# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 182/1200


data_global

_publ_section_title 
;

    Synthesis of the Functionalised Core of Neoliacinic Acid

; 

_journal_name_full                 'Chemical Communications'
_journal_volume                    '?'
_journal_page_first                '?'
_journal_page_last                 '?'
_journal_year                       1999
_ccdc_journal_depnumber            '?'

_publ_contact_author_name          'Dr A.J. Blake'
_publ_contact_author_address
;
  School of Chemistry
  The University of Nottingham
  University Park
  Nottingham  NG7 2RD
  England
;
_publ_contact_author_email        A.J.Blake@Nottingham.ac.uk
_publ_contact_author_fax          '0115 951 3563'
_publ_contact_author_phone        '0115 951 3488'


data_EPSIPR
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          'C25 H44 O6 Si' 
_chemical_formula_sum             'C25 H44 O6 Si' 
 _chemical_formula_weight          468.69 
  
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            orthorhombic 
_symmetry_space_group_name_H-M   'P 21 21 21'
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
  
_cell_length_a                    8.638(5) 
_cell_length_b                    9.693(9) 
_cell_length_c                    32.149(16) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      2692(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     26 
_cell_measurement_theta_min       12.5 
_cell_measurement_theta_max       17.0 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.42 
_exptl_crystal_size_mid           0.32 
_exptl_crystal_size_min           0.22 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.157 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1024 
_exptl_absorpt_coefficient_mu     0.122 
_exptl_absorpt_correction_type    numerical 
_exptl_absorpt_correction_T_min   0.962 
_exptl_absorpt_correction_T_max   0.974 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       150(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   'Stoe Stadi-4 four-circle' 
_diffrn_measurement_method        omega 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   60 
_diffrn_standards_decay_%         'variation +/-5.2' 
_diffrn_reflns_number             5481 
_diffrn_reflns_av_R_equivalents   0.023
_diffrn_reflns_av_sigmaI/netI     0.0342 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -38 
_diffrn_reflns_limit_l_max        38 
_diffrn_reflns_theta_min          2.53 
_diffrn_reflns_theta_max          25.03 
_reflns_number_total              5481 
_reflns_number_gt                 4688 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'STADI4 (Stoe & Cie, 1997a)' 
_computing_cell_refinement        'STADI4 (Stoe & Cie, 1997a)' 
_computing_data_reduction         'X-RED (Stoe & Cie, 1997b)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL/PC (Sheldrick, 1994)' 
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
  
