#------------------------------------------------------------------------------
#$Date: 2015-09-05 22:32:59 +0200 (Sat 05 de Sep de 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513285.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_4513285
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             2015-02-04
_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                 143.183(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5859(5)
_cell_length_b                   4.3845(5)
_cell_length_c                   16.5934(9)
_cell_measurement_pressure       5.14e6(7)
_cell_measurement_reflns_used    764
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.9850
_cell_measurement_theta_min      2.8680
_cell_volume                     548.73(8)
_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         5.14e6(7)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.454
_diffrn_measured_fraction_theta_max 0.261
_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      0.0312827000
_diffrn_orient_matrix_UB_12      0.0082453000
_diffrn_orient_matrix_UB_13      -0.0198267000
_diffrn_orient_matrix_UB_21      0.0148009000
_diffrn_orient_matrix_UB_22      0.0739300000
_diffrn_orient_matrix_UB_23      0.0176474000
_diffrn_orient_matrix_UB_31      0.0232164000
_diffrn_orient_matrix_UB_32      -0.0582433000
_diffrn_orient_matrix_UB_33      0.0195884000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_laue_measured_fraction_full 0.454
_diffrn_reflns_laue_measured_fraction_max 0.261
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1594
_diffrn_reflns_point_group_measured_fraction_full 0.454
_diffrn_reflns_point_group_measured_fraction_max 0.261
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.747
_diffrn_reflns_theta_min         2.868
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    5.534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64426
_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    4.790
_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         2.448
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.301
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         753
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0488
_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)+(0.0780P)²+5.9690P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                664
_reflns_number_total             753
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_010_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        548.73(7)
_cod_database_code               4513285
_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
;
    mclau_010_pl.res created by SHELXL-2014/7

TITL mclau_010_a.res in P2(1)/c
CELL 0.41427 12.5859 4.3845 16.5934 90 143.183 90
ZERR 4 0.0005 0.000488 0.0009 0 0.003 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 5 4 1
OMIT -18 1 11
OMIT 5 4 2
OMIT 6 3 3
OMIT 5 4 4
OMIT -14 2 7
OMIT 0 2 0
OMIT -4 -1 2
OMIT -9 5 6
REM <olex2.extras>
REM <HklSrc "%./mclau_010_pl.hkl">
REM </olex2.extras>

WGHT    0.078000    5.969000
FVAR       0.40005
AS1   1    0.669418    0.279809    0.392734    11.00000    0.01176    0.01442 =
         0.02014    0.00130    0.01230   -0.00074
AS2   1    0.378951    0.201369    0.348488    11.00000    0.01294    0.00898 =
         0.01847    0.00094    0.01249    0.00148
AS3   1   -0.194877   -0.339098    0.096825    11.00000    0.01187    0.01119 =
         0.01944   -0.00120    0.01200    0.00001
AS4   1    0.099527   -0.301572    0.145679    11.00000    0.01057    0.00859 =
         0.01426   -0.00081    0.00911   -0.00054
O1    2    0.694452    0.461094    0.503451    11.00000    0.01656
O2    2    0.463485    0.132220    0.301187    11.00000    0.01734
O3    2    0.159441    0.091847    0.184423    11.00000    0.00993
O4    2   -0.268590   -0.230186   -0.047798    11.00000    0.01870
O5    2    0.033905   -0.324668    0.211354    11.00000    0.01463
O6    2    0.324149   -0.407175    0.306267    11.00000    0.01002
HKLF 4 1 0 0 -1 0 -1 0 -1 0 1

REM  mclau_010_a.res in P2(1)/c
REM R1 =  0.0488 for     664 Fo > 4sig(Fo)  and  0.0548 for all     753 data
REM     61 parameters refined using      0 restraints

