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

data_7251206
_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         'As F6, 2(C2 H2 F3 N O), H3 O'
_chemical_formula_sum            'C4 H7 As F12 N2 O3'
_chemical_formula_weight         434.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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            4
_cell_length_a                   11.5349(2)
_cell_length_b                   14.0649(3)
_cell_length_c                   7.78994(14)
_cell_measurement_reflns_used    17089
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1150
_cell_measurement_theta_min      3.7540
_cell_volume                     1263.82(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.115a 64-bit (release 15-03-2024))'
_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      100.00(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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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 -17.00   0.50    0.40    --  -82.50  45.00-180.00   74
  2  \w    -57.00 -18.00   0.50    0.40    --  -82.50  52.00-102.46   78
  3  \w    -47.00 -19.00   0.50    0.40    --  -82.50  45.00   0.00   56
  4  \w    -49.00 -23.00   0.50    0.40    --  -82.50  45.00  30.00   52
  5  \w    -54.00 -24.00   0.50    0.40    --  -82.50  45.00 113.54   60
  6  \w    -54.00 -24.00   0.50    0.40    --  -48.19  57.00 120.00   60
  7  \w    -20.00  15.00   0.50    0.40    --  -48.19  57.00 120.00   70
  8  \w    -57.00   2.00   0.50    0.40    --  -48.19  77.00  30.00  118
  9  \w    -65.00   7.00   0.50    0.40    --  -48.19  77.00 -60.00  144
 10  \w    -40.00   7.00   0.50    0.40    --  -48.19  57.00-150.00   94
 11  \w    -94.00 -42.00   0.50    0.40    --  -48.19 -41.00   9.50  104
 12  \w    -52.00 -27.00   0.50    0.40    --  -48.19 -77.00 120.00   50
 13  \w    -76.00 -27.00   0.50    0.40    --  -48.19 -77.00 150.00   98
 14  \w    -73.00 -28.00   0.50    0.40    --  -48.19 -77.00  90.00   90
 15  \w    -53.00 -27.00   0.50    0.40    --  -48.19 -77.00   0.00   52
 16  \w    -53.00 -27.00   0.50    0.40    --  -48.19 -77.00 -30.00   52
 17  \w    -53.00 -27.00   0.50    0.40    --  -48.19 -77.00 -60.00   52
 18  \w    -54.00 -27.00   0.50    0.40    --  -48.19 -77.00 -90.00   54
 19  \w   -105.00 -38.00   0.50    0.40    --  -48.19 -53.00 -63.24  134
 20  \w    -75.00 -42.00   0.50    0.40    --  -48.19 -42.00  74.18   66
 21  \w    -88.00 -43.00   0.50    0.40    --  -48.19 -42.00 -12.77   90
 22  \w    -66.00 -28.00   0.50    0.40    --  -48.19 -77.00-120.00   76
 23  \w    -53.00 -27.00   0.50    0.40    --  -48.19 -77.00-180.00   52
 24  \w    -66.00 -28.00   0.50    0.40    --  -48.19 -77.00-150.00   76
 25  \w    -93.00 -66.00   0.50    0.40    --  -82.50 -64.00-153.94   54
 26  \w    -87.00 -61.00   0.50    0.40    --  -82.50 -77.00 -90.00   52
 27  \w    -87.00 -61.00   0.50    0.40    --  -82.50 -77.00 -60.00   52
 28  \w    -87.00 -61.00   0.50    0.40    --  -82.50 -77.00 -71.21   52
 29  \w    -91.00 -61.00   0.50    0.40    --  -82.50 -77.00 -30.00   60
 30  \w    -87.00 -61.00   0.50    0.40    --  -82.50 -77.00   0.00   52
 31  \w    -87.00 -61.00   0.50    0.40    --  -82.50 -77.00  30.00   52
 32  \w    -87.00 -61.00   0.50    0.40    --  -82.50 -77.00  90.00   52
 33  \w    -89.00 -62.00   0.50    0.40    --  -82.50 -77.00 171.55   54
 34  \w    -87.00 -61.00   0.50    0.40    --  -82.50 -77.00 150.00   52
 35  \w    -89.00 -62.00   0.50    0.40    --  -82.50 -77.00 120.00   54
 36  \w    -87.00 -62.00   0.50    0.40    --  -82.50 -75.00 132.06   50
 37  \w    -88.00 -61.00   0.50    0.40    --  -82.50 -76.00  77.06   54
 38  \w    -88.00 -62.00   0.50    0.40    --  -82.50 -75.00  45.79   52
 39  \w    -90.00 -64.00   0.50    0.40    --  -82.50 -73.00  61.89   52
 40  \w    -89.00 -63.00   0.50    0.40    --  -82.50 -73.00 -24.81   52
