# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_pca21
_database_code_depnum_ccdc_archive 'CCDC 1039794'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;
#============================================================================== 

#==============================================================================
_audit_creation_date             '9 February 2011'
_audit_creation_method           SHELXL-97

#==============================================================================

#  CHEMICAL DATA

#==============================================================================

_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H26 O5 Si'
_chemical_formula_sum            'C15 H26 O5 Si'
_chemical_formula_weight         314.45
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_absolute_configuration unk

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'

#==============================================================================

#   CRYSTAL DATA

#==============================================================================


_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c a 21    '
_symmetry_space_group_name_Hall  'P 2c -2ac '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   15.0354(13)
_cell_length_b                   6.2653(5)
_cell_length_c                   36.895(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3475.5(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    90
_cell_measurement_reflns_used    9973
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      27.50
_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9572
_exptl_absorpt_correction_T_max  0.9717
_exptl_absorpt_process_details   
;
SADABS Sheldrick 1996
;
_exptl_special_details           
; 
 ? 
;
#==============================================================================

#   EXPERIMENTAL DATA

#==============================================================================

_diffrn_ambient_temperature      90
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            18545
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         1.10
_diffrn_reflns_theta_max         27.54
_reflns_number_total             7833
_reflns_number_gt                7498
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_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)+(0.0570P)²+0.4476P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.75(7)
_refine_ls_number_reflns         7833
_refine_ls_number_parameters     396
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0866
_refine_ls_wR_factor_gt          0.0855
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.002
_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 0.10137(9) 0.1143(2) 0.14736(4) 0.0168(3) Uani 1 1 d . . .
C2 C 0.22295(8) -0.0550(2) 0.12312(4) 0.0179(3) Uani 1 1 d . . .
H2A H 0.2464 -0.0249 0.0986 0.021 Uiso 1 1 calc R . .
H2B H 0.2432 -0.1984 0.1308 0.021 Uiso 1 1 calc R . .
C3 C 0.25171(9) 0.1116(2) 0.14943(4) 0.0142(3) Uani 1 1 d . . .
C4 C 0.34582(8) 0.1533(2) 0.16071(4) 0.0143(3) Uani 1 1 d . . .
H4 H 0.3650 0.0382 0.1778 0.017 Uiso 1 1 calc R . .
C5 C 0.35208(9) 0.3708(2) 0.18039(4) 0.0149(3) Uani 1 1 d . . .
C6 C 0.27620(9) 0.3908(2) 0.20845(4) 0.0167(3) Uani 1 1 d . . .
H6 H 0.2834 0.5279 0.2220 0.020 Uiso 1 1 calc R . .
C7 C 0.18478(9) 0.3890(2) 0.19002(4) 0.0163(3) Uani 1 1 d . . .
H7A H 0.1376 0.3692 0.2084 0.020 Uiso 1 1 calc R . .
H7B H 0.1744 0.5271 0.1777 0.020 Uiso 1 1 calc R . .
C8 C 0.18123(8) 0.2116(2) 0.16304(4) 0.0148(3) Uani 1 1 d . . .
C9 C 0.44307(9) 0.3957(3) 0.19842(4) 0.0206(3) Uani 1 1 d . . .
H9A H 0.4900 0.3724 0.1804 0.031 Uiso 1 1 calc R . .
H9B H 0.4490 0.2908 0.2180 0.031 Uiso 1 1 calc R . .
H9C H 0.4485 0.5400 0.2084 0.031 Uiso 1 1 calc R . .
C10 C 0.14414(11) -0.0681(3) 0.25123(5) 0.0323(4) Uani 1 1 d . . .
H10A H 0.1024 -0.0012 0.2343 0.048 Uiso 1 1 calc R . .
H10B H 0.1113 -0.1255 0.2720 0.048 Uiso 1 1 calc R . .
H10C H 0.1757 -0.1843 0.2390 0.048 Uiso 1 1 calc R . .
C11 C 0.16346(15) 0.3574(3) 0.28931(6) 0.0381(5) Uani 1 1 d . . .
H11A H 0.2054 0.4681 0.2971 0.057 Uiso 1 1 calc R . .
H11B H 0.1311 0.3028 0.3104 0.057 Uiso 1 1 calc R . .
H11C H 0.1211 0.4183 0.2720 0.057 Uiso 1 1 calc R . .
C12 C 0.31030(12) 0.0168(3) 0.29961(4) 0.0289(4) Uani 1 1 d . . .
C13 C 0.36292(14) -0.1621(3) 0.28120(5) 0.0361(4) Uani 1 1 d . . .
H13A H 0.4101 -0.2115 0.2975 0.054 Uiso 1 1 calc R . .
H13B H 0.3894 -0.1081 0.2587 0.054 Uiso 1 1 calc R . .
H13C H 0.3229 -0.2810 0.2756 0.054 Uiso 1 1 calc R . .
C14 C 0.37534(14) 0.1932(3) 0.31135(5) 0.0397(5) Uani 1 1 d . . .
H14A H 0.3428 0.3047 0.3244 0.060 Uiso 1 1 calc R . .
H14B H 0.4037 0.2552 0.2899 0.060 Uiso 1 1 calc R . .
H14C H 0.4210 0.1322 0.3272 0.060 Uiso 1 1 calc R . .
C15 C 0.26328(16) -0.0712(3) 0.33355(5) 0.0409(5) Uani 1 1 d . . .
H15A H 0.2223 -0.1853 0.3265 0.061 Uiso 1 1 calc R . .
H15B H 0.2299 0.0438 0.3454 0.061 Uiso 1 1 calc R . .
