HF-addition to haloacetyl fluorides in superacidic media
Steiner, Sebastian; Shafiq, Zurwa M.; Nitzer, Alexander; Hollenwäger, Dirk; Kornath, Andreas J.; New Journal of Chemistry 48 (2024) 13846–13853; doi:10.1039/D4NJ02884H

data_7063352
_publ_section_title
;
 HF-addition to haloacetyl fluorides in superacidic media
;
_journal_issue                   31
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13846
_journal_page_last               13853
_journal_paper_doi               10.1039/D4NJ02884H
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C2 H4 F4 O, F6 Sb'
_chemical_formula_sum            'C2 H3 F10 O Sb'
_chemical_formula_weight         354.79
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive,Oxygen-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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-12-08
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-12-07 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                85.971(5)
_cell_angle_beta                 87.605(6)
_cell_angle_gamma                85.482(6)
_cell_formula_units_Z            2
_cell_length_a                   6.3267(5)
_cell_length_b                   7.8117(5)
_cell_length_c                   8.5217(5)
_cell_measurement_reflns_used    2881
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2130
_cell_measurement_theta_min      2.6060
_cell_volume                     418.54(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics
'ORTEP-3, Version ORTEP-III (1.0.3), L. J. Farrugia, J. Appl. Cryst. (2012),45, 849-854'
_computing_publication_material
'PLATON (A.L.Spek, Acta Cryst. 2009, D65, 148-155.) '
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
'SHELXT (Sheldrick, G. M. (2015). Acta Cryst. A71, 3-8.)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    0.5
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8217
_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         30.507
_diffrn_reflns_theta_min         2.398
_diffrn_source_current           40
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             328
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Anhydrous Hydrogen Fluoride'
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.118
_refine_diff_density_max         1.199
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2548
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0173P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2248
_reflns_number_total             2548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj02884h2.cif
_cod_data_source_block           xh063
_cod_depositor_comments          'Adding full bibliography for 7063352.cif.'
_cod_database_code               7063352
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.360
_shelx_estimated_absorpt_t_max   0.687
_oxdiff_exptl_absorpt_empirical_full_min 0.817
_oxdiff_exptl_absorpt_empirical_full_max 1.581
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              81698