 41  \w    -96.00 -63.00   0.50    0.40    --  -82.50 -72.00 -46.52   66
 42  \w    -88.00 -62.00   0.50    0.40    --  -82.50 -75.00-159.18   52
 43  \w    -87.00 -61.00   0.50    0.40    --  -82.50 -77.00-120.00   52
 44  \w    -89.00 -63.00   0.50    0.40    --  -82.50 -73.00-108.38   52
 45  \w   -139.00-102.00   0.50    0.40    --  -82.50 -72.00 -46.52   74
 46  \w    -90.00 -64.00   0.50    0.40    --  -82.50 -69.00  -0.17   52
 47  \w    -90.00 -63.00   0.50    0.40    --  -82.50 -71.00 101.55   54
 48  \w    -90.00 -64.00   0.50    0.40    --  -82.50 -69.00 176.80   52
 49  \w     28.00  54.00   0.50    0.40    --   48.19  77.00  30.00   52
 50  \w     38.00  63.00   0.50    0.40    --   48.19  57.00  60.00   50
 51  \w     27.00  53.00   0.50    0.40    --   48.19  77.00  90.00   52
 52  \w     41.00  69.00   0.50    0.40    --   48.19  57.00 150.00   56
 53  \w     84.00 124.00   0.50    0.40    --  104.00  77.00 120.00   80
 54  \w    125.00 161.00   0.50    0.40    --  104.00  77.00  90.00   72
 55  \w    131.00 160.00   0.50    0.40    --  104.00  77.00 120.00   58
 56  \w     84.00 117.00   0.50    0.40    --  104.00  77.00  90.00   66
 57  \w     83.00 113.00   0.50    0.40    --  104.00  77.00   0.00   60
 58  \w     83.00 109.00   0.50    0.40    --  104.00  77.00 -30.00   52
 59  \w     88.00 114.00   0.50    0.40    --  104.00  77.00 -90.00   52
 60  \w    125.00 159.00   0.50    0.40    --  104.00  77.00   0.00   68
 61  \w    118.00 161.00   0.50    0.40    --  104.00  77.00 -30.00   86
 62  \w    123.00 160.00   0.50    0.40    --  104.00  77.00  30.00   74
 63  \w     84.00 113.00   0.50    0.40    --  104.00  77.00  30.00   58
 64  \w    126.00 161.00   0.50    0.40    --  104.00  77.00 -60.00   70
 65  \w    135.00 161.00   0.50    0.40    --  104.00  77.00 -90.00   52
 66  \w     83.00 114.00   0.50    0.40    --  104.00  77.00 -60.00   62
 67  \w    135.00 161.00   0.50    0.40    --  104.00  77.00-150.00   52
 68  \w    132.00 161.00   0.50    0.40    --  104.00  77.00-120.00   58
 69  \w    129.00 160.00   0.50    0.40    --  104.00  77.00-180.00   62
 70  \w     84.00 121.00   0.50    0.40    --  104.00  77.00-180.00   74
 71  \w     85.00 115.00   0.50    0.40    --  104.00  77.00-150.00   60
 72  \w     84.00 110.00   0.50    0.40    --  104.00  77.00-120.00   52
 73  \w    129.00 159.00   0.50    0.40    --  104.00  77.00  60.00   60
 74  \w     84.00 110.00   0.50    0.40    --  104.00  77.00 150.00   52
 75  \w    131.00 161.00   0.50    0.40    --  104.00  77.00 150.00   60
 76  \w     91.00 160.00   0.50    0.40    --  104.00  61.00 120.00  138
 77  \w     85.00 121.00   0.50    0.40    --  104.00  77.00  60.00   72
 78  \w     92.00 122.00   0.50    0.40    --  104.00  61.00  60.00   60
 79  \w     94.00 121.00   0.50    0.40    --  104.00  61.00 -90.00   54
 80  \w     91.00 116.00   0.50    0.40    --  104.00  61.00-180.00   50
 81  \w     93.00 143.00   0.50    0.40    --  104.00  61.00-120.00  100
 82  \w    134.00 159.00   0.50    0.40    --  104.00  61.00-150.00   50
 83  \w    128.00 156.00   0.50    0.40    --  104.00  61.00 -90.00   56
 84  \w     91.00 132.00   0.50    0.40    --  104.00  61.00-150.00   82
 85  \w     90.00 156.00   0.50    0.40    --  104.00  61.00 -30.00  132
 86  \w    123.00 163.00   0.50    0.40    --  104.00  61.00   0.00   80
 87  \w    135.00 165.00   0.50    0.40    --  104.00  61.00  90.00   60
 88  \w     91.00 117.00   0.50    0.40    --  104.00  61.00  90.00   52
 89  \w     92.00 119.00   0.50    0.40    --  104.00  61.00   0.00   54
 90  \w    117.00 169.00   0.50    0.40    --  104.00  52.00  76.20  104
 91  \w    132.00 158.00   0.50    0.40    --  104.00  61.00  30.00   52
 92  \w     95.00 126.00   0.50    0.40    --  104.00  61.00  30.00   62
 93  \w    138.00 170.00   0.50    0.40    --  104.00  45.00 -60.00   64
