Compressing arsenic⋯halogen secondary bonds: a high-pressure structural study of arsenic(iii) oxide intercalates with ammonium halides
Guńka, Piotr A.; Milos, Sofija; Ende, Martin; Alabarse, Frederico; Miletich, Ronald; Dziubek, Kamil F.; CrystEngComm 27 (2025) 5983–5988; doi:10.1039/D5CE00593K

data_7250713
_publ_section_title
;
 Compressing arsenic&#x22EF;halogen secondary bonds: a high-pressure
 structural study of arsenic(iii) oxide intercalates with ammonium halides
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5983
_journal_page_last               5988
_journal_paper_doi               10.1039/D5CE00593K
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         '2(As2 O3), 2(H4 N), H2 O, 2(Cl)'
_chemical_formula_sum            'As4 Cl2 H10 N2 O7'
_chemical_formula_weight         520.68
_space_group_crystal_system      hexagonal
_space_group_IT_number           191
_space_group_name_Hall           '-P 6 2'
_space_group_name_H-M_alt        'P 6/m m m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2024-01-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec141 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-04-03 deposited with the CCDC.	2025-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   5.19055(19)
_cell_length_b                   5.19055(19)
_cell_length_c                   11.151(6)
_cell_measurement_pressure       5.65e+06(5)
_cell_measurement_reflns_used    388
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7470
_cell_measurement_theta_min      3.4110
_cell_volume                     260.18(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023) (IMPORT)'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_pressure         5.65e+06(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.404
_diffrn_measured_fraction_theta_max 0.273
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -37.00  37.00   0.50    0.25   0.00   0.00   0.00    --   148
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0146052000
_diffrn_orient_matrix_UB_12      -0.0071463000
_diffrn_orient_matrix_UB_13      -0.0440872000
_diffrn_orient_matrix_UB_21      0.0195356000
_diffrn_orient_matrix_UB_22      0.1037618000
_diffrn_orient_matrix_UB_23      -0.0009300000
_diffrn_orient_matrix_UB_31      0.1075724000
_diffrn_orient_matrix_UB_32      0.0367310000
_diffrn_orient_matrix_UB_33      -0.0057489000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.49585
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_unetI/netI     0.0081
_diffrn_reflns_Laue_measured_fraction_full 0.404
_diffrn_reflns_Laue_measured_fraction_max 0.273
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            585
_diffrn_reflns_point_group_measured_fraction_full 0.404
_diffrn_reflns_point_group_measured_fraction_max 0.273
_diffrn_reflns_theta_full        17.308
_diffrn_reflns_theta_max         26.105
_diffrn_reflns_theta_min         3.162
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    4.970
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             246
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.066(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     12
_refine_ls_number_reflns         102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.276
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+0.0880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                101
_reflns_number_total             102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00593k3.cif
_cod_data_source_block           ynh4cl_p5
_cod_depositor_comments
'Adding full bibliography for 7250713--7250749.cif.'
_cod_original_cell_volume        260.17(15)
_cod_database_code               7250713
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         As4H10Cl2N2O7
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.564
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All N(H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(O2) = Uiso(N2)
3. Others
 Fixed Sof: H1A(0.041667) H1B(0.125) O2(0.041667) H2(0.083333) N2(0.041667)
 H2B(0.083333) H2A(0.083333)
 Fixed X: H1A(0) H1B(0) H2(0.34924) H2B(0.358271) H2A(0.58084)
 Fixed Y: H1A(0) H1B(0.163661) H2(0) H2B(0) H2A(0.161671)
 Fixed Z: H1A(0.0808) H1B(-0.026931) H2(0.45038) H2B(0.45335) H2A(0.546649)
;
_shelx_res_checksum              55158
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.822