Synthesis of the fluorohydridoborate anions [BHF<sub>3</sub>]<sup>-</sup> and [1-HF<sub>2</sub>B-9,12-X<sub>2</sub>-closo-1,2-C<sub>2</sub>B<sub>10</sub>H<sub>9</sub>]<sup>-</sup> (X = H, I): deboronation of 1,2- and 1,7-dicarba-closo-dodecaboranes with anhydrous [Me<sub>4</sub>N]F.
Duda, Katharina; Himmelspach, Alexander; Landmann, Johannes; Kraus, Florian; Finze, Maik; Chemical communications (Cambridge, England) 52 (2016) 13241–13244; doi:10.1039/c6cc07711k

data_7125220
_publ_section_title
;
 Synthesis of the fluorohydridoborate anions [BHF<sub>3</sub>]<sup>-</sup>
 and
 [1-HF<sub>2</sub>B-9,12-X<sub>2</sub>-closo-1,2-C<sub>2</sub>B<sub>10</sub>H<sub>9</sub>]<sup>-</sup>
 (X = H, I): deboronation of 1,2- and 1,7-dicarba-closo-dodecaboranes with
 anhydrous [Me<sub>4</sub>N]F.
;
_journal_issue                   90
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13241
_journal_page_last               13244
_journal_paper_doi               10.1039/c6cc07711k
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C2 H12 B11 F2, C4 H12 N'
_chemical_formula_sum            'C6 H24 B11 F2 N'
_chemical_formula_weight         267.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-09-21 deposited with the CCDC.
2016-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.102(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.452(3)
_cell_length_b                   13.828(3)
_cell_length_c                   10.773(2)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.8165
_cell_measurement_theta_min      2.401
_cell_volume                     1557.0(6)
_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)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            36594
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.811
_diffrn_reflns_theta_min         1.473
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         6631
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+2.2027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1949
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.918
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                6554
_reflns_number_total             6631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07711k2.cif
_cod_data_source_block           Me4NBHF2oC2B10H11
_cod_original_cell_volume        1557.1(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7125220
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              3426