#------------------------------------------------------------------------------
#$Date: 2015-09-05 23:32:59 +0300 (Sat, 05 Sep 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513293.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_4513293
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         '0.5(As4 O6)'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 106.84(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3192(9)
_cell_length_b                   4.0286(2)
_cell_length_c                   7.298(3)
_cell_measurement_pressure       1.444e7(5)
_cell_measurement_reflns_used    389
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.2780
_cell_measurement_theta_min      1.4860
_cell_volume                     234.10(11)
_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)'
_diffrn_ambient_environment      He
_diffrn_ambient_pressure         1.444e7(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.405
_diffrn_measured_fraction_theta_max 0.256
_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      -0.0590319000
_diffrn_orient_matrix_UB_12      0.0078491000
_diffrn_orient_matrix_UB_13      -0.0138974000
_diffrn_orient_matrix_UB_21      0.0029250000
_diffrn_orient_matrix_UB_22      0.0833130000
_diffrn_orient_matrix_UB_23      -0.0284288000
_diffrn_orient_matrix_UB_31      -0.0036277000
_diffrn_orient_matrix_UB_32      -0.0599152000
_diffrn_orient_matrix_UB_33      -0.0413079000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_unetI/netI     0.0809
_diffrn_reflns_laue_measured_fraction_full 0.405
_diffrn_reflns_laue_measured_fraction_max 0.256
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            682
_diffrn_reflns_point_group_measured_fraction_full 0.433
_diffrn_reflns_point_group_measured_fraction_max 0.263
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.655
_diffrn_reflns_theta_min         1.491
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    6.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38058
_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    5.613
_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         1.736
_refine_diff_density_min         -1.804
_refine_diff_density_rms         0.426
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         532
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0867
_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)+(0.1700P)²+3.8330P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2291
_refine_ls_wR_factor_ref         0.2406
_reflns_Friedel_coverage         0.846
_reflns_friedel_fraction_full    0.471
_reflns_friedel_fraction_max     0.270
_reflns_number_gt                484
_reflns_number_total             532
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_018_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_database_code               4513293
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.0(5) 0.0(5)
2. Restrained distances
 As1-O1 \\sim As1-O2 \\sim As2-O2 \\sim As2-O3 \\sim As3-O4 \\sim As3-O5 \\sim
As4-O5 \\sim As4-O6 \\sim As1-
 O1 \\sim As1-O1 \\sim As1-O1_$1 \\sim As2-O3_$2 \\sim As3-O4_$3 \\sim As4-O6_$4
 with sigma of 0.01
;
_shelx_res_file
;
    mclau2_018_pl.res created by SHELXL-2014/7

TITL mclau2_018_a.res in P2(1)
CELL 0.41427 8.3192 4.0286 7.298 90 106.84 90
ZERR 4 0.0009 0.0002 0.003 0 0.03 0
LATT -1
SYMM -X,0.5+Y,-Z
SFAC As O
DISP As 0.311 0.799 1882.762
DISP O 0.002 0.002 10.067
UNIT 8 12
EQIV $1 1-X,-0.5+Y,-Z
EQIV $2 -X,-0.5+Y,-Z
EQIV $3 1-X,0.5+Y,1-Z
EQIV $4 -X,-0.5+Y,1-Z
SADI 0.01 As1 O1 As1 O2 As2 O2 As2 O3 As3 O4 As3 O5 As4 O5 As4 O6 As1 O1 As1 =
 O1 AS1 O1_$1 AS2 O3_$2 AS3 O4_$3 AS4 O6_$4

L.S. 25
PLAN  -20
BOND $H
CONF
MORE -1
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
OMIT -8 4 4
OMIT 8 -3 1
OMIT 4 -2 0
OMIT -7 3 3
REM <olex2.extras>
REM <HklSrc "%./mclau2_018_pl.hkl">
REM </olex2.extras>

WGHT    0.170000    3.833000
BASF   0.04243
FVAR       1.29702
AS1   1    0.370836    0.228723   -0.113849    11.00000    0.02585    0.01875 =
         0.03813    0.00400    0.02067    0.00362
AS2   1    0.119502    0.017424    0.126853    11.00000    0.02300    0.01884 =
         0.02272    0.00122    0.00964   -0.00086
O1    2    0.577750    0.306816    0.042265    11.00000    0.02050
O2    2    0.257712    0.299972    0.057049    11.00000    0.02101
O3    2   -0.035773    0.335728    0.105866    11.00000    0.03027
AS3   1    0.398636    0.601039    0.352918    11.00000    0.02380    0.02090 =
         0.02265    0.00497    0.01377   -0.00019
AS4   1    0.143591    0.656726    0.574399    11.00000    0.02175    0.02033 =
         0.04980    0.00240    0.01633    0.00132
O4    2    0.528171    0.237841    0.403066    11.00000    0.01976
O5    2    0.230983    0.408696    0.422733    11.00000    0.02203
O6    2   -0.024808    0.812391    0.379995    11.00000    0.02430
HKLF 4 1 0 0 -1 0 -1 0 -1 0 0

REM  mclau2_018_a.res in P2(1)
REM R1 =  0.0867 for     484 Fo > 4sig(Fo)  and  0.0943 for all     532 data
REM     62 parameters refined using     67 restraints

