#------------------------------------------------------------------------------
#$Date: 2021-02-05 01:04:31 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261628 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/18/7241855.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_7241855
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                 94.440(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.29025(13)
_cell_length_b                   12.8566(3)
_cell_length_c                   4.50200(12)
_cell_measurement_reflns_used    5868
_cell_measurement_temperature    230(1)
_cell_measurement_theta_max      25.9370
_cell_measurement_theta_min      1.8330
_cell_volume                     305.283(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      230(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    -25.74 334.26   0.50    0.30 114.30  15.00  73.80    --   720
;
_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      0.0448376816
_diffrn_orient_matrix_UB_12      0.0255223103
_diffrn_orient_matrix_UB_13      -0.0145644640
_diffrn_orient_matrix_UB_21      0.0496885874
_diffrn_orient_matrix_UB_22      -0.0188369652
_diffrn_orient_matrix_UB_23      -0.0416636531
_diffrn_orient_matrix_UB_31      -0.0407288103
_diffrn_orient_matrix_UB_32      0.0051338469
_diffrn_orient_matrix_UB_33      -0.0808720642
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0341
_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            8875
_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         17.497
_diffrn_reflns_theta_min         1.842
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    21.668
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84664
_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    4.304
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.255
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0294
_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)+(0.0407P)²+0.0604P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                848
_reflns_number_total             976
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01401j2.cif
_cod_data_source_block           clau1_5_230
_cod_depositor_comments
'Adding full bibliography for 7241824--7241862.cif.'
_cod_original_cell_volume        305.283(14)
_cod_database_code               7241855
_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   0.696
_shelx_estimated_absorpt_t_min   0.518
_reflns_odcompleteness_completeness 84.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.90
_olex2_refinement_description
;
;
_shelx_res_file
;
TITL clau1_5_230 in P21/n #14
    clau1_5_230.res
    created by SHELXL-2018/3 at 12:53:04 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.290251 12.856586 4.502005 90 94.4397 90
ZERR 4 0.000135 0.000336 0.000119 0 0.0025 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 12 8

L.S. 10 0 0
PLAN  5
SIZE 0.02 0.018 0.035
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_5_230.hkl">
REM </olex2.extras>

WGHT    0.040700    0.060400
FVAR       6.55736
AS1   2    0.258708    0.101011    0.041607    11.00000    0.01073    0.01379 =
         0.00824    0.00034    0.00080    0.00160
AS2   2    0.356161    0.350407    0.004529    11.00000    0.00903    0.01652 =
         0.00823   -0.00026    0.00292    0.00026
O1    1    0.431695    0.217647    0.070610    11.00000    0.01243    0.01594 =
         0.02005    0.00207   -0.00040   -0.00101
O2    1    0.656646    0.398281    0.157458    11.00000    0.01512    0.02391 =
         0.00695    0.00183    0.00163   -0.00522
O3    1   -0.045052    0.141209    0.138037    11.00000    0.01302    0.02807 =
         0.00650   -0.00007    0.00101    0.00354
HKLF 4




REM  clau1_5_230 in P21/n #14
REM wR2 = 0.0723, GooF = S = 1.045, Restrained GooF = 1.045 for all data
REM R1 = 0.0294 for 848 Fo > 4sig(Fo) and 0.0347 for all 976 data
REM 46 parameters refined using 0 restraints

END

WGHT      0.0407      0.0604

REM Highest difference peak  1.556,  deepest hole -0.927,  1-sigma level  0.255
Q1    1   0.2704  0.1715  0.0400  11.00000  0.05    1.56
Q2    1   0.3804  0.2807  0.0193  11.00000  0.05    1.52
Q3    1   0.2588  0.0380  0.0402  11.00000  0.05    1.44
Q4    1   0.3640  0.4184  0.0071  11.00000  0.05    1.28
Q5    1   0.4848  0.3577  0.1125  11.00000  0.05    0.89
;
_shelx_res_checksum              27835
_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 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.853
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 0.25871(7) 0.10101(3) 0.04161(8) 0.01092(12) Uani 1 1 d . . . . .
As2 As 0.35616(7) 0.35041(3) 0.00453(8) 0.01114(13) Uani 1 1 d . . . . .
O1 O 0.4317(5) 0.2176(2) 0.0706(7) 0.0162(5) Uani 1 1 d . . . . .
O2 O 0.6566(6) 0.3983(2) 0.1575(6) 0.0153(5) Uani 1 1 d . . . . .
O3 O -0.0451(5) 0.1412(2) 0.1380(6) 0.0159(5) 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 0.01073(19) 0.0138(2) 0.0082(2) 0.00034(12) 0.00080(14) 0.00160(12)
As2 0.00903(19) 0.0165(2) 0.0082(2) -0.00026(12) 0.00292(14) 0.00026(13)
O1 0.0124(11) 0.0159(12) 0.0200(14) 0.0021(10) -0.0004(11) -0.0010(10)
O2 0.0151(13) 0.0239(14) 0.0070(12) 0.0018(9) 0.0016(10) -0.0052(11)
O3 0.0130(12) 0.0281(14) 0.0065(12) -0.0001(10) 0.0010(10) 0.0035(11)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2879 0.7731 '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 100.71(13) . 4_565 ?
O1 As1 O3 102.11(13) . . ?
O2 As1 O3 91.37(13) 4_565 . ?
O1 As2 O2 94.85(13) . . ?
O3 As2 O1 97.81(13) 4_665 . ?
O3 As2 O2 91.15(12) 4_665 . ?
As1 O1 As2 134.44(16) . . ?
As1 O2 As2 124.83(15) 4_666 . ?
As2 O3 As1 125.71(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 1.756(3) . ?
As1 O2 1.771(3) 4_565 ?
As1 O3 1.774(3) . ?
As2 O1 1.773(3) . ?
As2 O2 1.792(3) . ?
As2 O3 1.772(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 -86.1(2) . . . 4_566 ?
O1 As2 O2 As1 -71.84(19) . . . 4_666 ?
O2 As1 O1 As2 60.4(3) 4_565 . . . ?
O2 As1 O3 As2 172.6(2) 4_565 . . 4_566 ?
O2 As2 O1 As1 171.9(2) . . . . ?
O3 As1 O1 As2 -33.4(3) . . . . ?
O3 As2 O1 As1 -96.3(2) 4_665 . . . ?
O3 As2 O2 As1 -169.78(19) 4_665 . . 4_666 ?
