 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C8 H22 O5 Si2'
_chemical_formula_weight          254.44
 
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                    6.2157(12)
_cell_length_b                    9.6972(19)
_cell_length_c                    11.921(2)
_cell_angle_alpha                 89.14(3)
_cell_angle_beta                  79.65(3)
_cell_angle_gamma                 81.51(3)
_cell_volume                      699.0(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     14964
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       30.51
 
_exptl_crystal_description        prismatic
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.12
_exptl_crystal_size_min           0.12
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.209
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              276
_exptl_absorpt_coefficient_mu     0.254
_exptl_absorpt_correction_type    Empirical
_exptl_absorpt_correction_T_min   0.9509
_exptl_absorpt_correction_T_max   0.9701
_exptl_absorpt_process_details    'SORTAV (R. H. Blessing, 1995, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       150(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        'π and θ 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             9740
_diffrn_reflns_av_R_equivalents   0.0513
_diffrn_reflns_av_sigmaI/netI     0.0510
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.37
_diffrn_reflns_theta_max          27.50
_reflns_number_total              3090
_reflns_number_gt                 2401
_reflns_threshold_expression      >2σ(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 > 2σ(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)+(0.0583P)²+0.2797P] 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        ?
_refine_ls_number_reflns          3090
_refine_ls_number_parameters      146
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0602
_refine_ls_R_factor_gt            0.0443
_refine_ls_wR_factor_ref          0.1264
_refine_ls_wR_factor_gt           0.1168
_refine_ls_goodness_of_fit_ref    1.065
_refine_ls_restrained_S_all       1.065
_refine_ls_shift/su_max           0.008
_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 0.13515(7) 0.55977(5) 0.65392(4) 0.01796(16) Uani 1 1 d . . .
Si2 Si 0.37321(7) 0.42319(5) 0.85330(4) 0.01735(16) Uani 1 1 d . . .
O1 O 0.2811(2) 0.50630(15) 0.53094(10) 0.0257(3) Uani 1 1 d . . .
H1 H 0.4157 0.5066 0.5321 0.039 Uiso 1 1 calc R . .
O2 O 0.23824(19) 0.47624(14) 0.75442(10) 0.0252(3) Uani 1 1 d . . .
O3 O 0.5912(2) 0.50060(15) 0.84278(10) 0.0248(3) Uani 1 1 d . . .
H3 H 0.6717 0.4824 0.7787 0.037 Uiso 1 1 calc R . .
O4 O 0.2193(2) 0.47152(15) 0.97594(10) 0.0249(3) Uani 1 1 d . . .
H4 H 0.2976 0.4634 1.0269 0.037 Uiso 1 1 calc R . .
O5 O -0.1081(2) 0.51656(16) 0.65453(11) 0.0264(3) Uani 1 1 d . . .
H5 H -0.1827 0.5263 0.7208 0.040 Uiso 1 1 calc R . .
C1 C 0.1232(3) 0.7498(2) 0.67451(17) 0.0287(4) Uani 1 1 d . . .
C2 C -0.0077(4) 0.7946(3) 0.7931(2) 0.0434(6) Uani 1 1 d . . .
H2A H -0.0151 0.8955 0.8030 0.065 Uiso 1 1 calc R . .
H2B H 0.0661 0.7458 0.8515 0.065 Uiso 1 1 calc R . .
H2C H -0.1577 0.7713 0.8007 0.065 Uiso 1 1 calc R . .
C3 C 0.0066(4) 0.8282(3) 0.5837(2) 0.0451(6) Uani 1 1 d . . .
H3A H -0.1456 0.8082 0.5932 0.068 Uiso 1 1 calc R . .
H3B H 0.0862 0.7977 0.5075 0.068 Uiso 1 1 calc R . .
H3C H 0.0049 0.9287 0.5925 0.068 Uiso 1 1 calc R . .
C4 C 0.3568(4) 0.7870(3) 0.6624(2) 0.0431(6) Uani 1 1 d . . .
H4A H 0.4404 0.7582 0.5866 0.065 Uiso 1 1 calc R . .
H4B H 0.4311 0.7386 0.7208 0.065 Uiso 1 1 calc R . .
H4C H 0.3486 0.8879 0.6719 0.065 Uiso 1 1 calc R . .
C5 C 0.4514(3) 0.2311(2) 0.84321(17) 0.0292(5) Uani 1 1 d . . .
C6 C 0.2448(4) 0.1599(3) 0.8589(2) 0.0438(6) Uani 1 1 d . . .
H6A H 0.2883 0.0585 0.8555 0.066 Uiso 1 1 calc R . .
H6B H 0.1610 0.1886 0.7981 0.066 Uiso 1 1 calc R . .
H6C H 0.1524 0.1868 0.9331 0.066 Uiso 1 1 calc R . .
C7 C 0.5840(4) 0.1818(3) 0.9370(2) 0.0432(6) Uani 1 1 d . . .
H7A H 0.4917 0.2047 1.0119 0.065 Uiso 1 1 calc R . .
H7B H 0.7152 0.2287 0.9288 0.065 Uiso 1 1 calc R . .
H7C H 0.6298 0.0807 0.9302 0.065 Uiso 1 1 calc R . .
C8 C 0.5933(4) 0.1910(3) 0.7263(2) 0.0463(6) Uani 1 1 d . . .
H8A H 0.6355 0.0895 0.7212 0.069 Uiso 1 1 calc R . .
H8B H 0.7267 0.2358 0.7165 0.069 Uiso 1 1 calc R . .
H8C H 0.5086 0.2220 0.6664 0.069 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 0.0123(3) 0.0322(3) 0.0096(3) 0.0003(2) -0.00269(18) -0.0031(2)
Si2 0.0127(3) 0.0298(3) 0.0099(3) 0.0003(2) -0.00277(18) -0.0030(2)
O1 0.0120(6) 0.0488(9) 0.0153(6) -0.0048(6) -0.0002(5) -0.0033(6)
O2 0.0243(7) 0.0361(8) 0.0172(7) 0.0021(6) -0.0117(5) -0.0018(6)
O3 0.0177(7) 0.0431(8) 0.0151(6) 0.0008(6) -0.0014(5) -0.0108(6)
O4 0.0177(7) 0.0436(8) 0.0131(6) -0.0029(6) -0.0019(5) -0.0044(6)
O5 0.0147(7) 0.0500(9) 0.0157(7) -0.0005(6) -0.0020(5) -0.0096(6)
C1 0.0256(11) 0.0316(11) 0.0264(10) 0.0028(8) 0.0005(8) -0.0023(8)
C2 0.0504(15) 0.0378(13) 0.0356(13) -0.0090(10) 0.0057(10) -0.0011(11)
C3 0.0446(14) 0.0421(14) 0.0429(14) 0.0162(11) -0.0027(11) 0.0042(11)
C4 0.0360(13) 0.0383(13) 0.0561(15) -0.0040(11) -0.0044(11) -0.0135(10)
C5 0.0289(11) 0.0317(11) 0.0248(10) 0.0012(8) -0.0009(8) -0.0017(8)
C6 0.0481(15) 0.0371(13) 0.0475(14) -0.0015(11) -0.0050(11) -0.0147(11)
C7 0.0422(14) 0.0421(14) 0.0421(14) 0.0124(11) -0.0088(10) 0.0051(10)
C8 0.0509(15) 0.0409(14) 0.0376(13) -0.0096(11) 0.0080(11) 0.0061(11)
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O2 1.6111(13) . ?
Si1 O5 1.6262(13) . ?
Si1 O1 1.6269(14) . ?
Si1 C1 1.851(2) . ?
Si2 O2 1.6024(12) . ?
Si2 O3 1.6284(13) . ?
Si2 O4 1.6302(14) . ?
Si2 C5 1.855(2) . ?
O1 H1 0.8400 . ?
O3 H3 0.8400 . ?
O4 H4 0.8400 . ?
O5 H5 0.8400 . ?
C1 C4 1.528(3) . ?
C1 C2 1.533(3) . ?
C1 C3 1.540(3) . ?
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 C6 1.527(3) . ?
C5 C8 1.531(3) . ?
C5 C7 1.535(3) . ?
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 . ?
 
