d . . . H13A H 0.9617 0.2730 0.2247 0.311 Uiso 1 1 calc R . . H13B H 0.9744 0.3454 0.1904 0.311 Uiso 1 1 calc R . . H13C H 0.8749 0.2913 0.1764 0.311 Uiso 1 1 calc R . . C14 C 0.2552(5) 0.6049(4) 0.2083(3) 0.084(2) Uani 1 1 d . . . H14A H 0.2435 0.6573 0.2146 0.126 Uiso 1 1 calc R . . H14B H 0.2161 0.5757 0.2324 0.126 Uiso 1 1 calc R . . H14C H 0.2291 0.5927 0.1721 0.126 Uiso 1 1 calc R . . C15 C 0.4458(5) 0.6130(4) 0.2886(2) 0.0653(17) Uani 1 1 d . . . H15A H 0.4339 0.6659 0.2922 0.098 Uiso 1 1 calc R . . H15B H 0.5223 0.6020 0.2968 0.098 Uiso 1 1 calc R . . H15C H 0.4040 0.5862 0.3129 0.098 Uiso 1 1 calc R . . C16 C 0.4726(5) 0.6396(3) 0.1724(3) 0.0664(17) Uani 1 1 d . . . H16A H 0.4624 0.6920 0.1793 0.100 Uiso 1 1 calc R . . H16B H 0.4430 0.6280 0.1366 0.100 Uiso 1 1 calc R . . H16C H 0.5495 0.6280 0.1766 0.100 Uiso 1 1 calc R . . C17 C 0.9599(5) 0.3637(4) 0.0444(3) 0.078(2) Uani 1 1 d . . . H17A H 1.0096 0.4023 0.0354 0.118 Uiso 1 1 calc R . . H17B H 1.0008 0.3220 0.0601 0.118 Uiso 1 1 calc R . . H17C H 0.9127 0.3831 0.0695 0.118 Uiso 1 1 calc R . . C18 C 0.9677(5) 0.2964(4) -0.0649(3) 0.0689(18) Uani 1 1 d . . . H18A H 1.0208 0.3340 -0.0716 0.103 Uiso 1 1 calc R . . H18B H 0.9249 0.2841 -0.0978 0.103 Uiso 1 1 calc R . . H18C H 1.0048 0.2523 -0.0506 0.103 Uiso 1 1 calc R . . C19 C 0.8043(5) 0.4149(3) -0.0463(3) 0.0691(18) Uani 1 1 d . . . H19A H 0.8564 0.4536 -0.0521 0.104 Uiso 1 1 calc R . . H19B H 0.7535 0.4331 -0.0226 0.104 Uiso 1 1 calc R . . H19C H 0.7653 0.4011 -0.0798 0.104 Uiso 1 1 calc R . . C20 C 0.6976(5) 0.2150(4) -0.0725(2) 0.0606(15) Uani 1 1 d . . . H20A H 0.6582 0.2569 -0.0888 0.091 Uiso 1 1 calc R . . H20B H 0.6491 0.1728 -0.0716 0.091 Uiso 1 1 calc R . . H20C H 0.7573 0.2023 -0.0929 0.091 Uiso 1 1 calc R . . C21 C 0.5183(5) 0.1086(3) -0.0038(3) 0.0700(18) Uani 1 1 d . . . H21A H 0.4614 0.0714 -0.0068 0.105 Uiso 1 1 calc R . . H21B H 0.5844 0.0871 0.0134 0.105 Uiso 1 1 calc R . . H21C H 0.5313 0.1259 -0.0389 0.105 Uiso 1 1 calc R . . C22 C 0.5216(5) 0.1274(3) 0.1683(2) 0.0617(16) Uani 1 1 d . . . H22A H 0.4904 0.1064 0.1986 0.092 Uiso 1 1 calc R . . H22B H 0.5536 0.1753 0.1779 0.092 Uiso 1 1 calc R . . H22C H 0.5771 0.0944 0.1575 0.092 Uiso 1 1 calc R . . C23 C 0.3025(5) 0.1932(4) 0.1374(2) 0.0707(18) Uani 1 1 d . . . H23A H 0.2802 0.1697 0.1690 0.106 Uiso 1 1 calc R . . H23B H 0.2414 0.1949 0.1104 0.106 Uiso 1 1 calc R . . H23C H 0.3273 0.2433 0.1458 0.106 Uiso 1 1 calc R . . C24 C 0.3591(7) 0.0457(4) 0.0947(3) 0.100(3) Uani 1 1 d . . . H24A H 0.3323 0.0227 0.1254 0.149 Uiso 1 1 calc R . . H24B H 0.4163 0.0153 0.0825 0.149 Uiso 1 1 calc R . . H24C H 0.3002 0.0501 0.0667 0.149 Uiso 1 1 calc R . . C25 C 0.9874(6) 0.1639(4) 0.0663(3) 0.092(2) Uani 1 1 d . . . H25A H 1.0235 0.1204 0.0821 0.138 Uiso 1 1 calc R . . H25B H 0.9821 0.2015 0.0933 0.138 Uiso 1 1 calc R . . H25C H 1.0287 0.1833 0.0388 0.138 Uiso 1 1 calc R . . C26 C 0.7834(6) 0.0927(5) 0.0905(3) 0.109(3) Uani 1 1 d . . . H26A H 0.8280 0.0516 0.1044 0.163 Uiso 1 1 calc R . . H26B H 0.7126 0.0743 0.0767 0.163 Uiso 1 1 calc R . . H26C H 0.7752 0.1283 0.1185 0.163 Uiso 1 1 calc R . . C27 C 0.8677(6) 0.0713(4) -0.0159(3) 0.089(2) Uani 1 1 d . . . H27A H 0.9070 0.0283 -0.0011 0.133 Uiso 1 1 calc R . . H27B H 0.9088 0.0945 -0.0421 0.133 Uiso 1 1 calc R . . H27C H 0.7975 0.0558 -0.0325 0.133 Uiso 1 1 calc R . . C28 C 0.2280(5) 0.1614(4) -0.0341(3) 0.084(2) Uani 1 1 d . . . H28A H 0.1661 0.1815 -0.0558 0.126 Uiso 1 1 calc R . . H28B H 0.2038 0.1395 -0.0024 0.126 Uiso 1 1 calc R . . H28C H 0.2627 0.1237 -0.0538 0.126 Uiso 1 1 calc R . . C29 C 0.3742(5) 0.2758(5) -0.0763(2) 0.082(2) Uani 1 1 d . . . H29A H 0.3128 0.2962 -0.0982 0.123 Uiso 1 1 calc R . . H29B H 0.4071 0.2365 -0.0953 0.123 Uiso 1 1 calc R . . H29C H 0.4271 0.3146 -0.0675 0.123 Uiso 1 1 calc R . . C30 C 0.2606(5) 0.3125(3) 0.0201(3) 0.0699(17) Uani 1 1 d . . . H30A H 0.1993 0.3316 -0.0026 0.105 Uiso 1 1 calc R . . H30B H 0.3119 0.3523 0.0290 0.105 Uiso 1 1 calc R . . H30C H 0.2354 0.2926 0.0522 0.105 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 Al1 0.0320(7) 0.0239(7) 0.0238(6) 0.0006(5) 0.0019(5) 0.0030(5) Si1 0.0367(8) 0.0563(9) 0.0390(8) -0.0003(7) 0.0010(6) -0.0155(6) Si2 0.0288(6) 0.0331(7) 0.0307(6) 0.0024(5) -0.0029(5) -0.0023(5) Si3 0.0261(6) 0.0229(6) 0.0221(6) -0.0002(5) 0.0026(4) -0.0007(4) Si4 0.0320(7) 0.0331(7) 0.0286(6) -0.0036(5) 0.0078(5) -0.0001(5) Si5 0.0744(11) 0.0597(10) 0.0396(8) 0.0063(7) 0.0259(8) -0.0035(8) Si6 0.0775(13) 0.0527(11) 0.1188(17) 0.0411(11) -0.0590(12) -0.0158(9) Si7 0.0436(8) 0.0377(8) 0.0505(8) -0.0113(7) 0.0073(6) 0.0058(6) Si8 0.0466(9) 0.0526(9) 0.0518(9) 0.0030(7) 0.0187(7) 0.0058(7) Si9 0.0445(8) 0.0372(7) 0.0373(7) 0.0027(6) 0.0143(6) 0.0107(6) Si10 0.0318(6) 0.0228(6) 0.0298(6) -0.0013(5) 