#------------------------------------------------------------------------------
#$Date: 2015-09-05 23:32:59 +0300 (Sat, 05 Sep 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513279.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_4513279
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         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-02
_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                 102.155(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9615(4)
_cell_length_b                   4.53586(14)
_cell_length_c                   8.911(3)
_cell_measurement_pressure       7.4e5(5)
_cell_measurement_reflns_used    436
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.5460
_cell_measurement_theta_min      2.9490
_cell_volume                     314.58(11)
_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         7.4e5(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.444
_diffrn_measured_fraction_theta_max 0.266
_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      0.0097067000
_diffrn_orient_matrix_UB_12      -0.0081001000
_diffrn_orient_matrix_UB_13      0.0473782000
_diffrn_orient_matrix_UB_21      0.0318410000
_diffrn_orient_matrix_UB_22      -0.0712462000
_diffrn_orient_matrix_UB_23      -0.0024593000
_diffrn_orient_matrix_UB_31      0.0415172000
_diffrn_orient_matrix_UB_32      0.0565303000
_diffrn_orient_matrix_UB_33      0.0036861000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_laue_measured_fraction_full 0.444
_diffrn_reflns_laue_measured_fraction_max 0.266
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            878
_diffrn_reflns_point_group_measured_fraction_full 0.444
_diffrn_reflns_point_group_measured_fraction_max 0.266
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.544
_diffrn_reflns_theta_min         2.951
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    4.826
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63134
_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    4.177
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         426
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0338
_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)+(0.0480P)²+0.3110P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                399
_reflns_number_total             426
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_003
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        314.59(11)
_cod_database_code               4513279
_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_003.res created by SHELXL-2014/7

TITL mclau2_003_a.res in P2(1)/n
REM Old TITL mclau2_003 in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.123, Rweak 0.011, Alpha 0.035, Orientation as input
REM Formula found by SHELXT: O As
CELL 0.41427 7.961526 4.535859 8.911145 90 102.1552 90
ZERR 4 0.000401 0.000138 0.003056 0 0.0141 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.311 0.799 1882.762
DISP O 0.002 0.002 10.067
UNIT 12 8

L.S. 10
PLAN  20
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta
OMIT 1 1 1
OMIT -6 4 5
OMIT -6 4 5
REM <olex2.extras>
REM <HklSrc "%./mclau2_003.hkl">
REM </olex2.extras>

WGHT    0.048000    0.311000
FVAR       0.79708
AS1   2    0.682848    0.215072    0.124646    11.00000    0.01309    0.01670 =
         0.01696    0.00187    0.00397   -0.00150
AS2   2    0.385416    0.175605    0.303622    11.00000    0.01437    0.01142 =
         0.02269    0.00031    0.00515    0.00155
O1    1    0.728490    0.367171    0.314571    11.00000    0.03885    0.02950 =
         0.02460   -0.00301    0.00106   -0.02243
O2    1    0.464816    0.151624    0.129499    11.00000    0.01321    0.04058 =
         0.03626   -0.01228    0.01256    0.00069
O3    1    0.175077    0.051688    0.212232    11.00000    0.01386    0.01103 =
         0.05334   -0.00036    0.00833    0.00001
HKLF 4

REM  mclau2_003_a.res in P2(1)/n
REM R1 =  0.0338 for     399 Fo > 4sig(Fo)  and  0.0362 for all     426 data
REM     46 parameters refined using      0 restraints

END

WGHT      0.0480      0.3116

REM Highest difference peak  0.658,  deepest hole -0.723,  1-sigma level  0.198
Q1    1   0.7830  0.1175 -0.0261  11.00000  0.05    0.66
Q2    1   0.2608  0.1186  0.2601  11.00000  0.05    0.65
Q3    1   0.7273  0.4970  0.3523  11.00000  0.05    0.63
Q4    1   0.8208  0.2058  0.1912  11.00000  0.05    0.58
Q5    1   0.1349  0.1449  0.3455  11.00000  0.05    0.57
Q6    1   0.4781  0.3953  0.2753  11.00000  0.05    0.56
Q7    1   0.4989  0.1922  0.0265  11.00000  0.05    0.56
Q8    1   0.7643  0.1705  0.4153  11.00000  0.05    0.53
Q9    1   0.8218  0.3481  0.3384  11.00000  0.05    0.53
Q10   1   0.5572  0.1464  0.1232  11.00000  0.05    0.53
Q11   1   0.7968  0.3359  0.2879  11.00000  0.05    0.52
Q12   1   0.3822 -0.0019  0.3032  11.00000  0.05    0.51
Q13   1   0.5038  0.2776  0.2765  11.00000  0.05    0.50
Q14   1  -0.0572  0.2118  0.1036  11.00000  0.05    0.49
Q15   1  -0.0008 -0.0498  0.0456  11.00000  0.05    0.49
Q16   1   0.5200  0.2716  0.3131  11.00000  0.05    0.48
Q17   1   0.4855  0.2753 -0.0447  11.00000  0.05    0.48
Q18   1   0.0163 -0.0654  0.1239  11.00000  0.05    0.47
Q19   1   0.2211  0.3249  0.0424  11.00000  0.05    0.47
Q20   1   0.1923  0.1449  0.1841  11.00000  0.05    0.47
;
_shelx_res_checksum              62251
_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+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.68285(7) 0.21507(12) 0.12465(17) 0.0155(7) Uani 1 1 d
As2 As 0.38542(7) 0.17561(11) 0.30362(17) 0.0160(7) Uani 1 1 d
O1 O 0.7285(8) 0.3672(11) 0.3146(17) 0.032(6) Uani 1 1 d
O2 O 0.4648(6) 0.1516(12) 0.1295(14) 0.029(5) Uani 1 1 d
O3 O 0.1751(5) 0.0517(8) 0.2122(12) 0.026(5) Uani 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 0.0131(3) 0.0167(3) 0.017(2) 0.0019(4) 0.0040(6) -0.00150(18)
As2 0.0144(3) 0.0114(3) 0.023(2) 0.0003(3) 0.0051(6) 0.00155(17)
O1 0.039(3) 0.030(2) 0.025(19) -0.003(4) 0.001(5) -0.022(2)
O2 0.0132(16) 0.041(3) 0.036(17) -0.012(4) 0.013(4) 0.0007(17)
O3 0.0139(14) 0.0110(13) 0.053(15) 0.000(3) 0.008(4) 0.0000(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.3110 0.7990 '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
O1 As1 O1 93.8(3) 2_645
O1 As1 O2 100.3(3) 2_645
O2 As1 O1 92.5(4) .
O3 As2 O2 93.1(4) .
O3 As2 O2 97.4(4) 2
O3 As2 O3 93.07(14) 2
As1 O1 As1 128.4(7) 2_655
As1 O2 As2 122.4(6) .
As2 O3 As2 123.5(3) 2_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 O1 1.767(6) 2_645
As1 O1 1.793(14) .
As1 O2 1.769(4) .
As2 O2 1.798(11) .
As2 O3 1.791(5) .
As2 O3 1.770(4) 2
O1 As1 1.767(6) 2_655
O3 As2 1.770(4) 2_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 135.2(6) 2_645 2_655
O1 As1 O2 As2 -12.3(4) . .
O1 As1 O2 As2 82.0(6) 2_645 .
O2 As1 O1 As1 -124.3(5) . 2_655
O2 As2 O3 As2 88.8(6) . 2_545
O3 As2 O2 As1 -174.8(4) . .
O3 As2 O2 As1 91.7(4) 2 .
O3 As2 O3 As2 -173.6(9) 2 2_545
