#------------------------------------------------------------------------------
#$Date: 2024-10-06 15:22:31 +0200 (Sun 06 de Oct de 2024) $
#$Revision: 295357 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/28/1572812.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_1572812
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         'Ag0.61 Pb1.79 Sb2.61 Se6'
_chemical_formula_sum            'Ag0.61 Pb1.79 Sb2.61 Se6'
_chemical_formula_weight         1226.96
_chemical_name_common            'silver lead antimony selenide'
_chemical_name_systematic        'silver lead antimony selenide'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_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                90
_cell_formula_units_Z            4
_cell_length_a                   4.2118(1)
_cell_length_b                   13.859(1)
_cell_length_c                   20.862(1)
_cell_measurement_reflns_used    2806
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.5730
_cell_measurement_theta_min      2.7450
_cell_volume                     1217.74(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.995
_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     0.5001
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9589
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        17.461
_diffrn_reflns_theta_max         22.618
_diffrn_reflns_theta_min         2.179
_diffrn_source                   'DESY PetraIII P24'
_exptl_absorpt_coefficient_mu    19.408
_exptl_absorpt_correction_T_max  0.7599
_exptl_absorpt_correction_T_min  0.4754
_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    6.692
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.746
_refine_diff_density_min         -2.632
_refine_diff_density_rms         0.312
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.349
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         1325
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.348
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0313P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0991
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1160
_reflns_number_total             1325
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Ag0.61Pb1.79Sb2.61Se6_FINAL.cif
_cod_data_source_block           Ag0.61Pb1.79Sb2.61Se6
_cod_database_code               1572812
_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'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
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 0.000000 0.81198(4) 0.250000 0.05015(17) Uani 1 4 d S T P . .
Sb2 Sb 0.000000 0.36267(3) 0.05046(3) 0.03887(16) Uani 0.6849(9) 2 d S T P . .
Pb2 Pb 0.000000 0.36267(3) 0.05046(3) 0.03887(16) Uani 0.2610(13) 2 d S T P . .
Ag2 Ag 0.000000 0.36267(3) 0.05046(3) 0.03887(16) Uani 0.0542(12) 2 d S T P . .
Sb3 Sb 0.000000 0.08599(4) 0.13111(3) 0.03991(17) Uani 0.6179(9) 2 d S T P . .
Pb3 Pb 0.000000 0.08599(4) 0.13111(3) 0.03991(17) Uani 0.1336(13) 2 d S T P . .
Ag3 Ag 0.000000 0.08599(4) 0.13111(3) 0.03991(17) Uani 0.2486(12) 2 d S T P . .
Se4 Se 0.000000 0.45716(5) 0.16526(4) 0.03065(17) Uani 1 2 d S T P . .
Se5 Se 0.000000 0.16678(8) 0.250000 0.0366(2) Uani 1 4 d S T P . .
Se6 Se 0.000000 0.25856(6) 0.59909(4) 0.03623(19) Uani 1 2 d S T P . .
Se7 Se 0.000000 0.000000 0.000000 0.0404(3) Uani 1 4 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
Pb Pb -0.7066 5.7775 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -1.3531 0.8253 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -2.9138 0.5843 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se 0.2909 1.2188 '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
Se5 Pb1 Se5 92.60(4) 5_455 5 ?
Se5 Pb1 Se6 78.178(13) 5_455 2_564 ?
Se5 Pb1 Se6 78.178(13) 5 2_564 ?
Se5 Pb1 Se6 78.178(13) 5_455 9_566 ?
Se5 Pb1 Se6 78.178(13) 5 9_566 ?
Se6 Pb1 Se6 145.50(3) 2_564 9_566 ?
Se5 Pb1 Se4 148.746(12) 5_455 14_556 ?
Se5 Pb1 Se4 87.771(16) 5 14_556 ?
Se6 Pb1 Se4 132.115(14) 2_564 14_556 ?
Se6 Pb1 Se4 71.314(17) 9_566 14_556 ?
Se5 Pb1 Se4 148.746(12) 5_455 5 ?