0.0093(5) 0.0010(5) Si11 0.0452(8) 0.0347(7) 0.0411(7) -0.0019(6) 0.0056(6) -0.0059(6) Si12 0.0570(9) 0.0365(8) 0.0413(8) 0.0060(6) 0.0064(7) -0.0172(6) Si13 0.0555(9) 0.0444(8) 0.0487(9) 0.0044(7) 0.0135(7) 0.0154(7) Si14 0.0484(9) 0.0592(10) 0.0561(10) -0.0017(8) -0.0008(7) -0.0005(7) O1 0.0321(16) 0.0309(16) 0.0294(16) 0.0045(13) 0.0010(13) 0.0026(12) O2 0.0348(16) 0.0239(15) 0.0229(14) 0.0001(12) 0.0016(12) 0.0008(12) O3 0.0370(17) 0.0258(15) 0.0283(15) -0.0022(13) 0.0052(13) 0.0046(12) C1 0.032(2) 0.024(2) 0.029(2) 0.0013(18) 0.0056(18) -0.0030(17) C2 0.028(2) 0.026(2) 0.033(2) 0.0003(19) 0.0019(18) 0.0008(17) C3 0.053(3) 0.080(4) 0.041(3) -0.004(3) 0.010(3) -0.015(3) C4 0.144(7) 0.066(4) 0.054(4) 0.004(3) -0.001(4) -0.048(4) C5 0.038(4) 0.201(10) 0.091(6) 0.019(6) 0.004(4) -0.005(5) C6 0.052(3) 0.086(4) 0.040(3) -0.022(3) 0.006(3) -0.013(3) C7 0.032(3) 0.047(3) 0.059(3) -0.010(3) 0.001(2) 0.000(2) C8 0.134(7) 0.061(4) 0.063(4) 0.009(3) 0.031(4) -0.029(4) C9 0.127(8) 0.192(11) 0.161(9) 0.087(8) 0.116(7) 0.048(7) C10 0.266(13) 0.105(7) 0.039(4) 0.010(4) -0.013(6) -0.070(8) C11 0.072(4) 0.090(5) 0.076(4) 0.023(4) -0.039(4) -0.003(4) C12 0.168(11) 0.258(15) 0.36(2) 0.272(16) -0.170(13) -0.138(11) C13 0.236(13) 0.119(8) 0.235(14) -0.075(9) -0.146(11) 0.132(9) C14 0.054(4) 0.074(4) 0.122(6) -0.037(4) 0.000(4) 0.023(3) C15 0.064(4) 0.067(4) 0.065(4) -0.032(3) 0.010(3) 0.004(3) C16 0.079(4) 0.044(3) 0.078(4) 0.010(3) 0.014(3) -0.001(3) C17 0.071(4) 0.083(5) 0.080(5) -0.020(4) 0.001(4) -0.004(4) C18 0.063(4) 0.076(4) 0.074(4) -0.002(3) 0.040(3) -0.001(3) C19 0.077(4) 0.059(4) 0.076(4) 0.020(3) 0.030(3) 0.012(3) C20 0.069(4) 0.070(4) 0.044(3) -0.008(3) 0.010(3) 0.011(3) C21 0.076(4) 0.047(3) 0.090(5) -0.024(3) 0.023(4) -0.006(3) C22 0.078(4) 0.056(4) 0.050(3) 0.021(3) 0.001(3) -0.009(3) C23 0.056(4) 0.100(5) 0.059(4) 0.014(4) 0.017(3) -0.005(3) C24 0.157(8) 0.059(4) 0.080(5) 0.005(4) 0.000(5) -0.060(5) C25 0.073(5) 0.102(6) 0.095(5) 0.022(5) -0.022(4) 0.002(4) C26 0.090(6) 0.112(7) 0.133(7) 0.072(6) 0.053(5) 0.035(5) C27 0.111(6) 0.060(4) 0.093(5) -0.023(4) -0.003(4) 0.042(4) C28 0.056(4) 0.083(5) 0.108(6) -0.018(4) -0.017(4) -0.007(3) C29 0.075(5) 0.121(6) 0.048(4) 0.017(4) 0.000(3) 0.015(4) C30 0.075(4) 0.058(4) 0.079(4) 0.003(3) 0.019(4) 0.009(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 Al1 O2 1.697(3) . ? Al1 O3 1.701(3) . ? Al1 O1 