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

data_7251204
_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 H2 F7 N O'
_chemical_formula_sum            'C4 H2 F7 N O'
_chemical_formula_weight         213.07
_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             2025-08-28
_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                95.467(2)
_cell_angle_beta                 91.890(3)
_cell_angle_gamma                105.584(3)
_cell_formula_units_Z            2
_cell_length_a                   5.11713(18)
_cell_length_b                   5.27137(14)
_cell_length_c                   12.7768(3)
_cell_measurement_reflns_used    4498
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.4590
_cell_measurement_theta_min      3.4820
_cell_volume                     329.848(17)
_computing_cell_refinement       'CrysAlisPro 1.171.44.117a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.111a 64-bit (release 13-05-2025))'
_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      100.00(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 0.988
_diffrn_measured_fraction_theta_max 0.972
_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     48.00  98.00   0.50    0.10    --  104.00 -77.00-120.00  100
  2  \w     83.00 118.00   0.50    0.10    --  104.00 -80.00  14.61   70
  3  \w     48.00  78.00   0.50    0.10    --  104.00 -80.00  14.61   60
  4  \w     48.00  74.00   0.50    0.10    --  104.00 -80.00  90.95   52
  5  \w     48.00  75.00   0.50    0.10    --  104.00 -77.00 120.00   54
  6  \w     87.00 116.00   0.50    0.10    --  104.00 -80.00  90.95   58
  7  \w     54.00  80.00   0.50    0.10    --  104.00 -77.00  30.00   52
  8  \w     49.00  87.00   0.50    0.10    --  104.00 -77.00  60.00   76
  9  \w     48.00  73.00   0.50    0.10    --  104.00 -77.00   0.00   50
 10  \w     48.00  73.00   0.50    0.10    --  104.00 -77.00 150.00   50
 11  \w     57.00  89.00   0.50    0.10    --  104.00 -77.00 -60.00   64
 12  \w     50.00  96.00   0.50    0.10    --  104.00 -77.00 -30.00   92
 13  \w     54.00  97.00   0.50    0.10    --  104.00 -77.00 -90.00   86
 14  \w     54.00  87.00   0.50    0.10    --  104.00 -77.00-150.00   66
 15  \w     48.00  86.00   0.50    0.10    --  104.00 -77.00-180.00   76
 16  \w    139.00 165.00   0.50    0.10    --  104.00  45.00 -60.00   52
 17  \w    131.00 157.00   0.50    0.10    --  104.00  77.00 -60.00   52
 18  \w     88.00 116.00   0.50    0.10    --  104.00  77.00 -60.00   56
 19  \w     86.00 129.00   0.50    0.10    --  104.00  77.00 -90.00   86
 20  \w    134.00 159.00   0.50    0.10    --  104.00  77.00-180.00   50
 21  \w     86.00 117.00   0.50    0.10    --  104.00  77.00-180.00   62
 22  \w     85.00 160.00   0.50    0.10    --  104.00  77.00 -30.00  150
 23  \w    128.00 160.00   0.50    0.10    --  104.00  77.00-120.00   64
 24  \w    131.00 158.00   0.50    0.10    --  104.00  77.00  60.00   54
 25  \w    134.00 159.00   0.50    0.10    --  104.00  77.00 120.00   50
 26  \w     88.00 159.00   0.50    0.10    --  104.00  77.00 150.00  142
 27  \w     89.00 115.00   0.50    0.10    --  104.00  77.00 120.00   52
 28  \w    102.00 128.00   0.50    0.10    --  104.00  77.00  60.00   52
 29  \w    118.00 161.00   0.50    0.10    --  104.00  77.00  90.00   86
 30  \w    127.00 159.00   0.50    0.10    --  104.00  77.00   0.00   64
 31  \w     84.00 118.00   0.50    0.10    --  104.00  77.00   0.00   68
 32  \w     84.00 111.00   0.50    0.10    --  104.00  77.00  90.00   54
 33  \w    132.00 157.00   0.50    0.10    --  104.00  75.00  49.50   50
 34  \w     97.00 134.00   0.50    0.10    --  104.00  77.00  30.00   74
 35  \w     96.00 122.00   0.50    0.10    --  104.00  75.00  49.50   52
 36  \w     92.00 119.00   0.50    0.10    --  104.00  61.00  30.00   54
 37  \w     97.00 127.00   0.50    0.10    --  104.00  61.00 150.00   60
 38  \w    127.00 161.00   0.50    0.10    --  104.00  77.00-150.00   68
 39  \w     96.00 121.00   0.50    0.10    --  104.00  61.00-150.00   50
 40  \w     86.00 117.00   0.50    0.10    --  104.00  77.00-150.00   62
 41  \w     83.00 119.00   0.50    0.10    --  104.00  77.00-120.00   72
 42  \w     93.00 120.00   0.50    0.10    --  104.00  61.00 -90.00   54
 43  \w    139.00 165.00   0.50    0.10    --  104.00  45.00-180.00   52
 44  \w    142.00 171.00   0.50    0.10    --  104.00  45.00-150.00   58
 45  \w    128.00 165.00   0.50    0.10    --  104.00  61.00 -90.00   74
 46  \w    101.00 129.00   0.50    0.10    --  104.00  61.00   0.00   56
