# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_f101117e _database_code_depnum_ccdc_archive 'CCDC 912730' #TrackingRef 'web_deposit_cif_file_0_Xu-QiongXiao_1354000663.f101117e.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H48 Cl2 Si9' _chemical_formula_sum 'C16 H48 Cl2 Si9' _chemical_formula_weight 564.25 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.581(4) _cell_length_b 9.272(2) _cell_length_c 22.553(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.961(4) _cell_angle_gamma 90.00 _cell_volume 3448.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5943 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.22 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.087 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 0.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9056 _exptl_absorpt_correction_T_max 0.9418 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13337 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3210 _reflns_number_gt 2654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3210 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Cl1 Cl 0.09854(5) 0.52940(7) 0.25417(3) 0.0764(3) Uani 1 1 d . . . Si1 Si 0.0000 0.38796(7) 0.2500 0.0425(2) Uani 1 2 d S . . Si2 Si 0.00279(3) 0.24863(5) 0.33709(2) 0.04094(19) Uani 1 1 d . . . Si3 Si -0.01801(4) 0.01232(6) 0.29908(3) 0.0508(2) Uani 1 1 d . . . Si4 Si -0.09957(5) 0.32451(7) 0.39526(3) 0.0615(2) Uani 1 1 d . . . Si5 Si 0.13226(4) 0.27235(7) 0.38968(3) 0.0643(2) Uani 1 1 d . . . C1 C -0.20386(18) 0.3065(4) 0.35452(17) 0.0986(10) Uani 1 1 d . . . H1A H -0.2436 0.3329 0.3806 0.148 Uiso 1 1 calc R . . H1B H -0.2126 0.2084 0.3418 0.148 Uiso 1 1 calc R . . H1C H -0.2086 0.3688 0.3204 0.148 Uiso 1 1 calc R . . C2 C -0.0821(2) 0.5178(3) 0.41741(13) 0.0841(9) Uani 1 1 d . . . H2A H -0.1255 0.5504 0.4391 0.126 Uiso 1 1 calc R . . H2B H -0.0802 0.5759 0.3823 0.126 Uiso 1 1 calc R . . H2C H -0.0316 0.5262 0.4421 0.126 Uiso 1 1 calc R . . C3 C -0.0954(3) 0.2081(4) 0.46357(14) 0.1188(14) Uani 1 1 d . . . H3A H -0.0435 0.2187 0.4863 0.178 Uiso 1 1 calc R . . H3B H -0.1032 0.1090 0.4519 0.178 Uiso 1 1 calc R . . H3C H -0.1373 0.2368 0.4874 0.178 Uiso 1 1 calc R . . C4 C 0.1533(2) 0.4631(3) 0.41372(13) 0.0902(10) Uani 1 1 d . . . H4A H 0.1131 0.4943 0.4386 0.135 Uiso 1 1 calc R . . H4B H 0.1517 0.5241 0.3792 0.135 Uiso 1 1 calc R . . H4C H 0.2060 0.4688 0.4357 0.135 Uiso 1 1 calc R . . C5 C 0.21143(18) 0.2130(4) 0.34112(18) 0.1029(11) Uani 1 1 d . . . H5A H 0.2631 0.2071 0.3646 0.154 Uiso 1 1 calc R . . H5B H 0.2145 0.2814 0.3095 0.154 Uiso 1 1 calc R . . H5C H 0.1972 0.1200 0.3245 0.154 Uiso 1 1 calc R . . C6 C 0.1393(2) 0.1562(4) 0.45838(15) 0.1134(13) Uani 1 1 d . . . H6A H 0.1952 0.1442 0.4735 0.170 Uiso 1 1 calc R . . H6B H 0.1157 0.0635 0.4485 0.170 Uiso 1 1 calc R . . H6C H 0.1106 0.2015 0.4882 0.170 Uiso 1 1 calc R . . C7 C 0.0440(2) -0.1241(3) 0.34602(13) 0.0860(9) Uani 1 1 d . . . H7A H 0.0275 -0.1245 0.3856 0.129 Uiso 1 1 calc R . . H7B H 0.1004 -0.0991 0.3478 0.129 Uiso 1 1 calc R . . H7C H 0.0357 -0.2181 0.3286 0.129 Uiso 1 1 calc R . . C8 C -0.12651(18) -0.0433(3) 0.29870(16) 0.0873(9) Uani 1 1 d . . . H8A H -0.1346 -0.1348 0.2790 0.131 Uiso 1 1 calc R . . H8B H -0.1608 0.0277 0.2779 0.131 Uiso 1 1 calc R . . H8C H -0.1398 -0.0515 0.3390 0.131 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 Cl1 0.1098(6) 0.0588(4) 0.0606(4) -0.0020(3) 0.0085(3) -0.0424(4) Si1 0.0602(5) 0.0283(4) 0.0390(4) 0.000 0.0047(3) 0.000 Si2 0.0475(3) 0.0338(3) 0.0414(3) 0.00343(19) 0.0039(2) -0.0013(2) Si3 0.0629(4) 0.0316(3) 0.0592(4) 0.0038(2) 0.0121(3) -0.0041(2) Si4 0.0755(5) 0.0547(4) 0.0580(4) 0.0051(3) 0.0245(3) 0.0061(3) Si5 0.0599(4) 0.0555(4) 0.0727(5) 0.0186(3) -0.0152(3) -0.0107(3) C1 0.0655(18) 0.088(2) 0.146(3) -0.010(2) 0.0299(18) 0.0016(16) C2 0.115(2) 0.0670(16) 0.0713(17) -0.0178(13) 0.0144(16) 0.0122(16) C3 0.177(4) 0.103(3) 0.088(2) 0.0378(19) 0.067(2) 0.022(3) C4 0.105(2) 0.0777(19) 0.0796(19) 0.0016(15) -0.0273(17) -0.0299(17) C5 0.0532(16) 0.089(2) 0.166(3) 0.017(2) 0.0131(18) 0.0020(15) C6 0.121(3) 0.110(2) 0.097(2) 0.051(2) -0.048(2) -0.034(2) C7 0.128(3) 0.0449(14) 0.0853(18) 0.0174(13) 0.0103(17) 0.0136(15) C8 0.0797(19) 0.0729(18) 0.113(2) -0.0196(17) 0.0284(17) -0.0322(15) _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 Cl1 Si1 2.0896(8) . ? Si1 Cl1 2.0896(8) 2 ? Si1 Si2 2.3474(7) 2 ? Si1 Si2 2.3474(7) . ? Si2 Si5 2.3526(10) . ? Si2 Si4 2.3579(9) . ? Si2 Si3 2.3651(9) . ? Si3 C8 1.871(3) . ? Si3 C7 1.884(3) . ? Si3 Si3 2.3519(13) 2 ? Si4 C3 1.877(3) . ? Si4 C2 1.875(3) . ? Si4 C1 1.879(3) . ? Si5 C4 1.872(3) . ? Si5 C5 1.877(3) . ? Si5 C6 1.881(3) . ? 