#------------------------------------------------------------------------------
#$Date: 2015-09-05 22:32:59 +0200 (Sat 05 de Sep de 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513282.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_4513282
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                 143.381(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8439(14)
_cell_length_b                   4.46320(10)
_cell_length_c                   17.122(3)
_cell_measurement_pressure       2.59e6(5)
_cell_measurement_reflns_used    522
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.8560
_cell_measurement_theta_min      2.9010
_cell_volume                     585.47(16)
_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         2.59e6(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.426
_diffrn_measured_fraction_theta_max 0.237
_diffrn_measurement_details
;
  1 phi    151.50  197.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
   0.0000    0.0000    0.0000     -     91
;
_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      -0.0300386000
_diffrn_orient_matrix_UB_12      0.0082574000
_diffrn_orient_matrix_UB_13      0.0193266000
_diffrn_orient_matrix_UB_21      -0.0147095000
_diffrn_orient_matrix_UB_22      0.0724996000
_diffrn_orient_matrix_UB_23      -0.0174640000
_diffrn_orient_matrix_UB_31      -0.0229187000
_diffrn_orient_matrix_UB_32      -0.0574517000
_diffrn_orient_matrix_UB_33      -0.0192306000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_laue_measured_fraction_full 0.426
_diffrn_reflns_laue_measured_fraction_max 0.237
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1167
_diffrn_reflns_point_group_measured_fraction_full 0.426
_diffrn_reflns_point_group_measured_fraction_max 0.237
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.839
_diffrn_reflns_theta_min         2.274
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    5.187
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59082
_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    4.489
_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         2.285
_refine_diff_density_min         -1.809
_refine_diff_density_rms         0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         735
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0646
_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)+(0.1004P)²+11.5502P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                638
_reflns_number_total             735
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_006middle_frames_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        585.47(14)
_cod_database_code               4513282
_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_006middle_frames_pl.res created by SHELXL-2014/7

TITL mclau2_006middle_frames_a.res in P2(1)/c
CELL 0.41427 12.8439 4.4632 17.122 90 143.381 90
ZERR 4 0.0014 0.0001 0.003 0 0.008 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 4
OMIT -17 1 9
OMIT -2 7 6
REM <olex2.extras>
REM <HklSrc "%./mclau2_006middle_frames_pl.hkl">
REM </olex2.extras>

WGHT    0.100400   11.550200
FVAR       0.39973
AS1   1    0.674458    0.259390    0.397090    11.00000    0.01482
AS2   1    0.381538    0.190938    0.346387    11.00000    0.01202
AS3   1   -0.190104   -0.318756    0.096480    11.00000    0.01443
AS4   1    0.105766   -0.310809    0.150341    11.00000    0.01139
O1    2    0.705514    0.435631    0.509650    11.00000    0.02548
O2    2    0.464677    0.139097    0.300620    11.00000    0.01885
O3    2    0.165379    0.075171    0.188193    11.00000    0.00845
O4    2   -0.256534   -0.196710   -0.035279    11.00000    0.02932
O5    2    0.034768   -0.326281    0.204637    11.00000    0.02456
O6    2    0.325351   -0.425533    0.307691    11.00000    0.01240
HKLF 4 1 0 0 -1 0 -1 0 -1 0 1

REM  mclau2_006middle_frames_a.res in P2(1)/c
REM R1 =  0.0646 for     638 Fo > 4sig(Fo)  and  0.0725 for all     735 data
REM     41 parameters refined using      0 restraints

