#------------------------------------------------------------------------------
#$Date: 2015-09-05 22:32:59 +0200 (Sat 05 de Sep de 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513299.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_4513299
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                 102.53(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9307(6)
_cell_length_b                   4.51054(18)
_cell_length_c                   8.783(5)
_cell_measurement_pressure       1.30e6(5)
_cell_measurement_reflns_used    386
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.6230
_cell_measurement_theta_min      2.9690
_cell_volume                     306.70(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      He
_diffrn_ambient_pressure         1.30e6(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.399
_diffrn_measured_fraction_theta_max 0.206
_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      0.0102979000
_diffrn_orient_matrix_UB_12      -0.0070294000
_diffrn_orient_matrix_UB_13      0.0481552000
_diffrn_orient_matrix_UB_21      0.0326839000
_diffrn_orient_matrix_UB_22      -0.0707977000
_diffrn_orient_matrix_UB_23      -0.0020980000
_diffrn_orient_matrix_UB_31      0.0411039000
_diffrn_orient_matrix_UB_32      0.0581083000
_diffrn_orient_matrix_UB_33      0.0033125000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_laue_measured_fraction_full 0.399
_diffrn_reflns_laue_measured_fraction_max 0.206
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            789
_diffrn_reflns_point_group_measured_fraction_full 0.399
_diffrn_reflns_point_group_measured_fraction_max 0.206
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         21.795
_diffrn_reflns_theta_min         2.974
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    4.950
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20481
_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    4.284
_exptl_crystal_description       block
_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         1.318
_refine_diff_density_min         -1.430
_refine_diff_density_rms         0.295
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0850
_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)+(0.1610P)²+3.8550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                319
_reflns_number_total             383
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_024
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        306.72(16)
_cod_database_code               4513299
_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 38.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     15.01
_olex2_refinement_description
;
;
_shelx_res_file
;
    mclau2_024.res created by SHELXL-2014/7

TITL mclau2_024_a.res in P2(1)/n
REM Old TITL mclau2_024 in P21/n #14
CELL 0.41427 7.930652 4.510538 8.783477 90 102.5274 90
ZERR 4 0.000567 0.000184 0.004527 0 0.0213 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 $H
MORE -1
CONF
fmap 2
acta
OMIT 7 4 2
OMIT 7 4 1
OMIT 2 4 3
OMIT 8 1 2
OMIT 3 5 4
OMIT 6 5 3
OMIT 11 1 0
OMIT -5 6 2
OMIT -7 4 4
OMIT 1 6 5
OMIT -11 2 4
REM <olex2.extras>
REM <HklSrc "%./mclau2_024.hkl">
REM </olex2.extras>

WGHT    0.161000    3.855000
FVAR       4.01407
AS1   2    0.681700    0.219757    0.122514    11.00000    0.02373    0.02748 =
         0.04986    0.00134    0.00836   -0.00244
AS2   2    0.386310    0.180185    0.305688    11.00000    0.02562    0.01892 =
         0.07121    0.00091    0.01425    0.00176
O1    1    0.721856    0.375763    0.313622    11.00000    0.05045
O2    1    0.464268    0.151188    0.126839    11.00000    0.03599
O3    1    0.173632    0.061891    0.211284    11.00000    0.02487
HKLF 4

REM  mclau2_024_a.res in P2(1)/n
REM R1 =  0.0850 for     319 Fo > 4sig(Fo)  and  0.0966 for all     383 data
REM     31 parameters refined using      0 restraints

END

WGHT      0.1615      3.8445

REM Highest difference peak  1.318,  deepest hole -1.430,  1-sigma level  0.295
Q1    1   0.1165 -0.1092  0.2047  11.00000  0.05    1.32
Q2    1   0.3984  0.3819  0.3333  11.00000  0.05    1.29
Q3    1   0.6941  0.4232  0.1610  11.00000  0.05    1.12
Q4    1   0.5969  0.2458  0.1661  11.00000  0.05    1.04
Q5    1   0.5827  0.2203  0.1238  11.00000  0.05    0.97
Q6    1   0.6796  0.0193  0.1647  11.00000  0.05    0.95
Q7    1   0.5762  0.2503 -0.0521  11.00000  0.05    0.90
Q8    1   0.4761  0.2669  0.1481  11.00000  0.05    0.89
Q9    1   0.2599  0.1586  0.4467  11.00000  0.05    0.86
Q10   1   0.4737  0.3824  0.2888  11.00000  0.05    0.86
Q11   1   0.7780  0.3088 -0.0052  11.00000  0.05    0.84
Q12   1   0.7760  0.2280  0.1179  11.00000  0.05    0.82
Q13   1   0.4015  0.1965  0.5196  11.00000  0.05    0.79
Q14   1   0.5795  0.0400  0.1803  11.00000  0.05    0.79
Q15   1   0.2836  0.1764  0.2719  11.00000  0.05    0.79
Q16   1   0.1873  0.0340  0.3349  11.00000  0.05    0.78
Q17   1   0.2459  0.0437  0.1951  11.00000  0.05    0.75
Q18   1   0.5773  0.3200  0.4536  11.00000  0.05    0.75
Q19   1   0.5641  0.1707  0.0789  11.00000  0.05    0.73
Q20   1   0.6443  0.3962  0.3350  11.00000  0.05    0.70
;
_shelx_res_checksum              49618
_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 0.6817(2) 0.2198(4) 0.1225(5) 0.034(2) Uani 1 1 d
As2 As 0.3863(2) 0.1802(3) 0.3057(4) 0.038(2) Uani 1 1 d
O1 O 0.722(2) 0.376(3) 0.314(4) 0.050(4) Uiso 1 1 d
O2 O 0.4643(19) 0.151(3) 0.127(4) 0.036(3) Uiso 1 1 d
O3 O 0.1736(14) 0.062(2) 0.211(3) 0.025(2) 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 0.0237(9) 0.0275(9) 0.050(7) 0.0013(10) 0.0084(19) -0.0024(5)
As2 0.0256(10) 0.0189(8) 0.071(7) 0.0009(8) 0.0143(18) 0.0018(5)
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 94.1(8) 2_645 .
O2 As1 O1 101.4(7) . 2_645
O2 As1 O1 91.4(10) . .
O3 As2 O2 92.4(10) . .
O3 As2 O2 97.6(8) 2 .
O3 As2 O3 92.4(4) 2 .
As1 O1 As1 128.5(17) 2_655 .
As1 O2 As2 121.7(16) . .
As2 O3 As2 122.2(8) 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 1.767(19) 2_645
As1 O1 1.78(4) .
As1 O2 1.760(12) .
As2 O2 1.81(3) .
As2 O3 1.792(15) .
As2 O3 1.784(10) 2
O1 As1 1.767(19) 2_655
O3 As2 1.784(10) 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 129.7(15) 2_645 2_655
O1 As1 O2 As2 82.4(14) 2_645 .
O1 As1 O2 As2 -12.0(11) . .
O2 As1 O1 As1 -128.8(11) . 2_655
O2 As2 O3 As2 88.0(14) . 2_545
O3 As2 O2 As1 90.3(9) 2 .
O3 As2 O2 As1 -177.0(8) . .
O3 As2 O3 As2 -174(2) 2 2_545
