Arsenic(III)-oxide Intercalates with Potassium Chloride: Water-Induced Varieties and New Synthesis Methods
Domański, Mateusz A.; Kraszewski, Karol; Paluch, Piotr; Guńka, Piotr A.; Crystal Growth & Design  (2021) –; doi:10.1021/acs.cgd.1c00555

data_4518919
_publ_section_title
;
 Arsenic(III)-oxide Intercalates with Potassium Chloride: Water-Induced
 Varieties and New Synthesis Methods
;
_journal_name_full               'Crystal Growth &amp; Design'
_journal_paper_doi               10.1021/acs.cgd.1c00555
_journal_year                    2021
_chemical_formula_moiety         'As4 O6, 2(K), 2(Cl), 1(O)'
_chemical_formula_sum            'As4 Cl2 K2 O7'
_chemical_formula_weight         560.78
_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_primary     iterative
_audit_creation_date             2021-01-27
_audit_creation_method
;
Olex2 1.3-dev
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   5.24015(14)
_cell_length_b                   5.24015(14)
_cell_length_c                   12.2944(4)
_cell_measurement_reflns_used    3325
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.3190
_cell_measurement_theta_min      4.4690
_cell_volume                     292.365(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3-dev (Bourhis et al., 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 0.985
_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    -45.00  35.00   1.00    4.50    --  -19.50  38.00 -60.00   80
  2  \w    -13.00  25.00   1.00    4.50    --   19.81  77.00 150.00   38
  3  \w    -95.00   7.00   1.00    4.50    --  -19.50 -38.00 120.00  102
  4  \w    -98.00 -40.00   1.00    4.50    --  -19.50 -77.00 -60.00   58
  5  \w   -108.00 -32.00   1.00    4.50    --  -19.50 179.00  30.00   76
  6  \w    -95.00   7.00   1.00    4.50    --  -19.50 -38.00 -30.00  102
  7  \w    -93.00  10.00   1.00    4.50    --  -19.50 -57.00-120.00  103
  8  \w     45.00  87.00   1.00    4.50    --   19.97-166.00 -45.00   42
  9  \w     -4.00  62.00   1.00    4.50    --   19.97 -99.00  30.00   66
;
_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      -0.1541029000
_diffrn_orient_matrix_UB_12      -0.0659466000
_diffrn_orient_matrix_UB_13      0.0083702000
_diffrn_orient_matrix_UB_21      0.0114746000
_diffrn_orient_matrix_UB_22      0.1404462000
_diffrn_orient_matrix_UB_23      -0.0037406000
_diffrn_orient_matrix_UB_31      -0.0233666000
_diffrn_orient_matrix_UB_32      -0.0188574000
_diffrn_orient_matrix_UB_33      -0.0569657000
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0148
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6016
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.709
_diffrn_reflns_theta_min         3.314
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.506
_exptl_absorpt_correction_T_max  0.586
_exptl_absorpt_correction_T_min  0.157
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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)
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    3.185
_exptl_crystal_description       plate
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.218
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.119(4)
_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   1.130
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0153
_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^)+(0.0170P)^2^+0.1336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                260
_reflns_number_total             267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg1c00555_si_002.cif
_cod_data_source_block           pg48intercalateY_KCl
_cod_original_cell_volume        292.365(18)
_cod_database_code               4518919
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'K1 As2 O3 Cl1'
_shelx_estimated_absorpt_t_max   0.641
_shelx_estimated_absorpt_t_min   0.171
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(K2) = Uanis(O2)
2. Others
 Fixed Sof: K2(0.04167) O2(0.04167)
;
_shelx_res_checksum              26155
_shelx_hkl_checksum              2593
_olex2_date_sample_data_collection 2018-12-05
_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 1.104
_oxdiff_exptl_absorpt_empirical_full_min 0.891