#------------------------------------------------------------------------------
#$Date: 2015-09-05 22:32:59 +0200 (Sat 05 de Sep de 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513290.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_4513290
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                 106.90(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3570(10)
_cell_length_b                   4.0889(2)
_cell_length_c                   7.400(4)
_cell_measurement_pressure       1.168e7(7)
_cell_measurement_reflns_used    290
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.0730
_cell_measurement_theta_min      1.4840
_cell_volume                     241.94(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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      He
_diffrn_ambient_pressure         1.168e7(7)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.427
_diffrn_measured_fraction_theta_max 0.222
_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      0.0583176000
_diffrn_orient_matrix_UB_12      0.0072593000
_diffrn_orient_matrix_UB_13      0.0140262000
_diffrn_orient_matrix_UB_21      -0.0027333000
_diffrn_orient_matrix_UB_22      0.0816713000
_diffrn_orient_matrix_UB_23      0.0285722000
_diffrn_orient_matrix_UB_31      0.0035016000
_diffrn_orient_matrix_UB_32      -0.0595390000
_diffrn_orient_matrix_UB_33      0.0409064000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.1105
_diffrn_reflns_av_unetI/netI     0.1345
_diffrn_reflns_laue_measured_fraction_full 0.427
_diffrn_reflns_laue_measured_fraction_max 0.222
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            738
_diffrn_reflns_point_group_measured_fraction_full 0.454
_diffrn_reflns_point_group_measured_fraction_max 0.227
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         22.039
_diffrn_reflns_theta_min         1.484
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    6.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66147
_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    5.431
_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         2.098
_refine_diff_density_min         -1.739
_refine_diff_density_rms         0.448
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         573
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.1179
_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)+(0.1840P)²+0.9780P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3061
_refine_ls_wR_factor_ref         0.3373
_reflns_Friedel_coverage         0.853
_reflns_friedel_fraction_full    0.490
_reflns_friedel_fraction_max     0.232
_reflns_number_gt                384
_reflns_number_total             573
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_015_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_database_code               4513290
_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: 1.1(8) -0.1(8)
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_015_pl.res created by SHELXL-2014/7

TITL mclau2_015_a.res in P2(1)
CELL 0.41427 8.357 4.0889 7.4 90 106.9 90
ZERR 4 0.001 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 -3 1 1
REM <olex2.extras>
REM <HklSrc "%./mclau2_015_pl.hkl">
REM </olex2.extras>

WGHT    0.184000    0.978000
BASF  -0.10662
FVAR       4.25112
AS1   1    0.370885    0.222775   -0.111824    11.00000    0.04205    0.02896 =
         0.07032    0.00806    0.02734    0.00465
PART 1
AS2   1    0.118046    0.026510    0.125615    11.00000    0.03417    0.03286 =
         0.07952    0.00588    0.01712   -0.00225
PART 0
O1    2    0.580006    0.314413    0.027250    11.00000    0.03179
O2    2    0.258433    0.296098    0.056291    11.00000    0.04972
O3    2   -0.028771    0.354692    0.104387    11.00000    0.03805
AS3   1    0.397240    0.605425    0.355217    11.00000    0.03822    0.03057 =
         0.06677    0.01339    0.02445    0.00219
AS4   1    0.141516    0.655882    0.572680    11.00000    0.03871    0.03613 =
         0.11077    0.00628    0.03848    0.00264
O4    2    0.522989    0.244083    0.406070    11.00000    0.03715
O5    2    0.226527    0.421465    0.417873    11.00000    0.03391
O6    2   -0.026715    0.812066    0.382976    11.00000    0.05047
HKLF 4 1 0 0 -1 0 -1 0 -1 0 0

REM  mclau2_015_a.res in P2(1)
REM R1 =  0.1179 for     384 Fo > 4sig(Fo)  and  0.1383 for all     573 data
REM     62 parameters refined using     67 restraints

