Rapid, iterative syntheses of unsymmetrical di- and triarylboranes from crystalline aryldifluoroboranes.
Turnbull, Douglas; Légaré, Marc-André; Chemical science 14 (2023) 14256–14261; doi:10.1039/d3sc05071h

data_1570345
_publ_section_title
;
 Rapid, iterative syntheses of unsymmetrical di- and triarylboranes from
 crystalline aryldifluoroboranes.
;
_journal_issue                   48
_journal_name_full               'Chemical science'
_journal_page_first              14256
_journal_page_last               14261
_journal_paper_doi               10.1039/d3sc05071h
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C20 H26 B F'
_chemical_formula_sum            'C20 H26 B F'
_chemical_formula_weight         296.252
_chemical_name_systematic
fluoro(mesityl)(2,3,4,5,6-pentamethylphenyl)borane
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_Int_Tables_number      9
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-09-03 deposited with the CCDC.	2023-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.716(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6399(4)
_cell_length_b                   25.3455(11)
_cell_length_c                   8.6121(3)
_cell_measurement_reflns_used    2467
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      54.50
_cell_measurement_theta_min      3.03
_cell_volume                     1713.14(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.9808
_diffrn_measured_fraction_theta_max 0.9609
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.9808
_diffrn_reflns_Laue_measured_fraction_max 0.9609
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8471
_diffrn_reflns_point_group_measured_fraction_full 0.9207
_diffrn_reflns_point_group_measured_fraction_max 0.8745
_diffrn_reflns_theta_full        53.5942
_diffrn_reflns_theta_max         57.02
_diffrn_reflns_theta_min         5.13
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1298 before and 0.0450 after correction.
The Ratio of minimum to maximum transmission is 0.7187.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       plate
_exptl_crystal_F_000             641.454
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.1878
_refine_diff_density_min         -0.1878
_refine_diff_density_rms         0.0431
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.11(11)
_refine_ls_d_res_high            0.7995
_refine_ls_d_res_low             7.4972
_refine_ls_goodness_of_fit_ref   1.0411
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    36
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3072
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0411
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+0.2820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.787
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              31
_reflns_limit_k_min              -31
_reflns_limit_l_max              10
_reflns_limit_l_min              -10
_reflns_number_gt                2765
_reflns_number_total             3072
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3sc05071h2.cif
_cod_data_source_block           4b_C6Me5MesBF
_cod_depositor_comments
'Adding full bibliography for 1570333--1570346.cif.'
_cod_original_sg_symbol_Hall     ' C -2yc'
_cod_database_code               1570345
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7(2)
 0.3(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16)
3.b Idealised Me refined as rotating group:
 C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c),
 C11(H11a,H11b,H11c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20(H20a,H20b,
 H20c)
;
_olex2_submission_special_instructions 'No special instructions were received'