#------------------------------------------------------------------------------
#$Date: 2015-09-05 22:32:59 +0200 (Sat 05 de Sep de 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513295.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_4513295
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                 107.03(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3873(8)
_cell_length_b                   4.1360(2)
_cell_length_c                   7.490(4)
_cell_measurement_pressure       9.54e6(11)
_cell_measurement_reflns_used    455
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.3580
_cell_measurement_theta_min      1.4740
_cell_volume                     248.43(14)
_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         9.54e6(11)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.405
_diffrn_measured_fraction_theta_max 0.264
_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      0.0575631000
_diffrn_orient_matrix_UB_12      0.0084531000
_diffrn_orient_matrix_UB_13      0.0134811000
_diffrn_orient_matrix_UB_21      -0.0026391000
_diffrn_orient_matrix_UB_22      0.0773243000
_diffrn_orient_matrix_UB_23      0.0306807000
_diffrn_orient_matrix_UB_31      0.0044391000
_diffrn_orient_matrix_UB_32      -0.0631870000
_diffrn_orient_matrix_UB_33      0.0393064000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_laue_measured_fraction_full 0.405
_diffrn_reflns_laue_measured_fraction_max 0.264
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            681
_diffrn_reflns_point_group_measured_fraction_full 0.428
_diffrn_reflns_point_group_measured_fraction_max 0.269
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.359
_diffrn_reflns_theta_min         1.480
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    6.111
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79052
_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    5.289
_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         1.496
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.343
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         551
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0694
_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)+(0.1320P)²+1.4650P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.1919
_reflns_Friedel_coverage         0.838
_reflns_friedel_fraction_full    0.459
_reflns_friedel_fraction_max     0.275
_reflns_number_gt                495
_reflns_number_total             551
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_020_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_database_code               4513295
_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: 0.3(4) 0.7(4)
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_020_pl.res created by SHELXL-2014/7

TITL mclau2_020_a.res in P2(1)
CELL 0.41427 8.3873 4.136 7.49 90 107.03 90
ZERR 4 0.0008 0.0002 0.004 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. 10
PLAN  -20
BOND $H
CONF
MORE -1
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
OMIT 8 -3 1
OMIT -8 4 4
OMIT -13 1 6
OMIT 4 -2 0
OMIT -2 -1 2
REM <olex2.extras>
REM <HklSrc "%./mclau2_020_pl.hkl">
REM </olex2.extras>

WGHT    0.132000    1.465000
BASF   0.73296
FVAR       1.14002
AS1   1    0.372130    0.218879   -0.110502    11.00000    0.02191    0.01827 =
         0.06000    0.00559    0.01900    0.00346
AS2   1    0.117084    0.029206    0.122663    11.00000    0.02106    0.01745 =
         0.04934    0.00448    0.01267   -0.00001
O1    2    0.576593    0.309664    0.038522    11.00000    0.01683
O2    2    0.255448    0.291291    0.050301    11.00000    0.02292
O3    2   -0.038782    0.336135    0.099351    11.00000    0.02182
AS3   1    0.399161    0.605651    0.357535    11.00000    0.02196    0.02010 =
         0.07151    0.00481    0.02265    0.00148
AS4   1    0.141347    0.653355    0.574028    11.00000    0.01925    0.01948 =
         0.07951    0.00130    0.02050    0.00077
O4    2    0.527272    0.253566    0.408773    11.00000    0.01983
O5    2    0.231008    0.424695    0.424245    11.00000    0.02177
O6    2   -0.026188    0.812861    0.388159    11.00000    0.02115
HKLF 4 1 0 0 -1 0 -1 0 -1 0 0

REM  mclau2_020_a.res in P2(1)
REM R1 =  0.0694 for     495 Fo > 4sig(Fo)  and  0.0754 for all     551 data
REM     62 parameters refined using     67 restraints

