# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_294k_02_0
_database_code_depnum_ccdc_archive 'CCDC 2031535'
loop_
_audit_author_name
_audit_author_address
'Piotr A. Gunka'
;Warsaw University of Technology, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_audit_creation_date             2020-05-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'claudetite I'
_chemical_name_systematic        ?
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'As2 O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   5.29402(16)
_cell_length_b                   12.8850(4)
_cell_length_c                   4.50656(13)
_cell_angle_alpha                90
_cell_angle_beta                 94.329(3)
_cell_angle_gamma                90
_cell_volume                     306.531(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5130
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.3850
_cell_measurement_theta_min      1.8290
_shelx_estimated_absorpt_T_max   0.958
_shelx_estimated_absorpt_T_min   0.519
_exptl_absorpt_coefficient_mu    21.580
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            8702
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.493
_diffrn_reflns_theta_min         1.838
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.37   0.50    0.30 154.30  15.00  73.80    --   720
  2  φ    -25.74 334.37   0.50    0.30 114.30  15.00  73.80    --   720
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0151618000
_diffrn_orient_matrix_UB_12      -0.0251200000
_diffrn_orient_matrix_UB_13      0.0457520000
_diffrn_orient_matrix_UB_21      -0.0414884000
_diffrn_orient_matrix_UB_22      0.0192407000
_diffrn_orient_matrix_UB_23      0.0488541000
_diffrn_orient_matrix_UB_31      -0.0807550000
_diffrn_orient_matrix_UB_32      -0.0051854000
_diffrn_orient_matrix_UB_33      -0.0405514000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                824
_reflns_number_total             980
_reflns_odcompleteness_completeness 98.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     14.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.491
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         980
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0309
_refine_ls_restrained_S_all      1.043
_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)+(0.0408P)²+0.1718P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0776
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.25850(8) 0.10135(3) 0.04083(9) 0.01376(13) Uani 1 1 d . . . . .
As2 As 0.35659(7) 0.35021(3) 0.00477(9) 0.01411(14) Uani 1 1 d . . . . .
O1 O 0.4315(6) 0.2174(2) 0.0697(8) 0.0203(6) Uani 1 1 d . . . . .
O2 O 0.6565(6) 0.3976(2) 0.1580(7) 0.0182(6) Uani 1 1 d . . . . .
O3 O -0.0451(6) 0.1413(3) 0.1372(7) 0.0197(6) 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 0.0135(2) 0.0171(2) 0.0106(2) 0.00054(13) 0.00028(15) 0.00205(14)
As2 0.0117(2) 0.0206(2) 0.0104(2) -0.00038(13) 0.00332(15) 0.00018(15)
O1 0.0163(13) 0.0195(14) 0.0249(17) 0.0004(12) 0.0004(12) -0.0023(12)
O2 0.0174(14) 0.0272(16) 0.0101(14) 0.0006(10) 0.0012(11) -0.0053(12)
O3 0.0152(14) 0.0349(17) 0.0092(14) 0.0002(11) 0.0020(11) 0.0028(13)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.754(3) . ?
As1 O2 1.768(3) 4_565 ?
As1 O3 1.772(3) . ?
As2 O1 1.776(3) . ?
As2 O2 1.790(3) . ?
As2 O3 1.777(3) 4_665 ?

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
_geom_angle_publ_flag
O1 As1 O2 100.67(15) . 4_565 ?
O1 As1 O3 102.26(14) . . ?
O2 As1 O3 91.20(14) 4_565 . ?
O1 As2 O2 94.85(14) . . ?
O1 As2 O3 97.77(15) . 4_665 ?
O3 As2 O2 91.43(14) 4_665 . ?
As1 O1 As2 134.48(18) . . ?
As1 O2 As2 125.14(17) 4_666 . ?
As1 O3 As2 125.53(18) . 4_566 ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O3 As2 -85.9(2) . . . 4_566 ?
O1 As2 O2 As1 -72.1(2) . . . 4_666 ?
O2 As1 O1 As2 60.5(3) 4_565 . . . ?
O2 As1 O3 As2 172.9(2) 4_565 . . 4_566 ?
O2 As2 O1 As1 171.6(3) . . . . ?
O3 As1 O1 As2 -33.1(3) . . . . ?
O3 As2 O1 As1 -96.2(3) 4_665 . . . ?
O3 As2 O2 As1 -170.1(2) 4_665 . . 4_666 ?

_shelx_res_file                  
;
TITL 294K_02_0 in P21/n #14
    294k_02_0.res
    created by SHELXL-2018/3 at 16:35:02 on 18-May-2020
REM reset to P21/n #14
CELL 0.41328 5.294017 12.885006 4.506555 90 94.3289 90
ZERR 4 0.000155 0.000405 0.000129 0 0.0028 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC As O
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 8 12

L.S. 10
PLAN  5
SIZE 0.035 0.018 0.002
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\294K_02_0.hkl">
REM </olex2.extras>

WGHT    0.040800    0.171800
FVAR       6.63920
AS1   1    0.258496    0.101346    0.040832    11.00000    0.01350    0.01712 =
         0.01057    0.00054    0.00028    0.00205
AS2   1    0.356589    0.350214    0.004766    11.00000    0.01172    0.02059 =
         0.01042   -0.00038    0.00332    0.00018
O1    2    0.431544    0.217436    0.069652    11.00000    0.01631    0.01952 =
         0.02486    0.00041    0.00039   -0.00230
O2    2    0.656455    0.397612    0.158018    11.00000    0.01736    0.02716 =
         0.01008    0.00061    0.00118   -0.00532
O3    2   -0.045053    0.141308    0.137187    11.00000    0.01517    0.03489 =
         0.00922    0.00015    0.00203    0.00278
HKLF 4




REM  294K_02_0 in P21/n #14
REM wR2 = 0.0776, GooF = S = 1.043, Restrained GooF = 1.043 for all data
REM R1 = 0.0309 for 824 Fo > 4sig(Fo) and 0.0378 for all 980 data
REM 46 parameters refined using 0 restraints

END

WGHT      0.0408      0.1718

REM Highest difference peak  1.491,  deepest hole -0.865,  1-sigma level  0.260
Q1    1   0.3660  0.2808  0.0159  11.00000  0.05    1.49
Q2    1   0.2852  0.1647  0.0269  11.00000  0.05    1.38
Q3    1   0.2373  0.0378  0.0282  11.00000  0.05    1.29
Q4    1   0.3591  0.4194  0.0150  11.00000  0.05    1.15
Q5    1  -0.2103  0.1995  0.1668  11.00000  0.05    0.90
;
_shelx_res_checksum              1377
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.183
_oxdiff_exptl_absorpt_empirical_full_min 0.842
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_clau1_5_100
_database_code_depnum_ccdc_archive 'CCDC 2031541'
loop_
_audit_author_name
_audit_author_address
'Piotr A. Gunka'
;Warsaw University of Technology, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_audit_creation_date             2020-05-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'claudetite I'
_chemical_name_systematic        ?
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'As2 O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   5.27066(19)
_cell_length_b                   12.7806(5)
_cell_length_c                   4.48685(19)
_cell_angle_alpha                90
_cell_angle_beta                 94.579(4)
_cell_angle_gamma                90
_cell_volume                     301.28(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7960
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      26.7830
_cell_measurement_theta_min      1.8430
_shelx_estimated_absorpt_T_max   0.957
_shelx_estimated_absorpt_T_min   0.514
_exptl_absorpt_coefficient_mu    21.956
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            11248
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.454
_diffrn_reflns_theta_min         1.853
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.26   0.50    0.30 154.30  15.00  73.80    --   720
  2  φ    -25.74 334.26   0.50    0.30 114.30  15.00  73.80    --   720
  3  φ    -25.74 334.26   0.50    0.30  74.30  15.00  73.80    --   720
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0427114746
_diffrn_orient_matrix_UB_12      0.0264643934
_diffrn_orient_matrix_UB_13      -0.0130027574
_diffrn_orient_matrix_UB_21      0.0516043950
_diffrn_orient_matrix_UB_22      -0.0178349974
_diffrn_orient_matrix_UB_23      -0.0424964389
_diffrn_orient_matrix_UB_31      -0.0412100647
_diffrn_orient_matrix_UB_32      0.0051177351
_diffrn_orient_matrix_UB_33      -0.0811010011
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                847
_reflns_number_total             965
_reflns_odcompleteness_completeness 85.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.86
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.174
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.312
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         965
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.044
_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)+(0.0513P)²+0.0168P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0803
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.25928(7) 0.10027(3) 0.04245(8) 0.00564(13) Uani 1 1 d . . . . .
As2 As 0.35540(7) 0.35088(3) 0.00388(8) 0.00569(13) Uani 1 1 d . . . . .
O1 O 0.4326(5) 0.2175(2) 0.0711(6) 0.0091(5) Uani 1 1 d . . . . .
O2 O 0.6567(5) 0.3993(2) 0.1563(6) 0.0081(5) Uani 1 1 d . . . . .
O3 O -0.0461(6) 0.1410(2) 0.1348(6) 0.0097(5) Uani 1 1 d . U . . .

