#------------------------------------------------------------------------------
#$Date: 2026-04-18 01:17:08 +0200 (Sat, 18 Apr 2026) $
#$Revision: 305577 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/7/72/08/7720886.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_7720886
loop_
_publ_author_name
'Huang, Yen-Han'
'Chen, Guan-Ruei'
'Lee, Chi-Shen'
_publ_section_title
;
 Layered Mixed-Anion Chalcohalides Pb4Sb4Q9Cl2 (Q = S, Se): Puckered 2D
 Frameworks, Indirect Band Gaps, and Low Thermal Conductivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D6DT00115G
_journal_year                    2026
_chemical_formula_sum            'Cl2 Pb4 S9 Sb4'
_chemical_formula_weight         1675.20
_chemical_melting_point          793
_chemical_name_systematic        Pb4Sb4S9Cl2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           55
_space_group_name_Hall           '-P 2 2ab'
_space_group_name_H-M_alt        'P b a m'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.25505/fiz.icsd.cc2qd1v1
_audit_update_record
;
2026-03-19 deposited with the CCDC.	2026-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.0310(17)
_cell_length_b                   15.5373(16)
_cell_length_c                   4.0769(4)
_cell_measurement_reflns_used    1106
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.95
_cell_volume                     952.12(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'profile data from phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            6507
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.95
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Bruker Mo microfocus source'
_exptl_absorpt_coefficient_mu    42.058
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            grey-black
_exptl_crystal_density_diffrn    5.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1420
_exptl_crystal_recrystallization_method 'Solid State Reaction'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.118
_refine_diff_density_min         -2.352
_refine_ls_extinction_coef       0.0022(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.269
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0822P)²+9.7005P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                1033
_reflns_number_total             1106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d6dt00115g2.cif
_cod_data_source_block           I
_cod_database_code               7720886
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb Pb1 0.87258(5) 0.06986(4) 0.5 0.0220(3) Uani d S 1 . .
Pb Pb2 0.75966(4) 0.31819(4) 0.5 0.0193(3) Uani d S 1 . .
Sb Sb1 1.00491(9) 0.27249(9) 0.0559(10) 0.0276(12) Uani d P 0.5 . .
Sb Sb2 0.87681(9) 0.51828(10) 0.0584(8) 0.0267(10) Uani d P 0.5 . .
S S1 0.7307(2) 0.4497(2) 0 0.0140(7) Uani d S 1 . .
S S2 0.8557(3) 0.2078(2) 0 0.0131(7) Uani d S 1 . .
S S3 0.9299(3) 0.3957(3) 0.5 0.0235(9) Uani d SP 0.93 . .
Cl Cl2 0.9299(3) 0.3957(3) 0.5 0.0235(9) Uani d SP 0.07 . .
S S4 0.6809(3) 0.1218(3) 0.5 0.0222(8) Uani d SP 0.87 . .
Cl Cl3 0.6809(3) 0.1218(3) 0.5 0.0222(8) Uani d SP 0.13 . .
S S5 0.5496(3) 0.3298(3) 0.5 0.0275(10) Uani d SP 0.75 . .
Cl Cl4 0.5496(3) 0.3298(3) 0.5 0.0275(10) Uani d SP 0.25 . .
Cl Cl1 1.0 0 0 0.0224(12) Uani d S 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 Pb1 S2 1_556 . 86.71(9) ?
S2 Pb1 S4 1_556 . 73.91(9) ?
S2 Pb1 S4 . . 73.91(9) ?
S2 Pb1 Cl1 1_556 1_556 81.33(6) ?
S2 Pb1 Cl1 . 1_556 141.46(8) ?
S4 Pb1 Cl1 . 1_556 135.42(2) ?
S2 Pb1 Cl1 1_556 . 141.46(8) ?
S2 Pb1 Cl1 . . 81.33(6) ?
S4 Pb1 Cl1 . . 135.42(2) ?
Cl1 Pb1 Cl1 1_556 . 85.596(19) ?
S2 Pb1 S5 1_556 7_665 73.06(9) ?
S2 Pb1 S5 . 7_665 73.06(9) ?
S4 Pb1 S5 . 7_665 133.97(11) ?
Cl1 Pb1 S5 1_556 7_665 68.42(6) ?
Cl1 Pb1 S5 . 7_665 68.42(6) ?
S2 Pb1 Cl4 1_556 7_665 73.06(9) ?
S2 Pb1 Cl4 . 7_665 73.06(9) ?
S4 Pb1 Cl4 . 7_665 133.97(11) ?
Cl1 Pb1 Cl4 1_556 7_665 68.42(6) ?
Cl1 Pb1 Cl4 . 7_665 68.42(6) ?
S5 Pb1 Cl4 7_665 7_665 0.00(15) ?
