#------------------------------------------------------------------------------
#$Date: 2015-09-05 23:32:59 +0300 (Sat, 05 Sep 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513296.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_4513296
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                 107.025(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4114(5)
_cell_length_b                   4.18950(10)
_cell_length_c                   7.614(3)
_cell_measurement_pressure       7.42e6(37)
_cell_measurement_reflns_used    464
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.2810
_cell_measurement_theta_min      1.4750
_cell_volume                     256.56(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         7.42e6(37)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.402
_diffrn_measured_fraction_theta_max 0.260
_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      0.0567506000
_diffrn_orient_matrix_UB_12      0.0080716000
_diffrn_orient_matrix_UB_13      0.0134075000
_diffrn_orient_matrix_UB_21      -0.0023811000
_diffrn_orient_matrix_UB_22      0.0762566000
_diffrn_orient_matrix_UB_23      0.0306251000
_diffrn_orient_matrix_UB_31      0.0043023000
_diffrn_orient_matrix_UB_32      -0.0623591000
_diffrn_orient_matrix_UB_33      0.0391316000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_laue_measured_fraction_full 0.402
_diffrn_reflns_laue_measured_fraction_max 0.260
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            700
_diffrn_reflns_point_group_measured_fraction_full 0.426
_diffrn_reflns_point_group_measured_fraction_max 0.264
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.540
_diffrn_reflns_theta_min         1.476
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    5.918
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17231
_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    5.122
_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         1.443
_refine_diff_density_min         -1.366
_refine_diff_density_rms         0.373
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         560
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0833
_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)+(0.1540P)²+3.2490P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2236
_refine_ls_wR_factor_ref         0.2288
_reflns_Friedel_coverage         0.840
_reflns_friedel_fraction_full    0.458
_reflns_friedel_fraction_max     0.270
_reflns_number_gt                504
_reflns_number_total             560
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_021_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_database_code               4513296
_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: 0.0(5) 1.0(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_021_pl.res created by SHELXL-2014/7

TITL mclau2_021_a.res in P2(1)
rem BASF 0.9
rem TWIN -1 0 0 0 -1 0 0 0 -1 2
CELL 0.41427 8.4114 4.1895 7.614 90 107.025 90
ZERR 4 0.0005 0.0001 0.003 0 0.019 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 4 -2 0
OMIT -6 -4 4
OMIT 1 7 2
OMIT -2 -1 2
REM <olex2.extras>
REM <HklSrc "%./mclau2_021_pl.hkl">
REM </olex2.extras>

WGHT    0.154000    3.249000
BASF   0.96583
FVAR       7.67553
AS1   1    0.372948    0.215479   -0.106334    11.00000    0.02750    0.02400 =
         0.04905    0.00459    0.01505    0.00383
AS2   1    0.115646    0.034340    0.120626    11.00000    0.02544    0.02386 =
         0.02651    0.00295    0.00483   -0.00111
O1    2    0.574764    0.310804    0.040861    11.00000    0.02498
O2    2    0.257113    0.287633    0.051513    11.00000    0.02932
O3    2   -0.038203    0.338111    0.094969    11.00000    0.02506
AS3   1    0.399001    0.609327    0.360692    11.00000    0.02825    0.02713 =
         0.03764    0.00652    0.01376    0.00190
AS4   1    0.139793    0.648831    0.571976    11.00000    0.02514    0.02703 =
         0.03033    0.00176    0.00853   -0.00051
O4    2    0.526899    0.263377    0.411875    11.00000    0.02978
O5    2    0.229529    0.432788    0.422132    11.00000    0.03019
O6    2   -0.028406    0.806202    0.391277    11.00000    0.02580
HKLF 4 1 0 0 -1 0 -1 0 -1 0 0

REM  mclau2_021_a.res in P2(1)
REM R1 =  0.0833 for     504 Fo > 4sig(Fo)  and  0.0874 for all     560 data
REM     62 parameters refined using     67 restraints

