Enantioselective synthesis of acyclic monohydrosilanes by steric hindrance assisted C–H silylation
Mu, Delong; Pan, Shuqiong; Wang, Xiaoyu; Liao, Xiaoyun; Huang, Yong; Chen, Jiean; Chemical Communications  (2022) –; doi:10.1039/D2CC02307E

data_7130209
_publ_section_title
;
 Enantioselective synthesis of acyclic monohydrosilanes by steric
 hindrance assisted C--H silylation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02307E
_journal_year                    2022
_chemical_formula_sum            'C22 H22 S2 Si0.25'
_chemical_formula_weight         357.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-15 deposited with the CCDC.	2022-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.21480(10)
_cell_length_b                   7.6293(2)
_cell_length_c                   38.5427(4)
_cell_measurement_temperature    100(2)
_cell_volume                     1827.49(6)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.962
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            9046
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.900
_diffrn_reflns_theta_min         2.293
_exptl_absorpt_coefficient_mu    2.774
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_F_000             758
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.350
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 1432 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.034(8)
_refine_ls_extinction_coef       0.0020(15)
_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   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          4.010
_refine_ls_shift/su_mean         0.040
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0894P)^2^+2.6449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.661
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.914
_reflns_number_gt                3635
_reflns_number_total             3650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02307e2.cif
_cod_data_source_block           mdl-03-18c-220223_auto
_cod_database_code               7130209
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.490
_shelx_estimated_absorpt_t_max   0.607
_shelx_res_checksum              57810