#------------------------------------------------------------------------------
#$Date: 2015-09-05 23:32:59 +0300 (Sat, 05 Sep 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513281.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_4513281
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'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-04
_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                 143.480(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9231(8)
_cell_length_b                   4.48160(10)
_cell_length_c                   17.2952(15)
_cell_measurement_pressure       2.08e6(11)
_cell_measurement_reflns_used    702
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.0130
_cell_measurement_theta_min      2.8920
_cell_volume                     596.10(9)
_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         2.08e6(11)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.449
_diffrn_measured_fraction_theta_max 0.282
_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      -0.0297266000
_diffrn_orient_matrix_UB_12      0.0080920000
_diffrn_orient_matrix_UB_13      0.0191700000
_diffrn_orient_matrix_UB_21      -0.0147356000
_diffrn_orient_matrix_UB_22      0.0721586000
_diffrn_orient_matrix_UB_23      -0.0173622000
_diffrn_orient_matrix_UB_31      -0.0228043000
_diffrn_orient_matrix_UB_32      -0.0572326000
_diffrn_orient_matrix_UB_33      -0.0191604000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_laue_measured_fraction_full 0.449
_diffrn_reflns_laue_measured_fraction_max 0.282
_diffrn_reflns_limit_h_max       19
_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            1606
_diffrn_reflns_point_group_measured_fraction_full 0.449
_diffrn_reflns_point_group_measured_fraction_max 0.282
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.193
_diffrn_reflns_theta_min         2.267
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    5.094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59384
_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    4.409
_exptl_crystal_description       block
_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         1.174
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       0.020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         816
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0481
_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)+(0.0540P)²+5.9860P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                652
_reflns_number_total             816
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_005_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        596.10(7)
_cod_database_code               4513281
_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
;
;
_shelx_res_file
;
    mclau2_005_pl.res created by SHELXL-2014/7

TITL mclau2_005_a.res in P2(1)/a
CELL 0.41427 12.9231 4.4816 17.2952 90 143.48 90
ZERR 4 0.0008 0.0001 0.0015 0 0.004 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

L.S. 10
PLAN  -20
BOND $H
CONF
MORE -1
fmap 2
acta
OMIT -6 6 8
OMIT 5 4 4
OMIT -8 6 5
REM <olex2.extras>
REM <HklSrc "%./mclau2_005_pl.hkl">
REM </olex2.extras>

WGHT    0.054000    5.986000
EXTI    0.020354
FVAR       2.19062
AS1   1    0.676745    0.247099    0.398581    11.00000    0.01347    0.01884 =
         0.01876    0.00004    0.01210   -0.00207
AS2   1    0.383180    0.186398    0.345868    11.00000    0.01448    0.01039 =
         0.01910    0.00101    0.01268    0.00124
AS3   1   -0.186668   -0.303939    0.097066    11.00000    0.01440    0.02059 =
         0.01690    0.00137    0.01261    0.00401
AS4   1    0.108469   -0.314576    0.151400    11.00000    0.01306    0.01037 =
         0.01812   -0.00085    0.01113   -0.00140
O1    2    0.710035    0.416970    0.511283    11.00000    0.02739
O2    2    0.463866    0.142097    0.299154    11.00000    0.02106
O3    2    0.168007    0.069875    0.188156    11.00000    0.01025
O4    2   -0.241115   -0.169781   -0.029671    11.00000    0.04416
O5    2    0.037138   -0.335669    0.207737    11.00000    0.02467
O6    2    0.323978   -0.430750    0.306223    11.00000    0.01155
HKLF 4 1 0 0 -1 0 -1 0 -1 0 1

REM  mclau2_005_a.res in P2(1)/a
REM R1 =  0.0481 for     652 Fo > 4sig(Fo)  and  0.0627 for all     816 data
REM     62 parameters refined using      0 restraints