 94  \w    140.00 171.00   0.50    0.40    --  104.00  45.00 -90.00   62
 95  \w    101.00 131.00   0.50    0.40    --  104.00  45.00 -60.00   60
 96  \w    103.00 134.00   0.50    0.40    --  104.00  45.00 -90.00   62
 97  \w    128.00 155.00   0.50    0.40    --  104.00  61.00-180.00   54
 98  \w    146.00 171.00   0.50    0.40    --  104.00  45.00-180.00   50
 99  \w    108.00 136.00   0.50    0.40    --  104.00  45.00-180.00   56
100  \w    137.00 168.00   0.50    0.40    --  104.00  45.00-120.00   62
101  \w    100.00 133.00   0.50    0.40    --  104.00  45.00  60.00   66
102  \w    137.00 169.00   0.50    0.40    --  104.00  45.00  60.00   64
103  \w    129.00 171.00   0.50    0.40    --  104.00  45.00 150.00   84
104  \w     81.00 110.00   0.50    0.40    --  104.00 -80.00 168.70   58
105  \w     53.00  79.00   0.50    0.40    --  104.00 -80.00  83.35   52
106  \w     48.00  75.00   0.50    0.40    --  104.00 -80.00 168.70   54
107  \w     90.00 123.00   0.50    0.40    --  104.00 -80.00  83.35   66
108  \w     86.00 113.00   0.50    0.40    --  104.00 -80.00 -49.84   54
109  \w     48.00  83.00   0.50    0.40    --  104.00 -80.00 -49.84   70
110  \w     50.00 104.00   0.50    0.40    --  104.00 -80.00-104.51  108
111  \w     47.00 103.00   0.50    0.40    --  104.00 -79.00-119.91  112
112  \w     51.00 101.00   0.50    0.40    --  104.00 -80.00 -93.87  100
113  \w     76.00 119.00   0.50    0.40    --  104.00 -80.00  21.32   86
114  \w     48.00  73.00   0.50    0.40    --  104.00 -80.00  21.32   50
115  \w     54.00  79.00   0.50    0.40    --  104.00 -77.00  30.00   50
116  \w     48.00  97.00   0.50    0.40    --  104.00 -77.00  60.00   98
117  \w     48.00  73.00   0.50    0.40    --  104.00 -77.00 120.00   50
118  \w     47.00  72.00   0.50    0.40    --  104.00 -78.00 150.05   50
119  \w     47.00 104.00   0.50    0.40    --  104.00 -79.00 130.22  114
120  \w     50.00  90.00   0.50    0.40    --  104.00 -77.00  90.00   80
121  \w     49.00  88.00   0.50    0.40    --  104.00 -77.00   0.00   78
122  \w     48.00  90.00   0.50    0.40    --  104.00 -77.00 -30.00   84
123  \w     48.00  73.00   0.50    0.40    --  104.00 -77.00 -60.00   50
124  \w     52.00  90.00   0.50    0.40    --  104.00 -77.00-150.00   76
125  \w     51.00  88.00   0.50    0.40    --  104.00 -77.00-180.00   74
;
_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      0.1063050620
_diffrn_orient_matrix_UB_12      0.0272625261
_diffrn_orient_matrix_UB_13      -0.1091518609
_diffrn_orient_matrix_UB_21      0.0760701728
_diffrn_orient_matrix_UB_22      0.0001865011
_diffrn_orient_matrix_UB_23      0.1625742241
_diffrn_orient_matrix_UB_31      0.0274701543
_diffrn_orient_matrix_UB_32      -0.1060690649
_diffrn_orient_matrix_UB_33      -0.0276859252
_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  0.0948
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            35878
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.209
_diffrn_reflns_theta_min         6.294
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.345
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.312
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         1378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0263P)^2^+4.0350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1202
_reflns_number_total             1378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00956a2.cif
_cod_data_source_block           (o)nh2_oh3_as_1_1
_cod_database_code               7251206
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C4 H7 As F12 N2 O3'
_chemical_oxdiff_usercomment     'EU, 100 K, LT mounting'
_shelx_estimated_absorpt_t_max   0.501
_shelx_estimated_absorpt_t_min   0.316
_olex2_refinement_description
;
;
_shelx_res_checksum              14162
_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 2.338
_oxdiff_exptl_absorpt_empirical_full_min 0.441