#------------------------------------------------------------------------------
#$Date: 2015-09-05 22:32:59 +0200 (Sat 05 de Sep de 2015) $
#$Revision: 154542 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/32/4513284.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_4513284
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                 143.209(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6524(7)
_cell_length_b                   4.40820(10)
_cell_length_c                   16.7237(14)
_cell_measurement_pressure       4.54e6(36)
_cell_measurement_reflns_used    757
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.9680
_cell_measurement_theta_min      2.8520
_cell_volume                     558.62(8)
_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         4.54e6(36)
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.458
_diffrn_measured_fraction_theta_max 0.269
_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      0.0309362000
_diffrn_orient_matrix_UB_12      0.0082600000
_diffrn_orient_matrix_UB_13      -0.0196867000
_diffrn_orient_matrix_UB_21      0.0147498000
_diffrn_orient_matrix_UB_22      0.0735642000
_diffrn_orient_matrix_UB_23      0.0175934000
_diffrn_orient_matrix_UB_31      0.0231485000
_diffrn_orient_matrix_UB_32      -0.0579677000
_diffrn_orient_matrix_UB_33      0.0194997000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41427
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_laue_measured_fraction_full 0.458
_diffrn_reflns_laue_measured_fraction_max 0.269
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1614
_diffrn_reflns_point_group_measured_fraction_full 0.458
_diffrn_reflns_point_group_measured_fraction_max 0.269
_diffrn_reflns_theta_full        14.392
_diffrn_reflns_theta_max         20.623
_diffrn_reflns_theta_min         2.297
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    5.436
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70663
_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    4.705
_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         2.371
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.337
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0524
_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)+(0.0890P)²+6.8710P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                671
_reflns_number_total             776
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5b00567_si_002.cif
_cod_data_source_block           mclau2_009_pl
_cod_depositor_comments
'Adding full bibliography for 4513277--4513300.cif.'
_cod_original_cell_volume        558.62(7)
_cod_database_code               4513284
_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_009_pl.res created by SHELXL-2014/7

TITL mclau_009_a.res in P2(1)/c
CELL 0.41427 12.6524 4.4082 16.7237 90 143.209 90
ZERR 4 0.0007 0.0001 0.0014 0 0.004 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 1
OMIT -6 7 4
OMIT 0 2 0
REM <olex2.extras>
REM <HklSrc "%./mclau_009_pl.hkl">
REM </olex2.extras>

WGHT    0.089000    6.871000
FVAR       0.39944
AS1   1    0.670669    0.275918    0.393779    11.00000    0.01311    0.01558 =
         0.02059    0.00191    0.01354   -0.00040
AS2   1    0.379557    0.198873    0.347892    11.00000    0.01467    0.01046 =
         0.01999    0.00186    0.01412    0.00241
AS3   1   -0.193663   -0.334552    0.096697    11.00000    0.01375    0.01213 =
         0.02056   -0.00038    0.01379    0.00036
AS4   1    0.100760   -0.303373    0.146730    11.00000    0.01200    0.00963 =
         0.01697   -0.00103    0.01095   -0.00086
O1    2    0.698075    0.454920    0.505874    11.00000    0.02102
O2    2    0.465080    0.134696    0.301490    11.00000    0.01555
O3    2    0.159972    0.089522    0.183940    11.00000    0.00998
O4    2   -0.264851   -0.222004   -0.044621    11.00000    0.02122
O5    2    0.034003   -0.325522    0.209659    11.00000    0.01873
O6    2    0.324969   -0.410450    0.306844    11.00000    0.01137
HKLF 4 1 0 0 -1 0 -1 0 -1 0 1

REM  mclau_009_a.res in P2(1)/c
REM R1 =  0.0524 for     671 Fo > 4sig(Fo)  and  0.0603 for all     776 data
REM     61 parameters refined using      0 restraints

