#------------------------------------------------------------------------------
#$Date: 2015-09-05 22:32:59 +0200 (Sat 05 de Sep de 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513292.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_4513292
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'
_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                 107.04(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3557(17)
_cell_length_b                   4.0829(3)
_cell_length_c                   7.385(7)
_cell_measurement_pressure       1.192e7(5)
_cell_measurement_reflns_used    502
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.2270
_cell_measurement_theta_min      1.4740
_cell_volume                     240.9(2)
_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         1.192e7(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.401
_diffrn_measured_fraction_theta_max 0.258
_diffrn_measurement_details
;
  1 phi    142.00  218.00   0.5000    2.0000
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      -0.0584155000
_diffrn_orient_matrix_UB_12      0.0074234000
_diffrn_orient_matrix_UB_13      -0.0140107000
_diffrn_orient_matrix_UB_21      0.0027694000
_diffrn_orient_matrix_UB_22      0.0819439000
_diffrn_orient_matrix_UB_23      -0.0285094000
_diffrn_orient_matrix_UB_31      -0.0034688000
_diffrn_orient_matrix_UB_32      -0.0595068000
_diffrn_orient_matrix_UB_33      -0.0409741000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_laue_measured_fraction_full 0.401
_diffrn_reflns_laue_measured_fraction_max 0.258
_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            701
_diffrn_reflns_point_group_measured_fraction_full 0.428
_diffrn_reflns_point_group_measured_fraction_max 0.265
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.562
_diffrn_reflns_theta_min         1.486
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    6.303
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37992
_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    5.455
_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         1.488
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.374
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         542
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1443P)²+4.2271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2007
_reflns_Friedel_coverage         0.854
_reflns_friedel_fraction_full    0.464
_reflns_friedel_fraction_max     0.274
_reflns_number_gt                522
_reflns_number_total             542
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_017_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_database_code               4513292
_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: 0.8(4) 0.2(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_017_pl.res created by SHELXL-2014/7

TITL mclau2_017_a.res in P2(1)
CELL 0.41427 8.3557 4.0829 7.385 90 107.04 90
ZERR 4 0.0017 0.0003 0.007 0 0.05 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 6 -4 0
OMIT -13 -1 6
OMIT -8 4 4
OMIT 8 -3 1
OMIT -10 3 5
OMIT 6 -2 0
REM <olex2.extras>
REM <HklSrc "%./mclau2_017_pl.hkl">
REM </olex2.extras>

WGHT    0.144300    4.227100
BASF   0.21474
FVAR       1.19005
AS1   1    0.372115    0.224064   -0.110807    11.00000    0.02444    0.01410 =
         0.05208    0.00111    0.02116    0.00240
AS2   1    0.118423    0.022709    0.124630    11.00000    0.02336    0.01532 =
         0.04766    0.00429    0.01655   -0.00095
O1    2    0.578107    0.305897    0.044004    11.00000    0.01680
O2    2    0.256701    0.296790    0.054699    11.00000    0.02147
O3    2   -0.036813    0.335271    0.103659    11.00000    0.02371
AS3   1    0.399258    0.602299    0.355503    11.00000    0.02367    0.01567 =
         0.05444    0.00217    0.02060   -0.00108
AS4   1    0.142583    0.655331    0.573964    11.00000    0.02293    0.01680 =
         0.06918    0.00071    0.02130    0.00123
O4    2    0.526167    0.240366    0.403875    11.00000    0.01788
O5    2    0.227454    0.421012    0.418539    11.00000    0.02483
O6    2   -0.024635    0.815155    0.382704    11.00000    0.02209
HKLF 4 1 0 0 -1 0 -1 0 -1 0 0

REM  mclau2_017_a.res in P2(1)
REM R1 =  0.0742 for     522 Fo > 4sig(Fo)  and  0.0784 for all     542 data
REM     62 parameters refined using     67 restraints

