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_4107621
_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         'C42 H64 B F2 K O7 Si'
_chemical_formula_sum            'C42 H64 B F2 K O7 Si'
_chemical_formula_weight         796.93
_chemical_melting_point          428
_chemical_name_common            Compound_7a
_chemical_name_systematic
; 
Potassium 18-Crown-6 [(2-(Fluorodimethylsilyl)phenyl]fluorodimesitylborate  
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.4780(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5490(2)
_cell_length_b                   21.1460(4)
_cell_length_c                   18.4960(4)
_cell_measurement_temperature    173(2)
_cell_volume                     4467.64(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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    0.0282
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10467
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.9428
_exptl_absorpt_correction_T_min  0.9247
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_description       prism
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.219
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.16(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     989
_refine_ls_number_reflns         10467
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1022P)^2^+0.7796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1683
_reflns_number_gt                9394
_reflns_number_total             10467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja710615r-file003.cif
_cod_data_source_block           Compound_7a
_cod_database_code               4107621