END

WGHT      0.0884      6.9175

REM Highest difference peak  2.371,  deepest hole -1.304,  1-sigma level  0.337
Q1    1  -0.1821 -0.2052  0.0978  11.00000  0.05    2.37
Q2    1   0.8104  0.6306  0.6022  11.00000  0.05    1.49
Q3    1   0.7905  0.3067  0.3033  11.00000  0.05    1.24
Q4    1   0.9757  0.2938  0.6279  11.00000  0.05    1.15
Q5    1   0.5884  0.2513  0.3662  11.00000  0.05    1.13
Q6    1   0.1920 -0.0836  0.2112  11.00000  0.05    1.08
Q7    1  -0.0009 -0.5548  0.1694  11.00000  0.05    1.06
Q8    1   0.7188  0.6921  0.3108  11.00000  0.05    1.06
Q9    1   0.2795  0.3170  0.2194  11.00000  0.05    1.05
Q10   1  -0.1262 -0.1992 -0.0182  11.00000  0.05    1.03
Q11   1  -0.1885 -0.1348  0.0118  11.00000  0.05    0.97
Q12   1   0.2526 -0.2958  0.3070  11.00000  0.05    0.97
Q13   1   0.5397  0.1971  0.2696  11.00000  0.05    0.96
Q14   1   0.8896  0.2904  0.4576  11.00000  0.05    0.95
Q15   1   0.0307 -0.4922  0.1179  11.00000  0.05    0.89
Q16   1   0.2328 -0.0278  0.1447  11.00000  0.05    0.87
Q17   1  -0.0268 -0.6526  0.1081  11.00000  0.05    0.87
Q18   1   0.0470 -0.6637  0.0090  11.00000  0.05    0.87
Q19   1   1.0347  0.1862  0.6307  11.00000  0.05    0.86
Q20   1   1.0053  0.5374  0.5781  11.00000  0.05    0.86
;
_shelx_res_checksum              95659
_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 0.67067(14) 0.2759(2) 0.3938(2) 0.0164(10) Uani 1 1 d
As2 As 0.37956(15) 0.19887(19) 0.3479(2) 0.0147(11) Uani 1 1 d
As3 As -0.19366(14) -0.3346(2) 0.09670(19) 0.0154(11) Uani 1 1 d
As4 As 0.10076(14) -0.30337(19) 0.1467(2) 0.0138(10) Uani 1 1 d
O1 O 0.6981(11) 0.4549(17) 0.5059(16) 0.0210(16) Uiso 1 1 d
O2 O 0.4651(10) 0.1347(15) 0.3015(14) 0.0155(14) Uiso 1 1 d
O3 O 0.1600(9) 0.0895(13) 0.1839(13) 0.0100(12) Uiso 1 1 d
O4 O -0.2649(12) -0.2220(19) -0.0446(16) 0.0212(17) Uiso 1 1 d
O5 O 0.0340(11) -0.3255(16) 0.2097(16) 0.0187(16) Uiso 1 1 d
O6 O 0.3250(9) -0.4104(14) 0.3068(13) 0.0114(12) 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 0.0131(5) 0.0156(5) 0.021(2) 0.0019(5) 0.0135(8) -0.0004(3)
As2 0.0147(5) 0.0105(4) 0.020(2) 0.0019(4) 0.0141(8) 0.0024(3)
As3 0.0138(5) 0.0121(4) 0.021(2) -0.0004(4) 0.0138(8) 0.0004(3)
As4 0.0120(4) 0.0096(4) 0.017(2) -0.0010(4) 0.0109(7) -0.0009(3)
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 96.4(3) 2_646 .
O1 As1 O2 89.1(6) . .
O1 As1 O2 98.9(4) 2_646 .
O2 As2 O3 91.6(6) . .
O2 As2 O6 99.7(5) . 1_565
O6 As2 O3 91.3(4) 1_565 .
O4 As3 O4 88.9(5) . 2_445
O4 As3 O5 94.0(7) . .
O4 As3 O5 97.6(4) 2_445 .
O3 As4 O6 90.8(3) . .
O5 As4 O3 96.4(5) . .
O5 As4 O6 92.0(6) . .
As1 O1 As1 126.4(7) 2_656 .
As2 O2 As1 123.1(8) . .
As4 O3 As2 119.5(5) . .
As3 O4 As3 123.0(9) . 2_455
As3 O5 As4 119.9(10) . .
As2 O6 As4 119.2(4) 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 1.764(9) 2_646
As1 O1 1.793(18) .
As1 O2 1.762(7) .
As2 O2 1.788(14) .
As2 O3 1.808(10) .
As2 O6 1.776(6) 1_565
As3 O4 1.798(19) .
As3 O4 1.794(10) 2_445
As3 O5 1.775(7) .
As4 O3 1.789(6) .
As4 O5 1.804(17) .
As4 O6 1.809(9) .
O1 As1 1.764(9) 2_656
O4 As3 1.794(10) 2_455
O6 As2 1.776(6) 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 106.0(8) 2_646 2_656
O1 As1 O2 As2 94.5(8) 2_646 .
O1 As1 O2 As2 -1.8(7) . .
O2 As1 O1 As1 -155.2(7) . 2_656
O2 As2 O3 As4 84.2(8) . .
O3 As2 O2 As1 163.9(6) . .
O3 As4 O5 As3 103.9(5) . .
O3 As4 O6 As2 -178.6(10) . 1_545
O4 As3 O4 As3 168.9(7) 2_445 2_455
O4 As3 O5 As4 76.1(7) 2_445 .
O4 As3 O5 As4 -13.3(5) . .
O5 As3 O4 As3 -93.5(5) . 2_455
O5 As4 O3 As2 86.3(8) . .
O5 As4 O6 As2 85.0(9) . 1_545
O6 As2 O2 As1 72.3(7) 1_565 .
O6 As2 O3 As4 -176.0(10) 1_565 .
O6 As4 O3 As2 -5.8(8) . .
O6 As4 O5 As3 -165.0(4) . .