_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 w=1/[\s^2^(Fo^2^)+(0.033P)^2^+3.10P] 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      SHELXL 
_refine_ls_extinction_coef        0.0046(6) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.00(8) 
_refine_ls_number_reflns          5481 
_refine_ls_number_parameters      291 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0639 
_refine_ls_R_factor_gt            0.0506 
_refine_ls_wR_factor_ref          0.1167 
_refine_ls_wR_factor_gt           0.1066 
_refine_ls_goodness_of_fit_ref    1.041 
_refine_ls_restrained_S_all       1.041 
_refine_ls_shift/su_max           0.012 
_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_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
O1 O 0.0143(2) 0.81412(18) 0.25161(6) 0.0232(4) Uani 1 d . . . 
C1 C 0.0317(3) 0.7423(3) 0.21257(8) 0.0226(6) Uani 1 d . . . 
H1 H 0.0191 0.8137 0.1904 0.027 Uiso 1 calc R . . 
C2 C 0.1997(3) 0.6918(3) 0.20937(8) 0.0245(6) Uani 1 d . . . 
C2"' C 0.3079(3) 0.8156(3) 0.20859(9) 0.0303(7) Uani 1 d . . . 
H2"A H 0.2720 0.8818 0.1877 0.045 Uiso 1 calc R . . 
H2"B H 0.4129 0.7850 0.2016 0.045 Uiso 1 calc R . . 
H2"C H 0.3087 0.8598 0.2360 0.045 Uiso 1 calc R . . 
C3 C 0.2465(3) 0.5833(3) 0.24198(8) 0.0265(6) Uani 1 d . . . 
H3A H 0.1635 0.5131 0.2436 0.032 Uiso 1 calc R . . 
H3B H 0.3414 0.5362 0.2322 0.032 Uiso 1 calc R . . 
C4 C 0.2760(3) 0.6379(3) 0.28500(8) 0.0266(6) Uani 1 d . . . 
H4 H 0.3690 0.6984 0.2881 0.032 Uiso 1 calc R . . 
O O 0.2538(2) 0.53483(19) 0.31782(6) 0.0314(5) Uani 1 d . . . 
C5 C 0.1547(3) 0.6556(3) 0.31682(8) 0.0246(6) Uani 1 d . . . 
C6 C -0.0112(3) 0.6275(3) 0.30423(8) 0.0250(6) Uani 1 d . . . 
H6A H -0.0730 0.6039 0.3292 0.030 Uiso 1 calc R . . 
H6B H -0.0146 0.5480 0.2849 0.030 Uiso 1 calc R . . 
C7 C -0.0811(3) 0.7543(3) 0.28299(9) 0.0250(6) Uani 1 d . . . 
H7 H -0.0945 0.8260 0.3051 0.030 Uiso 1 calc R . . 
C1' C -0.0955(3) 0.6363(3) 0.20517(9) 0.0267(6) Uani 1 d . . . 
H1'A H -0.0705 0.5498 0.2201 0.032 Uiso 1 calc R . . 
H1'B H -0.1028 0.6151 0.1751 0.032 Uiso 1 calc R . . 
C2' C -0.2497(3) 0.6935(3) 0.22069(9) 0.0303(7) Uani 1 d . . . 
H2'A H -0.2740 0.7801 0.2058 0.036 Uiso 1 calc R . . 
H2'B H -0.3332 0.6263 0.2148 0.036 Uiso 1 calc R . . 
C3' C -0.2420(3) 0.7210(3) 0.26674(9) 0.0292(7) Uani 1 d . . . 
O3' O -0.3506(2) 0.7155(3) 0.29004(7) 0.0465(6) Uani 1 d . . . 
C1" C 0.1758(3) 0.7517(3) 0.35385(8) 0.0283(6) Uani 1 d . . . 
H1" H 0.0881 0.8191 0.3537 0.034 Uiso 1 calc R . . 