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 Cl1 Si1 Cl1 102.26(6) . 2 ? Cl1 Si1 Si2 109.30(2) . 2 ? Cl1 Si1 Si2 111.12(2) 2 2 ? Cl1 Si1 Si2 111.12(2) . . ? Cl1 Si1 Si2 109.30(2) 2 . ? Si2 Si1 Si2 113.22(4) 2 . ? Si1 Si2 Si5 107.94(3) . . ? Si1 Si2 Si4 110.40(3) . . ? Si5 Si2 Si4 111.31(4) . . ? Si1 Si2 Si3 102.54(3) . . ? Si5 Si2 Si3 111.13(3) . . ? Si4 Si2 Si3 113.07(3) . . ? C8 Si3 C7 106.61(15) . . ? C8 Si3 Si3 109.50(11) . 2 ? C7 Si3 Si3 110.59(10) . 2 ? C8 Si3 Si2 111.16(10) . . ? C7 Si3 Si2 111.56(10) . . ? Si3 Si3 Si2 107.43(2) 2 . ? C3 Si4 C2 109.87(16) . . ? C3 Si4 C1 107.69(19) . . ? C2 Si4 C1 108.93(15) . . ? C3 Si4 Si2 108.51(12) . . ? C2 Si4 Si2 109.45(11) . . ? C1 Si4 Si2 112.35(11) . . ? C4 Si5 C5 108.98(16) . . ? C4 Si5 C6 108.00(16) . . ? C5 Si5 C6 108.99(19) . . ? C4 Si5 Si2 111.55(11) . . ? C5 Si5 Si2 109.58(12) . . ? C6 Si5 Si2 109.69(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.360 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.047 data_f110410b _database_code_depnum_ccdc_archive 'CCDC 912731' #TrackingRef 'web_deposit_cif_file_1_Xu-QiongXiao_1354000663.f110410b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H48 Br2 Si9' _chemical_formula_sum 'C16 H48 Br2 Si9' _chemical_formula_weight 653.17 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.3991(19) _cell_length_b 9.4161(11) _cell_length_c 22.631(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.312(3) _cell_angle_gamma 90.00 _cell_volume 3479.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 8967 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 26.59 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 2.644 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5366 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25067 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3423 _reflns_number_gt 2831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0488P)^2^+6.5990P] 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 3423 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0925 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.10754(2) 0.46143(4) 0.254079(16) 0.06685(15) Uani 1 1 d . . . Si1 Si 0.0000 0.61240(10) 0.2500 0.0371(2) Uani 1 2 d S . . Si2 Si 0.00217(5) 0.74917(8) 0.33712(3) 0.03816(19) Uani 1 1 d . . . Si3 Si -0.02005(6) 0.98061(8) 0.29861(4) 0.0493(2) Uani 1 1 d . . . Si4 Si 0.13272(6) 0.72965(11) 0.38969(5) 0.0619(3) Uani 1 1 d . . . Si5 Si -0.10075(7) 0.67550(11) 0.39643(4) 0.0607(3) Uani 1 1 d . . . C1 C 0.2125(2) 0.7885(5) 0.3417(2) 0.0960(15) Uani 1 1 d . . . H1A H 0.2655 0.7820 0.3635 0.144 Uiso 1 1 calc R . . H1B H 0.2023 0.8851 0.3297 0.144 Uiso 1 1 calc R . . H1C H 0.2110 0.7288 0.3072 0.144 Uiso 1 1 calc R . . C2 C 0.1553(3) 0.5434(5) 0.4150(2) 0.0860(14) Uani 1 1 d . . . H2A H 0.1510 0.4809 0.3813 0.129 Uiso 1 1 calc R . . H2B H 0.1167 0.5150 0.4421 0.129 Uiso 1 1 calc R . . H2C H 0.2098 0.5387 0.4345 0.129 Uiso 1 1 calc R . . C3 C 0.1379(3) 0.8470(6) 0.4572(2) 0.113(2) Uani 1 1 d . . . H3A H 0.1003 0.8127 0.4840 0.170 Uiso 1 1 calc R . . H3B H 0.1235 0.9424 0.4455 0.170 Uiso 1 1 calc R . . H3C H 0.1925 0.8456 0.4766 0.170 Uiso 1 1 calc R . . C4 C -0.0837(3) 0.4854(5) 0.41852(19) 0.0844(13) Uani 1 1 d . . . H4A H -0.1265 0.4550 0.4418 0.127 Uiso 1 1 calc R . . H4B H -0.0318 0.4762 0.4415 0.127 Uiso 1 1 calc R . . H4C H -0.0842 0.4275 0.3836 0.127 Uiso 1 1 calc R . . C5 C -0.0948(4) 0.7893(6) 0.4648(2) 0.122(2) Uani 1 1 d . . . H5A H -0.1062 0.8862 0.4537 0.182 Uiso 1 1 calc R . . H5B H -0.0409 0.7828 0.4851 0.182 Uiso 1 1 calc R . . H5C H -0.1344 0.7571 0.4905 0.182 Uiso 1 1 calc R . . C6 C -0.2062(2) 0.6934(5) 0.3585(2) 0.0936(15) Uani 1 1 d . . . H6A H -0.2454 0.6626 0.3848 0.140 Uiso 1 1 calc R . . H6B H -0.2111 0.6359 0.3233 0.140 Uiso 1 1 calc R . . H6C H -0.2163 0.7910 0.3479 0.140 Uiso 1 1 calc R . . C7 C 0.0399(3) 1.1164(4) 0.3463(2) 0.0883(14) Uani 1 1 d . . . H7A H 0.0310 1.2091 0.3292 0.133 Uiso 1 1 calc R . . H7B H 0.0972 1.0938 0.3484 0.133 Uiso 1 1 calc R . . H7C H 0.0220 1.1154 0.3855 0.133 Uiso 1 1 calc R . . C8 C -0.1303(3) 1.0306(5) 0.2968(2) 0.0894(14) Uani 1 1 d . . . H8A H -0.1453 1.0394 0.3366 0.134 Uiso 1 1 calc R . . H8B H -0.1632 0.9585 0.2762 0.134 Uiso 1 1 calc R . . H8C H -0.1391 1.1196 0.2765 0.134 