Sila-metalation Route to Hydrido(trialkylsilyl)silyllithiums
Takeaki Iwamoto; Junichiro Okita; Chizuko Kabuto; Mitsuo Kira; Journal of the American Chemical Society 124 (2002) 11604–11605; doi:10.1021/ja026705d

data_4115173
_publ_contact_author_email       ' mkira@si.chem.tohoku.ac.jp '
_publ_contact_author_fax         ' +81-22-217-6589 '
_publ_contact_author_name        ' Mitsuo Kira'
_publ_contact_author_phone       ' +81-22-217-6585 '
_publ_section_title
;
 Sila-metalation Route to Hydrido(trialkylsilyl)silyllithiums
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11604
_journal_page_last               11605
_journal_paper_doi               10.1021/ja026705d
_journal_volume                  124
_journal_year                    2002
_chemical_formula_moiety         'C32 H78 Li2 O2 Si6 '
_chemical_formula_sum            'C32 H78 Li2 O2 Si6'
_chemical_formula_weight         677.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 107.467(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.8427(4)
_cell_length_b                   15.943(1)
_cell_length_c                   12.7700(4)
_cell_measurement_reflns_used    6635
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      28.1
_cell_volume                     2299.91(19)
_computing_data_reduction        'teXsan Ver.1.11'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_detector_area_resol_mean 0.137
_diffrn_measured_fraction_theta_full 0.804
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5185
_diffrn_reflns_theta_full        29.54
_diffrn_reflns_theta_max         29.54
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.978
_exptl_crystal_description       prism
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         5185
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+1.4710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1615
_reflns_number_gt                3959
_reflns_number_total             5185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja026705d_s2_2.cif
_cod_data_source_block           Hydrosilyllithium
_cod_original_cell_volume        2299.9(2)
_cod_original_formula_sum        'C32 H78 Li2 O2 Si6 '
_cod_database_code               4115173