Double Silylation of Olefin with HSiCl3 in the Presence of Bu4PCl. New Synthetic Method for α,β-Bis(trichlorosilyl)alkanes
Seung-Hyun Kang; Joon Soo Han; Weon Cheol Lim; Il Nam Jung; Myong Euy Lee; Bok Ryul Yoo; Organometallics 25 (2006) 318–319; doi:10.1021/om050880w

data_4063305
_publ_section_title
;
 Double Silylation of Olefin with HSiCl3 in the Presence of Bu4PCl. New
 Synthetic Method for \a,\b-Bis(trichlorosilyl)alkanes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              318
_journal_page_last               319
_journal_paper_doi               10.1021/om050880w
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C7 H6 Cl3 Si'
_chemical_formula_weight         224.56
_chemical_name_common
1R(S),2S(R)-1,2-Bis(trichlorosilyl)-1,2-diphenylethane
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.85(2)
_cell_angle_beta                 71.86(2)
_cell_angle_gamma                68.32(2)
_cell_formula_units_Z            2
_cell_length_a                   6.4332(15)
_cell_length_b                   8.6245(15)
_cell_length_c                   9.584(2)
_cell_measurement_temperature    293(2)
_cell_volume                     468.47(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.766
_diffrn_measured_fraction_theta_max 0.766
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1703
_diffrn_reflns_theta_full        26.96
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.037
_exptl_absorpt_correction_T_max  0.7260
_exptl_absorpt_correction_T_min  0.6045
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             226
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1305P)^2^+0.2200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1794
_refine_ls_wR_factor_ref         0.1798
_reflns_number_gt                1532
_reflns_number_total             1546
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               4063305