High-pressure and low-temperature structural study of claudetite I, a monoclinic layered As2O3 polymorph
Guńka, Piotr A.; Hanfland, Michael; Chen, Yu-Sheng; Zachara, Janusz; CrystEngComm 23 (2021) 638–644; doi:10.1039/D0CE01401J

data_7241859
_publ_section_title
;
 High-pressure and low-temperature structural study of claudetite I, a
 monoclinic layered As2O3 polymorph
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              638
_journal_page_last               644
_journal_paper_doi               10.1039/D0CE01401J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'As2 O3'
_chemical_formula_sum            'As2 O3'
_chemical_formula_weight         197.84
_chemical_name_common            'claudetite I'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2020-05-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-09-11 deposited with the CCDC.	2020-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.731(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.27158(13)
_cell_length_b                   12.7597(3)
_cell_length_c                   4.48224(11)
_cell_measurement_reflns_used    6347
_cell_measurement_temperature    20(1)
_cell_measurement_theta_max      31.1280
_cell_measurement_theta_min      1.8340
_cell_volume                     300.465(13)
_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)'
_diffrn_ambient_temperature      20(1)
_diffrn_detector                 'CCD plate'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -25.74 334.26   0.50    0.30 154.30  25.00  73.80    --   720
  2  \f    -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       '\f 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_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_source                   synchrotron
_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_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.373
_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
_refine_diff_density_max         2.687
_refine_diff_density_min         -3.016
_refine_diff_density_rms         0.354
_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_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0410
_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/[\s^2^(Fo^2^)+(0.0869P)^2^+0.3074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                801
_reflns_number_total             863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01401j2.cif
_cod_data_source_block           clau1_1_20
_cod_depositor_comments
'Adding full bibliography for 7241824--7241862.cif.'
_cod_original_cell_volume        300.466(12)
_cod_database_code               7241859
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'As2 O3'
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.473
_reflns_odcompleteness_completeness 81.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.19
_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
;
_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