#------------------------------------------------------------------------------
#$Date: 2015-09-05 23:32:59 +0300 (Sat, 05 Sep 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513298.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_4513298
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                 143.483(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.905(3)
_cell_length_b                   4.4711(3)
_cell_length_c                   17.262(6)
_cell_measurement_pressure       2.31e6(18)
_cell_measurement_reflns_used    577
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.1780
_cell_measurement_theta_min      2.8930
_cell_volume                     592.7(4)
_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         2.31e6(19)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.438
_diffrn_measured_fraction_theta_max 0.269
_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      -0.0296042000
_diffrn_orient_matrix_UB_12      0.0082386000
_diffrn_orient_matrix_UB_13      0.0193782000
_diffrn_orient_matrix_UB_21      -0.0153206000
_diffrn_orient_matrix_UB_22      0.0711991000
_diffrn_orient_matrix_UB_23      -0.0176962000
_diffrn_orient_matrix_UB_31      -0.0227230000
_diffrn_orient_matrix_UB_32      -0.0587024000
_diffrn_orient_matrix_UB_33      -0.0187302000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_laue_measured_fraction_full 0.438
_diffrn_reflns_laue_measured_fraction_max 0.269
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1632
_diffrn_reflns_point_group_measured_fraction_full 0.438
_diffrn_reflns_point_group_measured_fraction_max 0.269
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.360
_diffrn_reflns_theta_min         2.270
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    5.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30779
_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    4.434
_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         3.093
_refine_diff_density_min         -2.533
_refine_diff_density_rms         0.421
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         793
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.1066
_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          0.2737
_refine_ls_wR_factor_ref         0.3006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                604
_reflns_number_total             793
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_023_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        592.7(3)
_cod_database_code               4513298
_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_023_pl.res created by SHELXL-2014/7

TITL mclau2_023_a.res in P2(1)/c
CELL 0.41427 12.905 4.4711 17.262 90 143.483 90
ZERR 4 0.003 0.0003 0.006 0 0.019 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 7 3 1
OMIT -11 2 1
OMIT -11 4 8
OMIT -16 0 12
REM <olex2.extras>
REM <HklSrc "%./mclau2_023_pl.hkl">
REM </olex2.extras>

WGHT    0.200000
FVAR       3.48345
AS1   1    0.675335    0.254299    0.397997    11.00000    0.02696    0.02350 =
         0.03926    0.00031    0.02473   -0.00200
AS2   1    0.382088    0.189553    0.346226    11.00000    0.02770    0.01587 =
         0.04251   -0.00110    0.02641    0.00022
AS3   1   -0.188530   -0.311296    0.096519    11.00000    0.02623    0.02399 =
         0.03465    0.00157    0.02280    0.00329
AS4   1    0.107062   -0.312269    0.150671    11.00000    0.02510    0.01723 =
         0.03535    0.00007    0.02170    0.00027
O1    2    0.708064    0.426128    0.509036    11.00000    0.03445
O2    2    0.465123    0.141106    0.301221    11.00000    0.02989
O3    2    0.168580    0.071559    0.192668    11.00000    0.02016
O4    2   -0.244993   -0.181265   -0.031505    11.00000    0.04867
O5    2    0.034502   -0.331047    0.204788    11.00000    0.03605
O6    2    0.322680   -0.427158    0.304442    11.00000    0.02190
HKLF 4 1 0 0 -1 0 -1 0 -1 0 1

REM  mclau2_023_a.res in P2(1)/c
REM R1 =  0.1066 for     604 Fo > 4sig(Fo)  and  0.1257 for all     793 data
REM     61 parameters refined using     66 restraints