C2" C 0.1672(4) 0.6700(3) 0.39438(9) 0.0352(7) Uani 1 d . . . 
H2"D H 0.2522 0.6015 0.3953 0.042 Uiso 1 calc R . . 
H2"E H 0.1799 0.7334 0.4183 0.042 Uiso 1 calc R . . 
C3" C 0.3262(4) 0.8337(3) 0.35345(9) 0.0388(8) Uani 1 d . . . 
H3"A H 0.3327 0.8875 0.3277 0.058 Uiso 1 calc R . . 
H3"B H 0.4142 0.7701 0.3550 0.058 Uiso 1 calc R . . 
H3"C H 0.3285 0.8962 0.3774 0.058 Uiso 1 calc R . . 
O3" O 0.0220(2) 0.6011(2) 0.39740(6) 0.0377(5) Uani 1 d . . . 
Si Si -0.04311(10) 0.50459(9) 0.43562(2) 0.0306(2) Uani 1 d . . . 
C1S C 0.0872(4) 0.3529(3) 0.44522(9) 0.0379(8) Uani 1 d . . . 
H1S H 0.0312 0.2895 0.4646 0.045 Uiso 1 calc R . . 
C2S C 0.2426(4) 0.3903(4) 0.46604(10) 0.0440(8) Uani 1 d . . . 
H2SA H 0.3036 0.3062 0.4704 0.066 Uiso 1 calc R . . 
H2SB H 0.2228 0.4346 0.4929 0.066 Uiso 1 calc R . . 
H2SC H 0.3002 0.4538 0.4481 0.066 Uiso 1 calc R . . 
C3S C 0.1169(5) 0.2719(4) 0.40466(11) 0.0560(10) Uani 1 d . . . 
H3SA H 0.1847 0.1932 0.4105 0.084 Uiso 1 calc R . . 
H3SB H 0.1665 0.3326 0.3843 0.084 Uiso 1 calc R . . 
H3SC H 0.0182 0.2385 0.3935 0.084 Uiso 1 calc R . . 
C4S C -0.0510(4) 0.6121(4) 0.48420(9) 0.0435(8) Uani 1 d . . . 
H4S H 0.0593 0.6304 0.4919 0.052 Uiso 1 calc R . . 
C5S C -0.1213(5) 0.5369(5) 0.52162(10) 0.0694(13) Uani 1 d . . . 
H5SA H -0.1199 0.5979 0.5459 0.104 Uiso 1 calc R . . 
H5SB H -0.0606 0.4538 0.5276 0.104 Uiso 1 calc R . . 
H5SC H -0.2283 0.5108 0.5153 0.104 Uiso 1 calc R . . 
C6S C -0.1245(6) 0.7534(4) 0.47827(13) 0.0733(13) Uani 1 d . . . 
H6SA H -0.1259 0.8025 0.5049 0.110 Uiso 1 calc R . . 
H6SB H -0.2307 0.7422 0.4681 0.110 Uiso 1 calc R . . 
H6SC H -0.0642 0.8063 0.4580 0.110 Uiso 1 calc R . . 
C7S C -0.2330(4) 0.4438(3) 0.41397(10) 0.0389(8) Uani 1 d . . . 
H7S H -0.2059 0.3958 0.3874 0.047 Uiso 1 calc R . . 
C8S C -0.3455(4) 0.5570(4) 0.40140(12) 0.0539(10) Uani 1 d . . . 
H8SA H -0.4398 0.5153 0.3900 0.081 Uiso 1 calc R . . 
H8SB H -0.2975 0.6158 0.3802 0.081 Uiso 1 calc R . . 
H8SC H -0.3719 0.6127 0.4258 0.081 Uiso 1 calc R . . 
C9S C -0.3164(4) 0.3353(4) 0.44013(12) 0.0598(11) Uani 1 d . . . 
H9SA H -0.4131 0.3088 0.4263 0.090 Uiso 1 calc R . . 
H9SB H -0.3397 0.3735 0.4677 0.090 Uiso 1 calc R . . 
H9SC H -0.2500 0.2539 0.4432 0.090 Uiso 1 calc R . . 
O21 O 0.1931(2) 0.6204(2) 0.16863(6) 0.0302(5) Uani 1 d . . . 
C21 C 0.3216(4) 0.5747(3) 0.14920(9) 0.0346(7) Uani 1 d . . . 
O22 O 0.4512(3) 0.5968(3) 0.16007(7) 0.0474(6) Uani 1 d . . . 
C22 C 0.2772(4) 0.4878(4) 0.11236(10) 0.0490(9) Uani 1 d . . . 
