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_1566156
_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, C29 H49 B N3, 2(C6 H6)'
_chemical_formula_sum            'C41 H61 Al B Br4 N3'
_chemical_formula_weight         953.35
_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             2021-04-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-16 deposited with the CCDC.	2022-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                65.411(6)
_cell_angle_beta                 78.295(5)
_cell_angle_gamma                80.201(4)
_cell_formula_units_Z            2
_cell_length_a                   10.2658(5)
_cell_length_b                   15.8170(9)
_cell_length_c                   15.9702(11)
_cell_measurement_reflns_used    8581
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      75.3800
_cell_measurement_theta_min      3.0720
_cell_volume                     2298.2(3)
_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_environment      N~2~
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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     74.00 106.00   1.00    3.30    --  106.49 -99.00  90.00   32
  2  \w     36.00  65.00   1.00    3.30    --  106.49 -99.00 -30.00   29
  3  \w     72.00 106.00   1.00    3.30    --  106.49 -99.00 -30.00   34
  4  \w     67.00 132.00   1.00    3.30    --  106.49 -84.00-109.00   65
  5  \w     72.00 103.00   1.00    3.30    --  106.49 -99.00-120.00   31
  6  \w     34.00  69.00   1.00    3.30    --  106.49 -99.00-120.00   35
  7  \w     38.00 111.00   1.00    3.30    --  106.49-125.00-120.00   73
  8  \w     35.00  64.00   1.00    3.30    --  106.49 -57.00  30.00   29
  9  \w     35.00  70.00   1.00    3.30    --  106.49 -99.00  90.00   35
 10  \w     34.00  66.00   1.00    3.30    --  106.49 -57.00  90.00   32
 11  \w     36.00  77.00   1.00    3.30    --  106.49   0.00 120.00   41
 12  \w     93.00 177.00   1.00    3.30    --  106.49   0.00 120.00   84
 13  \w    101.00 157.00   1.00    3.30    --  106.49  84.00  10.00   56
 14  \w    139.00 178.00   1.00    3.30    --  106.49  19.00 -30.00   39
 15  \w    125.00 178.00   1.00    3.30    --  106.49 125.00-150.00   53
 16  \w    129.00 178.00   1.00    3.30    --  106.49 125.00 -90.00   49
 17  \w     95.00 121.00   1.00    3.30    --  106.49 125.00-150.00   26
 18  \w     95.00 121.00   1.00    3.30    --  106.49 125.00 -90.00   26
 19  \w     94.00 124.00   1.00    3.30    --  106.49  19.00 -30.00   30
 20  \w     95.00 166.00   1.00    3.30    --  106.49  19.00-180.00   71
 21  \w     36.00  66.00   1.00    3.30    --  106.49 -57.00 -60.00   30
 22  \w     39.00  66.00   1.00    3.30    --  106.49 -57.00-120.00   27
 23  \w     35.00  64.00   1.00    3.30    --  106.49 -84.00-109.00   29
 24  \w     34.00 104.00   1.00    3.30    --  106.49 -99.00  30.00   70
 25  \w    -21.00  40.00   1.00    0.50    --   48.32 -84.00-109.00   61
 26  \w    -24.00  27.00   1.00    0.50    --   48.32 -19.00 -30.00   51
 27  \w    -74.00  24.00   1.00    0.50    --  -48.32  84.00  10.00   98
 28  \w    -62.00  24.00   1.00    0.50    --  -48.32  57.00 150.00   86
 29  \w    -83.00 -39.00   1.00    3.30    --  -86.25  84.00  10.00   44
 30  \w    -43.00 -13.00   1.00    3.30    --  -86.25  38.00 -60.00   30
 31  \w   -114.00 -88.00   1.00    3.30    --  -86.25 -84.00-109.00   26
 32  \w   -120.00 -73.00   1.00    0.50    --  -48.32-125.00 -30.00   47
 33  \w   -150.00-122.00   1.00    3.30    --  -86.25 -84.00-109.00   28
;
_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      0.0777351000
_diffrn_orient_matrix_UB_12      0.0855813000
_diffrn_orient_matrix_UB_13      -0.0610468000
_diffrn_orient_matrix_UB_21      -0.0521637000
_diffrn_orient_matrix_UB_22      0.0428641000
_diffrn_orient_matrix_UB_23      0.0726923000
_diffrn_orient_matrix_UB_31      0.1222416000
_diffrn_orient_matrix_UB_32      -0.0491858000
_diffrn_orient_matrix_UB_33      0.0499308000
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21862
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         3.077
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66522
_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    1.378
_exptl_crystal_description       needle
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         8060
_refine_ls_number_restraints     406
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0421P)^2^+5.1920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6907
_reflns_number_total             8060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00002d2.cif
_cod_data_source_block           klb-95
_cod_depositor_comments
'Adding full bibliography for 1566151--1566160.cif.'
