Synthesis of [1,3]-thiasilolanes <i>via</i> rare-earth-catalysed intramolecular α-C(sp<sup>3</sup>)-H silylation of alkyl sulphides with hydrosilanes.
An, Kun; Liu, Mengqing; Wang, Jingxia; Nishiura, Masayoshi; Cong, Xuefeng; Hou, Zhaomin; Chemical communications (Cambridge, England) 61 (2025) 17181–17184; doi:10.1039/d5cc04330a

data_7135048
_publ_section_title
;
 Synthesis of [1,3]-thiasilolanes <i>via</i> rare-earth-catalysed
 intramolecular &#x3b1;-C(sp<sup>3</sup>)-H silylation of alkyl sulphides
 with hydrosilanes.
;
_journal_issue                   88
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              17181
_journal_page_last               17184
_journal_paper_doi               10.1039/d5cc04330a
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C12 H20 O S Si2'
_chemical_formula_sum            'C12 H20 O S Si2'
_chemical_formula_weight         268.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-06-01 deposited with the CCDC.	2025-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.531(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7711(5)
_cell_length_b                   9.9230(5)
_cell_length_c                   15.3315(7)
_cell_measurement_reflns_used    288
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     1534.57(13)
_computing_cell_refinement       'Bruker SMART APEX3 v2016.1-0'
_computing_data_collection       'Bruker SMART APEX3 v2016.1-0'
_computing_data_reduction        'Bruker SMART APEX3 v2016.1-0'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest with CMOS'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11707
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.137
_diffrn_reflns_theta_max         25.137
_diffrn_reflns_theta_min         2.020
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       plate
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0522P)^2^+0.9125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2348
_reflns_number_total             2736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04330a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7135048.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7135048
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.851
_shelx_estimated_absorpt_t_max   0.924
_shelx_res_checksum              85970
_shelx_hkl_checksum              75721