 
data_01src993 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 PG Taylor
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C16 H36 O6 Si4' 
_chemical_formula_weight          436.81 
 
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
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    9.9881(13) 
_cell_length_b                    10.8183(14) 
_cell_length_c                    10.9540(18) 
_cell_angle_alpha                 96.541(8) 
_cell_angle_beta                  91.269(7) 
_cell_angle_gamma                 99.439(7) 
_cell_volume                      1159.0(3) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     21077 
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.10 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.252 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              472 
_exptl_absorpt_coefficient_mu     0.283 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.9722 
_exptl_absorpt_correction_T_max   0.9722 
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       120(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD'
_diffrn_measurement_method        'Φ & ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             10942 
_diffrn_reflns_av_R_equivalents   0.2177 
_diffrn_reflns_av_sigmaI/netI     0.2690 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          3.05 
_diffrn_reflns_theta_max          25.03 
_reflns_number_total              3921 
_reflns_number_gt                 1619 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' 
_computing_cell_refinement        'DENZO & COLLECT'
_computing_data_reduction         'DENZO & COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0533P)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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3921 
_refine_ls_number_parameters      243 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.2189 
_refine_ls_R_factor_gt            0.0841 
_refine_ls_wR_factor_ref          0.2024 
_refine_ls_wR_factor_gt           0.1572 
_refine_ls_goodness_of_fit_ref    0.968 
_refine_ls_restrained_S_all       0.968 
_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 
C1 C 0.0886(7) 0.7969(6) 0.7397(6) 0.0324(19) Uani 1 1 d . . . 
H1A H 0.1878 0.8096 0.7286 0.039 Uiso 1 1 calc R . . 
H1B H 0.0439 0.7605 0.6591 0.039 Uiso 1 1 calc R . . 
C2 C 0.0486(8) 0.9261(7) 0.7727(6) 0.041(2) Uani 1 1 d . . . 
H2 H -0.0477 0.9114 0.7981 0.049 Uiso 1 1 calc R . . 
C3 C 0.0517(8) 0.9966(7) 0.6616(7) 0.056(2) Uani 1 1 d . . . 
H3A H 0.1446 1.0121 0.6333 0.085 Uiso 1 1 calc R . . 
H3B H 0.0208 1.0774 0.6835 0.085 Uiso 1 1 calc R . . 
H3C H -0.0084 0.9463 0.5958 0.085 Uiso 1 1 calc R . . 
C4 C 0.1322(9) 1.0044(7) 0.8793(7) 0.061(3) Uani 1 1 d . . . 
H4A H 0.2275 1.0218 0.8574 0.091 Uiso 1 1 calc R . . 
H4B H 0.1249 0.9581 0.9514 0.091 Uiso 1 1 calc R . . 
H4C H 0.0985 1.0842 0.8984 0.091 Uiso 1 1 calc R . . 
C5 C 0.2424(7) 0.3568(6) 0.6863(6) 0.0330(18) Uani 1 1 d . . . 
H5A H 0.3307 0.4148 0.6938 0.040 Uiso 1 1 calc R . . 
H5B H 0.2610 0.2731 0.7030 0.040 Uiso 1 1 calc R . . 
C6 C 0.1894(8) 0.3441(7) 0.5504(6) 0.042(2) Uani 1 1 d . . . 
H6 H 0.0926 0.3010 0.5460 0.051 Uiso 1 1 calc R . . 
C7 C 0.2683(8) 0.2634(7) 0.4675(6) 0.053(2) Uani 1 1 d . . . 
H7A H 0.2328 0.2570 0.3825 0.080 Uiso 1 1 calc R . . 
H7B H 0.2588 0.1789 0.4938 0.080 Uiso 1 1 calc R . . 
H7C H 0.3644 0.3019 0.4725 0.080 Uiso 1 1 calc R . . 
C8 C 0.1928(10) 0.4707(7) 0.5055(7) 0.066(3) Uani 1 1 d . . . 
H8A H 0.2870 0.5145 0.5075 0.098 Uiso 1 1 calc R . . 
H8B H 0.1392 0.5210 0.5588 0.098 Uiso 1 1 calc R . . 
H8C H 0.1544 0.4591 0.4211 0.098 Uiso 1 1 calc R . . 