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 0.0044(2) 0.0089(2) 0.0037(2) 0.00012(11) 0.00157(14) 0.00074(12)
As2 0.0038(2) 0.0099(2) 0.0037(2) -0.00009(11) 0.00274(14) 0.00010(12)
O1 0.0068(10) 0.0110(12) 0.0094(13) 0.0005(10) 0.0001(10) -0.0010(10)
O2 0.0067(12) 0.0144(12) 0.0036(13) 0.0001(9) 0.0026(10) -0.0023(10)
O3 0.0085(12) 0.0180(13) 0.0028(12) 0.0002(9) 0.0019(10) 0.0023(10)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.754(3) . ?
As1 O2 1.773(3) 4_565 ?
As1 O3 1.772(3) . ?
As2 O1 1.773(3) . ?
As2 O2 1.789(3) . ?
As2 O3 1.778(3) 4_665 ?

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
_geom_angle_publ_flag
O1 As1 O2 100.68(13) . 4_565 ?
O1 As1 O3 102.08(12) . . ?
O3 As1 O2 90.91(13) . 4_565 ?
O1 As2 O2 94.76(12) . . ?
O1 As2 O3 97.72(13) . 4_665 ?
O3 As2 O2 91.12(13) 4_665 . ?
As1 O1 As2 134.25(16) . . ?
As1 O2 As2 124.52(15) 4_666 . ?
As1 O3 As2 124.98(17) . 4_566 ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O3 As2 -86.5(2) . . . 4_566 ?
O1 As2 O2 As1 -71.67(19) . . . 4_666 ?
O2 As1 O1 As2 60.5(2) 4_565 . . . ?
O2 As1 O3 As2 172.4(2) 4_565 . . 4_566 ?
O2 As2 O1 As1 172.0(2) . . . . ?
O3 As1 O1 As2 -32.7(3) . . . . ?
O3 As2 O1 As1 -96.2(2) 4_665 . . . ?
O3 As2 O2 As1 -169.51(19) 4_665 . . 4_666 ?

_shelx_res_file                  
;
TITL clau1_5_100 in P21/n #14
    clau1_5_100.res
    created by SHELXL-2018/3 at 13:35:43 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.270664 12.780567 4.486851 90 94.5792 90
ZERR 4 0.000193 0.000473 0.000193 0 0.0037 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 12 8
ISOR 0.005 0.01 O3

L.S. 10 0 0
PLAN  5
SIZE 0.002 0.018 0.035
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_5_100.hkl">
REM </olex2.extras>

WGHT    0.051300    0.016800
FVAR       5.15739
AS1   2    0.259279    0.100267    0.042445    11.00000    0.00443    0.00895 =
         0.00374    0.00012    0.00157    0.00074
AS2   2    0.355397    0.350884    0.003884    11.00000    0.00380    0.00995 =
         0.00371   -0.00009    0.00274    0.00010
O1    1    0.432597    0.217517    0.071053    11.00000    0.00682    0.01096 =
         0.00936    0.00051    0.00013   -0.00104
O2    1    0.656710    0.399322    0.156298    11.00000    0.00673    0.01444 =
         0.00362    0.00008    0.00265   -0.00235
O3    1   -0.046095    0.141009    0.134815    11.00000    0.00849    0.01802 =
         0.00277    0.00016    0.00190    0.00228
HKLF 4




REM  clau1_5_100 in P21/n #14
REM wR2 = 0.0803, GooF = S = 1.045, Restrained GooF = 1.044 for all data
REM R1 = 0.0311 for 847 Fo > 4sig(Fo) and 0.0353 for all 965 data
REM 46 parameters refined using 6 restraints

END

WGHT      0.0510      0.0169

REM Highest difference peak  2.174,  deepest hole -1.208,  1-sigma level  0.312
Q1    1   0.2685  0.1642  0.0344  11.00000  0.05    2.17
Q2    1   0.2585  0.0372  0.0426  11.00000  0.05    2.15
Q3    1   0.3531  0.2856  0.0062  11.00000  0.05    2.04
Q4    1   0.3494  0.4127  0.0085  11.00000  0.05    1.94
Q5    1   0.6648  0.3986  0.3536  11.00000  0.05    0.97
;
_shelx_res_checksum              82459
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.136
_oxdiff_exptl_absorpt_empirical_full_min 0.589
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_clau1_1_35
_database_code_depnum_ccdc_archive 'CCDC 2031543'
loop_
_audit_author_name
_audit_author_address
'Piotr A. Gunka'
;Warsaw University of Technology, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_audit_creation_date             2020-05-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'claudetite I'
_chemical_name_systematic        ?
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'As2 O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   5.26373(14)
_cell_length_b                   12.7447(3)
_cell_length_c                   4.47691(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.687(3)
_cell_angle_gamma                90
_cell_volume                     299.328(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6413
_cell_measurement_temperature    35(1)
_cell_measurement_theta_max      31.1680
_cell_measurement_theta_min      1.8400
_shelx_estimated_absorpt_T_max   0.957
_shelx_estimated_absorpt_T_min   0.472
_exptl_absorpt_coefficient_mu    22.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.390
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.825
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3930
_diffrn_reflns_point_group_measured_fraction_full 0.825
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.489
_diffrn_reflns_theta_min         1.858
_diffrn_ambient_temperature      35(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.825
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.26   0.50    0.30 154.30  25.00  73.80    --   720
  2  φ    -25.74 154.26   0.50    0.30 114.30  25.00  73.80    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0431872129
_diffrn_orient_matrix_UB_12      -0.0166621635
_diffrn_orient_matrix_UB_13      0.0566526051
_diffrn_orient_matrix_UB_21      0.0296615122
_diffrn_orient_matrix_UB_22      -0.0277251146
_diffrn_orient_matrix_UB_23      -0.0298632465
_diffrn_orient_matrix_UB_31      0.0588658555
_diffrn_orient_matrix_UB_32      0.0017244601
_diffrn_orient_matrix_UB_33      0.0670359258
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                802
_reflns_number_total             863
_reflns_odcompleteness_completeness 81.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.23
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.642
_refine_diff_density_min         -1.947
_refine_diff_density_rms         0.309
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         863
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0343
_refine_ls_restrained_S_all      1.139
_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)+(0.0709P)²+0.2933P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0948
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.0005 and sigma for
terminal atoms of 0.001
Uanis(As2) \\sim Ueq: with sigma of 0.0002 and sigma for terminal atoms of
0.0004
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.25899(5) 0.10014(2) 0.04256(7) 0.00299(16) Uani 1 1 d . . . . .
As2 As 0.35506(5) 0.35099(2) 0.00339(7) 0.00269(16) Uani 1 1 d . U . . .
O1 O 0.4331(4) 0.21731(17) 0.0718(5) 0.0062(4) Uani 1 1 d . . . . .
O2 O 0.6574(5) 0.39916(16) 0.1564(6) 0.0045(4) Uani 1 1 d . U . . .
O3 O -0.0473(4) 0.14093(17) 0.1352(6) 0.0056(4) Uani 1 1 d . U . . .

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 0.0030(2) 0.0045(2) 0.0016(2) -0.00017(8) 0.00080(13) 0.00034(8)
As2 0.0026(2) 0.0041(2) 0.0015(2) 0.00013(8) 0.00130(12) 0.00009(8)
O1 0.0055(8) 0.0058(9) 0.0073(9) 0.0012(8) 0.0009(7) -0.0010(8)
O2 0.0042(6) 0.0054(6) 0.0039(6) 0.0002(4) 0.0003(4) -0.0007(4)
O3 0.0051(6) 0.0068(6) 0.0050(6) -0.0002(4) 0.0014(4) 0.0003(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.751(2) . ?
As1 O2 1.767(3) 4_565 ?
As1 O3 1.775(2) . ?
As2 O1 1.773(2) . ?
As2 O2 1.789(2) . ?
As2 O3 1.769(2) 4_665 ?

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
_geom_angle_publ_flag
O1 As1 O2 100.58(10) . 4_565 ?
O1 As1 O3 102.27(10) . . ?
O2 As1 O3 91.09(11) 4_565 . ?
O1 As2 O2 94.44(10) . . ?
O3 As2 O1 97.82(10) 4_665 . ?
O3 As2 O2 91.13(11) 4_665 . ?
As1 O1 As2 133.94(13) . . ?
As1 O2 As2 124.39(13) 4_666 . ?
As2 O3 As1 124.98(14) 4_566 . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O3 As2 -86.34(16) . . . 4_566 ?
O1 As2 O2 As1 -71.93(15) . . . 4_666 ?
O2 As1 O1 As2 60.50(19) 4_565 . . . ?
O2 As1 O3 As2 172.59(15) 4_565 . . 4_566 ?
O2 As2 O1 As1 172.17(18) . . . . ?
O3 As1 O1 As2 -33.0(2) . . . . ?
O3 As2 O1 As1 -96.07(18) 4_665 . . . ?
O3 As2 O2 As1 -169.87(14) 4_665 . . 4_666 ?

