#------------------------------------------------------------------------------
#$Date: 2015-09-05 23:32:59 +0300 (Sat, 05 Sep 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/33/4513300.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_4513300
loop_
_publ_author_name
'Guńka, Piotr A.'
'Dranka, Maciej'
'Hanfland, Michael'
'Dziubek, Kamil F.'
'Katrusiak, Andrzej'
'Zachara, Janusz'
_publ_section_title
;
 Cascade of High-Pressure Transitions of Claudetite II and the First Polar
 Phase of Arsenic(III) Oxide
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3950
_journal_paper_doi               10.1021/acs.cgd.5b00567
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-13
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.11.28 svn.r3107 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.65(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0290(6)
_cell_length_b                   4.57732(16)
_cell_length_c                   9.141(5)
_cell_measurement_pressure       100(1)
_cell_measurement_reflns_used    434
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.8580
_cell_measurement_theta_min      2.9120
_cell_volume                     329.02(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      He
_diffrn_ambient_pressure         100(1)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.419
_diffrn_measured_fraction_theta_max 0.268
_diffrn_measurement_details
;
  1 phi    142.00  218.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
   0.0000    0.0000    0.0000     -     152
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'MAR-CrysAlisPro-abstract goniometer: imported MAR images'
_diffrn_measurement_method       'π scans'
_diffrn_orient_matrix_UB_11      0.0095115000
_diffrn_orient_matrix_UB_12      -0.0067822000
_diffrn_orient_matrix_UB_13      0.0460753000
_diffrn_orient_matrix_UB_21      0.0273794000
_diffrn_orient_matrix_UB_22      -0.0760473000
_diffrn_orient_matrix_UB_23      -0.0023927000
_diffrn_orient_matrix_UB_31      0.0440139000
_diffrn_orient_matrix_UB_32      0.0487234000
_diffrn_orient_matrix_UB_33      0.0026244000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_laue_measured_fraction_full 0.419
_diffrn_reflns_laue_measured_fraction_max 0.268
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            845
_diffrn_reflns_point_group_measured_fraction_full 0.419
_diffrn_reflns_point_group_measured_fraction_max 0.268
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.543
_diffrn_reflns_theta_min         2.913
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    4.615
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    3.994
_exptl_crystal_description
;
;
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.557
_refine_diff_density_min         -1.776
_refine_diff_density_rms         0.331
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.1051
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2772
_refine_ls_wR_factor_ref         0.2894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                399
_reflns_number_total             448
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_025
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        329.00(18)
_cod_database_code               4513300
_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.
;
_reflns_odcompleteness_completeness 39.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     15.01
_olex2_refinement_description
;
;
_shelx_res_file
;
    mclau2_025.res created by SHELXL-2014/7

TITL mclau2_025 in P21/n #14
REM reset to P21/n #14
CELL 0.41427 8.028982 4.577323 9.140534 90 101.6522 90
ZERR 4 0.000633 0.000164 0.005018 0 0.0241 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.311 0.799 1882.762
DISP O 0.002 0.002 10.067
UNIT 12 8

L.S. 10
PLAN  20
BOND
MORE -1
BOND $H
CONF
fmap 2
acta
OMIT -8 4 2
OMIT 11 2 0
OMIT 13 1 0
OMIT -5 2 2
OMIT -3 1 1
OMIT -4 0 0
OMIT -6 1 0
OMIT -8 3 4
OMIT -4 2 -1
REM <olex2.extras>
REM <HklSrc "%./mclau2_025.hkl">
REM </olex2.extras>

WGHT    0.200000
FVAR       8.09381
AS1   2    0.683802    0.208294    0.128559    11.00000    0.03302    0.02764 =
         0.09834    0.00251    0.02281   -0.00201
AS2   2    0.384428    0.168356    0.302457    11.00000    0.03288    0.02368 =
         0.09635    0.00183    0.02094    0.00139
O1    1    0.732417    0.361254    0.314833    11.00000    0.05224
O2    1    0.468848    0.145074    0.141365    11.00000    0.03846
O3    1    0.173692    0.041845    0.205351    11.00000    0.03076
HKLF 4