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 Br1 0.0850(3) 0.0543(2) 0.0609(2) 0.00075(15) 0.00479(18) 0.03360(18) Si1 0.0466(6) 0.0259(5) 0.0386(5) 0.000 0.0030(4) 0.000 Si2 0.0416(4) 0.0316(4) 0.0411(4) -0.0032(3) 0.0026(3) 0.0005(3) Si3 0.0594(5) 0.0298(4) 0.0597(5) -0.0033(4) 0.0114(4) 0.0038(4) Si4 0.0549(5) 0.0568(6) 0.0698(6) -0.0195(5) -0.0164(5) 0.0099(4) Si5 0.0724(6) 0.0539(5) 0.0593(6) -0.0081(4) 0.0253(5) -0.0102(5) C1 0.050(2) 0.080(3) 0.157(5) -0.021(3) 0.007(2) -0.008(2) C2 0.099(3) 0.080(3) 0.073(3) 0.001(2) -0.024(2) 0.030(2) C3 0.115(4) 0.112(4) 0.103(4) -0.058(3) -0.049(3) 0.031(3) C4 0.110(4) 0.074(3) 0.069(3) 0.020(2) 0.009(2) -0.019(3) C5 0.168(6) 0.113(4) 0.094(3) -0.048(3) 0.067(4) -0.035(4) C6 0.060(2) 0.078(3) 0.148(4) 0.001(3) 0.036(3) -0.005(2) C7 0.134(4) 0.042(2) 0.089(3) -0.017(2) 0.007(3) -0.017(2) C8 0.083(3) 0.077(3) 0.113(4) 0.024(3) 0.037(3) 0.039(2) _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 Br1 Si1 2.2604(7) . ? Si1 Br1 2.2604(7) 2 ? Si1 Si2 2.3526(9) . ? Si1 Si2 2.3526(9) 2 ? Si2 Si5 2.3560(12) . ? Si2 Si4 2.3581(12) . ? Si2 Si3 2.3628(11) . ? Si3 C8 1.865(4) . ? Si3 C7 1.889(4) . ? Si3 Si3 2.3541(18) 2 ? Si4 C1 1.861(5) . ? Si4 C2 1.872(4) . ? Si4 C3 1.881(4) . ? Si5 C6 1.865(5) . ? Si5 C4 1.873(4) . ? Si5 C5 1.876(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 Si1 Br1 102.06(5) 2 . ? Br1 Si1 Si2 109.25(2) 2 . ? Br1 Si1 Si2 111.03(2) . . ? Br1 Si1 Si2 111.03(2) 2 2 ? Br1 Si1 Si2 109.25(2) . 2 ? Si2 Si1 Si2 113.62(5) . 2 ? Si1 Si2 Si5 111.11(4) . . ? Si1 Si2 Si4 108.83(4) . . ? Si5 Si2 Si4 110.76(5) . . ? Si1 Si2 Si3 101.88(4) . . ? Si5 Si2 Si3 112.80(5) . . ? Si4 Si2 Si3 111.09(5) . . ? C8 Si3 C7 107.1(2) . . ? C8 Si3 Si3 109.46(17) . 2 ? C7 Si3 Si3 110.98(16) . 2 ? C8 Si3 Si2 110.93(14) . . ? C7 Si3 Si2 111.07(15) . . ? Si3 Si3 Si2 107.33(3) 2 . ? C1 Si4 C2 109.1(2) . . ? C1 Si4 C3 108.5(3) . . ? C2 Si4 C3 108.0(2) . . ? C1 Si4 Si2 109.71(16) . . ? C2 Si4 Si2 111.85(16) . . ? C3 Si4 Si2 109.55(16) . . ? C6 Si5 C4 108.5(2) . . ? C6 Si5 C5 107.6(3) . . ? C4 Si5 C5 109.3(3) . . ? C6 Si5 Si2 113.18(15) . . ? C4 Si5 Si2 109.68(16) . . ? C5 Si5 Si2 108.42(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.022 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.066 data_f111208a _database_code_depnum_ccdc_archive 'CCDC 912732' #TrackingRef '15697_web_deposit_cif_file_2_Xu-QiongXiao_1354000663.f111208a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H81 K O3 Si10' _chemical_formula_weight 821.96 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' Si Si 0.0817 0.0704 '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' K K 0.2009 0.2494 '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.925(3) _cell_length_b 25.574(7) _cell_length_c 18.928(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.712(5) _cell_angle_gamma 90.00 _cell_volume 5252(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6686 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.71 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.354 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.377 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details sadabs _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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34999 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.55 _reflns_number_total 12071 _reflns_number_gt 7287 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^2^+0.3019P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12071 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1210 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1892 _refine_ls_wR_factor_gt 0.1574 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 Si1 Si 0.30198(8) 0.55936(4) 0.76346(5) 0.0249(2) Uani 1 1 d . . . Si2 Si 0.29384(8) 0.59538(4) 0.64697(5) 0.0259(2) Uani 1 1 d . . . Si3 Si 0.11106(9) 0.64521(4) 0.62975(5) 0.0344(2) Uani 1 1 d . . . Si4 Si 0.01402(9) 0.62964(4) 0.73195(5) 0.0342(2) Uani 1 1 d . . . Si5 Si 0.17690(9) 0.61599(4) 0.82308(5) 0.0283(2) Uani 1 1 d . . . Si6 Si 0.26477(10) 0.51992(4) 0.57603(5) 0.0341(2) Uani 1 1 d . . . Si7 Si 0.44796(11) 0.64396(5) 0.59995(6) 0.0419(3) Uani 1 1 d . . . Si8 Si 0.23637(10) 0.69593(4) 0.87797(6) 0.0421(3) Uani 1 1 d . . . Si9 Si 0.09239(11) 0.56902(5) 0.91264(6) 0.0457(3) Uani 1 1 d . . . Si10 Si 0.50324(9) 0.56362(4) 0.82045(5) 0.0337(2) Uani 1 1 d . . . K1 K 0.21102(9) 0.43125(3) 0.75958(5) 0.0497(3) Uani 1 1 d . . . O1 O -0.0220(3) 0.39299(15) 