Approach to the “Missing” Diarylsilylene: Formation, Characterization, and Intramolecular C–H Bond Activation of Blue Diarylsilylenes with Bulky Rind Groups
Mochihara, Kazuki; Morimoto, Tatsuto; Ota, Kei; Marumoto, Shinsuke; Hashizume, Daisuke; Matsuo, Tsukasa; International Journal of Molecular Sciences 25 (2024) 3761–; doi:10.3390/ijms25073761

data_1571395
_publ_section_title
;
 Approach to the &#x201C;Missing&#x201D; Diarylsilylene: Formation,
 Characterization, and Intramolecular C--H Bond Activation of Blue
 Diarylsilylenes with Bulky Rind Groups
;
_journal_issue                   7
_journal_name_full               'International Journal of Molecular Sciences'
_journal_page_first              3761
_journal_paper_doi               10.3390/ijms25073761
_journal_volume                  25
_journal_year                    2024
_chemical_formula_moiety         'C56 H90 Si'
_chemical_formula_sum            'C56 H90 Si'
_chemical_formula_weight         791.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 104.756(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.720(7)
_cell_length_b                   18.594(4)
_cell_length_c                   16.662(4)
_cell_measurement_reflns_used    14839
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.36
_cell_measurement_theta_min      1.90
_cell_volume                     9803(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    SIR2008
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724+'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40049
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.672
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.9929
_exptl_absorpt_correction_T_min  0.9813
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description       block
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.709
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         11249
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0757
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+14.2765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1823
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8955
_reflns_number_total             11249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CrystalA.cif
_cod_data_source_block           Eind-Silylene
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1571395
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.977
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              53818
_shelx_hkl_checksum              15611