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_1571394
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                84.557(5)
_cell_angle_beta                 85.566(5)
_cell_angle_gamma                78.612(5)
_cell_formula_units_Z            2
_cell_length_a                   10.1298(6)
_cell_length_b                   10.1400(6)
_cell_length_c                   24.4558(13)
_cell_measurement_reflns_used    3522
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.5790
_cell_measurement_theta_min      2.0460
_cell_volume                     2447.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 39.46e (release 04-06-2018))'
_computing_data_reduction        'CrysAlisPro 1.171.43.109a (Rigaku OD, 2024)'
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    SHELXT-2018/2
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.1584
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20736
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.265
_diffrn_reflns_theta_min         2.055
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.109a (Rigaku Oxford Diffraction, 2024)
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_density_diffrn    1.074
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         11460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1496
_refine_ls_R_factor_gt           0.0768
_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^)+(0.0588P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1630
_refine_ls_wR_factor_ref         0.1914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6257
_reflns_number_total             11460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CrystalB.cif
_cod_data_source_block           Cyclic
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/MDPI/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               1571394
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              38279
_shelx_hkl_checksum              74130