Facile synthesis of tribenzosilepins from terphenyls and dihydrosilanes by electrophilic double silylation.
Dong, Yafang; Sekine, Kohei; Kuninobu, Yoichiro; Chemical communications (Cambridge, England) 57 (2021) 7007–7010; doi:10.1039/d1cc02326h

data_7128496
_publ_section_title
;
 Facile synthesis of tribenzosilepins from terphenyls and dihydrosilanes
 by electrophilic double silylation.
;
_journal_issue                   57
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7007
_journal_page_last               7010
_journal_paper_doi               10.1039/d1cc02326h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C48 H42 N2 O2 Si'
_chemical_formula_sum            'C48 H42 N2 O2 Si'
_chemical_formula_weight         706.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2021-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.337(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1920(3)
_cell_length_b                   20.3292(6)
_cell_length_c                   20.1781(5)
_cell_measurement_reflns_used    20902
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.0870
_cell_measurement_theta_min      2.2150
_cell_volume                     3770.54(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -56.00 -29.00   0.50    2.00    --    5.00  45.00 120.00   54
  2  \w    -80.00 -54.00   0.50    2.00    --  -10.00  45.00 150.00   52
  3  \w    -89.00  61.00   0.50    2.00    --  -10.00  45.00   0.00  300
  4  \w    -70.00 -45.00   0.50    2.00    --    5.00  45.00  30.00   50
  5  \w      2.00  29.00   0.50    2.00    --    5.00  45.00 173.99   54
  6  \w    -98.00 -66.00   0.50    2.00    --  -10.20  45.00 120.00   64
  7  \w    -26.00  23.00   0.50    2.00    --  -10.20  45.00 120.00   98
  8  \w     39.00  78.00   0.50    2.00    --  -10.20  45.00 120.00   78
  9  \w    -87.00 -62.00   0.50    2.00    --  -10.20  45.00  60.00   50
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC HyPix-6000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0605486000
_diffrn_orient_matrix_UB_12      -0.0132482000
_diffrn_orient_matrix_UB_13      0.0174381000
_diffrn_orient_matrix_UB_21      -0.0064156000
_diffrn_orient_matrix_UB_22      -0.0295746000
_diffrn_orient_matrix_UB_23      -0.0184297000
_diffrn_orient_matrix_UB_31      0.0475338000
_diffrn_orient_matrix_UB_32      0.0129000000
_diffrn_orient_matrix_UB_33      -0.0242935000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44667
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.019
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              FR-E+
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8637
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0471P)^2^+1.7430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7351
_reflns_number_total             8637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02326h2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7128494--7128496.cif.'
_cod_database_code               7128496
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.969
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C12(H12), C16(H16), C17(H17), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
  C31(H31), C34(H34), C37(H37), C38(H38), C41(H41), C42(H42), C45(H45), C48(H48)
1.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C36(H36A,H36B,H36C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              53838
_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 1.100
_oxdiff_exptl_absorpt_empirical_full_min 0.902