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

data_7251211
_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         'C3 H3 F5 N O, As F6, F2 Xe'
_chemical_formula_sum            'C3 H3 As F13 N O Xe'
_chemical_formula_weight         522.28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-10-02
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.67561(10)
_cell_length_b                   31.0125(4)
_cell_length_c                   8.65174(9)
_cell_measurement_reflns_used    40781
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.4070
_cell_measurement_theta_min      1.9660
_cell_volume                     2327.77(5)
_computing_cell_refinement       'CrysAlisPro 1.171.44.117a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.120a 64-bit (release 22-08-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.117a (Rigaku OD, 2025)'
_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 0.940
_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    -54.00  11.00   0.50    5.00    --   -0.38 -57.00   0.00  130
  2  \w    -22.00  46.00   0.50    5.00    --   -0.38  77.00  90.00  136
  3  \w     17.00  43.00   0.50    5.00    --   -2.00  66.00 147.29   52
  4  \w    -64.00   8.00   0.50    5.00    --    2.00 -42.00  52.20  144
  5  \w    -27.00   8.00   0.50    5.00    --    2.00 -41.00 -96.68   70
  6  \w    -18.00  50.00   0.50    5.00    --   -2.00  63.00-170.89  136
  7  \w    -64.00 -28.00   0.50    5.00    --    2.00 -42.00-174.61   72
  8  \w    -61.00   8.00   0.50    5.00    --    2.00 -41.00 105.23  138
  9  \w    -22.00   8.00   0.50    5.00    --    2.00 -42.00-174.61   60
 10  \w    -56.00 -30.00   0.50    5.00    --    2.00 -41.00 -96.68   52
 11  \w    -19.00   9.00   0.50    5.00    --   -2.00  66.00 147.29   56
 12  \w    -19.00  27.00   0.50    5.00    --   -2.00  66.00 -10.78   92
 13  \w     33.00  58.00   0.50    5.00    --   -2.00  66.00 -10.78   50
 14  \w    -24.00  21.00   0.50    5.00    --   -2.00  78.00-104.26   90
 15  \w     35.00  62.00   0.50    5.00    --   -2.95  21.00  74.37   54
 16  \w    -12.00  14.00   0.50    5.00    --   -2.95  19.00 150.00   52
 17  \w     42.00  68.00   0.50    5.00    --   -2.95  19.00 150.00   52
 18  \w    -12.00  37.00   0.50    5.00    --   -2.95  19.00 120.00   98
 19  \w    -12.00  26.00   0.50    5.00    --   -2.95  19.00  30.00   76
 20  \w     40.00  66.00   0.50    5.00    --   -2.95  19.00  30.00   52
 21  \w    -12.00  56.00   0.50    5.00    --   -2.95  19.00 -30.00  136
 22  \w    -69.00  48.00   0.50    5.00    --   -2.95   0.00 -90.00  234
 23  \w    -12.00  28.00   0.50    5.00    --   -2.95  21.00  74.37   80
 24  \w    -65.00  55.00   0.50    5.00    --    2.32   0.00  60.00  240
 25  \w    -65.00  55.00   0.50    5.00    --    2.32   0.00 -90.00  240
;
_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      0.0319349000
_diffrn_orient_matrix_UB_12      -0.0111372000
_diffrn_orient_matrix_UB_13      0.0395130000
_diffrn_orient_matrix_UB_21      -0.0412549000
_diffrn_orient_matrix_UB_22      -0.0132625000
_diffrn_orient_matrix_UB_23      -0.0144933000
_diffrn_orient_matrix_UB_31      0.0378994000
_diffrn_orient_matrix_UB_32      -0.0050482000
_diffrn_orient_matrix_UB_33      -0.0490763000
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            111431
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         30.759
_diffrn_reflns_theta_min         1.852
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    3.146
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.458
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.117a (Rigaku Oxford Diffraction, 2025)
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    2.981
_exptl_crystal_description       plate
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.00014(4)
_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   1.039
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         6484
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0175
_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^)+(0.0141P)^2^+0.6274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0362
_refine_ls_wR_factor_ref         0.0381
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.937
_reflns_number_gt                5368
_reflns_number_total             6484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00956a2.cif
_cod_data_source_block           pfpah_xef2_3_eu
_cod_original_cell_volume        2327.77(4)
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               7251211
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C3 As Xe N O F13'
_chemical_oxdiff_usercomment     '100 K, EU, LT mount'
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.484
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name pfpaH_XeF2_3.par
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.423(18)
 0.099(11) 0.357(10) 0.121(11)
;
_shelx_res_checksum              83365
_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 1.338
_oxdiff_exptl_absorpt_empirical_full_min 0.820