C9 C 0.3974(7) 0.4117(6) 1.1478(6) 0.039(2) Uani 1 1 d . . . 
H9A H 0.4712 0.4644 1.1091 0.046 Uiso 1 1 calc R . . 
H9B H 0.4042 0.4415 1.2369 0.046 Uiso 1 1 calc R . . 
C10 C 0.4251(7) 0.2770(6) 1.1319(7) 0.038(2) Uani 1 1 d . . . 
H10 H 0.3449 0.2212 1.1606 0.046 Uiso 1 1 calc R . . 
C11 C 0.5486(8) 0.2656(8) 1.2094(8) 0.062(3) Uani 1 1 d . . . 
H11A H 0.5619 0.1773 1.2015 0.093 Uiso 1 1 calc R . . 
H11B H 0.5352 0.2942 1.2957 0.093 Uiso 1 1 calc R . . 
H11C H 0.6289 0.3180 1.1813 0.093 Uiso 1 1 calc R . . 
C12 C 0.4452(9) 0.2309(8) 0.9985(7) 0.063(3) Uani 1 1 d . . . 
H12A H 0.3645 0.2368 0.9484 0.095 Uiso 1 1 calc R . . 
H12B H 0.4593 0.1429 0.9918 0.095 Uiso 1 1 calc R . . 
H12C H 0.5248 0.2832 0.9692 0.095 Uiso 1 1 calc R . . 
C13 C 0.2621(7) 0.8507(6) 1.1965(6) 0.0376(19) Uani 1 1 d . . . 
H13A H 0.3199 0.8864 1.1325 0.045 Uiso 1 1 calc R . . 
H13B H 0.2061 0.9143 1.2271 0.045 Uiso 1 1 calc R . . 
C14 C 0.3565(9) 0.8296(7) 1.3055(7) 0.052(2) Uani 1 1 d . . . 
H14 H 0.3970 0.7526 1.2796 0.063 Uiso 1 1 calc R . . 
C15 C 0.4714(9) 0.9393(9) 1.3325(7) 0.075(3) Uani 1 1 d . . . 
H15A H 0.4350 1.0148 1.3646 0.112 Uiso 1 1 calc R . . 
H15B H 0.5185 0.9546 1.2568 0.112 Uiso 1 1 calc R . . 
H15C H 0.5354 0.9199 1.3938 0.112 Uiso 1 1 calc R . . 
C16 C 0.2755(9) 0.8056(8) 1.4166(7) 0.066(3) Uani 1 1 d . . . 
H16A H 0.3371 0.8005 1.4862 0.099 Uiso 1 1 calc R . . 
H16B H 0.2121 0.7258 1.3992 0.099 Uiso 1 1 calc R . . 
H16C H 0.2245 0.8746 1.4372 0.099 Uiso 1 1 calc R . . 
O1 O -0.1132(4) 0.6501(4) 0.8592(4) 0.0350(13) Uani 1 1 d . . . 
O2 O 0.1187(5) 0.7260(4) 0.9824(4) 0.0357(13) Uani 1 1 d . . . 
O3 O 0.2212(4) 0.5873(4) 1.1308(4) 0.0336(12) Uani 1 1 d . . . 
O4 O 0.2207(5) 0.4193(4) 0.9376(4) 0.0353(13) Uani 1 1 d . . . 
O5 O -0.0046(5) 0.3156(4) 0.8090(4) 0.0373(13) Uani 1 1 d . . . 
O6 O 0.1032(4) 0.5511(4) 0.7942(4) 0.0324(12) Uani 1 1 d . . . 
Si1 Si 0.0494(2) 0.67926(18) 0.84734(18) 0.0308(6) Uani 1 1 d . . . 
Si2 Si 0.1373(2) 0.41232(18) 0.80820(17) 0.0305(6) Uani 1 1 d . . . 
Si3 Si 0.2349(2) 0.44238(18) 1.08624(17) 0.0320(6) Uani 1 1 d . . . 
Si4 Si 0.1486(2) 0.70958(18) 1.12495(17) 0.0324(6) Uani 1 1 d . . . 
 
 
_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 C2 1.523(9) . ? 
C1 Si1 1.833(6) . ? 