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 Si1 O5 108.05(7) . . ?
O2 Si1 O1 109.57(7) . . ?
O5 Si1 O1 105.26(7) . . ?
O2 Si1 C1 110.00(9) . . ?
O5 Si1 C1 112.11(9) . . ?
O1 Si1 C1 111.69(9) . . ?
O2 Si2 O3 109.60(7) . . ?
O2 Si2 O4 108.41(7) . . ?
O3 Si2 O4 106.34(7) . . ?
O2 Si2 C5 109.85(9) . . ?
O3 Si2 C5 110.99(9) . . ?
O4 Si2 C5 111.55(9) . . ?
Si1 O1 H1 109.5 . . ?
Si2 O2 Si1 166.50(10) . . ?
Si2 O3 H3 109.5 . . ?
Si2 O4 H4 109.5 . . ?
Si1 O5 H5 109.5 . . ?
C4 C1 C2 109.50(19) . . ?
C4 C1 C3 109.04(17) . . ?
C2 C1 C3 108.92(18) . . ?
C4 C1 Si1 110.17(15) . . ?
C2 C1 Si1 109.95(14) . . ?
C3 C1 Si1 109.24(15) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C8 109.40(19) . . ?
C6 C5 C7 108.82(18) . . ?
C8 C5 C7 109.40(18) . . ?
C6 C5 Si2 110.32(15) . . ?
C8 C5 Si2 109.51(14) . . ?
C7 C5 Si2 109.36(15) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
 
_diffrn_measured_fraction_theta_max    0.967
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.967
_refine_diff_density_max    0.371
_refine_diff_density_min   -0.531
_refine_diff_density_rms    0.065
