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_4106770
_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 Cl15, C7 H8'
_chemical_formula_sum            'C25 H8 B Cl15'
_chemical_formula_weight         850.94
_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
_audit_creation_date             10-05-17
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                96.8119(7)
_cell_angle_beta                 99.4211(8)
_cell_angle_gamma                90.0255(9)
_cell_formula_units_Z            2
_cell_length_a                   8.9324(2)
_cell_length_b                   13.3079(2)
_cell_length_c                   13.4168(3)
_cell_measurement_reflns_used    6553
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1561.94(5)
_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 0.990
_diffrn_measured_fraction_theta_max 0.984
_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  0.031
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27296
_diffrn_reflns_theta_full        25.274
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         5.118
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.341
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.78
_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    1.809
_exptl_crystal_description       plate
_exptl_crystal_F_000             836.000
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.67
_refine_ls_extinction_coef       64(4)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9641
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7050
_refine_ls_number_restraints     256
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.0039271
_refine_ls_shift/su_mean         0.0001460
_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: 
 16.7 24.0 11.6 2.99 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0944
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0944
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                5350
_reflns_number_total             7050
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.26
_oxford_diffrn_Wilson_scale      9.24
_oxford_refine_ls_r_factor_ref   0.0547
_oxford_refine_ls_scale          0.3311(3)
_oxford_reflns_number_all        7050
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 6259
_cod_data_source_file            ja205037t_si_002_1.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C25 H8 B1 Cl15'
_cod_database_code               4106770