H15C H 0.3077 -0.1280 0.3504 0.061 Uiso 1 1 calc R . .
C16 C 1.17458(9) 0.3897(2) 1.06359(4) 0.0168(3) Uani 1 1 d . . .
C17 C 1.05344(8) 0.5587(2) 1.08835(4) 0.0175(3) Uani 1 1 d . . .
H17A H 1.0334 0.7026 1.0808 0.021 Uiso 1 1 calc R . .
H17B H 1.0300 0.5279 1.1129 0.021 Uiso 1 1 calc R . .
C18 C 1.02397(9) 0.3933(2) 1.06182(4) 0.0140(3) Uani 1 1 d . . .
C19 C 0.92994(8) 0.3510(2) 1.05101(4) 0.0137(3) Uani 1 1 d . . .
H19 H 0.9101 0.4666 1.0342 0.016 Uiso 1 1 calc R . .
C20 C 0.92337(9) 0.1344(2) 1.03104(4) 0.0155(3) Uani 1 1 d . . .
C21 C 0.99835(9) 0.1174(2) 1.00267(4) 0.0168(3) Uani 1 1 d . . .
H21 H 0.9910 -0.0191 0.9889 0.020 Uiso 1 1 calc R . .
C22 C 1.09071(9) 0.1184(2) 1.02063(4) 0.0161(3) Uani 1 1 d . . .
H22A H 1.1016 -0.0204 1.0327 0.019 Uiso 1 1 calc R . .
H22B H 1.1372 0.1398 1.0020 0.019 Uiso 1 1 calc R . .
C23 C 1.09473(8) 0.2940(2) 1.04785(4) 0.0148(3) Uani 1 1 d . . .
C24 C 0.83219(10) 0.1092(3) 1.01336(4) 0.0212(3) Uani 1 1 d . . .
H24A H 0.8263 -0.0358 1.0037 0.032 Uiso 1 1 calc R . .
H24B H 0.8261 0.2127 0.9936 0.032 Uiso 1 1 calc R . .
H24C H 0.7857 0.1344 1.0315 0.032 Uiso 1 1 calc R . .
C25 C 1.10932(13) 0.1621(3) 0.92127(5) 0.0339(4) Uani 1 1 d . . .
H25A H 1.1565 0.1113 0.9374 0.051 Uiso 1 1 calc R . .
H25B H 1.1357 0.2162 0.8988 0.051 Uiso 1 1 calc R . .
H25C H 1.0689 0.0440 0.9156 0.051 Uiso 1 1 calc R . .
C26 C 1.12718(11) 0.5845(3) 0.96030(6) 0.0321(4) Uani 1 1 d . . .
H26A H 1.0957 0.6941 0.9742 0.048 Uiso 1 1 calc R . .
H26B H 1.1566 0.6509 0.9395 0.048 Uiso 1 1 calc R . .
H26C H 1.1718 0.5157 0.9757 0.048 Uiso 1 1 calc R . .
C27 C 0.95998(11) 0.4982(3) 0.91258(4) 0.0267(3) Uani 1 1 d . . .
C28 C 0.90503(12) 0.6689(3) 0.93238(5) 0.0332(4) Uani 1 1 d . . .
H28A H 0.9441 0.7858 0.9400 0.050 Uiso 1 1 calc R . .
H28B H 0.8768 0.6055 0.9538 0.050 Uiso 1 1 calc R . .
H28C H 0.8591 0.7243 0.9160 0.050 Uiso 1 1 calc R . .
C29 C 0.89614(15) 0.3209(3) 0.89964(6) 0.0438(5) Uani 1 1 d . . .
H29A H 0.8695 0.2503 0.9207 0.066 Uiso 1 1 calc R . .
H29B H 0.9293 0.2160 0.8853 0.066 Uiso 1 1 calc R . .
H29C H 0.8491 0.3839 0.8847 0.066 Uiso 1 1 calc R . .
C30 C 1.00490(15) 0.6011(3) 0.87932(5) 0.0381(4) Uani 1 1 d . . .
H30A H 0.9598 0.6724 0.8644 0.057 Uiso 1 1 calc R . .
H30B H 1.0344 0.4903 0.8649 0.057 Uiso 1 1 calc R . .
H30C H 1.0490 0.7059 0.8874 0.057 Uiso 1 1 calc R . .
O1 O 0.02350(7) 0.15200(17) 0.15307(3) 0.0224(2) Uani 1 1 d . . .
O2 O 0.12644(6) -0.04059(17) 0.12377(3) 0.0207(2) Uani 1 1 d . . .
O3 O 0.40262(6) 0.15021(17) 0.12967(3) 0.0171(2) Uani 1 1 d . . .
H3 H 0.4465 0.0710 0.1338 0.026 Uiso 1 1 calc R . .
O4 O 0.33576(6) 0.54190(16) 0.15575(3) 0.0172(2) Uani 1 1 d . . .
H4A H 0.3729 0.5369 0.1388 0.026 Uiso 1 1 calc R . .
O5 O 0.28669(7) 0.21724(19) 0.23304(3) 0.0225(2) Uani 1 1 d . . .
O6 O 1.25240(7) 0.35031(17) 1.05800(3) 0.0217(2) Uani 1 1 d . . .
O7 O 1.14999(6) 0.54346(17) 1.08764(3) 0.0203(2) Uani 1 1 d . . .
O8 O 0.87386(6) 0.35239(16) 1.08224(3) 0.0171(2) Uani 1 1 d . . .
H8 H 0.8315 0.4376 1.0789 0.026 Uiso 1 1 calc R . .
O9 O 0.94070(6) -0.03709(17) 1.05536(3) 0.0181(2) Uani 1 1 d . . .
H9 H 0.9015 -0.0393 1.0716 0.027 Uiso 1 1 calc R . .
O10 O 0.98690(7) 0.29179(19) 0.97832(3) 0.0235(2) Uani 1 1 d . . .
Si1 Si 0.22586(3) 0.13455(6) 0.267315(11) 0.02130(10) Uani 1 1 d . . .
Si2 Si 1.04613(3) 0.38049(6) 0.944014(11) 0.01921(9) 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 O1 1.2129(17) . ?
C1 O2 1.3567(18) . ?
C1 C8 1.4657(18) . ?
C2 O2 1.4541(15) . ?
C2 C3 1.4897(19) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C8 1.3294(19) . ?
C3 C4 1.4979(18) . ?
C4 O3 1.4288(16) . ?
C4 C5 1.547(2) . ?
C4 H4 1.0000 . ?
C5 O4 1.4269(17) . ?
C5 C9 1.5290(18) . ?
C5 C6 1.5455(19) . ?
C6 O5 1.4247(18) . ?
C6 C7 1.5335(19) . ?
C6 H6 1.0000 . ?
C7 C8 1.493(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 Si1 1.8641(17) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 Si1 1.8677(18) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.531(3) . ?
C12 C14 1.538(2) . ?
C12 C15 1.540(2) . ?
C12 Si1 1.8910(18) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 O6 1.2134(18) . ?
C16 O7 1.3610(18) . ?
C16 C23 1.4621(19) . ?
C17 O7 1.4550(15) . ?
C17 C18 1.493(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C23 1.3360(19) . ?
C18 C19 1.4928(18) . ?
C19 O8 1.4279(16) . ?
C19 C20 1.5473(19) . ?
C19 H19 1.0000 . ?
C20 O9 1.4239(17) . ?
C20 C24 1.5264(19) . ?
C20 C21 1.5420(19) . ?
C21 O10 1.4253(18) . ?
C21 C22 1.5386(19) . ?
C21 H21 1.0000 . ?
C22 C23 1.491(2) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 Si2 1.8652(17) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 Si2 1.8653(17) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.536(3) . ?
C27 C30 1.542(3) . ?
C27 C29 1.544(2) . ?
C27 Si2 1.8886(17) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O3 H3 0.8400 . ?
O4 H4A 0.8400 . ?
O5 Si1 1.6444(11) . ?
O8 H8 0.8400 . ?
O9 H9 0.8400 . ?
O10 Si2 1.6443(11) . ?