_shelx_res_file                  
;
TITL clau1_1_35 in P21/n #14
    clau1_1_35.res
    created by SHELXL-2018/3 at 13:51:53 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.263732 12.744724 4.476907 90 94.6873 90
ZERR 4 0.00014 0.000285 0.000114 0 0.0027 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 12 8
ISOR 0.0005 0.001 O3 O2
ISOR 0.0002 0.0004 As2

L.S. 10 0 0
PLAN  5
SIZE 0.002 0.02 0.04
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_1_35.hkl">
REM </olex2.extras>

WGHT    0.070900    0.293300
FVAR       9.42813
AS1   2    0.258989    0.100145    0.042562    11.00000    0.00303    0.00445 =
         0.00158   -0.00017    0.00080    0.00034
AS2   2    0.355059    0.350991    0.003392    11.00000    0.00262    0.00411 =
         0.00154    0.00013    0.00130    0.00009
O1    1    0.433063    0.217305    0.071842    11.00000    0.00549    0.00582 =
         0.00725    0.00118    0.00086   -0.00102
O2    1    0.657382    0.399155    0.156391    11.00000    0.00423    0.00542 =
         0.00394    0.00016    0.00034   -0.00073
O3    1   -0.047309    0.140931    0.135193    11.00000    0.00514    0.00682 =
         0.00496   -0.00024    0.00136    0.00026
HKLF 4




REM  clau1_1_35 in P21/n #14
REM wR2 = 0.0948, GooF = S = 1.072, Restrained GooF = 1.139 for all data
REM R1 = 0.0343 for 802 Fo > 4sig(Fo) and 0.0364 for all 863 data
REM 46 parameters refined using 18 restraints

END

WGHT      0.0707      0.3063

REM Highest difference peak  1.642,  deepest hole -1.947,  1-sigma level  0.309
Q1    1   0.3658  0.3184  0.0134  11.00000  0.05    1.64
Q2    1   0.3210  0.3848 -0.0277  11.00000  0.05    1.53
Q3    1   0.2867  0.1357  0.0537  11.00000  0.05    1.17
Q4    1   0.6212  0.3937  0.3590  11.00000  0.05    1.08
Q5    1   0.6476  0.3590  0.0452  11.00000  0.05    1.02
;
_shelx_res_checksum              46081
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.817
_oxdiff_exptl_absorpt_empirical_full_min 0.450
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_clau1_5_230
_database_code_depnum_ccdc_archive 'CCDC 2031537'
loop_
_audit_author_name
_audit_author_address
'Piotr A. Gunka'
;Warsaw University of Technology, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_audit_creation_date             2020-05-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'claudetite I'
_chemical_name_systematic        ?
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'As2 O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   5.29025(13)
_cell_length_b                   12.8566(3)
_cell_length_c                   4.50200(12)
_cell_angle_alpha                90
_cell_angle_beta                 94.440(3)
_cell_angle_gamma                90
_cell_volume                     305.283(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5868
_cell_measurement_temperature    230(1)
_cell_measurement_theta_max      25.9370
_cell_measurement_theta_min      1.8330
_shelx_estimated_absorpt_T_max   0.696
_shelx_estimated_absorpt_T_min   0.518
_exptl_absorpt_coefficient_mu    21.668
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.304
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.018
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            8875
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.497
_diffrn_reflns_theta_min         1.842
_diffrn_ambient_temperature      230(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.26   0.50    0.30 154.30  15.00  73.80    --   720
  2  φ    -25.74 334.26   0.50    0.30 114.30  15.00  73.80    --   720
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0448376816
_diffrn_orient_matrix_UB_12      0.0255223103
_diffrn_orient_matrix_UB_13      -0.0145644640
_diffrn_orient_matrix_UB_21      0.0496885874
_diffrn_orient_matrix_UB_22      -0.0188369652
_diffrn_orient_matrix_UB_23      -0.0416636531
_diffrn_orient_matrix_UB_31      -0.0407288103
_diffrn_orient_matrix_UB_32      0.0051338469
_diffrn_orient_matrix_UB_33      -0.0808720642
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                848
_reflns_number_total             976
_reflns_odcompleteness_completeness 84.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.90
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.556
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.255
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         976
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0294
_refine_ls_restrained_S_all      1.045
_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)+(0.0407P)²+0.0604P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0723
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.25871(7) 0.10101(3) 0.04161(8) 0.01092(12) Uani 1 1 d . . . . .
As2 As 0.35616(7) 0.35041(3) 0.00453(8) 0.01114(13) Uani 1 1 d . . . . .
O1 O 0.4317(5) 0.2176(2) 0.0706(7) 0.0162(5) Uani 1 1 d . . . . .
O2 O 0.6566(6) 0.3983(2) 0.1575(6) 0.0153(5) Uani 1 1 d . . . . .
O3 O -0.0451(5) 0.1412(2) 0.1380(6) 0.0159(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 0.01073(19) 0.0138(2) 0.0082(2) 0.00034(12) 0.00080(14) 0.00160(12)
As2 0.00903(19) 0.0165(2) 0.0082(2) -0.00026(12) 0.00292(14) 0.00026(13)
O1 0.0124(11) 0.0159(12) 0.0200(14) 0.0021(10) -0.0004(11) -0.0010(10)
O2 0.0151(13) 0.0239(14) 0.0070(12) 0.0018(9) 0.0016(10) -0.0052(11)
O3 0.0130(12) 0.0281(14) 0.0065(12) -0.0001(10) 0.0010(10) 0.0035(11)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.756(3) . ?
As1 O2 1.771(3) 4_565 ?
As1 O3 1.774(3) . ?
As2 O1 1.773(3) . ?
As2 O2 1.792(3) . ?
As2 O3 1.772(3) 4_665 ?

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
_geom_angle_publ_flag
O1 As1 O2 100.71(13) . 4_565 ?
O1 As1 O3 102.11(13) . . ?
O2 As1 O3 91.37(13) 4_565 . ?
O1 As2 O2 94.85(13) . . ?
O3 As2 O1 97.81(13) 4_665 . ?
O3 As2 O2 91.15(12) 4_665 . ?
As1 O1 As2 134.44(16) . . ?
As1 O2 As2 124.83(15) 4_666 . ?
As2 O3 As1 125.71(16) 4_566 . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O3 As2 -86.1(2) . . . 4_566 ?
O1 As2 O2 As1 -71.84(19) . . . 4_666 ?
O2 As1 O1 As2 60.4(3) 4_565 . . . ?
O2 As1 O3 As2 172.6(2) 4_565 . . 4_566 ?
O2 As2 O1 As1 171.9(2) . . . . ?
O3 As1 O1 As2 -33.4(3) . . . . ?
O3 As2 O1 As1 -96.3(2) 4_665 . . . ?
O3 As2 O2 As1 -169.78(19) 4_665 . . 4_666 ?

_shelx_res_file                  
;
TITL clau1_5_230 in P21/n #14
    clau1_5_230.res
    created by SHELXL-2018/3 at 12:53:04 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.290251 12.856586 4.502005 90 94.4397 90
ZERR 4 0.000135 0.000336 0.000119 0 0.0025 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 12 8

L.S. 10 0 0
PLAN  5
SIZE 0.02 0.018 0.035
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_5_230.hkl">
REM </olex2.extras>

WGHT    0.040700    0.060400
FVAR       6.55736
AS1   2    0.258708    0.101011    0.041607    11.00000    0.01073    0.01379 =
         0.00824    0.00034    0.00080    0.00160
AS2   2    0.356161    0.350407    0.004529    11.00000    0.00903    0.01652 =
         0.00823   -0.00026    0.00292    0.00026
O1    1    0.431695    0.217647    0.070610    11.00000    0.01243    0.01594 =
         0.02005    0.00207   -0.00040   -0.00101
O2    1    0.656646    0.398281    0.157458    11.00000    0.01512    0.02391 =
         0.00695    0.00183    0.00163   -0.00522
O3    1   -0.045052    0.141209    0.138037    11.00000    0.01302    0.02807 =
         0.00650   -0.00007    0.00101    0.00354
HKLF 4




REM  clau1_5_230 in P21/n #14
REM wR2 = 0.0723, GooF = S = 1.045, Restrained GooF = 1.045 for all data
REM R1 = 0.0294 for 848 Fo > 4sig(Fo) and 0.0347 for all 976 data
REM 46 parameters refined using 0 restraints

