Facile Synthesis of (3,5-(CF3)2C6H3)2BX (X = H, OMe, F, Cl, Br): Reagents for the Introduction of a Strong Boryl Acceptor Unit
Samigullin, Kamil; Bolte, Michael; Lerner, Hans-Wolfram; Wagner, Matthias; Organometallics  (2014) 140626134355006–; doi:10.1021/om500476d

data_4083771
_publ_section_title
;
 Facile Synthesis of (3,5-(CF3)2C6H3)2BX (X = H, OMe, F, Cl, Br):
 Reagents for the Introduction of a Strong Boryl Acceptor Unit
;
_journal_name_full               Organometallics
_journal_page_first              140626134355006
_journal_paper_doi               10.1021/om500476d
_journal_year                    2014
_chemical_formula_moiety         'C16 H6 B Br F12'
_chemical_formula_sum            'C16 H6 B Br F12'
_chemical_formula_weight         516.93
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-1997
_cell_angle_alpha                106.284(6)
_cell_angle_beta                 102.371(6)
_cell_angle_gamma                99.235(6)
_cell_formula_units_Z            2
_cell_length_a                   8.2816(6)
_cell_length_b                   9.2342(7)
_cell_length_c                   12.7869(9)
_cell_measurement_reflns_used    22056
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      3.4
_cell_volume                     891.11(12)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14745
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.429
_diffrn_reflns_theta_min         3.352
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    2.427
_exptl_absorpt_correction_T_max  0.683
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         3625
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+2.4443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3364
_reflns_number_total             3625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500476d_si_002.cif
_cod_data_source_block           wa1728
_cod_database_code               4083771
_shelx_estimated_absorpt_t_min   0.669
_shelx_estimated_absorpt_t_max   0.683
_shelxl_version_number           2013-3
_shelx_res_checksum              13217