 
data_s92 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C16 H24 O12 Si8' 
_chemical_formula_weight          633.07 
 
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                    8.8240(5) 
_cell_length_b                    8.8434(5) 
_cell_length_c                    9.1388(6) 
_cell_angle_alpha                 94.442(2) 
_cell_angle_beta                  100.154(3) 
_cell_angle_gamma                 94.770(3) 
_cell_volume                      696.45(7) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     5260 
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       26.02
 
_exptl_crystal_description        Block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.04 
_exptl_crystal_size_mid           0.04 
_exptl_crystal_size_min           0.04 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.509 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              328 
_exptl_absorpt_coefficient_mu     0.441 
_exptl_absorpt_correction_type    Empirical
_exptl_absorpt_correction_T_min   0.9826 
_exptl_absorpt_correction_T_max   0.9826 
_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             4248 
_diffrn_reflns_av_R_equivalents   0.0699 
_diffrn_reflns_av_sigmaI/netI     0.1440 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -10 
_diffrn_reflns_limit_l_max        9 
_diffrn_reflns_theta_min          3.09 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              2377 
_reflns_number_gt                 1403 
_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)+(0.0324P)²+0.0000P] 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          2377 
_refine_ls_number_parameters      175 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1255 
_refine_ls_R_factor_gt            0.0568 
_refine_ls_wR_factor_ref          0.1170 
_refine_ls_wR_factor_gt           0.1029 
_refine_ls_goodness_of_fit_ref    0.914 
_refine_ls_restrained_S_all       0.914 
_refine_ls_shift/su_max           0.007 
_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 0.07998(14) 0.87847(14) 0.76213(13) 0.0185(4) Uani 1 1 d . . . 
Si2 Si -0.25484(14) 0.94789(14) 0.62319(13) 0.0186(3) Uani 1 1 d . . . 
Si4 Si 0.21199(14) 1.19458(14) 0.68660(12) 0.0190(4) Uani 1 1 d . . . 
Si3 Si -0.12390(14) 1.26378(14) 0.54814(12) 0.0186(4) Uani 1 1 d . . . 
O3 O 0.0537(3) 1.2700(3) 0.6333(3) 0.0233(8) Uani 1 1 d . . . 
O1 O -0.1031(3) 0.8934(3) 0.7242(3) 0.0249(8) Uani 1 1 d . . . 
O2 O -0.2262(3) 1.1278(3) 0.6034(3) 0.0228(8) Uani 1 1 d . . . 
O6 O -0.2845(3) 0.8557(3) 0.4590(3) 0.0231(8) Uani 1 1 d . . . 
O5 O 0.1268(3) 0.7694(3) 0.6297(3) 0.0236(8) Uani 1 1 d . . . 
O4 O 0.1760(3) 1.0441(3) 0.7702(3) 0.0234(8) Uani 1 1 d . . . 
C10 C 0.1253(6) 0.7961(5) 0.9390(5) 0.0232(11) Uani 1 1 d . . . 
H10 H 0.2281 0.8141 0.9936 0.025(12) Uiso 1 1 calc R . . 
C11 C 0.0243(7) 0.7138(6) 0.9948(5) 0.0377(14) Uani 1 1 d . . . 
H11A H -0.0794 0.6940 0.9426 0.043(15) Uiso 1 1 calc R . . 
H11B H 0.0543 0.6735 1.0878 0.041(14) Uiso 1 1 calc R . . 
C20 C -0.4242(5) 0.9115(5) 0.7107(5) 0.0190(11) Uani 1 1 d . . . 
H20 H -0.5236 0.9180 0.6528 0.047(15) Uiso 1 1 calc R . . 
C21 C -0.4162(6) 0.8769(5) 0.8488(5) 0.0319(13) Uani 1 1 d . . . 
H21A H -0.3184 0.8696 0.9095 0.058(17) Uiso 1 1 calc R . . 
H21B H -0.5081 0.8592 0.8881 0.029(14) Uiso 1 1 calc R . . 