END

WGHT      0.0407      0.0604

REM Highest difference peak  1.556,  deepest hole -0.927,  1-sigma level  0.255
Q1    1   0.2704  0.1715  0.0400  11.00000  0.05    1.56
Q2    1   0.3804  0.2807  0.0193  11.00000  0.05    1.52
Q3    1   0.2588  0.0380  0.0402  11.00000  0.05    1.44
Q4    1   0.3640  0.4184  0.0071  11.00000  0.05    1.28
Q5    1   0.4848  0.3577  0.1125  11.00000  0.05    0.89
;
_shelx_res_checksum              27835
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.158
_oxdiff_exptl_absorpt_empirical_full_min 0.853
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_clau1_5_150
_database_code_depnum_ccdc_archive 'CCDC 2031539'
loop_
_audit_author_name
_audit_author_address
'Piotr A. Gunka'
;Warsaw University of Technology, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_audit_creation_date             2020-05-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'claudetite I'
_chemical_name_systematic        ?
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'As2 O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   5.28841(13)
_cell_length_b                   12.8335(3)
_cell_length_c                   4.50014(13)
_cell_angle_alpha                90
_cell_angle_beta                 94.541(3)
_cell_angle_gamma                90
_cell_volume                     304.460(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6391
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      26.7350
_cell_measurement_theta_min      1.8390
_shelx_estimated_absorpt_T_max   0.958
_shelx_estimated_absorpt_T_min   0.517
_exptl_absorpt_coefficient_mu    21.727
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.316
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            9732
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.498
_diffrn_reflns_theta_min         1.845
_diffrn_ambient_temperature      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.26   0.50    0.30 154.30  15.00  73.80    --   720
  2  φ    -25.74 255.26   0.50    0.30 114.30  15.00  73.80    --   562
  3  φ    -25.74 154.26   0.50    0.30 114.30  15.00  73.80    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0434705468
_diffrn_orient_matrix_UB_12      0.0260554915
_diffrn_orient_matrix_UB_13      -0.0135120876
_diffrn_orient_matrix_UB_21      0.0507262023
_diffrn_orient_matrix_UB_22      -0.0181794489
_diffrn_orient_matrix_UB_23      -0.0422576767
_diffrn_orient_matrix_UB_31      -0.0409893327
_diffrn_orient_matrix_UB_32      0.0051722219
_diffrn_orient_matrix_UB_33      -0.0808213541
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                836
_reflns_number_total             973
_reflns_odcompleteness_completeness 83.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.88
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.897
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.311
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         973
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0314
_refine_ls_restrained_S_all      1.071
_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)+(0.0484P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0821
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.25895(7) 0.10059(3) 0.04212(9) 0.00770(14) Uani 1 1 d . . . . .
As2 As 0.35561(7) 0.35065(3) 0.00422(9) 0.00775(14) Uani 1 1 d . . . . .
O1 O 0.4321(5) 0.2177(2) 0.0703(7) 0.0119(6) Uani 1 1 d . . . . .
O2 O 0.6566(6) 0.3989(2) 0.1576(7) 0.0101(6) Uani 1 1 d . U . . .
O3 O -0.0458(6) 0.1410(2) 0.1358(7) 0.0114(6) 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 0.0069(2) 0.0111(2) 0.0052(2) 0.00009(13) 0.00124(15) 0.00128(13)
As2 0.0058(2) 0.0129(2) 0.0049(2) -0.00015(13) 0.00273(15) 0.00014(14)
O1 0.0087(11) 0.0124(13) 0.0145(16) 0.0006(11) 0.0003(11) -0.0012(11)
O2 0.0103(9) 0.0128(9) 0.0074(9) 0.0012(7) 0.0015(8) -0.0018(7)
O3 0.0075(12) 0.0233(15) 0.0036(14) 0.0010(10) 0.0013(11) 0.0022(11)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.759(3) . ?
As1 O2 1.772(3) 4_565 ?
As1 O3 1.775(3) . ?
As2 O1 1.773(3) . ?
As2 O2 1.794(3) . ?
As2 O3 1.780(3) 4_665 ?

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
_geom_angle_publ_flag
O1 As1 O2 100.61(14) . 4_565 ?
O1 As1 O3 102.12(14) . . ?
O2 As1 O3 91.04(14) 4_565 . ?
O1 As2 O2 94.80(13) . . ?
O1 As2 O3 97.72(15) . 4_665 ?
O3 As2 O2 91.21(14) 4_665 . ?
As1 O1 As2 134.39(17) . . ?
As1 O2 As2 124.76(17) 4_666 . ?
As1 O3 As2 125.26(18) . 4_566 ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O3 As2 -86.4(2) . . . 4_566 ?
O1 As2 O2 As1 -71.8(2) . . . 4_666 ?
O2 As1 O1 As2 60.6(3) 4_565 . . . ?
O2 As1 O3 As2 172.5(2) 4_565 . . 4_566 ?
O2 As2 O1 As1 171.7(3) . . . . ?
O3 As1 O1 As2 -32.8(3) . . . . ?
O3 As2 O1 As1 -96.4(3) 4_665 . . . ?
O3 As2 O2 As1 -169.6(2) 4_665 . . 4_666 ?

_shelx_res_file                  
;
TITL clau1_5_150 in P21/n #14
    clau1_5_150.res
    created by SHELXL-2018/3 at 13:21:29 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.288408 12.833474 4.50014 90 94.5406 90
ZERR 4 0.000127 0.000346 0.000133 0 0.0026 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC As O
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 8 12
ISOR 0.001 0.001 O2

L.S. 9 0 0
PLAN  5
SIZE 0.002 0.018 0.035
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_5_150.hkl">
REM </olex2.extras>

WGHT    0.048400
FVAR       6.32848
AS1   1    0.258955    0.100589    0.042118    11.00000    0.00695    0.01111 =
         0.00516    0.00009    0.00124    0.00128
AS2   1    0.355607    0.350651    0.004217    11.00000    0.00582    0.01293 =
         0.00488   -0.00015    0.00273    0.00014
O1    2    0.432065    0.217706    0.070345    11.00000    0.00868    0.01244 =
         0.01447    0.00062    0.00031   -0.00123
O2    2    0.656638    0.398859    0.157608    11.00000    0.01025    0.01281 =
         0.00738    0.00122    0.00150   -0.00175
O3    2   -0.045756    0.141031    0.135849    11.00000    0.00750    0.02328 =
         0.00358    0.00103    0.00126    0.00222
HKLF 4




REM  clau1_5_150 in P21/n #14
REM wR2 = 0.0821, GooF = S = 1.063, Restrained GooF = 1.071 for all data
REM R1 = 0.0314 for 836 Fo > 4sig(Fo) and 0.0377 for all 973 data
REM 46 parameters refined using 6 restraints

END

WGHT      0.0484      0.0000

REM Highest difference peak  1.897,  deepest hole -1.199,  1-sigma level  0.311
Q1    1   0.2836  0.1625  0.0212  11.00000  0.05    1.90
Q2    1   0.3473  0.2864  0.0200  11.00000  0.05    1.66
Q3    1   0.2724  0.0388  0.0229  11.00000  0.05    1.55
Q4    1   0.1818  0.1009 -0.1403  11.00000  0.05    1.31
Q5    1   0.3746  0.4154  0.0105  11.00000  0.05    1.29
;
_shelx_res_checksum              58562
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.123
_oxdiff_exptl_absorpt_empirical_full_min 0.867
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_clau1_1_50
_database_code_depnum_ccdc_archive 'CCDC 2031542'
loop_
_audit_author_name
_audit_author_address
'Piotr A. Gunka'
;Warsaw University of Technology, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_audit_creation_date             2020-05-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'claudetite I'
_chemical_name_systematic        ?
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'As2 O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   5.26753(12)
_cell_length_b                   12.7667(2)
_cell_length_c                   4.48007(10)
_cell_angle_alpha                90
_cell_angle_beta                 94.738(2)
_cell_angle_gamma                90
_cell_volume                     300.252(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6302
_cell_measurement_temperature    50(1)
_cell_measurement_theta_max      31.1330
_cell_measurement_theta_min      1.8360
_shelx_estimated_absorpt_T_max   0.957
_shelx_estimated_absorpt_T_min   0.473
_exptl_absorpt_coefficient_mu    22.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.377
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.859
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3960
_diffrn_reflns_point_group_measured_fraction_full 0.859
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.466
_diffrn_reflns_theta_min         1.855
_diffrn_ambient_temperature      50(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.859
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.48   0.50    0.30 154.30  25.00  73.80    --   720
  2  φ    -25.74 154.37   0.50    0.30 114.30  25.00  73.80    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0431965805
_diffrn_orient_matrix_UB_12      -0.0165940599
_diffrn_orient_matrix_UB_13      0.0566853484
_diffrn_orient_matrix_UB_21      0.0295742595
_diffrn_orient_matrix_UB_22      -0.0277261924
_diffrn_orient_matrix_UB_23      -0.0297013967
_diffrn_orient_matrix_UB_31      0.0588030224
_diffrn_orient_matrix_UB_32      0.0017498966
_diffrn_orient_matrix_UB_33      0.0669306143
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                816
_reflns_number_total             883
_reflns_odcompleteness_completeness 86.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     14.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.178
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.246
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         883
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0271
_refine_ls_restrained_S_all      1.131
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0509P)²+0.0508P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0761
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.25932(5) 0.10014(2) 0.04256(6) 0.00325(13) Uani 1 1 d . . . . .
As2 As 0.35529(5) 0.35100(2) 0.00370(6) 0.00322(13) Uani 1 1 d . . . . .
O1 O 0.4334(4) 0.21751(15) 0.0721(5) 0.0066(4) Uani 1 1 d . . . . .
O2 O 0.6573(4) 0.39928(14) 0.1567(5) 0.0052(4) Uani 1 1 d . . . . .
O3 O -0.0471(4) 0.14092(16) 0.1339(5) 0.0060(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 0.00352(18) 0.00492(18) 0.00135(19) 0.00000(8) 0.00052(12) 0.00047(8)
As2 0.00322(18) 0.00551(18) 0.00112(18) 0.00006(8) 0.00131(12) 0.00002(8)
O1 0.0065(8) 0.0071(8) 0.0062(9) 0.0016(7) 0.0001(7) -0.0001(7)
O2 0.0048(8) 0.0097(8) 0.0011(9) 0.0003(6) 0.0002(7) -0.0023(6)
O3 0.0042(8) 0.0125(9) 0.0015(9) 0.0002(7) 0.0009(7) 0.0018(7)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.7561(19) . ?
As1 O2 1.767(2) 4_565 ?
As1 O3 1.7757(19) . ?
As2 O1 1.7740(19) . ?
As2 O2 1.789(2) . ?
As2 O3 1.778(2) 4_665 ?

