 
data_s92 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C32 H72 O12 Si8' 
_chemical_formula_weight          873.62 
 
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                    10.0025(3) 
_cell_length_b                    10.8274(4) 
_cell_length_c                    10.9642(4) 
_cell_angle_alpha                 96.668(2) 
_cell_angle_beta                  91.162(2) 
_cell_angle_gamma                 99.3920(10) 
_cell_volume                      1162.66(7) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     6642 
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       26.02
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.15 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.248 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              472 
_exptl_absorpt_coefficient_mu     0.282 
_exptl_absorpt_correction_type    Empirical 
_exptl_absorpt_correction_T_min   0.9589 
_exptl_absorpt_correction_T_max   0.9589 
_exptl_absorpt_process_details    'SORTAV (R.H. Blessing, 1995, 1997)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       120(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'ω and φ scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'
_diffrn_reflns_number             8484 
_diffrn_reflns_av_R_equivalents   0.0301 
_diffrn_reflns_av_sigmaI/netI     0.0553 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -13 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          3.05 
_diffrn_reflns_theta_max          25.98 
_reflns_number_total              4427 
_reflns_number_gt                 3464 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        
;
'DENZO (Otwinowski and Minor, 1997) & COLLECT (Hooft, 1998) '
;
_computing_cell_refinement        'DENZO and COLLECT'
_computing_data_reduction         'DENZO and COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     ?
_computing_publication_material   SHELXL-97
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0481P)²+0.2692P] where P=(Fo²+2Fc²)/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        0 
_refine_ls_number_reflns          4427 
_refine_ls_number_parameters      235 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0560 
_refine_ls_R_factor_gt            0.0382 
_refine_ls_wR_factor_ref          0.0991 
_refine_ls_wR_factor_gt           0.0930 
_refine_ls_goodness_of_fit_ref    0.994 
_refine_ls_restrained_S_all       0.994 
_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 0.45045(5) 0.82092(5) 0.15271(4) 0.01473(15) Uani 1 1 d . . . 
Si2 Si 0.35219(5) 0.79029(5) -0.12479(4) 0.01509(15) Uani 1 1 d . . . 
Si3 Si 0.26473(5) 1.05736(5) -0.08603(4) 0.01488(15) Uani 1 1 d . . . 
Si4 Si 0.36242(5) 1.08788(5) 0.19174(4) 0.01486(15) Uani 1 1 d . . . 
O1 O 0.38128(14) 0.77314(13) 0.01754(11) 0.0214(3) Uani 1 1 d . . . 
O2 O 0.27930(14) 0.91244(12) -0.12974(12) 0.0209(3) Uani 1 1 d . . . 
O3 O 0.27834(13) 1.08126(13) 0.06279(11) 0.0212(3) Uani 1 1 d . . . 
O4 O 0.39786(14) 0.94974(12) 0.20615(12) 0.0212(3) Uani 1 1 d . . . 
O5 O 0.61374(13) 0.85022(13) 0.14143(12) 0.0205(3) Uani 1 1 d . . . 
O6 O 0.49595(13) 0.81400(12) -0.19129(12) 0.0201(3) Uani 1 1 d . . . 
C10 C 0.4106(2) 0.70276(18) 0.26002(17) 0.0186(4) Uani 1 1 d . . . 
H10A H 0.4533 0.7394 0.3412 0.022 Uiso 1 1 calc R . . 
H10B H 0.3112 0.6885 0.2695 0.022 Uiso 1 1 calc R . . 
C11 C 0.4539(2) 0.57372(18) 0.22699(17) 0.0214(5) Uani 1 1 d . . . 
H11 H 0.5500 0.5881 0.2013 0.026 Uiso 1 1 calc R . . 
C12 C 0.3673(3) 0.4951(2) 0.1214(2) 0.0403(6) Uani 1 1 d . . . 
H12A H 0.3718 0.5418 0.0498 0.060 Uiso 1 1 calc R . . 
H12B H 0.2731 0.4772 0.1458 0.060 Uiso 1 1 calc R . . 
H12C H 0.4011 0.4156 0.1005 0.060 Uiso 1 1 calc R . . 
C13 C 0.4477(3) 0.5023(2) 0.3386(2) 0.0343(6) Uani 1 1 d . . . 
H13A H 0.5031 0.5538 0.4066 0.051 Uiso 1 1 calc R . . 
H13B H 0.4824 0.4231 0.3182 0.051 Uiso 1 1 calc R . . 
H13C H 0.3535 0.4837 0.3630 0.051 Uiso 1 1 calc R . . 
C20 C 0.2376(2) 0.64896(19) -0.19764(17) 0.0208(5) Uani 1 1 d . . . 
