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

data_7251207
_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         'C2 H3 F3 N O, As F6, F2 Xe'
_chemical_formula_sum            'C2 H3 As F11 N O Xe'
_chemical_formula_weight         472.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-08-29
_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                 99.4517(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.41785(9)
_cell_length_b                   9.84875(11)
_cell_length_c                   14.90113(17)
_cell_measurement_reflns_used    59909
_cell_measurement_temperature    100.00(12)
_cell_measurement_theta_max      38.9280
_cell_measurement_theta_min      2.2760
_cell_volume                     1073.85(2)
_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(12)
_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 1.000
_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     17.00  90.00   0.50   17.00    --   28.36  57.00-180.00  146
  2  \w      9.00  85.00   0.50   17.00    --   28.36  77.00  90.00  152
  3  \w     17.00  91.00   0.50   17.00    --   28.36  57.00  90.00  148
  4  \w     22.00  91.00   0.50   17.00    --   28.36  57.00   0.00  138
  5  \w     10.00  83.00   0.50   17.00    --   28.36  77.00   0.00  146
  6  \w     21.00  82.00   0.50   17.00    --   28.36  57.00 -60.00  122
  7  \w      7.00  85.00   0.50   17.00    --   28.36  77.00-150.00  156
  8  \w    -51.00  27.00   0.50   17.00    --  -29.30  77.00-180.00  156
  9  \w    -51.00 -21.00   0.50   17.00    --  -29.30  77.00  45.98   60
 10  \w    -84.00 -11.00   0.50   17.00    --  -29.30 -77.00-120.00  146
 11  \w    -51.00  27.00   0.50   17.00    --  -29.30  77.00  90.00  156
 12  \w    -50.00 -23.00   0.50   17.00    --  -29.30 -41.00  36.82   54
 13  \w    -87.00 -57.00   0.50   17.00    --  -29.30 -41.00  36.82   60
 14  \w    -51.00  27.00   0.50   17.00    --  -29.30  77.00 -60.00  156
 15  \w    -51.00  21.00   0.50   17.00    --  -29.30  77.00-150.00  144
 16  \w     -6.00  26.00   0.50   17.00    --  -29.30  77.00  45.98   64
 17  \w    -51.00 -16.00   0.50   17.00    --  -29.30  77.00  30.00   70
 18  \w    -13.00  23.00   0.50   17.00    --  -29.30  77.00  30.00   72
 19  \w    -51.00  27.00   0.50   17.00    --  -29.30  77.00  -4.57  156
 20  \w    -51.00  24.00   0.50   17.00    --  -29.30  77.00 120.00  150
 21  \w    -52.00  21.00   0.50   17.00    --  -29.30  80.00-103.55  146
;
_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      -0.0461208000
_diffrn_orient_matrix_UB_12      0.0382338000
_diffrn_orient_matrix_UB_13      0.0122816000
_diffrn_orient_matrix_UB_21      -0.0513532000
_diffrn_orient_matrix_UB_22      -0.0407432000
_diffrn_orient_matrix_UB_23      0.0026675000
_diffrn_orient_matrix_UB_31      0.0329113000
_diffrn_orient_matrix_UB_32      -0.0100257000
_diffrn_orient_matrix_UB_33      0.0359414000
_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  0.0947
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            100779
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         34.115
_diffrn_reflns_theta_min         1.964
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    3.386
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.504
_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    2.921
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.591
_refine_diff_density_min         -1.948
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         8994
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.002
_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^+0.6744P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7982
_reflns_number_total             8994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00956a2.cif
_cod_data_source_block           f3cc(oh)nh2_xef2_as_2
_cod_database_code               7251207
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C2 H3 As F11 N O Xe'
_chemical_oxdiff_usercomment     'EU, 100 K, LT mounting'
_shelx_estimated_absorpt_t_max   0.773
_shelx_estimated_absorpt_t_min   0.497
_olex2_refinement_description
;
1. Restrained distances
 F1A-C2 \\sim F1B-C2
 with sigma of 0.005
 F2A-C2 \\sim F2B-C2
 with sigma of 0.001
 C2-F3A \\sim C2-F3B
 with sigma of 0.001
 F1A-F2A \\sim F1B-F2B
 with sigma of 0.04
 F1A-C1 \\sim F1B-C1
 with sigma of 0.04
 F1A-F3A \\sim F1B-F3B
 with sigma of 0.01
 F2A-C1 \\sim F2B-C1
 with sigma of 0.005
 F2A-F3A \\sim F2B-F3B
 with sigma of 0.04
 C1-F3A \\sim C1-F3B
 with sigma of 0.04
2. Rigid body (RIGU) restrains
 C2, F1B, F2B, F3B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2, F1A, F2A, F3A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
;
_shelx_res_checksum              40033
_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 1.368
_oxdiff_exptl_absorpt_empirical_full_min 0.750