0.74882(19) 0.0759(10) Uani 1 1 d . . . O2 O 0.2745(4) 0.36273(14) 0.8608(2) 0.0864(13) Uani 1 1 d . . . O3 O 0.2735(3) 0.35264(13) 0.67909(19) 0.0689(9) Uani 1 1 d . . . C1 C 0.1175(5) 0.4866(2) 0.5937(3) 0.0451(10) Uani 1 1 d . . . C2 C 0.3955(4) 0.47295(17) 0.6005(3) 0.0527(11) Uani 1 1 d . . . H2A H 0.3821 0.4417 0.5725 0.079 Uiso 1 1 calc R . . H2B H 0.3994 0.4643 0.6500 0.079 Uiso 1 1 calc R . . H2C H 0.4716 0.4889 0.5913 0.079 Uiso 1 1 calc R . . C3 C 0.2531(4) 0.53004(19) 0.4770(2) 0.0535(11) Uani 1 1 d . . . H3A H 0.3319 0.5404 0.4641 0.080 Uiso 1 1 calc R . . H3B H 0.1935 0.5568 0.4632 0.080 Uiso 1 1 calc R . . H3C H 0.2279 0.4980 0.4532 0.080 Uiso 1 1 calc R . . C4 C 0.5951(4) 0.6069(2) 0.6003(3) 0.0653(14) Uani 1 1 d . . . H4A H 0.6523 0.6271 0.5767 0.098 Uiso 1 1 calc R . . H4B H 0.5793 0.5743 0.5760 0.098 Uiso 1 1 calc R . . H4C H 0.6295 0.6004 0.6485 0.098 Uiso 1 1 calc R . . C5 C 0.3956(6) 0.6606(2) 0.5037(3) 0.0735(16) Uani 1 1 d . . . H5A H 0.4554 0.6830 0.4858 0.110 Uiso 1 1 calc R . . H5B H 0.3176 0.6782 0.5005 0.110 Uiso 1 1 calc R . . H5C H 0.3874 0.6290 0.4761 0.110 Uiso 1 1 calc R . . C6 C 0.4855(5) 0.70738(18) 0.6476(3) 0.0689(14) Uani 1 1 d . . . H6A H 0.5052 0.7008 0.6976 0.103 Uiso 1 1 calc R . . H6B H 0.4157 0.7303 0.6402 0.103 Uiso 1 1 calc R . . H6C H 0.5548 0.7234 0.6294 0.103 Uiso 1 1 calc R . . C7 C 0.0052(4) 0.6288(2) 0.5465(2) 0.0598(13) Uani 1 1 d . . . H7A H -0.0654 0.6514 0.5429 0.090 Uiso 1 1 calc R . . H7B H -0.0213 0.5931 0.5487 0.090 Uiso 1 1 calc R . . H7C H 0.0484 0.6335 0.5056 0.090 Uiso 1 1 calc R . . C8 C 0.1426(5) 0.71841(17) 0.6230(2) 0.0569(12) Uani 1 1 d . . . H8A H 0.1741 0.7257 0.5788 0.085 Uiso 1 1 calc R . . H8B H 0.2020 0.7289 0.6618 0.085 Uiso 1 1 calc R . . H8C H 0.0674 0.7375 0.6250 0.085 Uiso 1 1 calc R . . C9 C -0.0825(4) 0.56816(18) 0.7166(2) 0.0520(11) Uani 1 1 d . . . H9A H -0.1364 0.5652 0.7529 0.078 Uiso 1 1 calc R . . H9B H -0.0293 0.5382 0.7182 0.078 Uiso 1 1 calc R . . H9C H -0.1306 0.5700 0.6708 0.078 Uiso 1 1 calc R . . C10 C -0.0950(4) 0.68538(19) 0.7460(2) 0.0559(12) Uani 1 1 d . . . H10A H -0.1582 0.6872 0.7063 0.084 Uiso 1 1 calc R . . H10B H -0.0500 0.7177 0.7499 0.084 Uiso 1 1 calc R . . H10C H -0.1320 0.6795 0.7888 0.084 Uiso 1 1 calc R . . C11 C 0.3661(4) 0.68751(18) 0.9514(2) 0.0557(12) Uani 1 1 d . . . H11A H 0.4405 0.6793 0.9313 0.084 Uiso 1 1 calc R . . H11B H 0.3467 0.6596 0.9821 0.084 Uiso 1 1 calc R . . H11C H 0.3774 0.7193 0.9782 0.084 Uiso 1 1 calc R . . C12 C 0.2897(6) 0.74480(18) 0.8154(3) 0.0734(16) Uani 1 1 d . . . H12A H 0.3277 0.7737 0.8419 0.110 Uiso 1 1 calc R . . H12B H 0.2205 0.7571 0.7839 0.110 Uiso 1 1 calc R . . H12C H 0.3485 0.7288 0.7882 0.110 Uiso 1 1 calc R . . C13 C 0.1045(5) 0.7270(2) 0.9188(3) 0.0751(17) Uani 1 1 d . . . H13A H 0.0862 0.7065 0.9588 0.113 Uiso 1 1 calc R . . H13B H 0.0331 0.7284 0.8841 0.113 Uiso 1 1 calc R . . H13C H 0.1271 0.7618 0.9343 0.113 Uiso 1 1 calc R . . C14 C 0.1860(5) 0.5730(3) 1.0030(2) 0.0802(18) Uani 1 1 d . . . H14A H 0.1825 0.6080 1.0211 0.120 Uiso 1 1 calc R . . H14B H 0.2702 0.5640 0.9987 0.120 Uiso 1 1 calc R . . H14C H 0.1531 0.5492 1.0350 0.120 Uiso 1 1 calc R . . C15 C 0.0847(8) 0.4972(3) 0.8903(4) 0.083(2) Uani 1 1 d . . . C16 C -0.0687(5) 0.5916(2) 0.9239(3) 0.0766(17) Uani 1 1 d . . . H16A H -0.0968 0.5740 0.9638 0.115 Uiso 1 1 calc R . . H16B H -0.1229 0.5836 0.8816 0.115 Uiso 1 1 calc R . . H16C H -0.0684 0.6287 0.9320 0.115 Uiso 1 1 calc R . . C17 C 0.5036(4) 0.5440(2) 0.9169(2) 0.0604(13) Uani 1 1 d . . . H17A H 0.5870 0.5407 0.9388 0.091 Uiso 1 1 calc R . . H17B H 0.4621 0.5110 0.9195 0.091 Uiso 1 1 calc R . . H17C H 0.4617 0.5701 0.9414 0.091 Uiso 1 1 calc R . . C18 C 0.6007(4) 0.51295(18) 0.7816(3) 0.0575(12) Uani 1 1 d . . . H18A H 0.6021 0.5197 0.7318 0.086 Uiso 1 1 calc R . . H18B H 0.5666 0.4789 0.7877 0.086 Uiso 1 1 calc R . . H18C H 0.6832 0.5144 0.8055 0.086 Uiso 1 1 calc R . . C19 C 0.5912(4) 0.62683(18) 0.8197(3) 0.0551(12) Uani 1 1 d . . . H19A H 0.6655 0.6244 0.8521 0.083 Uiso 1 1 calc R . . H19B H 0.5413 0.6549 0.8342 0.083 Uiso 1 1 calc R . . H19C H 0.6116 0.6335 0.7726 0.083 Uiso 1 1 calc R . . C20 C -0.1096(5) 0.3974(4) 0.6876(3) 0.107(3) Uani 1 1 d . . . H20A H -0.1009 0.3680 0.6561 0.129 Uiso 1 1 calc R . . H20B H -0.0950 0.4293 0.6622 0.129 Uiso 1 1 calc R . . C21 C -0.2326(5) 0.3980(3) 0.7083(3) 0.0847(18) Uani 1 1 d . . . H21A H -0.2853 0.3736 0.6799 0.102 Uiso 1 1 calc R . . H21B H -0.2681 0.4327 