Hexamethylbenzene elimination enables the generation of transient, sterically unhindered multiply bonded boron species
Zhang, Chonghe; Dabringhaus, Philipp; Tra, Bi Youan E.; Gilliard, Robert J.; Cummins, Christopher C.; Chemical Science 16 (2025) 11841–11848; doi:10.1039/D5SC02645H

data_1574657
_publ_section_title
;
 Hexamethylbenzene elimination enables the generation of transient,
 sterically unhindered multiply bonded boron species
;
_journal_issue                   26
_journal_name_full               'Chemical Science'
_journal_page_first              11841
_journal_page_last               11848
_journal_paper_doi               10.1039/D5SC02645H
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C45 H50 B N3'
_chemical_formula_sum            'C45 H50 B N3'
_chemical_formula_weight         643.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-04 deposited with the CCDC.	2025-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.417(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4580(13)
_cell_length_b                   14.7741(11)
_cell_length_c                   16.2688(12)
_cell_measurement_reflns_used    9786
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.095
_cell_measurement_theta_min      2.408
_cell_volume                     4064.0(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1206
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            144514
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.830
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  0.7432
_exptl_absorpt_correction_T_min  0.6709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1055 before and 0.0747 after correction.
The Ratio of minimum to maximum transmission is 0.9027.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.052
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.021
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0680P)^2^+2.1358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4886
_reflns_number_total             7184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02645h3.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1574650--1574657.cif.'
_cod_database_code               1574657
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00I(H00I), C00M(H00M), C00O(H00O), C00P(H00P), C00Z(H00Z),
 C011(H011), C012(H012), C015(H015), C018(H018), C019(H019), C01A(H01P),
 C01B(H01Q), C01D(H01R)
1.b Idealised Me refined as rotating group:
 C00K(H00A,H00B,H00C), C00Q(H00D,H00E,H00F), C00S(H00H,H00J,H00K), C00T(H00L,
 H00N,H00Q), C00W(H00R,H00S,H00T), C00X(H00U,H00V,H00W), C00Y(H00X,H00Y,H),
 C010(H01A,H01B,H01C), C013(H01D,H01E,H01F), C014(H01G,H01H,H01I), C016(H01J,
 H01K,H01L), C017(H01M,H01N,H01O)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              85570
_shelx_fab_checksum              38092
_olex2_submission_special_instructions 'No special instructions were received'