 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C10 H20 O2 Si'
_chemical_formula_weight          200.35
 
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                    5.14490(10)
_cell_length_b                    10.2655(3)
_cell_length_c                    11.7941(3)
_cell_angle_alpha                 104.7620(10)
_cell_angle_beta                  98.9520(10)
_cell_angle_gamma                 101.329(2)
_cell_volume                      576.55(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     4209
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.50
_exptl_crystal_size_mid           0.25
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.154
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              220
_exptl_absorpt_coefficient_mu     0.174
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.9179
_exptl_absorpt_correction_T_max   0.9660
_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          'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'ω and φ scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'
_diffrn_reflns_number             7070
_diffrn_reflns_av_R_equivalents   0.0518
_diffrn_reflns_av_sigmaI/netI     0.0411
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -15
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          3.18
_diffrn_reflns_theta_max          27.50
_reflns_number_total              2617
_reflns_number_gt                 2221
_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)+(0.0861P)²+0.1561P] 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      SHELXL
_refine_ls_extinction_coef        0.08(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          2617
_refine_ls_number_parameters      121
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0620
_refine_ls_R_factor_gt            0.0532
_refine_ls_wR_factor_ref          0.1600
_refine_ls_wR_factor_gt           0.1488
_refine_ls_goodness_of_fit_ref    1.043
_refine_ls_restrained_S_all       1.043
_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 0.7135(4) 0.9285(2) 0.7097(2) 0.0595(5) Uani 1 1 d . . .
H1 H 0.5500 0.9597 0.6804 0.071 Uiso 1 1 calc R . .
C2 C 0.8394(6) 0.8805(3) 0.6008(2) 0.0902(8) Uani 1 1 d . . .
H2A H 0.7881 0.9261 0.5391 0.108 Uiso 1 1 calc R . .
H2B H 1.0399 0.9048 0.6258 0.108 Uiso 1 1 calc R . .
C3 C 0.7302(7) 0.7237(3) 0.5505(3) 0.0977(9) Uani 1 1 d . . .
H3A H 0.6413 0.6978 0.4645 0.117 Uiso 1 1 calc R . .
H3B H 0.8796 0.6766 0.5585 0.117 Uiso 1 1 calc R . .
C4 C 0.5306(6) 0.6827(3) 0.6214(3) 0.0940(9) Uani 1 1 d . . .
H4A H 0.5374 0.5910 0.6327 0.113 Uiso 1 1 calc R . .
H4B H 0.3442 0.6771 0.5800 0.113 Uiso 1 1 calc R . .
C5 C 0.6112(6) 0.7943(3) 0.7407(3) 0.0807(7) Uani 1 1 d . . .
H5A H 0.7562 0.7763 0.7959 0.097 Uiso 1 1 calc R . .
H5B H 0.4535 0.7994 0.7787 0.097 Uiso 1 1 calc R . .
C6 C 1.0624(4) 1.2292(2) 0.78580(19) 0.0557(5) Uani 1 1 d . . .
H6 H 1.1892 1.2038 0.7324 0.067 Uiso 1 1 calc R . .
C7 C 0.8429(5) 1.2754(3) 0.7139(3) 0.0866(8) Uani 1 1 d . . .
H7A H 0.6702 1.2555 0.7407 0.104 Uiso 1 1 calc R . .
H7B H 0.8109 1.2265 0.6272 0.104 Uiso 1 1 calc R . .
C8 C 0.9521(7) 1.4325(3) 0.7384(4) 0.1104(11) Uani 1 1 d . . .
H8A H 0.9892 1.4529 0.6641 0.132 Uiso 1 1 calc R . .
H8B H 0.8163 1.4822 0.7660 0.132 Uiso 1 1 calc R . .
C9 C 1.2060(9) 1.4788(3) 0.8326(4) 0.1138(12) Uani 1 1 d . . .
H9A H 1.2037 1.5634 0.8952 0.137 Uiso 1 1 calc R . .
H9B H 1.3656 1.5000 0.7971 0.137 Uiso 1 1 calc R . .
C10 C 1.2189(6) 1.3603(3) 0.8862(3) 0.0857(8) Uani 1 1 d . . .
H10A H 1.1335 1.3709 0.9566 0.103 Uiso 1 1 calc R . .
H10B H 1.4095 1.3570 0.9117 0.103 Uiso 1 1 calc R . .
O1 O 1.2073(2) 1.03530(17) 0.89498(13) 0.0609(4) Uani 1 1 d . . .
H1A H 1.1631 0.9808 0.9350 0.091 Uiso 1 1 calc R . .
O2 O 0.7692(2) 1.11455(16) 0.94199(13) 0.0573(4) Uani 1 1 d . . .
H2 H 0.6036 1.1000 0.9112 0.086 Uiso 1 1 calc R . .
Si1 Si 0.93664(8) 1.07593(5) 0.83502(4) 0.0483(2) Uani 1 1 d . . .
 