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 C1 O2 121.26(13) . . ?
O1 C1 C8 129.88(14) . . ?
O2 C1 C8 108.85(12) . . ?
O2 C2 C3 103.61(11) . . ?
O2 C2 H2A 111.0 . . ?
C3 C2 H2A 111.0 . . ?
O2 C2 H2B 111.0 . . ?
C3 C2 H2B 111.0 . . ?
H2A C2 H2B 109.0 . . ?
C8 C3 C2 110.18(12) . . ?
C8 C3 C4 124.47(13) . . ?
C2 C3 C4 125.26(12) . . ?
O3 C4 C3 109.86(11) . . ?
O3 C4 C5 110.59(11) . . ?
C3 C4 C5 109.96(11) . . ?
O3 C4 H4 108.8 . . ?
C3 C4 H4 108.8 . . ?
C5 C4 H4 108.8 . . ?
O4 C5 C9 110.76(11) . . ?
O4 C5 C6 103.84(11) . . ?
C9 C5 C6 111.16(12) . . ?
O4 C5 C4 110.62(11) . . ?
C9 C5 C4 110.39(11) . . ?
C6 C5 C4 109.91(11) . . ?
O5 C6 C7 112.09(12) . . ?
O5 C6 C5 106.45(11) . . ?
C7 C6 C5 111.36(12) . . ?
O5 C6 H6 109.0 . . ?
C7 C6 H6 109.0 . . ?
C5 C6 H6 109.0 . . ?
C8 C7 C6 109.44(11) . . ?
C8 C7 H7A 109.8 . . ?
C6 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
C6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
C3 C8 C1 107.93(13) . . ?
C3 C8 C7 125.04(12) . . ?
C1 C8 C7 127.03(12) . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C14 108.82(16) . . ?
C13 C12 C15 109.63(15) . . ?
C14 C12 C15 108.67(15) . . ?
C13 C12 Si1 110.66(12) . . ?
C14 C12 Si1 108.91(12) . . ?
C15 C12 Si1 110.11(14) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O6 C16 O7 121.11(13) . . ?
O6 C16 C23 129.86(14) . . ?
O7 C16 C23 109.03(12) . . ?
O7 C17 C18 103.82(11) . . ?
O7 C17 H17A 111.0 . . ?
C18 C17 H17A 111.0 . . ?
O7 C17 H17B 111.0 . . ?
C18 C17 H17B 111.0 . . ?
H17A C17 H17B 109.0 . . ?
C23 C18 C17 109.87(12) . . ?
C23 C18 C19 124.64(13) . . ?
C17 C18 C19 125.43(12) . . ?
O8 C19 C18 110.03(11) . . ?
O8 C19 C20 110.60(11) . . ?
C18 C19 C20 110.09(11) . . ?
O8 C19 H19 108.7 . . ?
C18 C19 H19 108.7 . . ?
C20 C19 H19 108.7 . . ?
O9 C20 C24 110.82(12) . . ?
O9 C20 C21 103.99(11) . . ?
C24 C20 C21 111.06(12) . . ?
O9 C20 C19 110.50(12) . . ?
C24 C20 C19 110.58(11) . . ?
C21 C20 C19 109.71(11) . . ?
O10 C21 C22 112.17(11) . . ?
O10 C21 C20 106.65(11) . . ?
C22 C21 C20 111.55(12) . . ?
O10 C21 H21 108.8 . . ?
C22 C21 H21 108.8 . . ?
C20 C21 H21 108.8 . . ?
C23 C22 C21 109.25(11) . . ?
C23 C22 H22A 109.8 . . ?
C21 C22 H22A 109.8 . . ?
C23 C22 H22B 109.8 . . ?
C21 C22 H22B 109.8 . . ?
H22A C22 H22B 108.3 . . ?
C18 C23 C16 108.05(13) . . ?
C18 C23 C22 124.84(12) . . ?
C16 C23 C22 127.11(12) . . ?
C20 C24 H24A 109.5 . . ?
C20 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C20 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2 C25 H25A 109.5 . . ?
Si2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C30 108.86(15) . . ?
C28 C27 C29 108.27(16) . . ?
C30 C27 C29 109.06(15) . . ?
C28 C27 Si2 110.42(11) . . ?
C30 C27 Si2 110.58(13) . . ?
C29 C27 Si2 109.60(12) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C1 O2 C2 109.41(11) . . ?
C4 O3 H3 109.5 . . ?
C5 O4 H4A 109.5 . . ?
C6 O5 Si1 131.96(9) . . ?
C16 O7 C17 109.22(10) . . ?
C19 O8 H8 109.5 . . ?
C20 O9 H9 109.5 . . ?
C21 O10 Si2 132.76(9) . . ?
O5 Si1 C10 109.66(8) . . ?
O5 Si1 C11 112.21(7) . . ?
C10 Si1 C11 108.46(9) . . ?
O5 Si1 C12 103.53(7) . . ?
C10 Si1 C12 112.18(8) . . ?
C11 Si1 C12 110.80(9) . . ?
O10 Si2 C25 111.97(8) . . ?
O10 Si2 C26 109.73(8) . . ?
C25 Si2 C26 108.35(9) . . ?
O10 Si2 C27 103.48(7) . . ?
C25 Si2 C27 111.08(9) . . ?
C26 Si2 C27 112.22(8) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.043
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p-1
_database_code_depnum_ccdc_archive 'CCDC 1039795'
_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;
#============================================================================== 
# SI-87-2
#==============================================================================
_audit_creation_date             '28 September 2012'
_audit_creation_method           SHELXL-97

