#------------------------------------------------------------------------------
#$Date: 2021-02-05 01:04:31 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261628 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/18/7241859.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_7241859
loop_
_publ_author_name
'Guńka, Piotr A.'
'Hanfland, Michael'
'Chen, Yu-Sheng'
'Zachara, Janusz'
_publ_section_title
;
 High-pressure and low-temperature structural study of claudetite I, a
 monoclinic layered As2O3 polymorph
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              638
_journal_page_last               644
_journal_paper_doi               10.1039/D0CE01401J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_name_common            'claudetite I'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2020-05-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.731(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.27158(13)
_cell_length_b                   12.7597(3)
_cell_length_c                   4.48224(11)
_cell_measurement_reflns_used    6347
_cell_measurement_temperature    20(1)
_cell_measurement_theta_max      31.1280
_cell_measurement_theta_min      1.8340
_cell_volume                     300.465(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      20(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.824
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.26   0.50    0.30 154.30  25.00  73.80    --   720
  2  φ    -25.74 154.26   0.50    0.30 114.30  25.00  73.80    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0431632896
_diffrn_orient_matrix_UB_12      -0.0166139123
_diffrn_orient_matrix_UB_13      0.0566020771
_diffrn_orient_matrix_UB_21      0.0294535954
_diffrn_orient_matrix_UB_22      -0.0277235343
_diffrn_orient_matrix_UB_23      -0.0298903582
_diffrn_orient_matrix_UB_31      0.0588256994
_diffrn_orient_matrix_UB_32      0.0016709630
_diffrn_orient_matrix_UB_33      0.0668912092
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.824
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3950
_diffrn_reflns_point_group_measured_fraction_full 0.824
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.466
_diffrn_reflns_theta_min         1.856
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    22.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
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    4.373
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.002
_refine_diff_density_max         2.687
_refine_diff_density_min         -3.016
_refine_diff_density_rms         0.354
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         863
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0410
_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)+(0.0869P)²+0.3074P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                801
_reflns_number_total             863
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01401j2.cif
_cod_data_source_block           clau1_1_20
_cod_depositor_comments
'Adding full bibliography for 7241824--7241862.cif.'
_cod_original_cell_volume        300.466(12)
_cod_database_code               7241859
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'As2 O3'
_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   0.957
_shelx_estimated_absorpt_t_min   0.473
_reflns_odcompleteness_completeness 81.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.19
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(As2) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
;
_shelx_res_file
;
TITL clau1_1_20 in P21/n #14
    clau1_1_20.res
    created by SHELXL-2018/3 at 14:00:10 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.271585 12.759731 4.48224 90 94.7309 90
ZERR 4 0.000132 0.000268 0.000107 0 0.0025 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC As O
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 8 12
ISOR 0.0001 0.0002 As2
ISOR 0.001 0.002 O3

L.S. 10 0 0
PLAN  5
SIZE 0.002 0.02 0.04
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_1_20.hkl">
REM </olex2.extras>

WGHT    0.086900    0.307400
FVAR       9.74235
AS1   1    0.258722    0.100168    0.042527    11.00000    0.00298    0.00430 =
         0.00241   -0.00022    0.00061    0.00028
AS2   1    0.355024    0.350963    0.003357    11.00000    0.00273    0.00333 =
         0.00251    0.00010    0.00085    0.00005
O1    2    0.432799    0.217407    0.072058    11.00000    0.00550    0.00575 =
         0.00808    0.00060    0.00063   -0.00141
O2    2    0.656541    0.398992    0.157267    11.00000    0.00423    0.00772 =
         0.00294    0.00023   -0.00005   -0.00189
O3    2   -0.046921    0.140992    0.135087    11.00000    0.00578    0.00869 =
         0.00493    0.00006    0.00208    0.00092
HKLF 4




REM  clau1_1_20 in P21/n #14
REM wR2 = 0.1133, GooF = S = 1.080, Restrained GooF = 1.125 for all data
REM R1 = 0.0410 for 801 Fo > 4sig(Fo) and 0.0427 for all 863 data
REM 46 parameters refined using 12 restraints

END

WGHT      0.0873      0.2896

REM Highest difference peak  2.687,  deepest hole -3.016,  1-sigma level  0.354
Q1    1   0.3705  0.3197  0.0231  11.00000  0.05    2.69
Q2    1   0.3506  0.3819  0.0023  11.00000  0.05    2.59
Q3    1   0.2656  0.1378  0.0421  11.00000  0.05    1.82
Q4    1   0.2311  0.0669  0.0159  11.00000  0.05    1.25
Q5    1   0.3422  0.1979 -0.0452  11.00000  0.05    1.14
;
_shelx_res_checksum              57855
_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 1.716
_oxdiff_exptl_absorpt_empirical_full_min 0.462
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.25872(6) 0.10017(2) 0.04253(8) 0.0032(2) Uani 1 1 d . . . . .
As2 As 0.35502(6) 0.35096(2) 0.00336(8) 0.00282(19) Uani 1 1 d . U . . .
O1 O 0.4328(5) 0.21741(19) 0.0721(6) 0.0064(5) Uani 1 1 d . . . . .
O2 O 0.6565(5) 0.39899(18) 0.1573(6) 0.0050(5) Uani 1 1 d . . . . .
O3 O -0.0469(5) 0.14099(19) 0.1351(6) 0.0064(5) Uani 1 1 d . U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As1 0.0030(2) 0.0043(2) 0.0024(3) -0.00022(10) 0.00061(14) 0.00028(10)
As2 0.0027(2) 0.0033(2) 0.0025(2) 0.00010(7) 0.00085(9) 0.00005(7)
O1 0.0055(9) 0.0058(10) 0.0081(11) 0.0006(9) 0.0006(8) -0.0014(9)
O2 0.0042(11) 0.0077(10) 0.0029(11) 0.0002(7) -0.0001(9) -0.0019(8)
O3 0.0058(8) 0.0087(8) 0.0049(9) 0.0001(6) 0.0021(7) 0.0009(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 O2 100.61(12) . 4_565 ?
O1 As1 O3 102.21(12) . . ?
O2 As1 O3 90.99(13) 4_565 . ?
O1 As2 O2 94.41(11) . . ?
O3 As2 O1 97.83(12) 4_665 . ?
O3 As2 O2 91.22(12) 4_665 . ?
As1 O1 As2 133.96(15) . . ?
As1 O2 As2 124.69(15) 4_666 . ?
As2 O3 As1 125.08(16) 4_566 . ?
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 1.754(2) . ?
As1 O2 1.766(3) 4_565 ?
As1 O3 1.775(3) . ?
As2 O1 1.774(2) . ?
As2 O2 1.788(3) . ?
As2 O3 1.773(3) 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 O3 As2 -86.40(18) . . . 4_566 ?
O1 As2 O2 As1 -71.86(17) . . . 4_666 ?
O2 As1 O1 As2 60.3(2) 4_565 . . . ?
O2 As1 O3 As2 172.53(18) 4_565 . . 4_566 ?
O2 As2 O1 As1 172.1(2) . . . . ?
O3 As1 O1 As2 -33.1(2) . . . . ?
O3 As2 O1 As1 -96.1(2) 4_665 . . . ?
O3 As2 O2 As1 -169.82(17) 4_665 . . 4_666 ?