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
C1 0.0453(10) 0.0664(12) 0.0673(12) 0.0285(10) 0.0090(8) 0.0061(8)
C2 0.0860(18) 0.103(2) 0.0682(15) 0.0220(14) 0.0227(13) -0.0065(15)
C3 0.095(2) 0.096(2) 0.0905(19) 0.0123(16) 0.0249(17) 0.0142(16)
C4 0.0903(19) 0.0679(15) 0.116(2) 0.0209(15) 0.0213(17) 0.0102(14)
C5 0.0807(16) 0.0735(15) 0.0876(17) 0.0335(13) 0.0250(13) 0.0007(12)
C6 0.0406(9) 0.0685(12) 0.0646(11) 0.0324(10) 0.0147(8) 0.0089(8)
C7 0.0644(14) 0.0980(19) 0.110(2) 0.0637(17) 0.0055(14) 0.0171(13)
C8 0.103(2) 0.094(2) 0.163(3) 0.073(2) 0.034(2) 0.0389(18)
C9 0.139(3) 0.0740(17) 0.127(3) 0.0422(18) 0.025(2) 0.0093(19)
C10 0.0836(17) 0.0759(15) 0.0852(17) 0.0280(13) 0.0091(14) -0.0067(13)
O1 0.0349(6) 0.0934(11) 0.0713(9) 0.0459(8) 0.0176(6) 0.0214(6)
O2 0.0361(6) 0.0810(9) 0.0649(8) 0.0341(7) 0.0164(6) 0.0166(6)
Si1 0.0310(3) 0.0651(4) 0.0556(4) 0.0304(3) 0.0107(2) 0.0099(2)
 
_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
C1 C5 1.530(3) . ?
C1 C2 1.541(3) . ?
C1 Si1 1.855(2) . ?
C1 H1 1.0000 . ?
C2 C3 1.521(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.485(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.509(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C10 1.525(3) . ?
C6 C7 1.528(3) . ?
C6 Si1 1.8478(19) . ?
C6 H6 1.0000 . ?
C7 C8 1.535(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.483(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.515(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O1 Si1 1.6386(13) . ?
O1 H1A 0.8400 . ?
O2 Si1 1.6459(14) . ?
O2 H2 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
C5 C1 C2 103.6(2) . . ?
C5 C1 Si1 116.08(16) . . ?
C2 C1 Si1 115.29(15) . . ?
C5 C1 H1 107.1 . . ?
C2 C1 H1 107.1 . . ?
Si1 C1 H1 107.1 . . ?
C3 C2 C1 107.1(2) . . ?
C3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
C3 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
C4 C3 C2 106.6(2) . . ?
C4 C3 H3A 110.4 . . ?
C2 C3 H3A 110.4 . . ?
C4 C3 H3B 110.4 . . ?
C2 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
C3 C4 C5 105.8(2) . . ?
C3 C4 H4A 110.6 . . ?
C5 C4 H4A 110.6 . . ?
C3 C4 H4B 110.6 . . ?
C5 C4 H4B 110.6 . . ?
H4A C4 H4B 108.7 . . ?
C4 C5 C1 104.4(2) . . ?
C4 C5 H5A 110.9 . . ?
C1 C5 H5A 110.9 . . ?
C4 C5 H5B 110.9 . . ?
C1 C5 H5B 110.9 . . ?
H5A C5 H5B 108.9 . . ?
C10 C6 C7 104.7(2) . . ?
C10 C6 Si1 115.39(16) . . ?
C7 C6 Si1 114.89(14) . . ?
C10 C6 H6 107.1 . . ?
C7 C6 H6 107.1 . . ?
Si1 C6 H6 107.1 . . ?
C6 C7 C8 105.6(2) . . ?
C6 C7 H7A 110.6 . . ?
C8 C7 H7A 110.6 . . ?
C6 C7 H7B 110.6 . . ?
C8 C7 H7B 110.6 . . ?
H7A C7 H7B 108.8 . . ?
C9 C8 C7 108.1(3) . . ?
C9 C8 H8A 110.1 . . ?
C7 C8 H8A 110.1 . . ?
C9 C8 H8B 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C8 C9 C10 106.7(3) . . ?
C8 C9 H9A 110.4 . . ?
C10 C9 H9A 110.4 . . ?
C8 C9 H9B 110.4 . . ?
C10 C9 H9B 110.4 . . ?
H9A C9 H9B 108.6 . . ?
C9 C10 C6 105.1(2) . . ?
C9 C10 H10A 110.7 . . ?
C6 C10 H10A 110.7 . . ?
C9 C10 H10B 110.7 . . ?
C6 C10 H10B 110.7 . . ?
H10A C10 H10B 108.8 . . ?
Si1 O1 H1A 109.5 . . ?
Si1 O2 H2 109.5 . . ?
O1 Si1 O2 106.54(7) . . ?
O1 Si1 C6 105.98(8) . . ?
O2 Si1 C6 111.26(9) . . ?
O1 Si1 C1 111.84(10) . . ?
O2 Si1 C1 108.70(9) . . ?
C6 Si1 C1 112.37(9) . . ?
 
_diffrn_measured_fraction_theta_max    0.985
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.985
_refine_diff_density_max    0.285
_refine_diff_density_min   -0.271
_refine_diff_density_rms    0.047