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
_geom_angle_publ_flag
O1 As1 O2 100.65(9) . 4_565 ?
O1 As1 O3 102.21(9) . . ?
O2 As1 O3 90.89(10) 4_565 . ?
O1 As2 O2 94.50(9) . . ?
O1 As2 O3 97.81(9) . 4_665 ?
O3 As2 O2 91.18(9) 4_665 . ?
As1 O1 As2 133.98(12) . . ?
As1 O2 As2 124.40(11) 4_666 . ?
As1 O3 As2 124.76(12) . 4_566 ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O3 As2 -86.36(15) . . . 4_566 ?
O1 As2 O2 As1 -71.81(14) . . . 4_666 ?
O2 As1 O1 As2 60.44(17) 4_565 . . . ?
O2 As1 O3 As2 172.54(14) 4_565 . . 4_566 ?
O2 As2 O1 As1 172.21(16) . . . . ?
O3 As1 O1 As2 -32.82(18) . . . . ?
O3 As2 O1 As1 -95.98(16) 4_665 . . . ?
O3 As2 O2 As1 -169.75(13) 4_665 . . 4_666 ?

_shelx_res_file                  
;
TITL clau1_1_50 in P21/n #14
    clau1_1_50.res
    created by SHELXL-2018/3 at 13:46:20 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.267534 12.766744 4.480071 90 94.7383 90
ZERR 4 0.000122 0.000248 0.0001 0 0.0023 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 12 8

L.S. 10 0 0
PLAN  5
SIZE 0.002 0.018 0.04
CONF
fmap 2 53
MORE -1
ACTA
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_1_50.hkl">
REM </olex2.extras>

WGHT    0.050900    0.050800
FVAR       8.48909
AS1   2    0.259316    0.100137    0.042559    11.00000    0.00352    0.00492 =
         0.00135    0.00000    0.00052    0.00047
AS2   2    0.355285    0.351002    0.003703    11.00000    0.00322    0.00551 =
         0.00112    0.00006    0.00131    0.00002
O1    1    0.433441    0.217507    0.072135    11.00000    0.00645    0.00706 =
         0.00616    0.00156    0.00012   -0.00008
O2    1    0.657333    0.399278    0.156695    11.00000    0.00481    0.00969 =
         0.00106    0.00026    0.00021   -0.00229
O3    1   -0.047123    0.140915    0.133886    11.00000    0.00423    0.01247 =
         0.00150    0.00020    0.00094    0.00177
HKLF 4




REM  clau1_1_50 in P21/n #14
REM wR2 = 0.0761, GooF = S = 1.131, Restrained GooF = 1.131 for all data
REM R1 = 0.0271 for 816 Fo > 4sig(Fo) and 0.0291 for all 883 data
REM 46 parameters refined using 0 restraints

END

WGHT      0.0509      0.0508

REM Highest difference peak  1.178,  deepest hole -1.125,  1-sigma level  0.246
Q1    1   0.3343  0.0596  0.1201  11.00000  0.05    1.18
Q2    1   0.2871  0.3156 -0.0934  11.00000  0.05    0.95
Q3    1   0.2387  0.3822 -0.0735  11.00000  0.05    0.87
Q4    1   0.3575  0.1385  0.1128  11.00000  0.05    0.81
Q5    1   0.0838  0.1034 -0.0586  11.00000  0.05    0.79
;
_shelx_res_checksum              7671
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.733
_oxdiff_exptl_absorpt_empirical_full_min 0.486
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_clau1_5_270
_database_code_depnum_ccdc_archive 'CCDC 2031536'
loop_
_audit_author_name
_audit_author_address
'Piotr A. Gunka'
;Warsaw University of Technology, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_audit_creation_date             2020-05-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'claudetite I'
_chemical_name_systematic        ?
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'As2 O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   5.29393(13)
_cell_length_b                   12.8775(4)
_cell_length_c                   4.50545(12)
_cell_angle_alpha                90
_cell_angle_beta                 94.381(3)
_cell_angle_gamma                90
_cell_volume                     306.252(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5622
_cell_measurement_temperature    270(1)
_cell_measurement_theta_max      24.8360
_cell_measurement_theta_min      1.8300
_shelx_estimated_absorpt_T_max   0.958
_shelx_estimated_absorpt_T_min   0.519
_exptl_absorpt_coefficient_mu    21.600
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.291
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            8886
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.496
_diffrn_reflns_theta_min         1.839
_diffrn_ambient_temperature      270(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.26   0.50    0.30 154.30  15.00  73.80    --   720
  2  φ    -25.74 334.26   0.50    0.30 114.30  15.00  73.80    --   720
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0454160990
_diffrn_orient_matrix_UB_12      0.0252580418
_diffrn_orient_matrix_UB_13      -0.0149813423
_diffrn_orient_matrix_UB_21      0.0491594298
_diffrn_orient_matrix_UB_22      -0.0190969304
_diffrn_orient_matrix_UB_23      -0.0414774439
_diffrn_orient_matrix_UB_31      -0.0406235423
_diffrn_orient_matrix_UB_32      0.0051496391
_diffrn_orient_matrix_UB_33      -0.0807984155
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                850
_reflns_number_total             978
_reflns_odcompleteness_completeness 84.31
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.88
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.245
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         978
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0294
_refine_ls_restrained_S_all      1.060
_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)+(0.0387P)²+0.0547P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0729
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.25856(7) 0.10121(3) 0.04121(8) 0.01251(13) Uani 1 1 d . . . . .
As2 As 0.35638(7) 0.35031(3) 0.00475(8) 0.01286(13) Uani 1 1 d . . . . .
O1 O 0.4312(5) 0.2179(2) 0.0700(7) 0.0183(6) Uani 1 1 d . . . . .
O2 O 0.6567(6) 0.3977(2) 0.1578(6) 0.0170(6) Uani 1 1 d . . . . .
O3 O -0.0460(5) 0.1414(2) 0.1375(6) 0.0180(6) 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 0.0123(2) 0.0158(2) 0.0094(2) 0.00037(12) 0.00045(14) 0.00186(13)
As2 0.0107(2) 0.0188(2) 0.0094(2) -0.00028(12) 0.00326(14) 0.00032(14)
O1 0.0144(12) 0.0171(13) 0.0233(15) 0.0001(11) -0.0001(11) -0.0015(11)
O2 0.0184(14) 0.0256(14) 0.0068(12) 0.0020(10) 0.0010(11) -0.0055(11)
O3 0.0131(13) 0.0333(16) 0.0077(12) 0.0007(10) 0.0006(10) 0.0035(12)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.758(3) . ?
As1 O2 1.770(3) 4_565 ?
As1 O3 1.778(3) . ?
As2 O1 1.770(3) . ?
As2 O2 1.791(3) . ?
As2 O3 1.774(3) 4_665 ?

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
_geom_angle_publ_flag
O1 As1 O2 100.55(14) . 4_565 ?
O1 As1 O3 102.06(13) . . ?
O2 As1 O3 91.24(13) 4_565 . ?
O1 As2 O2 94.81(13) . . ?
O1 As2 O3 97.77(14) . 4_665 ?
O3 As2 O2 91.44(13) 4_665 . ?
As1 O1 As2 134.64(17) . . ?
As1 O2 As2 124.99(16) 4_666 . ?
As2 O3 As1 125.39(16) 4_566 . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O3 As2 -86.1(2) . . . 4_566 ?
O1 As2 O2 As1 -72.2(2) . . . 4_666 ?
O2 As1 O1 As2 60.4(3) 4_565 . . . ?
O2 As1 O3 As2 172.8(2) 4_565 . . 4_566 ?
O2 As2 O1 As1 171.8(2) . . . . ?
O3 As1 O1 As2 -33.2(3) . . . . ?
O3 As2 O1 As1 -96.1(3) 4_665 . . . ?
O3 As2 O2 As1 -170.1(2) 4_665 . . 4_666 ?

_shelx_res_file                  
;
TITL clau1_5_270 in P21/n #14
    clau1_5_270.res
    created by SHELXL-2018/3 at 16:39:09 on 18-May-2020
REM reset to P21/n #14
CELL 0.41328 5.293935 12.877539 4.505449 90 94.3811 90
ZERR 4 0.000135 0.000352 0.000118 0 0.0025 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 12 8

L.S. 10
PLAN  5
SIZE 0.002 0.018 0.035
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_5_270.hkl">
REM </olex2.extras>

WGHT    0.038700    0.054700
FVAR       6.70920
AS1   2    0.258559    0.101206    0.041213    11.00000    0.01233    0.01577 =
         0.00936    0.00037    0.00045    0.00186
AS2   2    0.356376    0.350309    0.004755    11.00000    0.01074    0.01883 =
         0.00940   -0.00028    0.00326    0.00032
O1    1    0.431164    0.217887    0.069952    11.00000    0.01439    0.01712 =
         0.02327    0.00012   -0.00014   -0.00155
O2    1    0.656744    0.397732    0.157798    11.00000    0.01845    0.02563 =
         0.00682    0.00201    0.00095   -0.00549
O3    1   -0.045972    0.141418    0.137486    11.00000    0.01308    0.03329 =
         0.00775    0.00073    0.00061    0.00351
HKLF 4




REM  clau1_5_270 in P21/n #14
REM wR2 = 0.0729, GooF = S = 1.060, Restrained GooF = 1.060 for all data
REM R1 = 0.0294 for 850 Fo > 4sig(Fo) and 0.0348 for all 978 data
REM 46 parameters refined using 0 restraints

