Synthesis of B/Si Bidentate Lewis Acids, o-(Fluorosilyl)(dimesitylboryl)benzenes, and Their Fluoride Ion Affinity
Atsushi Kawachi; Atsushi Tani; Junpei Shimada; Yohsuke Yamamoto; Journal of the American Chemical Society 130 (2008) 4222–4223; doi:10.1021/ja710615r

data_4107623
_publ_section_title
;
 Synthesis of B/Si Bidentate Lewis Acids,
 o-(Fluorosilyl)(dimesitylboryl)benzenes, and Their Fluoride Ion Affinity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4222
_journal_page_last               4223
_journal_paper_doi               10.1021/ja710615r
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C56 H76 B F2 K O8 Si'
_chemical_formula_sum            'C56 H76 B F2 K O8 Si'
_chemical_formula_weight         993.17
_chemical_melting_point          441
_chemical_name_common            Compound_8a
_chemical_name_systematic
; 
Potassium 18-Crown-6 [(2-(Fluorodiphenylsilyl)phenyl]fluorodimesitylborate  
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.7180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9410(2)
_cell_length_b                   16.5240(3)
_cell_length_c                   19.8770(3)
_cell_measurement_temperature    173(2)
_cell_volume                     5467.16(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.3845
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            12080
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.9167
_exptl_absorpt_correction_T_min  0.9167
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       prism
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.279
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       0.051(3)
_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   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         12080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1425P)^2^+2.5795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2128
_refine_ls_wR_factor_ref         0.2271
_reflns_number_gt                10086
_reflns_number_total             12080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja710615r-file005.cif
_cod_data_source_block           Compound_8a
_cod_original_cell_volume        5467.16(14)
_cod_database_code               4107623