H22A H 0.2449 0.3962 0.1219 0.074 Uiso 1 calc R . . 
H22B H 0.3663 0.4786 0.0937 0.074 Uiso 1 calc R . . 
H22C H 0.1916 0.5319 0.0974 0.074 Uiso 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 
O1 0.0236(9) 0.0214(9) 0.0244(8) -0.0015(8) 0.0024(8) 0.0007(8) 
C1 0.0259(14) 0.0202(13) 0.0218(13) 0.0005(11) -0.0035(12) 0.0032(12) 
C2 0.0229(14) 0.0252(15) 0.0253(14) -0.0049(12) -0.0007(12) 0.0024(12) 
C2"' 0.0262(15) 0.0308(16) 0.0340(16) 0.0012(13) 0.0020(13) -0.0027(13) 
C3 0.0198(13) 0.0251(14) 0.0346(15) -0.0001(12) 0.0000(13) 0.0025(13) 
C4 0.0204(14) 0.0287(15) 0.0306(14) 0.0058(13) -0.0024(12) -0.0022(13) 
O 0.0303(10) 0.0301(11) 0.0338(10) 0.0060(9) -0.0019(9) 0.0047(10) 
C5 0.0237(14) 0.0212(14) 0.0288(14) 0.0060(12) -0.0035(12) 0.0013(12) 
C6 0.0233(14) 0.0239(14) 0.0277(14) 0.0004(12) -0.0021(12) -0.0044(12) 
C7 0.0210(14) 0.0280(14) 0.0262(14) 0.0005(12) 0.0021(12) -0.0004(13) 
C1' 0.0239(14) 0.0281(15) 0.0283(14) -0.0010(12) -0.0053(12) -0.0016(13) 
C2' 0.0196(14) 0.0292(15) 0.0420(17) 0.0001(13) -0.0073(13) -0.0017(13) 
C3' 0.0198(15) 0.0309(16) 0.0369(16) 0.0009(13) -0.0012(14) 0.0034(13) 
O3' 0.0239(12) 0.0713(17) 0.0443(13) 0.0019(13) 0.0067(11) -0.0016(12) 
C1" 0.0262(15) 0.0309(15) 0.0278(14) 0.0030(13) -0.0030(13) -0.0033(14) 
C2" 0.0322(16) 0.0464(19) 0.0272(15) 0.0052(14) -0.0038(13) -0.0103(16) 
C3" 0.0399(18) 0.0428(18) 0.0339(16) -0.0031(15) -0.0032(15) -0.0148(17) 
O3" 0.0331(11) 0.0498(13) 0.0302(10) 0.0112(10) -0.0015(9) -0.0114(11) 
Si 0.0300(4) 0.0364(4) 0.0253(4) 0.0040(4) 0.0023(3) -0.0011(4) 
C1S 0.0332(17) 0.0440(19) 0.0366(17) 0.0030(15) 0.0006(14) -0.0025(16) 
C2S 0.0389(18) 0.0471(19) 0.0461(18) 0.0059(17) -0.0063(16) 0.0027(18) 
C3S 0.058(2) 0.055(2) 0.055(2) -0.0149(19) 0.000(2) 0.017(2) 
C4S 0.0429(19) 0.052(2) 0.0356(16) -0.0035(16) -0.0026(16) 0.0052(19) 
C5S 0.085(3) 0.093(3) 0.0302(17) -0.005(2) 0.012(2) -0.006(3) 
C6S 0.086(3) 0.068(3) 0.066(3) -0.018(2) -0.001(3) 0.026(3) 
C7S 0.0321(16) 0.0466(19) 0.0381(16) 0.0053(15) 0.0026(14) -0.0013(16) 
C8S 0.0354(19) 0.058(2) 0.069(2) 0.015(2) -0.0029(19) -0.0016(18) 
C9S 0.047(2) 0.067(3) 0.065(2) 0.021(2) -0.003(2) -0.021(2) 
O21 0.0301(11) 0.0344(11) 0.0260(10) -0.0063(9) 0.0012(9) 0.0018(10) 
C21 0.0338(17) 0.0342(17) 0.0357(16) -0.0006(14) 0.0048(15) 0.0082(16) 
O22 0.0304(12) 0.0625(15) 0.0493(13) -0.0153(12) 0.0001(11) 0.0078(13) 
C22 0.049(2) 0.054(2) 0.0440(18) -0.0142(18) 0.0038(16) 0.007(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 
