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_4115172
_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         'C16 H31 Ge Li O Si2 '
_chemical_formula_sum            'C16 H31 Ge Li O Si2'
_chemical_formula_weight         375.12
_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'
_cell_angle_alpha                90
_cell_angle_beta                 107.2502(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.880(2)
_cell_length_b                   15.941(2)
_cell_length_c                   12.802(1)
_cell_measurement_reflns_used    5850
_cell_measurement_temperature    123.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.8
_cell_volume                     2315.4(5)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 7.32
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21429
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    1.422
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       Prism
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.35
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3215
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          -0.0020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0501P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                3215
_reflns_number_total             5299
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ja026705d_s2_1.cif
_cod_data_source_block
'_bis(tert-butyldimethylsilyl)germyllithium-THF'
_cod_original_cell_volume        2315.3(5)
_cod_original_formula_sum        'C16 H31 Ge Li O Si2 '
_cod_database_code               4115172