 47  \w    132.00 165.00   0.50    0.10    --  104.00  61.00  30.00   66
 48  \w    119.00 161.00   0.50    0.10    --  104.00  45.00 120.00   84
 49  \w     37.00  65.00   0.50    0.05    --   48.06  57.00 120.00   56
 50  \w     27.00  60.00   0.50    0.05    --   48.06  77.00 120.00   66
 51  \w     31.00  57.00   0.50    0.05    --   48.06  77.00  60.00   52
 52  \w     28.00  54.00   0.50    0.05    --   48.06  77.00   0.00   52
 53  \w     28.00  60.00   0.50    0.05    --   48.06  77.00 -30.00   64
 54  \w     38.00  63.00   0.50    0.05    --   48.06  57.00 -60.00   50
 55  \w     27.00  81.00   0.50    0.05    --   48.06  77.00 -90.00  108
 56  \w     41.00  67.00   0.50    0.05    --   48.06  57.00-120.00   52
 57  \w     29.00  58.00   0.50    0.05    --   48.06  77.00-180.00   58
 58  \w     81.00 106.00   0.50    0.05    --   48.06  57.00-120.00   50
 59  \w     38.00  76.00   0.50    0.05    --   48.06  57.00  30.00   76
 60  \w    -69.00 -10.00   0.50    0.05    --  -48.06  77.00 -60.00  118
 61  \w    -41.00   4.00   0.50    0.05    --  -48.06  57.00   0.00   90
 62  \w    -69.00   8.00   0.50    0.05    --  -48.06  77.00  60.00  154
 63  \w    -48.00 -22.00   0.50    0.10    --  -82.50  45.00 -30.00   52
 64  \w    -69.00 -37.00   0.50    0.10    --  -82.50  61.00 -60.00   64
 65  \w    -54.00 -25.00   0.50    0.10    --  -82.50  45.00-120.00   58
 66  \w   -113.00 -74.00   0.50    0.05    --  -48.06 -41.00 -96.38   78
 67  \w    -72.00 -45.00   0.50    0.05    --  -48.06 -41.00 -96.38   54
 68  \w    -87.00 -61.00   0.50    0.10    --  -82.50 -77.00 -30.00   52
 69  \w    -91.00 -65.00   0.50    0.10    --  -82.50 -77.00 -60.00   52
 70  \w    -91.00 -65.00   0.50    0.10    --  -82.50 -77.00-150.00   52
 71  \w    -96.00 -64.00   0.50    0.10    --  -82.50 -77.00  30.00   64
 72  \w    -88.00 -61.00   0.50    0.10    --  -82.50 -77.00  90.00   54
 73  \w   -111.00 -61.00   0.50    0.10    --  -82.50 -77.00 120.00  100
 74  \w    -96.00 -71.00   0.50    0.10    --  -82.50 -77.00 150.00   50
 75  \w    -53.00 -27.00   0.50    0.05    --  -48.06 -77.00 150.00   52
 76  \w    -97.00 -66.00   0.50    0.10    --  -82.50 -77.00  60.00   62
 77  \w    -89.00 -64.00   0.50    0.10    --  -82.50 -72.00 163.58   50
 78  \w    -95.00 -69.00   0.50    0.10    --  -82.50 -64.00  59.49   52
 79  \w    -97.00 -63.00   0.50    0.10    --  -82.50 -77.00   0.00   68
 80  \w    -90.00 -64.00   0.50    0.10    --  -82.50 -73.00 -90.50   52
 81  \w   -126.00-100.00   0.50    0.10    --  -82.50 -73.00 -90.50   52
 82  \w    -99.00 -73.00   0.50    0.10    --  -82.50 -61.00-120.00   52
 83  \w    -95.00 -69.00   0.50    0.10    --  -82.50 -61.00-150.00   52
 84  \w    -94.00 -69.00   0.50    0.10    --  -82.50 -61.00-180.00   50
;
_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      -0.0062864000
_diffrn_orient_matrix_UB_12      -0.2155282000
_diffrn_orient_matrix_UB_13      -0.0911293000
_diffrn_orient_matrix_UB_21      0.1446853000
_diffrn_orient_matrix_UB_22      0.2148746000
_diffrn_orient_matrix_UB_23      -0.0683112000
_diffrn_orient_matrix_UB_31      0.2776332000
_diffrn_orient_matrix_UB_32      -0.0228230000
_diffrn_orient_matrix_UB_33      0.0418987000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6558
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.025
_diffrn_reflns_theta_min         3.482
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.622
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.425
_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    2.145
_exptl_crystal_description       plank
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0043(11)
_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   1.058
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.1316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1292
_reflns_number_total             1342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00956a2.cif
_cod_data_source_block           pfba_2_1_new
_cod_original_cell_volume        329.847(18)
_cod_database_code               7251204
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C4 H2 N O F7'
_chemical_oxdiff_usercomment     '100 K, LT, EU'
_shelx_estimated_absorpt_t_max   0.880
_shelx_estimated_absorpt_t_min   0.269
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name pfba_2.par
_olex2_refinement_description
;
;
_shelx_res_checksum              31514
_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 1.198
_oxdiff_exptl_absorpt_empirical_full_min 0.775