Synthesis of Silenyllithiums Li(R'3Si)Si=C(SiR3)(1-Ad) via Transient Silyne-Silylidene Intermediates
Lieby Zborovsky; Roman Dobrovetsky; Mark Botoshansky; Dmitry Bravo-Zhivotovskii; Yitzhak Apeloig; Journal of the American Chemical Society 134 (2012) 18229–18232; doi:10.1021/ja308777v

data_4118871
_publ_section_title
;
 Synthesis of Silenyllithiums Li(R'3Si)Si=C(SiR3)(1-Ad) via Transient
 Silyne-Silylidene Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18229
_journal_page_last               18232
_journal_paper_doi               10.1021/ja308777v
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C37 H73 Li O2 Si3'
_chemical_formula_weight         641.16
_chemical_name_common            Dimitry-171
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.99(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.155(3)
_cell_length_b                   14.310(3)
_cell_length_c                   17.608(4)
_cell_measurement_reflns_used    33812
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      1.84
_cell_volume                     4055.2(15)
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 2006)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'TEXSAN  (MSC, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_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  0.0900
_diffrn_reflns_av_sigmaI/netI    0.0945
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33812
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.050
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         6726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0740P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1571
_reflns_number_gt                3666
_reflns_number_total             6726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja308777v_si_001.cif
_cod_data_source_block           Dimitry-171
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4118871