1.829(3) 3_665 ? Al1 O1 1.835(3) . ? Al1 Al1 2.818(2) 3_665 ? Si1 C5 1.853(7) . ? Si1 C4 1.873(7) . ? Si1 C3 1.886(5) . ? Si1 Si2 2.3502(18) . ? Si2 C6 1.893(5) . ? Si2 Si6 2.351(2) . ? Si2 Si3 2.3782(16) . ? Si3 O2 1.643(3) . ? Si3 C1 1.889(4) . ? Si3 Si4 2.3673(16) . ? Si4 C7 1.906(5) . ? Si4 Si5 2.3506(19) . ? Si4 Si7 2.3529(18) . ? Si5 C9 1.852(8) . ? Si5 C8 1.859(7) . ? Si5 C10 1.860(8) . ? Si6 C12 1.835(9) . ? Si6 C11 1.862(6) . ? Si6 C13 1.914(12) . ? Si7 C16 1.869(6) . ? Si7 C14 1.872(6) . ? Si7 C15 1.874(6) . ? Si8 C19 1.874(6) . ? Si8 C17 1.876(7) . ? Si8 C18 1.885(5) . ? Si8 Si9 2.341(2) . ? Si9 C20 1.913(6) . ? Si9 Si10 2.3678(17) . ? Si9 Si13 2.3855(19) . ? Si10 O3 1.638(3) . ? Si10 C2 1.882(4) . ? Si10 Si11 2.3736(17) . ? Si11 C21 1.912(6) . ? Si11 Si14 2.339(2) . ? Si11 Si12 2.3520(19) . ? Si12 C23 1.857(6) . ? Si12 C24 1.878(6) . ? Si12 C22 1.881(6) . ? Si13 C26 1.854(7) . ? Si13 C27 1.856(6) . ? Si13 C25 1.883(7) . ? Si14 C29 1.858(6) . ? Si14 C30 1.872(6) . ? Si14 C28 1.902(7) . ? O1 Al1 1.829(3) 3_665 ? C1 C2 1.550(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 Al1 O3 115.88(15) . . ? O2 Al1 O1 115.45(14) . 3_665 ? O3 Al1 O1 112.44(15) . 3_665 ? O2 Al1 O1 113.67(14) . . ? O3 Al1 O1 114.84(15) . . ? O1 Al1 O1 79.43(14) 3_665 . ? O2 Al1 Al1 122.70(12) . 3_665 ? O3 Al1 Al1 121.42(12) . 3_665 ? O1 Al1 Al1 39.78(9) 3_665 3_665 ? O1 Al1 Al1 39.65(9) . 3_665 ? C5 Si1 C4 107.6(4) . . ? C5 Si1 C3 108.4(3) . . ? C4 Si1 C3 107.9(3) . . ? C5 Si1 Si2 113.5(3) . . ? C4 Si1 Si2 107.9(2) . . ? C3 Si1 Si2 111.40(18) . . ? C6 Si2 Si1 105.42(19) . . ? C6 Si2 Si6 104.7(2) . . ? Si1 Si2 Si6 109.82(9) . . ? C6 Si2 Si3 107.38(18) . . ? Si1 Si2 Si3 113.62(6) . . ? Si6 Si2 Si3 115.05(7) . . ? O2 Si3 C1 108.04(17) . . ? O2 Si3 Si4 106.20(11) . . ? C1 Si3 Si4 106.87(13) . . ? O2 Si3 Si2 112.75(11) . . ? C1 Si3 Si2 109.34(14) . . ? Si4 Si3 Si2 113.35(6) . . ? C7 Si4 Si5 105.31(18) . . ? C7 Si4 Si7 105.09(17) . . ? Si5 Si4 Si7 109.77(7) . . ? C7 Si4 Si3 102.72(16) . . ? Si5 Si4 Si3 117.86(7) . . ? Si7 Si4 Si3 114.56(7) . . ? C9 Si5 C8 108.1(5) . . ? C9 Si5 C10 108.2(5) . . ? C8 Si5 C10 107.5(4) . . ? C9 Si5 Si4 106.1(3) . . ? C8 Si5 Si4 112.5(2) . . ? C10 Si5 Si4 114.2(3) . . ? C12 Si6 C11 109.3(5) . . ? C12 Si6 C13 105.5(8) . . ? C11 Si6 C13 106.6(4) . . ? C12 Si6 Si2 113.7(4) . . ? C11 Si6 Si2 108.5(2) . . ? C13 Si6 Si2 112.9(4) . . ? C16 Si7 