END

WGHT      0.0387      0.0547

REM Highest difference peak  1.318,  deepest hole -1.084,  1-sigma level  0.245
Q1    1   0.3649  0.2804  0.0049  11.00000  0.05    1.32
Q2    1   0.2714  0.0373  0.0331  11.00000  0.05    1.27
Q3    1   0.2753  0.1711  0.0332  11.00000  0.05    1.22
Q4    1   0.6928  0.4007  0.3413  11.00000  0.05    1.09
Q5    1   0.3770  0.4207 -0.0033  11.00000  0.05    1.03
;
_shelx_res_checksum              31286
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.850
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_clau1_1_20
_database_code_depnum_ccdc_archive 'CCDC 2031544'
loop_
_audit_author_name
_audit_author_address
'Piotr A. Gunka'
;Warsaw University of Technology, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_audit_creation_date             2020-05-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'claudetite I'
_chemical_name_systematic        ?
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'As2 O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   5.27158(13)
_cell_length_b                   12.7597(3)
_cell_length_c                   4.48224(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.731(3)
_cell_angle_gamma                90
_cell_volume                     300.466(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6347
_cell_measurement_temperature    20(1)
_cell_measurement_theta_max      31.1280
_cell_measurement_theta_min      1.8340
_shelx_estimated_absorpt_T_max   0.957
_shelx_estimated_absorpt_T_min   0.473
_exptl_absorpt_coefficient_mu    22.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.373
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.824
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3950
_diffrn_reflns_point_group_measured_fraction_full 0.824
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.466
_diffrn_reflns_theta_min         1.856
_diffrn_ambient_temperature      20(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.824
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.26   0.50    0.30 154.30  25.00  73.80    --   720
  2  φ    -25.74 154.26   0.50    0.30 114.30  25.00  73.80    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0431632896
_diffrn_orient_matrix_UB_12      -0.0166139123
_diffrn_orient_matrix_UB_13      0.0566020771
_diffrn_orient_matrix_UB_21      0.0294535954
_diffrn_orient_matrix_UB_22      -0.0277235343
_diffrn_orient_matrix_UB_23      -0.0298903582
_diffrn_orient_matrix_UB_31      0.0588256994
_diffrn_orient_matrix_UB_32      0.0016709630
_diffrn_orient_matrix_UB_33      0.0668912092
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                801
_reflns_number_total             863
_reflns_odcompleteness_completeness 81.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.19
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.687
_refine_diff_density_min         -3.016
_refine_diff_density_rms         0.354
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         863
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0410
_refine_ls_restrained_S_all      1.125
_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)+(0.0869P)²+0.3074P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1133
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(As2) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(O3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.25872(6) 0.10017(2) 0.04253(8) 0.0032(2) Uani 1 1 d . . . . .
As2 As 0.35502(6) 0.35096(2) 0.00336(8) 0.00282(19) Uani 1 1 d . U . . .
O1 O 0.4328(5) 0.21741(19) 0.0721(6) 0.0064(5) Uani 1 1 d . . . . .
O2 O 0.6565(5) 0.39899(18) 0.1573(6) 0.0050(5) Uani 1 1 d . . . . .
O3 O -0.0469(5) 0.14099(19) 0.1351(6) 0.0064(5) Uani 1 1 d . U . . .

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 0.0030(2) 0.0043(2) 0.0024(3) -0.00022(10) 0.00061(14) 0.00028(10)
As2 0.0027(2) 0.0033(2) 0.0025(2) 0.00010(7) 0.00085(9) 0.00005(7)
O1 0.0055(9) 0.0058(10) 0.0081(11) 0.0006(9) 0.0006(8) -0.0014(9)
O2 0.0042(11) 0.0077(10) 0.0029(11) 0.0002(7) -0.0001(9) -0.0019(8)
O3 0.0058(8) 0.0087(8) 0.0049(9) 0.0001(6) 0.0021(7) 0.0009(6)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.754(2) . ?
As1 O2 1.766(3) 4_565 ?
As1 O3 1.775(3) . ?
As2 O1 1.774(2) . ?
As2 O2 1.788(3) . ?
As2 O3 1.773(3) 4_665 ?

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
_geom_angle_publ_flag
O1 As1 O2 100.61(12) . 4_565 ?
O1 As1 O3 102.21(12) . . ?
O2 As1 O3 90.99(13) 4_565 . ?
O1 As2 O2 94.41(11) . . ?
O3 As2 O1 97.83(12) 4_665 . ?
O3 As2 O2 91.22(12) 4_665 . ?
As1 O1 As2 133.96(15) . . ?
As1 O2 As2 124.69(15) 4_666 . ?
As2 O3 As1 125.08(16) 4_566 . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O3 As2 -86.40(18) . . . 4_566 ?
O1 As2 O2 As1 -71.86(17) . . . 4_666 ?
O2 As1 O1 As2 60.3(2) 4_565 . . . ?
O2 As1 O3 As2 172.53(18) 4_565 . . 4_566 ?
O2 As2 O1 As1 172.1(2) . . . . ?
O3 As1 O1 As2 -33.1(2) . . . . ?
O3 As2 O1 As1 -96.1(2) 4_665 . . . ?
O3 As2 O2 As1 -169.82(17) 4_665 . . 4_666 ?

_shelx_res_file                  
;
TITL clau1_1_20 in P21/n #14
    clau1_1_20.res
    created by SHELXL-2018/3 at 14:00:10 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.271585 12.759731 4.48224 90 94.7309 90
ZERR 4 0.000132 0.000268 0.000107 0 0.0025 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC As O
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 8 12
ISOR 0.0001 0.0002 As2
ISOR 0.001 0.002 O3

L.S. 10 0 0
PLAN  5
SIZE 0.002 0.02 0.04
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_1_20.hkl">
REM </olex2.extras>

WGHT    0.086900    0.307400
FVAR       9.74235
AS1   1    0.258722    0.100168    0.042527    11.00000    0.00298    0.00430 =
         0.00241   -0.00022    0.00061    0.00028
AS2   1    0.355024    0.350963    0.003357    11.00000    0.00273    0.00333 =
         0.00251    0.00010    0.00085    0.00005
O1    2    0.432799    0.217407    0.072058    11.00000    0.00550    0.00575 =
         0.00808    0.00060    0.00063   -0.00141
O2    2    0.656541    0.398992    0.157267    11.00000    0.00423    0.00772 =
         0.00294    0.00023   -0.00005   -0.00189
O3    2   -0.046921    0.140992    0.135087    11.00000    0.00578    0.00869 =
         0.00493    0.00006    0.00208    0.00092
HKLF 4




REM  clau1_1_20 in P21/n #14
REM wR2 = 0.1133, GooF = S = 1.080, Restrained GooF = 1.125 for all data
REM R1 = 0.0410 for 801 Fo > 4sig(Fo) and 0.0427 for all 863 data
REM 46 parameters refined using 12 restraints

END

WGHT      0.0873      0.2896

REM Highest difference peak  2.687,  deepest hole -3.016,  1-sigma level  0.354
Q1    1   0.3705  0.3197  0.0231  11.00000  0.05    2.69
Q2    1   0.3506  0.3819  0.0023  11.00000  0.05    2.59
Q3    1   0.2656  0.1378  0.0421  11.00000  0.05    1.82
Q4    1   0.2311  0.0669  0.0159  11.00000  0.05    1.25
Q5    1   0.3422  0.1979 -0.0452  11.00000  0.05    1.14
;
_shelx_res_checksum              57855
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.716
_oxdiff_exptl_absorpt_empirical_full_min 0.462
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_clau1_5_190
_database_code_depnum_ccdc_archive 'CCDC 2031538'
loop_
_audit_author_name
_audit_author_address
'Piotr A. Gunka'
;Warsaw University of Technology, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_audit_creation_date             2020-05-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'claudetite I'
_chemical_name_systematic        ?
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'As2 O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   5.29150(15)
_cell_length_b                   12.8527(4)
_cell_length_c                   4.50173(14)
_cell_angle_alpha                90
_cell_angle_beta                 94.533(3)
_cell_angle_gamma                90
_cell_volume                     305.206(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4530
_cell_measurement_temperature    190(1)
_cell_measurement_theta_max      25.9430
_cell_measurement_theta_min      1.8280
_shelx_estimated_absorpt_T_max   0.958
_shelx_estimated_absorpt_T_min   0.518
_exptl_absorpt_coefficient_mu    21.674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.306
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            6652
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.497
_diffrn_reflns_theta_min         1.843
_diffrn_ambient_temperature      190(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.26   0.50    0.30 154.30  15.00  73.80    --   720
  2  φ    -25.74 334.26   0.50    0.30 114.30  15.00  73.80    --   720
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0440806699
_diffrn_orient_matrix_UB_12      0.0257933629
_diffrn_orient_matrix_UB_13      -0.0140356647
_diffrn_orient_matrix_UB_21      0.0502538070
_diffrn_orient_matrix_UB_22      -0.0184649279
_diffrn_orient_matrix_UB_23      -0.0419633973
_diffrn_orient_matrix_UB_31      -0.0408833531
_diffrn_orient_matrix_UB_32      0.0051238512
_diffrn_orient_matrix_UB_33      -0.0808329714
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                837
_reflns_number_total             977
_reflns_odcompleteness_completeness 84.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.84
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.539
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.266
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         977
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0296
_refine_ls_restrained_S_all      1.037
_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)+(0.0428P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0760
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.25886(7) 0.10083(3) 0.04173(9) 0.00943(13) Uani 1 1 d . . . . .
As2 As 0.35592(7) 0.35055(3) 0.00435(8) 0.00962(13) Uani 1 1 d . . . . .
O1 O 0.4312(6) 0.2178(2) 0.0704(7) 0.0145(6) Uani 1 1 d . . . . .
O2 O 0.6567(6) 0.3983(2) 0.1571(6) 0.0127(6) Uani 1 1 d . . . . .
O3 O -0.0460(6) 0.1412(2) 0.1366(6) 0.0139(6) 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 0.0090(2) 0.0124(2) 0.0069(2) 0.00036(12) 0.00072(14) 0.00122(13)
As2 0.0078(2) 0.0147(2) 0.0067(2) -0.00025(13) 0.00285(14) 0.00027(14)
O1 0.0131(12) 0.0135(13) 0.0167(15) 0.0008(11) -0.0004(11) -0.0026(11)
O2 0.0129(13) 0.0200(14) 0.0056(13) 0.0000(10) 0.0028(11) -0.0042(11)
O3 0.0100(13) 0.0266(16) 0.0054(13) -0.0001(11) 0.0028(10) 0.0016(12)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.757(3) . ?
As1 O2 1.773(3) 4_565 ?
As1 O3 1.778(3) . ?
As2 O1 1.772(3) . ?
As2 O2 1.791(3) . ?
As2 O3 1.777(3) 4_665 ?

