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_1566158
_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, C31 H52 B N4'
_chemical_formula_sum            'C31 H52 Al B Br4 N4'
_chemical_formula_weight         838.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                90
_cell_angle_beta                 93.4263(16)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.78100(19)
_cell_length_b                   15.9628(3)
_cell_length_c                   41.3531(7)
_cell_measurement_reflns_used    10130
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      76.2710
_cell_measurement_theta_min      2.9640
_cell_volume                     7762.9(2)
_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 2018/2 (Sheldrick, 2018)'
_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 0.980
_diffrn_measured_fraction_theta_max 0.934
_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    -55.00 -11.00   1.00    0.13    --  -48.45 122.00 143.00   44
  2  \w    -27.00  27.00   1.00    0.13    --  -48.45  19.00   0.00   54
  3  \w    -27.00  27.00   1.00    0.13    --  -48.45  19.00  60.00   54
  4  \w   -105.00 -57.00   1.00    0.13    --  -48.45-150.00 -99.00   48
  5  \w     52.00 111.00   1.00    0.13    --   48.45-150.00 -99.00   59
  6  \w     39.00  64.00   1.00    0.13    --   48.45-122.00  62.00   25
  7  \w    -43.00 -13.00   1.00    0.63    --  -86.25  38.00   0.00   30
  8  \w   -141.00-116.00   1.00    0.63    --  -86.25-122.00  62.00   25
  9  \w   -104.00 -65.00   1.00    0.63    --  -86.25-150.00 -99.00   39
 10  \w     94.00 178.00   1.00    0.63    --  106.49  57.00 120.00   84
 11  \w     80.00 143.00   1.00    0.63    --  106.49 150.00 -54.00   63
 12  \w     94.00 178.00   1.00    0.63    --  106.49  19.00 -90.00   84
 13  \w     34.00  97.00   1.00    0.63    --  106.49 -77.00-150.00   63
 14  \w     34.00  66.00   1.00    0.63    --  106.49 -57.00  60.00   32
 15  \w     34.00 104.00   1.00    0.63    --  106.49 -99.00  90.00   70
 16  \w     40.00 109.00   1.00    0.63    --  106.49-122.00  62.00   69
 17  \w     55.00  82.00   1.00    0.63    --  106.49-150.00 -99.00   27
 18  \w     96.00 129.00   1.00    0.63    --  106.49-150.00 -99.00   33
;
_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      -0.0130395000
_diffrn_orient_matrix_UB_12      0.0220151000
_diffrn_orient_matrix_UB_13      0.0358689000
_diffrn_orient_matrix_UB_21      0.0099575000
_diffrn_orient_matrix_UB_22      -0.0934746000
_diffrn_orient_matrix_UB_23      0.0089754000
_diffrn_orient_matrix_UB_31      0.1299574000
_diffrn_orient_matrix_UB_32      0.0093754000
_diffrn_orient_matrix_UB_33      0.0051496000
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            23469
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.447
_diffrn_reflns_theta_min         2.968
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.459
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52578
_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    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.000037(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         7618
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0380P)^2^+16.5692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6769
_reflns_number_total             7618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00002d2.cif
_cod_data_source_block           klb-112
_cod_depositor_comments
'Adding full bibliography for 1566151--1566160.cif.'
_cod_database_code               1566158
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CBN
_shelx_estimated_absorpt_t_max   0.291
_shelx_estimated_absorpt_t_min   0.219
_reflns_odcompleteness_completeness 98.25
_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,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C31A \\sim N4A \\sim N4 \\sim C31: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(N4A) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C31A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(N4A)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(N4)=Sof(C31)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C25(H25), C22(H22)
4.b Secondary CH2 refined with riding coordinates:
 C30(H30C,H30D), C30(H30A,H30B)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C5(H5), C3(H3)
4.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C26(H26A,H26B,H26C), C29(H29A,H29B,
 H29C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C24(H24A,H24B,H24C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C8(H8A,H8B,H8C), C23(H23A,H23B,H23C),
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C)
;
_shelx_res_checksum              9736
_shelx_hkl_checksum              19314
_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 1.755
_oxdiff_exptl_absorpt_empirical_full_min 0.635