H20A H 0.2936 0.5857 -0.2292 0.025 Uiso 1 1 calc R . . 
H20B H 0.1807 0.6127 -0.1335 0.025 Uiso 1 1 calc R . . 
C21 C 0.1431(2) 0.6693(2) -0.30406(19) 0.0300(5) Uani 1 1 d . . . 
H21 H 0.1025 0.7462 -0.2777 0.036 Uiso 1 1 calc R . . 
C22 C 0.2239(3) 0.6933(3) -0.4175(2) 0.0453(7) Uani 1 1 d . . . 
H22A H 0.2964 0.7659 -0.3969 0.068 Uiso 1 1 calc R . . 
H22B H 0.1637 0.7110 -0.4826 0.068 Uiso 1 1 calc R . . 
H22C H 0.2635 0.6186 -0.4460 0.068 Uiso 1 1 calc R . . 
C23 C 0.0277(3) 0.5584(3) -0.3317(2) 0.0461(7) Uani 1 1 d . . . 
H23A H -0.0226 0.5459 -0.2571 0.069 Uiso 1 1 calc R . . 
H23B H 0.0649 0.4821 -0.3595 0.069 Uiso 1 1 calc R . . 
H23C H -0.0334 0.5758 -0.3961 0.069 Uiso 1 1 calc R . . 
C30 C 0.10168(19) 1.08629(18) -0.14736(17) 0.0188(4) Uani 1 1 d . . . 
H30A H 0.0946 1.0557 -0.2363 0.023 Uiso 1 1 calc R . . 
H30B H 0.0283 1.0340 -0.1079 0.023 Uiso 1 1 calc R . . 
C31 C 0.0744(2) 1.2226(2) -0.1315(2) 0.0260(5) Uani 1 1 d . . . 
H31 H 0.1545 1.2779 -0.1606 0.031 Uiso 1 1 calc R . . 
C32 C 0.0552(3) 1.2690(2) 0.0019(2) 0.0410(6) Uani 1 1 d . . . 
H32A H 0.0384 1.3562 0.0085 0.061 Uiso 1 1 calc R . . 
H32B H 0.1371 1.2655 0.0510 0.061 Uiso 1 1 calc R . . 
H32C H -0.0224 1.2153 0.0324 0.061 Uiso 1 1 calc R . . 
C33 C -0.0500(2) 1.2338(2) -0.2097(2) 0.0418(6) Uani 1 1 d . . . 
H33A H -0.0365 1.2047 -0.2959 0.063 Uiso 1 1 calc R . . 
H33B H -0.0632 1.3220 -0.2021 0.063 Uiso 1 1 calc R . . 
H33C H -0.1301 1.1817 -0.1814 0.063 Uiso 1 1 calc R . . 
C40 C 0.2576(2) 1.14452(19) 0.31591(16) 0.0197(4) Uani 1 1 d . . . 
H40A H 0.2389 1.2282 0.2995 0.024 Uiso 1 1 calc R . . 
H40B H 0.1695 1.0868 0.3095 0.024 Uiso 1 1 calc R . . 
C41 C 0.3119(2) 1.1573(2) 0.44958(17) 0.0260(5) Uani 1 1 d . . . 
H41 H 0.4085 1.2006 0.4534 0.031 Uiso 1 1 calc R . . 
C42 C 0.2318(3) 1.2378(2) 0.5340(2) 0.0393(6) Uani 1 1 d . . . 
H42A H 0.2694 1.2462 0.6184 0.059 Uiso 1 1 calc R . . 
H42B H 0.1366 1.1973 0.5311 0.059 Uiso 1 1 calc R . . 
H42C H 0.2381 1.3215 0.5067 0.059 Uiso 1 1 calc R . . 
C43 C 0.3084(3) 1.0287(2) 0.4946(2) 0.0446(7) Uani 1 1 d . . . 
H43A H 0.3613 0.9782 0.4407 0.067 Uiso 1 1 calc R . . 
H43B H 0.2143 0.9853 0.4933 0.067 Uiso 1 1 calc R . . 
H43C H 0.3473 1.0400 0.5787 0.067 Uiso 1 1 calc R . . 
 
 
_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 1.6144(14) . ? 
Si1 O4 1.6211(14) . ? 
Si1 O5 1.6223(14) . ? 
Si1 C10 1.8391(18) . ? 
Si2 O2 1.6166(13) . ? 
Si2 O1 1.6190(13) . ? 
Si2 O6 1.6220(14) . ? 
Si2 C20 1.844(2) . ? 
Si3 O2 1.6173(14) . ? 
Si3 O5 1.6193(14) 2_675 ? 