END

WGHT      0.1715      3.8433

REM Highest difference peak  1.736,  deepest hole -1.804,  1-sigma level  0.426
Q1    1   0.0935 -0.1504 -0.3550  11.00000  0.05    1.56
Q2    1   0.3597 -0.5848 -0.5488  11.00000  0.05    1.48
Q3    1   0.2042 -0.0881 -0.4052  11.00000  0.05    1.46
Q4    1   0.4359  0.1091  0.0813  11.00000  0.05    1.42
Q5    1   0.0984 -0.2555  0.4216  11.00000  0.05    1.42
Q6    1   0.2003 -0.2553 -0.2813  11.00000  0.05    1.39
Q7    1   0.3456 -0.1600  0.3991  11.00000  0.05    1.38
Q8    1   0.3417  0.0268 -0.0730  11.00000  0.05    1.37
Q9    1   0.4466  0.4462 -0.1089  11.00000  0.05    1.34
Q10   1   0.0996  0.4372 -0.4270  11.00000  0.05    1.27
Q11   1   0.1463  0.1081  0.2572  11.00000  0.05    1.23
Q12   1   0.1177  0.3776 -0.2744  11.00000  0.05    1.22
Q13   1   0.2223  0.6436  0.5225  11.00000  0.05    1.22
Q14   1   0.5569  0.4729  0.1190  11.00000  0.05    1.20
Q15   1   0.4846  0.2288  0.2367  11.00000  0.05    1.19
Q16   1   0.5171  0.0933 -0.3112  11.00000  0.05    1.19
Q17   1   0.2386  0.6238 -0.4243  11.00000  0.05    1.18
Q18   1   0.1746  0.5013  0.4270  11.00000  0.05    1.15
Q19   1   0.6367  0.1112  0.0398  11.00000  0.05    1.14
Q20   1   0.6202  0.0909 -0.0101  11.00000  0.05    1.13
;
_shelx_res_checksum              882
_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, y+1/2, -z'
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
As1 As 0.3708(5) 0.2287(8) -0.1138(13) 0.025(4) Uani 1 1 d D
As2 As 0.1195(4) 0.0174(8) 0.1269(12) 0.021(4) Uani 1 1 d D
O1 O 0.5778(19) 0.307(4) 0.042(5) 0.021(5) Uiso 1 1 d D
O2 O 0.258(3) 0.300(5) 0.057(4) 0.021(5) Uiso 1 1 d D
O3 O -0.036(2) 0.336(5) 0.106(3) 0.030(6) Uiso 1 1 d D
As3 As 0.3986(5) 0.6010(10) 0.3529(12) 0.021(4) Uani 1 1 d D
As4 As 0.1436(5) 0.6567(9) 0.5744(15) 0.029(4) Uani 1 1 d D
O4 O 0.528(2) 0.238(4) 0.403(2) 0.020(5) Uiso 1 1 d D
O5 O 0.231(3) 0.409(5) 0.423(4) 0.022(5) Uiso 1 1 d D
O6 O -0.025(2) 0.812(5) 0.380(3) 0.024(5) Uiso 1 1 d 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 0.0259(17) 0.0187(17) 0.038(13) 0.004(2) 0.021(4) 0.0036(14)
As2 0.0230(17) 0.0188(15) 0.023(14) 0.001(3) 0.010(4) -0.0009(14)
As3 0.0238(16) 0.0209(16) 0.023(12) 0.005(2) 0.014(4) -0.0002(14)
As4 0.0218(16) 0.0203(17) 0.050(14) 0.002(2) 0.016(4) 0.0013(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
As As 0.3110 0.7990 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0020 0.0020 '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 83.0(4) 2_645 .
O2 As1 O1 94.5(14) . 2_645
O2 As1 O1 97.5(14) . .
O2 As2 O3 95.5(9) . 2_545
O3 As2 O2 91.6(10) . .
O3 As2 O3 97.9(7) . 2_545
As1 O1 As1 117.1(10) 2_655 .
As1 O2 As2 127.3(11) . .
As2 O3 As2 116.4(11) . 2
O4 As3 O4 92.1(7) . 2_656
O4 As3 O5 93.5(11) . .
O5 As3 O4 85.4(11) . 2_656
O6 As4 O5 94.0(13) . .
O6 As4 O5 91.6(10) 2_546 .
O6 As4 O6 94.1(8) 2_546 .
As3 O4 As3 117.7(11) . 2_646
As3 O5 As4 115.0(9) . .
As4 O6 As4 118.1(11) 2_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 O1 1.793(11) 2_645
As1 O1 1.795(12) .
As1 O2 1.790(12) .
As2 O2 1.793(11) .
As2 O3 1.794(12) 2_545
As2 O3 1.795(11) .
O1 As1 1.793(11) 2_655
O3 As2 1.794(12) 2
As3 O4 1.791(11) .
As3 O4 1.794(12) 2_656
As3 O5 1.794(11) .
As4 O5 1.794(12) .
As4 O6 1.794(13) .
As4 O6 1.789(12) 2_546
O4 As3 1.794(12) 2_646
O6 As4 1.789(12) 2_556
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 -165(3) 2_645 2_655
O1 As1 O2 As2 -39(2) 2_645 .
O1 As1 O2 As2 -122.8(19) . .
O2 As1 O1 As1 -71(2) . 2_655
O2 As2 O3 As2 61.0(17) . 2
O3 As2 O2 As1 -36(2) 2_545 .
O3 As2 O2 As1 -134(2) . .
O3 As2 O3 As2 -34.8(16) 2_545 2
O4 As3 O4 As3 20.5(11) 2_656 2_646
O4 As3 O5 As4 134.2(18) . .
O4 As3 O5 As4 42.4(19) 2_656 .
O5 As3 O4 As3 -64.9(16) . 2_646
O5 As4 O6 As4 -167.1(14) . 2_556
O6 As4 O5 As3 -170.2(19) 2_546 .
O6 As4 O5 As3 96(2) . .
O6 As4 O6 As4 101(2) 2_546 2_556
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.0(5)
2 0.0(5)
