Separating Electrophilicity and Lewis Acidity: The Synthesis, Characterization, and Electrochemistry of the Electron Deficient Tris(aryl)boranes B(C6F5)3-n(C6Cl5)n (n= 1-3)
Andrew E. Ashley; Thomas J. Herrington; Gregory G. Wildgoose; Hasna Zaher; Amber L. Thompson; Nicholas H. Rees; Tobias Krämer; Dermot O'Hare; Journal of the American Chemical Society 133 (2011) 14727–14740; doi:10.1021/ja205037t

data_4106772
_publ_contact_author
;
Dermot O'Hare
;
_publ_contact_author_email       dermot.ohare@chem.ox.ac.uk
_publ_section_title
;
 Separating Electrophilicity and Lewis Acidity: The Synthesis,
 Characterization, and Electrochemistry of the Electron Deficient
 Tris(aryl)boranes B(C6F5)3-n(C6Cl5)n (n= 1-3)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14727
_journal_page_last               14740
_journal_paper_doi               10.1021/ja205037t
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C18 B1 Cl10 F5'
_chemical_formula_sum            'C18 B Cl10 F5'
_chemical_formula_weight         676.53
_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_primary     direct
_audit_creation_date             10-08-27
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                69.5030(7)
_cell_angle_beta                 85.0590(7)
_cell_angle_gamma                70.2181(11)
_cell_formula_units_Z            2
_cell_length_a                   9.6279(1)
_cell_length_b                   11.0451(2)
_cell_length_c                   12.3145(3)
_cell_measurement_reflns_used    4987
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1153.47(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20665
_diffrn_reflns_theta_full        26.970
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         5.148
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.257
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9498
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5265
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.0005041
_refine_ls_shift/su_mean         0.0000307
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 20.1 30.8 15.4 4.13 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1251
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1251
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -13
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                3999
_reflns_number_total             5265
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.59
_oxford_diffrn_Wilson_scale      9.94
_oxford_refine_ls_r_factor_ref   0.0593
_oxford_refine_ls_scale          0.3132(4)
_oxford_reflns_number_all        5265
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 6296
_cod_data_source_file            ja205037t_si_002_3.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C18 B1 Cl10 F5'
_cod_database_code               4106772