Si3 O3 1.6216(13) . ? 
Si3 C30 1.8389(19) . ? 
Si4 O4 1.6166(14) . ? 
Si4 O3 1.6186(13) . ? 
Si4 O6 1.6266(14) 2_675 ? 
Si4 C40 1.8446(18) . ? 
O5 Si3 1.6193(14) 2_675 ? 
O6 Si4 1.6266(14) 2_675 ? 
C10 C11 1.535(3) . ? 
C10 H10A 0.9900 . ? 
C10 H10B 0.9900 . ? 
C11 C12 1.518(3) . ? 
C11 C13 1.519(3) . ? 
C11 H11 1.0000 . ? 
C12 H12A 0.9800 . ? 
C12 H12B 0.9800 . ? 
C12 H12C 0.9800 . ? 
C13 H13A 0.9800 . ? 
C13 H13B 0.9800 . ? 
C13 H13C 0.9800 . ? 
C20 C21 1.545(3) . ? 
C20 H20A 0.9900 . ? 
C20 H20B 0.9900 . ? 
C21 C23 1.521(3) . ? 
C21 C22 1.521(3) . ? 
C21 H21 1.0000 . ? 
C22 H22A 0.9800 . ? 
C22 H22B 0.9800 . ? 
C22 H22C 0.9800 . ? 
C23 H23A 0.9800 . ? 
C23 H23B 0.9800 . ? 
C23 H23C 0.9800 . ? 
C30 C31 1.536(3) . ? 
C30 H30A 0.9900 . ? 
C30 H30B 0.9900 . ? 
C31 C32 1.517(3) . ? 
C31 C33 1.525(3) . ? 
C31 H31 1.0000 . ? 
C32 H32A 0.9800 . ? 
C32 H32B 0.9800 . ? 
C32 H32C 0.9800 . ? 
C33 H33A 0.9800 . ? 
C33 H33B 0.9800 . ? 
C33 H33C 0.9800 . ? 
C40 C41 1.536(3) . ? 
C40 H40A 0.9900 . ? 
C40 H40B 0.9900 . ? 
C41 C42 1.525(3) . ? 
C41 C43 1.526(3) . ? 
C41 H41 1.0000 . ? 
C42 H42A 0.9800 . ? 
C42 H42B 0.9800 . ? 
C42 H42C 0.9800 . ? 
C43 H43A 0.9800 . ? 
C43 H43B 0.9800 . ? 
C43 H43C 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 O4 108.85(7) . . ? 
O1 Si1 O5 108.77(7) . . ? 
O4 Si1 O5 108.99(7) . . ? 
O1 Si1 C10 112.35(8) . . ? 
O4 Si1 C10 109.41(8) . . ? 
O5 Si1 C10 108.42(8) . . ? 
O2 Si2 O1 108.83(7) . . ? 
O2 Si2 O6 108.80(7) . . ? 
O1 Si2 O6 108.64(7) . . ? 
O2 Si2 C20 109.20(8) . . ? 
O1 Si2 C20 108.69(8) . . ? 
O6 Si2 C20 112.62(8) . . ? 
O2 Si3 O5 109.08(7) . 2_675 ? 
O2 Si3 O3 108.48(7) . . ? 
O5 Si3 O3 108.89(7) 2_675 . ? 
O2 Si3 C30 108.65(8) . . ? 
O5 Si3 C30 108.80(8) 2_675 . ? 
O3 Si3 C30 112.88(8) . . ? 
O4 Si4 O3 108.88(7) . . ? 
O4 Si4 O6 108.36(7) . 2_675 ? 
O3 Si4 O6 109.61(7) . 2_675 ? 
O4 Si4 C40 112.61(8) . . ? 
O3 Si4 C40 107.75(8) . . ? 
O6 Si4 C40 109.61(8) 2_675 . ? 
Si1 O1 Si2 152.67(10) . . ? 
Si2 O2 Si3 152.39(10) . . ? 
Si4 O3 Si3 151.89(9) . . ? 
Si4 O4 Si1 152.08(9) . . ? 
Si3 O5 Si1 143.38(8) 2_675 . ? 
Si2 O6 Si4 143.32(9) . 2_675 ? 
C11 C10 Si1 117.69(13) . . ? 
C11 C10 H10A 107.9 . . ? 
Si1 C10 H10A 107.9 . . ? 
C11 C10 H10B 107.9 . . ? 
Si1 C10 H10B 107.9 . . ? 
H10A C10 H10B 107.2 . . ? 
C12 C11 C13 109.91(19) . . ? 
C12 C11 C10 112.08(17) . . ? 
C13 C11 C10 110.22(16) . . ? 
C12 C11 H11 108.2 . . ? 
