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

data_7710515
_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     SiClC4(C6H5)2(Si(CH3)3)2(C6H5)
_chemical_formula_sum            'C28 H33 Cl Si3'
_chemical_formula_weight         489.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 118.1815(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5478(8)
_cell_length_b                   6.5819(2)
_cell_length_c                   22.2436(8)
_cell_measurement_reflns_used    9290
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.08
_cell_measurement_theta_min      2.17
_cell_volume                     2780.74(17)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            112810
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.971
_diffrn_reflns_theta_min         1.811
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  0.9863
_exptl_absorpt_correction_T_min  0.9251
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         12238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0450P)^2^+0.7500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9877
_reflns_number_total             12238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01446g3.cif
_cod_data_source_block           ww144
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7710515
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.896
_shelx_estimated_absorpt_t_max   0.978
_exptl_absorpt_special_details
;
 numerical absorption correction followed by correction based on
 symmetry-related measurements (multi-scan)
;
_shelx_res_checksum              28575