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_1566159
_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, C40 H64 B N4 O, C H Cl3'
_chemical_formula_sum            'C41 H65 Al B Br4 Cl3 N4 O'
_chemical_formula_weight         1093.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 106.7667(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.64878(13)
_cell_length_b                   21.8402(2)
_cell_length_c                   19.4954(2)
_cell_measurement_reflns_used    27821
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.2170
_cell_measurement_theta_min      3.0540
_cell_volume                     5156.68(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     80.00 105.00   0.50    0.28    --  106.49 -99.00  30.00   50
  2  \w     35.00  66.00   0.50    0.28    --  106.49 -57.00  58.00   62
  3  \w     46.00  72.00   0.50    0.28    --  106.49 -99.00  30.00   52
  4  \w     41.00 105.00   0.50    0.28    --  106.49 -77.00 -30.00  128
  5  \w     49.00 106.00   0.50    0.28    --  106.49 -99.00-120.00  114
  6  \w     34.00  59.00   0.50    0.28    --  106.49 -57.00 -90.00   50
  7  \w     36.00  63.00   0.50    0.28    --  106.49 -57.00  30.00   54
  8  \w     34.00  65.00   0.50    0.28    --  106.49 -57.00  90.00   62
  9  \w     34.00  60.00   0.50    0.28    --  106.49 -57.00 120.00   52
 10  \w    -14.00  60.00   0.50    0.07    --   48.45 -57.00  58.00  148
 11  \w     98.00 124.00   0.50    0.28    --  106.49  57.00 120.00   52
 12  \w    151.00 176.00   0.50    0.28    --  106.49  57.00 120.00   50
 13  \w     95.00 156.00   0.50    0.28    --  106.49 125.00  60.00  122
 14  \w    104.00 139.00   0.50    0.28    --  106.49  77.00 -60.00   70
 15  \w    144.00 175.00   0.50    0.28    --  106.49  77.00 -60.00   62
 16  \w    131.00 157.00   0.50    0.28    --  106.49 125.00 -90.00   52
 17  \w    153.00 178.00   0.50    0.28    --  106.49 125.00-150.00   50
 18  \w     97.00 125.00   0.50    0.28    --  106.49 125.00-150.00   56
 19  \w     97.00 126.00   0.50    0.28    --  106.49 125.00 -90.00   58
 20  \w     93.00 176.00   0.50    0.28    --  106.49  57.00-160.00  166
 21  \w     77.00 118.00   0.50    0.07    --   48.45  57.00-160.00   82
 22  \w    -29.00  -3.00   0.50    0.07    --  -48.45  77.00-150.00   52
 23  \w    -63.00  24.00   0.50    0.07    --  -48.45  57.00-160.00  174
 24  \w    -64.00 -39.00   0.50    0.28    --  -86.25  57.00-160.00   50
 25  \w    -41.00 -13.00   0.50    0.28    --  -86.25  38.00   0.00   56
 26  \w    -41.00 -13.00   0.50    0.28    --  -86.25  38.00  30.00   56
 27  \w   -119.00 -37.00   0.50    0.07    --  -48.45 -57.00  58.00  164
 28  \w   -118.00 -93.00   0.50    0.07    --  -48.45-125.00 -90.00   50
 29  \w   -117.00 -85.00   0.50    0.07    --  -48.45-125.00-150.00   64
 30  \w   -150.00 -73.00   0.50    0.28    --  -86.25 -57.00  30.00  154
 31  \w   -139.00-114.00   0.50    0.28    --  -86.25 -57.00  58.00   50
;
_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      0.0102162000
_diffrn_orient_matrix_UB_12      -0.0304508000
_diffrn_orient_matrix_UB_13      -0.0690873000
_diffrn_orient_matrix_UB_21      0.1054089000
_diffrn_orient_matrix_UB_22      0.0374471000
_diffrn_orient_matrix_UB_23      0.0054299000
_diffrn_orient_matrix_UB_31      0.0704524000
_diffrn_orient_matrix_UB_32      -0.0514513000
_diffrn_orient_matrix_UB_33      0.0447813000
_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  0.0650
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41048
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         3.114
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55944
_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    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.403
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00017(4)
_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   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         9185
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0796P)^2^+12.1450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8034
_reflns_number_total             9185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00002d2.cif
_cod_data_source_block           klb-119
_cod_depositor_comments
'Adding full bibliography for 1566151--1566160.cif.'
_cod_original_cell_volume        5156.69(10)
_cod_database_code               1566159
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CBN
_shelx_estimated_absorpt_t_max   0.602
_shelx_estimated_absorpt_t_min   0.398
_reflns_odcompleteness_completeness 99.81
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H25C-C25
 1.52 with sigma of 0.02
 Br4B-Al1 \\sim Br4A-Al1
 with sigma of 0.02
3. Rigid bond restraints
 Cl1A, Cl2A, Cl3A, Cl1B, Cl2B, Cl3B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Br4A \\sim Br4B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C16B \\sim C17B \\sim C18B \\sim C16A \\sim C17A \\sim C18A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Cl1A \\sim Cl2A \\sim Cl3A \\sim Cl1B \\sim Cl2B \\sim Cl3B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(Br4A) \\sim Ueq, Uanis(Br4B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C16A) \\sim Ueq, Uanis(C16B) \\sim Ueq, Uanis(C18B) \\sim Ueq,
Uanis(C18A) \\sim Ueq, Uanis(C17B) \\sim Ueq, Uanis(C17A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl1B) \\sim Ueq, Uanis(Cl2A) \\sim Ueq, Uanis(Cl2B) \\sim Ueq,
Uanis(Cl3A) \\sim Ueq, Uanis(Cl3B) \\sim Ueq, Uanis(Cl1A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 Cl1A, Cl2A, Cl3A, Cl1B, Cl2B, Cl3B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(Br4B)=Sof(H41A)=Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=1-FVAR(1)
 Sof(Br4A)=Sof(H41)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=FVAR(1)
 Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(2)
 Sof(C16B)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17B)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C24(H24), C27(H27), C34(H34), C41(H41A), C41(H41)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
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), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C16B(H16A,H16B,H16C), C17B(H17A,H17B,H17C), C18B(H18A,H18B,H18C), C16A(H16D,
 H16E,H16F), C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F)
;
_shelx_res_checksum              49730
_shelx_hkl_checksum              45324
_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 1.538
_oxdiff_exptl_absorpt_empirical_full_min 0.715