END

WGHT      0.1929      1.2526

REM Highest difference peak  2.098,  deepest hole -1.739,  1-sigma level  0.448
Q1    1   0.4601  0.0123 -0.1062  11.00000  0.05    2.08
Q2    1   0.3596 -0.1560  0.4313  11.00000  0.05    1.79
Q3    1   0.6755  0.5072  0.0818  11.00000  0.05    1.74
Q4    1   0.1096  0.4164 -0.3881  11.00000  0.05    1.60
Q5    1   0.4457  0.4561 -0.1081  11.00000  0.05    1.59
Q6    1  -0.0797  0.3620  0.3900  11.00000  0.05    1.50
Q7    1   0.1993  0.2448  0.0952  11.00000  0.05    1.43
Q8    1   0.4746  0.1068  0.0827  11.00000  0.05    1.42
Q9    1  -0.1856  0.3053 -0.0920  11.00000  0.05    1.36
Q10   1   0.5750  0.2874  0.4428  11.00000  0.05    1.25
Q11   1   0.2792  0.3530 -0.5034  11.00000  0.05    1.23
Q12   1   0.3622  0.4227  0.4574  11.00000  0.05    1.21
Q13   1   0.1193  0.3260  0.1823  11.00000  0.05    1.20
Q14   1  -0.0199  1.0312  0.5396  11.00000  0.05    1.20
Q15   1   0.3419  0.3990  0.3978  11.00000  0.05    1.12
Q16   1   0.0598  0.1498 -0.0675  11.00000  0.05    1.11
Q17   1   0.2834 -0.2337  0.2908  11.00000  0.05    1.11
Q18   1   0.3047  0.3586  0.3001  11.00000  0.05    1.11
Q19   1   0.2572  0.5474 -0.0132  11.00000  0.05    1.09
Q20   1  -0.0362  0.0468 -0.1176  11.00000  0.05    1.05
;
_shelx_res_checksum              36541
_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
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.3709(9) 0.2228(14) -0.112(2) 0.045(7) Uani 1 1 d D . .
As2 As 0.1180(7) 0.0265(13) 0.126(2) 0.049(9) Uani 1 1 d D A 1
O1 O 0.580(3) 0.314(6) 0.027(7) 0.032(8) Uiso 1 1 d D . .
O2 O 0.258(5) 0.296(7) 0.056(6) 0.050(12) Uiso 1 1 d D . .
O3 O -0.029(4) 0.355(6) 0.104(4) 0.038(10) Uiso 1 1 d D . .
As3 As 0.3972(8) 0.6054(16) 0.3552(19) 0.043(7) Uani 1 1 d D . .
As4 As 0.1415(9) 0.6559(15) 0.573(3) 0.058(8) Uani 1 1 d D . .
O4 O 0.523(4) 0.244(6) 0.406(4) 0.037(9) Uiso 1 1 d D . .
O5 O 0.227(5) 0.421(7) 0.418(7) 0.034(9) Uiso 1 1 d D . .
O6 O -0.027(4) 0.812(8) 0.383(4) 0.050(12) 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 0.042(4) 0.029(3) 0.07(2) 0.008(4) 0.027(8) 0.005(2)
As2 0.034(4) 0.033(3) 0.08(3) 0.006(5) 0.017(10) -0.002(2)
As3 0.038(3) 0.031(3) 0.07(2) 0.013(5) 0.024(7) 0.002(3)
As4 0.039(3) 0.036(4) 0.11(3) 0.006(4) 0.038(9) 0.003(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 84.7(8) 2_645 .
O1 As1 O2 92(2) 2_645 .
O2 As1 O1 101(2) . .
O2 As2 O3 90.2(17) . .
O2 As2 O3 95.5(14) . 2_545
O3 As2 O3 97.2(11) 2_545 .
As1 O1 As1 118.9(15) 2_655 .
As1 O2 As2 128.1(17) . .
As2 O3 As2 117.5(16) 2 .
O4 As3 O4 91.5(11) . 2_656
O4 As3 O5 93.6(17) . .
O5 As3 O4 88.5(15) . 2_656
O6 As4 O5 93(2) . .
O6 As4 O5 91.7(17) 2_546 .
O6 As4 O6 94.8(13) 2_546 .
As3 O4 As3 119.8(18) . 2_646
As3 O5 As4 115.8(14) . .
As4 O6 As4 118.6(17) 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 1.789(15) 2_645
As1 O1 1.791(15) .
As1 O2 1.789(15) .
As2 O2 1.790(15) .
As2 O3 1.791(16) 2_545
As2 O3 1.794(15) .
O1 As1 1.789(15) 2_655
O3 As2 1.791(16) 2
As3 O4 1.789(15) .
As3 O4 1.789(16) 2_656
As3 O5 1.789(14) .
As4 O5 1.791(15) .
As4 O6 1.791(16) .
As4 O6 1.785(16) 2_546
O4 As3 1.789(16) 2_646
O6 As4 1.785(15) 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 -155(5) 2_645 2_655
O1 As1 O2 As2 -42(4) 2_645 .
O1 As1 O2 As2 -126(4) . .
O2 As1 O1 As1 -64(4) . 2_655
O2 As2 O3 As2 64(3) . 2
O3 As2 O2 As1 -134(4) . .
O3 As2 O2 As1 -37(4) 2_545 .
O3 As2 O3 As2 -32(2) 2_545 2
O4 As3 O4 As3 20.5(18) 2_656 2_646
O4 As3 O5 As4 132(3) . .
O4 As3 O5 As4 40(3) 2_656 .
O5 As3 O4 As3 -68(3) . 2_646
O5 As4 O6 As4 -165(3) . 2_556
O6 As4 O5 As3 -167(3) 2_546 .
O6 As4 O5 As3 98(3) . .
O6 As4 O6 As4 103(4) 2_546 2_556
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.1(8)
2 -0.1(8)
