Palladium-Catalyzed (4 + 4) Annulation of Silacyclobutanes and 2-Iodobiarenes to Eight-Membered Silacycles via C–H and C–Si Bond Activation
Zhu, Ming-Hui; Zhang, Xiao-Wen; Usman, Muhammad; Cong, Hengjiang; Liu, Wen-Bo; ACS Catalysis  (2021) 5703–5708; doi:10.1021/acscatal.1c00975

data_4518630
_publ_section_title
;
 Palladium-Catalyzed (4 + 4) Annulation of Silacyclobutanes and
 2-Iodobiarenes to Eight-Membered Silacycles via C--H and C--Si Bond
 Activation
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              5703
_journal_page_last               5708
_journal_paper_doi               10.1021/acscatal.1c00975
_journal_year                    2021
_chemical_formula_moiety         'C29 H26 O2 Si'
_chemical_formula_sum            'C29 H26 O2 Si'
_chemical_formula_weight         434.59
_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'
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_atom_sites_solution_primary     dual
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;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
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_diffrn_ambient_environment      air
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_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
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_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    -84.00  94.00   0.50    0.50    --    5.00 -14.00  90.00  356
  2  \w   -136.00  43.00   0.50    0.50    --  -46.80  14.00 -98.00  358
  3  \w   -136.00  43.00   0.50    0.50    --  -46.80 -14.00  90.00  358
  4  \w   -192.00 -13.00   0.50    0.50    -- -102.80 -14.00  90.00  358
  5  \w   -192.00 -13.00   0.50    0.50    -- -102.80  14.00 -98.00  358
  6  \w    -28.00  94.00   0.50    0.50    --    5.00  57.00-180.00  244
  7  \w   -136.00  -8.00   0.50    0.50    --  -46.80 -76.00 -60.00  256
  8  \w    -80.00  43.00   0.50    0.50    --  -46.80  57.00 120.00  246
  9  \w   -136.00 -13.00   0.50    0.50    --  -46.80 -57.00 -30.00  246
 10  \w    -90.00 -64.00   0.50    0.50    -- -102.80 -74.00  12.03   52
 11  \w    -90.00 -64.00   0.50    0.50    -- -102.80 -76.00 -30.00   52
 12  \w    -90.00 -64.00   0.50    0.50    -- -102.80 -76.00   0.00   52
 13  \w    -38.00 -13.00   0.50    0.50    -- -102.80  76.00  90.00   50
 14  \w   -128.00-102.00   0.50    0.50    -- -102.80  76.00  90.00   52
 15  \w    -93.00 -67.00   0.50    0.50    -- -102.80 -66.00 -12.40   52
 16  \w    -90.00 -64.00   0.50    0.50    -- -102.80 -76.00  34.42   52
 17  \w    -70.00 -14.00   0.50    0.50    -- -102.80  57.00  30.00  112
 18  \w    -91.00 -65.00   0.50    0.50    -- -102.80 -74.00 -23.41   52
 19  \w   -141.00 -64.00   0.50    0.50    -- -102.80 -76.00 -60.00  154
 20  \w    -53.00 -27.00   0.50    0.50    -- -102.80  76.00  60.00   52
 21  \w   -141.00 -58.00   0.50    0.50    -- -102.80  76.00  60.00  166
 22  \w   -102.00 -65.00   0.50    0.50    -- -102.80 -76.00  60.00   74
 23  \w    -94.00 -68.00   0.50    0.50    -- -102.80 -65.00  62.51   52
 24  \w   -167.00-112.00   0.50    0.50    -- -102.80 -68.00  37.43  110
 25  \w    -99.00 -67.00   0.50    0.50    -- -102.80 -68.00  37.43   64
 26  \w    -92.00 -66.00   0.50    0.50    -- -102.80 -69.00 -24.33   52
 27  \w    -89.00 -64.00   0.50    0.50    -- -102.80 -74.00 -45.39   50
 28  \w   -104.00 -67.00   0.50    0.50    -- -102.80 -75.00 -50.93   74
 29  \w   -191.00 -69.00   0.50    0.50    -- -102.80 -59.00  11.14  244
 30  \w    -91.00 -64.00   0.50    0.50    -- -102.80 -76.00  30.00   54
 31  \w   -149.00-123.00   0.50    0.50    -- -102.80 -74.00 -45.39   52
 32  \w    -90.00 -65.00   0.50    0.50    -- -102.80 -73.00  63.43   50
 33  \w   -191.00-165.00   0.50    0.50    -- -102.80 -76.00  60.00   52
 34  \w   -191.00 -71.00   0.50    0.50    -- -102.80 -57.00  60.00  240
 35  \w   -191.00-145.00   0.50    0.50    -- -102.80 -76.00 -60.00   92
 36  \w   -191.00 -69.00   0.50    0.50    -- -102.80 -58.00 -13.31  244
 37  \w    -90.00 -65.00   0.50    0.50    -- -102.80 -73.00 -44.14   50
 38  \w    -92.00 -67.00   0.50    0.50    -- -102.80 -72.00 -29.69   50
 39  \w    -90.00 -64.00   0.50    0.50    -- -102.80 -76.00  25.16   52
 40  \w   -141.00 -13.00   0.50    0.50    -- -102.80  76.00 -30.00  256
;
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'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0287024000
_diffrn_orient_matrix_UB_12      -0.0403325000
_diffrn_orient_matrix_UB_13      -0.0843831000
_diffrn_orient_matrix_UB_21      0.0777701000
_diffrn_orient_matrix_UB_22      0.0031002000
_diffrn_orient_matrix_UB_23      -0.0192436000
_diffrn_orient_matrix_UB_31      0.0065947000
_diffrn_orient_matrix_UB_32      -0.2126886000
_diffrn_orient_matrix_UB_33      0.0157365000
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_wavelength     1.54184
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_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42493
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.236
_diffrn_reflns_theta_min         4.773
_diffrn_source                   'Rotating-anode X-ray tube'
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_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73011
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_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
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_exptl_crystal_F_000             920
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_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         4679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0580P)^2^+0.4082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4436
_reflns_number_total             4679
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs1c00975_si_002.cif
_cod_data_source_block           liuwenbo-zmh-iv-193-20200716-rt
_cod_original_cell_volume        2331.74(2)
_cod_database_code               4518630
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'H C O Si'
_shelx_estimated_absorpt_t_max   0.959
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_reflns_odcompleteness_completeness 99.18
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     39.93
_olex2_refinement_description
;
;
_shelx_res_checksum              90800
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_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 1.371
_oxdiff_exptl_absorpt_empirical_full_min 0.576