END

WGHT      0.1496      4.5960

REM Highest difference peak  1.488,  deepest hole -1.450,  1-sigma level  0.374
Q1    1   0.0959 -0.2579  0.4246  11.00000  0.05    1.49
Q2    1   0.0924  0.4640 -0.3999  11.00000  0.05    1.47
Q3    1   0.3426 -0.1848  0.4041  11.00000  0.05    1.32
Q4    1   0.6219  0.3806  0.4709  11.00000  0.05    1.29
Q5    1   0.3581  0.4055  0.4472  11.00000  0.05    1.26
Q6    1   0.5654  0.1995  0.4947  11.00000  0.05    1.23
Q7    1  -0.0967  0.3516  0.3641  11.00000  0.05    1.22
Q8    1   0.2193  0.6466  0.5057  11.00000  0.05    1.18
Q9    1   0.0780  0.1127 -0.0454  11.00000  0.05    1.16
Q10   1   0.1382  0.4899 -0.3493  11.00000  0.05    1.15
Q11   1   0.3607  0.5097  0.1938  11.00000  0.05    1.14
Q12   1   0.6359  0.2041 -0.2509  11.00000  0.05    1.14
Q13   1   0.1372  0.1090  0.2462  11.00000  0.05    1.11
Q14   1   0.4563  0.4709 -0.1042  11.00000  0.05    1.10
Q15   1   0.4766  0.1635  0.5282  11.00000  0.05    1.07
Q16   1   0.3395  0.1453 -0.2367  11.00000  0.05    1.07
Q17   1   0.2615  0.5592 -0.0474  11.00000  0.05    1.07
Q18   1  -0.0602  0.4288  0.0436  11.00000  0.05    1.06
Q19   1   0.1239  0.3680 -0.2606  11.00000  0.05    1.05
Q20   1   0.1633  0.5273 -0.3080  11.00000  0.05    1.04
;
_shelx_res_checksum              22805
_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) 0.2241(6) -0.1108(11) 0.028(3) Uani 1 1 d D
As2 As 0.1184(4) 0.0227(7) 0.1246(11) 0.027(4) Uani 1 1 d D
O1 O 0.5781(16) 0.306(3) 0.044(4) 0.017(4) Uiso 1 1 d D
O2 O 0.257(3) 0.297(4) 0.055(3) 0.021(4) Uiso 1 1 d D
O3 O -0.0368(19) 0.335(4) 0.104(2) 0.024(4) Uiso 1 1 d D
As3 As 0.3993(4) 0.6023(8) 0.3555(10) 0.029(3) Uani 1 1 d D
As4 As 0.1426(4) 0.6553(7) 0.5740(12) 0.035(4) Uani 1 1 d D
O4 O 0.526(2) 0.240(3) 0.404(2) 0.018(4) Uiso 1 1 d D
O5 O 0.227(3) 0.421(5) 0.419(4) 0.025(5) Uiso 1 1 d D
O6 O -0.0246(19) 0.815(4) 0.383(3) 0.022(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 0.0244(15) 0.0141(14) 0.052(11) 0.0011(19) 0.021(4) 0.0024(11)
As2 0.0234(16) 0.0153(12) 0.048(12) 0.004(2) 0.017(4) -0.0010(12)
As3 0.0237(14) 0.0157(12) 0.054(10) 0.0022(19) 0.021(3) -0.0011(12)
As4 0.0229(15) 0.0168(14) 0.069(11) 0.001(2) 0.021(4) 0.0012(11)
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 84.3(4) 2_645 .
O2 As1 O1 95.6(12) . 2_645
O2 As1 O1 98.2(12) . .
O2 As2 O3 95.5(9) . 2_545
O3 As2 O2 92.4(8) . .
O3 As2 O3 99.0(6) . 2_545
As1 O1 As1 117.0(8) 2_655 .
As1 O2 As2 128.0(10) . .
As2 O3 As2 116.8(10) . 2
O4 As3 O4 92.8(6) . 2_656
O4 As3 O5 94.6(10) . .
O5 As3 O4 86.8(10) . 2_656
O5 As4 O6 93.0(12) . .
O6 As4 O5 92.4(8) 2_546 .
O6 As4 O6 94.6(7) 2_546 .
As3 O4 As3 118.0(9) . 2_646
As4 O5 As3 116.3(9) . .
As4 O6 As4 119.0(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 1.792(10) 2_645
As1 O1 1.797(11) .
As1 O2 1.790(11) .
As2 O2 1.790(10) .
As2 O3 1.794(11) 2_545
As2 O3 1.794(10) .
O1 As1 1.792(10) 2_655
O3 As2 1.794(11) 2
As3 O4 1.793(10) .
As3 O4 1.793(11) 2_656
As3 O5 1.794(10) .
As4 O5 1.792(11) .
As4 O6 1.793(11) .
As4 O6 1.785(11) 2_546
O4 As3 1.793(11) 2_646
O6 As4 1.785(10) 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 -166(3) 2_645 2_655
O1 As1 O2 As2 -38.0(19) 2_645 .
O1 As1 O2 As2 -123.0(18) . .
O2 As1 O1 As1 -71.3(17) . 2_655
O2 As2 O3 As2 59.2(14) . 2
O3 As2 O2 As1 -35.5(19) 2_545 .
O3 As2 O2 As1 -134.7(18) . .
O3 As2 O3 As2 -36.7(13) 2_545 2
O4 As3 O4 As3 20.6(9) 2_656 2_646
O4 As3 O5 As4 132.1(17) . .
O4 As3 O5 As4 39.6(17) 2_656 .
O5 As3 O4 As3 -66.4(14) . 2_646
O5 As4 O6 As4 -166.0(12) . 2_556
O6 As4 O5 As3 -167.5(18) 2_546 .
O6 As4 O5 As3 97.7(18) . .
O6 As4 O6 As4 101.3(19) 2_546 2_556
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.8(4)
2 0.2(4)