#==============================================================================

#  CHEMICAL DATA

#==============================================================================

_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H16 O5'
_chemical_formula_sum            'C13 H16 O5'
_chemical_formula_weight         252.26
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_absolute_configuration .

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'

#==============================================================================

#   CRYSTAL DATA

#==============================================================================


_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                   7.353(2)
_cell_length_b                   12.521(4)
_cell_length_c                   13.790(4)
_cell_angle_alpha                109.346(3)
_cell_angle_beta                 90.415(4)
_cell_angle_gamma                98.193(3)
_cell_volume                     1183.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    90
_cell_measurement_reflns_used    2906
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      27.53
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.9476
_exptl_absorpt_correction_T_max  0.9733
_exptl_absorpt_process_details   
;
Crystal Faces plugin in Bruker APEX2 software
;
_exptl_special_details           
; 
 ? 
;

#==============================================================================

#   EXPERIMENTAL DATA

#==============================================================================

_diffrn_ambient_temperature      90
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            11419
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.71
_diffrn_reflns_theta_max         25.02
_reflns_number_total             4163
_reflns_number_gt                3146
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_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)+(0.0604P)²+0.3390P] 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         4163
_refine_ls_number_parameters     333
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1149
_refine_ls_wR_factor_gt          0.1045
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.3868(3) 0.24743(17) 0.75425(14) 0.0159(4) Uani 1 1 d . . .
C2 C 0.5163(3) 0.15820(17) 0.71232(15) 0.0171(4) Uani 1 1 d . . .
C3 C 0.7027(3) 0.21618(17) 0.68833(16) 0.0192(5) Uani 1 1 d . . .
H3 H 0.6776 0.2513 0.6351 0.023 Uiso 1 1 calc R . .
C4 C 0.8027(3) 0.31118(17) 0.78194(15) 0.0189(5) Uani 1 1 d . . .
H4A H 0.8419 0.2780 0.8331 0.023 Uiso 1 1 calc R . .
H4B H 0.9137 0.3506 0.7607 0.023 Uiso 1 1 calc R . .
C5 C 0.6746(3) 0.39471(17) 0.82840(14) 0.0153(4) Uani 1 1 d . . .
C6 C 0.7048(3) 0.50815(17) 0.88604(15) 0.0162(4) Uani 1 1 d . . .
C7 C 0.4031(3) 0.45851(16) 0.86405(15) 0.0169(4) Uani 1 1 d . . .
H7 H 0.2749 0.4618 0.8669 0.020 Uiso 1 1 calc R . .
C8 C 0.4783(3) 0.36243(17) 0.81430(15) 0.0160(4) Uani 1 1 d . . .
C9 C 0.8725(3) 0.59065(17) 0.92620(15) 0.0174(4) Uani 1 1 d . . .
C10 C 0.8528(3) 0.70920(17) 0.99516(16) 0.0207(5) Uani 1 1 d . . .
H10A H 0.8365 0.7080 1.0660 0.025 Uiso 1 1 calc R . .
H10B H 0.7399 0.7307 0.9721 0.025 Uiso 1 1 calc R . .
C11 C 1.0147(3) 0.80072(17) 0.99783(16) 0.0227(5) Uani 1 1 d . . .
H11A H 1.1308 0.7741 1.0095 0.027 Uiso 1 1 calc R . .
H11B H 1.0179 0.8130 0.9305 0.027 Uiso 1 1 calc R . .
C12 C 1.0007(3) 0.91305(18) 1.08239(17) 0.0284(5) Uani 1 1 d . . .
H12A H 0.8861 0.9397 1.0708 0.043 Uiso 1 1 calc R . .
H12B H 1.1058 0.9705 1.0817 0.043 Uiso 1 1 calc R . .
H12C H 1.0011 0.9015 1.1493 0.043 Uiso 1 1 calc R . .
C13 C 0.5334(3) 0.09773(19) 0.79022(17) 0.0252(5) Uani 1 1 d . . .
H13A H 0.4130 0.0558 0.7958 0.038 Uiso 1 1 calc R . .
H13B H 0.5765 0.1545 0.8575 0.038 Uiso 1 1 calc R . .
H13C H 0.6216 0.0439 0.7676 0.038 Uiso 1 1 calc R . .
