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

data_7251202
_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, C4 H3 F7 N O'
_chemical_formula_sum            'C4 H3 As F13 N O'
_chemical_formula_weight         402.99
_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             2025-08-29
_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                 96.014(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.17592(15)
_cell_length_b                   7.94187(19)
_cell_length_c                   21.7914(5)
_cell_measurement_reflns_used    21436
_cell_measurement_temperature    100.02(18)
_cell_measurement_theta_max      29.7990
_cell_measurement_theta_min      2.1200
_cell_volume                     1062.95(4)
_computing_cell_refinement       'CrysAlisPro 1.171.44.117a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.120a 64-bit (release 22-08-2025))'
_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      100.02(18)
_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 0.990
_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    -31.00   8.00   0.50    1.50    --   -0.45 -57.00 150.00   78
  2  \w    -18.00  52.00   0.50    1.50    --   -2.00  63.00 -38.27  140
  3  \w     -4.00  22.00   0.50    1.50    --    2.00 -72.00  83.30   52
  4  \w    -18.00  47.00   0.50    1.50    --   -2.00  63.00 176.23  130
  5  \w    -23.00  46.00   0.50    1.50    --   -2.00  75.00-122.47  138
  6  \w    -54.00 -26.00   0.50    1.50    --    2.00 -72.00  83.30   56
  7  \w    -23.00  36.00   0.50    1.50    --   -2.00  75.00 125.15  118
  8  \w    -18.00  52.00   0.50    1.50    --   -2.00  64.00  -4.22  140
  9  \w    -25.00  12.00   0.50    1.50    --   -2.00  80.00  56.53   74
 10  \w     -8.00  62.00   0.50    1.50    --   -2.00  42.00-125.05  140
 11  \w    -18.00  39.00   0.50    1.50    --   -2.00  63.00 -71.68  114
 12  \w     -8.00  60.00   0.50    1.50    --   -2.00  42.00 108.43  136
;
_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      -0.0806965000
_diffrn_orient_matrix_UB_12      0.0323036000
_diffrn_orient_matrix_UB_13      -0.0041245000
_diffrn_orient_matrix_UB_21      -0.0416064000
_diffrn_orient_matrix_UB_22      -0.0590697000
_diffrn_orient_matrix_UB_23      0.0063670000
_diffrn_orient_matrix_UB_31      0.0071767000
_diffrn_orient_matrix_UB_32      0.0206626000
_diffrn_orient_matrix_UB_33      0.0246782000
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            48154
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         27.864
_diffrn_reflns_theta_min         2.155
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    1.788
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.277
_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    2.518
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.0025(7)
_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   1.054
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         5105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0304P)^2^+0.3665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4403
_reflns_number_total             5105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00956a2.cif
_cod_data_source_block           pfbahas_1
_cod_database_code               7251202
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C4 F13 As N H3 O'
_chemical_oxdiff_usercomment     '100 K, EU, LT mount'
_shelx_estimated_absorpt_t_max   0.663
_shelx_estimated_absorpt_t_min   0.394
_diffrn_oxdiff_digest_od_ed
;

;
_diffrn_oxdiff_measurement_exp_name pfbaHAs_1.par
_olex2_refinement_description
;
1. Others
 Sof(F9B)=Sof(F8B)=Sof(F13B)=Sof(F12B)=Sof(F11B)=Sof(F10B)=1-FVAR(1)
 Sof(F11A)=Sof(F10A)=Sof(F12A)=Sof(F8A)=Sof(F13A)=Sof(F9A)=FVAR(1)
;
_shelx_res_checksum              59176
_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 1.233
_oxdiff_exptl_absorpt_empirical_full_min 0.892