Hydrogen-bonded salt cocrystals of xenon difluoride and protonated perfluoroamides
Uran, Erik; Lozinšek, Matic; CrystEngComm  (2025) –; doi:10.1039/D5CE00956A

data_7251208
_publ_section_title
;
 Hydrogen-bonded salt cocrystals of xenon difluoride and protonated
 perfluoroamides
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D5CE00956A
_journal_year                    2025
_chemical_formula_moiety         'C4 H3 F7 N O, C4 H2 F7 N O, As F6'
_chemical_formula_sum            'C8 H5 As F20 N2 O2'
_chemical_formula_weight         616.06
_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     iterative
_audit_creation_date             2025-09-01
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2025-10-03 deposited with the CCDC.	2025-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.5740(6)
_cell_angle_beta                 90.8760(6)
_cell_angle_gamma                103.0402(7)
_cell_formula_units_Z            2
_cell_length_a                   5.32051(4)
_cell_length_b                   10.45222(9)
_cell_length_c                   16.10170(12)
_cell_measurement_reflns_used    56836
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.0550
_cell_measurement_theta_min      1.9940
_cell_volume                     872.157(12)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 44.112a 64-bit (release 21-05-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_detector_type            'Eiger2 R CdTe 1M'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -55.00   3.00   0.50    1.00    --   -0.57 -19.00 -90.00  116
  2  \w    -63.00  46.00   0.50    1.00    --   -0.57   0.00 -90.00  218
  3  \w     -8.00  58.00   0.50    1.00    --   -0.57  19.00  90.00  132
  4  \w    -65.00   9.00   0.50    1.00    --   -0.57  -8.00   2.52  148
  5  \w    -28.00  10.00   0.50    1.00    --   -0.57  -8.00  40.59   76
  6  \w     -9.00  49.00   0.50    1.00    --   -0.57  19.00 150.00  116
  7  \w    -69.00   6.00   0.50    1.00    --   -0.57 -38.00 150.00  150
  8  \w    -19.00  31.00   0.50    1.00    --   -0.57 -99.00   0.00  100
  9  \w    -23.00  31.00   0.50    1.00    --   -0.57 -99.00  90.00  108
 10  \w    -23.00  29.00   0.50    1.00    --   -0.57 -99.00 -30.00  104
 11  \w    -22.00  25.00   0.50    1.00    --   -0.57 -99.00-120.00   94
 12  \w    -63.00  11.00   0.50    1.00    --   -0.57 -57.00 120.00  148
 13  \w    -22.00  56.00   0.50    1.00    --   -0.57  77.00 -30.00  156
 14  \w    -12.00  62.00   0.50    1.00    --   -0.57  57.00-180.00  148
 15  \w    -22.00  56.00   0.50    1.00    --   -0.57  77.00  60.00  156
 16  \w    -22.00  56.00   0.50    1.00    --   -0.57  77.00 120.00  156
 17  \w    -63.00  46.00   0.50    1.00    --   -0.57   0.00 -90.00  218
 18  \w    -22.00  56.00   0.50    1.00    --   -0.57  77.00-180.00  156
 19  \w    -22.00  56.00   0.50    1.00    --   -0.57  77.00-150.00  156
 20  \w    -57.00  21.00   0.50    1.00    --   -0.57 -77.00-120.00  156
 21  \w    -22.00  47.00   0.50    1.00    --   -0.57  77.00 -90.00  138
 22  \w    -22.00  56.00   0.50    1.00    --   -0.57  77.00-120.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku OD, XtaLAB Synergy-S, Dualflex, Eiger2 R CdTe 1M'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0493150000
_diffrn_orient_matrix_UB_12      0.0351593000
_diffrn_orient_matrix_UB_13      -0.0159187000
_diffrn_orient_matrix_UB_21      -0.0218514000
_diffrn_orient_matrix_UB_22      0.0195278000
_diffrn_orient_matrix_UB_23      0.0308856000
_diffrn_orient_matrix_UB_31      0.0934994000
_diffrn_orient_matrix_UB_32      0.0374321000
_diffrn_orient_matrix_UB_33      -0.0004553000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ag K\a'
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            99695
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         30.022
_diffrn_reflns_theta_min         1.856
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.184
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.144a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.346
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0048(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         9247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0258P)^2^+0.1772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8391
_reflns_number_total             9247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00956a2.cif
_cod_data_source_block           pfbah_hemi_2_1
_cod_original_cell_volume        872.156(12)
_cod_database_code               7251208
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'As F C H N O'
_chemical_oxdiff_usercomment     '100 K, EU, LT mount'
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.500
_olex2_refinement_description
;
;
_shelx_res_checksum              34534
_olex2_exptl_crystal_mounting_method 'MiTeGen loop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.260
_oxdiff_exptl_absorpt_empirical_full_min 0.837