C14 107.8(3) . . ? C16 Si7 C15 110.3(3) . . ? C14 Si7 C15 106.3(3) . . ? C16 Si7 Si4 110.3(2) . . ? C14 Si7 Si4 107.9(2) . . ? C15 Si7 Si4 114.0(2) . . ? C19 Si8 C17 107.8(3) . . ? C19 Si8 C18 108.0(3) . . ? C17 Si8 C18 109.5(3) . . ? C19 Si8 Si9 109.6(2) . . ? C17 Si8 Si9 114.3(2) . . ? C18 Si8 Si9 107.5(2) . . ? C20 Si9 Si8 102.3(2) . . ? C20 Si9 Si10 109.78(19) . . ? Si8 Si9 Si10 113.14(7) . . ? C20 Si9 Si13 109.5(2) . . ? Si8 Si9 Si13 108.16(8) . . ? Si10 Si9 Si13 113.38(7) . . ? O3 Si10 C2 108.36(17) . . ? O3 Si10 Si9 109.74(12) . . ? C2 Si10 Si9 110.14(14) . . ? O3 Si10 Si11 111.04(12) . . ? C2 Si10 Si11 110.16(14) . . ? Si9 Si10 Si11 107.40(7) . . ? C21 Si11 Si14 103.3(2) . . ? C21 Si11 Si12 106.6(2) . . ? Si14 Si11 Si12 108.21(8) . . ? C21 Si11 Si10 110.6(2) . . ? Si14 Si11 Si10 107.70(7) . . ? Si12 Si11 Si10 119.32(7) . . ? C23 Si12 C24 107.4(4) . . ? C23 Si12 C22 108.1(3) . . ? C24 Si12 C22 107.3(3) . . ? C23 Si12 Si11 113.2(2) . . ? C24 Si12 Si11 106.8(2) . . ? C22 Si12 Si11 113.74(19) . . ? C26 Si13 C27 110.3(4) . . ? C26 Si13 C25 105.8(4) . . ? C27 Si13 C25 106.0(4) . . ? C26 Si13 Si9 115.0(2) . . ? C27 Si13 Si9 107.0(2) . . ? C25 Si13 Si9 112.4(2) . . ? C29 Si14 C30 109.3(3) . . ? C29 Si14 C28 107.9(4) . . ? C30 Si14 C28 109.9(3) . . ? C29 Si14 Si11 108.9(2) . . ? C30 Si14 Si11 111.4(2) . . ? C28 Si14 Si11 109.3(2) . . ? Al1 O1 Al1 100.56(14) 3_665 . ? Si3 O2 Al1 141.54(18) . . ? Si10 O3 Al1 143.22(19) . . ? C2 C1 Si3 116.4(3) . . ? C2 C1 H1A 108.2 . . ? Si3 C1 H1A 108.2 . . ? C2 C1 H1B 108.2 . . ? Si3 C1 H1B 108.2 . . ? H1A C1 H1B 107.3 . . ? C1 C2 Si10 114.8(3) . . ? C1 C2 H2A 108.6 . . ? Si10 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? Si10 C2 H2B 108.6 . . ? H2A C2 H2B 107.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si4 C7 H7A 109.5 . . ? Si4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si5 C8 H8A 109.5 . . ? Si5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si5 C9 H9A 109.5 . . ? Si5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si5 C10 H10A 109.5 . . ? Si5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si6 C11 H11A 109.5 . . ? Si6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si6 C12 H12A 109.5 . . ? Si6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si6 C13 H13A 109.5 . . ? Si6 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si6 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si7 