Arylsilylation of Electron-Deficient Alkenes via Cooperative Photoredox and Nickel Catalysis
Zhang, Zhikun; Hu, Xile; ACS Catalysis 10 (2019) 777–; doi:10.1021/acscatal.9b04916

data_4517218
_publ_section_title
;
 Arylsilylation of Electron-Deficient Alkenes via Cooperative Photoredox
 and Nickel Catalysis
;
_journal_issue                   1
_journal_name_full               'ACS Catalysis'
_journal_page_first              777
_journal_paper_doi               10.1021/acscatal.9b04916
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         'C20 H40 O4 S Si4'
_chemical_formula_sum            'C20 H40 O4 S Si4'
_chemical_formula_weight         488.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 107.915(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0893(4)
_cell_length_b                   9.47947(15)
_cell_length_c                   14.2315(3)
_cell_measurement_reflns_used    11230
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.4180
_cell_measurement_theta_min      3.2290
_cell_volume                     2835.51(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Mercury 4.1.3 (CCDC, 2019)'
_computing_publication_material  'CIFTab (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -98.00 -72.00   1.00    1.00    --  -43.01 -57.00  30.00   26
  2  \w   -106.00 -10.00   1.00    1.00    --  -43.01 -77.00  60.00   96
  3  \w   -116.00 -79.00   1.00    1.00    --  -43.01 -99.00-180.00   37
  4  \w   -117.00 -79.00   1.00    1.00    --  -43.01 -99.00 120.00   38
  5  \w    -71.00  28.00   1.00    1.00    --  -43.01  57.00-150.00   99
  6  \w     24.00  77.00   1.00    1.00    --   43.01-125.00   0.00   53
  7  \w     39.00 112.00   1.00    4.00    --  103.49-111.00 120.00   73
  8  \w     28.00 132.00   1.00    4.00    --  103.49 -30.00  90.00  104
  9  \w    100.00 149.00   1.00    4.00    --  103.49 111.00 150.00   49
 10  \w    110.00 143.00   1.00    4.00    --  103.49 111.00-120.00   33
 11  \w    148.00 174.00   1.00    4.00    --  103.49 111.00-120.00   26
 12  \w     75.00 110.00   1.00    4.00    --  103.49-111.00   0.00   35
 13  \w     26.00 143.00   1.00    4.00    --  103.49 -15.00-180.00  117
 14  \w     78.00 113.00   1.00    4.00    --  103.49  45.00  60.00   35
 15  \w     37.00 126.00   1.00    4.00    --  103.49 -61.00-150.00   89
 16  \w    102.00 176.00   1.00    4.00    --  103.49 111.00 120.00   74
 17  \w     63.00  89.00   1.00    4.00    --  103.49-111.00  60.00   26
 18  \w     81.00 107.00   1.00    4.00    --  103.49-111.00 -90.00   26
 19  \w     29.00  55.00   1.00    4.00    --  103.49-111.00 -90.00   26
 20  \w     45.00  98.00   1.00    4.00    --  103.49 -94.00-180.00   53
 21  \w     81.00 120.00   1.00    4.00    --  103.49  45.00  90.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19497
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.466
_diffrn_reflns_theta_min         4.207
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.806
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.068
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pale colourless'
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.825
_exptl_crystal_size_mid          0.683
_exptl_crystal_size_min          0.417
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00083(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   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0709P)^2^+1.0047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5290
_reflns_number_total             5533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs9b04916_si_002.cif
_cod_data_source_block           zzk-4-76-1
_cod_depositor_comments          'Adding full bibliography for 4517218.cif.'
_cod_original_cell_volume        2835.53(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4517218
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.206
_shelx_estimated_absorpt_t_max   0.387
_shelx_res_checksum              63312
_shelx_hkl_checksum              54948