#------------------------------------------------------------------------------
#$Date: 2015-09-05 22:32:59 +0200 (Sat 05 de Sep de 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513278.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_4513278
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                 102.014(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9853(4)
_cell_length_b                   4.55112(13)
_cell_length_c                   9.000(3)
_cell_measurement_pressure       3.7e5(5)
_cell_measurement_reflns_used    438
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.4690
_cell_measurement_theta_min      2.9340
_cell_volume                     319.91(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         3.7e5(5)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.452
_diffrn_measured_fraction_theta_max 0.272
_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      0.0094893000
_diffrn_orient_matrix_UB_12      -0.0081209000
_diffrn_orient_matrix_UB_13      0.0468819000
_diffrn_orient_matrix_UB_21      0.0317300000
_diffrn_orient_matrix_UB_22      -0.0710356000
_diffrn_orient_matrix_UB_23      -0.0024546000
_diffrn_orient_matrix_UB_31      0.0413983000
_diffrn_orient_matrix_UB_32      0.0562996000
_diffrn_orient_matrix_UB_33      0.0036641000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_laue_measured_fraction_full 0.452
_diffrn_reflns_laue_measured_fraction_max 0.272
_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            857
_diffrn_reflns_point_group_measured_fraction_full 0.452
_diffrn_reflns_point_group_measured_fraction_max 0.272
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.474
_diffrn_reflns_theta_min         2.937
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    4.746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77594
_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    4.107
_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         0.663
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.093(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0327
_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)+(0.0500P)²+0.6220P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0891
_reflns_Friedel_coverage         0.000
_reflns_number_gt                406
_reflns_number_total             440
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_002
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        319.93(11)
_cod_database_code               4513278
_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_002.res created by SHELXL-2014/7

TITL mclau2_002_a.res in P2(1)/n
REM Old TITL mclau2_002 in P21/n #14
REM SHELXT solution in P2(1)/n
REM R1 0.095, Rweak 0.006, Alpha 0.041, Orientation as input
REM Formula found by SHELXT: O3 As2
CELL 0.41427 7.985299 4.551121 9.000353 90 102.0135 90
ZERR 4 0.000404 0.000134 0.002897 0 0.0134 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 0 0
PLAN  20
BOND $H
LIST 6
MORE -1
CONF
fmap 2 53
acta
OMIT -6 4 5
OMIT -9 3 3
OMIT -9 3 3
OMIT -9 3 4
OMIT 3 7 3
OMIT -7 4 4
REM <olex2.extras>
REM <HklSrc "%./mclau2_002.hkl">
REM </olex2.extras>

WGHT    0.050000    0.622000
EXTI    0.092753
FVAR       0.89153
AS1   2    0.683186    0.212145    0.126133    11.00000    0.01572    0.01941 =
         0.01812    0.00208    0.00369   -0.00133
AS2   2    0.385025    0.173032    0.302820    11.00000    0.01687    0.01444 =
         0.02508    0.00071    0.00459    0.00177
O1    1    0.730381    0.366101    0.313886    11.00000    0.04048    0.03121 =
         0.01235   -0.00612    0.00579   -0.02013
O2    1    0.464688    0.150739    0.129971    11.00000    0.01113    0.04390 =
         0.03210   -0.01107    0.00466   -0.00257
O3    1    0.175148    0.049842    0.211750    11.00000    0.01659    0.01514 =
         0.04215    0.00029    0.00498   -0.00211
HKLF 4

REM  mclau2_002_a.res in P2(1)/n
REM R1 =  0.0327 for     406 Fo > 4sig(Fo)  and  0.0355 for all     440 data
REM     47 parameters refined using      0 restraints

