Unraveling the reactivity of a cationic iminoborane: avenues to unusual boron cations
Guo, Rui; Zhang, Xin; Li, Tong; Li, Qianli; Ruiz, David A.; Liu, Liu Leo; Tung, Chen-Ho; Kong, Lingbing; Chemical Science 13 (2022) 2303–2309; doi:10.1039/D2SC00002D

data_1566157
_publ_section_title
;
 Unraveling the reactivity of a cationic iminoborane: avenues to unusual
 boron cations
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2303
_journal_page_last               2309
_journal_paper_doi               10.1039/D2SC00002D
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'Al Br4, C33 H59 B N5 Si'
_chemical_formula_sum            'C33 H59 Al B Br4 N5 Si'
_chemical_formula_weight         911.37
_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
_audit_creation_date             2021-09-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-11 deposited with the CCDC.	2022-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                109.980(4)
_cell_angle_beta                 104.192(3)
_cell_angle_gamma                102.755(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9613(4)
_cell_length_b                   13.4134(6)
_cell_length_c                   15.2453(6)
_cell_measurement_reflns_used    9154
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.9790
_cell_measurement_theta_min      3.2770
_cell_volume                     2100.41(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     35.00 120.00   1.00    0.10    --   48.45  56.00 159.00   85
  2  \w    -23.00  53.00   1.00    0.10    --   48.45 -56.00  16.00   76
  3  \w    -19.00  19.00   1.00    0.10    --  -48.45  56.00 159.00   38
  4  \w    -27.00  27.00   1.00    0.10    --  -48.45  19.00 150.00   54
  5  \w    -61.00 -33.00   1.00    0.10    --  -48.45  56.00 159.00   28
  6  \w   -119.00 -81.00   1.00    0.10    --  -48.45 -56.00  16.00   38
  7  \w    -80.00 -34.00   1.00    0.10    --  -48.45 -56.00  16.00   46
  8  \w    -59.00 -15.00   1.00    0.14    --  -86.25  56.00 159.00   44
  9  \w    -43.00 -13.00   1.00    0.14    --  -86.25  38.00 120.00   30
 10  \w    -43.00 -15.00   1.00    0.14    --  -86.25  38.00   0.00   28
 11  \w    -62.00 -14.00   1.00    0.14    --  -86.25  57.00 -60.00   48
 12  \w   -156.00 -72.00   1.00    0.14    --  -86.25 -56.00  16.00   84
 13  \w     92.00 176.00   1.00    0.14    --  106.49  57.00-120.00   84
 14  \w     92.00 175.00   1.00    0.14    --  106.49  57.00-180.00   83
 15  \w     93.00 155.00   1.00    0.14    --  106.49  56.00 159.00   62
 16  \w     95.00 174.00   1.00    0.14    --  106.49 125.00  60.00   79
 17  \w     95.00 126.00   1.00    0.14    --  106.49 125.00   0.00   31
 18  \w    129.00 178.00   1.00    0.14    --  106.49 125.00   0.00   49
 19  \w     39.00  65.00   1.00    0.14    --  106.49 -57.00-180.00   26
 20  \w     34.00 111.00   1.00    0.14    --  106.49-125.00   0.00   77
 21  \w     34.00 110.00   1.00    0.14    --  106.49-125.00  30.00   76
 22  \w     39.00 105.00   1.00    0.14    --  106.49 -99.00  30.00   66
 23  \w     37.00  64.00   1.00    0.14    --  106.49 -56.00  16.00   27
 24  \w     34.00 106.00   1.00    0.14    --  106.49 -99.00  90.00   72
 25  \w     35.00 106.00   1.00    0.14    --  106.49 -99.00 150.00   71
 26  \w     35.00 106.00   1.00    0.14    --  106.49 -99.00-150.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0278533000
_diffrn_orient_matrix_UB_12      0.1073951000
_diffrn_orient_matrix_UB_13      0.0020531000
_diffrn_orient_matrix_UB_21      0.1292729000
_diffrn_orient_matrix_UB_22      0.0724573000
_diffrn_orient_matrix_UB_23      0.0765071000
_diffrn_orient_matrix_UB_31      0.0488055000
_diffrn_orient_matrix_UB_32      -0.0054482000
_diffrn_orient_matrix_UB_33      -0.0855298000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20493
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.293
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.361
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7354
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+0.0586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6066
_reflns_number_total             7354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00002d2.cif
_cod_data_source_block           klb-113
_cod_depositor_comments
'Adding full bibliography for 1566151--1566160.cif.'
_cod_original_cell_volume        2100.41(16)
_cod_database_code               1566157
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CBN
_shelx_estimated_absorpt_t_max   0.296
_shelx_estimated_absorpt_t_min   0.296
_reflns_odcompleteness_completeness 98.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1-C33B \\sim Si1-C33A
 with sigma of 0.02
3. Rigid bond restraints
 C33A, C33B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C33B \\sim C33A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C33A) \\sim Ueq, Uanis(C33B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Others
 Sof(C33B)=Sof(H33A)=Sof(H33B)=Sof(H33C)=1-FVAR(1)
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C27(H27), C24(H24)
6.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C5(H5), C3(H3)
6.c Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C),
 C18(H18A,H18B,H18C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33B(H33A,H33B,H33C),
 C33A(H33D,H33E,H33F)
;
_shelx_res_checksum              45626
_shelx_hkl_checksum              68435
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.517
_oxdiff_exptl_absorpt_empirical_full_min 0.711