#------------------------------------------------------------------------------
#$Date: 2015-09-05 23:32:59 +0300 (Sat, 05 Sep 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513283.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_4513283
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                 143.284(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7203(7)
_cell_length_b                   4.42690(10)
_cell_length_c                   16.8699(13)
_cell_measurement_pressure       3.75e6(5)
_cell_measurement_reflns_used    741
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.3700
_cell_measurement_theta_min      2.9300
_cell_volume                     567.94(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         3.75e6(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.458
_diffrn_measured_fraction_theta_max 0.271
_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      0.0306254000
_diffrn_orient_matrix_UB_12      0.0082714000
_diffrn_orient_matrix_UB_13      -0.0195544000
_diffrn_orient_matrix_UB_21      0.0147769000
_diffrn_orient_matrix_UB_22      0.0730938000
_diffrn_orient_matrix_UB_23      0.0175745000
_diffrn_orient_matrix_UB_31      0.0230330000
_diffrn_orient_matrix_UB_32      -0.0578974000
_diffrn_orient_matrix_UB_33      0.0193840000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_laue_measured_fraction_full 0.458
_diffrn_reflns_laue_measured_fraction_max 0.271
_diffrn_reflns_limit_h_max       16
_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       -11
_diffrn_reflns_number            1648
_diffrn_reflns_point_group_measured_fraction_full 0.458
_diffrn_reflns_point_group_measured_fraction_max 0.271
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.521
_diffrn_reflns_theta_min         2.289
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    5.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60276
_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    4.628
_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         2.049
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0452
_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)+(0.0718P)²+6.3956P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                672
_reflns_number_total             784
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_008_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        567.94(6)
_cod_database_code               4513283
_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_008_pl.res created by SHELXL-2014/7

TITL mclau2_008_a.res in P2(1)/c
CELL 0.41427 12.7203 4.4269 16.8699 90 143.284 90
ZERR 4 0.0007 0.0001 0.0013 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 -9 6 6
OMIT 5 4 4
OMIT -10 6 8
REM <olex2.extras>
REM <HklSrc "%./mclau2_008_pl.hkl">
REM </olex2.extras>

WGHT    0.071800    6.395600
FVAR       0.38845
AS1   1    0.671718    0.271255    0.394653    11.00000    0.01047    0.01436 =
         0.01819    0.00166    0.01033   -0.00080
AS2   1    0.380153    0.196529    0.347364    11.00000    0.01230    0.00880 =
         0.01356    0.00179    0.01033    0.00222
AS3   1   -0.192660   -0.330178    0.096442    11.00000    0.01207    0.01121 =
         0.01695    0.00002    0.01129    0.00086
AS4   1    0.102485   -0.305566    0.147977    11.00000    0.01026    0.00846 =
         0.01333   -0.00097    0.00846   -0.00123
O1    2    0.699610    0.451874    0.505971    11.00000    0.02128
O2    2    0.464307    0.135290    0.301276    11.00000    0.01564
O3    2    0.162339    0.084523    0.185485    11.00000    0.00786
O4    2   -0.264789   -0.214528   -0.046097    11.00000    0.02366
O5    2    0.034700   -0.323794    0.209981    11.00000    0.01780
O6    2    0.323506   -0.416160    0.305720    11.00000    0.00803
HKLF 4 1 0 0 -1 0 -1 0 -1 0 1

REM  mclau2_008_a.res in P2(1)/c
REM R1 =  0.0452 for     672 Fo > 4sig(Fo)  and  0.0537 for all     784 data
REM     61 parameters refined using      0 restraints