O1 C7 1.426(3) . ? 
O1 C1 1.443(3) . ? 
C1 C1' 1.523(4) . ? 
C1 C2 1.535(4) . ? 
C2 O21 1.482(3) . ? 
C2 C2"' 1.522(4) . ? 
C2 C3 1.539(4) . ? 
C3 C4 1.502(4) . ? 
C4 O 1.465(3) . ? 
C4 C5 1.474(4) . ? 
O C5 1.451(3) . ? 
C5 C6 1.514(4) . ? 
C5 C1" 1.523(4) . ? 
C6 C7 1.530(4) . ? 
C7 C3' 1.519(4) . ? 
C1' C2' 1.526(4) . ? 
C2' C3' 1.506(4) . ? 
C3' O3' 1.202(3) . ? 
C1" C3" 1.523(4) . ? 
C1" C2" 1.526(4) . ? 
C2" O3" 1.424(4) . ? 
O3" Si 1.643(2) . ? 
Si C7S 1.876(3) . ? 
Si C1S 1.877(4) . ? 
Si C4S 1.879(3) . ? 
C1S C3S 1.543(4) . ? 
C1S C2S 1.544(4) . ? 
C4S C6S 1.522(5) . ? 
C4S C5S 1.532(5) . ? 
C7S C8S 1.520(5) . ? 
C7S C9S 1.528(5) . ? 
O21 C21 1.348(3) . ? 
C21 O22 1.193(4) . ? 
C21 C22 1.503(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 
C7 O1 C1 118.7(2) . . ? 
O1 C1 C1' 112.7(2) . . ? 
O1 C1 C2 108.1(2) . . ? 
C1' C1 C2 117.1(2) . . ? 
O21 C2 C2"' 112.2(2) . . ? 
O21 C2 C1 99.9(2) . . ? 
C2"' C2 C1 109.3(2) . . ? 
O21 C2 C3 107.0(2) . . ? 
C2"' C2 C3 112.9(2) . . ? 
C1 C2 C3 114.9(2) . . ? 
C4 C3 C2 115.5(2) . . ? 
O C4 C5 59.13(17) . . ? 
O C4 C3 113.6(2) . . ? 
C5 C4 C3 124.0(2) . . ? 
C5 O C4 60.74(17) . . ? 
O C5 C4 60.13(17) . . ? 
O C5 C6 114.8(2) . . ? 
C4 C5 C6 117.8(2) . . ? 
O C5 C1" 113.9(2) . . ? 
C4 C5 C1" 121.9(2) . . ? 
C6 C5 C1" 115.6(2) . . ? 
C5 C6 C7 110.4(2) . . ? 
O1 C7 C3' 111.8(2) . . ? 
O1 C7 C6 114.5(2) . . ? 
C3' C7 C6 110.1(2) . . ? 
C1 C1' C2' 109.5(2) . . ? 
C3' C2' C1' 110.3(2) . . ? 
O3' C3' C2' 124.8(3) . . ? 
O3' C3' C7 120.6(3) . . ? 
C2' C3' C7 114.6(2) . . ? 
C5 C1" C3" 114.5(2) . . ? 
C5 C1" C2" 110.1(2) . . ? 
C3" C1" C2" 108.6(2) . . ? 
O3" C2" C1" 110.2(2) . . ? 
C2" O3" Si 128.28(18) . . ? 
O3" Si C7S 101.56(13) . . ? 
O3" Si C1S 111.31(14) . . ? 
C7S Si C1S 109.82(16) . . ? 
O3" Si C4S 108.58(15) . . ? 
C7S Si C4S 116.78(16) . . ? 
C1S Si C4S 108.63(15) . . ? 
C3S C1S C2S 110.0(3) . . ? 
C3S C1S Si 111.0(2) . . ? 
C2S C1S Si 114.1(2) . . ? 
C6S C4S C5S 111.2(3) . . ? 
C6S C4S Si 114.2(2) . . ? 
C5S C4S Si 113.8(3) . . ? 
C8S C7S C9S 110.0(3) . . ? 
C8S C7S Si 115.6(2) . . ? 
C9S C7S Si 115.1(2) . . ? 
C21 O21 C2 122.1(2) . . ? 
O22 C21 O21 125.3(3) . . ? 
O22 C21 C22 124.8(3) . . ? 
O21 C21 C22 109.9(3) . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C7 O1 C1 C1' 18.9(3) . . . . ? 
C7 O1 C1 C2 -112.2(2) . . . . ? 
O1 C1 C2 O21 178.99(19) . . . . ? 
C1' C1 C2 O21 50.4(3) . . . . ? 
O1 C1 C2 C2"' -63.2(3) . . . . ? 
C1' C1 C2 C2"' 168.2(2) . . . . ? 
