An Electroreductive Approach to Radical Silylation via the Activation of Strong Si-Cl Bond.
Lu, Lingxiang; Siu, Juno C.; Lai, Yihuan; Lin, Song; Journal of the American Chemical Society 142 (2020) 21272–21278; doi:10.1021/jacs.0c10899

data_4135389
_publ_section_title
;
 An Electroreductive Approach to Radical Silylation via the Activation of
 Strong Si-Cl Bond.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              21272
_journal_page_last               21278
_journal_paper_doi               10.1021/jacs.0c10899
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C20 H28 Si3'
_chemical_formula_sum            'C20 H28 Si3'
_chemical_formula_weight         352.69
_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
_audit_creation_date             2020-03-24
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.10.09 svn.r3662 for Rigaku Oxford Diffraction, GUI svn.r5959)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.006(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0621(2)
_cell_length_b                   11.3639(2)
_cell_length_c                   15.1141(2)
_cell_measurement_reflns_used    7335
_cell_measurement_temperature    103(5)
_cell_measurement_theta_max      76.1590
_cell_measurement_theta_min      4.8660
_cell_volume                     2071.73(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      103(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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    -17.00   9.00   0.50    4.00    --   50.23 -19.00 -30.00   52
  2  \w     55.00 103.00   0.50   14.00    --  104.00 -94.00  35.00   96
  3  \w     73.00 106.00   0.50   14.00    --  104.00 -77.00  60.00   66
  4  \w     79.00 105.00   0.50   14.00    --  104.00 -94.00  90.00   52
  5  \w     44.00 108.00   0.50   14.00    --  104.00-125.00 120.00  128
  6  \w     32.00  70.00   0.50   14.00    --  104.00 -61.00  60.00   76
  7  \w    101.00 140.00   0.50   14.00    --  104.00  15.00  30.00   78
  8  \w    126.00 152.00   0.50   14.00    --  104.00  35.00  27.00   52
  9  \w    134.00 160.00   0.50   14.00    --  104.00  30.00 -60.00   52
 10  \w    142.00 170.00   0.50   14.00    --  104.00 106.00-123.00   56
 11  \w    108.00 172.00   0.50   14.00    --  104.00 106.00 -63.37  128
 12  \w     92.00 118.00   0.50   14.00    --  104.00  61.00 120.00   52
 13  \w     99.00 148.00   0.50   14.00    --  104.00  61.00 150.00   98
 14  \w     57.00 111.00   0.50   14.00    --  104.00   0.00 -60.00  108
 15  \w     60.00  89.00   0.50   14.00    --  104.00 -77.00-150.00   58
 16  \w     97.00 122.00   0.50   14.00    --  104.00 -81.00 -81.12   50
 17  \w     72.00 104.00   0.50   14.00    --  104.00   0.00-180.00   64
 18  \w     35.00  91.00   0.50   14.00    --  104.00 -94.00-120.00  112
 19  \w     35.00  64.00   0.50   14.00    --  104.00 -61.00-120.00   58
 20  \w     33.00  58.00   0.50   14.00    --  104.00 -61.00 -60.00   50
 21  \w     33.00  58.00   0.50   14.00    --  104.00 -55.00 -81.73   50
 22  \w     35.00  60.00   0.50   14.00    --  104.00 -81.00 -81.12   50
 23  \w    -15.00  26.00   0.50    4.00    --   50.23 -19.00 120.00   82
 24  \w    -80.00 -10.00   0.50    4.00    --  -50.23 106.00-123.00  140
 25  \w   -108.00 -77.00   0.50    4.00    --  -50.23-125.00-150.00   62
 26  \w   -140.00-115.00   0.50   14.00    --  -82.50 -35.00-130.00   50
 27  \w   -114.00 -83.00   0.50    4.00    --  -50.23-125.00  90.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1226074000
_diffrn_orient_matrix_UB_12      0.0021794000
_diffrn_orient_matrix_UB_13      0.0286587000
_diffrn_orient_matrix_UB_21      0.0150381000
_diffrn_orient_matrix_UB_22      -0.1259730000
_diffrn_orient_matrix_UB_23      -0.0358653000
_diffrn_orient_matrix_UB_31      0.0325127000
_diffrn_orient_matrix_UB_32      0.0501281000
_diffrn_orient_matrix_UB_33      -0.0909648000
_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  0.0549
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15249
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.975
_diffrn_reflns_theta_min         2.924
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.071
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.74a (Rigaku Oxford Diffraction, 2020)
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 colourless'
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         4148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0796P)^2^+0.6568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3801
_reflns_number_total             4148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c10899_si_002.cif
_cod_data_source_block           rjcs7_abs
_cod_depositor_comments          'Adding full bibliography for 4135389.cif.'
_cod_database_code               4135389
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C20H28Si3
_chemical_oxdiff_usercomment     'Crystallized from hexanes.'
_reflns_odcompleteness_completeness 93.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.49
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7846(16)
 0.2154(16)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              9531
_shelx_hkl_checksum              85651
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.183
_oxdiff_exptl_absorpt_empirical_full_min 0.663