C14 H14A 109.5 . . ? Si7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si7 C15 H15A 109.5 . . ? Si7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si7 C16 H16A 109.5 . . ? Si7 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si7 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si8 C17 H17A 109.5 . . ? Si8 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si8 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si8 C18 H18A 109.5 . . ? Si8 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si8 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si8 C19 H19A 109.5 . . ? Si8 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si8 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si9 C20 H20A 109.5 . . ? Si9 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si9 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si11 C21 H21A 109.5 . . ? Si11 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si11 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si12 C22 H22A 109.5 . . ? Si12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si12 C23 H23A 109.5 . . ? Si12 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si12 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si12 C24 H24A 109.5 . . ? Si12 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si12 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si13 C25 H25A 109.5 . . ? Si13 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si13 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si13 C26 H26A 109.5 . . ? Si13 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si13 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si13 C27 H27A 109.5 . . ? Si13 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si13 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si14 C28 H28A 109.5 . . ? Si14 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si14 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si14 C29 H29A 109.5 . . ? Si14 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si14 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si14 C30 H30A 109.5 . . ? Si14 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si14 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 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 C5 Si1 Si2 C6 108.8(4) . . . . ? C4 Si1 Si2 C6 -10.4(3) . . . . ? C3 Si1 Si2 C6 -128.6(3) . . . . ? C5 