Arsenic(III) oxide intercalate with ammonium chloride: crystal structure revision and thermal characterization.
Wrześniewska, Weronika; Paluch, Piotr; Guńka, Piotr A; Acta crystallographica Section B, Structural science, crystal engineering and materials 79 (2023) 207–212; doi:10.1107/S2052520623003086

data_2312082
_publ_section_title
;
 Arsenic(III) oxide intercalate with ammonium chloride: crystal structure
 revision and thermal characterization.
;
_journal_coeditor_code           XK5099
_journal_issue                   3
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              207
_journal_page_last               212
_journal_paper_doi               10.1107/S2052520623003086
_journal_volume                  79
_journal_year                    2023
_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     dual
_audit_creation_date             2023-03-27
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c185 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   5.25420(10)
_cell_length_b                   5.25420(10)
_cell_length_c                   12.6308(3)
_cell_measurement_reflns_used    10181
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.2830
_cell_measurement_theta_min      4.4460
_cell_volume                     301.978(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.88a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.88a (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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3347
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_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    -96.00   7.00   1.00   30.00    --  -19.65 -38.00 -60.00  103
  2  \w     -6.00  96.00   1.00   30.00    --   19.96  38.00-180.00  102
  3  \w    -53.00  39.00   1.00   30.00    --  -19.65  77.00-120.00   92
  4  \w    -46.00  56.00   1.00   30.00    --  -19.65  38.00  90.00  102
  5  \w     60.00 110.00   1.00   30.00    --   19.96 179.00 -90.00   50
  6  \w    -14.00  39.00   1.00   30.00    --   19.96  77.00 120.00   53
  7  \w    -14.00  39.00   1.00   30.00    --   19.96  77.00 -90.00   53
  8  \w     60.00 110.00   1.00   30.00    --   19.96 179.00  30.00   50
  9  \w    -49.00  54.00   1.00   30.00    --  -19.65  57.00  90.00  103
 10  \w    -72.00   6.00   1.00   30.00    --  -19.65 117.00 113.00   78
 11  \w    -99.00 -52.00   1.00   30.00    --  -19.65-162.00-123.00   47
 12  \w    -12.00  96.00   1.00   30.00    --   19.96  69.00-166.00  108
 13  \w      1.00  62.00   1.00   30.00    --   19.96 -99.00  30.00   61
 14  \w    -14.00  39.00   1.00   30.00    --   19.96  77.00 -30.00   53
 15  \w   -109.00 -78.00   1.00   30.00    --  -19.65   0.00 -90.00   31
 16  \w   -109.00  70.00   1.00   30.00    --  -19.65   0.00-180.00  179
 17  \w   -109.00  70.00   1.00   30.00    --  -19.65   0.00-150.00  179
 18  \w   -109.00  70.00   1.00   30.00    --  -19.65   0.00-120.00  179
 19  \w     16.00  72.00   1.00   30.00    --   19.96-117.00  25.00   56
 20  \w     -6.00  96.00   1.00   30.00    --   19.96  38.00 120.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1286930000
_diffrn_orient_matrix_UB_12      0.0538906000
_diffrn_orient_matrix_UB_13      -0.0313810000
_diffrn_orient_matrix_UB_21      0.0479317000
_diffrn_orient_matrix_UB_22      0.1444302000
_diffrn_orient_matrix_UB_23      0.0185794000
_diffrn_orient_matrix_UB_31      0.0737465000
_diffrn_orient_matrix_UB_32      -0.0231674000
_diffrn_orient_matrix_UB_33      0.0427021000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0826
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_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       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16612
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.834
_diffrn_reflns_theta_min         3.226
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.428
_exptl_absorpt_correction_T_max  0.756
_exptl_absorpt_correction_T_min  0.258
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.88a (Rigaku Oxford Diffraction, 2023)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.863
_exptl_crystal_description       plate
_exptl_crystal_F_000             246
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.330(12)
_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   1.231
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.231
_refine_ls_R_factor_all          0.0164
_refine_ls_R_factor_gt           0.0157
_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^)+(0.0247P)^2^+0.1074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0420
_refine_ls_wR_factor_ref         0.0424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                275
_reflns_number_total             282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xk5099sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2312082.cif.'
_cod_original_cell_volume        301.977(14)
_cod_database_code               2312082
_cod_database_fobs_code          2312082
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'As2 O3.5 N H5 Cl1'
_chemical_oxdiff_usercomment     'WW4 '
_shelx_estimated_absorpt_t_max   0.763
_shelx_estimated_absorpt_t_min   0.259
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All N(H,H) groups, All O(H) groups
2. Shared sites
{N2, O2}
3. Uiso/Uaniso restraints and constraints
Uanis(N2) = Uanis(O2)
4. Others
 Fixed Sof: H1B(0.041667) H1A(0.125) O2(0.041667) H2(0.083333) N2(0.041667)
 H2A(0.083333) H2B(0.083333)
 Fixed X: H1B(0) H1A(0) H2(0.35107) H2A(0.35999) H2B(0.58084)
 Fixed Y: H1B(0) H1A(0.161671) H2(0) H2A(0) H2B(0.161671)
 Fixed Z: H1B(0.071341) H1A(-0.023781) H2(0.456189) H2A(0.45882) H2B(0.541181)
;
_shelx_res_checksum              3456
_shelx_hkl_checksum              92275
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.160
_oxdiff_exptl_absorpt_empirical_full_min 0.866