Yttrium-Catalyzed Regioselective α-C‒H Silylation of Methyl Sulfides with Hydrosilanes
Luo, Yong; Teng, Huai-Long; Xue, Can; Nishiura, Masayoshi; Hou, Zhaomin; ACS Catalysis 8 (2018) 8027–; doi:10.1021/acscatal.8b02405

data_4515736
_publ_section_title
;
 Yttrium-Catalyzed Regioselective \a-C--H Silylation of Methyl Sulfides
 with Hydrosilanes
;
_journal_issue                   9
_journal_name_full               'ACS Catalysis'
_journal_page_first              8027
_journal_paper_doi               10.1021/acscatal.8b02405
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C43 H60 S Y2'
_chemical_formula_sum            'C43 H60 S Y2'
_chemical_formula_weight         786.79
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.372(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6411(13)
_cell_length_b                   16.3119(16)
_cell_length_c                   19.7095(18)
_cell_measurement_reflns_used    198
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     3899.3(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8Quest with CMOS'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1109
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73023
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.921
_diffrn_reflns_theta_min         1.649
_exptl_absorpt_coefficient_mu    3.043
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         9337
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0211P)^2^+4.6649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6030
_reflns_number_total             9337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02405_si_002.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4515736
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.462
_shelx_estimated_absorpt_t_max   0.658
_shelx_res_checksum              62256
_shelx_hkl_checksum              96796