#------------------------------------------------------------------------------
#$Date: 2015-09-05 22:32:59 +0200 (Sat 05 de Sep de 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513291.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_4513291
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                 106.91(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3494(10)
_cell_length_b                   4.0797(2)
_cell_length_c                   7.388(5)
_cell_measurement_pressure       1.195e7(5)
_cell_measurement_reflns_used    310
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.6600
_cell_measurement_theta_min      1.4820
_cell_volume                     240.78(17)
_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         1.195e7(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.425
_diffrn_measured_fraction_theta_max 0.216
_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      0.0584491000
_diffrn_orient_matrix_UB_12      0.0073258000
_diffrn_orient_matrix_UB_13      0.0139978000
_diffrn_orient_matrix_UB_21      -0.0027099000
_diffrn_orient_matrix_UB_22      0.0818863000
_diffrn_orient_matrix_UB_23      0.0285663000
_diffrn_orient_matrix_UB_31      0.0034558000
_diffrn_orient_matrix_UB_32      -0.0596044000
_diffrn_orient_matrix_UB_33      0.0409397000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.1089
_diffrn_reflns_laue_measured_fraction_full 0.425
_diffrn_reflns_laue_measured_fraction_max 0.216
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_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            726
_diffrn_reflns_point_group_measured_fraction_full 0.453
_diffrn_reflns_point_group_measured_fraction_max 0.220
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         22.151
_diffrn_reflns_theta_min         1.486
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    6.306
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08910
_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    5.458
_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         2.560
_refine_diff_density_min         -2.280
_refine_diff_density_rms         0.520
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         562
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.1068
_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)+(0.1645P)²+6.9951P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2565
_refine_ls_wR_factor_ref         0.2726
_reflns_Friedel_coverage         0.854
_reflns_friedel_fraction_full    0.490
_reflns_friedel_fraction_max     0.226
_reflns_number_gt                449
_reflns_number_total             562
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_016_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_database_code               4513291
_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: 0.6(6) 0.4(6)
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_016_pl.res created by SHELXL-2014/7

TITL mclau2_016_a.res in P2(1)
CELL 0.41427 8.3494 4.0797 7.388 90 106.91 90
ZERR 4 0.001 0.0002 0.005 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. 30
PLAN  -20
BOND $H
CONF
MORE -1
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
OMIT -8 3 2
OMIT 12 -1 0
OMIT 8 -3 1
OMIT -10 3 5
OMIT -3 1 1
REM <olex2.extras>
REM <HklSrc "%./mclau2_016_pl.hkl">
REM </olex2.extras>

WGHT    0.164500    6.995100
BASF   0.37630
FVAR       0.71754
AS1   1    0.370563    0.222618   -0.110847    11.00000    0.02316    0.01373 =
         0.06349    0.00911    0.01975    0.00256
AS2   1    0.118659    0.023714    0.122929    11.00000    0.02119    0.02370 =
         0.07409    0.00499    0.01944   -0.00205
O1    2    0.580303    0.311592    0.028775    11.00000    0.01025
O2    2    0.257994    0.301198    0.057020    11.00000    0.03282
O3    2   -0.032850    0.342723    0.105880    11.00000    0.02794
AS3   1    0.398636    0.605237    0.356321    11.00000    0.02340    0.01670 =
         0.08197    0.01200    0.02832    0.00151
AS4   1    0.142124    0.654212    0.571104    11.00000    0.01685    0.02888 =
         0.06716    0.00272    0.01898    0.00025
O4    2    0.527804    0.246110    0.403941    11.00000    0.02461
O5    2    0.225504    0.418963    0.414418    11.00000    0.01881
O6    2   -0.023912    0.817193    0.380359    11.00000    0.03291
HKLF 4 1 0 0 -1 0 -1 0 -1 0 0

REM  mclau2_016_a.res in P2(1)
REM R1 =  0.1068 for     449 Fo > 4sig(Fo)  and  0.1184 for all     562 data
REM     62 parameters refined using     67 restraints