O1 C1 C2 C3 64.8(3) . . . . ? 
C1' C1 C2 C3 -63.8(3) . . . . ? 
O21 C2 C3 C4 173.9(2) . . . . ? 
C2"' C2 C3 C4 50.0(3) . . . . ? 
C1 C2 C3 C4 -76.2(3) . . . . ? 
C2 C3 C4 O 155.0(2) . . . . ? 
C2 C3 C4 C5 87.3(3) . . . . ? 
C3 C4 O C5 -116.7(3) . . . . ? 
C4 O C5 C6 109.1(3) . . . . ? 
C4 O C5 C1" -114.3(3) . . . . ? 
C3 C4 C5 O 99.2(3) . . . . ? 
O C4 C5 C6 -104.2(3) . . . . ? 
C3 C4 C5 C6 -5.0(4) . . . . ? 
O C4 C5 C1" 101.2(3) . . . . ? 
C3 C4 C5 C1" -159.6(3) . . . . ? 
O C5 C6 C7 -151.1(2) . . . . ? 
C4 C5 C6 C7 -83.2(3) . . . . ? 
C1" C5 C6 C7 73.1(3) . . . . ? 
C1 O1 C7 C3' -53.5(3) . . . . ? 
C1 O1 C7 C6 72.6(3) . . . . ? 
C5 C6 C7 O1 47.6(3) . . . . ? 
C5 C6 C7 C3' 174.5(2) . . . . ? 
O1 C1 C1' C2' 38.7(3) . . . . ? 
C2 C1 C1' C2' 165.0(2) . . . . ? 
C1 C1' C2' C3' -61.6(3) . . . . ? 
C1' C2' C3' O3' -150.6(3) . . . . ? 
C1' C2' C3' C7 28.0(4) . . . . ? 
O1 C7 C3' O3' -154.5(3) . . . . ? 
C6 C7 C3' O3' 77.1(4) . . . . ? 
O1 C7 C3' C2' 26.9(3) . . . . ? 
C6 C7 C3' C2' -101.5(3) . . . . ? 
O C5 C1" C3" 72.5(3) . . . . ? 
C4 C5 C1" C3" 3.9(4) . . . . ? 
C6 C5 C1" C3" -151.3(3) . . . . ? 
O C5 C1" C2" -50.3(3) . . . . ? 
C4 C5 C1" C2" -118.9(3) . . . . ? 
C6 C5 C1" C2" 85.9(3) . . . . ? 
C5 C1" C2" O3" -58.7(3) . . . . ? 
C3" C1" C2" O3" 175.2(2) . . . . ? 
C1" C2" O3" Si -178.2(2) . . . . ? 
C2" O3" Si C7S -176.1(3) . . . . ? 
C2" O3" Si C1S -59.2(3) . . . . ? 
C2" O3" Si C4S 60.3(3) . . . . ? 
O3" Si C1S C3S -52.5(3) . . . . ? 
C7S Si C1S C3S 59.2(3) . . . . ? 
C4S Si C1S C3S -172.0(2) . . . . ? 
O3" Si C1S C2S 72.5(2) . . . . ? 
C7S Si C1S C2S -175.8(2) . . . . ? 
C4S Si C1S C2S -47.0(3) . . . . ? 
O3" Si C4S C6S 46.6(3) . . . . ? 
C7S Si C4S C6S -67.4(3) . . . . ? 
C1S Si C4S C6S 167.8(3) . . . . ? 
O3" Si C4S C5S 175.8(3) . . . . ? 
C7S Si C4S C5S 61.8(3) . . . . ? 
C1S Si C4S C5S -63.0(3) . . . . ? 
O3" Si C7S C8S -57.4(3) . . . . ? 
C1S Si C7S C8S -175.3(2) . . . . ? 
C4S Si C7S C8S 60.5(3) . . . . ? 
O3" Si C7S C9S 172.7(3) . . . . ? 
C1S Si C7S C9S 54.8(3) . . . . ? 
C4S Si C7S C9S -69.4(3) . . . . ? 
C2"' C2 O21 C21 54.6(3) . . . . ? 
C1 C2 O21 C21 170.2(2) . . . . ? 
C3 C2 O21 C21 -69.7(3) . . . . ? 
C2 O21 C21 O22 -7.2(5) . . . . ? 
C2 O21 C21 C22 171.1(2) . . . . ? 
  
_diffrn_measured_fraction_theta_max    0.998 
_diffrn_reflns_theta_full              25.03 
_diffrn_measured_fraction_theta_full   0.998 
_refine_diff_density_max    0.19
_refine_diff_density_min   -0.22 
_refine_diff_density_rms    0.04