#------------------------------------------------------------------------------
#$Date: 2015-09-05 22:32:59 +0200 (Sat 05 de Sep de 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513297.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_4513297
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         'As4 O6'
_chemical_formula_sum            'As4 O6'
_chemical_formula_weight         395.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 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                 143.199(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.588(3)
_cell_length_b                   4.3812(2)
_cell_length_c                   16.593(4)
_cell_measurement_pressure       4.85e6(10)
_cell_measurement_reflns_used    526
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.6990
_cell_measurement_theta_min      2.8640
_cell_volume                     548.2(3)
_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         4.85e6(10)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.419
_diffrn_measured_fraction_theta_max 0.242
_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      -0.0308675000
_diffrn_orient_matrix_UB_12      0.0029269000
_diffrn_orient_matrix_UB_13      0.0205698000
_diffrn_orient_matrix_UB_21      -0.0171357000
_diffrn_orient_matrix_UB_22      0.0727673000
_diffrn_orient_matrix_UB_23      -0.0169090000
_diffrn_orient_matrix_UB_31      -0.0221911000
_diffrn_orient_matrix_UB_32      -0.0600148000
_diffrn_orient_matrix_UB_33      -0.0195364000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_laue_measured_fraction_full 0.419
_diffrn_reflns_laue_measured_fraction_max 0.242
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1471
_diffrn_reflns_point_group_measured_fraction_full 0.419
_diffrn_reflns_point_group_measured_fraction_max 0.242
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.763
_diffrn_reflns_theta_min         2.306
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    5.539
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14056
_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    4.794
_exptl_crystal_description
;
;
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.862
_refine_diff_density_min         -3.336
_refine_diff_density_rms         0.524
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.291
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         700
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.248
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.1208
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3017
_refine_ls_wR_factor_ref         0.3232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                536
_reflns_number_total             700
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_022_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        548.2(2)
_cod_database_code               4513297
_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. 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 As4-
 O3 \\sim As1-O1_$1 \\sim As2-O6_$2 \\sim As3-O4_$3
 with sigma of 0.01
;
_shelx_res_file
;
    mclau2_022_pl.res created by SHELXL-2014/7

TITL mclau2_022_a.res in P2(1)/c
CELL 0.41427 12.588 4.3812 16.593 90 143.199 90
ZERR 4 0.003 0.0002 0.004 0 0.013 0
LATT 1
SYMM 0.5-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 16 24
EQIV $1 1.5-X,-0.5+Y,1-Z
EQIV $2 +X,1+Y,+Z
EQIV $3 -0.5-X,-0.5+Y,-Z
SADI 0.01 As1 O1 As1 O2 As2 O2 As2 O3 As3 O4 As3 O5 As4 O5 As4 O6 As4 O3 As1 =
 O1_$1 AS2 O6_$2 AS3 O4_$3

L.S. 10
PLAN  -20
BOND $H
CONF
MORE -1
fmap 2
acta
OMIT -10 4 10
OMIT -7 7 8
OMIT 1 5 6
REM <olex2.extras>
REM <HklSrc "%./mclau2_022_pl.hkl">
REM </olex2.extras>

WGHT    0.200000
FVAR       3.23629
AS1   1    0.669611    0.279451    0.393340    11.00000    0.02562    0.02318 =
         0.03852    0.00527    0.02411    0.00135
AS2   1    0.378962    0.200817    0.348555    11.00000    0.02581    0.01600 =
         0.02969    0.00139    0.02199    0.00238
AS3   1   -0.194093   -0.337142    0.097589    11.00000    0.02720    0.02099 =
         0.03420    0.00199    0.02429    0.00225
AS4   1    0.099987   -0.301878    0.146296    11.00000    0.02109    0.01791 =
         0.02072   -0.00416    0.01434   -0.00171
O1    2    0.697055    0.458072    0.504951    11.00000    0.03277
O2    2    0.464797    0.130596    0.303172    11.00000    0.02586
O3    2    0.160719    0.089576    0.188861    11.00000    0.01754
O4    2   -0.262443   -0.220000   -0.041649    11.00000    0.03430
O5    2    0.032599   -0.324949    0.207550    11.00000    0.02624
O6    2    0.322453   -0.410093    0.301342    11.00000    0.02135
HKLF 4 1 0 0 -1 0 -1 0 -1 0 1

