#------------------------------------------------------------------------------
#$Date: 2022-07-23 06:48:14 +0300 (Sat, 23 Jul 2022) $
#$Revision: 276890 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/90/2109025.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2109025
loop_
_publ_author_name
'Cametti, Georgia'
'Nagashima, Mariko'
'Churakov, Sergey V.'
_publ_section_title
;
 Role of lone-pair electron localization in temperature-induced phase
 transitions in mimetite
;
_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            'As3 Cl O12 Pb5'
_chemical_formula_weight         1488.16
_chemical_name_common            mimetite
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.2722(3)
_cell_length_b                   10.2722(3)
_cell_length_c                   7.4537(3)
_cell_measurement_reflns_used    7991
_cell_measurement_temperature    393(2)
_cell_measurement_theta_max      29.1690
_cell_measurement_theta_min      2.7800
_cell_volume                     681.13(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a'
_computing_data_collection       'CrysAlisPro 1.171.41.104a'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Scheldrick, 2008)'
_diffrn_ambient_temperature      393(2)
_diffrn_detector_area_resol_mean 0.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Hypix'
_diffrn_measurement_method       'o scan'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11659
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         29.196
_diffrn_reflns_theta_min         1.806
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    37.599
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.36744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE 3 ABSPACK'
_exptl_crystal_colour            pale-orange
_exptl_crystal_density_diffrn    7.256
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.411
_refine_diff_density_min         -3.928
_refine_diff_density_rms         0.503
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     39
_refine_ls_number_reflns         1202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0265
_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)+(0.0248P)²+4.3496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1060
_reflns_number_total             1202
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            tq5003sup1.cif
_cod_data_source_block           Mim393K
_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_cell_volume        681.13(5)
_cod_database_code               2109025
_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.
;
_shelxl_version_number           2014-1
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'y, -x+y, z+1/2'
'-x+y, -x, z'
'x-y, x, z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'y, -x+y, -z'
'-y, x-y, -z-1/2'
'x-y, x, -z'
'-x+y, -x, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.3333 0.6667 0.50673(4) 0.02062(8) Uani 1 3 d S T P . .
Pb2 Pb 0.00503(3) 0.25169(3) 0.2500 0.02343(8) Uani 1 2 d S T P . .
As3 As 0.38361(6) 0.40888(7) 0.2500 0.01097(10) Uani 1 2 d S T P . .
O1 O 0.4935(6) 0.3303(7) 0.2500 0.0217(10) Uani 1 2 d S T P . .
O2 O 0.4853(7) 0.5985(6) 0.2500 0.0384(17) Uani 1 2 d S T P . .
O3 O 0.2691(7) 0.3587(7) 0.0720(7) 0.0481(15) Uani 1 1 d . . . . .
Cl Cl 0.0000 0.0000 0.0000 0.0261(6) Uani 1 6 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.2758 1.3314 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -1.1676 6.9287 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O1 74.30(13) 9_566 11_556 ?
O1 Pb1 O1 74.30(13) 9_566 7_666 ?
O1 Pb1 O1 74.30(13) 11_556 7_666 ?
O1 Pb1 O2 90.95(12) 9_566 3_665 ?
O1 Pb1 O2 150.75(17) 11_556 3_665 ?
O1 Pb1 O2 126.57(17) 7_666 3_665 ?
O1 Pb1 O2 126.57(17) 9_566 5_565 ?
O1 Pb1 O2 90.95(12) 11_556 5_565 ?
O1 Pb1 O2 150.75(17) 7_666 5_565 ?
O2 Pb1 O2 77.57(13) 3_665 5_565 ?
O1 Pb1 O2 150.75(17) 9_566 . ?
O1 Pb1 O2 126.57(17) 11_556 . ?
O1 Pb1 O2 90.95(12) 7_666 . ?
O2 Pb1 O2 77.57(13) 3_665 . ?
O2 Pb1 O2 77.57(13) 5_565 . ?