C30 C -0.2015(6) 1.4451(6) 0.5888(5) 0.0269(12) Uani 1 1 d . . . 
H30 H -0.1417 1.5369 0.5792 0.08(2) Uiso 1 1 calc R . . 
C31 C -0.3348(7) 1.4545(7) 0.6304(6) 0.0481(16) Uani 1 1 d . . . 
H31A H -0.3969 1.3644 0.6409 0.057(18) Uiso 1 1 calc R . . 
H31B H -0.3697 1.5515 0.6501 0.08(2) Uiso 1 1 calc R . . 
C40 C 0.3501(5) 1.3327(5) 0.8129(5) 0.0237(12) Uani 1 1 d . . . 
H40 H 0.4433 1.2986 0.8624 0.017(11) Uiso 1 1 calc R . . 
C41 C 0.3273(6) 1.4762(6) 0.8388(5) 0.0361(14) Uani 1 1 d . . . 
H41A H 0.2350 1.5132 0.7908 0.032(13) Uiso 1 1 calc R . . 
H41B H 0.4029 1.5431 0.9055 0.059(17) 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 0.0205(7) 0.0155(8) 0.0194(7) 0.0030(6) 0.0021(6) 0.0026(6) 
Si2 0.0218(7) 0.0143(8) 0.0199(7) 0.0014(6) 0.0043(6) 0.0021(6) 
Si4 0.0218(7) 0.0151(8) 0.0196(7) 0.0018(6) 0.0032(6) -0.0003(6) 
Si3 0.0213(7) 0.0130(8) 0.0207(7) 0.0011(6) 0.0021(6) 0.0011(6) 
O3 0.0254(18) 0.0193(19) 0.0239(16) -0.0012(14) 0.0029(14) 0.0010(15) 
O1 0.0261(18) 0.028(2) 0.0220(15) 0.0068(15) 0.0048(14) 0.0033(15) 
O2 0.0270(18) 0.0142(18) 0.0292(16) 0.0050(14) 0.0090(15) 0.0033(15) 
O6 0.0251(17) 0.0227(19) 0.0217(16) 0.0017(14) 0.0042(14) 0.0032(14) 
O5 0.0275(18) 0.026(2) 0.0190(16) 0.0035(14) 0.0047(14) 0.0088(15) 
O4 0.0295(18) 0.0168(19) 0.0240(16) 0.0052(14) 0.0059(15) -0.0019(15) 
C10 0.025(3) 0.022(3) 0.023(2) 0.005(2) 0.005(2) 0.000(2) 
C11 0.051(4) 0.038(4) 0.026(3) 0.009(3) 0.008(3) 0.009(3) 
C20 0.023(3) 0.007(3) 0.027(3) 0.000(2) 0.007(2) -0.002(2) 
C21 0.036(3) 0.024(3) 0.036(3) 0.001(2) 0.011(3) -0.001(3) 
C30 0.032(3) 0.018(3) 0.031(3) 0.005(2) 0.006(2) 0.003(2) 
C31 0.048(4) 0.020(4) 0.086(4) 0.001(3) 0.035(3) 0.011(3) 
C40 0.027(3) 0.024(3) 0.019(2) 0.005(2) 0.000(2) 0.003(2) 
C41 0.043(3) 0.016(3) 0.043(3) -0.005(3) -0.005(3) 0.001(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 O1 1.610(3) . ? 
Si1 O4 1.620(3) . ? 
Si1 O5 1.621(3) . ? 
Si1 C10 1.819(5) . ? 
Si2 O1 1.618(3) . ? 
Si2 O6 1.619(3) . ? 
Si2 O2 1.620(3) . ? 
Si2 C20 1.833(5) . ? 
Si4 O3 1.612(3) . ? 
Si4 O4 1.621(3) . ? 
Si4 O6 1.623(3) 2_576 ? 
Si4 C40 1.830(5) . ? 
Si3 O2 1.609(3) . ? 
Si3 O3 1.617(3) . ? 
Si3 O5 1.624(3) 2_576 ? 
Si3 C30 1.832(5) . ? 