END

WGHT      0.0724      6.3466

REM Highest difference peak  2.049,  deepest hole -1.359,  1-sigma level  0.280
Q1    1  -0.1771 -0.2075  0.1075  11.00000  0.05    2.05
Q2    1   0.8102  0.6299  0.6022  11.00000  0.05    1.34
Q3    1  -0.1932 -0.1243  0.0017  11.00000  0.05    1.01
Q4    1  -0.1822 -0.5415  0.0874  11.00000  0.05    0.95
Q5    1   0.4687  0.2632  0.3198  11.00000  0.05    0.94
Q6    1   0.4502  0.1966  0.2587  11.00000  0.05    0.92
Q7    1   0.5541  0.4075  0.3496  11.00000  0.05    0.87
Q8    1   0.2039 -0.0871  0.2067  11.00000  0.05    0.79
Q9    1   0.3376 -0.1099  0.2414  11.00000  0.05    0.77
Q10   1   0.0936  0.2769  0.0615  11.00000  0.05    0.76
Q11   1   0.3775  0.4267  0.3484  11.00000  0.05    0.76
Q12   1   0.7747  0.3126  0.4109  11.00000  0.05    0.76
Q13   1   0.5055  0.3214  0.3999  11.00000  0.05    0.75
Q14   1   0.2661  0.1212  0.2812  11.00000  0.05    0.74
Q15   1   0.8317 -0.0554  0.5911  11.00000  0.05    0.74
Q16   1   0.2559 -0.2881  0.3076  11.00000  0.05    0.74
Q17   1   0.5580  0.2938  0.4582  11.00000  0.05    0.72
Q18   1  -0.2001 -0.0274  0.0806  11.00000  0.05    0.72
Q19   1   0.4934  0.3538  0.2603  11.00000  0.05    0.70
Q20   1   0.7999  0.7403  0.4850  11.00000  0.05    0.70
;
_shelx_res_checksum              63959
_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 0.67172(13) 0.2713(2) 0.39465(18) 0.0161(10) Uani 1 1 d
As2 As 0.38015(13) 0.19653(17) 0.34736(18) 0.0116(10) Uani 1 1 d
As3 As -0.19266(13) -0.33018(19) 0.09644(18) 0.0139(10) Uani 1 1 d
As4 As 0.10248(12) -0.30557(17) 0.14798(18) 0.0122(10) Uani 1 1 d
O1 O 0.6996(10) 0.4519(16) 0.5060(15) 0.0213(15) Uiso 1 1 d
O2 O 0.4643(10) 0.1353(15) 0.3013(13) 0.0156(13) Uiso 1 1 d
O3 O 0.1623(8) 0.0845(12) 0.1855(12) 0.0079(11) Uiso 1 1 d
O4 O -0.2648(12) -0.2145(17) -0.0461(16) 0.0237(17) Uiso 1 1 d
O5 O 0.0347(10) -0.3238(14) 0.2100(15) 0.0178(15) Uiso 1 1 d
O6 O 0.3235(8) -0.4162(12) 0.3057(12) 0.0080(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 0.0105(4) 0.0144(4) 0.0182(18) 0.0017(5) 0.0103(7) -0.0008(3)
As2 0.0123(4) 0.0088(4) 0.0136(19) 0.0018(4) 0.0103(7) 0.0022(3)
As3 0.0121(4) 0.0112(4) 0.0169(19) 0.0000(4) 0.0113(7) 0.0009(3)
As4 0.0103(4) 0.0085(4) 0.0133(18) -0.0010(4) 0.0085(7) -0.0012(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 96.2(3) 2_646 .
O1 As1 O2 99.2(4) 2_646 .
O2 As1 O1 89.2(5) . .
O2 As2 O3 91.6(5) . .
O6 As2 O2 99.8(5) 1_565 .
O6 As2 O3 91.3(3) 1_565 .
O4 As3 O4 90.0(5) 2_445 .
O5 As3 O4 94.6(6) . .
O5 As3 O4 98.0(3) . 2_445
O3 As4 O5 95.9(5) . .
O3 As4 O6 91.3(3) . .
O6 As4 O5 92.1(5) . .
As1 O1 As1 127.4(7) 2_656 .
As1 O2 As2 123.3(7) . .
As4 O3 As2 120.2(4) . .
As3 O4 As3 122.3(9) 2_455 .
As3 O5 As4 119.7(9) . .
As2 O6 As4 120.4(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 1.758(9) 2_646
As1 O1 1.795(17) .
As1 O2 1.772(6) .
As2 O2 1.777(14) .
As2 O3 1.803(9) .
As2 O6 1.772(6) 1_565
As3 O4 1.830(19) .
As3 O4 1.781(9) 2_445
As3 O5 1.776(7) .
As4 O3 1.786(5) .
As4 O5 1.814(16) .
As4 O6 1.797(8) .
O1 As1 1.758(9) 2_656
O4 As3 1.781(9) 2_455
O6 As2 1.772(5) 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 106.8(7) 2_646 2_656
O1 As1 O2 As2 -3.1(6) . .
O1 As1 O2 As2 93.1(7) 2_646 .
O2 As1 O1 As1 -154.1(7) . 2_656
O2 As2 O3 As4 84.6(8) . .
O3 As2 O2 As1 165.6(6) . .
O3 As4 O5 As3 104.0(4) . .
O3 As4 O6 As2 -178.0(9) . 1_545
O4 As3 O4 As3 167.5(7) 2_445 2_455
O4 As3 O5 As4 -14.0(5) . .
O4 As3 O5 As4 76.7(7) 2_445 .
O5 As3 O4 As3 -94.5(5) . 2_455
O5 As4 O3 As2 86.7(8) . .
O5 As4 O6 As2 86.0(8) . 1_545
O6 As2 O2 As1 74.0(6) 1_565 .
O6 As2 O3 As4 -175.6(9) 1_565 .
O6 As4 O3 As2 -5.5(8) . .
O6 As4 O5 As3 -164.5(4) . .
