Reactivity study of Lewis superacidic carborane-based analogue of 9-bromo-9-borafluorene towards Lewis bases.
Xiang, Libo; Matler, Alexander; Tan, Leibo; Ye, Qing; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11655–11658; doi:10.1039/d4dt01615g

data_7716432
_publ_section_title
;
 Reactivity study of Lewis superacidic carborane-based analogue of
 9-bromo-9-borafluorene towards Lewis bases.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11655
_journal_page_last               11658
_journal_paper_doi               10.1039/d4dt01615g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C14 H31 B21 Br N'
_chemical_formula_sum            'C14 H31 B21 Br N'
_chemical_formula_weight         520.32
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-08-04
_audit_creation_method           'CIF-fill 1.4m (K.Radacki, 2005-23)'
_audit_update_record
;
2024-06-02 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                76.466(9)
_cell_angle_beta                 85.047(10)
_cell_angle_gamma                89.247(9)
_cell_formula_units_Z            2
_cell_length_a                   7.326(2)
_cell_length_b                   12.897(4)
_cell_length_c                   14.448(4)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.79
_cell_volume                     1322.2(7)
_computing_cell_refinement       'Saint+ ver. 8.40B (Bruker AXS)'
_computing_data_collection       'BIS 6.2.14 / APEX4 ver. 2021.10 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 8.40B (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)''
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPA
_diffrn_detector_area_resol_mean 7.5
_diffrn_detector_type            'Photon II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
;
 Sparks R.A., Computational Crystallography p1-18 (Clarendon Press, 1982)
;
_diffrn_orient_matrix_UB_11      0,0100925
_diffrn_orient_matrix_UB_12      -0,0656519
_diffrn_orient_matrix_UB_13      -0,0256349
_diffrn_orient_matrix_UB_21      -0,1211674
_diffrn_orient_matrix_UB_22      0,0159609
_diffrn_orient_matrix_UB_23      -0,0270033
_diffrn_orient_matrix_UB_31      0,0631596
_diffrn_orient_matrix_UB_32      0,0423734
_diffrn_orient_matrix_UB_33      -0,0609853
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39789
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         1.911
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.564
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       plate
_exptl_crystal_F_000             524
_exptl_crystal_preparation
;
 For data collection the crystal was immersed in a film of perfluoropolyether 
 oil, mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 800).
;
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.191
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0341P)^2^+0.6842P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5320
_reflns_number_total             5841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01615g2.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 7716430--7716433.cif.'
_cod_database_code               7716432
_shelx_shelxl_version_number     2019/1
_exptl_absorpt_special_details
;
 Incident beam scaling, empirical absorption correction using spherical 
 harmonics, and outlier rejection was employed as implemented in SADABS. 
 Additional spherical absorption correction with mu*r value set to 0.2 was 
 applied.
;
_shelx_estimated_absorpt_t_min   0.650
_shelx_estimated_absorpt_t_max   0.754
_shelx_res_checksum              39801