A Bis(silylene)silole - synthesis, properties and reactivity.
Liu, Chenghuan; Schmidtmann, Marc; Müller, Thomas; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10446–10452; doi:10.1039/d4dt01112k

data_7716218
_publ_section_title
;
 A Bis(silylene)silole - synthesis, properties and reactivity.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10446
_journal_page_last               10452
_journal_paper_doi               10.1039/d4dt01112k
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_structural
'SiC4(C6H5)2(Si(CH3)3)2(SiTe(C15H23N2))2 *O(C2H5)2'
_chemical_formula_sum            'C56 H84 N4 O Si5 Te2'
_chemical_formula_weight         1224.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-04-30 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3105(6)
_cell_length_b                   15.4573(6)
_cell_length_c                   30.3266(12)
_cell_measurement_reflns_used    9648
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.55
_cell_measurement_theta_min      4.08
_cell_volume                     6239.5(4)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Photon III CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            103794
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.489
_diffrn_reflns_theta_min         2.914
_diffrn_source                   'I\mS microfocus'
_exptl_absorpt_coefficient_mu    8.586
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       plate
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 5324 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0136(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         12768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0269
_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^)+(0.0400P)^2^+1.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12347
_reflns_number_total             12768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01112k3.cif
_cod_data_source_block           lch_1017si2te
_cod_depositor_comments
'Adding full bibliography for 7716218--7716222.cif.'
_cod_database_code               7716218
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.426
_shelx_estimated_absorpt_t_max   0.919
_shelx_res_checksum              56902