0.7024 0.102 Uiso 1 1 calc R . . C22 C -0.2185(6) 0.3824(3) 0.7847(3) 0.095(2) Uani 1 1 d . . . H22A H -0.2661 0.3512 0.7915 0.115 Uiso 1 1 calc R . . H22B H -0.2458 0.4102 0.8140 0.115 Uiso 1 1 calc R . . C23 C -0.0851(6) 0.3724(3) 0.8029(4) 0.103(2) Uani 1 1 d . . . H23A H -0.0561 0.3887 0.8480 0.124 Uiso 1 1 calc R . . H23B H -0.0703 0.3350 0.8073 0.124 Uiso 1 1 calc R . . C24 C 0.2276(7) 0.3117(2) 0.8502(3) 0.0800(18) Uani 1 1 d . . . C25 C 0.2066(7) 0.2931(3) 0.9230(3) 0.099(2) Uani 1 1 d . . . H25A H 0.1248 0.3026 0.9337 0.119 Uiso 1 1 calc R . . H25B H 0.2160 0.2555 0.9268 0.119 Uiso 1 1 calc R . . C26 C 0.3004(6) 0.3196(3) 0.9706(3) 0.094(2) Uani 1 1 d . . . H26A H 0.3717 0.2972 0.9820 0.113 Uiso 1 1 calc R . . H26B H 0.2685 0.3293 1.0145 0.113 Uiso 1 1 calc R . . C27 C 0.3340(8) 0.3670(3) 0.9312(4) 0.130(3) Uani 1 1 d . . . H27A H 0.3068 0.3983 0.9537 0.155 Uiso 1 1 calc R . . H27B H 0.4226 0.3689 0.9310 0.155 Uiso 1 1 calc R . . C28 C 0.1816(6) 0.3251(2) 0.6369(3) 0.0885(19) Uani 1 1 d . . . H28A H 0.1348 0.3485 0.6038 0.106 Uiso 1 1 calc R . . H28B H 0.1256 0.3088 0.6665 0.106 Uiso 1 1 calc R . . C29 C 0.2438(7) 0.2850(3) 0.5982(4) 0.113(3) Uani 1 1 d . . . H29A H 0.1966 0.2528 0.5941 0.136 Uiso 1 1 calc R . . H29B H 0.2562 0.2971 0.5510 0.136 Uiso 1 1 calc R . . C30 C 0.3599(7) 0.2777(3) 0.6418(5) 0.125(3) Uani 1 1 d . . . H30A H 0.4236 0.2682 0.6125 0.150 Uiso 1 1 calc R . . H30B H 0.3532 0.2501 0.6762 0.150 Uiso 1 1 calc R . . C31 C 0.3897(5) 0.3271(2) 0.6777(4) 0.0809(17) Uani 1 1 d . . . H31A H 0.4295 0.3213 0.7256 0.097 Uiso 1 1 calc R . . H31B H 0.4439 0.3478 0.6518 0.097 Uiso 1 1 calc R . . H24A H 0.126(6) 0.320(3) 0.829(4) 0.12(2) Uiso 1 1 d . . . H24B H 0.307(6) 0.290(3) 0.832(3) 0.11(2) Uiso 1 1 d . . . H15A H 0.049(5) 0.490(2) 0.924(3) 0.080(18) Uiso 1 1 d . . . H15B H 0.036(6) 0.490(2) 0.845(4) 0.09(2) Uiso 1 1 d . . . H15C H 0.157(13) 0.469(5) 0.897(7) 0.28(7) Uiso 1 1 d . . . H1A H 0.106(3) 0.4930(14) 0.637(2) 0.030(10) Uiso 1 1 d . . . H1B H 0.044(5) 0.502(2) 0.565(3) 0.081(17) Uiso 1 1 d . . . H1C H 0.124(5) 0.460(2) 0.583(3) 0.069(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0228(4) 0.0246(5) 0.0265(5) 0.0005(4) -0.0006(3) -0.0003(4) Si2 0.0248(5) 0.0253(5) 0.0270(5) 0.0014(4) 0.0007(4) 0.0003(4) Si3 0.0325(5) 0.0384(6) 0.0301(5) 0.0009(4) -0.0058(4) 0.0101(5) Si4 0.0233(5) 0.0413(6) 0.0365(5) -0.0044(4) -0.0026(4) 0.0057(4) Si5 0.0255(5) 0.0315(5) 0.0275(5) -0.0025(4) 0.0004(4) 0.0008(4) Si6 0.0371(6) 0.0346(6) 0.0302(5) -0.0050(4) 0.0016(4) 0.0021(4) Si7 0.0403(6) 0.0406(6) 0.0462(6) 0.0102(5) 0.0116(5) -0.0048(5) Si8 0.0412(6) 0.0371(6) 0.0446(6) -0.0133(5) -0.0090(5) 0.0070(5) Si9 0.0431(6) 0.0581(8) 0.0387(6) 0.0049(5) 0.0165(5) 0.0012(6) Si10 0.0259(5) 0.0362(6) 0.0371(5) 0.0014(4) -0.0048(4) 0.0057(4) K1 0.0625(6) 0.0291(5) 0.0555(6) 0.0022(4) -0.0020(5) -0.0040(4) O1 0.065(2) 0.094(3) 0.064(2) 0.016(2) -0.0128(18) -0.023(2) O2 0.128(3) 0.053(2) 0.067(2) 0.0103(18) -0.037(2) -0.011(2) O3 0.073(2) 0.053(2) 0.079(2) -0.0147(18) 0.0008(19) 0.0097(18) C1 0.047(3) 0.040(3) 0.046(3) -0.006(2) -0.006(2) -0.009(2) C2 0.057(3) 0.041(2) 0.059(3) -0.005(2) 0.005(2) 0.010(2) C3 0.062(3) 0.062(3) 0.036(2) -0.009(2) 0.005(2) 0.000(2) C4 0.042(2) 0.077(4) 0.082(4) 0.012(3) 0.024(2) 0.001(2) C5 0.097(4) 0.072(4) 0.054(3) 0.028(3) 0.020(3) -0.001(3) C6 0.065(3) 0.047(3) 0.095(4) 0.001(3) 0.010(3) -0.018(3) C7 0.057(3) 0.072(3) 0.044(2) -0.008(2) -0.020(2) 0.022(2) C8 0.068(3) 0.043(3) 0.059(3) 0.014(2) 0.002(2) 0.019(2) C9 0.031(2) 0.061(3) 0.062(3) -0.008(2) -0.0034(19) -0.010(2) C10 0.043(2) 0.067(3) 0.056(3) -0.006(2) 0.002(2) 0.020(2) C11 0.054(3) 0.051(3) 0.056(3) -0.014(2) -0.020(2) -0.004(2) C12 0.100(4) 0.040(3) 0.073(3) -0.002(2) -0.016(3) -0.011(3) C13 0.059(3) 0.083(4) 0.080(4) -0.041(3) -0.005(3) 0.023(3) C14 0.073(4) 0.129(5) 0.041(3) 0.021(3) 0.016(2) -0.012(4) C15 0.126(6) 0.067(4) 0.064(4) 0.009(3) 0.045(4) -0.018(4) C16 0.055(3) 0.113(5) 0.068(3) 0.015(3) 0.035(3) 0.014(3) C17 0.055(3) 0.080(3) 0.042(2) 0.008(2) -0.012(2) 0.010(3) C18 0.039(2) 0.053(3) 0.078(3) -0.001(2) -0.003(2) 0.015(2) C19 0.034(2) 0.060(3) 0.068(3) -0.008(2) -0.006(2) -0.010(2) C20 0.061(4) 0.191(8) 0.065(4) 0.024(4) -0.011(3) -0.027(5) C21 0.070(4) 0.102(5) 0.081(4) 0.000(4) 0.003(3) 0.029(4) C22 0.099(5) 0.101(5) 0.091(5) 0.021(4) 0.035(4) 0.034(4) C23 0.093(5) 0.129(6) 0.085(5) 0.037(4) -0.001(4) -0.022(4) C24 0.116(6) 0.055(3) 0.061(3) 0.002(3) -0.023(3) 0.009(4) C25 