O6 Si4 1.623(3) 2_576 ? 
O5 Si3 1.624(3) 2_576 ? 
C10 C11 1.301(7) . ? 
C10 H10 0.9500 . ? 
C11 H11A 0.9500 . ? 
C11 H11B 0.9500 . ? 
C20 C21 1.312(6) . ? 
C20 H20 0.9500 . ? 
C21 H21A 0.9500 . ? 
C21 H21B 0.9500 . ? 
C30 C31 1.305(7) . ? 
C30 H30 0.9500 . ? 
C31 H31A 0.9500 . ? 
C31 H31B 0.9500 . ? 
C40 C41 1.312(6) . ? 
C40 H40 0.9500 . ? 
C41 H41A 0.9500 . ? 
C41 H41B 0.9500 . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
O1 Si1 O4 110.22(16) . . ? 
O1 Si1 O5 108.83(16) . . ? 
O4 Si1 O5 108.12(17) . . ? 
O1 Si1 C10 109.0(2) . . ? 
O4 Si1 C10 110.54(19) . . ? 
O5 Si1 C10 110.06(18) . . ? 
O1 Si2 O6 109.25(16) . . ? 
O1 Si2 O2 109.65(17) . . ? 
O6 Si2 O2 107.95(16) . . ? 
O1 Si2 C20 110.20(18) . . ? 
O6 Si2 C20 109.72(19) . . ? 
O2 Si2 C20 110.03(18) . . ? 
O3 Si4 O4 109.71(17) . . ? 
O3 Si4 O6 108.96(14) . 2_576 ? 
O4 Si4 O6 108.63(17) . 2_576 ? 
O3 Si4 C40 109.84(19) . . ? 
O4 Si4 C40 110.03(18) . . ? 
O6 Si4 C40 109.65(19) 2_576 . ? 
O2 Si3 O3 109.57(15) . . ? 
O2 Si3 O5 109.36(17) . 2_576 ? 
O3 Si3 O5 107.86(16) . 2_576 ? 
O2 Si3 C30 109.4(2) . . ? 
O3 Si3 C30 109.9(2) . . ? 
O5 Si3 C30 110.75(17) 2_576 . ? 
Si4 O3 Si3 153.1(2) . . ? 
Si1 O1 Si2 152.2(2) . . ? 
Si3 O2 Si2 148.3(2) . . ? 
Si2 O6 Si4 146.8(2) . 2_576 ? 
Si1 O5 Si3 147.11(18) . 2_576 ? 
Si1 O4 Si4 147.67(19) . . ? 
C11 C10 Si1 123.5(4) . . ? 
C11 C10 H10 118.2 . . ? 
Si1 C10 H10 118.2 . . ? 
C10 C11 H11A 120.0 . . ? 
C10 C11 H11B 120.0 . . ? 
H11A C11 H11B 120.0 . . ? 
C21 C20 Si2 123.8(4) . . ? 
C21 C20 H20 118.1 . . ? 
Si2 C20 H20 118.1 . . ? 
C20 C21 H21A 120.0 . . ? 
C20 C21 H21B 120.0 . . ? 
H21A C21 H21B 120.0 . . ? 
C31 C30 Si3 123.4(4) . . ? 
C31 C30 H30 118.3 . . ? 
Si3 C30 H30 118.3 . . ? 
C30 C31 H31A 120.0 . . ? 
C30 C31 H31B 120.0 . . ? 
H31A C31 H31B 120.0 . . ? 
C41 C40 Si4 123.5(4) . . ? 
C41 C40 H40 118.3 . . ? 
Si4 C40 H40 118.3 . . ? 
C40 C41 H41A 120.0 . . ? 
C40 C41 H41B 120.0 . . ? 
H41A C41 H41B 120.0 . . ? 
 
_diffrn_measured_fraction_theta_max    0.963 
_diffrn_reflns_theta_full              25.00 
_diffrn_measured_fraction_theta_full   0.963 
_refine_diff_density_max    0.458 
_refine_diff_density_min   -0.507 
_refine_diff_density_rms    0.101 
