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_7716433
_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         '2(C15 H39 B21 N2), C7 H8'
_chemical_formula_sum            'C37 H86 B42 N4'
_chemical_formula_weight         1041.11
_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             2023-02-02
_audit_creation_method           'CIF-fill 1.3q (K.Radacki, 2005-22)'
_audit_update_record
;
2024-06-02 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                67.709(3)
_cell_angle_beta                 86.457(3)
_cell_angle_gamma                76.241(3)
_cell_formula_units_Z            1
_cell_length_a                   10.4445(3)
_cell_length_b                   11.4808(4)
_cell_length_c                   14.0816(5)
_cell_measurement_reflns_used    10984
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.9120
_cell_measurement_theta_min      3.3920
_cell_volume                     1516.76(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w    -86.00 -51.00   0.50    1.50    --  -38.00 -51.00 -30.51   70
  2  \w    -98.00 -63.00   0.50    1.50    --  -50.00 -51.00  69.15   70
  3  \w    -99.00 -64.00   0.50    1.50    --  -50.00 -47.00 178.46   70
  4  \w   -102.00 -67.00   0.50    1.50    --  -54.00 -52.00 -50.06   70
  5  \w   -120.00 -82.00   0.50    1.50    --  -70.00 -42.00-121.31   76
  6  \w   -121.00 -86.00   0.50    1.50    --  -74.00 -58.00  39.79   70
  7  \w   -124.00 -86.00   0.50    1.50    --  -74.00 -42.00 -76.39   76
  8  \w    -92.00 -31.00   0.50    1.50    --  -76.35 112.00 120.00  122
  9  \w    -98.00 -32.00   0.50    1.50    --  -78.00 118.00-143.13  132
 10  \w   -107.00 -33.00   0.50    1.50    --  -79.50 138.00-139.62  148
 11  \w    -97.00 -33.00   0.50    1.50    --  -79.50 117.00 -28.90  128
 12  \w   -127.00 -92.00   0.50    1.50    --  -79.50 -54.00 126.44   70
 13  \w    -97.00 -33.00   0.50    1.50    --  -79.50 115.00  19.22  128
 14  \w   -125.00 -91.00   0.50    1.50    --  -79.50 -60.00 178.76   68
 15  \w   -125.00 -96.00   0.50    1.50    --  -79.50-115.00-115.73   58
 16  \w   -126.00 -92.00   0.50    1.50    --  -79.50-123.00  91.90   68
 17  \w   -126.00 -92.00   0.50    1.50    --  -79.50 -57.00-138.97   68
 18  \w   -125.00 -91.00   0.50    1.50    --  -79.50 -61.00  47.11   68
 19  \w   -127.00 -92.00   0.50    1.50    --  -79.50 -53.00 -33.69   70
 20  \w   -127.00 -90.00   0.50    1.50    --  -79.50-126.00 138.04   74
 21  \w   -125.00 -91.00   0.50    1.50    --  -79.50 -60.00-122.64   68
 22  \w   -130.00 -90.00   0.50    1.50    --  -79.50 -38.00  72.95   80
 23  \w    -92.00 -34.00   0.50    1.50    --  -79.50 104.00 -25.90  116
 24  \w     40.00  90.00   0.50    1.50    --   82.28 -95.00 -30.00  100
 25  \w     40.00  90.00   0.50    1.50    --   82.28 -95.00-150.00  100
 26  \w     46.00 133.00   0.50    1.50    --   82.28  15.00  30.00  174
 27  \w     40.00  90.00   0.50    1.50    --   82.28 -95.00 150.00  100
 28  \w     40.00  90.00   0.50    1.50    --   82.28 -95.00  90.00  100
 29  \w     40.00  90.00   0.50    1.50    --   82.28 -95.00   0.00  100
 30  \w     40.00  90.00   0.50    1.50    --   82.28 -95.00 120.00  100
 31  \w     46.00 133.00   0.50    1.50    --   82.28  15.00-180.00  174
 32  \w     37.00  93.00   0.50    1.50    --   82.28-112.00-120.00  112
 33  \w     40.00  90.00   0.50    1.50    --   82.28 -95.00  60.00  100
 34  \w     37.00  93.00   0.50    1.50    --   82.28-112.00 120.00  112
 35  \w     40.00  90.00   0.50    1.50    --   82.28 -95.00-120.00  100
 36  \w     40.00  90.00   0.50    1.50    --   82.28 -95.00 -90.00  100
 37  \w     46.00 133.00   0.50    1.50    --   82.28  15.00 150.00  174
 38  \w     40.00  90.00   0.50    1.50    --   82.28 -95.00  30.00  100
 39  \w     46.00 133.00   0.50    1.50    --   82.28  15.00-120.00  174
 40  \w     40.00  90.00   0.50    1.50    --   82.28 -95.00 -60.00  100
 41  \w    103.00 131.00   0.50    1.50    --   85.25 114.00-156.99   56
 42  \w     40.00  93.00   0.50    1.50    --   85.25-105.00-163.14  106
 43  \w    -54.00 -26.00   0.50    1.50    --  -14.00 -57.00  68.83   56
 44  \w    -42.00 -14.00   0.50    1.50    --  -14.00 126.00 128.29   56
 45  \w    -95.00 -60.00   0.50    1.50    --  -46.00 -48.00-105.93   70
 46  \w    -94.00 -59.00   0.50    1.50    --  -46.00 -51.00  27.04   70
 47  \w   -125.00 -90.00   0.50    1.50    --  -78.00 -55.00   7.90   70
 48  \w   -127.00 -89.00   0.50    1.50    --  -79.50-129.00-169.60   76
 49  \w   -126.00 -92.00   0.50    1.50    --  -79.50-123.00  58.61   68
 50  \w   -125.00 -97.00   0.50    1.50    --  -79.50-113.00 -24.63   56
 51  \w   -126.00 -93.00   0.50    1.50    --  -79.50-120.00  28.32   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      0.1479262000
_diffrn_orient_matrix_UB_12      -0.0593323000
_diffrn_orient_matrix_UB_13      -0.0042181000
_diffrn_orient_matrix_UB_21      -0.0217288000
_diffrn_orient_matrix_UB_22      -0.1350711000
_diffrn_orient_matrix_UB_23      0.0665722000
_diffrn_orient_matrix_UB_31      -0.0270100000
_diffrn_orient_matrix_UB_32      -0.0215757000
_diffrn_orient_matrix_UB_33      -0.0976976000
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29929
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.860
_diffrn_reflns_theta_min         3.394
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022) Numerical 
 absorption correction based on gaussian integration over a multifaceted 
 crystal model Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       block
_exptl_crystal_F_000             546
_exptl_crystal_preparation
;
 Crystals were grown from saturated solution. 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          0.142
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0768
_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^)+(0.1782P)^2^+0.2248P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2164
_refine_ls_wR_factor_ref         0.2324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4804
_reflns_number_total             5998
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01615g2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7716430--7716433.cif.'
_cod_original_cell_volume        1516.77(9)
_cod_database_code               7716433
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              13616