Synthesis of perhalogenated silylboranes (X = Cl, I) and their application in regiodivergent alkene silaboration.
Heller, Jan; Buch, Christoph D.; Virovets, Alexander V.; Peresypkina, Eugenia; Lerner, Hans-Wolfram; Fantuzzi, Felipe; Wagner, Matthias; Chemical science 16 (2025) 20329–20343; doi:10.1039/d5sc06234a

data_1575674
_publ_section_title
;
 Synthesis of perhalogenated silylboranes (X = Cl, I) and their
 application in regiodivergent alkene silaboration.
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              20329
_journal_page_last               20343
_journal_paper_doi               10.1039/d5sc06234a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C4 H10 B I5 S Si'
_chemical_formula_sum            'C4 H10 B I5 S Si'
_chemical_formula_weight         763.58
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-07-08 deposited with the CCDC.	2025-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.266(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.2014(4)
_cell_length_b                   10.4366(5)
_cell_length_c                   10.9255(5)
_cell_measurement_reflns_used    8583
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.3440
_cell_measurement_theta_min      4.2190
_cell_volume                     820.94(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
_computing_publication_material  'IUCr PublCIF online service'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'image plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5249
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         3.882
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    9.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.43a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.089
_exptl_crystal_description       plank
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.779
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.242
_refine_ls_abs_structure_details
;
 Flack x determined using 1449 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         5249
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0872P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.868
_reflns_Friedel_fraction_max     0.847
_reflns_number_gt                4305
_reflns_number_total             5249
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.8677\% 
around [1.00 -0.00 -0.03] (reciprocal) or [1.00 -0.00 0.00] (direct).

Component 3 is generated from the component 1 using HKLF5tools routine  
by applying the (-1 0 0 / 0 -1 0 / 0 0 -1) matrix.

Analogously, the component 4 is generated from the component 2  
by applying the (-1 0 0 / 0 -1 0 / 0 0 -1) matrix.

In this way the racemic twinning additional to the pseudo-merohedry 
one was taken into account.
;
_cod_data_source_file            d5sc06234a3.cif
_cod_data_source_block           5_SMe2_wa3368
_cod_depositor_comments
'Adding full bibliography for 1575660--1575680.cif.'
_cod_original_cell_volume        820.95(7)
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               1575674
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.110
_shelx_estimated_absorpt_t_max   0.761
_shelx_res_checksum              22386