Synthesis, crystal structure, solid-state optical property and C–H activation of sp3 carbon of highly-stable 1-(2′,6′-dimesitylphenyl)-2,3,4,5-tetraphenylborole
Himeno, Ryoji; Ito, Shunichiro; Tanaka, Kazuo; Chujo, Yoshiki; New Journal of Chemistry 45 (2021) 22569–22573; doi:10.1039/D1NJ04666G

data_7061062
_publ_section_title
;
 Synthesis, crystal structure, solid-state optical property and C--H
 activation of sp3 carbon of highly-stable
 1-(2&#x2032;,6&#x2032;-dimesitylphenyl)-2,3,4,5-tetraphenylborole
;
_journal_issue                   48
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              22569
_journal_page_last               22573
_journal_paper_doi               10.1039/D1NJ04666G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C52 H45 B, 0.5 (C6 H14)'
_chemical_formula_sum            'C55 H52 B'
_chemical_formula_weight         723.8258
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-10-25 deposited with the CCDC.	2021-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.517(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6520(9)
_cell_length_b                   12.8989(6)
_cell_length_c                   12.7196(7)
_cell_measurement_reflns_used    11509
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.21
_cell_volume                     2147.4(2)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2017)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2017)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2017)'
_computing_molecular_graphics
'ShelXle (J. Appl. Cryst., 44, (2011) 1281-1284.)'
_computing_publication_material
'ShelXle (J. Appl. Cryst., 44, (2011) 1281-1284.)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Raxis Rapid'
_diffrn_measurement_method       'oscillation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20177
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.217
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4370
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSCOR, (Rigaku, 1995)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
The unit cell contains one hexane molecule which have been treated
as a diffuse contribution to the overall scattering without specific atom
positions by SQUEEZE/PLATON. 
;
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0796
_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^)+(0.0909P)^2^+1.1530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.2060
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3317
_reflns_number_total             4916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04666g2.cif
_cod_data_source_block           B_blue_a_sq
_cod_depositor_comments
'Adding full bibliography for 7061061--7061063.cif.'
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7061062
_shelx_shelxl_version_number     2018/3
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              42543
_shelx_fab_checksum              67850