C1B C 1.1279(3) 0.76867(17) 0.53877(15) 0.0170(4) Uani 1 1 d . . .
C2B C 0.9916(3) 0.84939(17) 0.59168(15) 0.0177(4) Uani 1 1 d . . .
C3B C 0.8171(3) 0.82790(17) 0.52088(16) 0.0192(5) Uani 1 1 d . . .
H3B H 0.8525 0.8455 0.4573 0.023 Uiso 1 1 calc R . .
C4B C 0.7157(3) 0.70530(16) 0.48984(15) 0.0174(4) Uani 1 1 d . . .
H4B1 H 0.6637 0.6903 0.5509 0.021 Uiso 1 1 calc R . .
H4B2 H 0.6131 0.6942 0.4389 0.021 Uiso 1 1 calc R . .
C5B C 0.8477(3) 0.62436(17) 0.44433(15) 0.0156(4) Uani 1 1 d . . .
C6B C 0.8225(3) 0.51565(17) 0.37570(15) 0.0168(4) Uani 1 1 d . . .
C7B C 1.1217(3) 0.56367(17) 0.41310(15) 0.0184(4) Uani 1 1 d . . .
H7B H 1.2500 0.5607 0.4146 0.022 Uiso 1 1 calc R . .
C8B C 1.0418(3) 0.65546(17) 0.46882(15) 0.0159(4) Uani 1 1 d . . .
C9B C 0.6555(3) 0.43656(17) 0.32456(15) 0.0177(4) Uani 1 1 d . . .
C10B C 0.6792(3) 0.32632(17) 0.24152(15) 0.0192(5) Uani 1 1 d . . .
H10C H 0.7752 0.2918 0.2660 0.023 Uiso 1 1 calc R . .
H10D H 0.7234 0.3441 0.1801 0.023 Uiso 1 1 calc R . .
C11B C 0.5049(3) 0.23892(18) 0.20997(16) 0.0230(5) Uani 1 1 d . . .
H11C H 0.4010 0.2774 0.2003 0.028 Uiso 1 1 calc R . .
H11D H 0.4763 0.2069 0.2658 0.028 Uiso 1 1 calc R . .
C12B C 0.5243(3) 0.14177(19) 0.11076(17) 0.0272(5) Uani 1 1 d . . .
H12D H 0.5468 0.1728 0.0546 0.041 Uiso 1 1 calc R . .
H12E H 0.4108 0.0861 0.0940 0.041 Uiso 1 1 calc R . .
H12F H 0.6278 0.1039 0.1199 0.041 Uiso 1 1 calc R . .
C13B C 0.9475(3) 0.83039(19) 0.69402(15) 0.0229(5) Uani 1 1 d . . .
H13D H 1.0589 0.8546 0.7401 0.034 Uiso 1 1 calc R . .
H13E H 0.9034 0.7490 0.6810 0.034 Uiso 1 1 calc R . .
H13F H 0.8520 0.8755 0.7262 0.034 Uiso 1 1 calc R . .
O1 O 0.21987(18) 0.22154(12) 0.73934(10) 0.0221(3) Uani 1 1 d . . .
O2 O 0.53647(17) 0.54779(11) 0.90842(10) 0.0178(3) Uani 1 1 d . . .
O3 O 1.02282(18) 0.56005(12) 0.90539(11) 0.0223(3) Uani 1 1 d . . .
O4 O 0.44364(18) 0.07896(12) 0.61503(10) 0.0207(3) Uani 1 1 d . . .
H4 H 0.3450 0.0404 0.6227 0.031 Uiso 1 1 calc R . .
O5 O 0.82450(18) 0.13659(12) 0.64782(12) 0.0259(4) Uani 1 1 d . . .
H5 H 0.7639 0.0731 0.6128 0.039 Uiso 1 1 calc R . .
O1B O 1.29359(18) 0.79593(12) 0.55737(11) 0.0228(3) Uani 1 1 d . . .
O2B O 0.99200(17) 0.47778(11) 0.35561(10) 0.0183(3) Uani 1 1 d . . .
O3B O 0.50413(18) 0.46362(12) 0.34905(11) 0.0237(3) Uani 1 1 d . . .
O4B O 1.08631(18) 0.96320(12) 0.61186(11) 0.0223(3) Uani 1 1 d . . .
H4B3 H 1.0141 1.0104 0.6365 0.033 Uiso 1 1 calc R . .
O5B O 0.70013(19) 0.90666(12) 0.57642(11) 0.0242(4) Uani 1 1 d . . .
H5B H 0.6094 0.9036 0.5377 0.036 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
C1 O1 1.222(2) . ?
C1 C8 1.462(3) . ?
C1 C2 1.540(3) . ?
C2 O4 1.424(2) . ?
C2 C13 1.519(3) . ?
C2 C3 1.548(3) . ?
C3 O5 1.414(2) . ?
C3 C4 1.530(3) . ?
C3 H3 1.0000 . ?
C4 C5 1.496(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.363(3) . ?
C5 C8 1.436(3) . ?
C6 O2 1.397(2) . ?
C6 C9 1.464(3) . ?
C7 O2 1.346(2) . ?
C7 C8 1.368(3) . ?
C7 H7 0.9500 . ?
C9 O3 1.226(2) . ?
C9 C10 1.502(3) . ?
C10 C11 1.521(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.518(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C1B O1B 1.219(2) . ?
C1B C8B 1.473(3) . ?
C1B C2B 1.539(3) . ?
C2B O4B 1.430(2) . ?
C2B C13B 1.536(3) . ?
C2B C3B 1.543(3) . ?
C3B O5B 1.432(2) . ?
C3B C4B 1.526(3) . ?
C3B H3B 1.0000 . ?
C4B C5B 1.494(3) . ?
C4B H4B1 0.9900 . ?
C4B H4B2 0.9900 . ?
C5B C6B 1.362(3) . ?
C5B C8B 1.432(3) . ?
C6B O2B 1.394(2) . ?
C6B C9B 1.471(3) . ?
C7B O2B 1.351(2) . ?
C7B C8B 1.367(3) . ?
C7B H7B 0.9500 . ?
C9B O3B 1.227(2) . ?
C9B C10B 1.507(3) . ?
C10B C11B 1.518(3) . ?
C10B H10C 0.9900 . ?
C10B H10D 0.9900 . ?
C11B C12B 1.524(3) . ?
C11B H11C 0.9900 . ?
C11B H11D 0.9900 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
O4 H4 0.8400 . ?
O5 H5 0.8400 . ?
O4B H4B3 0.8400 . ?
O5B H5B 0.8400 . ?

