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_7716431
_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         'C4 H20 B21 Br1.34, C15 H40 B21 N2'
_chemical_formula_sum            'C19 H60 B42 Br1.35 N2'
_chemical_formula_weight         878.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2024-06-02 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.692(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3887(13)
_cell_length_b                   12.963(2)
_cell_length_c                   29.552(3)
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.383
_cell_measurement_theta_min      2.275
_cell_volume                     4740.7(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            129764
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.448
_diffrn_reflns_theta_min         2.091
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1253 before and 0.0787 after correction.
The Ratio of minimum to maximum transmission is 0.8810.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         9751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+2.2939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7894
_reflns_number_total             9751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01615g2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7716430--7716433.cif.'
_cod_original_cell_volume        4740.5(10)
_cod_database_code               7716431
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.798
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00B(H00B), C00F(H00F)
2.b Idealised Me refined as rotating group:
 C00E(H00A,H00C,H00D), C00J(H00E,H00G,H00H), C00K(H00I,H00J,H00K), C00L(H00L,
 H00M,H00N), C00M(H00O,H00P,H00Q), C00N(H00R,H00S,H00T)
2.c Boron cage BH refined with riding coordinates:
 B00O(H00U), B00P(H00V), B00Q(H00W), B00R(H1AA), B00S(H00X), B00T(H2AA),
 B00U(H00Y), B00V(H00Z), B00W(H3AA), B00X(H00), B00Y(H4AA), B00Z(H0AA),
 B01A(H01A), B01B(H01B), B01C(H01C), B01D(H01D), B01E(H01E), B01F(H01F),
 B01G(H01G), B01H(H01H), B01I(H01I), B01J(H01J), B01K(H01K), B01L(H01L),
 B01M(H01M), B01N(H01N), B01O(H01O), B01P(H01P), B01Q(H01Q), B01R(H01R),
 B01S(H01S), B01T(H01T), B010(H010), B011(H011), B012(H012), B014(H014),
 B015(H015), B016(H016), B017(H017), B019(H019)
;
_shelx_res_checksum              36846
_olex2_submission_special_instructions 'No special instructions were received'