#------------------------------------------------------------------------------
#$Date: 2021-07-25 01:20:33 +0300 (Sun, 25 Jul 2021) $
#$Revision: 267735 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/89/4518919.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_4518919
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_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  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -45.00  35.00   1.00    4.50    --  -19.50  38.00 -60.00   80
  2  ω    -13.00  25.00   1.00    4.50    --   19.81  77.00 150.00   38
  3  ω    -95.00   7.00   1.00    4.50    --  -19.50 -38.00 120.00  102
  4  ω    -98.00 -40.00   1.00    4.50    --  -19.50 -77.00 -60.00   58
  5  ω   -108.00 -32.00   1.00    4.50    --  -19.50 179.00  30.00   76
  6  ω    -95.00   7.00   1.00    4.50    --  -19.50 -38.00 -30.00  102
  7  ω    -93.00  10.00   1.00    4.50    --  -19.50 -57.00-120.00  103
  8  ω     45.00  87.00   1.00    4.50    --   19.97-166.00 -45.00   42
  9  ω     -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       'ω 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0170P)²+0.1336P] where P=(Fo²+2Fc²)/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 > 2σ(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_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.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z'
'-y, x-y, z'
'-x, -y, z'
'-x+y, -x, z'
'y, -x+y, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'-x+y, -x, -z'
'y, -x+y, -z'
'x, y, -z'
'x-y, x, -z'
'-y, x-y, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, 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 0.333333 0.666667 0.21026(2) 0.01105(12) Uani 1 6 d S T P . .
K1 K 0.000000 0.000000 0.000000 0.0274(3) Uani 1 24 d S T P . .
Cl1 Cl 0.000000 0.000000 0.32424(12) 0.0303(3) Uani 1 12 d S T P . .
O1 O 0.500000 0.500000 0.13226(13) 0.0147(3) Uani 1 4 d S T P . .
K2 K 0.500000 0.000000 0.500000 0.0624(9) Uani 0.3334 8 d S T P A 1
O2 O 0.500000 0.000000 0.500000 0.0624(9) Uani 0.3334 8 d S T P B 2
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 0.0196
0 1 0 0.1013
0 -1 0 0.0857
-1 1 0 0.0827
1 -1 0 0.0983
-1 0 0 0.1034
1 0 0 0.0878
0 0 1 0.0196
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 94.01(6) 2 3_665 ?
O1 As1 O1 94.01(6) 3_665 . ?
O1 As1 O1 94.01(6) 2 . ?
As1 O1 As1 115.25(9) 2_655 . ?
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 1.7911(9) 2 ?
As1 O1 1.7911(9) . ?
As1 O1 1.7911(9) 3_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 -132.84(4) 2 . . 2_655 ?
O1 As1 O1 As1 132.84(4) 3_665 . . 2_655 ?
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
-0.0001 0.0000 -0.9985 -0.0083 0.0037 0.0569
-0.0009 0.9980 0.0001 -0.0657 0.1402 -0.0188
0.0009 -0.9980 -0.0001 0.0657 -0.1402 0.0188
-0.9983 0.9979 0.0004 0.0880 0.1287 0.0045
0.9983 -0.9979 -0.0004 -0.0880 -0.1287 -0.0045
-0.9975 -0.0001 0.0003 0.1537 -0.0115 0.0233
0.9975 0.0001 -0.0003 -0.1537 0.0115 -0.0233
0.0001 -0.0000 0.9985 0.0083 -0.0037 -0.0569
