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_4346310
_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            'C60 H51 B3 N12'
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_space_group_name_H-M_alt        'P 21 21 21'
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_cell_angle_gamma                90
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_cell_length_b                   19.3899(17)
_cell_length_c                   22.940(2)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.82
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_computing_cell_refinement       'Bruker SAINT'
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_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.675
_diffrn_measured_fraction_theta_max 0.973
_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  0.1189
_diffrn_reflns_av_unetI/netI     0.1092
_diffrn_reflns_Laue_measured_fraction_full 0.675
_diffrn_reflns_Laue_measured_fraction_max 0.973
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_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_point_group_measured_fraction_full 0.667
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_diffrn_reflns_theta_max         54.597
_diffrn_reflns_theta_min         2.984
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.7507
_exptl_absorpt_correction_T_min  0.6141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       plate
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.340
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_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_restraints     736
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+11.9205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.776
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_reflns_Friedel_fraction_max     0.974
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01287_si_002.cif
_cod_data_source_block           cu_molan236_0m
_cod_original_cell_volume        4913.1(8)
_cod_database_code               4346310
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2014-3
_shelx_res_checksum              37306
_shelx_hkl_checksum              6143