Selective one- and two-electron reductions of a haloborane enabled by a π-withdrawing carbene ligand.
Roy, Dipak Kumar; Krummenacher, Ivo; Stennett, Tom E.; Lenczyk, Carsten; Thiess, Torsten; Welz, Eileen; Engels, Bernd; Braunschweig, Holger; Chemical communications (Cambridge, England) 54 (2018) 9015–9018; doi:10.1039/c8cc03433h

data_7121924
_publ_section_title
;
 Selective one- and two-electron reductions of a haloborane enabled by a
 \p-withdrawing carbene ligand.
;
_journal_issue                   65
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9015
_journal_page_last               9018
_journal_paper_doi               10.1039/c8cc03433h
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C30 H28 B Br2 Cl0 F5 N2 O2'
_chemical_formula_sum            'C30 H28 B Br2 Cl0 F5 N2 O2'
_chemical_formula_weight         714.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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;
2018-04-24 deposited with the CCDC.
2018-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   15.351(7)
_cell_length_c                   22.229(11)
_cell_measurement_reflns_used    2471
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      21.92
_cell_measurement_theta_min      2.57
_cell_volume                     2898(3)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
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_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0929
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17218
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
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_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.262
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_exptl_absorpt_coefficient_mu    2.862
_exptl_absorpt_correction_T_max  0.5950
_exptl_absorpt_correction_T_min  0.4692
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.444
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 1747 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.765
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4666
_reflns_number_total             5708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03433h2.cif
_cod_data_source_block           ToTh069_a
_cod_depositor_comments
'Adding full bibliography for 7121923--7121927.cif.'
_cod_database_code               7121924
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.363
_shelx_estimated_absorpt_t_max   0.673
_shelx_res_checksum              78623