A neutral crystalline imino-substituted silyl radical.
Kiefer, Fiona J.; Kostenko, Arseni; Holzner, Richard; Inoue, Shigeyoshi; Chemical communications (Cambridge, England) 60 (2024) 8577–8580; doi:10.1039/d4cc02167c

data_7133310
_publ_section_title
;
 A neutral crystalline imino-substituted silyl radical.
;
_journal_issue                   65
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8577
_journal_page_last               8580
_journal_paper_doi               10.1039/d4cc02167c
_journal_volume                  60
_journal_year                    2024
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C29 H62 N3 Si3'
_chemical_formula_sum            'C29 H62 N3 Si3'
_chemical_formula_weight         537.09
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2024-07-05 deposited with the CCDC.	2024-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                69.558(3)
_cell_angle_beta                 80.011(3)
_cell_angle_gamma                82.655(3)
_cell_formula_units_Z            4
_cell_length_a                   11.5884(10)
_cell_length_b                   17.2210(16)
_cell_length_c                   18.5360(17)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.4251
_cell_measurement_theta_min      2.2783
_cell_volume                     3404.5(5)
_computing_cell_refinement       'SAINT (Bruker, 2017)'
_computing_data_collection       'APEX III Control Software (Bruker, 2016)'
_computing_data_reduction        'SAINT (Bruker, 2017)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'
_computing_structure_refinement
'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  ' Apex II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'Triumph monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            119802
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5, Bruker, 2014'
_exptl_crystal_colour            'clear red-orange'
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.332
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.138
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         12891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0254P)^2^+3.6880P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                11639
_reflns_number_total             12891
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d4cc02167c2.cif
_cod_data_source_block           holri25_0m-auto
_cod_depositor_comments          'Adding full bibliography for 7133310.cif.'
_cod_original_cell_volume        3404.6(5)
_cod_database_code               7133310
_shelx_res_checksum              83952
_shelx_hkl_checksum              73591