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
_geom_angle_publ_flag
O1 As1 O2 100.52(14) . 4_565 ?
O1 As1 O3 102.00(14) . . ?
O2 As1 O3 91.16(14) 4_565 . ?
O1 As2 O2 94.84(14) . . ?
O1 As2 O3 97.77(15) . 4_665 ?
O3 As2 O2 91.21(14) 4_665 . ?
As1 O1 As2 134.65(18) . . ?
As1 O2 As2 124.76(16) 4_666 . ?
As2 O3 As1 125.33(18) 4_566 . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O3 As2 -86.3(2) . . . 4_566 ?
O1 As2 O2 As1 -72.0(2) . . . 4_666 ?
O2 As1 O1 As2 60.4(3) 4_565 . . . ?
O2 As1 O3 As2 172.7(2) 4_565 . . 4_566 ?
O2 As2 O1 As1 172.0(3) . . . . ?
O3 As1 O1 As2 -33.1(3) . . . . ?
O3 As2 O1 As1 -96.2(3) 4_665 . . . ?
O3 As2 O2 As1 -169.9(2) 4_665 . . 4_666 ?

_shelx_res_file                  
;
TITL clau1_5_190 in P21/n #14
    clau1_5_190.res
    created by SHELXL-2018/3 at 13:10:48 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.291505 12.852706 4.501727 90 94.5326 90
ZERR 4 0.000152 0.00038 0.000136 0 0.0028 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 12 8

L.S. 9
PLAN  5
SIZE 0.002 0.018 0.035
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_5_190.hkl">
REM </olex2.extras>

WGHT    0.042800
FVAR       6.68048
AS1   2    0.258865    0.100825    0.041729    11.00000    0.00903    0.01241 =
         0.00685    0.00036    0.00072    0.00122
AS2   2    0.355918    0.350550    0.004354    11.00000    0.00776    0.01474 =
         0.00673   -0.00025    0.00285    0.00027
O1    1    0.431199    0.217759    0.070389    11.00000    0.01307    0.01346 =
         0.01673    0.00079   -0.00044   -0.00256
O2    1    0.656697    0.398291    0.157054    11.00000    0.01292    0.02000 =
         0.00563    0.00000    0.00283   -0.00422
O3    1   -0.045961    0.141233    0.136552    11.00000    0.01004    0.02659 =
         0.00538   -0.00008    0.00283    0.00157
HKLF 4




REM  clau1_5_190 in P21/n #14
REM wR2 = 0.0760, GooF = S = 1.037, Restrained GooF = 1.037 for all data
REM R1 = 0.0296 for 837 Fo > 4sig(Fo) and 0.0361 for all 977 data
REM 46 parameters refined using 0 restraints

END

WGHT      0.0428      0.0000

REM Highest difference peak  1.539,  deepest hole -0.966,  1-sigma level  0.266
Q1    1   0.2874  0.1649  0.0337  11.00000  0.05    1.54
Q2    1   0.3545  0.2831  0.0062  11.00000  0.05    1.41
Q3    1   0.2384  0.0381  0.0173  11.00000  0.05    1.29
Q4    1   0.3747  0.4170  0.0091  11.00000  0.05    1.21
Q5    1   0.3919  0.0579  0.0576  11.00000  0.05    1.20
;
_shelx_res_checksum              54115
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.318
_oxdiff_exptl_absorpt_empirical_full_min 0.827
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_clau1_5_120
_database_code_depnum_ccdc_archive 'CCDC 2031540'
loop_
_audit_author_name
_audit_author_address
'Piotr A. Gunka'
;Warsaw University of Technology, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_audit_creation_date             2020-05-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'claudetite I'
_chemical_name_systematic        ?
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         'As2 O3'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   5.28379(13)
_cell_length_b                   12.8173(3)
_cell_length_c                   4.49485(12)
_cell_angle_alpha                90
_cell_angle_beta                 94.618(2)
_cell_angle_gamma                90
_cell_volume                     303.421(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6462
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      26.7650
_cell_measurement_theta_min      1.8340
_shelx_estimated_absorpt_T_max   0.958
_shelx_estimated_absorpt_T_min   0.516
_exptl_absorpt_coefficient_mu    21.801
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.331
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            9603
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.497
_diffrn_reflns_theta_min         1.848
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.26   0.50    0.30 154.30  15.00  73.80    --   720
  2  φ    -25.74 228.76   0.50    0.30 114.30  15.00  73.80    --   509
  3  φ    154.26 334.26   0.50    0.30 114.30  15.00  73.80    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0424792643
_diffrn_orient_matrix_UB_12      0.0264254758
_diffrn_orient_matrix_UB_13      -0.0130193873
_diffrn_orient_matrix_UB_21      0.0515613449
_diffrn_orient_matrix_UB_22      -0.0177401590
_diffrn_orient_matrix_UB_23      -0.0423975422
_diffrn_orient_matrix_UB_31      -0.0411663610
_diffrn_orient_matrix_UB_32      0.0050576263
_diffrn_orient_matrix_UB_33      -0.0809491181
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                839
_reflns_number_total             971
_reflns_odcompleteness_completeness 84.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.83
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.915
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.302
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         971
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0308
_refine_ls_restrained_S_all      1.089
_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)+(0.0423P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0765
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.25900(7) 0.10041(3) 0.04233(9) 0.00652(13) Uani 1 1 d . . . . .
As2 As 0.35532(7) 0.35081(3) 0.00382(8) 0.00648(13) Uani 1 1 d . . . . .
O1 O 0.4316(5) 0.2176(2) 0.0696(7) 0.0108(6) Uani 1 1 d . . . . .
O2 O 0.6565(6) 0.3992(2) 0.1569(6) 0.0089(5) Uani 1 1 d . U . . .
O3 O -0.0466(6) 0.1411(2) 0.1357(6) 0.0099(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 0.0055(2) 0.0102(2) 0.0039(2) 0.00006(12) 0.00089(14) 0.00094(13)
As2 0.0046(2) 0.0116(2) 0.0036(2) -0.00001(12) 0.00239(15) 0.00012(13)
O1 0.0085(12) 0.0115(13) 0.0123(15) 0.0004(10) 0.0009(11) -0.0009(11)
O2 0.0088(12) 0.0154(12) 0.0027(12) -0.0001(9) 0.0019(10) -0.0026(10)
O3 0.0058(12) 0.0208(14) 0.0033(13) 0.0011(10) 0.0012(10) 0.0023(11)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.756(3) . ?
As1 O2 1.773(3) 4_565 ?
As1 O3 1.779(3) . ?
As2 O1 1.774(3) . ?
As2 O2 1.793(3) . ?
As2 O3 1.776(3) 4_665 ?

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
_geom_angle_publ_flag
O1 As1 O2 100.48(14) . 4_565 ?
O1 As1 O3 102.05(13) . . ?
O2 As1 O3 91.04(13) 4_565 . ?
O1 As2 O2 94.95(13) . . ?
O1 As2 O3 97.59(13) . 4_665 ?
O3 As2 O2 91.19(13) 4_665 . ?
As1 O1 As2 134.58(18) . . ?
As1 O2 As2 124.58(16) 4_666 . ?
As2 O3 As1 125.12(17) 4_566 . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O3 As2 -86.7(2) . . . 4_566 ?
O1 As2 O2 As1 -71.8(2) . . . 4_666 ?
O2 As1 O1 As2 60.9(3) 4_565 . . . ?
O2 As1 O3 As2 172.4(2) 4_565 . . 4_566 ?
O2 As2 O1 As1 171.6(2) . . . . ?
O3 As1 O1 As2 -32.5(3) . . . . ?
O3 As2 O1 As1 -96.6(2) 4_665 . . . ?
O3 As2 O2 As1 -169.5(2) 4_665 . . 4_666 ?

