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_7125221
_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 H10 B11 F2 I2, C4 H12 N'
_chemical_formula_sum            'C6 H22 B11 F2 I2 N'
_chemical_formula_weight         518.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_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                60.7590(10)
_cell_angle_beta                 72.300(2)
_cell_angle_gamma                86.331(2)
_cell_formula_units_Z            4
_cell_length_a                   12.4538(7)
_cell_length_b                   13.5015(8)
_cell_length_c                   13.5440(8)
_cell_measurement_reflns_used    9280
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.761
_cell_measurement_theta_min      2.197
_cell_volume                     1883.28(19)
_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_detector                 'CCD area detector (Apex2)'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.988
_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  0.0202
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19760
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.779
_diffrn_reflns_theta_min         1.725
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_exptl_absorpt_coefficient_mu    3.343
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+1.8320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0528
_refine_ls_wR_factor_ref         0.0555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7021
_reflns_number_total             7950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07711k2.cif
_cod_data_source_block           Me4NBHF2oC2B10I2H9
_cod_database_code               7125221
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              35760