C2 C3 1.506(9) . ? 
C2 C4 1.510(9) . ? 
C5 C6 1.553(9) . ? 
C5 Si2 1.825(7) . ? 
C6 C8 1.502(9) . ? 
C6 C7 1.511(9) . ? 
C9 C10 1.519(9) . ? 
C9 Si3 1.838(7) . ? 
C10 C11 1.512(9) . ? 
C10 C12 1.518(9) . ? 
C13 C14 1.565(9) . ? 
C13 Si4 1.830(7) . ? 
C14 C16 1.501(10) . ? 
C14 C15 1.507(10) . ? 
O1 Si1 1.614(5) . ? 
O1 Si3 1.614(5) 2_567 ? 
O2 Si1 1.611(5) . ? 
O2 Si4 1.618(4) . ? 
O3 Si4 1.616(4) . ? 
O3 Si3 1.617(4) . ? 
O4 Si2 1.616(4) . ? 
O4 Si3 1.619(4) . ? 
O5 Si2 1.618(5) . ? 
O5 Si4 1.622(5) 2_567 ? 
O6 Si2 1.615(4) . ? 
O6 Si1 1.620(4) . ? 
Si3 O1 1.614(5) 2_567 ? 
Si4 O5 1.622(5) 2_567 ? 
 
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 
C2 C1 Si1 118.0(5) . . ? 
C3 C2 C4 111.1(6) . . ? 
C3 C2 C1 110.7(6) . . ? 
C4 C2 C1 113.6(6) . . ? 
C6 C5 Si2 119.2(5) . . ? 
C8 C6 C7 110.5(6) . . ? 
C8 C6 C5 111.7(6) . . ? 
C7 C6 C5 111.2(6) . . ? 
C10 C9 Si3 118.4(5) . . ? 
C11 C10 C12 109.4(6) . . ? 
C11 C10 C9 110.7(6) . . ? 
C12 C10 C9 112.0(6) . . ? 
C14 C13 Si4 115.4(5) . . ? 
C16 C14 C15 112.1(7) . . ? 
C16 C14 C13 110.5(7) . . ? 
C15 C14 C13 110.7(6) . . ? 
Si1 O1 Si3 143.7(3) . 2_567 ? 
Si1 O2 Si4 153.3(3) . . ? 
Si4 O3 Si3 151.9(3) . . ? 
Si2 O4 Si3 152.5(3) . . ? 
Si2 O5 Si4 144.2(3) . 2_567 ? 
Si2 O6 Si1 152.1(3) . . ? 
O2 Si1 O1 108.5(2) . . ? 
O2 Si1 O6 108.3(2) . . ? 
O1 Si1 O6 109.6(2) . . ? 
O2 Si1 C1 112.9(3) . . ? 
O1 Si1 C1 108.5(3) . . ? 
O6 Si1 C1 109.1(3) . . ? 
O6 Si2 O4 108.2(2) . . ? 
O6 Si2 O5 108.4(2) . . ? 
O4 Si2 O5 109.5(2) . . ? 
O6 Si2 C5 112.6(3) . . ? 
O4 Si2 C5 107.6(3) . . ? 
O5 Si2 C5 110.4(3) . . ? 
O1 Si3 O3 109.2(2) 2_567 . ? 
O1 Si3 O4 108.6(3) 2_567 . ? 
O3 Si3 O4 108.6(2) . . ? 
O1 Si3 C9 108.5(3) 2_567 . ? 
O3 Si3 C9 108.8(3) . . ? 
O4 Si3 C9 113.1(3) . . ? 
O3 Si4 O2 108.9(2) . . ? 
O3 Si4 O5 108.1(2) . 2_567 ? 
O2 Si4 O5 108.4(2) . 2_567 ? 
O3 Si4 C13 109.6(3) . . ? 
O2 Si4 C13 108.7(3) . . ? 
O5 Si4 C13 113.1(3) 2_567 . ? 
 
_diffrn_measured_fraction_theta_max    0.960 
_diffrn_reflns_theta_full              25.03 
_diffrn_measured_fraction_theta_full   0.960 
_refine_diff_density_max    0.445 
_refine_diff_density_min   -0.403 
_refine_diff_density_rms    0.090 