0.117(5) 0.105(5) 0.070(4) 0.017(4) -0.011(4) -0.038(4) C26 0.089(4) 0.130(6) 0.057(3) 0.009(4) -0.017(3) -0.014(4) C27 0.176(8) 0.106(6) 0.086(5) 0.018(4) -0.072(5) -0.039(5) C28 0.078(4) 0.083(4) 0.098(5) -0.035(4) -0.018(3) 0.020(3) C29 0.093(5) 0.121(6) 0.122(6) -0.060(5) 0.001(4) 0.028(5) C30 0.094(5) 0.077(5) 0.207(9) -0.040(5) 0.034(6) 0.020(4) C31 0.064(4) 0.072(4) 0.102(5) 0.001(3) -0.008(3) 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 Si1 Si10 2.3356(14) . ? Si1 Si5 2.3661(13) . ? Si1 Si2 2.3818(14) . ? Si1 K1 3.4220(15) . ? Si2 Si7 2.3495(14) . ? Si2 Si6 2.3512(14) . ? Si2 Si3 2.3591(14) . ? Si3 C7 1.890(4) . ? Si3 C8 1.910(5) . ? Si3 Si4 2.3460(15) . ? Si4 C9 1.896(4) . ? Si4 C10 1.896(4) . ? Si4 Si5 2.3549(14) . ? Si5 Si8 2.3502(15) . ? Si5 Si9 2.3528(15) . ? Si6 C3 1.882(4) . ? Si6 C1 1.885(5) . ? Si6 C2 1.882(4) . ? Si7 C4 1.865(5) . ? Si7 C6 1.878(5) . ? Si7 C5 1.892(5) . ? Si8 C12 1.861(5) . ? Si8 C11 1.878(4) . ? Si8 C13 1.888(5) . ? Si9 C16 1.888(5) . ? Si9 C15 1.884(7) . ? Si9 C14 1.890(5) . ? Si10 C19 1.881(4) . ? Si10 C18 1.881(4) . ? Si10 C17 1.894(4) . ? K1 O2 2.629(4) . ? K1 O3 2.659(3) . ? K1 O1 2.713(4) . ? O1 C23 1.402(7) . ? O1 C20 1.417(6) . ? O2 C24 1.408(7) . ? O2 C27 1.418(7) . ? O3 C28 1.398(6) . ? O3 C31 1.430(6) . ? C20 C21 1.443(8) . ? C21 C22 1.490(8) . ? C22 C23 1.480(9) . ? C24 C25 1.500(8) . ? C25 C26 1.451(8) . ? C26 C27 1.491(9) . ? C28 C29 1.471(8) . ? C29 C30 1.442(10) . ? C30 C31 1.454(9) . ? 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 Si10 Si1 Si5 108.43(5) . . ? Si10 Si1 Si2 109.93(5) . . ? Si5 Si1 Si2 104.10(5) . . ? Si10 Si1 K1 108.05(4) . . ? Si5 Si1 K1 114.45(4) . . ? Si2 Si1 K1 111.78(4) . . ? Si7 Si2 Si6 105.82(5) . . ? Si7 Si2 Si3 107.13(6) . . ? Si6 Si2 Si3 107.99(5) . . ? Si7 Si2 Si1 127.18(5) . . ? Si6 Si2 Si1 101.49(5) . . ? Si3 Si2 Si1 106.03(5) . . ? C7 Si3 C8 105.1(2) . . ? C7 Si3 Si4 110.99(17) . . ? C8 Si3 Si4 108.89(15) . . ? C7 Si3 Si2 114.88(15) . . ? C8 Si3 Si2 112.48(16) . . ? Si4 Si3 Si2 104.55(5) . . ? C9 Si4 C10 107.3(2) . . ? C9 Si4 Si3 108.12(15) . . ? C10 Si4 Si3 109.85(16) . . ? C9 Si4 Si5 110.39(15) . . ? C10 Si4 Si5 116.24(15) . . ? Si3 Si4 Si5 104.69(5) . . ? Si8 Si5 Si9 103.72(6) . . ? Si8 Si5 Si4 109.94(5) . . ? Si9 Si5 Si4 106.08(6) . . ? Si8 Si5 Si1 126.73(6) . . ? Si9 Si5 Si1 109.16(6) . . ? Si4 Si5 Si1 99.81(5) . . ? C3 Si6 C1 106.2(2) . . ? C3 Si6 C2 107.1(2) . . ? C1 Si6 C2 107.8(2) . . ? C3 Si6 Si2 116.41(15) . . ? C1 Si6 Si2 109.35(18) . . ? C2 Si6 Si2 109.61(15) . . ? C4 Si7 C6 107.3(3) . . ? C4 Si7 C5 106.3(2) . . ? C6 Si7 C5 107.0(3) . . ? C4 Si7 Si2 112.69(16) . . ? C6 Si7 Si2 113.63(17) . . ? C5 Si7 Si2 109.52(18) . . ? C12 Si8 C11 106.4(2) . . ? C12 Si8 C13 106.8(3) . . ? C11 Si8 C13 106.9(2) . . ? C12 Si8 Si5 113.19(17) . . ? C11 Si8 Si5 111.91(15) . . ? C13 Si8 Si5 111.22(18) . . ? C16 Si9 C15 107.8(3) . . ? C16 Si9 C14 107.1(2) . . ? C15 Si9 C14 105.2(3) . . ? C16 Si9 Si5 112.01(17) . . ? C15 Si9 Si5 110.29(19) . . ? C14 Si9 Si5 114.05(17) . . ? C19 Si10 C18 106.0(2) . . ? C19 Si10 C17 107.0(2) . . ? C18 Si10 C17 104.9(2) . . ? C19 Si10 Si1 119.37(15) . . ? C18 Si10 Si1 109.44(16) . . ? C17 Si10 Si1 109.18(16) . . ? O2 K1 O3 81.37(12) . . ? O2 K1 O1 88.83(13) . . ? O3 K1 O1 89.19(12) . . ? O2 K1 Si1 124.84(9) . . ? O3 K1 Si1 130.00(9) . . ? O1 K1 Si1 127.92(9) . . ? C23 O1 C20 106.5(4) . . ? C23 O1 K1 128.2(3) . . ? C20 O1 K1 124.8(3) . . ? C24 O2 C27 108.9(4) . . ? C24 O2 K1 117.0(3) . . ? C27 O2 K1 133.4(4) . . ? C28 O3 C31 109.8(4) . . ? C28 O3 K1 119.5(3) . . ? C31 O3 K1 130.1(3) . . ? O1 C20 C21 109.9(5) . . ? C20 C21 C22 105.5(5) . . ? C21 C22 C23 105.0(5) . . ? O1 C23 C22 108.6(5) . . ? O2 C24 C25 104.8(5) . . ? C26 C25 C24 104.5(5) . . ? C25 C26 C27 105.4(5) . . ? O2 C27 C26 107.2(5) . . ? O3 C28 C29 107.0(5) . . ? C30 C29 C28 103.4(6) . . ? C29 C30 C31 106.7(6) . . ? O3 C31 C30 104.8(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.564 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.078 data_f110510b _database_code_depnum_ccdc_archive 'CCDC 912733' #TrackingRef 'web_deposit_cif_file_3_Xu-QiongXiao_1354000663.f110510b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H96 Si18' _chemical_formula_sum 'C32 H96 Si18' _chemical_formula_weight 986.71 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.289(2) _cell_length_b 12.4843(10) _cell_length_c 20.2377(16) _cell_angle_alpha 90.00 _cell_angle_beta 113.0010(10) _cell_angle_gamma 90.00 _cell_volume 6346.