END

WGHT      0.1680      2.5053

REM Highest difference peak  1.443,  deepest hole -1.366,  1-sigma level  0.373
Q1    1   0.3596 -0.2007  0.4494  11.00000  0.05    1.44
Q2    1   0.5581  0.5099  0.1454  11.00000  0.05    1.41
Q3    1   0.1161  0.4600 -0.4113  11.00000  0.05    1.30
Q4    1   0.1950  0.6483 -0.1323  11.00000  0.05    1.24
Q5    1   0.4545  0.0030 -0.1023  11.00000  0.05    1.23
Q6    1   0.3027  0.2179 -0.3912  11.00000  0.05    1.21
Q7    1   0.0635  0.0278 -0.1660  11.00000  0.05    1.20
Q8    1   0.1184  0.4219 -0.2343  11.00000  0.05    1.15
Q9    1   0.3190  0.3167  0.0186  11.00000  0.05    1.13
Q10   1   0.0036  0.4233  0.0791  11.00000  0.05    1.10
Q11   1   0.0457  0.0078 -0.2286  11.00000  0.05    1.10
Q12   1   0.6048  0.4601 -0.2624  11.00000  0.05    1.09
Q13   1   0.1800  0.4327  0.3327  11.00000  0.05    1.06
Q14   1   0.4621  0.2052 -0.1216  11.00000  0.05    1.04
Q15   1   0.4357  0.6070 -0.3756  11.00000  0.05    1.03
Q16   1   0.2257 -0.1138 -0.3839  11.00000  0.05    1.01
Q17   1   0.0430 -0.0806  0.3155  11.00000  0.05    1.00
Q18   1   0.4759  0.0842  0.0854  11.00000  0.05    1.00
Q19   1   0.3421  0.0783  0.0586  11.00000  0.05    0.98
Q20   1   0.2581  0.3484  0.4628  11.00000  0.05    0.96
;
_shelx_res_checksum              34110
_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 0.3729(4) 0.2155(7) -0.1063(11) 0.033(4) Uani 1 1 d D
As2 As 0.1156(4) 0.0343(7) 0.1206(12) 0.026(4) Uani 1 1 d D
O1 O 0.5748(17) 0.311(3) 0.041(4) 0.025(4) Uiso 1 1 d D
O2 O 0.257(3) 0.288(4) 0.052(4) 0.029(5) Uiso 1 1 d D
O3 O -0.038(2) 0.338(4) 0.095(2) 0.025(4) Uiso 1 1 d D
As3 As 0.3990(4) 0.6093(8) 0.3607(11) 0.030(4) Uani 1 1 d D
As4 As 0.1398(4) 0.6488(7) 0.5720(12) 0.027(4) Uani 1 1 d D
O4 O 0.527(2) 0.263(4) 0.412(2) 0.030(5) Uiso 1 1 d D
O5 O 0.230(3) 0.433(5) 0.422(4) 0.030(5) Uiso 1 1 d D
O6 O -0.028(2) 0.806(4) 0.391(3) 0.026(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 0.0275(14) 0.0240(17) 0.049(13) 0.005(2) 0.015(4) 0.0038(13)
As2 0.0254(15) 0.0239(15) 0.027(12) 0.003(2) 0.005(4) -0.0011(12)
As3 0.0283(14) 0.0271(17) 0.038(12) 0.007(2) 0.014(4) 0.0019(15)
As4 0.0251(14) 0.0270(18) 0.030(11) 0.002(2) 0.009(3) -0.0005(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
_geom_angle_site_symmetry_3
O1 As1 O1 85.7(4) . 2_645
O2 As1 O1 96.4(14) . 2_645
O2 As1 O1 98.4(14) . .
O3 As2 O2 95.6(9) 2_545 .
O3 As2 O2 93.9(10) . .
O3 As2 O3 99.8(6) 2_545 .
As1 O1 As1 119.9(10) . 2_655
As1 O2 As2 129.9(12) . .
As2 O3 As2 119.2(11) 2 .
O4 As3 O4 93.7(7) 2_656 .
O4 As3 O5 88.5(9) 2_656 .
O4 As3 O5 94.8(11) . .
O5 As4 O6 94.7(13) . .
O6 As4 O5 91.8(9) 2_546 .
O6 As4 O6 94.8(7) 2_546 .
As3 O4 As3 121.7(12) 2_646 .
As3 O5 As4 118.4(10) . .
As4 O6 As4 120.7(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 1.784(11) .
As1 O1 1.785(10) 2_645
As1 O2 1.781(11) .
As2 O2 1.785(10) .
As2 O3 1.784(10) .
As2 O3 1.780(12) 2_545
O1 As1 1.785(10) 2_655
O3 As2 1.780(12) 2
As3 O4 1.781(12) 2_656
As3 O4 1.779(10) .
As3 O5 1.786(10) .
As4 O5 1.787(11) .
As4 O6 1.786(12) .
As4 O6 1.780(11) 2_546
O4 As3 1.781(12) 2_646
O6 As4 1.780(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 -167(3) 2_645 2_655
O1 As1 O2 As2 -40(2) 2_645 .
O1 As1 O2 As2 -126(2) . .
O2 As1 O1 As1 -71(2) . 2_655
O2 As2 O3 As2 56.2(16) . 2
O3 As2 O2 As1 -133(2) . .
O3 As2 O2 As1 -33(2) 2_545 .
O3 As2 O3 As2 -40.2(14) 2_545 2
O4 As3 O4 As3 24.7(13) 2_656 2_646
O4 As3 O5 As4 131.0(19) . .
O4 As3 O5 As4 37(2) 2_656 .
O5 As3 O4 As3 -64.2(17) . 2_646
O5 As4 O6 As4 -160.3(14) . 2_556
O6 As4 O5 As3 -167.2(19) 2_546 .
O6 As4 O5 As3 97.8(19) . .
O6 As4 O6 As4 107(2) 2_546 2_556
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.0(5)
2 1.0(5)