END

WGHT      0.1342      2.2764

REM Highest difference peak  1.496,  deepest hole -1.359,  1-sigma level  0.343
Q1    1   0.0573  0.0165 -0.1596  11.00000  0.05    1.50
Q2    1   0.1189  0.4521 -0.4137  11.00000  0.05    1.37
Q3    1   0.4350  0.6990 -0.5319  11.00000  0.05    1.35
Q4    1   0.5784  1.1855 -0.4233  11.00000  0.05    1.33
Q5    1   0.1584  0.6211 -0.3833  11.00000  0.05    1.30
Q6    1   0.6217  0.1897 -0.2988  11.00000  0.05    1.29
Q7    1   0.1621  0.0000  0.3594  11.00000  0.05    1.25
Q8    1   0.6338  0.2011 -0.2548  11.00000  0.05    1.25
Q9    1   0.3594 -0.1914  0.4581  11.00000  0.05    1.25
Q10   1   0.4437  0.2428  0.1757  11.00000  0.05    1.24
Q11   1   0.3635  0.0642 -0.1015  11.00000  0.05    1.21
Q12   1   0.3147  0.2309 -0.3525  11.00000  0.05    1.21
Q13   1   0.1766  0.5639 -0.3092  11.00000  0.05    1.17
Q14   1   0.1003 -0.3449  0.3121  11.00000  0.05    1.16
Q15   1   0.2437  0.6645  0.5760  11.00000  0.05    1.12
Q16   1  -0.0844  0.3511  0.3894  11.00000  0.05    1.07
Q17   1   0.2802 -0.3916  0.3925  11.00000  0.05    1.04
Q18   1   0.4753  0.2031  0.4420  11.00000  0.05    1.04
Q19   1   0.2408  0.4138 -0.3798  11.00000  0.05    0.98
Q20   1   0.3024  0.3365  0.2672  11.00000  0.05    0.97
;
_shelx_res_checksum              9316
_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 0.3721(4) 0.2189(6) -0.1105(10) 0.032(3) Uani 1 1 d D
As2 As 0.1171(4) 0.0292(6) 0.1227(10) 0.029(4) Uani 1 1 d D
O1 O 0.5766(15) 0.310(3) 0.039(4) 0.017(4) Uiso 1 1 d D
O2 O 0.255(3) 0.291(4) 0.050(3) 0.023(4) Uiso 1 1 d D
O3 O -0.0388(18) 0.336(4) 0.099(2) 0.022(4) Uiso 1 1 d D
As3 As 0.3992(4) 0.6057(7) 0.3575(10) 0.036(3) Uani 1 1 d D
As4 As 0.1413(4) 0.6534(7) 0.5740(11) 0.038(3) Uani 1 1 d D
O4 O 0.527(2) 0.254(3) 0.409(2) 0.020(4) Uiso 1 1 d D
O5 O 0.231(2) 0.425(4) 0.424(4) 0.022(4) Uiso 1 1 d D
O6 O -0.0262(18) 0.813(4) 0.388(3) 0.021(4) 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 0.0219(12) 0.0183(17) 0.060(11) 0.0056(19) 0.019(3) 0.0035(11)
As2 0.0211(14) 0.0174(13) 0.049(11) 0.004(2) 0.013(3) 0.0000(11)
As3 0.0220(13) 0.0201(15) 0.072(11) 0.005(2) 0.023(3) 0.0015(13)
As4 0.0193(13) 0.0195(16) 0.080(11) 0.001(2) 0.021(3) 0.0008(12)
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
O1 As1 O1 84.8(4) 2_645
O1 As1 O2 94.9(12) 2_645
O2 As1 O1 99.1(12) .
O2 As2 O3 93.5(9) .
O3 As2 O2 94.8(8) 2_545
O3 As2 O3 99.6(6) 2_545
As1 O1 As1 119.2(8) 2_655
As2 O2 As1 129.5(10) .
As2 O3 As2 117.7(9) 2
O4 As3 O4 93.2(6) 2_656
O4 As3 O5 94.2(9) .
O4 As3 O5 86.8(9) 2_656
O6 As4 O5 94.9(11) .
O6 As4 O5 91.7(8) 2_546
O6 As4 O6 94.4(6) 2_546
As3 O4 As3 120.3(10) 2_646
As3 O5 As4 117.6(8) .
As4 O6 As4 120.5(10) 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 1.790(10) 2_645
As1 O1 1.791(10) .
As1 O2 1.786(11) .
As2 O2 1.784(10) .
As2 O3 1.794(10) .
As2 O3 1.787(11) 2_545
O1 As1 1.790(10) 2_655
O3 As2 1.787(11) 2
As3 O4 1.785(11) 2_656
As3 O4 1.784(10) .
As3 O5 1.792(10) .
As4 O5 1.792(11) .
As4 O6 1.789(11) .
As4 O6 1.777(11) 2_546
O4 As3 1.785(11) 2_646
O6 As4 1.777(11) 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 -163(3) 2_645 2_655
O1 As1 O2 As2 -39(2) 2_645 .
O1 As1 O2 As2 -124.1(18) . .
O2 As1 O1 As1 -69.1(18) . 2_655
O2 As2 O3 As2 56.5(13) . 2
O3 As2 O2 As1 -134.8(19) . .
O3 As2 O2 As1 -35(2) 2_545 .
O3 As2 O3 As2 -39.0(13) 2_545 2
O4 As3 O4 As3 23.1(10) 2_656 2_646
O4 As3 O5 As4 132.7(16) . .
O4 As3 O5 As4 39.7(16) 2_656 .
O5 As3 O4 As3 -63.9(14) . 2_646
O5 As4 O6 As4 -163.3(12) . 2_556
O6 As4 O5 As3 -169.4(16) 2_546 .
O6 As4 O5 As3 96.0(17) . .
O6 As4 O6 As4 104.7(18) 2_546 2_556
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.3(4)
2 0.7(4)
