Hydroboration of vinyl halides with mesitylborane: a direct access to (mesityl)(alkyl)haloboranes.
Devillard, Marc; Cordier, Marie; Roisnel, Thierry; Dinoi, Chiara; Del Rosal, Iker; Alcaraz, Gilles; Chemical communications (Cambridge, England) 58 (2022) 1589–1592; doi:10.1039/d1cc06365k

data_7129491
_publ_section_title
;
 Hydroboration of vinyl halides with mesitylborane: a direct access to
 (mesityl)(alkyl)haloboranes.
;
_journal_issue                   10
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1589
_journal_page_last               1592
_journal_paper_doi               10.1039/d1cc06365k
_journal_volume                  58
_journal_year                    2022
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H32 B N2, 1.5(C H2 Cl2), Br'
_chemical_formula_sum            'C27.5 H35 B Br Cl3 N2'
_chemical_formula_weight         590.64
_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
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-11-09 deposited with the CCDC.	2022-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.679(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.7324(16)
_cell_length_b                   13.6027(16)
_cell_length_c                   46.542(4)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.3780
_cell_measurement_theta_min      2.3503
_cell_measurement_wavelength     0.71073
_cell_volume                     11779(2)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2019)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            91544
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.594
_diffrn_reflns_theta_min         2.107
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.687
_exptl_absorpt_correction_T_max  0.573
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       prism
_exptl_crystal_F_000             4880
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.330
_refine_diff_density_max         1.108
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1263
_refine_ls_number_reflns         26999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+57.7240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16616
_reflns_number_total             26999
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1cc06365k2.cif
_cod_data_source_block           MD57
_cod_depositor_comments
;
Adding full bibliography for 7129491--7129494.cif.

2025-03-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C55 H70 B2 Br2 Cl6 N4'
_cod_original_formula_weight         1181.29
_cod_original_formula_moiety         '2(C26 H32 B N2), 3(C H2 Cl2), 2(Br)'
_cod_original_formula_units_Z            8
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7129491
_shelx_res_checksum              61391