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_1566151
_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 B Br N3'
_chemical_formula_sum            'C29 H49 B Br N3'
_chemical_formula_weight         530.43
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-16
_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            4
_cell_length_a                   16.6843(11)
_cell_length_b                   10.1022(8)
_cell_length_c                   17.8126(10)
_cell_measurement_reflns_used    5388
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.1470
_cell_measurement_theta_min      4.9410
_cell_volume                     3002.3(4)
_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_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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    106.00 168.00   1.00    0.40    --  106.49 122.00 133.00   62
  2  \w    100.00 175.00   1.00    0.40    --  106.49  19.00 -30.00   75
  3  \w    -15.00  10.00   1.00    0.10    --   48.45 -19.00 121.00   25
  4  \w     41.00 106.00   1.00    0.40    --  106.49-125.00  90.00   65
  5  \w    -27.00  27.00   1.00    0.10    --  -48.45  19.00 150.00   54
  6  \w    -27.00  27.00   1.00    0.10    --  -48.45  19.00  30.00   54
  7  \w   -121.00 -96.00   1.00    0.40    --  -86.25 -19.00 121.00   25
  8  \w   -159.00 -90.00   1.00    0.40    --  -86.25-109.00 -46.00   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      -0.0341270000
_diffrn_orient_matrix_UB_12      0.0899746000
_diffrn_orient_matrix_UB_13      0.0038208000
_diffrn_orient_matrix_UB_21      -0.0163328000
_diffrn_orient_matrix_UB_22      0.0021820000
_diffrn_orient_matrix_UB_23      -0.0859691000
_diffrn_orient_matrix_UB_31      -0.1477310000
_diffrn_orient_matrix_UB_32      -0.0206383000
_diffrn_orient_matrix_UB_33      0.0086532000
_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  0.0482
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8657
_diffrn_reflns_point_group_measured_fraction_full 0.756
_diffrn_reflns_point_group_measured_fraction_max 0.755
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         4.966
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45584
_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    1.174
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 1139 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4047
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+1.3491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.478
_reflns_Friedel_fraction_full    0.507
_reflns_Friedel_fraction_max     0.507
_reflns_number_gt                3776
_reflns_number_total             4047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00002d2.cif
_cod_data_source_block           klb-93
_cod_depositor_comments
'Adding full bibliography for 1566151--1566160.cif.'
_cod_database_code               1566151
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CNB
_shelx_estimated_absorpt_t_max   0.585
_shelx_estimated_absorpt_t_min   0.502
_reflns_odcompleteness_completeness 57.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18B-C15 = C18A-C15
 1.51 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C18A \\sim C18B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(C18A) \\sim Ueq, Uanis(C18B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(1)
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C22(H22), C25(H25)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3)
5.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C13(H13A,
 H13B,H13C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C9(H9A,
 H9B,H9C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18B(H18A,H18B,H18C),
 C18A(H18D,H18E,H18F)
;
_shelx_res_checksum              10361
_shelx_hkl_checksum              837
_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 2.136
_oxdiff_exptl_absorpt_empirical_full_min 0.595