Role of lone-pair electron localization in temperature-induced phase transitions in mimetite
Cametti, Georgia; Nagashima, Mariko; Churakov, Sergey V.; Acta Crystallographica Section B 78 (2022) –; doi:10.1107/S2052520622006254

data_2109020
_publ_section_title
;
 Role of lone-pair electron localization in temperature-induced phase
 transitions in mimetite
;
_journal_coeditor_code           TQ5003
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520622006254
_journal_volume                  78
_journal_year                    2022
_chemical_formula_sum            'As4 Cl1.33 O16 Pb6.67'
_chemical_formula_weight         1984.21
_chemical_name_common            mimetite
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 119.953(6)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   20.4487(9)
_cell_length_b                   7.4362(2)
_cell_length_c                   20.4513(9)
_cell_measurement_reflns_used    23365
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      2.8
_cell_volume                     2694.5(2)
_computing_cell_refinement
'CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)'
_computing_data_collection
'CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)'
_computing_data_reduction
'CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'XtalLAB, Synergy, Dualflex, Hypix'
_diffrn_measurement_method       'o scan'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            50947
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         25.559
_diffrn_reflns_theta_min         1.814
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    37.486
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30351
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    7.337
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4976
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         6.418
_refine_diff_density_min         -11.988
_refine_diff_density_rms         0.847
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         19430
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0551
_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^)+226.1430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                15378
_reflns_number_total             19430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tq5003sup1.cif
_cod_data_source_block           Mim123K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'Difmap' was changed
to 'difmap' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2109020
_oxdiff_exptl_absorpt_empirical_full_min 0.549
_oxdiff_exptl_absorpt_empirical_full_max 1.810
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_shelxl_version_number           2014-1
_shelx_res_checksum              28347
_shelx_hkl_checksum              32740
_cod_database_fobs_code 2109020