An unusual autocatalysis with an air-stable Pd complex to promote enantioselective synthesis of Si-stereogenic enynes.
Ling, Fang-Ying; Ye, Fei; Fang, Xiao-Jun; Zhou, Xiao-Hua; Huang, Wei-Sheng; Xu, Zheng; Xu, Li-Wen; Chemical science 14 (2023) 1123–1131; doi:10.1039/d2sc06181c

data_1568164
_publ_section_title
;
 An unusual autocatalysis with an air-stable Pd complex to promote
 enantioselective synthesis of Si-stereogenic enynes.
;
_journal_issue                   5
_journal_name_full               'Chemical science'
_journal_page_first              1123
_journal_page_last               1131
_journal_paper_doi               10.1039/d2sc06181c
_journal_volume                  14
_journal_year                    2023
_chemical_absolute_configuration rm
_chemical_formula_sum            'C24 H24 S Si'
_chemical_formula_weight         372.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-26 deposited with the CCDC.	2022-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.618(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1046(7)
_cell_length_b                   7.8073(6)
_cell_length_c                   15.4040(11)
_cell_measurement_reflns_used    1991
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.0100
_cell_measurement_theta_min      4.9440
_cell_volume                     1072.52(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3868
_diffrn_reflns_point_group_measured_fraction_full 0.731
_diffrn_reflns_point_group_measured_fraction_max 0.731
_diffrn_reflns_theta_full        67.169
_diffrn_reflns_theta_max         67.169
_diffrn_reflns_theta_min         2.929
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            WHITE
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.142
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 573 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         2808
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0538P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.358
_reflns_Friedel_fraction_full    0.419
_reflns_Friedel_fraction_max     0.419
_reflns_number_gt                2436
_reflns_number_total             2808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc06181c2.cif
_cod_data_source_block           exp_12869
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value 'RM' was changed
to 'rm' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 1568164.cif.

2025-07-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C48 H48 S2 Si2'
_cod_original_formula_weight         745.16
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1072.53(14)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1568164
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.819
_shelx_res_checksum              7062
_shelx_hkl_checksum              9526