Se5 Pb1 Se4 87.771(16) 5 5 ?
Se6 Pb1 Se4 71.314(17) 2_564 5 ?
Se6 Pb1 Se4 132.115(14) 9_566 5 ?
Se4 Pb1 Se4 62.51(2) 14_556 5 ?
Se5 Pb1 Se4 87.771(16) 5_455 5_455 ?
Se5 Pb1 Se4 148.746(12) 5 5_455 ?
Se6 Pb1 Se4 71.314(17) 2_564 5_455 ?
Se6 Pb1 Se4 132.115(14) 9_566 5_455 ?
Se4 Pb1 Se4 107.61(3) 14_556 5_455 ?
Se4 Pb1 Se4 76.356(18) 5 5_455 ?
Se5 Pb1 Se4 87.771(16) 5_455 14_456 ?
Se5 Pb1 Se4 148.746(12) 5 14_456 ?
Se6 Pb1 Se4 132.115(14) 2_564 14_456 ?
Se6 Pb1 Se4 71.314(17) 9_566 14_456 ?
Se4 Pb1 Se4 76.356(18) 14_556 14_456 ?
Se4 Pb1 Se4 107.61(3) 5 14_456 ?
Se4 Pb1 Se4 62.51(2) 5_455 14_456 ?
Se4 Sb2 Se6 88.33(2) . 6_454 ?
Se4 Sb2 Se6 88.33(2) . 6_554 ?
Se6 Sb2 Se6 94.03(3) 6_454 6_554 ?
Se4 Sb2 Se7 90.202(16) . 5 ?
Se6 Sb2 Se7 176.689(19) 6_454 5 ?
Se6 Sb2 Se7 88.888(12) 6_554 5 ?
Se4 Sb2 Se7 90.202(16) . 5_455 ?
Se6 Sb2 Se7 88.888(12) 6_454 5_455 ?
Se6 Sb2 Se7 176.689(19) 6_554 5_455 ?
Se7 Sb2 Se7 88.152(13) 5 5_455 ?
Se4 Sb2 Se6 176.15(3) . 10_556 ?
Se6 Sb2 Se6 94.29(2) 6_454 10_556 ?
Se6 Sb2 Se6 94.29(2) 6_554 10_556 ?
Se7 Sb2 Se6 87.035(15) 5 10_556 ?
Se7 Sb2 Se6 87.035(15) 5_455 10_556 ?
Se5 Sb3 Se4 91.71(3) . 5_445 ?
Se5 Sb3 Se4 91.71(3) . 5_545 ?
Se4 Sb3 Se4 95.21(3) 5_445 5_545 ?
Se5 Sb3 Se7 179.25(3) . . ?
Se4 Sb3 Se7 88.80(2) 5_445 . ?
Se4 Sb3 Se7 88.80(2) 5_545 . ?
Se5 Sb3 Se6 84.84(3) . 6_554 ?
Se4 Sb3 Se6 174.43(3) 5_445 6_554 ?
Se4 Sb3 Se6 89.270(15) 5_545 6_554 ?
Se7 Sb3 Se6 94.61(2) . 6_554 ?
Se5 Sb3 Se6 84.84(3) . 6_454 ?
Se4 Sb3 Se6 89.270(15) 5_445 6_454 ?
Se4 Sb3 Se6 174.43(3) 5_545 6_454 ?
Se7 Sb3 Se6 94.61(2) . 6_454 ?
Se6 Sb3 Se6 86.07(2) 6_554 6_454 ?
Sb2 Se4 Sb3 94.65(2) . 5 ?
Sb2 Se4 Sb3 94.65(2) . 5_455 ?
Sb3 Se4 Sb3 95.21(3) 5 5_455 ?
Sb2 Se4 Pb1 99.90(2) . 5_445 ?
Sb3 Se4 Pb1 162.93(3) 5 5_445 ?
Sb3 Se4 Pb1 92.464(12) 5_455 5_445 ?
Sb2 Se4 Pb1 99.90(2) . 5_545 ?
Sb3 Se4 Pb1 92.464(11) 5 5_545 ?
