Synthesis, Molecular Structure, and Reactivity of the Isolable Silylenoid with a Tricoordinate Silicon
Gregory Molev; Dmitry Bravo-Zhivotovskii; Miriam Karni; Boris Tumanskii; Mark Botoshansky; Yitzhak Apeloig; Journal of the American Chemical Society 128 (2006) 2784–2785; doi:10.1021/ja0575880

data_4110433
_publ_section_title
;
 Synthesis, Molecular Structure, and Reactivity of the Isolable Silylenoid
 with a Tricoordinate Silicon
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2784
_journal_page_last               2785
_journal_paper_doi               10.1021/ja0575880
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C30 H66 F Li O3 Si3'
_chemical_formula_weight         586.05
_chemical_name_common            'Dimitry-77 new'
_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                 111.40(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.181(2)
_cell_length_b                   18.490(4)
_cell_length_c                   19.334(4)
_cell_measurement_reflns_used    26845
_cell_measurement_temperature    180(1)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.58
_cell_volume                     3721.5(15)
_computing_cell_refinement       'DENZO SMN (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 2001)'
_computing_data_reduction        'DENZO SMN (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      180(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  0.094
_diffrn_reflns_av_sigmaI/netI    0.1037
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26840
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_description       plate
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.118
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         6890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0985P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1801
_reflns_number_gt                3879
_reflns_number_total             6890
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0575880si20051107_092003.cif
_cod_data_source_block           Dimitry77new
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4110433