S3 Pb2 S1 . 1_556 80.60(10) ?
S3 Pb2 S1 . . 80.60(10) ?
S1 Pb2 S1 1_556 . 88.61(11) ?
S3 Pb2 S2 . 1_556 79.04(10) ?
S1 Pb2 S2 1_556 1_556 89.84(7) ?
S1 Pb2 S2 . 1_556 159.57(11) ?
S3 Pb2 S2 . . 79.04(10) ?
S1 Pb2 S2 1_556 . 159.56(11) ?
S1 Pb2 S2 . . 89.84(7) ?
S2 Pb2 S2 1_556 . 84.57(9) ?
Sb1 Sb1 S2 6 . 84.70(9) ?
Sb1 Sb1 Cl4 6 7_665 136.39(10) ?
S2 Sb1 Cl4 . 7_665 93.01(14) ?
Sb1 Sb1 S5 6 7_665 136.39(10) ?
S2 Sb1 S5 . 7_665 93.01(14) ?
Cl4 Sb1 S5 7_665 7_665 0.00(15) ?
Sb1 Sb1 Cl4 6 7_664 37.28(9) ?
S2 Sb1 Cl4 . 7_664 85.06(13) ?
Cl4 Sb1 Cl4 7_665 7_664 99.11(15) ?
S5 Sb1 Cl4 7_665 7_664 99.11(15) ?
Sb1 Sb1 S5 6 7_664 37.28(9) ?
S2 Sb1 S5 . 7_664 85.06(13) ?
Cl4 Sb1 S5 7_665 7_664 99.11(15) ?
S5 Sb1 S5 7_665 7_664 99.11(15) ?
Cl4 Sb1 S5 7_664 7_664 0.00(14) ?
Sb1 Sb1 S3 6 . 129.18(9) ?
S2 Sb1 S3 . . 88.45(12) ?
Cl4 Sb1 S3 7_665 . 94.17(16) ?
S5 Sb1 S3 7_665 . 94.17(16) ?
Cl4 Sb1 S3 7_664 . 165.49(15) ?
S5 Sb1 S3 7_664 . 165.49(15) ?
Sb2 Sb2 S1 6 . 84.43(7) ?
Sb2 Sb2 Cl3 6 3_656 134.56(9) ?
S1 Sb2 Cl3 . 3_656 92.17(13) ?
Sb2 Sb2 S4 6 3_656 134.56(9) ?
S1 Sb2 S4 . 3_656 92.17(13) ?
Cl3 Sb2 S4 3_656 3_656 0.00(17) ?
Sb2 Sb2 S3 6 . 131.09(8) ?
S1 Sb2 S3 . . 91.30(12) ?
Cl3 Sb2 S3 3_656 . 94.20(14) ?
S4 Sb2 S3 3_656 . 94.20(14) ?
Sb2 Sb2 S4 6 3_655 38.77(8) ?
S1 Sb2 S4 . 3_655 84.13(12) ?
Cl3 Sb2 S4 3_656 3_655 95.80(13) ?
S4 Sb2 S4 3_656 3_655 95.80(13) ?
S3 Sb2 S4 . 3_655 169.15(14) ?
Sb2 S1 Sb2 6 . 11.14(15) ?
Sb2 S1 Pb2 6 1_554 95.91(11) ?
Sb2 S1 Pb2 . 1_554 103.80(13) ?
Sb2 S1 Pb2 6 . 103.80(13) ?
Sb2 S1 Pb2 . . 95.91(11) ?
Pb2 S1 Pb2 1_554 . 88.61(11) ?
Sb1 S2 Sb1 6 . 10.59(19) ?
Sb1 S2 Pb1 6 . 106.24(13) ?
Sb1 S2 Pb1 . . 98.80(12) ?
Sb1 S2 Pb1 6 1_554 98.80(12) ?
Sb1 S2 Pb1 . 1_554 106.24(13) ?
Pb1 S2 Pb1 . 1_554 86.71(9) ?
Sb1 S2 Pb2 6 1_554 98.08(11) ?
Sb1 S2 Pb2 . 1_554 105.36(13) ?
Pb1 S2 Pb2 . 1_554 155.67(14) ?
Pb1 S2 Pb2 1_554 1_554 89.28(3) ?
Sb1 S2 Pb2 6 . 105.36(13) ?
Sb1 S2 Pb2 . . 98.08(11) ?
Pb1 S2 Pb2 . . 89.28(3) ?
Pb1 S2 Pb2 1_554 . 155.67(14) ?
Pb2 S2 Pb2 1_554 . 84.57(9) ?
Sb2 S3 Sb2 6_556 . 82.18(17) ?
Sb2 S3 Pb2 6_556 . 91.85(12) ?
Sb2 S3 Pb2 . . 91.85(12) ?
