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

data_7251203
_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         'C4 H3 F7 N O, As F6, F2 Xe'
_chemical_formula_sum            'C4 H3 As F15 N O Xe'
_chemical_formula_weight         572.29
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_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                   8.62011(14)
_cell_length_b                   35.5418(5)
_cell_length_c                   8.71910(12)
_cell_measurement_reflns_used    46924
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.8600
_cell_measurement_theta_min      1.7910
_cell_volume                     2671.31(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.144a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 44.112a 64-bit (release 21-05-2025))'
_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      100.00(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 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    -12.00  52.00   0.25    3.00    --   -0.43  77.00   0.00  256
  2  \w    -62.00   8.00   0.25    3.00    --   -0.43 -57.00-180.00  280
  3  \w    -55.00  11.00   0.25    3.00    --   -0.43 -57.00  90.00  264
  4  \w    -19.00  41.00   0.25    3.00    --   -0.43  77.00 -90.00  240
  5  \w    -57.00   7.00   0.25    3.00    --   -0.43 -57.00-120.00  256
  6  \w     -1.00  40.00   0.25    3.00    --    2.16  77.00 150.00  164
  7  \w      0.00  35.00   0.25    3.00    --    2.16  57.00-120.00  140
  8  \w    -36.00   4.00   0.25    3.00    --   -3.10 -57.00 -60.00  160
  9  \w    -60.00  14.00   0.25    3.00    --    2.16 -57.00   0.00  296
 10  \w     -9.00  16.00   0.25    3.00    --    2.16  57.00  60.00  100
 11  \w    -60.00  14.00   0.25    3.00    --    2.16 -57.00 -90.00  296
 12  \w     31.00  56.00   0.25    3.00    --   -0.57  77.00   0.00  100
 13  \w    -12.00  62.00   0.25    3.00    --   -0.57  57.00-180.00  296
 14  \w    -57.00 -32.00   0.25    3.00    --   -0.57 -77.00  60.00  100
 15  \w    -22.00  56.00   0.25    3.00    --   -0.57  77.00  90.00  312
;
_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      -0.0065436000
_diffrn_orient_matrix_UB_12      -0.0155981000
_diffrn_orient_matrix_UB_13      0.0057200000
_diffrn_orient_matrix_UB_21      0.0543506000
_diffrn_orient_matrix_UB_22      -0.0020960000
_diffrn_orient_matrix_UB_23      -0.0340022000
_diffrn_orient_matrix_UB_31      0.0348665000
_diffrn_orient_matrix_UB_32      0.0003351000
_diffrn_orient_matrix_UB_33      0.0540958000
_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  0.0528
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            133848
_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         25.558
_diffrn_reflns_theta_min         1.898
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Ag) X-ray Source'
_exptl_absorpt_coefficient_mu    2.760
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.196
_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    2.846
_exptl_crystal_description       plate
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.616
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.00034(6)
_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   1.137
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         5099
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+6.5153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4461
_reflns_number_total             5099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00956a2.cif
_cod_data_source_block           pfbah_xef2_2_1
_cod_database_code               7251203
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Xe As F13 C4 N O'
_chemical_oxdiff_usercomment     '100 K, EU, LT mount'
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.428
_olex2_refinement_description
;
1. Restrained distances
 N1-H1B
 0.88 with sigma of 0.02
 H1A-N1
 0.88 with sigma of 0.02
;
_shelx_res_checksum              80002
_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 1.220
_oxdiff_exptl_absorpt_empirical_full_min 0.819
_publcif_funding_html
;
;