C13 C11 H11 108.2 . . ? 
C10 C11 H11 108.2 . . ? 
C11 C12 H12A 109.5 . . ? 
C11 C12 H12B 109.5 . . ? 
H12A C12 H12B 109.5 . . ? 
C11 C12 H12C 109.5 . . ? 
H12A C12 H12C 109.5 . . ? 
H12B C12 H12C 109.5 . . ? 
C11 C13 H13A 109.5 . . ? 
C11 C13 H13B 109.5 . . ? 
H13A C13 H13B 109.5 . . ? 
C11 C13 H13C 109.5 . . ? 
H13A C13 H13C 109.5 . . ? 
H13B C13 H13C 109.5 . . ? 
C21 C20 Si2 116.11(14) . . ? 
C21 C20 H20A 108.3 . . ? 
Si2 C20 H20A 108.3 . . ? 
C21 C20 H20B 108.3 . . ? 
Si2 C20 H20B 108.3 . . ? 
H20A C20 H20B 107.4 . . ? 
C23 C21 C22 111.5(2) . . ? 
C23 C21 C20 111.13(18) . . ? 
C22 C21 C20 110.36(19) . . ? 
C23 C21 H21 107.9 . . ? 
C22 C21 H21 107.9 . . ? 
C20 C21 H21 107.9 . . ? 
C21 C22 H22A 109.5 . . ? 
C21 C22 H22B 109.5 . . ? 
H22A C22 H22B 109.5 . . ? 
C21 C22 H22C 109.5 . . ? 
H22A C22 H22C 109.5 . . ? 
H22B C22 H22C 109.5 . . ? 
C21 C23 H23A 109.5 . . ? 
C21 C23 H23B 109.5 . . ? 
H23A C23 H23B 109.5 . . ? 
C21 C23 H23C 109.5 . . ? 
H23A C23 H23C 109.5 . . ? 
H23B C23 H23C 109.5 . . ? 
C31 C30 Si3 117.62(15) . . ? 
C31 C30 H30A 107.9 . . ? 
Si3 C30 H30A 107.9 . . ? 
C31 C30 H30B 107.9 . . ? 
Si3 C30 H30B 107.9 . . ? 
H30A C30 H30B 107.2 . . ? 
C32 C31 C33 109.86(19) . . ? 
C32 C31 C30 111.76(17) . . ? 
C33 C31 C30 110.44(19) . . ? 
C32 C31 H31 108.2 . . ? 
C33 C31 H31 108.2 . . ? 
C30 C31 H31 108.2 . . ? 
C31 C32 H32A 109.5 . . ? 
C31 C32 H32B 109.5 . . ? 
H32A C32 H32B 109.5 . . ? 
C31 C32 H32C 109.5 . . ? 
H32A C32 H32C 109.5 . . ? 
H32B C32 H32C 109.5 . . ? 
C31 C33 H33A 109.5 . . ? 
C31 C33 H33B 109.5 . . ? 
H33A C33 H33B 109.5 . . ? 
C31 C33 H33C 109.5 . . ? 
H33A C33 H33C 109.5 . . ? 
H33B C33 H33C 109.5 . . ? 
C41 C40 Si4 118.92(14) . . ? 
C41 C40 H40A 107.6 . . ? 
Si4 C40 H40A 107.6 . . ? 
C41 C40 H40B 107.6 . . ? 
Si4 C40 H40B 107.6 . . ? 
H40A C40 H40B 107.0 . . ? 
C42 C41 C43 110.02(18) . . ? 
C42 C41 C40 110.83(17) . . ? 
C43 C41 C40 111.53(19) . . ? 
C42 C41 H41 108.1 . . ? 
C43 C41 H41 108.1 . . ? 
C40 C41 H41 108.1 . . ? 
C41 C42 H42A 109.5 . . ? 
C41 C42 H42B 109.5 . . ? 
H42A C42 H42B 109.5 . . ? 
C41 C42 H42C 109.5 . . ? 
H42A C42 H42C 109.5 . . ? 
H42B C42 H42C 109.5 . . ? 
C41 C43 H43A 109.5 . . ? 
C41 C43 H43B 109.5 . . ? 
H43A C43 H43B 109.5 . . ? 
C41 C43 H43C 109.5 . . ? 
H43A C43 H43C 109.5 . . ? 
H43B C43 H43C 109.5 . . ? 
 
_diffrn_measured_fraction_theta_max    0.968 
_diffrn_reflns_theta_full              25.98 
_diffrn_measured_fraction_theta_full   0.968 
_refine_diff_density_max    0.306 
_refine_diff_density_min   -0.344 
_refine_diff_density_rms    0.057 
