Facile Arylation of Four-Coordinate Boron Halides by Borenium Cation Mediated Boro-desilylation and -destannylation.
Crossley, Daniel L.; Cid, Jessica; Curless, Liam D.; Turner, Michael L.; Ingleson, Michael J.; Organometallics 34 (2015) 5767–5774; doi:10.1021/acs.organomet.5b00857

data_4088116
_publ_section_title
;
 Facile Arylation of Four-Coordinate Boron Halides by Borenium Cation
 Mediated Boro-desilylation and -destannylation.
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5767
_journal_page_last               5774
_journal_paper_doi               10.1021/acs.organomet.5b00857
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C11 H8 B Cl N, Al Cl4'
_chemical_formula_sum            'C11 H8 Al B Cl5 N'
_chemical_formula_weight         369.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 98.563(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8789(4)
_cell_length_b                   14.6037(10)
_cell_length_c                   13.5927(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1546.56(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1793
_diffrn_reflns_av_unetI/netI     0.3258
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5635
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_preparation       'Cooled saturated DCM solution to 2 degrees'
_exptl_crystal_recrystallization_method
'Cooled saturated, DCM, solution to 2 degrees'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.2033
_refine_ls_R_factor_gt           0.0727
_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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.2019
_reflns_number_gt                1234
_reflns_number_total             3016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00857_si_002.cif
_cod_data_source_block           amji311red
_cod_database_code               4088116
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C11(H11), C13(H13), C14(H14), C15(H15), C19(H19), C24(H24), C26(H26)
;
_olex2_submission_special_instructions 'No special instructions were received'