#------------------------------------------------------------------------------
#$Date: 2021-02-05 00:04:31 +0100 (vie 05 de feb de 2021) $
#$Revision: 261628 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/18/7241856.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_7241856
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                 94.541(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.28841(13)
_cell_length_b                   12.8335(3)
_cell_length_c                   4.50014(13)
_cell_measurement_reflns_used    6391
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      26.7350
_cell_measurement_theta_min      1.8390
_cell_volume                     304.460(14)
_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      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_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  φ    -25.74 334.26   0.50    0.30 154.30  15.00  73.80    --   720
  2  φ    -25.74 255.26   0.50    0.30 114.30  15.00  73.80    --   562
  3  φ    -25.74 154.26   0.50    0.30 114.30  15.00  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      0.0434705468
_diffrn_orient_matrix_UB_12      0.0260554915
_diffrn_orient_matrix_UB_13      -0.0135120876
_diffrn_orient_matrix_UB_21      0.0507262023
_diffrn_orient_matrix_UB_22      -0.0181794489
_diffrn_orient_matrix_UB_23      -0.0422576767
_diffrn_orient_matrix_UB_31      -0.0409893327
_diffrn_orient_matrix_UB_32      0.0051722219
_diffrn_orient_matrix_UB_33      -0.0808213541
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.989
_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       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            9732
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.498
_diffrn_reflns_theta_min         1.845
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    21.727
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91336
_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    4.316
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.897
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.311
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         973
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0314
_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)+(0.0484P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                836
_reflns_number_total             973
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01401j2.cif
_cod_data_source_block           clau1_5_150
_cod_depositor_comments
'Adding full bibliography for 7241824--7241862.cif.'
_cod_database_code               7241856
_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   0.958
_shelx_estimated_absorpt_t_min   0.517
_reflns_odcompleteness_completeness 83.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.88
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
;
_shelx_res_file
;
TITL clau1_5_150 in P21/n #14
    clau1_5_150.res
    created by SHELXL-2018/3 at 13:21:29 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.288408 12.833474 4.50014 90 94.5406 90
ZERR 4 0.000127 0.000346 0.000133 0 0.0026 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 0.001 0.001 O2

L.S. 9 0 0
PLAN  5
SIZE 0.002 0.018 0.035
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_5_150.hkl">
REM </olex2.extras>

WGHT    0.048400
FVAR       6.32848
AS1   1    0.258955    0.100589    0.042118    11.00000    0.00695    0.01111 =
         0.00516    0.00009    0.00124    0.00128
AS2   1    0.355607    0.350651    0.004217    11.00000    0.00582    0.01293 =
         0.00488   -0.00015    0.00273    0.00014
O1    2    0.432065    0.217706    0.070345    11.00000    0.00868    0.01244 =
         0.01447    0.00062    0.00031   -0.00123
O2    2    0.656638    0.398859    0.157608    11.00000    0.01025    0.01281 =
         0.00738    0.00122    0.00150   -0.00175
O3    2   -0.045756    0.141031    0.135849    11.00000    0.00750    0.02328 =
         0.00358    0.00103    0.00126    0.00222
HKLF 4




REM  clau1_5_150 in P21/n #14
REM wR2 = 0.0821, GooF = S = 1.063, Restrained GooF = 1.071 for all data
REM R1 = 0.0314 for 836 Fo > 4sig(Fo) and 0.0377 for all 973 data
REM 46 parameters refined using 6 restraints

END

WGHT      0.0484      0.0000

REM Highest difference peak  1.897,  deepest hole -1.199,  1-sigma level  0.311
Q1    1   0.2836  0.1625  0.0212  11.00000  0.05    1.90
Q2    1   0.3473  0.2864  0.0200  11.00000  0.05    1.66
Q3    1   0.2724  0.0388  0.0229  11.00000  0.05    1.55
Q4    1   0.1818  0.1009 -0.1403  11.00000  0.05    1.31
Q5    1   0.3746  0.4154  0.0105  11.00000  0.05    1.29
;
_shelx_res_checksum              58562
_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 1.123
_oxdiff_exptl_absorpt_empirical_full_min 0.867
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 0.25895(7) 0.10059(3) 0.04212(9) 0.00770(14) Uani 1 1 d . . . . .
As2 As 0.35561(7) 0.35065(3) 0.00422(9) 0.00775(14) Uani 1 1 d . . . . .
O1 O 0.4321(5) 0.2177(2) 0.0703(7) 0.0119(6) Uani 1 1 d . . . . .
O2 O 0.6566(6) 0.3989(2) 0.1576(7) 0.0101(6) Uani 1 1 d . U . . .
O3 O -0.0458(6) 0.1410(2) 0.1358(7) 0.0114(6) Uani 1 1 d . . . . .
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 0.0069(2) 0.0111(2) 0.0052(2) 0.00009(13) 0.00124(15) 0.00128(13)
As2 0.0058(2) 0.0129(2) 0.0049(2) -0.00015(13) 0.00273(15) 0.00014(14)
O1 0.0087(11) 0.0124(13) 0.0145(16) 0.0006(11) 0.0003(11) -0.0012(11)
O2 0.0103(9) 0.0128(9) 0.0074(9) 0.0012(7) 0.0015(8) -0.0018(7)
O3 0.0075(12) 0.0233(15) 0.0036(14) 0.0010(10) 0.0013(11) 0.0022(11)
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(14) . 4_565 ?
O1 As1 O3 102.12(14) . . ?
O2 As1 O3 91.04(14) 4_565 . ?
O1 As2 O2 94.80(13) . . ?
O1 As2 O3 97.72(15) . 4_665 ?
O3 As2 O2 91.21(14) 4_665 . ?
As1 O1 As2 134.39(17) . . ?
As1 O2 As2 124.76(17) 4_666 . ?
As1 O3 As2 125.26(18) . 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 1.759(3) . ?
As1 O2 1.772(3) 4_565 ?
As1 O3 1.775(3) . ?
As2 O1 1.773(3) . ?
As2 O2 1.794(3) . ?
As2 O3 1.780(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 -86.4(2) . . . 4_566 ?
O1 As2 O2 As1 -71.8(2) . . . 4_666 ?
O2 As1 O1 As2 60.6(3) 4_565 . . . ?
O2 As1 O3 As2 172.5(2) 4_565 . . 4_566 ?
O2 As2 O1 As1 171.7(3) . . . . ?
O3 As1 O1 As2 -32.8(3) . . . . ?
O3 As2 O1 As1 -96.4(3) 4_665 . . . ?
O3 As2 O2 As1 -169.6(2) 4_665 . . 4_666 ?