Sb3 Se4 Pb1 162.93(3) 5_455 5_545 ?
Pb1 Se4 Pb1 76.354(18) 5_445 5_545 ?
Sb3 Se5 Sb3 131.41(5) . 10_556 ?
Sb3 Se5 Pb1 106.512(13) . 5_545 ?
Sb3 Se5 Pb1 106.512(12) 10_556 5_545 ?
Sb3 Se5 Pb1 106.512(13) . 5_445 ?
Sb3 Se5 Pb1 106.512(12) 10_556 5_445 ?
Pb1 Se5 Pb1 92.60(4) 5_545 5_445 ?
Sb2 Se6 Sb2 94.03(3) 6_455 6 ?
Sb2 Se6 Sb3 169.42(3) 6_455 6 ?
Sb2 Se6 Sb3 89.112(11) 6 6 ?
Sb2 Se6 Sb3 89.112(11) 6_455 6_455 ?
Sb2 Se6 Sb3 169.42(3) 6 6_455 ?
Sb3 Se6 Sb3 86.07(2) 6 6_455 ?
Sb2 Se6 Pb1 99.41(2) 6_455 9_566 ?
Sb2 Se6 Pb1 99.41(2) 6 9_566 ?
Sb3 Se6 Pb1 90.02(2) 6 9_566 ?
Sb3 Se6 Pb1 90.02(2) 6_455 9_566 ?
Sb2 Se6 Sb2 85.70(2) 6_455 10_556 ?
Sb2 Se6 Sb2 85.70(2) 6 10_556 ?
Sb3 Se6 Sb2 84.46(2) 6 10_556 ?
Sb3 Se6 Sb2 84.46(2) 6_455 10_556 ?
Pb1 Se6 Sb2 172.43(3) 9_566 10_556 ?
Sb3 Se7 Sb3 180.0 9 . ?
Sb3 Se7 Sb2 93.879(13) 9 5_445 ?
Sb3 Se7 Sb2 86.121(13) . 5_445 ?
Sb3 Se7 Sb2 86.121(13) 9 13 ?
Sb3 Se7 Sb2 93.879(13) . 13 ?
Sb2 Se7 Sb2 180.00(2) 5_445 13 ?
Sb3 Se7 Sb2 93.880(13) 9 5_545 ?
Sb3 Se7 Sb2 86.121(13) . 5_545 ?
Sb2 Se7 Sb2 88.151(13) 5_445 5_545 ?
Sb2 Se7 Sb2 91.849(13) 13 5_545 ?
Sb3 Se7 Sb2 86.120(13) 9 13_455 ?
Sb3 Se7 Sb2 93.879(13) . 13_455 ?
Sb2 Se7 Sb2 91.849(13) 5_445 13_455 ?
Sb2 Se7 Sb2 88.151(13) 13 13_455 ?
Sb2 Se7 Sb2 180.00(2) 5_545 13_455 ?
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 Se5 2.9128(9) 5_455 ?
Pb1 Se5 2.9128(9) 5 ?
Pb1 Se6 3.2966(9) 2_564 ?
Pb1 Se6 3.2966(9) 9_566 ?
Pb1 Se4 3.4070(7) 14_556 ?
Pb1 Se4 3.4070(7) 5 ?
Pb1 Se4 3.4070(7) 5_455 ?
Pb1 Se4 3.4070(7) 14_456 ?
Sb2 Se4 2.7296(9) . ?
Sb2 Se6 2.8787(6) 6_454 ?
Sb2 Se6 2.8787(6) 6_554 ?
Sb2 Se7 3.0274(3) 5 ?
Sb2 Se7 3.0274(3) 5_455 ?
Sb2 Se6 3.4374(10) 10_556 ?
Sb3 Se5 2.7213(8) . ?
Sb3 Se4 2.8515(6) 5_445 ?
Sb3 Se4 2.8515(6) 5_545 ?
Sb3 Se7 2.9835(6) . ?
Sb3 Se6 3.0858(7) 6_554 ?
Sb3 Se6 3.0858(7) 6_454 ?