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9941 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.033 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8949 _exptl_absorpt_correction_T_max 0.9560 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26224 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7254 _reflns_number_gt 5858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^2^+1.3003P] 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 7254 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1114 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.899 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.05637(12) 1.17649(19) 0.34566(16) 0.0768(8) Uani 1 1 d . . . H1A H 0.0245 1.1501 0.3493 0.115 Uiso 1 1 calc R . . H1B H 0.0473 1.2153 0.3015 0.115 Uiso 1 1 calc R . . H1C H 0.0746 1.2232 0.3854 0.115 Uiso 1 1 calc R . . C2 C 0.13752(9) 1.0190(2) 0.44286(12) 0.0599(6) Uani 1 1 d . . . H2A H 0.1615 0.9615 0.4449 0.090 Uiso 1 1 calc R . . H2B H 0.1125 0.9952 0.4625 0.090 Uiso 1 1 calc R . . H2C H 0.1574 1.0786 0.4702 0.090 Uiso 1 1 calc R . . C3 C 0.15377(12) 1.1153(3) 0.31911(17) 0.0840(9) Uani 1 1 d . . . H3A H 0.1782 1.1578 0.3573 0.126 Uiso 1 1 calc R . . H3B H 0.1377 1.1589 0.2770 0.126 Uiso 1 1 calc R . . H3C H 0.1725 1.0570 0.3087 0.126 Uiso 1 1 calc R . . C4 C 0.02006(9) 0.6453(2) 0.43008(13) 0.0565(5) Uani 1 1 d . . . H4A H -0.0134 0.6538 0.3901 0.085 Uiso 1 1 calc R . . H4B H 0.0237 0.7000 0.4650 0.085 Uiso 1 1 calc R . . H4C H 0.0213 0.5762 0.4514 0.085 Uiso 1 1 calc R . . C5 C 0.09715(9) 0.51678(19) 0.39141(14) 0.0606(6) Uani 1 1 d . . . H5A H 0.1114 0.4847 0.4382 0.091 Uiso 1 1 calc R . . H5B H 0.1240 0.5179 0.3718 0.091 Uiso 1 1 calc R . . H5C H 0.0672 0.4758 0.3606 0.091 Uiso 1 1 calc R . . C6 C 0.13096(9) 0.7286(2) 0.47079(12) 0.0592(6) Uani 1 1 d . . . H6A H 0.1170 0.7904 0.4857 0.089 Uiso 1 1 calc R . . H6B H 0.1571 0.7507 0.4527 0.089 Uiso 1 1 calc R . . H6C H 0.1472 0.6816 0.5110 0.089 Uiso 1 1 calc R . . C7 C 0.04764(12) 0.4220(2) 0.1882(2) 0.0953(11) Uani 1 1 d . . . H7A H 0.0525 0.3460 0.1870 0.143 Uiso 1 1 calc R . . H7B H 0.0202 0.4447 0.1439 0.143 Uiso 1 1 calc R . . H7C H 0.0375 0.4395 0.2273 0.143 Uiso 1 1 calc R . . C8 C 0.16508(11) 0.4077(2) 0.2658(2) 0.0845(9) Uani 1 1 d . . . H8A H 0.1631 0.3367 0.2467 0.127 Uiso 1 1 calc R . . H8B H 0.1605 0.4045 0.3105 0.127 Uiso 1 1 calc R . . H8C H 0.1992 0.4384 0.2737 0.127 Uiso 1 1 calc R . . C9 C 0.12131(18) 0.4830(3) 0.11455(19) 0.1107(13) Uani 1 1 d . . . H9A H 0.1545 0.5158 0.1203 0.166 Uiso 1 1 calc R . . H9B H 0.0927 0.5193 0.0774 0.166 Uiso 1 1 calc R . . H9C H 0.1217 0.4091 0.1016 0.166 Uiso 1 1 calc R . . C10 C 0.22745(9) 0.6036(2) 0.40815(15) 0.0728(7) Uani 1 1 d . . . H10A H 0.2643 0.6182 0.4366 0.109 Uiso 1 1 calc R . . H10B H 0.2234 0.5298 0.3937 0.109 Uiso 1 1 calc R . . H10C H 0.2066 0.6179 0.4360 0.109 Uiso 1 1 calc R . . C11 C 0.24954(10) 0.6569(2) 0.27957(18) 0.0753(8) Uani 1 1 d . . . H11A H 0.2418 0.7026 0.2385 0.113 Uiso 1 1 calc R . . H11B H 0.2442 0.5835 0.2643 0.113 Uiso 1 1 calc R . . H11C H 0.2859 0.6671 0.3120 0.113 Uiso 1 1 calc R . . C12 C 0.21787(12) 0.8322(2) 0.36134(17) 0.0772(8) Uani 1 1 d . . . H12A H 0.2465 0.8320 0.4078 0.116 Uiso 1 1 calc R . . H12B H 0.1865 0.8616 0.3650 0.116 Uiso 1 1 calc R . . H12C H 0.2276 0.8750 0.3290 0.116 Uiso 1 1 calc R . . C13 C 0.18140(9) 0.8673(2) 0.16878(16) 0.0702(7) Uani 1 1 d . . . H13A H 0.2066 0.8145 0.1678 0.105 Uiso 1 1 calc R . . H13B H 0.1941 0.9010 0.2151 0.105 Uiso 1 1 calc R . . H13C H 0.1771 0.9203 0.1325 0.105 Uiso 1 1 calc R . . C14 C 0.09562(12) 0.7515(2) 0.05574(13) 0.0693(7) Uani 1 1 d . . . H14A H 0.0905 0.8116 0.0242 0.104 Uiso 1 1 calc R . . H14B H 0.0631 0.7114 0.0417 0.104 Uiso 1 1 calc R . . H14C H 0.1233 0.7065 0.0530 0.104 Uiso 1 1 calc R . . C15 C 0.08568(10) 1.07120(19) 0.13599(14) 0.0620(6) Uani 1 1 d . . . H15A H 0.0838 1.0710 0.0876 0.093 Uiso 1 1 calc R . . H15B H 0.1221 1.0793 0.1687 0.093 Uiso 1 1 calc R . . H15C H 0.0650 1.1297 0.1421 0.093 Uiso 1 1 calc R . . C16 C -0.00812(8) 0.92709(19) 0.07748(11) 0.0520(5) Uani 1 1 d . . . H16A H -0.0254 0.9957 0.0672 0.078 Uiso 1 1 calc R . . H16B H -0.0299 0.8772 0.0899 0.078 Uiso 1 1 calc R . . H16C H -0.0030 0.9016 0.0359 0.078 Uiso 1 1 calc R . . Si1 Si 0.046848(17) 0.92885(4) 0.26494(2) 0.03020(12) Uani 1 1 d . . . Si2 Si 0.049189(16) 0.73821(3) 0.28349(2) 0.02671(11) Uani 1 1 d . . . Si3 Si 0.115010(18) 0.67354(4) 0.23920(3) 