Site-Selective Silylation of Aliphatic C-H Bonds Mediated by [1,5]-Hydrogen Transfer: Synthesis of α-Sila Benzamides.
Liu, Pei; Tang, Jinghua; Zeng, Xiaoming; Organic letters 18 (2016) 5536–5539; doi:10.1021/acs.orglett.6b02784

data_1544348
_publ_section_title
;
 Site-Selective Silylation of Aliphatic C-H Bonds Mediated by
 [1,5]-Hydrogen Transfer: Synthesis of \a-Sila Benzamides.
;
_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              5536
_journal_page_last               5539
_journal_paper_doi               10.1021/acs.orglett.6b02784
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C11 H17 N O Si'
_chemical_formula_weight         207.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 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                 108.216(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.178(4)
_cell_length_b                   10.104(4)
_cell_length_c                   12.720(5)
_cell_measurement_reflns_used    2698
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.53
_cell_measurement_theta_min      2.92
_cell_volume                     1242.5(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9597
_diffrn_reflns_theta_full        24.64
_diffrn_reflns_theta_max         24.64
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.926
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.792
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.163
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.261
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3768
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.273
_refine_ls_R_factor_all          0.1578
_refine_ls_R_factor_gt           0.1330
_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^)+(0.1941P)^2^+1.3972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3229
_refine_ls_wR_factor_ref         0.3530
_reflns_number_gt                2683
_reflns_number_total             3768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b02784_si_003.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1544348.cif.'
_cod_original_sg_symbol_H-M      Pc
_cod_database_code               1544348