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

data_7251205
_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, C2 H3 F3 N O'
_chemical_formula_sum            'C2 H3 As F9 N O'
_chemical_formula_weight         302.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-08-27
_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                 98.6498(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.81910(18)
_cell_length_b                   7.90095(13)
_cell_length_c                   20.5015(4)
_cell_measurement_reflns_used    30480
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      29.7620
_cell_measurement_theta_min      2.1040
_cell_volume                     1572.42(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.119a 64-bit (release 08-04-2024))'
_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(11)
_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 0.898
_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     34.00  64.00   0.50   35.00    --   -0.51  41.00-131.19   60
  2  \w    -17.00  28.00   0.50   35.00    --   -0.51  64.00 140.64   90
  3  \w    -17.00  40.00   0.50   35.00    --   -0.51  64.00   7.74  114
  4  \w    -14.00  58.00   0.50   35.00    --   -0.51  58.00 -30.46  144
  5  \w     -7.00  27.00   0.50   35.00    --   -0.51  42.00 -52.17   68
  6  \w    -25.00  21.00   0.50   35.00    --   -0.51 -77.00 -60.00   92
  7  \w    -51.00  21.00   0.50   35.00    --   -0.51 -77.00-120.00  144
  8  \w    -22.00  56.00   0.50   35.00    --   -0.51  77.00  30.00  156
  9  \w    -49.00  21.00   0.50   35.00    --   -0.51 -77.00  60.00  140
 10  \w     -7.00  22.00   0.50   35.00    --   -0.51  42.00-110.61   58
 11  \w     36.00  66.00   0.50   35.00    --   -0.51  42.00-110.61   60
 12  \w    -60.00   6.00   0.50   35.00    --   -0.51 -41.00 126.62  132
 13  \w    -33.00  21.00   0.50   35.00    --   -0.51 -77.00-180.00  108
 14  \w     -7.00  27.00   0.50   35.00    --   -0.51  41.00-131.19   68
;
_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      -0.0252806000
_diffrn_orient_matrix_UB_12      0.0613494000
_diffrn_orient_matrix_UB_13      -0.0083151000
_diffrn_orient_matrix_UB_21      0.0056705000
_diffrn_orient_matrix_UB_22      0.0219292000
_diffrn_orient_matrix_UB_23      0.0262151000
_diffrn_orient_matrix_UB_31      0.0514658000
_diffrn_orient_matrix_UB_32      0.0277364000
_diffrn_orient_matrix_UB_33      -0.0023293000
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            80745
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         30.045
_diffrn_reflns_theta_min         2.113
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    2.354
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.845
_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    2.560
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.120
_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     277
_refine_ls_number_reflns         8411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0424P)^2^+0.5963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6219
_reflns_number_total             8411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00956a2.cif
_cod_data_source_block           f3cc(oh)nh2_as_iii_2
_cod_database_code               7251205
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C2 F9 N O As H3 '
_chemical_oxdiff_usercomment     '100 K, EU, LT mounting'
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.782
_olex2_refinement_description
;
;
_shelx_res_checksum              10967
_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 1.133
_oxdiff_exptl_absorpt_empirical_full_min 0.887