Regio- and diastereoselective synthesis of multi-substituted silacyclopentanes by catalytic cyclosilylborylation of styryl(vinyl)silanes
Ueji, Kanta; Shintani, Ryo; Chemical Communications  (2026) –; doi:10.1039/D6CC00416D

data_7135689
_publ_section_title
;
 Regio- and diastereoselective synthesis of multi-substituted
 silacyclopentanes by catalytic cyclosilylborylation of
 styryl(vinyl)silanes.
;
_journal_issue                   33
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8461
_journal_page_last               8465
_journal_paper_doi               10.1039/d6cc00416d
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C29 H45 B O2 Si2'
_chemical_formula_sum            'C29 H45 B O2 Si2'
_chemical_formula_weight         492.64
_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             2025-02-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2026-01-21 deposited with the CCDC.	2026-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.7620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2241(2)
_cell_length_b                   14.3979(2)
_cell_length_c                   13.2285(2)
_cell_measurement_reflns_used    14677
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      75.7850
_cell_measurement_theta_min      2.8930
_cell_volume                     2896.25(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.960
_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    106.00 164.00   0.50    0.60    --  102.75  45.00 120.00  116
  2  \w     63.00  88.00   0.50    0.15    --   48.50 162.00  13.00   50
  3  \w    113.00 140.00   0.50    0.60    --  102.75 117.00-136.00   54
  4  \w    129.00 168.00   0.50    0.60    --  102.75  15.00-120.00   78
  5  \w     44.00 100.00   0.50    0.60    --  102.75 -94.00 -30.00  112
  6  \w     47.00 118.00   0.50    0.15    --   48.50-162.00 -14.00  142
  7  \w     62.00 102.00   0.50    0.60    --  102.75-117.00 135.00   80
  8  \w     14.00  73.00   0.50    0.15    --   48.50-117.00 135.00  118
  9  \w    104.00 135.00   0.50    0.60    --  102.75-162.00 -14.00   62
 10  \w     32.00  71.00   0.50    0.60    --  102.75 -61.00-120.00   78
 11  \w     37.00  67.00   0.50    0.60    --  102.75 -61.00 -90.00   60
 12  \w     31.00  78.00   0.50    0.60    --  102.75 -61.00 -60.00   94
 13  \w     34.00  79.00   0.50    0.60    --  102.75 -61.00   0.00   90
 14  \w    -23.00   4.00   0.50    0.15    --   48.50 -19.00-150.00   54
 15  \w     -6.00  19.00   0.50    0.15    --  -48.50  19.00-150.00   50
 16  \w    -62.00 -37.00   0.50    0.60    -- -102.00  61.00-180.00   50
 17  \w    -74.00 -49.00   0.50    0.60    -- -102.00  61.00-150.00   50
 18  \w     -6.00  21.00   0.50    0.15    --  -48.50  19.00  60.00   54
 19  \w     -4.00  26.00   0.50    0.15    --  -48.50  19.00  30.00   60
 20  \w    -72.00 -47.00   0.50    0.15    --  -48.50 117.00-136.00   50
 21  \w   -107.00 -70.00   0.50    0.60    -- -102.00 117.00-136.00   74
 22  \w   -168.00 -97.00   0.50    0.60    -- -102.00 -15.00 -60.00  142
 23  \w   -175.00 -92.00   0.50    0.60    -- -102.00 -30.00  30.00  166
 24  \w   -126.00 -81.00   0.50    0.60    -- -102.00-117.00 135.00   90
 25  \w   -100.00 -72.00   0.50    0.15    --  -48.50-162.00 -14.00   56
 26  \w   -116.00 -74.00   0.50    0.15    --  -48.50-125.00 -60.00   84
 27  \w   -119.00 -92.00   0.50    0.60    -- -102.00-162.00 -14.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1001951000
_diffrn_orient_matrix_UB_12      -0.0137334000
_diffrn_orient_matrix_UB_13      -0.0136939000
_diffrn_orient_matrix_UB_21      0.0008645000
_diffrn_orient_matrix_UB_22      -0.0566968000
_diffrn_orient_matrix_UB_23      0.0987755000
_diffrn_orient_matrix_UB_31      -0.0148387000
_diffrn_orient_matrix_UB_32      0.0897495000
_diffrn_orient_matrix_UB_33      0.0603578000
_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  0.0420
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21625
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.127
_diffrn_reflns_theta_min         2.906
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.119a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.649
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0984P)^2^+0.7803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5328
_reflns_number_total             5818
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cc00416d2.cif
_cod_data_source_block           exp_2271_auto
_cod_depositor_comments
'Adding full bibliography for 7135688--7135689.cif.'
_cod_database_code               7135689
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C29H45BO2Si2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C8(H8), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C26(H26A,H26B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C4(H4), C2(H2), C30(H30), C33(H33), C34(H34), C32(H32), C5(H5),
 C3(H3), C31(H31)
2.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C20(H20A,
 H20B,H20C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              33906
_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 1.928
_oxdiff_exptl_absorpt_empirical_full_min 0.508