END

WGHT      0.0543      5.9836

REM Highest difference peak  1.174,  deepest hole -1.602,  1-sigma level  0.260
Q1    1   0.4720  0.2928  0.3343  11.00000  0.05    1.11
Q2    1   0.0096 -0.1630  0.1210  11.00000  0.05    1.10
Q3    1   0.4848  0.3534  0.3870  11.00000  0.05    1.02
Q4    1  -0.1865 -0.0776  0.0093  11.00000  0.05    0.99
Q5    1  -0.2216 -0.0124 -0.0398  11.00000  0.05    0.92
Q6    1   0.0139 -0.2410  0.1804  11.00000  0.05    0.89
Q7    1  -0.4711 -0.4617 -0.0079  11.00000  0.05    0.85
Q8    1  -0.1877 -0.1811  0.0903  11.00000  0.05    0.81
Q9    1   0.5692  0.0682  0.3431  11.00000  0.05    0.76
Q10   1   0.7704 -0.1771  0.5109  11.00000  0.05    0.76
Q11   1   0.7694  0.3494  0.5415  11.00000  0.05    0.72
Q12   1   0.7851  0.3140  0.4105  11.00000  0.05    0.72
Q13   1   0.7468  0.1726  0.3079  11.00000  0.05    0.72
Q14   1   0.4599  0.4911  0.2804  11.00000  0.05    0.71
Q15   1   0.0301 -0.1302  0.0387  11.00000  0.05    0.70
Q16   1   0.5102  0.4908  0.1889  11.00000  0.05    0.69
Q17   1   0.9330 -0.0780  0.6298  11.00000  0.05    0.69
Q18   1   0.8058  0.6192  0.5713  11.00000  0.05    0.68
Q19   1  -0.0010 -0.3224  0.1014  11.00000  0.05    0.68
Q20   1  -0.1767 -0.2506  0.1674  11.00000  0.05    0.66
;
_shelx_res_checksum              89178
_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
As1 As 0.67674(13) 0.2471(2) 0.39858(18) 0.0183(10) Uani 1 1 d
As2 As 0.38318(13) 0.18640(18) 0.34587(18) 0.0159(10) Uani 1 1 d
As3 As -0.18667(13) -0.3039(2) 0.09707(19) 0.0173(11) Uani 1 1 d
As4 As 0.10847(12) -0.31458(18) 0.15140(17) 0.0160(10) Uani 1 1 d
O1 O 0.7100(11) 0.4170(16) 0.5113(15) 0.0274(17) Uiso 1 1 d
O2 O 0.4639(10) 0.1421(15) 0.2992(13) 0.0211(15) Uiso 1 1 d
O3 O 0.1680(8) 0.0699(12) 0.1882(11) 0.0103(11) Uiso 1 1 d
O4 O -0.2411(14) -0.170(2) -0.030(2) 0.044(3) Uiso 1 1 d
O5 O 0.0371(11) -0.3357(16) 0.2077(15) 0.0247(17) Uiso 1 1 d
O6 O 0.3240(8) -0.4307(12) 0.3062(12) 0.0116(11) Uiso 1 1 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 0.0135(4) 0.0188(5) 0.0188(19) 0.0000(5) 0.0121(7) -0.0021(3)
As2 0.0145(5) 0.0104(4) 0.0191(18) 0.0010(4) 0.0127(7) 0.0012(3)
As3 0.0144(5) 0.0206(5) 0.017(2) 0.0014(5) 0.0126(8) 0.0040(3)
As4 0.0131(4) 0.0104(4) 0.0181(18) -0.0009(4) 0.0111(7) -0.0014(3)
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 95.3(4) 2_646 .
O1 As1 O2 100.0(4) 2_646 .
O2 As1 O1 89.8(6) . .
O2 As2 O3 92.0(5) . .
O2 As2 O6 99.3(5) . 1_565
O6 As2 O3 91.9(3) 1_565 .
O4 As3 O4 91.4(5) 2_445 .
O5 As3 O4 92.5(6) . .
O5 As3 O4 100.1(4) . 2_445
O3 As4 O5 96.9(5) . .
O3 As4 O6 92.3(3) . .
O6 As4 O5 91.9(6) . .
As1 O1 As1 128.5(8) 2_656 .
As2 O2 As1 123.5(8) . .
As4 O3 As2 121.2(4) . .
As3 O4 As3 126.6(11) 2_455 .
As3 O5 As4 120.7(9) . .
As2 O6 As4 121.8(4) 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 1.759(9) 2_646
As1 O1 1.793(18) .
As1 O2 1.773(7) .
As2 O2 1.770(15) .
As2 O3 1.804(9) .
As2 O6 1.777(6) 1_565
As3 O4 1.78(2) .
As3 O4 1.780(12) 2_445
As3 O5 1.775(7) .
As4 O3 1.783(5) .
As4 O5 1.803(16) .
As4 O6 1.792(8) .
O1 As1 1.759(9) 2_656
O4 As3 1.780(12) 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 117.3(8) 2_646 2_656
O1 As1 O2 As2 87.9(7) 2_646 .
O1 As1 O2 As2 -7.4(6) . .
O2 As1 O1 As1 -142.6(7) . 2_656
O2 As2 O3 As4 86.9(8) . .
O3 As2 O2 As1 173.9(5) . .
O3 As4 O5 As3 97.3(5) . .
O3 As4 O6 As2 -174.9(10) . 1_545
O4 As3 O4 As3 148.2(9) 2_445 2_455
O4 As3 O5 As4 78.5(9) 2_445 .
O4 As3 O5 As4 -13.3(6) . .
O5 As3 O4 As3 -111.7(7) . 2_455
O5 As4 O3 As2 88.1(8) . .
O5 As4 O6 As2 88.1(8) . 1_545
O6 As2 O2 As1 81.6(6) 1_565 .
O6 As2 O3 As4 -173.7(9) 1_565 .
O6 As4 O3 As2 -4.0(8) . .
O6 As4 O5 As3 -170.1(4) . .
