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_7250724
_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), Br, H4 N'
_chemical_formula_sum            'As4 Br H4 N O6'
_chemical_formula_weight         493.63
_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     dual
_audit_creation_date             2024-01-18
_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                   5.1738(11)
_cell_length_b                   5.1738(11)
_cell_length_c                   8.30(3)
_cell_measurement_pressure       6.12e+06(5)
_cell_measurement_reflns_used    208
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.9720
_cell_measurement_theta_min      3.1650
_cell_volume                     192.4(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024) (IMPORT)'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_pressure         6.12e+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 0.396
_diffrn_measured_fraction_theta_max 0.323
_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      0.0060522000
_diffrn_orient_matrix_UB_12      -0.0020174000
_diffrn_orient_matrix_UB_13      -0.0598769000
_diffrn_orient_matrix_UB_21      0.0574446000
_diffrn_orient_matrix_UB_22      0.1102660000
_diffrn_orient_matrix_UB_23      -0.0010332000
_diffrn_orient_matrix_UB_31      0.0940916000
_diffrn_orient_matrix_UB_32      -0.0025935000
_diffrn_orient_matrix_UB_33      0.0043118000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.49585
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_av_unetI/netI     0.1019
_diffrn_reflns_Laue_measured_fraction_full 0.396
_diffrn_reflns_Laue_measured_fraction_max 0.323
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            367
_diffrn_reflns_point_group_measured_fraction_full 0.396
_diffrn_reflns_point_group_measured_fraction_max 0.323
_diffrn_reflns_theta_full        17.308
_diffrn_reflns_theta_max         23.586
_diffrn_reflns_theta_min         3.172
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    8.465
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
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    4.261
_exptl_crystal_description       plate
_exptl_crystal_F_000             226
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.015
_refine_diff_density_max         2.534
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.362
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     11
_refine_ls_number_reflns         71
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.428
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0716
_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^)+(0.1135P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.1918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                68
_reflns_number_total             71
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00593k2.cif
_cod_data_source_block           pnh4br_dec_p1
_cod_depositor_comments
'Adding full bibliography for 7250713--7250749.cif.'
_cod_original_formula_sum        'As4 H4 Br N O6'
_cod_database_code               7250724
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         As4H4BrNO6
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.544
_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
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(As1) \\sim Ueq, Uanis(Br1) \\sim Ueq: with sigma of
0.03 and sigma for terminal atoms of 0.06
3. Others
 Fixed Sof: H1A(0.041667) H1B(0.125)
 Fixed X: H1A(0) H1B(0)
 Fixed Y: H1A(0) H1B(0.164181)
 Fixed Z: H1A(0.10855) H1B(-0.03618)
;
_shelx_res_checksum              18767
_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 2.429
_oxdiff_exptl_absorpt_empirical_full_min 0.509