_cod_database_code               1566156
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CNB
_shelx_estimated_absorpt_t_max   0.652
_shelx_estimated_absorpt_t_min   0.256
_reflns_odcompleteness_completeness 98.14
_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
 C47B-C46B = C47B-C42B = C43B-C42B = C44B-C43B = C45B-C44B = C46B-C45B
 1.38 with sigma of 0.02
 C33-C34 \\sim C34-C35 \\sim C35-C30 \\sim C30-C31 \\sim C31-C32 \\sim C32-C33
 with sigma of 0.02
 C33-C31 \\sim C33-C31 \\sim C30-C34 \\sim C30-C32 \\sim C32-C34 \\sim C31-C35
 with sigma of 0.04
 C46A-C47A \\sim C47A-C42A \\sim C42A-C43A \\sim C43A-C44A \\sim C44A-C45A
\\sim C45A-C46A
 with sigma of 0.02
 C46A-C44A \\sim C46A-C44A \\sim C43A-C47A \\sim C43A-C45A \\sim C45A-C47A
\\sim C44A-C42A
 with sigma of 0.04
 C41-C36 \\sim C36-C37 \\sim C37-C38 \\sim C38-C39 \\sim C39-C40 \\sim C40-C41
 with sigma of 0.02
 C41-C39 \\sim C41-C39 \\sim C38-C36 \\sim C38-C40 \\sim C40-C36 \\sim C39-C37
 with sigma of 0.04
 C44B-C43B \\sim C43B-C42B \\sim C42B-C47B \\sim C47B-C46B \\sim C46B-C45B
\\sim C45B-C44B
 with sigma of 0.02
 C44B-C46B \\sim C44B-C46B \\sim C47B-C43B \\sim C47B-C45B \\sim C45B-C43B
\\sim C46B-C42B
 with sigma of 0.04
3. Restrained planarity
 C30, C31, C32, C33, C34, C35
 with sigma of 0.1
 C42A, C43A, C44A, C45A, C46A, C47A
 with sigma of 0.1
 C36, C37, C38, C39, C40, C41
 with sigma of 0.1
 C42B, C43B, C44B, C45B, C46B, C47B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C42A \\sim C43A \\sim C44A \\sim C45A \\sim C46A \\sim C47A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C42B \\sim C43B \\sim C44B \\sim C45B \\sim C46B \\sim C47B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 C30, C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42A, C43A, C44A, C45A, C46A, C47A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C36, C37, C38, C39, C40, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42B, C43B, C44B, C45B, C46B, C47B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C42B(0.5) H42B(0.5) C43B(0.5) H43B(0.5) C44B(0.5) H44B(0.5)
 C45B(0.5) H45B(0.5) C46B(0.5) H46B(0.5) C47B(0.5) H47B(0.5) C30(0.5) H30(0.5)
 C31(0.5) H31(0.5) C32(0.5) H32(0.5) C33(0.5) H33(0.5) C34(0.5) H34(0.5)
 C35(0.5) H35(0.5) C36(0.5) H36(0.5) C37(0.5) H37(0.5) C38(0.5) H38(0.5)
 C39(0.5) H39(0.5) C40(0.5) H40(0.5) C41(0.5) H41(0.5) C42A(0.5) H42A(0.5)
 C43A(0.5) H43A(0.5) C44A(0.5) H44A(0.5) C45A(0.5) H45A(0.5) C46A(0.5)
 H46A(0.5) C47A(0.5) H47A(0.5)
7.a Ternary CH refined with riding coordinates:
 C22(H22), C25(H25)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C42B(H42B), C43B(H43B), C44B(H44B), C45B(H45B), C46B(H46B),
 C47B(H47B), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42A(H42A),
 C43A(H43A), C44A(H44A), C45A(H45A), C46A(H46A), C47A(H47A)
7.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              39876
_shelx_hkl_checksum              74980
_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 1.705
_oxdiff_exptl_absorpt_empirical_full_min 0.598