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#$Date: 2024-10-06 16:22:15 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295356 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/28/1572811.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1572811
loop_
_publ_author_name
'Grauer, Maxim'
'Benndorf, Christopher'
'Rohr, Valentin'
'Paulmann, Carsten'
'Oeckler, Oliver'
_publ_contact_author
;
 Prof. Dr. 'Oliver Oeckler'
 Institute for Mineralogy, Crystallography and Materials Science
 Faculty of Chemistry and Mineralogy
 Leipzig University
 Scharnhorststr. 20
 04275 Leipzig, Germany
;
_publ_section_title
;
 Investigations of Some Disordered Quaternary Compounds in the Systems
 Ag/Pb/Sb/Se and Ag/Pb/Sb/Te
;
_journal_issue                   9
_journal_name_full               Crystals
_journal_page_first              789
_journal_paper_doi               10.3390/cryst14090789
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'Ag0.38 Pb0.25 Sb2.38 Te4'
_chemical_formula_sum            'Ag0.38 Pb0.25 Sb2.38 Te4'
_chemical_formula_weight         892.19
_chemical_name_common            'silver lead antimony telluride'
_chemical_name_systematic        'silver lead antimony telluride'
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   none
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   4.2887(1)
_cell_length_b                   4.2887(1)
_cell_length_c                   41.544(1)
_cell_measurement_reflns_used    2147
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      23.5620
_cell_measurement_theta_min      2.0610
_cell_volume                     661.74(3)
_computing_cell_refinement
'CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)'
_computing_data_collection       manual
_computing_data_reduction
'CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)'
_computing_molecular_graphics    'Diamond Version 4.6.3 (Brandenburg, 2020)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXs-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'Pilatus CdTe 1M'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device
'Four circle Kappa diffractometer with Euler cradle'
_diffrn_measurement_device_type  'Huber heavy-duty goniometer'
_diffrn_measurement_method       'oscillation ω scan'
_diffrn_radiation_monochromator
'Water cooled Double Crystal Monochromator Si(111)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.500
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            3975
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        17.458
_diffrn_reflns_theta_max         20.586
_diffrn_reflns_theta_min         2.069
_diffrn_source                   'DESY PetraIII P24'
_exptl_absorpt_coefficient_mu    9.902
_exptl_absorpt_correction_T_max  0.529
_exptl_absorpt_correction_T_min  0.478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            'metallic grey'
_exptl_crystal_density_diffrn    6.716
_exptl_crystal_description       plate
_exptl_crystal_F_000             1102
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   0.5292
_exptl_transmission_factor_min   0.4780
_refine_diff_density_max         2.126
_refine_diff_density_min         -2.081
_refine_diff_density_rms         0.227
_refine_ls_extinction_coef       0.00110(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_reflns         294
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0203
_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)+(0.0361P)²+3.0996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                279
_reflns_number_total             294
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Ag0.38Pb0.25Sb2.38Te4_FINAL.cif
_cod_data_source_block           Ag0.38Pb0.25Sb2.38Te4
_cod_database_code               1572811
_shelx_shelxl_version_number     2017/1
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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
Sb1 Sb 0.333333 0.666667 0.09644(2) 0.0346(2) Uani 0.8349(9) 6 d S T P . .
Pb1 Pb 0.333333 0.666667 0.09644(2) 0.0346(2) Uani 0.0767(13) 6 d S T P . .
Ag1 Ag 0.333333 0.666667 0.09644(2) 0.0346(2) Uani 0.0885(11) 6 d S T P . .
Sb2 Sb 0.000000 0.000000 0.000000 0.0291(3) Uani 0.7087(17) 12 d S T P . .
Pb2 Pb 0.000000 0.000000 0.000000 0.0291(3) Uani 0.0898(19) 12 d S T P . .
Ag2 Ag 0.000000 0.000000 0.000000 0.0291(3) Uani 0.2015(18) 12 d S T P . .
Te3 Te 0.666667 0.333333 0.04390(2) 0.0187(2) Uani 1 6 d S T P . .
Te4 Te 0.000000 0.000000 0.13540(2) 0.0248(2) 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
Ag Ag -2.9199 0.5841 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -1.3538 0.8250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -1.2277 0.8952 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -0.7062 5.7756 '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
Te4 Sb1 Te4 92.913(19) . 1_565 ?
Te4 Sb1 Te4 92.913(19) . 1_665 ?
Te4 Sb1 Te4 92.912(19) 1_565 1_665 ?
Te3 Sb2 Te3 88.427(9) 19 19_665 ?
Te3 Sb2 Te3 91.573(9) 19 1_445 ?
Te3 Sb2 Te3 180.000(12) 19_665 1_445 ?
Te3 Sb2 Te3 91.573(9) 19 1_455 ?
Te3 Sb2 Te3 91.573(9) 19_665 1_455 ?
Te3 Sb2 Te3 88.427(9) 1_445 1_455 ?
Te3 Sb2 Te3 88.427(9) 19 19_655 ?
Te3 Sb2 Te3 88.427(9) 19_665 19_655 ?
Te3 Sb2 Te3 91.573(9) 1_445 19_655 ?
Te3 Sb2 Te3 180.000(12) 1_455 19_655 ?
Te3 Sb2 Te3 180.0 19 . ?
Te3 Sb2 Te3 91.574(9) 19_665 . ?
Te3 Sb2 Te3 88.426(9) 1_445 . ?
Te3 Sb2 Te3 88.426(9) 1_455 . ?
Te3 Sb2 Te3 91.574(9) 19_655 . ?
Sb2 Te3 Sb2 88.424(9) 1_655 . ?
Sb2 Te3 Sb2 88.425(9) 1_655 1_665 ?
Sb2 Te3 Sb2 88.425(9) . 1_665 ?
Sb2 Te3 Pb1 95.171(6) 1_655 1_655 ?
Sb2 Te3 Pb1 174.974(15) . 1_655 ?
Sb2 Te3 Pb1 95.172(6) 1_665 1_655 ?
Sb1 Te4 Sb1 92.913(19) . 1_445 ?
Sb1 Te4 Sb1 92.913(19) . 1_545 ?
Sb1 Te4 Sb1 92.912(19) 1_445 1_545 ?
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
Sb1 Te4 2.9583(5) . ?
Sb1 Te4 2.9584(5) 1_565 ?
Sb1 Te4 2.9584(5) 1_665 ?
Sb2 Te3 3.0751(2) 19 ?
Sb2 Te3 3.0751(2) 19_665 ?
Sb2 Te3 3.0751(2) 1_445 ?
Sb2 Te3 3.0751(2) 1_455 ?
Sb2 Te3 3.0751(2) 19_655 ?
Sb2 Te3 3.0751(2) . ?