END

WGHT      0.0999     11.5652

REM Highest difference peak  2.285,  deepest hole -1.809,  1-sigma level  0.347
Q1    1   0.8037 -0.1734  0.5527  11.00000  0.05    1.50
Q2    1   0.0011 -0.1239  0.1004  11.00000  0.05    1.26
Q3    1  -0.4747 -0.1179 -0.0003  11.00000  0.05    1.22
Q4    1   0.4915  0.3469  0.3792  11.00000  0.05    1.15
Q5    1   0.0350 -0.4735  0.1433  11.00000  0.05    1.12
Q6    1   0.7772  0.3322  0.4206  11.00000  0.05    1.10
Q7    1  -0.1903 -0.0432  0.0607  11.00000  0.05    1.05
Q8    1   0.5359 -0.1690  0.2706  11.00000  0.05    1.03
Q9    1  -0.2128 -0.5394  0.0685  11.00000  0.05    1.02
Q10   1   0.5357 -0.0754  0.1832  11.00000  0.05    1.02
Q11   1  -0.0279 -0.3020  0.0331  11.00000  0.05    1.00
Q12   1   0.2616  0.6505  0.2900  11.00000  0.05    1.00
Q13   1   0.4503  0.0019  0.3775  11.00000  0.05    0.99
Q14   1   1.0028  0.5366  0.6319  11.00000  0.05    0.99
Q15   1   0.8070  0.3286  0.4983  11.00000  0.05    0.99
Q16   1   0.9554  0.0058  0.5596  11.00000  0.05    0.93
Q17   1   0.5387  0.4004  0.3617  11.00000  0.05    0.92
Q18   1   0.2786 -0.0460  0.1517  11.00000  0.05    0.92
Q19   1   0.4639  0.6410  0.1788  11.00000  0.05    0.91
Q20   1   0.4662  0.1998  0.2696  11.00000  0.05    0.87
;
_shelx_res_checksum              82031
_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 0.67446(18) 0.2594(3) 0.3971(3) 0.0148(4) Uiso 1 1 d
As2 As 0.38154(18) 0.1909(3) 0.3464(2) 0.0120(4) Uiso 1 1 d
As3 As -0.19010(18) -0.3188(3) 0.0965(3) 0.0144(4) Uiso 1 1 d
As4 As 0.10577(17) -0.3108(2) 0.1503(2) 0.0114(4) Uiso 1 1 d
O1 O 0.7055(15) 0.436(2) 0.510(2) 0.025(2) Uiso 1 1 d
O2 O 0.4647(14) 0.139(2) 0.301(2) 0.0188(19) Uiso 1 1 d
O3 O 0.1654(11) 0.0752(17) 0.1882(16) 0.0084(15) Uiso 1 1 d
O4 O -0.2565(17) -0.197(3) -0.035(3) 0.029(3) Uiso 1 1 d
O5 O 0.0348(16) -0.326(2) 0.205(2) 0.025(2) Uiso 1 1 d
O6 O 0.3254(12) -0.4255(18) 0.3077(17) 0.0124(16) Uiso 1 1 d
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(6) 2_646 .
O1 As1 O2 99.6(5) 2_646 .
O2 As1 O1 89.7(8) . .
O2 As2 O3 92.6(7) . .
O6 As2 O2 99.8(7) 1_565 .
O6 As2 O3 92.4(5) 1_565 .
O4 As3 O4 88.7(7) . 2_445
O4 As3 O5 93.0(10) . .
O5 As3 O4 97.4(6) . 2_445
O3 As4 O6 91.8(4) . .
O5 As4 O3 95.7(7) . .
O5 As4 O6 93.0(9) . .
As1 O1 As1 127.7(12) 2_656 .
As1 O2 As2 123.6(12) . .
As4 O3 As2 121.2(6) . .
As3 O4 As3 127.4(14) . 2_455
As4 O5 As3 123.2(15) . .
As2 O6 As4 120.8(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 1.750(13) 2_646
As1 O1 1.81(3) .
As1 O2 1.770(10) .
As2 O2 1.78(2) .
As2 O3 1.800(12) .
As2 O6 1.767(9) 1_565
As3 O4 1.74(3) .
As3 O4 1.806(15) 2_445
As3 O5 1.785(11) .
As4 O3 1.783(8) .
As4 O5 1.75(3) .
As4 O6 1.810(12) .
O1 As1 1.750(13) 2_656
O4 As3 1.806(15) 2_455
O6 As2 1.767(9) 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 112.2(11) 2_646 2_656
O1 As1 O2 As2 91.0(11) 2_646 .
O1 As1 O2 As2 -5.3(9) . .
O2 As1 O1 As1 -148.1(10) . 2_656
O2 As2 O3 As4 84.9(11) . .
O3 As2 O2 As1 170.2(8) . .
O3 As4 O5 As3 101.7(7) . .
O3 As4 O6 As2 -176.4(13) . 1_545
O4 As3 O4 As3 163.0(11) 2_445 2_455
O4 As3 O5 As4 74.3(12) 2_445 .
O4 As3 O5 As4 -14.8(8) . .
O5 As3 O4 As3 -99.6(9) . 2_455
O5 As4 O3 As2 89.5(11) . .
O5 As4 O6 As2 87.7(12) . 1_545
O6 As2 O2 As1 77.3(9) 1_565 .
O6 As2 O3 As4 -175.1(12) 1_565 .
O6 As4 O3 As2 -3.7(11) . .
O6 As4 O5 As3 -166.2(6) . .