END

WGHT      0.1695      7.7952

REM Highest difference peak  2.560,  deepest hole -2.280,  1-sigma level  0.520
Q1    1   0.3620  0.0194 -0.0777  11.00000  0.05    2.56
Q2    1   0.1330  0.4355 -0.3932  11.00000  0.05    2.39
Q3    1   0.6134  0.2771 -0.2984  11.00000  0.05    2.12
Q4    1   0.1125  0.2185  0.1484  11.00000  0.05    1.72
Q5    1   0.3572 -0.1476  0.4431  11.00000  0.05    1.68
Q6    1   0.5008  0.1124 -0.3467  11.00000  0.05    1.61
Q7    1   0.5586  0.4463  0.1845  11.00000  0.05    1.31
Q8    1   0.2995 -0.2177 -0.3198  11.00000  0.05    1.29
Q9    1   0.1359  0.3515  0.2103  11.00000  0.05    1.26
Q10   1   0.0410  0.1492 -0.3296  11.00000  0.05    1.24
Q11   1   0.4378  0.4993 -0.1168  11.00000  0.05    1.23
Q12   1   0.4589  0.0875  0.3486  11.00000  0.05    1.21
Q13   1   0.5812  0.1269  0.0589  11.00000  0.05    1.20
Q14   1   0.2811  0.3895 -0.4813  11.00000  0.05    1.18
Q15   1  -0.0187  0.3609  0.2635  11.00000  0.05    1.16
Q16   1   0.3171 -0.1833 -0.2625  11.00000  0.05    1.15
Q17   1   0.5207  0.2175  0.1514  11.00000  0.05    1.13
Q18   1   0.2576  0.5064 -0.0272  11.00000  0.05    1.13
Q19   1   0.0236  0.5089  0.1571  11.00000  0.05    1.12
Q20   1   0.0403  0.3856 -0.0240  11.00000  0.05    1.10
;
_shelx_res_checksum              73236
_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 0.3706(6) 0.2226(10) -0.1108(17) 0.032(5) Uani 1 1 d D
As2 As 0.1187(6) 0.0237(12) 0.1229(18) 0.038(7) Uani 1 1 d D
O1 O 0.580(2) 0.312(4) 0.029(5) 0.010(5) Uiso 1 1 d D
O2 O 0.258(5) 0.301(6) 0.057(5) 0.033(9) Uiso 1 1 d D
O3 O -0.033(3) 0.343(6) 0.106(3) 0.028(8) Uiso 1 1 d D
As3 As 0.3986(6) 0.6052(12) 0.3563(16) 0.038(5) Uani 1 1 d D
As4 As 0.1421(6) 0.6542(12) 0.5711(19) 0.036(6) Uani 1 1 d D
O4 O 0.528(3) 0.246(5) 0.404(3) 0.025(7) Uiso 1 1 d D
O5 O 0.226(4) 0.419(6) 0.414(5) 0.019(7) Uiso 1 1 d D
O6 O -0.024(3) 0.817(7) 0.380(3) 0.033(9) 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 0.023(3) 0.014(2) 0.063(17) 0.009(3) 0.020(6) 0.0026(18)
As2 0.021(3) 0.024(3) 0.07(2) 0.005(4) 0.019(8) -0.0021(19)
As3 0.023(3) 0.017(2) 0.082(17) 0.012(4) 0.028(6) 0.002(2)
As4 0.017(3) 0.029(3) 0.067(19) 0.003(4) 0.019(6) 0.000(2)
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 84.6(6) 2_645 .
O1 As1 O2 92.7(18) 2_645 .
O2 As1 O1 100.8(18) . .
O2 As2 O3 96.7(12) . 2_545
O2 As2 O3 91.3(15) . .
O3 As2 O3 98.8(10) . 2_545
As1 O1 As1 118.3(11) 2_655 .
As1 O2 As2 126.1(13) . .
As2 O3 As2 116.5(13) . 2
O4 As3 O4 93.1(10) . 2_656
O4 As3 O5 95.0(14) . .
O5 As3 O4 88.2(13) . 2_656
O5 As4 O6 92.7(16) . .
O6 As4 O5 93.4(14) 2_546 .
O6 As4 O6 95.6(10) 2_546 .
As3 O4 As3 118.0(14) . 2_646
As3 O5 As4 114.8(11) . .
As4 O6 As4 118.2(13) 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(12) 2_645
As1 O1 1.792(13) .
As1 O2 1.790(13) .
As2 O2 1.789(13) .
As2 O3 1.794(13) .
As2 O3 1.792(14) 2_545
O1 As1 1.790(12) 2_655
O3 As2 1.792(14) 2
As3 O4 1.792(13) .
As3 O4 1.792(14) 2_656
As3 O5 1.792(12) .
As4 O5 1.793(13) .
As4 O6 1.793(14) .
As4 O6 1.789(13) 2_546
O4 As3 1.792(14) 2_646
O6 As4 1.789(13) 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 -156(4) 2_645 2_655
O1 As1 O2 As2 -41(3) 2_645 .
O1 As1 O2 As2 -126(3) . .
O2 As1 O1 As1 -64(3) . 2_655
O2 As2 O3 As2 62(2) . 2
O3 As2 O2 As1 -36(3) 2_545 .
O3 As2 O2 As1 -135(3) . .
O3 As2 O3 As2 -35(2) 2_545 2
O4 As3 O4 As3 21.5(15) 2_656 2_646
O4 As3 O5 As4 131(2) . .
O4 As3 O5 As4 38(2) 2_656 .
O5 As3 O4 As3 -67(2) . 2_646
O5 As4 O6 As4 -167(2) . 2_556
O6 As4 O5 As3 -166(2) 2_546 .
O6 As4 O5 As3 98(2) . .
O6 As4 O6 As4 99(3) 2_546 2_556
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6(6)
2 0.4(6)
