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_1575661
_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         'C18 H15 B I5 P Si'
_chemical_formula_structural     '[I2 B ((C6 H5)3 P) Si I3]'
_chemical_formula_sum            'C18 H15 B I5 P Si'
_chemical_formula_weight         935.67
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-07-08 deposited with the CCDC.	2025-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.9330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2424(2)
_cell_length_b                   21.4873(3)
_cell_length_c                   14.3571(2)
_cell_measurement_reflns_used    18695
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.0290
_cell_measurement_theta_min      2.6490
_cell_volume                     4974.07(12)
_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-2019/2 (Sheldrick, 2019)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0492
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            60760
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.127
_diffrn_reflns_theta_min         2.230
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    6.338
_exptl_absorpt_correction_T_max  0.06330
_exptl_absorpt_correction_T_min  0.04092
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.499
_exptl_crystal_description       plate
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.045
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.346
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.795
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         10970
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.795
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0269P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7706
_reflns_number_total             10970
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06234a3.cif
_cod_data_source_block           2_PPh3_beta_wa3596
_cod_depositor_comments
'Adding full bibliography for 1575660--1575680.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1575661
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.583
_shelx_estimated_absorpt_t_max   0.763
_oxdiff_exptl_absorpt_empirical_full_min 0.806
_oxdiff_exptl_absorpt_empirical_full_max 1.501
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelx_res_checksum              79174