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_1566152
_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 Cl N3'
_chemical_formula_sum            'C29 H49 B Cl N3'
_chemical_formula_weight         485.97
_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                   16.7035(10)
_cell_length_b                   10.0800(6)
_cell_length_c                   17.6907(7)
_cell_measurement_reflns_used    2304
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.5960
_cell_measurement_theta_min      4.9920
_cell_volume                     2978.6(3)
_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 0.982
_diffrn_measured_fraction_theta_max 0.911
_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     34.00  66.00   1.00    1.20    --  106.49 -57.00 120.00   32
  2  \w     40.00  66.00   1.00    1.20    --  106.49 -57.00  90.00   26
  3  \w     40.00  66.00   1.00    1.20    --  106.49 -57.00 -30.00   26
  4  \w     34.00  59.00   1.00    1.20    --  106.49 -53.00-162.00   25
  5  \w    -25.00  27.00   1.00    0.36    --   48.45 -19.00-150.00   52
  6  \w   -115.00 -55.00   1.00    0.36    --  -48.45 -53.00-162.00   60
  7  \w   -159.00-113.00   1.00    1.20    --  -86.25-110.00 -32.00   46
  8  \w    -58.00 -18.00   1.00    1.20    --  -86.25  53.00 -17.00   40
  9  \w    -40.00 -13.00   1.00    1.20    --  -86.25  38.00-120.00   27
 10  \w    -54.00 -18.00   1.00    1.20    --  -86.25  71.00-179.00   36
 11  \w    -87.00 -60.00   1.00    1.20    --  -86.25  71.00-179.00   27
 12  \w     53.00 103.00   1.00    1.20    --  106.49 -99.00 -30.00   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      -0.0307951000
_diffrn_orient_matrix_UB_12      0.1440247000
_diffrn_orient_matrix_UB_13      0.0001527000
_diffrn_orient_matrix_UB_21      0.0667213000
_diffrn_orient_matrix_UB_22      0.0394032000
_diffrn_orient_matrix_UB_23      -0.0559392000
_diffrn_orient_matrix_UB_31      -0.0557714000
_diffrn_orient_matrix_UB_32      -0.0323985000
_diffrn_orient_matrix_UB_33      -0.0667451000
_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  0.0733
_diffrn_reflns_av_unetI/netI     0.0960
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8994
_diffrn_reflns_point_group_measured_fraction_full 0.750
_diffrn_reflns_point_group_measured_fraction_max 0.681
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.647
_diffrn_reflns_theta_min         5.000
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60226
_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    1.084
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 828 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4268
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0743P)^2^+0.4025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.446
_reflns_Friedel_fraction_full    0.500
_reflns_Friedel_fraction_max     0.434
_reflns_number_gt                3541
_reflns_number_total             4268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00002d2.cif
_cod_data_source_block           klb-110
_cod_depositor_comments
'Adding full bibliography for 1566151--1566160.cif.'
_cod_database_code               1566152
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CNB
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.702
_reflns_odcompleteness_completeness 98.28
_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
 C17A-C15 = C17B-C15 = C18A-C15 = C18B-C15 = C16A-C15 = C16B-C15
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C15 \\sim C16A \\sim C17A \\sim C18A \\sim C16B \\sim C17B \\sim C18B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
Uanis(C15) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C16A)
\\sim Ueq, Uanis(C16B) \\sim Ueq, Uanis(C17B) \\sim Ueq, Uanis(C18B) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17B)=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(1)
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17A)=Sof(H17A)=Sof(H17B)=
 Sof(H17C)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C24(H24), C27(H27)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
5.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), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C18A(H18A,H18B,H18C),
 C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F), C18B(H18D,H18E,H18F)
;
_shelx_res_checksum              15368
_shelx_hkl_checksum              23799
_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 2.809
_oxdiff_exptl_absorpt_empirical_full_min 0.570