Reduction of (Formazanate)boron Difluoride Provides Evidence for an N-Heterocyclic B(I) Carbenoid Intermediate.
Chang, Mu-Chieh; Otten, Edwin; Inorganic chemistry 54 (2015) 8656–8664; doi:10.1021/acs.inorgchem.5b01287

data_4346313
_publ_section_title
;
 Reduction of (Formazanate)boron Difluoride Provides Evidence for an
 N-Heterocyclic B(I) Carbenoid Intermediate.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8656
_journal_page_last               8664
_journal_paper_doi               10.1021/acs.inorgchem.5b01287
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C76 H83 B3 N12 Na O4'
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_space_group_name_Hall           '-P 2yn'
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_atom_sites_solution_hydrogens   geom
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_cell_length_a                   11.1938(4)
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_cell_length_c                   31.0805(11)
_cell_measurement_reflns_used    9750
_cell_measurement_temperature    100(2)
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_computing_cell_refinement       'Bruker SAINT'
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_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.746
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_R_equivalents  0.0468
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_diffrn_reflns_Laue_measured_fraction_full 0.746
_diffrn_reflns_Laue_measured_fraction_max 0.931
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_diffrn_reflns_limit_l_max       34
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_diffrn_reflns_point_group_measured_fraction_full 0.746
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_diffrn_reflns_theta_max         59.214
_diffrn_reflns_theta_min         3.609
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       plate
_exptl_crystal_F_000             2724
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.557
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_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0936
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+19.7970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1851
_refine_ls_wR_factor_ref         0.1942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7747
_reflns_number_total             9451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01287_si_002.cif
_cod_data_source_block           cu_molan222_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4346313
_shelx_estimated_absorpt_t_min   0.891
_shelx_estimated_absorpt_t_max   0.987
_shelxl_version_number           2014-3
_shelx_res_checksum              252
_shelx_hkl_checksum              95958