Selective Aromatic C-F and C-H Bond Activation with Silylenes of Different Coordinate Silicon
Anukul Jana; Prinson P. Samuel; Gašper Tavčar; Herbert W. Roesky; Carola Schulzke; Journal of the American Chemical Society 132 (2010) 10164–10170; doi:10.1021/ja103988d

data_4102699
_publ_section_title
;
 Selective Aromatic C-F and C-H Bond Activation with Silylenes of
 Different Coordinate Silicon
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10164
_journal_page_last               10170
_journal_paper_doi               10.1021/ja103988d
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C22 H23 Cl F8 N2 Si'
_chemical_formula_weight         530.96
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.57(3)
_cell_angle_beta                 82.58(3)
_cell_angle_gamma                89.18(3)
_cell_formula_units_Z            2
_cell_length_a                   9.785(2)
_cell_length_b                   9.976(2)
_cell_length_c                   13.842(3)
_cell_measurement_reflns_used    11809
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      54.3
_cell_measurement_theta_min      3.0
_cell_volume                     1339.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  IPDSII
_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  0.0747
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11809
_diffrn_reflns_theta_full        27.14
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  0.9426
_exptl_absorpt_correction_T_min  0.7205
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.032(6)
_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   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5769
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0832
_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^)+(0.1160P)^2^+1.1808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2210
_refine_ls_wR_factor_ref         0.2396
_reflns_number_gt                3994
_reflns_number_total             5769
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja103988d_si_001_2.cif
_cod_data_source_block           psp03
_cod_original_cell_volume        1339.8(5)
_cod_database_code               4102699