Hydrosilylation of BB triple bonds: catalyst- and reductant-free construction of B-Si bonds and B<sub>2</sub>Si heterocycles.
Brückner, Tobias; Duwe, Dario; Fantuzzi, Felipe; Heß, Merlin; Dewhurst, Rian D.; Radacki, Krzysztof; Braunschweig, Holger; Chemical communications (Cambridge, England) 60 (2024) 3259–3262; doi:10.1039/d4cc00141a

data_7132639
_publ_section_title
;
 Hydrosilylation of B&#xe002;B triple bonds: catalyst- and reductant-free
 construction of B-Si bonds and B<sub>2</sub>Si heterocycles.
;
_journal_issue                   24
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3259
_journal_page_last               3262
_journal_paper_doi               10.1039/d4cc00141a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C54 H72 B2 N4 Si'
_chemical_formula_sum            'C54 H72 B2 N4 Si'
_chemical_formula_weight         826.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2y (K.Radacki, 2005-21)'
_audit_update_record
;
2023-10-13 deposited with the CCDC.	2024-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.4985(8)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   24.18452(19)
_cell_length_b                   11.44862(12)
_cell_length_c                   68.9173(7)
_cell_measurement_reflns_used    25300
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.1550
_cell_measurement_theta_min      3.6860
_cell_volume                     19081.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix 6000'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.975
_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      0.00  38.00   0.38    6.99    --   47.70 -66.00  16.00  100
   2  \w     36.00  78.18   0.38   27.96    --  107.75 -66.00  16.00  111
   3  \w     59.00  92.06   0.38   27.96    --  107.75 -77.00  60.00   87
   4  \w     37.00  81.08   0.38   27.96    --  107.75 -94.00   0.00  116
   5  \w     37.00  66.26   0.38   27.96    --  107.75 -61.00 -60.00   77
   6  \w     36.00  62.22   0.38   27.96    --  107.75 -61.00-120.00   69
   7  \w     35.00  60.08   0.38   27.96    --  107.75 -61.00-150.00   66
   8  \w     52.00 103.30   0.38   27.96    --  107.75 -94.00-180.00  135
   9  \w     80.00 105.08   0.38   27.96    --  107.75 -77.00-180.00   66
  10  \w     95.00 140.22   0.38   27.96    --  107.75  15.00-120.00  119
  11  \w    150.00 176.22   0.38   27.96    --  107.75  15.00-120.00   69
  12  \w    118.00 177.28   0.38   27.96    --  107.75  77.00-120.00  156
  13  \w    145.00 170.08   0.38   27.96    --  107.75 125.00-180.00   66
  14  \w     95.00 121.22   0.38   27.96    --  107.75 125.00-180.00   69
  15  \w     86.00 112.22   0.38   27.96    --  107.75  77.00-120.00   69
  16  \w    101.00 155.72   0.38   27.96    --  107.75  45.00  60.00  144
  17  \w    122.00 157.34   0.38   27.96    --  107.75  45.00  90.00   93
  18  \w     90.00 173.22   0.38   27.96    --  107.75  66.00 151.00  219
  19  \w     39.00  69.78   0.38   27.96    --  107.75 -61.00  90.00   81
  20  \w     35.00  69.20   0.38   27.96    --  107.75 -61.00  60.00   90
  21  \w     38.00  64.22   0.38   27.96    --  107.75 -61.00 -90.00   69
  22  \w     35.00  75.28   0.38   27.96    --  107.75 -77.00-180.00  106
  23  \w     36.00  86.16   0.38   27.96    --  107.75-125.00-180.00  132
  24  \w    -66.00  24.06   0.38    6.99    --  -47.70  66.00 151.00  237
  25  \w     30.00  84.34   0.38    6.99    --   47.70  66.00 151.00  143
  26  \w    -46.00 -19.78   0.38   27.96    --  -86.25  61.00 -60.00   69
  27  \w    -49.00 -19.74   0.38   27.96    --  -86.25  45.00-150.00   77
  28  \w   -119.00 -29.70   0.38    6.99    --  -47.70 -66.00  16.00  235
  29  \w    -71.00 -45.92   0.38   27.96    --  -86.25  66.00 151.00   66
  30  \w   -138.00-112.92   0.38   27.96    --  -86.25 -66.00  16.00   66
  31  \w   -118.00 -73.92   0.38    6.99    --  -47.70-125.00 -90.00  116
  32  \w   -117.00 -77.86   0.38    6.99    --  -47.70-125.00-180.00  103

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       85
_diffrn_reflns_limit_l_min       -86
_diffrn_reflns_number            79651
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.504
_diffrn_reflns_theta_min         2.565
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet X-ray Source'
_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019) Empirical 
absorption correction using spherical harmonics, implemented in SCALE3 
ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       plate
_exptl_crystal_F_000             7168
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1139
_refine_ls_number_reflns         19783
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+36.4586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17084
_reflns_number_total             19783
_reflns_threshold_expression     'I > 2\s(I)'
_twin_dimensionality             triperiodic
_twin_formation_mechanism        gt
_twin_morphology                 polysynthetic
_twin_special_details
;
Component 2 rotated by 136.7997\% around [0.49 0.04 -0.87] (reciprocal) or 
[0.91 0.36 -0.20] (direct).
Only hklf4 used (R~int~ higher than 90% and F2/\s < 1 for the second domain 
reflections).
;
_cod_data_source_file            d4cc00141a2.cif
_cod_data_source_block           KR998_ToBr2_twin1_hklf4_a
_cod_depositor_comments
'Adding full bibliography for 7132636--7132639.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7132639
_shelx_shelxl_version_number     2018/3
_oxdiff_twin_items               2
_shelx_res_checksum              60735
_shelx_hkl_checksum              31757