0.03233(13) Uani 1 1 d . . . Si4 Si 0.11523(2) 0.80079(5) 0.15090(3) 0.04156(14) Uani 1 1 d . . . Si5 Si 0.05844(2) 0.94027(4) 0.15477(3) 0.03805(14) Uani 1 1 d . . . Si6 Si 0.07552(2) 0.65662(4) 0.39852(3) 0.03828(14) Uani 1 1 d . . . Si7 Si 0.10073(2) 1.06090(4) 0.34714(3) 0.04525(15) Uani 1 1 d . . . Si8 Si 0.20408(2) 0.69148(5) 0.32651(3) 0.04755(16) Uani 1 1 d . . . Si9 Si 0.11147(2) 0.49207(5) 0.20078(4) 0.05268(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0876(19) 0.0427(13) 0.0768(18) -0.0128(12) 0.0068(15) 0.0111(12) C2 0.0541(12) 0.0594(14) 0.0501(13) -0.0100(11) 0.0027(10) -0.0015(10) C3 0.0863(19) 0.0791(19) 0.085(2) -0.0137(16) 0.0322(16) -0.0475(16) C4 0.0531(12) 0.0696(15) 0.0545(13) 0.0118(11) 0.0293(10) 0.0058(11) C5 0.0550(13) 0.0492(13) 0.0768(16) 0.0183(12) 0.0248(12) 0.0115(10) C6 0.0465(12) 0.0743(16) 0.0432(12) 0.0058(11) 0.0028(9) 0.0009(11) C7 0.0633(16) 0.0556(17) 0.151(3) -0.0028(18) 0.0248(18) -0.0167(13) C8 0.0707(17) 0.0480(14) 0.133(3) 0.0022(16) 0.0380(18) 0.0200(12) C9 0.176(4) 0.083(2) 0.104(3) -0.028(2) 0.089(3) 0.011(2) C10 0.0457(12) 0.0878(19) 0.0718(17) 0.0206(15) 0.0090(11) 0.0125(12) C11 0.0479(13) 0.0745(17) 0.118(2) 0.0154(16) 0.0486(15) 0.0143(11) C12 0.0708(17) 0.0712(18) 0.0783(18) -0.0187(15) 0.0168(14) -0.0176(13) C13 0.0500(13) 0.0783(17) 0.0909(19) 0.0198(15) 0.0368(13) -0.0108(12) C14 0.0833(18) 0.0887(19) 0.0530(14) -0.0034(13) 0.0452(14) -0.0094(14) C15 0.0693(15) 0.0547(14) 0.0652(15) 0.0145(11) 0.0296(12) -0.0137(11) C16 0.0495(11) 0.0669(14) 0.0359(10) 0.0085(10) 0.0127(9) -0.0037(10) Si1 0.0316(2) 0.0269(2) 0.0309(2) -0.00174(17) 0.01096(18) -0.00341(16) Si2 0.0257(2) 0.0273(2) 0.0273(2) 0.00148(17) 0.01047(17) 0.00119(15) Si3 0.0278(2) 0.0328(2) 0.0392(3) -0.00166(19) 0.0161(2) 0.00048(17) Si4 0.0393(3) 0.0494(3) 0.0439(3) 0.0023(2) 0.0248(2) -0.0050(2) Si5 0.0400(3) 0.0398(3) 0.0359(3) 0.0071(2) 0.0165(2) -0.0049(2) Si6 0.0346(3) 0.0444(3) 0.0347(3) 0.0106(2) 0.0123(2) 0.0059(2) Si7 0.0478(3) 0.0346(3) 0.0460(3) -0.0089(2) 0.0103(2) -0.0092(2) Si8 0.0277(3) 0.0524(3) 0.0584(4) 0.0016(3) 0.0124(2) 0.0026(2) Si9 0.0505(3) 0.0381(3) 0.0752(4) -0.0134(3) 0.0309(3) 0.0000(2) _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 Si7 1.876(3) . ? C2 Si7 1.875(2) . ? C3 Si7 1.876(3) . ? C4 Si6 1.864(2) . ? C5 Si6 1.866(2) . ? C6 Si6 1.873(2) . ? C7 Si9 1.876(3) . ? C8 Si9 1.865(3) . ? C9 Si9 1.870(3) . ? C10 Si8 1.875(3) . ? C11 Si8 1.884(3) . ? C12 Si8 1.875(3) . ? C13 Si4 1.890(2) . ? C14 Si4 1.889(2) . ? C15 Si5 1.895(2) . ? C16 Si5 1.885(2) . ? Si1 Si5 2.3755(7) . ? Si1 Si1 2.3865(9) 2 ? Si1 Si7 2.3949(7) . ? Si1 Si2 2.4063(6) . ? Si2 Si6 2.3803(7) . ? Si2 Si3 2.4370(6) . ? Si2 Si2 2.4902(8) 2 ? Si3 Si9 2.3850(8) . ? Si3 Si8 2.3925(7) . ? Si3 Si4 2.3928(7) . ? Si4 Si5 2.3526(8) . ? 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 Si5 Si1 Si1 106.54(3) . 2 ? Si5 Si1 Si7 109.87(3) . . ? Si1 Si1 Si7 118.83(2) 2 . ? Si5 Si1 Si2 101.58(2) . . ? Si1 Si1 Si2 90.001(15) 2 . ? Si7 Si1 Si2 126.92(3) . . ? Si6 Si2 Si1 123.73(3) . . ? Si6 Si2 Si3 103.52(2) . . ? Si1 Si2 Si3 104.40(2) . . ? Si6 Si2 Si2 112.43(3) . 2 ? Si1 Si2 Si2 87.583(15) . 2 ? Si3 Si2 Si2 126.34(3) . 2 ? Si9 Si3 Si8 103.28(3) . . ? Si9 Si3 Si4 113.50(3) . . ? Si8 Si3 Si4 101.02(3) . . ? Si9 Si3 Si2 119.53(3) . . ? Si8 Si3 Si2 112.31(3) . . ? Si4 Si3 Si2 105.78(2) . . ? C14 Si4 C13 101.96(13) . . ? C14 Si4 Si5 110.31(10) . . ? C13 Si4 Si5 105.11(10) . . ? C14 Si4 Si3 117.57(9) . . ? C13 Si4 Si3 115.46(9) . . ? Si5 Si4 Si3 105.82(3) . . ? C16 Si5 C15 103.60(11) . . ? C16 Si5 Si4 109.97(8) . . ? C15 Si5 Si4 108.47(9) . . ? C16 Si5 Si1 109.57(7) . . ? C15 Si5 Si1 116.53(9) . . ? Si4 Si5 Si1 108.53(3) . . ? C4 Si6 C5 106.20(11) . . ? C4 Si6 C6 106.57(12) . . ? C5 Si6 C6 109.00(11) . . ? C4 Si6 Si2 113.11(8) . . ? C5 Si6 Si2 107.98(9) . . ? C6 Si6 Si2 113.68(8) . . ? C3 Si7 C2 104.39(13) . . ? C3 Si7 C1 106.61(16) . . ? C2 Si7 C1 108.24(13) . . ? C3 Si7 Si1 112.08(10) . . ? C2 Si7 Si1 117.46(8) . . ? C1 Si7 Si1 107.53(9) . . ? C12 Si8 C10 105.51(15) . . ? C12 Si8 C11 109.22(14) . . ? C10 Si8 C11 104.26(13) . . ? C12 Si8 Si3 111.22(10) . . ? C10 Si8 Si3 119.57(9) . . ? C11 Si8 Si3 106.58(10) . . ? C8 Si9 C9 105.37(17) . . ? C8 Si9 C7 105.26(15) . . ? C9 Si9 C7 108.0(2) . . ? C8 Si9 Si3 112.71(10) . . ? C9 Si9 Si3 111.09(12) . . ? C7 Si9 Si3 113.85(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.320 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.054