END

WGHT      0.0500      0.6225

REM Highest difference peak  0.663,  deepest hole -0.576,  1-sigma level  0.179
Q1    1   0.5007  0.3396  0.3203  11.00000  0.05    0.66
Q2    1   0.2785  0.3071  0.3076  11.00000  0.05    0.62
Q3    1   0.8026  0.3017  0.1241  11.00000  0.05    0.60
Q4    1   0.7244  0.4989  0.3902  11.00000  0.05    0.55
Q5    1   0.8028  0.3379  0.3235  11.00000  0.05    0.54
Q6    1   0.2559  0.0648  0.3179  11.00000  0.05    0.52
Q7    1   0.2198  0.2449  0.0852  11.00000  0.05    0.50
Q8    1   0.5748  0.3547 -0.0421  11.00000  0.05    0.49
Q9    1   0.5861  0.3745  0.4192  11.00000  0.05    0.49
Q10   1   0.7285  0.1655  0.5158  11.00000  0.05    0.48
Q11   1   0.8057  0.1380  0.2448  11.00000  0.05    0.48
Q12   1   0.5525  0.1015  0.1123  11.00000  0.05    0.47
Q13   1   0.5017  0.2799  0.4538  11.00000  0.05    0.47
Q14   1   0.4782 -0.0336  0.3073  11.00000  0.05    0.46
Q15   1   0.3411  0.3424  0.4248  11.00000  0.05    0.44
Q16   1   0.5418  0.1740  0.2669  11.00000  0.05    0.44
Q17   1   0.4805 -0.2852  0.1147  11.00000  0.05    0.43
Q18   1   0.3548  0.0141  0.4466  11.00000  0.05    0.43
Q19   1   0.8452  0.2728  0.4124  11.00000  0.05    0.42
Q20   1   0.7049  0.4256 -0.0520  11.00000  0.05    0.42
;
_shelx_res_checksum              67512
_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 0.68319(7) 0.21214(12) 0.12613(17) 0.0177(7) Uani 1 1 d
As2 As 0.38503(7) 0.17303(12) 0.30282(16) 0.0188(7) Uani 1 1 d
O1 O 0.7304(8) 0.3661(11) 0.3139(16) 0.028(6) Uani 1 1 d
O2 O 0.4647(6) 0.1507(12) 0.1300(14) 0.029(5) Uani 1 1 d
O3 O 0.1751(5) 0.0498(8) 0.2118(12) 0.025(4) 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 0.0157(3) 0.0194(3) 0.018(2) 0.0021(3) 0.0037(5) -0.00133(17)
As2 0.0169(3) 0.0144(3) 0.025(2) 0.0007(3) 0.0046(6) 0.00177(17)
O1 0.040(2) 0.031(2) 0.012(19) -0.006(4) 0.006(5) -0.020(2)
O2 0.0111(14) 0.044(3) 0.032(17) -0.011(4) 0.005(4) -0.0026(18)
O3 0.0166(15) 0.0151(15) 0.042(14) 0.000(3) 0.005(3) -0.0021(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 93.9(3) 2_645
O1 As1 O2 100.2(3) 2_645
O2 As1 O1 93.3(4) .
O3 As2 O2 93.0(4) .
O3 As2 O2 97.4(4) 2
O3 As2 O3 93.17(15) 2
As1 O1 As1 129.1(6) 2_655
As1 O2 As2 122.2(6) .
As2 O3 As2 123.2(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 1.759(6) 2_645
As1 O1 1.795(13) .
As1 O2 1.774(4) .
As2 O2 1.802(11) .
As2 O3 1.795(5) .
As2 O3 1.778(4) 2
O1 As1 1.759(6) 2_655
O3 As2 1.778(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 136.4(6) 2_645 2_655
O1 As1 O2 As2 -13.1(4) . .
O1 As1 O2 As2 81.5(5) 2_645 .
O2 As1 O1 As1 -123.1(4) . 2_655
O2 As2 O3 As2 89.5(6) . 2_545
O3 As2 O2 As1 -174.4(3) . .
O3 As2 O2 As1 92.0(4) 2 .
O3 As2 O3 As2 -172.9(8) 2 2_545
