#------------------------------------------------------------------------------
#$Date: 2015-09-05 23:32:59 +0300 (Sat, 05 Sep 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513277.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_4513277
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                 101.666(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0256(3)
_cell_length_b                   4.57553(11)
_cell_length_c                   9.142(2)
_cell_measurement_pressure       100(1)
_cell_measurement_reflns_used    428
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.7390
_cell_measurement_theta_min      2.9140
_cell_volume                     328.77(7)
_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         100(1)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.440
_diffrn_measured_fraction_theta_max 0.281
_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      0.0090868000
_diffrn_orient_matrix_UB_12      -0.0081923000
_diffrn_orient_matrix_UB_13      0.0460421000
_diffrn_orient_matrix_UB_21      0.0170640000
_diffrn_orient_matrix_UB_22      -0.0846576000
_diffrn_orient_matrix_UB_23      -0.0034748000
_diffrn_orient_matrix_UB_31      0.0490095000
_diffrn_orient_matrix_UB_32      0.0309903000
_diffrn_orient_matrix_UB_33      0.0027256000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41414
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_laue_measured_fraction_full 0.440
_diffrn_reflns_laue_measured_fraction_max 0.281
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            940
_diffrn_reflns_point_group_measured_fraction_full 0.440
_diffrn_reflns_point_group_measured_fraction_max 0.281
_diffrn_reflns_theta_full        14.388
_diffrn_reflns_theta_max         20.735
_diffrn_reflns_theta_min         2.913
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    4.615
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61751
_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    3.997
_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         0.975
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0392
_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)+(0.0570P)²+1.0130P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                439
_reflns_number_total             483
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_001
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        328.79(9)
_cod_database_code               4513277
_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_003.res created by SHELXL-2014/7

TITL mclau_003_a.res in P2(1)/n
REM Old TITL mclau_003 in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.119, Rweak 0.007, Alpha 0.038, Orientation as input
REM Formula found by SHELXT: O1 As2
CELL 0.41414 8.025555 4.575534 9.142484 90 101.666 90
ZERR 4 0.000298 0.000112 0.002459 0 0.0106 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.311 0.798 1881.6
DISP O 0.002 0.002 10.063
UNIT 12 8

L.S. 10
PLAN  20
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta
OMIT -4 5 5
OMIT 2 0 0
OMIT -6 1 2
OMIT -3 1 1
OMIT -10 2 5
REM <olex2.extras>
REM <HklSrc "%./mclau_003.hkl">
REM </olex2.extras>

WGHT    0.057000    1.013000
FVAR       4.13754
AS1   2    0.683629    0.208258    0.128444    11.00000    0.01447    0.01672 =
         0.02728    0.00231    0.00599   -0.00095
AS2   2    0.384239    0.167955    0.301632    11.00000    0.01600    0.01303 =
         0.03414    0.00107    0.00701    0.00194
O1    1    0.733992    0.358975    0.317462    11.00000    0.03095
O2    1    0.465967    0.151056    0.132842    11.00000    0.00953    0.04073 =
         0.02530   -0.00773    0.00634   -0.00049
O3    1    0.177997    0.041772    0.211919    11.00000    0.01728    0.01444 =
         0.05387    0.00467    0.00959   -0.00033
HKLF 4

REM  mclau_003_a.res in P2(1)/n
REM R1 =  0.0392 for     439 Fo > 4sig(Fo)  and  0.0432 for all     483 data
REM     41 parameters refined using      0 restraints

END

WGHT      0.0572      1.0298

REM Highest difference peak  0.975,  deepest hole -1.026,  1-sigma level  0.230
Q1    1   0.6935  0.4345  0.3202  11.00000  0.05    0.98
Q2    1   0.7769  0.3212  0.2842  11.00000  0.05    0.93
Q3    1   0.6816 -0.0102  0.1128  11.00000  0.05    0.79
Q4    1   0.8197  0.1800  0.4280  11.00000  0.05    0.73
Q5    1   0.3933 -0.0319  0.2941  11.00000  0.05    0.71
Q6    1   0.7974  0.4684  0.4394  11.00000  0.05    0.71
Q7    1   0.4262  0.0253  0.3849  11.00000  0.05    0.68
Q8    1   0.4875  0.3208  0.2705  11.00000  0.05    0.57
Q9    1   0.3472  0.2412  0.4307  11.00000  0.05    0.57
Q10   1   0.3021  0.2135  0.3807  11.00000  0.05    0.56
Q11   1   0.4749  0.3943  0.4688  11.00000  0.05    0.54
Q12   1   0.9014  0.3659  0.0636  11.00000  0.05    0.54
Q13   1   0.1165 -0.1190  0.2196  11.00000  0.05    0.53
Q14   1   0.0839  0.1366  0.2789  11.00000  0.05    0.53
Q15   1   0.1183  0.1681  0.2233  11.00000  0.05    0.52
Q16   1   0.5824  0.3857  0.3088  11.00000  0.05    0.50
Q17   1   0.2844  0.0612  0.2222  11.00000  0.05    0.49
Q18   1   0.5458  0.2505  0.1356  11.00000  0.05    0.48
Q19   1   0.2850  0.3127  0.0186  11.00000  0.05    0.47
Q20   1  -0.0449  0.1951  0.1456  11.00000  0.05    0.46
;
_shelx_res_checksum              76773
_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 0.68363(8) 0.20826(13) 0.12844(18) 0.0192(8) Uani 1 1 d
As2 As 0.38424(8) 0.16795(12) 0.30163(19) 0.0208(7) Uani 1 1 d
O1 O 0.7340(8) 0.3590(13) 0.3175(19) 0.0310(13) Uiso 1 1 d
O2 O 0.4660(6) 0.1511(12) 0.1328(15) 0.025(5) Uani 1 1 d
O3 O 0.1780(6) 0.0418(9) 0.2119(14) 0.028(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 0.0145(3) 0.0167(3) 0.027(2) 0.0023(4) 0.0060(6) -0.00095(17)
As2 0.0160(3) 0.0130(3) 0.034(2) 0.0011(4) 0.0070(6) 0.00194(16)
O2 0.0095(18) 0.041(3) 0.025(18) -0.008(4) 0.006(4) -0.0005(16)
O3 0.0173(19) 0.0144(18) 0.054(15) 0.005(3) 0.010(4) -0.0003(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 0.7980 '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 94.5(3) 2_645
O1 As1 O2 100.1(3) 2_645
O2 As1 O1 93.7(5) .
O3 As2 O2 93.3(4) .
O3 As2 O2 97.3(4) 2
O3 As2 O3 93.31(19) 2
As1 O1 As1 127.3(8) 2_655
As1 O2 As2 123.0(7) .
As2 O3 As2 124.3(4) 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 1.762(7) 2_645
As1 O1 1.828(16) .
As1 O2 1.775(4) .
As2 O2 1.796(12) .
As2 O3 1.788(7) .
As2 O3 1.779(4) 2
O1 As1 1.762(7) 2_655
O3 As2 1.779(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 139.0(5) 2_645 2_655
O1 As1 O2 As2 -13.3(5) . .
O1 As1 O2 As2 81.9(6) 2_645 .
O2 As1 O1 As1 -120.6(4) . 2_655
O2 As2 O3 As2 90.9(7) . 2_545
O3 As2 O2 As1 -172.7(4) . .
O3 As2 O2 As1 93.5(4) 2 .
O3 As2 O3 As2 -171.6(10) 2 2_545
