#------------------------------------------------------------------------------
#$Date: 2021-07-25 01:20:33 +0300 (Sun, 25 Jul 2021) $
#$Revision: 267735 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/89/4518920.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4518920
loop_
_publ_author_name
'Domański, Mateusz A.'
'Kraszewski, Karol'
'Paluch, Piotr'
'Guńka, Piotr A.'
_publ_section_title
;
 Arsenic(III)-oxide Intercalates with Potassium Chloride: Water-Induced
 Varieties and New Synthesis Methods
;
_journal_name_full               'Crystal Growth & Design'
_journal_paper_doi               10.1021/acs.cgd.1c00555
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'As2 O3, 1(K), 1(Cl), 1.5(O2)'
_chemical_formula_sum            'As2 Cl K O6'
_chemical_formula_weight         320.39
_space_group_crystal_system      hexagonal
_space_group_IT_number           183
_space_group_name_Hall           'P 6 -2'
_space_group_name_H-M_alt        'P 6 m m'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-14
_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                   5.2774(2)
_cell_length_b                   5.2774(2)
_cell_length_c                   8.3169(6)
_cell_measurement_reflns_used    2124
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1690
_cell_measurement_theta_min      4.4240
_cell_volume                     200.601(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.990
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -44.00  59.00   1.00   24.00    --  -19.50  19.00  90.00  103
  2  ω    -49.00  54.00   1.00   24.00    --  -19.50  57.00 120.00  103
  3  ω   -109.00 -34.00   1.00   24.00    --  -19.50-179.00 150.00   75
  4  ω    -10.00  94.00   1.00   24.00    --   19.97  57.00  30.00  104
  5  ω    -59.00  54.00   1.00   24.00    --   19.97 -77.00 -30.00  113
  6  ω     56.00 110.00   1.00   24.00    --   19.97 179.00 -90.00   54
  7  ω    -20.00  26.00   1.00   24.00    --   19.97  97.00 156.00   46
  8  ω    -81.00 -42.00   1.00   24.00    --  -19.50 131.00 131.00   39
  9  ω    -46.00  56.00   1.00   24.00    --  -19.50  38.00-120.00  102
 10  ω     22.00  81.00   1.00   24.00    --   19.97-131.00  60.00   59
 11  ω     -4.00  62.00   1.00   24.00    --   19.97 -99.00  90.00   66
 12  ω    -10.00  94.00   1.00   24.00    --   19.97  57.00 -90.00  104
 13  ω    -10.00  94.00   1.00   24.00    --   19.97  57.00 150.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0303343000
_diffrn_orient_matrix_UB_12      -0.0523720000
_diffrn_orient_matrix_UB_13      -0.0802695000
_diffrn_orient_matrix_UB_21      0.1433974000
_diffrn_orient_matrix_UB_22      0.0216187000
_diffrn_orient_matrix_UB_23      -0.0070400000
_diffrn_orient_matrix_UB_31      -0.0509445000
_diffrn_orient_matrix_UB_32      -0.1445371000
_diffrn_orient_matrix_UB_33      0.0279446000
_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  0.0672
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.990
_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       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5769
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.374
_diffrn_reflns_theta_min         4.459
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.154
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    2.652
_exptl_crystal_description       plate
_exptl_crystal_F_000             150
_exptl_crystal_size_max          0.096
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.269
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     21
_refine_ls_number_reflns         285
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0279
_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/[σ²(Fo²)+(0.0534P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0680
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                278
_reflns_number_total             285
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg1c00555_si_002.cif
_cod_data_source_block           pg52intercalateX_KCl
_cod_original_cell_volume        200.60(2)
_cod_database_code               4518920
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'K As2 O3 Cl H4 O2'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(6)
 0.47(6)
2. Others
 Fixed Sof: O4(0.25)
;
_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 1.137
_oxdiff_exptl_absorpt_empirical_full_min 0.888
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.666667 0.333333 0.27610(18) 0.0138(3) Uani 1 6 d S T P . .
K1 K 0.000000 0.000000 -0.0018(5) 0.0318(10) Uani 1 12 d S T P . .
Cl1 Cl 1.000000 0.000000 0.4197(6) 0.0278(9) Uani 1 12 d S T P . .
O1 O 0.500000 0.500000 0.1580(9) 0.0148(14) Uani 1 4 d S T P . .
O4 O 0.369(6) 0.369(6) -0.256(5) 0.19(3) Uani 0.5 2 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 -1 0.0025
0 -1 0 0.0448
0 0 1 0.0025
-1 1 0 0.0341
1 -1 0 0.0210
1 0 0 0.0512
-1 0 0 0.0380
0 1 0 0.0316
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 As1 O1 93.4(3) 2_655 3_665 ?
O1 As1 O1 93.4(3) 3_665 . ?
O1 As1 O1 93.4(3) 2_655 . ?
As1 O1 As1 114.4(4) . 4_665 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.813(4) 2_655 ?
As1 O1 1.813(4) . ?
As1 O1 1.813(4) 3_665 ?
O4 O4 1.38(6) 4_665 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O1 As1 133.18(17) 2_655 . . 4_665 ?
O1 As1 O1 As1 -133.18(17) 3_665 . . 4_665 ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.53(6)
2 0.47(6)
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0000 -0.0001 -1.0010 0.0804 0.0070 -0.0280
-0.0001 -1.0006 -0.0004 0.0524 -0.0216 0.1446
0.0000 0.0001 1.0010 -0.0804 -0.0070 0.0280
-1.0006 1.0006 0.0003 -0.0221 -0.1219 -0.0936
1.0006 -1.0006 -0.0003 0.0221 0.1219 0.0936
1.0007 0.0000 0.0001 -0.0304 0.1435 -0.0510
-1.0007 -0.0000 -0.0001 0.0304 -0.1435 0.0510
0.0001 1.0006 0.0004 -0.0524 0.0216 -0.1446