Si1 Si2 Si6 -3.5(3) . . . . ? C4 Si1 Si2 Si6 -122.6(3) . . . . ? C3 Si1 Si2 Si6 119.2(2) . . . . ? C5 Si1 Si2 Si3 -133.9(3) . . . . ? C4 Si1 Si2 Si3 106.9(3) . . . . ? C3 Si1 Si2 Si3 -11.3(2) . . . . ? C6 Si2 Si3 O2 107.5(2) . . . . ? Si1 Si2 Si3 O2 -8.68(14) . . . . ? Si6 Si2 Si3 O2 -136.48(14) . . . . ? C6 Si2 Si3 C1 -132.3(2) . . . . ? Si1 Si2 Si3 C1 111.52(15) . . . . ? Si6 Si2 Si3 C1 -16.28(17) . . . . ? C6 Si2 Si3 Si4 -13.2(2) . . . . ? Si1 Si2 Si3 Si4 -129.37(8) . . . . ? Si6 Si2 Si3 Si4 102.83(10) . . . . ? O2 Si3 Si4 C7 50.6(2) . . . . ? C1 Si3 Si4 C7 -64.6(2) . . . . ? Si2 Si3 Si4 C7 174.91(18) . . . . ? O2 Si3 Si4 Si5 165.76(12) . . . . ? C1 Si3 Si4 Si5 50.60(16) . . . . ? Si2 Si3 Si4 Si5 -69.91(9) . . . . ? O2 Si3 Si4 Si7 -62.79(13) . . . . ? C1 Si3 Si4 Si7 -177.94(15) . . . . ? Si2 Si3 Si4 Si7 61.54(9) . . . . ? C7 Si4 Si5 C9 -50.5(5) . . . . ? Si7 Si4 Si5 C9 62.2(4) . . . . ? Si3 Si4 Si5 C9 -164.2(4) . . . . ? C7 Si4 Si5 C8 67.5(3) . . . . ? Si7 Si4 Si5 C8 -179.8(3) . . . . ? Si3 Si4 Si5 C8 -46.2(3) . . . . ? C7 Si4 Si5 C10 -169.6(5) . . . . ? Si7 Si4 Si5 C10 -56.9(4) . . . . ? Si3 Si4 Si5 C10 76.7(4) . . . . ? C6 Si2 Si6 C12 79.0(7) . . . . ? Si1 Si2 Si6 C12 -168.3(7) . . . . ? Si3 Si2 Si6 C12 -38.6(7) . . . . ? C6 Si2 Si6 C11 -42.9(3) . . . . ? Si1 Si2 Si6 C11 69.8(3) . . . . ? Si3 Si2 Si6 C11 -160.5(3) . . . . ? C6 Si2 Si6 C13 -160.9(5) . . . . ? Si1 Si2 Si6 C13 -48.2(5) . . . . ? Si3 Si2 Si6 C13 81.5(5) . . . . ? C7 Si4 Si7 C16 -88.9(3) . . . . ? Si5 Si4 Si7 C16 158.3(2) . . . . ? Si3 Si4 Si7 C16 23.0(2) . . . . ? C7 Si4 Si7 C14 28.6(3) . . . . ? Si5 Si4 Si7 C14 -84.2(3) . . . . ? Si3 Si4 Si7 C14 140.6(3) . . . . ? C7 Si4 Si7 C15 146.5(3) . . . . ? Si5 Si4 Si7 C15 33.7(2) . . . . ? Si3 Si4 Si7 C15 -101.6(2) . . . . ? C19 Si8 Si9 C20 65.7(3) . . . . ? C17 Si8 Si9 C20 -173.1(3) . . . . ? C18 Si8 Si9 C20 -51.4(3) . . . . ? C19 Si8 Si9 Si10 -52.3(2) . . . . ? C17 Si8 Si9 Si10 68.8(3) . . . . ? C18 Si8 Si9 Si10 -169.4(2) . . . . ? C19 Si8 Si9 Si13 -178.8(2) . . . . ? C17 Si8 Si9 Si13 -57.6(3) . . . . ? C18 Si8 Si9 Si13 64.1(2) . . . . ? C20 Si9 Si10 O3 -67.9(2) . . . . ? Si8 Si9 Si10 O3 45.71(14) . . . . ? Si13 Si9 Si10 O3 169.35(13) . . . . ? C20 Si9 Si10 C2 172.9(3) . . . . ? Si8 Si9 Si10 C2 -73.50(16) . . . . ? Si13 Si9 Si10 C2 50.14(17) . . . . ? C20 Si9 Si10 Si11 52.9(2) . . . . ? Si8 Si9 Si10 Si11 166.52(7) . . . . ? Si13 