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

data_7251210
_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'
_chemical_formula_sum            'C3 H3 As F11 N O'
_chemical_formula_weight         352.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.12957(13)
_cell_length_b                   25.2768(4)
_cell_length_c                   9.34322(16)
_cell_measurement_reflns_used    41325
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      30.4860
_cell_measurement_theta_min      2.5400
_cell_volume                     1919.93(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 44.113a 64-bit (release 02-06-2025))'
_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      100.01(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 0.911
_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    -24.00  21.00   0.50    4.00    --   -2.00  78.00 -36.00   90
  2  \w    -23.00  52.00   0.50    4.00    --   -2.00  75.00  94.92  150
  3  \w    -18.00  11.00   0.50    4.00    --   -2.00  63.00 -97.29   58
  4  \w     16.00  59.00   0.50    4.00    --   -2.00  63.00 -97.29   86
  5  \w    -22.00  48.00   0.50    4.00    --   -2.00  73.00 172.90  140
  6  \w    -25.00   7.00   0.50    4.00    --   -2.00  80.00  75.38   64
  7  \w    -18.00  58.00   0.50    4.00    --   -2.00  63.00  16.54  152
  8  \w    -24.00  11.00   0.50    4.00    --   -2.00  78.00 -90.20   70
  9  \w    -25.00  21.00   0.50    4.00    --   -2.00  80.00 -58.46   92
 10  \w    -20.00  53.00   0.50    4.00    --   -2.00  68.00-149.85  146
 11  \w    -22.00  25.00   0.50    4.00    --   -2.00  73.00  44.53   94
 12  \w     28.00  54.00   0.50    4.00    --   -2.00  73.00  44.53   52
 13  \w    -18.00  58.00   0.50    4.00    --   -2.00  63.00 146.82  152
;
_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      -0.0082385000
_diffrn_orient_matrix_UB_12      -0.0215119000
_diffrn_orient_matrix_UB_13      0.0120857000
_diffrn_orient_matrix_UB_21      0.0563994000
_diffrn_orient_matrix_UB_22      -0.0046915000
_diffrn_orient_matrix_UB_23      -0.0318586000
_diffrn_orient_matrix_UB_31      0.0385779000
_diffrn_orient_matrix_UB_32      0.0022626000
_diffrn_orient_matrix_UB_33      0.0492079000
_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  0.0426
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            89392
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         30.591
_diffrn_reflns_theta_min         2.544
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    1.954
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.233
_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    2.442
_exptl_crystal_description       plate
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         5471
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+1.3549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4374
_reflns_number_total             5471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00956a2.cif
_cod_data_source_block           pfpah_asf6_2_1
_cod_database_code               7251210
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C3 F11 As N H3 O'
_chemical_oxdiff_usercomment     '100 K, EU, LT mount'
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.397
_olex2_refinement_description
;
1. Restrained distances
 C2-C3A \\sim C2-C3B
 with sigma of 0.005
 C2-F2A \\sim C2-F2B
 with sigma of 0.005
 C2-F1A \\sim C2-F1B
 with sigma of 0.005
 F5A-C3A \\sim F5B-C3B
 with sigma of 0.005
 F3A-C3A \\sim F3B-C3B
 with sigma of 0.005
 F1A-F2A \\sim F1B-F2B
 with sigma of 0.005
 F3A-F5A \\sim F3B-F5B
 with sigma of 0.005
 F4A-F5A \\sim F4B-F5B
 with sigma of 0.04
 F3A-F4A \\sim F3B-F4B
 with sigma of 0.04
 F4A-C3A \\sim F4B-C3B
 with sigma of 0.005
2. Rigid body (RIGU) restrains
 C3B, F3B, F4B, F5B
 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(C3B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(C3A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=FVAR(1)
;
_shelx_res_checksum              73670
_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 1.592
_oxdiff_exptl_absorpt_empirical_full_min 0.604