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_1566153
_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         'C29 H49 Al B Br3 N6'
_chemical_formula_sum            'C29 H49 Al B Br3 N6'
_chemical_formula_weight         759.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.3035(4)
_cell_length_b                   18.6688(5)
_cell_length_c                   41.8373(8)
_cell_measurement_reflns_used    9105
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.8190
_cell_measurement_theta_min      3.5390
_cell_volume                     14296.0(6)
_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      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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    -43.00  25.00   1.00    1.30    --  -48.45  38.00  90.00   68
  2  \w    -25.00  27.00   1.00    1.30    --  -48.45  19.00  30.00   52
  3  \w    -89.00 -47.00   1.00    5.00    --  -86.25 132.00  93.00   42
  4  \w   -144.00 -22.00   1.00    5.00    --  -86.25   2.00 -46.00  122
  5  \w     35.00  66.00   1.00    5.00    --  106.49 -57.00-120.00   31
  6  \w     36.00 107.00   1.00    5.00    --  106.49-125.00-150.00   71
  7  \w     43.00 119.00   1.00    5.00    --  106.49-135.00 115.00   76
;
_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      -0.0012169000
_diffrn_orient_matrix_UB_12      0.0703053000
_diffrn_orient_matrix_UB_13      -0.0192638000
_diffrn_orient_matrix_UB_21      -0.0013318000
_diffrn_orient_matrix_UB_22      -0.0432453000
_diffrn_orient_matrix_UB_23      -0.0313875000
_diffrn_orient_matrix_UB_31      -0.0840974000
_diffrn_orient_matrix_UB_32      -0.0005114000
_diffrn_orient_matrix_UB_33      0.0007473000
_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  0.0563
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            45826
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         3.543
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.627
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48567
_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    1.411
_exptl_crystal_description       block
_exptl_crystal_F_000             6208
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.144
_refine_diff_density_min         -1.374
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         12612
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1325P)^2^+19.6278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9541
_reflns_number_total             12612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00002d2.cif
_cod_data_source_block           klb-109
_cod_depositor_comments
'Adding full bibliography for 1566151--1566160.cif.'
_cod_database_code               1566153
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CBN
_shelx_estimated_absorpt_t_max   0.458
_shelx_estimated_absorpt_t_min   0.259
_reflns_odcompleteness_completeness 98.64
_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-C44 = C46A-C44 = C46B-C44 = C45A-C44 = C45B-C44 = C47A-C44
 1.56 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C47B \\sim C47A \\sim C45B \\sim C45A \\sim C46A \\sim C46B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C45B) \\sim Ueq, Uanis(C45A) \\sim Ueq, Uanis(C46B) \\sim Ueq,
Uanis(C46A) \\sim Ueq, Uanis(C47B) \\sim Ueq, Uanis(C47A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C47B)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C45B)=Sof(H45D)=Sof(H45E)=
 Sof(H45F)=Sof(C46B)=Sof(H46D)=Sof(H46E)=Sof(H46F)=1-FVAR(1)
 Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C47A)=Sof(H47A)=Sof(H47B)=
 Sof(H47C)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C56(H56), C53(H53), C27(H27), C24(H24)
5.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C3(H3), C34(H34), C5(H5)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C58(H58A,H58B,H58C), C8(H8A,H8B,H8C), C57(H57A,H57B,
 H57C), C43(H43A,H43B,H43C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C37(H37A,
 H37B,H37C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C),
 C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C28(H28A,H28B,H28C), C55(H55A,H55B,
 H55C), C52(H52A,H52B,H52C), C9(H9A,H9B,H9C), C29(H29A,H29B,H29C), C42(H42A,
 H42B,H42C), C41(H41A,H41B,H41C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C),
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C23(H23A,H23B,H23C), C45A(H45A,H45B,H45C), C47A(H47A,H47B,H47C),
 C46A(H46A,H46B,H46C), C47B(H47D,H47E,H47F), C45B(H45D,H45E,H45F), C46B(H46D,
 H46E,H46F)
;
_shelx_res_checksum              32418
_shelx_hkl_checksum              38328
_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 2.090
_oxdiff_exptl_absorpt_empirical_full_min 0.618