REM  mclau2_022_a.res in P2(1)/c
REM R1 =  0.1208 for     536 Fo > 4sig(Fo)  and  0.1470 for all     700 data
REM     61 parameters refined using     66 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  3.862,  deepest hole -3.336,  1-sigma level  0.524
Q1    1  -0.1881 -0.1988  0.0983  11.00000  0.05    2.78
Q2    1   0.8207  0.6178  0.5939  11.00000  0.05    1.86
Q3    1  -0.3183 -0.2991  0.0321  11.00000  0.05    1.77
Q4    1   0.5615  0.3052  0.4205  11.00000  0.05    1.68
Q5    1   0.0110 -0.0470  0.1402  11.00000  0.05    1.64
Q6    1   0.2437  0.6116  0.2634  11.00000  0.05    1.60
Q7    1   0.2069 -0.2963  0.1827  11.00000  0.05    1.56
Q8    1   0.6533 -0.1293  0.3382  11.00000  0.05    1.56
Q9    1   0.3817  0.4100  0.3485  11.00000  0.05    1.56
Q10   1  -0.1968 -0.0381  0.0770  11.00000  0.05    1.53
Q11   1   0.0999 -0.0958  0.1464  11.00000  0.05    1.47
Q12   1   0.3339 -0.1787  0.2829  11.00000  0.05    1.46
Q13   1  -0.1069 -0.3687  0.1079  11.00000  0.05    1.45
Q14   1  -0.0354 -0.2001  0.0593  11.00000  0.05    1.43
Q15   1   0.3929  0.4568  0.1866  11.00000  0.05    1.42
Q16   1  -0.1767 -0.5596  0.0990  11.00000  0.05    1.40
Q17   1   0.0740  0.3103  0.0690  11.00000  0.05    1.33
Q18   1  -0.4074 -0.7901  0.0427  11.00000  0.05    1.32
Q19   1   0.7755  0.3089  0.3109  11.00000  0.05    1.28
Q20   1   0.4178 -0.1976  0.4430  11.00000  0.05    1.27
;
_shelx_res_checksum              4917
_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+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -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 0.6696(3) 0.2795(5) 0.3933(5) 0.031(3) Uani 1 1 d D
As2 As 0.3790(3) 0.2008(4) 0.3486(5) 0.024(3) Uani 1 1 d D
As3 As -0.1941(3) -0.3371(5) 0.0976(5) 0.028(3) Uani 1 1 d D
As4 As 0.1000(3) -0.3019(4) 0.1463(5) 0.023(3) Uani 1 1 d D
O1 O 0.6971(18) 0.458(3) 0.5050(14) 0.033(4) Uiso 1 1 d D
O2 O 0.4648(15) 0.131(3) 0.3032(16) 0.026(3) Uiso 1 1 d D
O3 O 0.1607(11) 0.0896(19) 0.1889(15) 0.018(3) Uiso 1 1 d D
O4 O -0.262(2) -0.220(2) -0.0416(13) 0.034(4) Uiso 1 1 d D
O5 O 0.0326(13) -0.325(3) 0.2076(14) 0.026(3) Uiso 1 1 d D
O6 O 0.3225(11) -0.410(2) 0.3013(18) 0.021(3) 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 0.0256(12) 0.0232(12) 0.039(6) 0.0053(13) 0.024(2) 0.0014(8)
As2 0.0258(12) 0.0160(10) 0.030(6) 0.0014(11) 0.022(2) 0.0024(7)
As3 0.0272(12) 0.0210(11) 0.034(6) 0.0020(11) 0.024(2) 0.0022(7)
As4 0.0211(11) 0.0179(10) 0.021(6) -0.0042(11) 0.0143(19) -0.0017(6)
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 96.5(4) 2_646 .
O1 As1 O2 98.1(7) 2_646 .
O2 As1 O1 88.8(5) . .
O2 As2 O3 93.4(9) . .
O2 As2 O6 98.3(10) . 1_565
O6 As2 O3 90.6(4) 1_565 .
O4 As3 O4 88.1(3) 2_445 .
O4 As3 O5 97.7(7) 2_445 .
O5 As3 O4 92.0(7) . .
O3 As4 O6 90.3(4) . .
O5 As4 O3 94.5(9) . .
O5 As4 O6 94.5(10) . .
As1 O1 As1 126.3(8) 2_656 .
As2 O2 As1 123.3(7) . .
As2 O3 As4 121.2(7) . .
As3 O4 As3 125.3(9) 2_455 .
As3 O5 As4 121.8(8) . .
As2 O6 As4 120.5(6) 1_545 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 O1 1.764(7) 2_646
As1 O1 1.771(8) .
As1 O2 1.770(7) .
As2 O2 1.770(8) .
As2 O3 1.774(8) .
As2 O6 1.770(7) 1_565
As3 O4 1.777(9) .
As3 O4 1.778(8) 2_445
As3 O5 1.771(8) .
As4 O3 1.778(7) .
As4 O5 1.773(9) .
As4 O6 1.774(8) .
O1 As1 1.764(7) 2_656
O4 As3 1.778(8) 2_455
O6 As2 1.770(7) 1_545
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 105.0(15) 2_646 2_656
O1 As1 O2 As2 0.0(11) . .
O1 As1 O2 As2 96.4(12) 2_646 .
O2 As1 O1 As1 -157.0(12) . 2_656
O2 As2 O3 As4 79.7(15) . .
O3 As2 O2 As1 162.6(10) . .
O3 As4 O5 As3 105.2(9) . .
O3 As4 O6 As2 175(2) . 1_545
O4 As3 O4 As3 168.2(15) 2_445 2_455
O4 As3 O5 As4 74.3(11) 2_445 .
O4 As3 O5 As4 -14.1(10) . .
O5 As3 O4 As3 -94.1(11) . 2_455
O5 As4 O3 As2 89.9(15) . .
O5 As4 O6 As2 80.6(17) . 1_545
O6 As2 O2 As1 71.5(11) 1_565 .
O6 As2 O3 As4 178.1(19) 1_565 .
O6 As4 O3 As2 -4.6(14) . .
O6 As4 O5 As3 -164.2(9) . .
