Covalent triflates as synthons for silolyl- and germolyl cations
Wohltmann, Wiebke Marie; Schmidtmann, Marc; Müller, Thomas; Dalton Transactions  (2022) –; doi:10.1039/D2DT01446G

data_7710516
_publ_section_title
;
 Covalent triflates as synthons for silolyl- and germolyl cations
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01446G
_journal_year                    2022
_chemical_formula_structural
'[SiC4(C6H5)2(Si(CH3)3)2(OP(C2H5)3)(C6H5)] [CF3SO3] *C6D6'
_chemical_formula_sum            'C41 H48 D6 F3 O4 P S Si3'
_chemical_formula_weight         821.18
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-05-03 deposited with the CCDC.	2022-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                113.086(2)
_cell_angle_beta                 90.170(2)
_cell_angle_gamma                92.016(3)
_cell_formula_units_Z            4
_cell_length_a                   11.0788(5)
_cell_length_b                   20.4400(10)
_cell_length_c                   20.8154(9)
_cell_measurement_reflns_used    5539
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.62
_cell_measurement_theta_min      2.35
_cell_volume                     4332.8(4)
_computing_cell_refinement       'Bruker SAINT V8.40B'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.947
_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_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44671
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.495
_diffrn_reflns_theta_min         2.308
_diffrn_source                   'I\mS microfocus'
_exptl_absorpt_coefficient_mu    2.233
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.873877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS-2012/1 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       plate
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         44671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0777
_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^)+(0.0500P)^2^+11.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.1972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                36780
_reflns_number_total             44671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01446g3.cif
_cod_data_source_block           ww151_5
_cod_database_code               7710516
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.957
_shelx_res_checksum              11423