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_1566154
_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         '2(Al Br4), 2(C29 H49 B N3)'
_chemical_formula_sum            'C58 H98 Al2 B2 Br8 N6'
_chemical_formula_weight         1594.28
_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
_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                109.017(3)
_cell_angle_beta                 98.006(2)
_cell_angle_gamma                96.256(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5926(2)
_cell_length_b                   18.3489(5)
_cell_length_c                   22.4133(7)
_cell_measurement_reflns_used    11681
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      75.4680
_cell_measurement_theta_min      2.6750
_cell_volume                     3642.84(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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     38.00  76.00   1.00    0.36    --   48.45-129.00 -13.00   38
  2  \w     43.00 101.00   1.00    0.36    --   48.45-141.00 174.00   58
  3  \w    -27.00  27.00   1.00    0.36    --  -48.45  19.00 -30.00   54
  4  \w    -83.00 -22.00   1.00    0.36    --  -48.45 129.00  60.00   61
  5  \w    -91.00 -66.00   1.00    0.36    --  -48.45 141.00-127.00   25
  6  \w     26.00 121.00   1.00    0.36    --   48.45  77.00 150.00   95
  7  \w    -98.00 -71.00   1.00    0.36    --  -48.45-129.00 -13.00   27
  8  \w   -106.00 -64.00   1.00    0.36    --  -48.45-141.00 174.00   42
  9  \w    -76.00 -51.00   1.00    2.96    --  -86.25 129.00  60.00   25
 10  \w    -76.00 -21.00   1.00    2.96    --  -86.25 141.00-127.00   55
 11  \w   -159.00 -73.00   1.00    2.96    --  -86.25 -38.00-150.00   86
 12  \w   -139.00-114.00   1.00    2.96    --  -86.25-129.00 -13.00   25
 13  \w    -88.00 -63.00   1.00    2.96    --  -86.25-141.00 174.00   25
 14  \w   -142.00-117.00   1.00    2.96    --  -86.25-141.00 174.00   25
 15  \w    102.00 178.00   1.00    2.96    --  106.49  38.00 -30.00   76
 16  \w    113.00 178.00   1.00    2.96    --  106.49   0.00-120.00   65
 17  \w     95.00 178.00   1.00    2.96    --  106.49  38.00  30.00   83
 18  \w     93.00 160.00   1.00    2.96    --  106.49 129.00  60.00   67
 19  \w     84.00 171.00   1.00    2.96    --  106.49 141.00-127.00   87
 20  \w     95.00 178.00   1.00    2.96    --  106.49 125.00-150.00   83
 21  \w     45.00 100.00   1.00    2.96    --  106.49   0.00-120.00   55
 22  \w     35.00 105.00   1.00    2.96    --  106.49 -77.00-150.00   70
 23  \w     86.00 114.00   1.00    2.96    --  106.49-129.00 -13.00   28
 24  \w     34.00  66.00   1.00    2.96    --  106.49 -57.00 120.00   32
 25  \w     34.00 107.00   1.00    2.96    --  106.49-104.00   9.40   73
 26  \w     97.00 122.00   1.00    2.96    --  106.49-141.00 174.00   25
 27  \w     35.00  95.00   1.00    2.96    --  106.49 -77.00  30.00   60
 28  \w     34.00  66.00   1.00    2.96    --  106.49 -57.00-120.00   32
 29  \w     36.00 106.00   1.00    2.96    --  106.49 -99.00-150.00   70
 30  \w     38.00 107.00   1.00    2.96    --  106.49-109.00-154.07   69
;
_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      0.0307896000
_diffrn_orient_matrix_UB_12      0.0621879000
_diffrn_orient_matrix_UB_13      0.0678669000
_diffrn_orient_matrix_UB_21      0.0240065000
_diffrn_orient_matrix_UB_22      -0.0638244000
_diffrn_orient_matrix_UB_23      0.0292929000
_diffrn_orient_matrix_UB_31      0.1597265000
_diffrn_orient_matrix_UB_32      0.0128862000
_diffrn_orient_matrix_UB_33      -0.0033191000
_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  0.0703
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40257
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.070
_diffrn_reflns_theta_min         2.716
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.778
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.453
_exptl_crystal_description       plate
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.150
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         12851
_refine_ls_number_restraints     306
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0619
_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^)+(0.1053P)^2^+3.2147P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9524
_reflns_number_total             12851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00002d2.cif
_cod_data_source_block           klb-118
_cod_depositor_comments
'Adding full bibliography for 1566151--1566160.cif.'
