#------------------------------------------------------------------------------
#$Date: 2015-09-05 23:32:59 +0300 (Sat, 05 Sep 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513280.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_4513280
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                 102.548(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9216(2)
_cell_length_b                   4.50673(7)
_cell_length_c                   8.7646(14)
_cell_measurement_pressure       1.42e6(5)
_cell_measurement_reflns_used    417
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.6570
_cell_measurement_theta_min      2.9790
_cell_volume                     305.43(5)
_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         1.42e6(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.445
_diffrn_measured_fraction_theta_max 0.226
_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      -0.0101928000
_diffrn_orient_matrix_UB_12      -0.0080076000
_diffrn_orient_matrix_UB_13      -0.0482198000
_diffrn_orient_matrix_UB_21      -0.0320152000
_diffrn_orient_matrix_UB_22      -0.0717070000
_diffrn_orient_matrix_UB_23      0.0024978000
_diffrn_orient_matrix_UB_31      -0.0417339000
_diffrn_orient_matrix_UB_32      0.0569616000
_diffrn_orient_matrix_UB_33      -0.0036738000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_laue_measured_fraction_full 0.445
_diffrn_reflns_laue_measured_fraction_max 0.226
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            824
_diffrn_reflns_point_group_measured_fraction_full 0.445
_diffrn_reflns_point_group_measured_fraction_max 0.226
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         21.908
_diffrn_reflns_theta_min         2.978
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    4.971
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65241
_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    4.302
_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         1.023
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.223
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0431
_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)+(0.0720P)²+0.5860P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                389
_reflns_number_total             423
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_004
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        305.42(5)
_cod_database_code               4513280
_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_004.res created by SHELXL-2014/7

TITL mclau2_004_a.res in P2(1)/n
REM Old TITL mclau2_004 in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.061, Rweak 0.006, Alpha 0.059, Orientation as input
REM Formula found by SHELXT: O3 As2
CELL 0.41427 7.921564 4.506729 8.764561 90 102.5476 90
ZERR 4 0.000202 0.000067 0.001442 0 0.0071 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
REM <olex2.extras>
REM <HklSrc "%./mclau2_004.hkl">
REM </olex2.extras>

WGHT    0.072000    0.586000
FVAR       4.43517
AS1   2    0.681796    0.220682    0.122012    11.00000    0.01435    0.01958 =
         0.02353    0.00293    0.00513   -0.00240
AS2   2    0.386364    0.180320    0.305450    11.00000    0.01560    0.01202 =
         0.02478   -0.00001    0.00567    0.00146
O1    1    0.724265    0.373954    0.315660    11.00000    0.04270    0.03886 =
         0.02783   -0.00485    0.01039   -0.02239
O2    1    0.464202    0.150942    0.129416    11.00000    0.01058    0.04368 =
         0.04185   -0.00722    0.00571    0.00077
O3    1    0.173733    0.061981    0.209864    11.00000    0.01383
HKLF 4

REM  mclau2_004_a.res in P2(1)/n
REM R1 =  0.0431 for     389 Fo > 4sig(Fo)  and  0.0464 for all     423 data
REM     41 parameters refined using      0 restraints

END

WGHT      0.0719      0.5853

REM Highest difference peak  1.023,  deepest hole -1.109,  1-sigma level  0.282
Q1    1   0.4928  0.3682  0.3265  11.00000  0.05    1.02
Q2    1   0.7666  0.4759  0.2862  11.00000  0.05    0.97
Q3    1   0.2061 -0.1318  0.1879  11.00000  0.05    0.90
Q4    1   0.0343 -0.0642  0.0630  11.00000  0.05    0.83
Q5    1   0.7538  0.1921  0.4265  11.00000  0.05    0.80
Q6    1   0.8020  0.3701  0.1390  11.00000  0.05    0.80
Q7    1   0.4409 -0.0369  0.3623  11.00000  0.05    0.77
Q8    1   0.0060 -0.0361  0.0326  11.00000  0.05    0.76
Q9    1   0.2700  0.0233  0.2842  11.00000  0.05    0.75
Q10   1   0.4831  0.5254  0.0339  11.00000  0.05    0.70
Q11   1   0.5593  0.1641  0.1140  11.00000  0.05    0.69
Q12   1   0.5000  0.5000  0.0000  10.50000  0.05    0.69
Q13   1   0.0364  0.1933  0.2156  11.00000  0.05    0.69
Q14   1   0.7804  0.1178  0.3218  11.00000  0.05    0.67
Q15   1   0.7824  0.3293  0.2706  11.00000  0.05    0.67
Q16   1   0.1450  0.0928  0.2710  11.00000  0.05    0.63
Q17   1   0.7151  0.4294  0.5037  11.00000  0.05    0.63
Q18   1   0.3300  0.2289  0.0008  11.00000  0.05    0.62
Q19   1   0.6438  0.0095  0.0746  11.00000  0.05    0.62
Q20   1   0.4965  0.0891  0.4627  11.00000  0.05    0.58
;
_shelx_res_checksum              89425
_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 0.68180(10) 0.22068(16) 0.1220(2) 0.0190(9) Uani 1 1 d
As2 As 0.38636(10) 0.18032(14) 0.3055(2) 0.0173(9) Uani 1 1 d
O1 O 0.7243(10) 0.3740(16) 0.316(2) 0.036(8) Uani 1 1 d
O2 O 0.4642(8) 0.1509(15) 0.1294(18) 0.032(7) Uani 1 1 d
O3 O 0.1737(6) 0.0620(10) 0.2099(14) 0.0138(9) 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 0.0144(4) 0.0196(4) 0.024(3) 0.0029(4) 0.0051(7) -0.0024(2)
As2 0.0156(4) 0.0120(3) 0.025(3) 0.0000(3) 0.0057(7) 0.0015(2)
O1 0.043(4) 0.039(3) 0.03(3) -0.005(5) 0.010(8) -0.022(3)
O2 0.011(2) 0.044(3) 0.04(2) -0.007(5) 0.006(6) 0.001(2)
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 93.9(4) 2_645
O1 As1 O2 100.4(4) 2_645
O2 As1 O1 91.0(5) .
O2 As2 O3 92.3(4) .
O3 As2 O2 98.2(4) 2
O3 As2 O3 92.49(19) 2
As1 O1 As1 127.8(8) 2_655
As1 O2 As2 122.7(8) .
As2 O3 As2 122.1(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 1.766(8) 2_645
As1 O1 1.795(17) .
As1 O2 1.767(5) .
As2 O2 1.786(13) .
As2 O3 1.782(4) 2
As2 O3 1.792(7) .
O1 As1 1.766(8) 2_655
O3 As2 1.782(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 131.7(8) 2_645 2_655
O1 As1 O2 As2 -10.9(6) . .
O1 As1 O2 As2 83.2(7) 2_645 .
O2 As1 O1 As1 -127.8(6) . 2_655
O2 As2 O3 As2 88.6(6) . 2_545
O3 As2 O2 As1 -177.5(5) . .
O3 As2 O2 As1 89.6(5) 2 .
O3 As2 O3 As2 -173.1(9) 2 2_545