Sb2 S3 Sb1 6_556 . 173.80(17) ?
Sb2 S3 Sb1 . . 99.43(9) ?
Pb2 S3 Sb1 . . 94.08(11) ?
Sb2 S3 Sb1 6_556 6_556 99.43(9) ?
Sb2 S3 Sb1 . 6_556 173.80(17) ?
Pb2 S3 Sb1 . 6_556 94.08(11) ?
Sb1 S3 Sb1 . 6_556 78.35(18) ?
Sb2 S4 Sb2 8_755 3_646 89.12(17) ?
Sb2 S4 Sb2 8_755 3_645 6.67(9) ?
Sb2 S4 Sb2 3_646 3_645 95.80(13) ?
Sb2 S4 Sb2 8_755 8_756 95.80(13) ?
Sb2 S4 Sb2 3_646 8_756 6.67(9) ?
Sb2 S4 Sb2 3_645 8_756 102.47(16) ?
Sb2 S4 Pb1 8_755 . 99.00(11) ?
Sb2 S4 Pb1 3_646 . 99.00(11) ?
Sb2 S4 Pb1 3_645 . 97.90(10) ?
Sb2 S4 Pb1 8_756 . 97.90(10) ?
Sb1 S5 Sb1 7_565 4_456 92.8(2) ?
Sb1 S5 Sb1 7_565 4_455 6.33(11) ?
Sb1 S5 Sb1 4_456 4_455 99.11(15) ?
Sb1 S5 Sb1 7_565 7_566 99.11(15) ?
Sb1 S5 Sb1 4_456 7_566 6.33(11) ?
Sb1 S5 Sb1 4_455 7_566 105.44(18) ?
Sb1 S5 Pb1 7_565 7_565 95.13(12) ?
Sb1 S5 Pb1 4_456 7_565 95.13(12) ?
Sb1 S5 Pb1 4_455 7_565 94.50(11) ?
Sb1 S5 Pb1 7_566 7_565 94.50(11) ?
Pb1 Cl1 Pb1 5_756 1_554 180.00(3) ?
Pb1 Cl1 Pb1 5_756 5_755 85.597(18) ?
Pb1 Cl1 Pb1 1_554 5_755 94.403(19) ?
Pb1 Cl1 Pb1 5_756 . 94.403(19) ?
Pb1 Cl1 Pb1 1_554 . 85.597(19) ?
Pb1 Cl1 Pb1 5_755 . 180.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 S2 1_556 2.969(3) ?
Pb1 S2 . 2.969(3) ?
Pb1 S4 . 2.992(4) ?
Pb1 Cl1 1_556 3.0003(5) ?
Pb1 Cl1 . 3.0003(5) ?
Pb1 S5 7_665 3.084(4) ?
Pb1 Cl4 7_665 3.084(4) ?
Pb2 S3 . 2.829(4) ?
Pb2 S1 1_556 2.918(3) ?
Pb2 S1 . 2.918(3) ?
Pb2 S2 1_556 3.030(3) ?
Pb2 S2 . 3.030(3) ?
Sb1 Sb1 6 0.456(8) ?
Sb1 S2 . 2.468(4) ?
Sb1 Cl4 7_665 2.501(4) ?
Sb1 S5 7_665 2.501(4) ?
Sb1 Cl4 7_664 2.848(4) ?
Sb1 S5 7_664 2.848(4) ?
Sb1 S3 . 2.866(5) ?
Sb2 Sb2 6 0.476(6) ?
Sb2 S1 . 2.453(4) ?
Sb2 Cl3 3_656 2.566(4) ?
Sb2 S4 3_656 2.566(4) ?
Sb2 S3 . 2.739(4) ?
Sb2 S4 3_655 2.920(4) ?
S1 Sb2 6 2.453(4) ?
S1 Pb2 1_554 2.918(3) ?
S2 Sb1 6 2.468(4) ?
S2 Pb1 1_554 2.969(3) ?
S2 Pb2 1_554 3.030(3) ?
S3 Sb2 6_556 2.739(4) ?
S3 Sb1 6_556 2.866(5) ?
S4 Sb2 8_755 2.566(4) ?
S4 Sb2 3_646 2.566(4) ?
S4 Sb2 3_645 2.920(4) ?
S4 Sb2 8_756 2.920(4) ?
S5 Sb1 7_565 2.501(4) ?
S5 Sb1 4_456 2.501(4) ?
S5 Sb1 4_455 2.848(4) ?
S5 Sb1 7_566 2.848(4) ?
S5 Pb1 7_565 3.084(4) ?
Cl1 Pb1 5_756 3.0003(5) ?
Cl1 Pb1 1_554 3.0003(5) ?
Cl1 Pb1 5_755 3.0003(5) ?
