Catalytic Generation of Borenium Ions by Cooperative B-H Bond Activation: The Elusive Direct Electrophilic Borylation of Nitrogen Heterocycles with Pinacolborane
Timo Stahl; Kristine Müther; Yasuhiro Ohki; Kazuyuki Tatsumi; Martin Oestreich; Journal of the American Chemical Society 135 (2013) 10978–10981; doi:10.1021/ja405925w

data_4120232
_publ_section_title
;
 Catalytic Generation of Borenium Ions by Cooperative B-H Bond Activation:
 The Elusive Direct Electrophilic Borylation of Nitrogen Heterocycles with
 Pinacolborane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10978
_journal_page_last               10981
_journal_paper_doi               10.1021/ja405925w
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C70 H67 B2 F24 P Ru S'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_formula_units_Z            2
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_cell_length_c                   21.754(15)
_cell_measurement_reflns_used    11027
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.50
_cell_volume                     3525(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
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_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
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_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0459
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_diffrn_reflns_limit_l_min       -28
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_diffrn_reflns_theta_max         27.53
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_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       block
_exptl_crystal_F_000             1576.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
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_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1237P)^2^+6.8487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2227
_reflns_number_gt                13355
_reflns_number_total             15916
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja405925w_si_002.cif
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