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_7132638
_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         'C98 H130 B4 N8 Si2, 2(C6 H6)'
_chemical_formula_sum            'C110 H142 B4 N8 Si2'
_chemical_formula_weight         1675.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-10-13 deposited with the CCDC.	2024-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                95.791(2)
_cell_angle_beta                 101.108(2)
_cell_angle_gamma                104.877(2)
_cell_formula_units_Z            1
_cell_length_a                   11.6410(2)
_cell_length_b                   12.3141(3)
_cell_length_c                   17.9847(3)
_cell_measurement_reflns_used    33203
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.1420
_cell_measurement_theta_min      2.5400
_cell_volume                     2414.05(9)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            90262
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.125
_diffrn_reflns_theta_min         2.536
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.724
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74209
_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            orange
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       plate
_exptl_crystal_F_000             906
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.028
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         9484
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0310P)^2^+4.1403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8645
_reflns_number_total             9484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00141a2.cif
_cod_data_source_block           ToBr102_ToBr_a
_cod_depositor_comments
'Adding full bibliography for 7132636--7132639.cif.'
_cod_database_code               7132638
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.885
_shelx_estimated_absorpt_t_max   0.980
_oxdiff_exptl_absorpt_empirical_full_min 0.700
_oxdiff_exptl_absorpt_empirical_full_max 1.569
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              78343
_shelx_hkl_checksum              40676