#------------------------------------------------------------------------------
#$Date: 2021-02-05 00:04:31 +0100 (vie 05 de feb de 2021) $
#$Revision: 261628 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/18/7241857.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_7241857
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                 94.738(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.26753(12)
_cell_length_b                   12.7667(2)
_cell_length_c                   4.48007(10)
_cell_measurement_reflns_used    6302
_cell_measurement_temperature    50(1)
_cell_measurement_theta_max      31.1330
_cell_measurement_theta_min      1.8360
_cell_volume                     300.251(11)
_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      50(1)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.859
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.48   0.50    0.30 154.30  25.00  73.80    --   720
  2  φ    -25.74 154.37   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      -0.0431965805
_diffrn_orient_matrix_UB_12      -0.0165940599
_diffrn_orient_matrix_UB_13      0.0566853484
_diffrn_orient_matrix_UB_21      0.0295742595
_diffrn_orient_matrix_UB_22      -0.0277261924
_diffrn_orient_matrix_UB_23      -0.0297013967
_diffrn_orient_matrix_UB_31      0.0588030224
_diffrn_orient_matrix_UB_32      0.0017498966
_diffrn_orient_matrix_UB_33      0.0669306143
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.859
_diffrn_reflns_Laue_measured_fraction_max 0.903
_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            3960
_diffrn_reflns_point_group_measured_fraction_full 0.859
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.466
_diffrn_reflns_theta_min         1.855
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    22.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55717
_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    4.377
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.178
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0509P)²+0.0508P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                816
_reflns_number_total             883
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01401j2.cif
_cod_data_source_block           clau1_1_50
_cod_depositor_comments
'Adding full bibliography for 7241824--7241862.cif.'
_cod_original_cell_volume        300.252(11)
_cod_database_code               7241857
_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 86.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     14.97
_olex2_refinement_description
;
;
_shelx_res_file
;
TITL clau1_1_50 in P21/n #14
    clau1_1_50.res
    created by SHELXL-2018/3 at 13:46:20 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.267534 12.766744 4.480071 90 94.7383 90
ZERR 4 0.000122 0.000248 0.0001 0 0.0023 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 0.002 0.018 0.04
CONF
fmap 2 53
MORE -1
ACTA
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_1_50.hkl">
REM </olex2.extras>

WGHT    0.050900    0.050800
FVAR       8.48909
AS1   2    0.259316    0.100137    0.042559    11.00000    0.00352    0.00492 =
         0.00135    0.00000    0.00052    0.00047
AS2   2    0.355285    0.351002    0.003703    11.00000    0.00322    0.00551 =
         0.00112    0.00006    0.00131    0.00002
O1    1    0.433441    0.217507    0.072135    11.00000    0.00645    0.00706 =
         0.00616    0.00156    0.00012   -0.00008
O2    1    0.657333    0.399278    0.156695    11.00000    0.00481    0.00969 =
         0.00106    0.00026    0.00021   -0.00229
O3    1   -0.047123    0.140915    0.133886    11.00000    0.00423    0.01247 =
         0.00150    0.00020    0.00094    0.00177
HKLF 4




REM  clau1_1_50 in P21/n #14
REM wR2 = 0.0761, GooF = S = 1.131, Restrained GooF = 1.131 for all data
REM R1 = 0.0271 for 816 Fo > 4sig(Fo) and 0.0291 for all 883 data
REM 46 parameters refined using 0 restraints

END

WGHT      0.0509      0.0508

REM Highest difference peak  1.178,  deepest hole -1.125,  1-sigma level  0.246
Q1    1   0.3343  0.0596  0.1201  11.00000  0.05    1.18
Q2    1   0.2871  0.3156 -0.0934  11.00000  0.05    0.95
Q3    1   0.2387  0.3822 -0.0735  11.00000  0.05    0.87
Q4    1   0.3575  0.1385  0.1128  11.00000  0.05    0.81
Q5    1   0.0838  0.1034 -0.0586  11.00000  0.05    0.79
;
_shelx_res_checksum              7671
_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 1.733
_oxdiff_exptl_absorpt_empirical_full_min 0.486
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 0.25932(5) 0.10014(2) 0.04256(6) 0.00325(13) Uani 1 1 d . . . . .
As2 As 0.35529(5) 0.35100(2) 0.00370(6) 0.00322(13) Uani 1 1 d . . . . .
O1 O 0.4334(4) 0.21751(15) 0.0721(5) 0.0066(4) Uani 1 1 d . . . . .
O2 O 0.6573(4) 0.39928(14) 0.1567(5) 0.0052(4) Uani 1 1 d . . . . .
O3 O -0.0471(4) 0.14092(16) 0.1339(5) 0.0060(4) 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 0.00352(18) 0.00492(18) 0.00135(19) 0.00000(8) 0.00052(12) 0.00047(8)
As2 0.00322(18) 0.00551(18) 0.00112(18) 0.00006(8) 0.00131(12) 0.00002(8)
O1 0.0065(8) 0.0071(8) 0.0062(9) 0.0016(7) 0.0001(7) -0.0001(7)
O2 0.0048(8) 0.0097(8) 0.0011(9) 0.0003(6) 0.0002(7) -0.0023(6)
O3 0.0042(8) 0.0125(9) 0.0015(9) 0.0002(7) 0.0009(7) 0.0018(7)
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 100.65(9) . 4_565 ?
O1 As1 O3 102.21(9) . . ?
O2 As1 O3 90.89(10) 4_565 . ?
O1 As2 O2 94.50(9) . . ?
O1 As2 O3 97.81(9) . 4_665 ?
O3 As2 O2 91.18(9) 4_665 . ?
As1 O1 As2 133.98(12) . . ?
As1 O2 As2 124.40(11) 4_666 . ?
As1 O3 As2 124.76(12) . 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 1.7561(19) . ?
As1 O2 1.767(2) 4_565 ?
As1 O3 1.7757(19) . ?
As2 O1 1.7740(19) . ?
As2 O2 1.789(2) . ?
As2 O3 1.778(2) 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 -86.36(15) . . . 4_566 ?
O1 As2 O2 As1 -71.81(14) . . . 4_666 ?
O2 As1 O1 As2 60.44(17) 4_565 . . . ?
O2 As1 O3 As2 172.54(14) 4_565 . . 4_566 ?
O2 As2 O1 As1 172.21(16) . . . . ?
O3 As1 O1 As2 -32.82(18) . . . . ?
O3 As2 O1 As1 -95.98(16) 4_665 . . . ?
O3 As2 O2 As1 -169.75(13) 4_665 . . 4_666 ?
