On the synthesis and structure of reactive halonium ions.
Fischer, Lukas; Lee, Michael H.; Wiesner, Anja; Müller, Carsten; Riedel, Sebastian; Chemical science 16 (2025) 13229–13234; doi:10.1039/d5sc03756e

data_1574896
_publ_section_title
;
 On the synthesis and structure of reactive halonium ions.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              13229
_journal_page_last               13234
_journal_paper_doi               10.1039/d5sc03756e
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'F30 O6 Sb Te6, C4 H4 Cl F6, 3(Cl F O2 S)'
_chemical_formula_sum            'C4 H4 Cl4 F39 O12 S3 Sb Te6'
_chemical_formula_weight         2110.40
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Heat-sensitive
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_method
;FinalCif V143 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-05-21 deposited with the CCDC.	2025-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                93.500(4)
_cell_angle_beta                 100.671(3)
_cell_angle_gamma                95.798(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8884(8)
_cell_length_b                   10.0411(8)
_cell_length_c                   22.687(2)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.506
_cell_measurement_theta_min      2.746
_cell_volume                     2195.0(3)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection
'Bruker BIS V6.2.18/2023-03-24 and APEX4 2022.1-1'
_computing_data_reduction        'SAINT V8.40B'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            63088
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.423
_diffrn_reflns_theta_min         2.110
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.40
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    5.133
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.0873
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: 
Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 
(2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.193
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.792
_exptl_crystal_size_mid          0.457
_exptl_crystal_size_min          0.402
_refine_diff_density_max         1.302
_refine_diff_density_min         -2.119
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         10988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+4.1358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10295
_reflns_number_total             10988
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
'The data was integrated as a 2-component twin.'
_twin_individual_id              2
_twin_individual_twin_matrix_11  -0.00056
_twin_individual_twin_matrix_12  -0.00014
_twin_individual_twin_matrix_13  0.99988
_twin_individual_twin_matrix_21  1.00004
_twin_individual_twin_matrix_22  -9e-05
_twin_individual_twin_matrix_23  0.00051
_twin_individual_twin_matrix_31  0.00077
_twin_individual_twin_matrix_32  1.00008
_twin_individual_twin_matrix_33  0.0007
_cod_data_source_file            d5sc03756e2.cif
_cod_data_source_block           LF427
_cod_depositor_comments
'Adding full bibliography for 1574893--1574896.cif.'
_cod_database_code               1574896
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.106
_shelx_estimated_absorpt_t_max   0.232
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              13175