END

WGHT      0.0780      5.9437

REM Highest difference peak  2.448,  deepest hole -1.219,  1-sigma level  0.301
Q1    1  -0.1762 -0.2062  0.1014  11.00000  0.05    2.45
Q2    1   0.8117  0.6359  0.6017  11.00000  0.05    1.77
Q3    1   0.8413 -0.0365  0.6113  11.00000  0.05    1.11
Q4    1   0.5896  0.2783  0.3681  11.00000  0.05    1.10
Q5    1  -0.2028 -0.5459  0.0696  11.00000  0.05    1.06
Q6    1   0.9957  0.3104  0.6599  11.00000  0.05    0.92
Q7    1  -0.0925 -0.3774  0.1285  11.00000  0.05    0.92
Q8    1   0.7595  0.4306  0.5302  11.00000  0.05    0.90
Q9    1   0.7172  0.6481  0.3123  11.00000  0.05    0.86
Q10   1   0.5210  0.1974  0.1803  11.00000  0.05    0.84
Q11   1   0.3796  0.4142  0.3622  11.00000  0.05    0.84
Q12   1   0.8036 -0.2138  0.4888  11.00000  0.05    0.83
Q13   1   0.2079 -0.0727  0.2294  11.00000  0.05    0.82
Q14   1   0.2817  0.3487  0.1995  11.00000  0.05    0.80
Q15   1  -0.3389 -0.1454  0.1201  11.00000  0.05    0.78
Q16   1   0.2673  0.2907  0.1183  11.00000  0.05    0.78
Q17   1   0.1855  0.6994  0.1905  11.00000  0.05    0.77
Q18   1   0.9891  0.1116  0.5203  11.00000  0.05    0.76
Q19   1  -0.0211 -0.6507  0.0698  11.00000  0.05    0.76
Q20   1   0.2773  0.1260  0.2506  11.00000  0.05    0.75
;
_shelx_res_checksum              51573
_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 0.66942(14) 0.2798(2) 0.3927(2) 0.0161(10) Uani 1 1 d
As2 As 0.37895(14) 0.20137(18) 0.34849(19) 0.0136(10) Uani 1 1 d
As3 As -0.19488(13) -0.3391(2) 0.09682(19) 0.0150(10) Uani 1 1 d
As4 As 0.09953(13) -0.30157(18) 0.14568(19) 0.0124(10) Uani 1 1 d
O1 O 0.6945(10) 0.4611(14) 0.5035(14) 0.0166(13) Uiso 1 1 d
O2 O 0.4635(10) 0.1322(15) 0.3012(14) 0.0173(15) Uiso 1 1 d
O3 O 0.1594(9) 0.0918(13) 0.1844(13) 0.0099(11) Uiso 1 1 d
O4 O -0.2686(11) -0.2302(17) -0.0478(15) 0.0187(15) Uiso 1 1 d
O5 O 0.0339(10) -0.3247(14) 0.2114(14) 0.0146(13) Uiso 1 1 d
O6 O 0.3241(9) -0.4072(13) 0.3063(12) 0.0100(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 0.0118(4) 0.0144(4) 0.0201(19) 0.0013(5) 0.0123(7) -0.0007(3)
As2 0.0129(4) 0.0090(4) 0.0185(19) 0.0009(4) 0.0125(7) 0.0015(3)
As3 0.0119(4) 0.0112(4) 0.0194(19) -0.0012(4) 0.0120(7) 0.0000(3)
As4 0.0106(4) 0.0086(4) 0.0143(18) -0.0008(4) 0.0091(7) -0.0005(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 96.6(3) 2_646 .
O1 As1 O2 99.1(4) 2_646 .
O2 As1 O1 88.7(6) . .
O2 As2 O3 91.3(5) . .
O6 As2 O2 99.9(5) 1_565 .
O6 As2 O3 91.2(4) 1_565 .
O4 As3 O4 88.7(4) 2_445 .
O5 As3 O4 94.6(6) . .
O5 As3 O4 97.3(3) . 2_445
O3 As4 O5 95.8(5) . .
O3 As4 O6 90.3(3) . .
O6 As4 O5 91.5(5) . .
As1 O1 As1 126.1(7) 2_656 .
As1 O2 As2 122.6(8) . .
As4 O3 As2 119.9(5) . .
As3 O4 As3 121.8(8) 2_455 .
As3 O5 As4 119.0(9) . .
As2 O6 As4 119.1(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 1.769(8) 2_646
As1 O1 1.783(16) .
As1 O2 1.772(7) .
As2 O2 1.782(14) .
As2 O3 1.798(9) .
As2 O6 1.772(6) 1_565
As3 O4 1.812(18) .
As3 O4 1.793(9) 2_445
As3 O5 1.773(7) .
As4 O3 1.784(6) .
As4 O5 1.822(15) .
As4 O6 1.802(8) .
O1 As1 1.769(8) 2_656
O4 As3 1.793(9) 2_455
O6 As2 1.772(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 103.0(7) 2_646 2_656
O1 As1 O2 As2 -1.3(6) . .
O1 As1 O2 As2 95.1(7) 2_646 .
O2 As1 O1 As1 -158.0(7) . 2_656
O2 As2 O3 As4 83.0(8) . .
O3 As2 O2 As1 162.6(6) . .
O3 As4 O5 As3 105.1(4) . .
O3 As4 O6 As2 -179.7(9) . 1_545
O4 As3 O4 As3 171.7(6) 2_445 2_455
O4 As3 O5 As4 -13.0(5) . .
O4 As3 O5 As4 76.3(7) 2_445 .
O5 As3 O4 As3 -91.1(5) . 2_455
O5 As4 O3 As2 86.1(8) . .
O5 As4 O6 As2 84.5(8) . 1_545
O6 As2 O2 As1 71.2(7) 1_565 .
O6 As2 O3 As4 -177.1(9) 1_565 .
O6 As4 O3 As2 -5.5(8) . .
O6 As4 O5 As3 -164.4(4) . .
