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_1575663
_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         'C5 H5 B I5 N Si'
_chemical_formula_sum            'C5 H5 B I5 N Si'
_chemical_formula_weight         752.50
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_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
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_cell_length_c                   13.3513(2)
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_cell_measurement_temperature    173(2)
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_computing_cell_refinement       'CrysAlisPro 1.171.42.43a (Rigaku OD, 2022)'
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_computing_publication_material  'IUCr PublCIF online service'
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_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'image plate'
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_diffrn_detector_type            'STOE image plate (34 cm diameter)'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
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_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16700
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.988
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_diffrn_reflns_theta_min         4.090
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
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_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    3.188
_exptl_crystal_description       prism
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.36(7)
_refine_ls_extinction_coef       0.0037(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3849
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0479P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                3718
_reflns_number_total             3849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc06234a3.cif
_cod_data_source_block           2_py_wa3352
_cod_depositor_comments
'Adding full bibliography for 1575660--1575680.cif.'
_cod_original_cell_volume        1567.94(5)
_cod_database_code               1575663
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.198
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_shelx_res_checksum              54365