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_4118872
_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            'C52 H109 Li3 O4 Si5'
_chemical_formula_weight         959.66
_chemical_name_common            Dimitry-180
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 92.25(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.474(4)
_cell_length_b                   11.565(2)
_cell_length_c                   50.33(1)
_cell_measurement_reflns_used    25569
_cell_measurement_temperature    240(1)
_cell_measurement_theta_max      25.38
_cell_volume                     12490(4)
_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      240(1)
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0725
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            25569
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.90
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_description       prism
_exptl_crystal_F_000             4256
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0880P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                6052
_reflns_number_total             9875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja308777v_si_002.cif
_cod_data_source_block           Dimitry-180
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4118872