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 C1 C8 123.42(18) . . ?
O1 C1 C2 121.43(18) . . ?
C8 C1 C2 115.14(16) . . ?
O4 C2 C13 111.00(16) . . ?
O4 C2 C1 109.87(15) . . ?
C13 C2 C1 107.72(16) . . ?
O4 C2 C3 104.02(15) . . ?
C13 C2 C3 113.84(16) . . ?
C1 C2 C3 110.36(16) . . ?
O5 C3 C4 107.59(15) . . ?
O5 C3 C2 112.10(16) . . ?
C4 C3 C2 113.50(16) . . ?
O5 C3 H3 107.8 . . ?
C4 C3 H3 107.8 . . ?
C2 C3 H3 107.8 . . ?
C5 C4 C3 108.70(16) . . ?
C5 C4 H4A 109.9 . . ?
C3 C4 H4A 109.9 . . ?
C5 C4 H4B 109.9 . . ?
C3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
C6 C5 C8 105.95(17) . . ?
C6 C5 C4 132.23(18) . . ?
C8 C5 C4 121.81(17) . . ?
C5 C6 O2 109.65(16) . . ?
C5 C6 C9 132.91(17) . . ?
O2 C6 C9 117.43(17) . . ?
O2 C7 C8 110.42(16) . . ?
O2 C7 H7 124.8 . . ?
C8 C7 H7 124.8 . . ?
C7 C8 C5 106.85(17) . . ?
C7 C8 C1 129.42(17) . . ?
C5 C8 C1 123.71(17) . . ?
O3 C9 C6 119.35(18) . . ?
O3 C9 C10 122.49(18) . . ?
C6 C9 C10 118.12(16) . . ?
C9 C10 C11 114.52(16) . . ?
C9 C10 H10A 108.6 . . ?
C11 C10 H10A 108.6 . . ?
C9 C10 H10B 108.6 . . ?
C11 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?
C12 C11 C10 111.34(17) . . ?
C12 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
C12 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
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 . . ?
C2 C13 H13A 109.5 . . ?
C2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1B C1B C8B 123.32(18) . . ?
O1B C1B C2B 121.79(18) . . ?
C8B C1B C2B 114.82(16) . . ?
O4B C2B C13B 109.50(16) . . ?
O4B C2B C1B 106.09(15) . . ?
C13B C2B C1B 107.83(16) . . ?
O4B C2B C3B 110.37(16) . . ?
C13B C2B C3B 112.14(16) . . ?
C1B C2B C3B 110.70(16) . . ?
O5B C3B C4B 110.15(16) . . ?
O5B C3B C2B 106.47(16) . . ?
C4B C3B C2B 113.38(16) . . ?
O5B C3B H3B 108.9 . . ?
C4B C3B H3B 108.9 . . ?
C2B C3B H3B 108.9 . . ?
C5B C4B C3B 108.98(16) . . ?
C5B C4B H4B1 109.9 . . ?
C3B C4B H4B1 109.9 . . ?
C5B C4B H4B2 109.9 . . ?
C3B C4B H4B2 109.9 . . ?
H4B1 C4B H4B2 108.3 . . ?
C6B C5B C8B 106.18(17) . . ?
C6B C5B C4B 131.92(18) . . ?
C8B C5B C4B 121.89(17) . . ?
C5B C6B O2B 109.69(17) . . ?
C5B C6B C9B 132.05(17) . . ?
O2B C6B C9B 118.25(17) . . ?
O2B C7B C8B 110.32(17) . . ?
O2B C7B H7B 124.8 . . ?
C8B C7B H7B 124.8 . . ?
C7B C8B C5B 106.81(17) . . ?
C7B C8B C1B 129.68(18) . . ?
C5B C8B C1B 123.47(17) . . ?
O3B C9B C6B 119.27(18) . . ?
O3B C9B C10B 122.82(18) . . ?
C6B C9B C10B 117.89(17) . . ?
C9B C10B C11B 114.17(16) . . ?
C9B C10B H10C 108.7 . . ?
C11B C10B H10C 108.7 . . ?
C9B C10B H10D 108.7 . . ?
C11B C10B H10D 108.7 . . ?
H10C C10B H10D 107.6 . . ?
C10B C11B C12B 111.83(17) . . ?
C10B C11B H11C 109.3 . . ?
C12B C11B H11C 109.3 . . ?
C10B C11B H11D 109.3 . . ?
C12B C11B H11D 109.3 . . ?
H11C C11B H11D 107.9 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C2B C13B H13D 109.5 . . ?
C2B C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C2B C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C7 O2 C6 107.13(15) . . ?
C2 O4 H4 109.5 . . ?
C3 O5 H5 109.5 . . ?
C7B O2B C6B 107.00(15) . . ?
C2B O4B H4B3 109.5 . . ?
C3B O5B H5B 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.048
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_p21n_a
_database_code_depnum_ccdc_archive 'CCDC 1039796'

_audit_update_record             
;
2014-12-17 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;
#============================================================================== 
# SI-7-90-1
#==============================================================================
_audit_creation_date             'Nobember 27 2014'
_audit_creation_method           SHELXL-97

#==============================================================================

#  CHEMICAL DATA

#==============================================================================

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H36 O5 Si'
_chemical_formula_sum            'C22 H36 O5 Si'
_chemical_formula_weight         408.60
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_absolute_configuration .

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'

#==============================================================================

#   CRYSTAL DATA

#==============================================================================


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.8360(15)
_cell_length_b                   9.2966(10)
_cell_length_c                   18.3676(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.4880(10)
_cell_angle_gamma                90.00
_cell_volume                     2323.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    90
_cell_measurement_reflns_used    3736
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      27.53
_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.9764
_exptl_absorpt_correction_T_max  0.9918
_exptl_absorpt_process_details   
;
Crystal Faces plugin in Bruker APEX2 software
;
_exptl_special_details           ?