END

WGHT      0.2000      0.0000

REM Highest difference peak  3.093,  deepest hole -2.533,  1-sigma level  0.421
Q1    1   0.3825  0.4094  0.3526  11.00000  0.05    1.95
Q2    1   0.1127 -0.0866  0.1616  11.00000  0.05    1.92
Q3    1   0.5798  0.2529  0.3616  11.00000  0.05    1.90
Q4    1  -0.1887 -0.0977  0.0929  11.00000  0.05    1.60
Q5    1   0.0322 -0.5286  0.1115  11.00000  0.05    1.51
Q6    1   0.0060 -0.1073  0.1102  11.00000  0.05    1.49
Q7    1  -0.0003 -0.2815  0.1199  11.00000  0.05    1.27
Q8    1   0.2303  0.6066  0.2195  11.00000  0.05    1.27
Q9    1   0.8230  0.5501  0.5981  11.00000  0.05    1.27
Q10   1  -0.0713 -0.3753  0.1604  11.00000  0.05    1.26
Q11   1   0.7850  0.2774  0.4399  11.00000  0.05    1.11
Q12   1   0.3358  0.1763  0.1731  11.00000  0.05    1.11
Q13   1   0.8209 -0.0739  0.5990  11.00000  0.05    1.10
Q14   1  -0.2837 -0.3137  0.0679  11.00000  0.05    0.99
Q15   1   0.2792  0.1638  0.2915  11.00000  0.05    0.99
Q16   1   0.4796  0.3941  0.3702  11.00000  0.05    0.98
Q17   1  -0.1396 -0.5425  0.1113  11.00000  0.05    0.97
Q18   1   0.9134  0.5386  0.6199  11.00000  0.05    0.96
Q19   1  -0.0807 -0.0967  0.1209  11.00000  0.05    0.95
Q20   1   0.7489  0.1850  0.3235  11.00000  0.05    0.95
;
_shelx_res_checksum              73090
_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 0.6753(2) 0.2543(4) 0.3980(3) 0.033(2) Uani 1 1 d D
As2 As 0.3821(2) 0.1896(3) 0.3462(3) 0.031(2) Uani 1 1 d D
As3 As -0.1885(2) -0.3113(4) 0.0965(3) 0.031(2) Uani 1 1 d D
As4 As 0.1071(2) -0.3123(3) 0.1507(3) 0.030(2) Uani 1 1 d D
O1 O 0.7081(12) 0.426(2) 0.5090(10) 0.034(3) Uiso 1 1 d D
O2 O 0.4651(11) 0.141(2) 0.3012(12) 0.030(3) Uiso 1 1 d D
O3 O 0.1686(9) 0.0716(16) 0.1927(12) 0.020(2) Uiso 1 1 d D
O4 O -0.2450(17) -0.181(2) -0.0315(11) 0.049(4) Uiso 1 1 d D
O5 O 0.0345(11) -0.331(3) 0.2048(12) 0.036(3) Uiso 1 1 d D
O6 O 0.3227(9) -0.4272(17) 0.3044(13) 0.022(2) 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 0.0270(10) 0.0235(9) 0.039(4) 0.0003(9) 0.0247(15) -0.0020(6)
As2 0.0277(10) 0.0159(8) 0.043(4) -0.0011(8) 0.0264(15) 0.0002(5)
As3 0.0262(9) 0.0240(9) 0.035(4) 0.0016(8) 0.0228(15) 0.0033(5)
As4 0.0251(9) 0.0172(8) 0.035(4) 0.0001(8) 0.0217(14) 0.0003(5)
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 95.1(3) 2_646 .
O1 As1 O2 99.3(5) 2_646 .
O2 As1 O1 89.8(4) . .
O2 As2 O3 93.9(7) . .
O2 As2 O6 99.0(7) . 1_565
O6 As2 O3 92.0(3) 1_565 .
O4 As3 O4 90.7(3) 2_445 .
O5 As3 O4 91.3(6) . .
O5 As3 O4 99.8(6) . 2_445
O3 As4 O5 94.7(7) . .
O3 As4 O6 91.1(3) . .
O6 As4 O5 93.1(7) . .
As1 O1 As1 129.2(7) 2_656 .
As1 O2 As2 124.1(7) . .
As2 O3 As4 122.9(6) . .
As3 O4 As3 126.5(8) 2_455 .
As3 O5 As4 122.6(7) . .
As2 O6 As4 122.0(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 1.772(8) .
As1 O2 1.767(7) .
As2 O2 1.771(8) .
As2 O3 1.777(7) .
As2 O6 1.777(6) 1_565
As3 O4 1.779(8) .
As3 O4 1.784(7) 2_445
As3 O5 1.772(7) .
As4 O3 1.782(6) .
As4 O5 1.778(8) .
As4 O6 1.783(7) .
O1 As1 1.764(7) 2_656
O4 As3 1.784(7) 2_455
O6 As2 1.777(6) 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 115.1(11) 2_646 2_656
O1 As1 O2 As2 -6.1(8) . .
O1 As1 O2 As2 89.1(8) 2_646 .
O2 As1 O1 As1 -145.6(9) . 2_656
O2 As2 O3 As4 82.8(11) . .
O3 As2 O2 As1 172.4(7) . .
O3 As4 O5 As3 100.4(8) . .
O3 As4 O6 As2 -178.6(14) . 1_545
O4 As3 O4 As3 152.2(13) 2_445 2_455
O4 As3 O5 As4 -14.0(8) . .
O4 As3 O5 As4 76.9(9) 2_445 .
O5 As3 O4 As3 -108.0(9) . 2_455
O5 As4 O3 As2 91.8(12) . .
O5 As4 O6 As2 86.6(11) . 1_545
O6 As2 O2 As1 79.7(8) 1_565 .
O6 As2 O3 As4 -178.1(14) 1_565 .
O6 As4 O3 As2 -1.5(10) . .
O6 As4 O5 As3 -168.2(8) . .