Si9 Si10 Si11 -69.84(9) . . . . ? O3 Si10 Si11 C21 121.3(3) . . . . ? C2 Si10 Si11 C21 -118.7(3) . . . . ? Si9 Si10 Si11 C21 1.3(3) . . . . ? O3 Si10 Si11 Si14 9.09(14) . . . . ? C2 Si10 Si11 Si14 129.14(15) . . . . ? Si9 Si10 Si11 Si14 -110.90(8) . . . . ? O3 Si10 Si11 Si12 -114.65(13) . . . . ? C2 Si10 Si11 Si12 5.40(17) . . . . ? Si9 Si10 Si11 Si12 125.37(8) . . . . ? C21 Si11 Si12 C23 -147.0(3) . . . . ? Si14 Si11 Si12 C23 -36.4(3) . . . . ? Si10 Si11 Si12 C23 87.0(3) . . . . ? C21 Si11 Si12 C24 -29.0(4) . . . . ? Si14 Si11 Si12 C24 81.5(3) . . . . ? Si10 Si11 Si12 C24 -155.0(3) . . . . ? C21 Si11 Si12 C22 89.2(3) . . . . ? Si14 Si11 Si12 C22 -160.3(2) . . . . ? Si10 Si11 Si12 C22 -36.8(2) . . . . ? C20 Si9 Si13 C26 -110.6(4) . . . . ? Si8 Si9 Si13 C26 138.7(4) . . . . ? Si10 Si9 Si13 C26 12.3(4) . . . . ? C20 Si9 Si13 C27 12.3(4) . . . . ? Si8 Si9 Si13 C27 -98.4(3) . . . . ? Si10 Si9 Si13 C27 135.2(3) . . . . ? C20 Si9 Si13 C25 128.3(4) . . . . ? Si8 Si9 Si13 C25 17.6(3) . . . . ? Si10 Si9 Si13 C25 -108.8(3) . . . . ? C21 Si11 Si14 C29 -65.8(3) . . . . ? Si12 Si11 Si14 C29 -178.6(3) . . . . ? Si10 Si11 Si14 C29 51.2(3) . . . . ? C21 Si11 Si14 C30 173.5(3) . . . . ? Si12 Si11 Si14 C30 60.8(2) . . . . ? Si10 Si11 Si14 C30 -69.5(2) . . . . ? C21 Si11 Si14 C28 51.9(3) . . . . ? Si12 Si11 Si14 C28 -60.9(3) . . . . ? Si10 Si11 Si14 C28 168.9(3) . . . . ? O2 Al1 O1 Al1 -113.29(16) . . . 3_665 ? O3 Al1 O1 Al1 109.98(17) . . . 3_665 ? O1 Al1 O1 Al1 0.0 3_665 . . 3_665 ? C1 Si3 O2 Al1 0.6(4) . . . . ? Si4 Si3 O2 Al1 -113.7(3) . . . . ? Si2 Si3 O2 Al1 121.6(3) . . . . ? O3 Al1 O2 Si3 -15.2(4) . . . . ? O1 Al1 O2 Si3 119.3(3) 3_665 . . . ? O1 Al1 O2 Si3 -151.4(3) . . . . ? Al1 Al1 O2 Si3 164.4(2) 3_665 . . . ? C2 Si10 O3 Al1 -6.0(4) . . . . ? Si9 Si10 O3 Al1 -126.2(3) . . . . ? Si11 Si10 O3 Al1 115.2(3) . . . . ? O2 Al1 O3 Si10 -3.2(4) . . . . ? O1 Al1 O3 Si10 -139.0(3) 3_665 . . . ? O1 Al1 O3 Si10 132.5(3) . . . . ? Al1 Al1 O3 Si10 177.2(2) 3_665 . . . ? O2 Si3 C1 C2 58.4(3) . . . . ? Si4 Si3 C1 C2 172.3(3) . . . . ? Si2 Si3 C1 C2 -64.6(3) . . . . ? Si3 C1 C2 Si10 -95.3(3) . . . . ? O3 Si10 C2 C1 56.6(3) . . . . ? Si9 Si10 C2 C1 176.6(2) . . . . ? Si11 Si10 C2 C1 -65.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.74 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.418 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.091