#==============================================================================

#   EXPERIMENTAL DATA

#==============================================================================

_diffrn_ambient_temperature      90
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            11033
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.50
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4094
_reflns_number_gt                3504
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_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)+(0.0384P)²+0.9937P] 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         4094
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.0900
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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
C1 C 0.07229(11) 0.73411(16) 0.65289(10) 0.0190(3) Uani 1 1 d . . .
H1 H 0.0246 0.7821 0.6086 0.023 Uiso 1 1 calc R . .
C2 C 0.15887(11) 0.68245(16) 0.65529(9) 0.0161(3) Uani 1 1 d . . .
C3 C 0.20038(11) 0.68824(16) 0.59289(9) 0.0161(3) Uani 1 1 d . . .
H3 H 0.2035 0.7903 0.5769 0.019 Uiso 1 1 calc R . .
C4 C 0.30295(11) 0.61898(16) 0.62085(9) 0.0160(3) Uani 1 1 d . . .
C5 C 0.36143(10) 0.62943(16) 0.71101(9) 0.0157(3) Uani 1 1 d . . .
H5 H 0.3699 0.7335 0.7260 0.019 Uiso 1 1 calc R . .
C6 C 0.30896(11) 0.55620(16) 0.75751(9) 0.0168(3) Uani 1 1 d . . .
H6A H 0.3041 0.4515 0.7469 0.020 Uiso 1 1 calc R . .
H6B H 0.3463 0.5713 0.8152 0.020 Uiso 1 1 calc R . .
C7 C 0.20814(11) 0.61995(15) 0.73199(9) 0.0161(3) Uani 1 1 d . . .
C8 C 0.14763(11) 0.63757(16) 0.77122(10) 0.0176(3) Uani 1 1 d . . .
C9 C 0.15778(11) 0.60553(16) 0.85188(10) 0.0195(4) Uani 1 1 d . . .
C10 C 0.08263(12) 0.66950(17) 0.87881(10) 0.0210(4) Uani 1 1 d . . .
H10A H 0.0163 0.6397 0.8413 0.025 Uiso 1 1 calc R . .
H10B H 0.0861 0.7757 0.8765 0.025 Uiso 1 1 calc R . .
C11 C 0.09618(13) 0.62559(18) 0.96235(10) 0.0259(4) Uani 1 1 d . . .
H11A H 0.0779 0.5231 0.9622 0.031 Uiso 1 1 calc R . .
H11B H 0.1663 0.6357 0.9983 0.031 Uiso 1 1 calc R . .
C12 C 0.03401(14) 0.7166(2) 0.99347(11) 0.0339(4) Uani 1 1 d . . .
H12A H 0.0531 0.8178 0.9950 0.051 Uiso 1 1 calc R . .
H12B H 0.0444 0.6847 1.0471 0.051 Uiso 1 1 calc R . .
H12C H -0.0356 0.7058 0.9584 0.051 Uiso 1 1 calc R . .
C13 C 0.18255(11) 0.45999(16) 0.53769(9) 0.0192(3) Uani 1 1 d . . .
C14 C 0.11984(12) 0.36221(17) 0.56494(10) 0.0242(4) Uani 1 1 d . . .
H14A H 0.1205 0.3977 0.6154 0.036 Uiso 1 1 calc R . .
H14B H 0.1464 0.2643 0.5722 0.036 Uiso 1 1 calc R . .
H14C H 0.0522 0.3617 0.5248 0.036 Uiso 1 1 calc R . .
C15 C 0.18825(13) 0.40789(19) 0.46172(10) 0.0278(4) Uani 1 1 d . . .
H15A H 0.1227 0.4117 0.4185 0.042 Uiso 1 1 calc R . .
H15B H 0.2125 0.3086 0.4687 0.042 Uiso 1 1 calc R . .
H15C H 0.2333 0.4696 0.4486 0.042 Uiso 1 1 calc R . .
C16 C 0.36042(12) 0.68041(18) 0.57531(10) 0.0227(4) Uani 1 1 d . . .
H16A H 0.4177 0.6196 0.5840 0.034 Uiso 1 1 calc R . .
H16B H 0.3823 0.7781 0.5941 0.034 Uiso 1 1 calc R . .
H16C H 0.3182 0.6831 0.5185 0.034 Uiso 1 1 calc R . .
C17 C 0.57055(13) 0.62028(19) 0.89865(10) 0.0283(4) Uani 1 1 d . . .
H17A H 0.5191 0.6775 0.9056 0.042 Uiso 1 1 calc R . .
H17B H 0.6352 0.6544 0.9354 0.042 Uiso 1 1 calc R . .
H17C H 0.5627 0.5189 0.9096 0.042 Uiso 1 1 calc R . .
C18 C 0.56482(13) 0.83445(18) 0.77137(12) 0.0330(4) Uani 1 1 d . . .
H18A H 0.5564 0.8448 0.7159 0.050 Uiso 1 1 calc R . .
H18B H 0.6284 0.8748 0.8063 0.050 Uiso 1 1 calc R . .
H18C H 0.5119 0.8859 0.7795 0.050 Uiso 1 1 calc R . .
C19 C 0.66106(11) 0.53512(17) 0.78056(10) 0.0192(3) Uani 1 1 d . . .
C20 C 0.65782(12) 0.37737(17) 0.80432(12) 0.0278(4) Uani 1 1 d . . .
H20A H 0.5938 0.3358 0.7713 0.042 Uiso 1 1 calc R . .
H20B H 0.6676 0.3725 0.8603 0.042 Uiso 1 1 calc R . .
H20C H 0.7099 0.3232 0.7965 0.042 Uiso 1 1 calc R . .
C21 C 0.64826(12) 0.5412(2) 0.69348(11) 0.0296(4) Uani 1 1 d . . .
H21A H 0.7031 0.4910 0.6876 0.044 Uiso 1 1 calc R . .
H21B H 0.6472 0.6418 0.6772 0.044 Uiso 1 1 calc R . .
H21C H 0.5863 0.4947 0.6600 0.044 Uiso 1 1 calc R . .
C22 C 0.76194(12) 0.59887(19) 0.83412(11) 0.0290(4) Uani 1 1 d . . .
H22A H 0.8143 0.5425 0.8280 0.044 Uiso 1 1 calc R . .
H22B H 0.7697 0.5957 0.8896 0.044 Uiso 1 1 calc R . .
H22C H 0.7658 0.6988 0.8187 0.044 Uiso 1 1 calc R . .
O1 O 0.06269(7) 0.70823(11) 0.72212(6) 0.0194(3) Uani 1 1 d . . .
O2 O 0.14449(7) 0.60375(11) 0.52423(6) 0.0179(2) Uani 1 1 d . . .
O3 O 0.27894(7) 0.46984(11) 0.60025(6) 0.0182(2) Uani 1 1 d . . .
O4 O 0.22737(8) 0.53272(12) 0.89552(7) 0.0270(3) Uani 1 1 d . . .
O5 O 0.45649(7) 0.56793(11) 0.73132(6) 0.0169(2) Uani 1 1 d . . .
Si1 Si 0.56039(3) 0.63936(4) 0.79493(3) 0.01751(12) 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 1.356(2) . ?
C1 O1 1.3563(19) . ?
C1 H1 0.9500 . ?
C2 C7 1.427(2) . ?
C2 C3 1.503(2) . ?
C3 O2 1.4358(18) . ?
C3 C4 1.540(2) . ?
C3 H3 1.0000 . ?
C4 O3 1.4439(18) . ?
C4 C16 1.524(2) . ?
C4 C5 1.536(2) . ?
C5 O5 1.4267(17) . ?
C5 C6 1.526(2) . ?
C5 H5 1.0000 . ?
C6 C7 1.500(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.366(2) . ?
C8 O1 1.3881(18) . ?
C8 C9 1.459(2) . ?
C9 O4 1.2276(19) . ?
C9 C10 1.510(2) . ?
C10 C11 1.522(2) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.521(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O2 1.4335(18) . ?
C13 O3 1.4367(18) . ?
C13 C15 1.511(2) . ?
C13 C14 1.521(2) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 Si1 1.8588(18) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 Si1 1.8718(18) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.535(2) . ?
C19 C20 1.536(2) . ?
C19 C22 1.544(2) . ?
C19 Si1 1.8851(16) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
O5 Si1 1.6573(11) . ?