REM  mclau2_025 in P21/n #14
REM R1 =  0.1051 for     399 Fo > 4sig(Fo)  and  0.1104 for all     448 data
REM     31 parameters refined using      0 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  2.557,  deepest hole -1.776,  1-sigma level  0.331
Q1    1   0.1122 -0.1070  0.1955  11.00000  0.05    1.15
Q2    1   0.4632  0.2515  0.1381  11.00000  0.05    1.13
Q3    1   0.4375 -0.0310  0.2987  11.00000  0.05    1.12
Q4    1   0.7206  0.5374  0.3506  11.00000  0.05    1.03
Q5    1   0.5765  0.0825  0.1343  11.00000  0.05    0.98
Q6    1   0.7023  0.5555  0.3176  11.00000  0.05    0.93
Q7    1   0.6000  0.3151  0.4535  11.00000  0.05    0.88
Q8    1   0.1968 -0.1574  0.2086  11.00000  0.05    0.88
Q9    1   0.4735  0.3053 -0.0001  11.00000  0.05    0.87
Q10   1   0.6324 -0.0380  0.1266  11.00000  0.05    0.84
Q11   1   0.3234 -0.0394  0.2864  11.00000  0.05    0.83
Q12   1   0.4798  0.3480  0.3102  11.00000  0.05    0.82
Q13   1   0.1981  0.0127  0.3389  11.00000  0.05    0.82
Q14   1   0.5965  0.3177 -0.0105  11.00000  0.05    0.81
Q15   1   0.2792  0.1639  0.3031  11.00000  0.05    0.79
Q16   1  -0.0444  0.1873  0.2642  11.00000  0.05    0.79
Q17   1   0.4732  0.0881  0.4306  11.00000  0.05    0.78
Q18   1   0.7939  0.1739  0.1083  11.00000  0.05    0.77
Q19   1   0.6969  0.3954  0.0407  11.00000  0.05    0.76
Q20   1   0.7545  0.3197 -0.0325  11.00000  0.05    0.73
;
_shelx_res_checksum              53117
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
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
As1 As 0.68380(19) 0.2083(3) 0.1286(4) 0.052(2) Uani 1 1 d
As2 As 0.38443(17) 0.1684(3) 0.3025(4) 0.050(2) Uani 1 1 d
O1 O 0.7324(18) 0.361(3) 0.315(4) 0.052(3) Uiso 1 1 d
O2 O 0.4688(14) 0.145(2) 0.141(3) 0.038(2) Uiso 1 1 d
O3 O 0.1737(11) 0.0418(18) 0.205(3) 0.0308(19) Uiso 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 0.0330(9) 0.0276(8) 0.098(7) 0.0025(9) 0.0228(16) -0.0020(4)
As2 0.0329(9) 0.0237(8) 0.096(7) 0.0018(8) 0.0209(17) 0.0014(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.3110 0.7990 '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
O1 As1 O1 94.3(7) 2_645 .
O2 As1 O1 98.8(6) . 2_645
O2 As1 O1 91.7(9) . .
O3 As2 O2 92.9(8) . .
O3 As2 O2 99.7(8) 2 .
O3 As2 O3 94.3(4) 2 .
As1 O1 As1 128.5(16) 2_655 .
As1 O2 As2 126.4(13) . .
As2 O3 As2 122.2(7) 2_545 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 O1 1.762(16) 2_645
As1 O1 1.81(3) .
As1 O2 1.777(10) .
As2 O2 1.74(2) .
As2 O3 1.838(13) .
As2 O3 1.770(8) 2
O1 As1 1.762(16) 2_655
O3 As2 1.770(8) 2_545
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_4
O1 As1 O1 As1 137.9(12) 2_645 2_655
O1 As1 O2 As2 83.3(14) 2_645 .
O1 As1 O2 As2 -11.3(10) . .
O2 As1 O1 As1 -123.2(10) . 2_655
O2 As2 O3 As2 91.7(12) . 2_545
O3 As2 O2 As1 89.4(9) 2 .
O3 As2 O2 As1 -175.8(8) . .
O3 As2 O3 As2 -168.3(18) 2 2_545