_shelx_res_file                  
;
TITL clau1_5_120 in P21/n #14
    clau1_5_120.res
    created by SHELXL-2018/3 at 13:28:21 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.283794 12.817305 4.494851 90 94.6182 90
ZERR 4 0.000129 0.000323 0.000118 0 0.0023 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 12 8
ISOR 0.003 0.006 O2

L.S. 10 0 0
PLAN  5
SIZE 0.002 0.018 0.035
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_5_120.hkl">
REM </olex2.extras>

WGHT    0.042300
FVAR       6.27116
AS1   2    0.259001    0.100406    0.042327    11.00000    0.00552    0.01018 =
         0.00395    0.00006    0.00089    0.00094
AS2   2    0.355325    0.350815    0.003821    11.00000    0.00463    0.01155 =
         0.00358   -0.00001    0.00239    0.00012
O1    1    0.431582    0.217575    0.069633    11.00000    0.00845    0.01148 =
         0.01235    0.00045    0.00094   -0.00093
O2    1    0.656541    0.399200    0.156850    11.00000    0.00879    0.01543 =
         0.00271   -0.00013    0.00192   -0.00258
O3    1   -0.046630    0.141114    0.135728    11.00000    0.00579    0.02079 =
         0.00332    0.00107    0.00124    0.00230
HKLF 4




REM  clau1_5_120 in P21/n #14
REM wR2 = 0.0765, GooF = S = 1.087, Restrained GooF = 1.089 for all data
REM R1 = 0.0308 for 839 Fo > 4sig(Fo) and 0.0365 for all 971 data
REM 46 parameters refined using 6 restraints

END

WGHT      0.0422      0.0000

REM Highest difference peak  1.915,  deepest hole -1.055,  1-sigma level  0.302
Q1    1   0.2685  0.1638  0.0324  11.00000  0.05    1.91
Q2    1   0.2419  0.0382  0.0147  11.00000  0.05    1.77
Q3    1   0.3639  0.2829  0.0026  11.00000  0.05    1.77
Q4    1   0.3580  0.4189  0.0054  11.00000  0.05    1.43
Q5    1   0.3086  0.4055  0.0199  11.00000  0.05    1.16
;
_shelx_res_checksum              95162
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.216
_oxdiff_exptl_absorpt_empirical_full_min 0.849
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_clau1_1_cdl_att4
_database_code_depnum_ccdc_archive 'CCDC 2031545'
loop_
_audit_author_name
_audit_author_address
'Piotr A. Gunka'
;Warsaw University of Technology, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_audit_creation_date             2020-05-20
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            'claudetite I'
_chemical_name_systematic        ?
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_melting_point          ?
_chemical_oxdiff_formula         As2O3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2879 0.7731 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   5.2635(2)
_cell_length_b                   12.7320(4)
_cell_length_c                   4.46891(16)
_cell_angle_alpha                90
_cell_angle_beta                 94.675(4)
_cell_angle_gamma                90
_cell_volume                     298.489(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6598
_cell_measurement_temperature    10(1)
_cell_measurement_theta_max      24.5140
_cell_measurement_theta_min      1.8500
_shelx_estimated_absorpt_T_max   0.957
_shelx_estimated_absorpt_T_min   0.471
_exptl_absorpt_coefficient_mu    22.162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.402
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.002
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            8688
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.499
_diffrn_reflns_theta_min         1.860
_diffrn_ambient_temperature      10(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ    -25.74 334.26   0.50    0.30 144.30  10.00  73.80    --   720
  2  φ    -25.74 334.26   0.50    0.30 124.30  10.00  73.80    --   720
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0432673552
_diffrn_orient_matrix_UB_12      -0.0165302902
_diffrn_orient_matrix_UB_13      0.0571496514
_diffrn_orient_matrix_UB_21      0.0296920354
_diffrn_orient_matrix_UB_22      -0.0278523070
_diffrn_orient_matrix_UB_23      -0.0293247555
_diffrn_orient_matrix_UB_31      0.0587471904
_diffrn_orient_matrix_UB_32      0.0019041418
_diffrn_orient_matrix_UB_33      0.0670329285
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                843
_reflns_number_total             951
_reflns_odcompleteness_completeness 78.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.430
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.366
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         951
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0344
_refine_ls_restrained_S_all      1.101
_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)+(0.0736P)²+0.1114P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1066
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.25790(8) 0.10075(3) 0.04198(10) 0.00773(17) Uani 1 1 d . . . . .
As2 As 0.35572(8) 0.35039(3) 0.00333(9) 0.00703(17) Uani 1 1 d . . . . .
O1 O 0.4325(6) 0.2173(2) 0.0705(7) 0.0111(6) Uani 1 1 d . . . . .
O2 O 0.6565(6) 0.3985(2) 0.1571(7) 0.0093(6) Uani 1 1 d . . . . .
O3 O -0.0461(6) 0.1419(3) 0.1353(7) 0.0103(6) 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 0.0073(3) 0.0111(3) 0.0049(3) -0.00058(13) 0.00121(17) 0.00062(14)
As2 0.0071(3) 0.0101(3) 0.0043(3) 0.00030(13) 0.00235(17) 0.00014(14)
O1 0.0110(12) 0.0116(14) 0.0102(14) 0.0005(11) -0.0020(11) 0.0002(12)
O2 0.0074(13) 0.0142(14) 0.0062(14) 0.0015(10) 0.0008(11) -0.0030(11)
O3 0.0076(13) 0.0188(16) 0.0045(14) -0.0008(11) 0.0012(11) 0.0016(12)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.744(3) . ?
As1 O2 1.759(3) 4_565 ?
As1 O3 1.766(3) . ?
As2 O1 1.762(3) . ?
As2 O2 1.782(3) . ?
As2 O3 1.766(3) 4_665 ?

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
_geom_angle_publ_flag
O1 As1 O2 100.53(14) . 4_565 ?
O1 As1 O3 102.29(14) . . ?
O2 As1 O3 91.20(15) 4_565 . ?
O1 As2 O2 94.62(14) . . ?
O1 As2 O3 97.58(15) . 4_665 ?
O3 As2 O2 91.24(15) 4_665 . ?
As1 O1 As2 133.90(18) . . ?
As1 O2 As2 124.61(18) 4_666 . ?
As1 O3 As2 125.17(19) . 4_566 ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 As1 O3 As2 -86.7(2) . . . 4_566 ?
O1 As2 O2 As1 -72.0(2) . . . 4_666 ?
O2 As1 O1 As2 60.8(3) 4_565 . . . ?
O2 As1 O3 As2 172.2(2) 4_565 . . 4_566 ?
O2 As2 O1 As1 171.7(3) . . . . ?
O3 As1 O1 As2 -32.8(3) . . . . ?
O3 As2 O1 As1 -96.5(3) 4_665 . . . ?
O3 As2 O2 As1 -169.7(2) 4_665 . . 4_666 ?

_shelx_res_file                  
;
TITL clau1_1_CDL_att4 in P21/n #14
    clau1_1_cdl_att4.res
    created by SHELXL-2018/3 at 14:02:57 on 20-May-2020
REM reset to P21/n #14
CELL 0.41328 5.263548 12.731985 4.468908 90 94.6754 90
ZERR 4 0.000198 0.000408 0.000164 0 0.0037 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC O As
DISP As 0.2879 0.7731
DISP O 0.0017 0.0018
UNIT 12 8

L.S. 10 0 0
PLAN  5
SIZE 0.002 0.02 0.04
CONF
MORE -1
fmap 2 53
acta
OMIT -2 35
REM <olex2.extras>
REM <HklSrc "%.\\clau1_1_CDL_att4.hkl">
REM </olex2.extras>

WGHT    0.073600    0.111400
FVAR       6.26907
AS1   2    0.257898    0.100754    0.041977    11.00000    0.00733    0.01107 =
         0.00490   -0.00058    0.00121    0.00062
AS2   2    0.355721    0.350391    0.003335    11.00000    0.00707    0.01005 =
         0.00427    0.00030    0.00235    0.00014
O1    1    0.432478    0.217279    0.070496    11.00000    0.01099    0.01162 =
         0.01018    0.00055   -0.00203    0.00023
O2    1    0.656540    0.398480    0.157063    11.00000    0.00741    0.01423 =
         0.00624    0.00146    0.00083   -0.00299
O3    1   -0.046104    0.141861    0.135299    11.00000    0.00761    0.01880 =
         0.00448   -0.00077    0.00118    0.00163
HKLF 4




REM  clau1_1_CDL_att4 in P21/n #14
REM wR2 = 0.1066, GooF = S = 1.101, Restrained GooF = 1.101 for all data
REM R1 = 0.0344 for 843 Fo > 4sig(Fo) and 0.0384 for all 951 data
REM 46 parameters refined using 0 restraints

END

WGHT      0.0737      0.1115

REM Highest difference peak  2.430,  deepest hole -1.236,  1-sigma level  0.366
Q1    1   0.2394  0.1593  0.0011  11.00000  0.05    2.43
Q2    1   0.3528  0.1399  0.0687  11.00000  0.05    1.85
Q3    1   0.1687  0.0614  0.0074  11.00000  0.05    1.69
Q4    1   0.4058  0.3997  0.0557  11.00000  0.05    1.52
Q5    1   0.3649  0.2837 -0.0011  11.00000  0.05    1.43
;
_shelx_res_checksum              54432
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.432
_oxdiff_exptl_absorpt_empirical_full_min 0.666