O1 Pb1 Pb1 135.79(8) 9_566 8_556 ?
O1 Pb1 Pb1 135.79(8) 11_556 8_556 ?
O1 Pb1 Pb1 135.79(8) 7_666 8_556 ?
O2 Pb1 Pb1 46.33(9) 3_665 8_556 ?
O2 Pb1 Pb1 46.33(9) 5_565 8_556 ?
O2 Pb1 Pb1 46.33(9) . 8_556 ?
O1 Pb1 O3 119.20(9) 9_566 7_656 ?
O1 Pb1 O3 69.83(14) 11_556 7_656 ?
O1 Pb1 O3 49.78(12) 7_666 7_656 ?
O2 Pb1 O3 138.52(11) 3_665 7_656 ?
O2 Pb1 O3 101.65(12) 5_565 7_656 ?
O2 Pb1 O3 62.16(10) . 7_656 ?
Pb1 Pb1 O3 103.52(2) 8_556 7_656 ?
O2 Pb2 O3 84.28(15) 5_565 11 ?
O2 Pb2 O3 84.28(15) 5_565 6 ?
O3 Pb2 O3 131.8(3) 11 6 ?
O2 Pb2 O3 74.44(17) 5_565 . ?
O3 Pb2 O3 81.64(8) 11 . ?
O3 Pb2 O3 138.46(16) 6 . ?
O2 Pb2 O3 74.44(17) 5_565 8_556 ?
O3 Pb2 O3 138.46(15) 11 8_556 ?
O3 Pb2 O3 81.64(8) 6 8_556 ?
O3 Pb2 O3 58.62(19) . 8_556 ?
O2 As3 O3 106.8(3) . 8_556 ?
O2 As3 O3 106.8(3) . . ?
O3 As3 O3 104.8(5) 8_556 . ?
O2 As3 O1 112.1(3) . . ?
O3 As3 O1 112.86(19) 8_556 . ?
O3 As3 O1 112.86(19) . . ?
As3 O1 Pb1 129.05(14) . 7_666 ?
As3 O1 Pb1 129.05(14) . 2_664 ?
Pb1 O1 Pb1 91.57(16) 7_666 2_664 ?
As3 O2 Pb2 128.2(3) . 3_665 ?
As3 O2 Pb1 100.9(2) . . ?
Pb2 O2 Pb1 115.53(16) 3_665 . ?
As3 O2 Pb1 100.9(2) . 8_556 ?
Pb2 O2 Pb1 115.53(16) 3_665 8_556 ?
Pb1 O2 Pb1 87.34(17) . 8_556 ?
As3 O3 Pb2 137.9(3) . 9 ?
As3 O3 Pb2 98.3(3) . . ?
Pb2 O3 Pb2 115.74(19) 9 . ?
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
Pb1 O1 2.530(3) 9_566 ?
Pb1 O1 2.530(4) 11_556 ?
Pb1 O1 2.530(3) 7_666 ?
Pb1 O2 2.771(4) 3_665 ?
Pb1 O2 2.771(4) 5_565 ?
Pb1 O2 2.771(4) . ?
Pb1 Pb1 3.8272(6) 8_556 ?
Pb1 O3 13.435(5) 7_656 ?
Pb2 O2 2.352(6) 5_565 ?
Pb2 O3 2.629(5) 11 ?
Pb2 O3 2.629(5) 6 ?
Pb2 O3 2.710(7) . ?
Pb2 O3 2.710(7) 8_556 ?
As3 O2 1.689(6) . ?
As3 O3 1.674(4) 8_556 ?
As3 O3 1.674(4) . ?
As3 O1 1.684(5) . ?
O1 Pb1 2.530(3) 7_666 ?
O1 Pb1 2.530(3) 2_664 ?
O2 Pb2 2.352(6) 3_665 ?
O2 Pb1 2.771(4) 8_556 ?
O3 Pb2 2.629(5) 9 ?