_cod_original_cell_volume        3642.84(18)
_cod_database_code               1566154
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CBN
_shelx_estimated_absorpt_t_max   0.596
_shelx_estimated_absorpt_t_min   0.206
_reflns_odcompleteness_completeness 98.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Br6A-Al2 = Br6B-Al2
 2.28 with sigma of 0.02
 C41B-C40B = C43-C40B
 1.52 with sigma of 0.02
 C31-C40 = C31-C40B
 1.53 with sigma of 0.02
 C43-C40 = C41B-C40B
 1.53 with sigma of 0.02
 C43-C40 = C41B-C40B = C40B-C43B = C40-C41 = C40B-C42B = C40-C42
 1.53 with sigma of 0.02
 C42B-B2 = C42-B2
 1.56 with sigma of 0.02
 C43-C41
 2.48 with sigma of 0.02
 C43B-C42B
 2.49 with sigma of 0.02
 C41B-C42B
 2.49 with sigma of 0.02
 C41B-C43B
 2.48 with sigma of 0.02
 C43-C42
 2.49 with sigma of 0.02
 C30-C42
 2.92 with sigma of 0.02
 C45-C44 = C45B-C44 = C46-C44 = C46B-C44 = C47-C44 = C47B-C44
 1.53 with sigma of 0.02
 H39C-H4
 2 with sigma of 0.02
 H1-H9A
 2.2 with sigma of 0.02
 C42-C40B \\sim C42B-C40B
 with sigma of 0.02
 C42-B2 \\sim C42B-B2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C42 \\sim C42B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Br6B \\sim Br6A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C41B \\sim C43: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C42B \\sim C42 \\sim C43 \\sim C41B \\sim C40 \\sim C40B: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002 within 2A
C42B \\sim C42 \\sim C40 \\sim C40B \\sim C43B \\sim C43 \\sim C41B \\sim C41:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C45 \\sim C45B \\sim C44 \\sim C47B \\sim C47 \\sim C46B \\sim C46: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C42B) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Br6A) \\sim Ueq, Uanis(Br6B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C43) \\sim Ueq, Uanis(C41B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(C41B) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C40B) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C42B) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.002
Uanis(C41) \\sim Ueq, Uanis(C41B) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C43B)
\\sim Ueq, Uanis(C40B) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C42B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C47) \\sim Ueq, Uanis(C47B) \\sim Ueq, Uanis(C46B) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C45B) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C40B)=Sof(C41B)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C42B)=Sof(H42C)=
 Sof(H42D)=Sof(C43B)=Sof(H43D)=Sof(H43E)=Sof(H43F)=1-FVAR(1)
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C40)=
 Sof(C41)=Sof(H41D)=Sof(H41E)=Sof(H41F)=FVAR(1)
 Sof(Br6B)=1-FVAR(2)
 Sof(Br6A)=FVAR(2)
 Sof(C45B)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C47)=Sof(H47A)=Sof(H47B)=
 Sof(H47C)=Sof(C46B)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(3)
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47B)=Sof(H47D)=Sof(H47E)=
 Sof(H47F)=Sof(C45)=Sof(H45D)=Sof(H45E)=Sof(H45F)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C22(H22), C27(H27), C51(H51), C54(H54)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C42(H42A,H42B), C42B(H42C,H42D)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C5(H5), C3(H3), N4(H4), C32(H32), C34(H34)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C10(H10A,H10B,H10C), C9(H9A,H9B,
 H9C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C29(H29A,H29B,H29C), C28(H28A,
 H28B,H28C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C41B(H41A,H41B,H41C),
 C39(H39A,H39B,H39C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C43(H43A,H43B,H43C), C43B(H43D,H43E,H43F),
 C41(H41D,H41E,H41F), C46(H46A,H46B,H46C), C45B(H45A,H45B,H45C), C47(H47A,H47B,
 H47C), C47B(H47D,H47E,H47F), C45(H45D,H45E,H45F), C46B(H46D,H46E,H46F)
;
_shelx_res_checksum              89346
_shelx_hkl_checksum              39223
_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 2.744
_oxdiff_exptl_absorpt_empirical_full_min 0.390