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 O1 111.03(14) . . ?
C2 C1 H1 124.5 . . ?
O1 C1 H1 124.5 . . ?
C1 C2 C7 106.39(14) . . ?
C1 C2 C3 129.32(14) . . ?
C7 C2 C3 124.28(13) . . ?
O2 C3 C2 112.43(12) . . ?
O2 C3 C4 102.25(11) . . ?
C2 C3 C4 112.43(13) . . ?
O2 C3 H3 109.8 . . ?
C2 C3 H3 109.8 . . ?
C4 C3 H3 109.8 . . ?
O3 C4 C16 110.47(12) . . ?
O3 C4 C5 108.52(12) . . ?
C16 C4 C5 111.65(12) . . ?
O3 C4 C3 101.91(11) . . ?
C16 C4 C3 110.80(12) . . ?
C5 C4 C3 113.06(12) . . ?
O5 C5 C6 110.27(12) . . ?
O5 C5 C4 109.35(12) . . ?
C6 C5 C4 112.34(12) . . ?
O5 C5 H5 108.3 . . ?
C6 C5 H5 108.3 . . ?
C4 C5 H5 108.3 . . ?
C7 C6 C5 108.45(12) . . ?
C7 C6 H6A 110.0 . . ?
C5 C6 H6A 110.0 . . ?
C7 C6 H6B 110.0 . . ?
C5 C6 H6B 110.0 . . ?
H6A C6 H6B 108.4 . . ?
C8 C7 C2 106.63(13) . . ?
C8 C7 C6 131.72(14) . . ?
C2 C7 C6 121.61(13) . . ?
C7 C8 O1 109.35(14) . . ?
C7 C8 C9 133.42(14) . . ?
O1 C8 C9 117.12(13) . . ?
O4 C9 C8 119.68(14) . . ?
O4 C9 C10 122.81(15) . . ?
C8 C9 C10 117.47(14) . . ?
C9 C10 C11 113.99(14) . . ?
C9 C10 H10A 108.8 . . ?
C11 C10 H10A 108.8 . . ?
C9 C10 H10B 108.8 . . ?
C11 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C12 C11 C10 111.94(15) . . ?
C12 C11 H11A 109.2 . . ?
C10 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
C10 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
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 . . ?
O2 C13 O3 106.06(11) . . ?
O2 C13 C15 107.62(13) . . ?
O3 C13 C15 110.79(12) . . ?
O2 C13 C14 111.31(12) . . ?
O3 C13 C14 108.62(13) . . ?
C15 C13 C14 112.28(14) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 C16 H16A 109.5 . . ?
C4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C21 C19 C20 109.05(14) . . ?
C21 C19 C22 109.61(13) . . ?
C20 C19 C22 108.51(13) . . ?
C21 C19 Si1 110.56(11) . . ?
C20 C19 Si1 109.55(10) . . ?
C22 C19 Si1 109.53(11) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C1 O1 C8 106.60(11) . . ?
C13 O2 C3 107.98(11) . . ?
C13 O3 C4 109.50(11) . . ?
C5 O5 Si1 124.64(9) . . ?
O5 Si1 C17 110.92(7) . . ?
O5 Si1 C18 109.50(7) . . ?
C17 Si1 C18 109.48(9) . . ?
O5 Si1 C19 105.16(6) . . ?
C17 Si1 C19 110.45(8) . . ?
C18 Si1 C19 111.28(8) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.041

