#------------------------------------------------------------------------------
#$Date: 2021-02-05 01:04:31 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261628 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/18/7241853.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_7241853
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                 94.579(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.27066(19)
_cell_length_b                   12.7806(5)
_cell_length_c                   4.48685(19)
_cell_measurement_reflns_used    7960
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      26.7830
_cell_measurement_theta_min      1.8430
_cell_volume                     301.28(2)
_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      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_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
  3  φ    -25.74 334.26   0.50    0.30  74.30  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      0.0427114746
_diffrn_orient_matrix_UB_12      0.0264643934
_diffrn_orient_matrix_UB_13      -0.0130027574
_diffrn_orient_matrix_UB_21      0.0516043950
_diffrn_orient_matrix_UB_22      -0.0178349974
_diffrn_orient_matrix_UB_23      -0.0424964389
_diffrn_orient_matrix_UB_31      -0.0412100647
_diffrn_orient_matrix_UB_32      0.0051177351
_diffrn_orient_matrix_UB_33      -0.0811010011
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_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       -6
_diffrn_reflns_number            11248
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.454
_diffrn_reflns_theta_min         1.853
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    21.956
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44318
_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    4.362
_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         2.174
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.312
_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         965
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0311
_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)+(0.0513P)²+0.0168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                847
_reflns_number_total             965
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01401j2.cif
_cod_data_source_block           clau1_5_100
_cod_depositor_comments
'Adding full bibliography for 7241824--7241862.cif.'
_cod_database_code               7241853
_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   0.514
_reflns_odcompleteness_completeness 85.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.86
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
;
_shelx_res_file
;
TITL clau1_5_100 in P21/n #14
    clau1_5_100.res
    created by SHELXL-2018/3 at 13:35:43 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.270664 12.780567 4.486851 90 94.5792 90
ZERR 4 0.000193 0.000473 0.000193 0 0.0037 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
ISOR 0.005 0.01 O3

L.S. 10 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_100.hkl">
REM </olex2.extras>

WGHT    0.051300    0.016800
FVAR       5.15739
AS1   2    0.259279    0.100267    0.042445    11.00000    0.00443    0.00895 =
         0.00374    0.00012    0.00157    0.00074
AS2   2    0.355397    0.350884    0.003884    11.00000    0.00380    0.00995 =
         0.00371   -0.00009    0.00274    0.00010
O1    1    0.432597    0.217517    0.071053    11.00000    0.00682    0.01096 =
         0.00936    0.00051    0.00013   -0.00104
O2    1    0.656710    0.399322    0.156298    11.00000    0.00673    0.01444 =
         0.00362    0.00008    0.00265   -0.00235
O3    1   -0.046095    0.141009    0.134815    11.00000    0.00849    0.01802 =
         0.00277    0.00016    0.00190    0.00228
HKLF 4




REM  clau1_5_100 in P21/n #14
REM wR2 = 0.0803, GooF = S = 1.045, Restrained GooF = 1.044 for all data
REM R1 = 0.0311 for 847 Fo > 4sig(Fo) and 0.0353 for all 965 data
REM 46 parameters refined using 6 restraints

END

WGHT      0.0510      0.0169

REM Highest difference peak  2.174,  deepest hole -1.208,  1-sigma level  0.312
Q1    1   0.2685  0.1642  0.0344  11.00000  0.05    2.17
Q2    1   0.2585  0.0372  0.0426  11.00000  0.05    2.15
Q3    1   0.3531  0.2856  0.0062  11.00000  0.05    2.04
Q4    1   0.3494  0.4127  0.0085  11.00000  0.05    1.94
Q5    1   0.6648  0.3986  0.3536  11.00000  0.05    0.97
;
_shelx_res_checksum              82459
_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 2.136
_oxdiff_exptl_absorpt_empirical_full_min 0.589
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 0.25928(7) 0.10027(3) 0.04245(8) 0.00564(13) Uani 1 1 d . . . . .
As2 As 0.35540(7) 0.35088(3) 0.00388(8) 0.00569(13) Uani 1 1 d . . . . .
O1 O 0.4326(5) 0.2175(2) 0.0711(6) 0.0091(5) Uani 1 1 d . . . . .
O2 O 0.6567(5) 0.3993(2) 0.1563(6) 0.0081(5) Uani 1 1 d . . . . .
O3 O -0.0461(6) 0.1410(2) 0.1348(6) 0.0097(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 0.0044(2) 0.0089(2) 0.0037(2) 0.00012(11) 0.00157(14) 0.00074(12)
As2 0.0038(2) 0.0099(2) 0.0037(2) -0.00009(11) 0.00274(14) 0.00010(12)
O1 0.0068(10) 0.0110(12) 0.0094(13) 0.0005(10) 0.0001(10) -0.0010(10)
O2 0.0067(12) 0.0144(12) 0.0036(13) 0.0001(9) 0.0026(10) -0.0023(10)
O3 0.0085(12) 0.0180(13) 0.0028(12) 0.0002(9) 0.0019(10) 0.0023(10)
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 100.68(13) . 4_565 ?
O1 As1 O3 102.08(12) . . ?
O3 As1 O2 90.91(13) . 4_565 ?
O1 As2 O2 94.76(12) . . ?
O1 As2 O3 97.72(13) . 4_665 ?
O3 As2 O2 91.12(13) 4_665 . ?
As1 O1 As2 134.25(16) . . ?
As1 O2 As2 124.52(15) 4_666 . ?
As1 O3 As2 124.98(17) . 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(3) . ?
As1 O2 1.773(3) 4_565 ?
As1 O3 1.772(3) . ?
As2 O1 1.773(3) . ?
As2 O2 1.789(3) . ?
As2 O3 1.778(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 -86.5(2) . . . 4_566 ?
O1 As2 O2 As1 -71.67(19) . . . 4_666 ?
O2 As1 O1 As2 60.5(2) 4_565 . . . ?
O2 As1 O3 As2 172.4(2) 4_565 . . 4_566 ?
O2 As2 O1 As1 172.0(2) . . . . ?
O3 As1 O1 As2 -32.7(3) . . . . ?
O3 As2 O1 As1 -96.2(2) 4_665 . . . ?
O3 As2 O2 As1 -169.51(19) 4_665 . . 4_666 ?
