# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_I
_audit_block_doi                 10.25505/fiz.icsd.cc2qd1v1
_database_code_depnum_ccdc_archive 'CCDC 2514033'
loop_
_audit_author_name
_audit_author_address
'Chi-Shen Lee'
;National Yang Ming Chiao Tung University
Taiwan
;
_audit_update_record             
;
2026-03-19 deposited with the CCDC.	2026-04-14 downloaded from the CCDC.
;
_chemical_name_systematic        Pb4Sb4S9Cl2
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cl2 Pb4 S9 Sb4'
_chemical_formula_iupac          ?
_chemical_formula_weight         1675.20

_chemical_melting_point          793

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P b a m'
_space_group_name_Hall           '-P 2 2ab'
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'

_cell_length_a                   15.0310(17)
_cell_length_b                   15.5373(16)
_cell_length_c                   4.0769(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     952.12(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1106
_cell_measurement_theta_min      2.95
_cell_measurement_theta_max      26.36
_cell_measurement_temperature    296.(2)

_exptl_crystal_description       needle
_exptl_crystal_colour            grey-black
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    5.843
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1420

_exptl_absorpt_coefficient_mu    42.058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_T_max  0.74

_exptl_special_details           
;
;

_diffrn_ambient_temperature      296.(2)

_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Bruker Mo microfocus source'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'profile data from phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            6507
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       5

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_reflns_number_total             1106
_reflns_number_gt                1033
_reflns_threshold_expression     >2sigma(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1371
_refine_ls_goodness_of_fit_ref   1.269
_refine_ls_restrained_S_all      1.269
_refine_ls_number_reflns         1106
_refine_ls_number_parameters     66
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    ?
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0822P)²+9.7005P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   ?
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         4.118
_refine_diff_density_min         -2.352
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0022(3)

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'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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 . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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) ?

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 ?

_exptl_crystal_recrystallization_method 'Solid State Reaction'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_I_CCDC1
_audit_block_doi                 10.25505/fiz.icsd.cc2qd1x3
_database_code_depnum_ccdc_archive 'CCDC 2514035'
loop_
_audit_author_name
_audit_author_address
'Chi-Shen Lee'
;National Yang Ming Chiao Tung University
Taiwan
;
_audit_update_record             
;
2026-03-19 deposited with the CCDC.	2026-04-14 downloaded from the CCDC.
;
_chemical_name_systematic        Pb4Sb4Se9Cl2
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cl2 Pb4 Sb4 Se9'
_chemical_formula_iupac          ?
_chemical_formula_weight         2097.30

_chemical_melting_point          793

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P b a m'
_space_group_name_Hall           '-P 2 2ab'
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'

_cell_length_a                   15.398(6)
_cell_length_b                   16.093(7)
_cell_length_c                   4.1760(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1034.8(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1044
_cell_measurement_theta_min      1.83
_cell_measurement_theta_max      25.02
_cell_measurement_temperature    296.(2)

_exptl_crystal_description       needle
_exptl_crystal_colour            grey-black
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    6.731
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744

_exptl_absorpt_coefficient_mu    53.618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_T_max  0.75

_exptl_special_details           
;
;

_diffrn_ambient_temperature      296.(2)

_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Bruker Mo microfocus source'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'profile data from phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            4700
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       4

_refine_special_details          
;
Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_reflns_number_total             1044
_reflns_number_gt                894
_reflns_threshold_expression     >2sigma(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1144
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_restrained_S_all      1.182
_refine_ls_number_reflns         1044
_refine_ls_number_parameters     69
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    ?
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0548P)²+35.7087P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   ?
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         2.936
_refine_diff_density_min         -3.290
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00106(14)

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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 0.73606(7) -0.18012(6) 0.5 0.0301(3) Uani d S 1 . .
Pb Pb2 0.87686(7) 0.07052(5) 0.5 0.0286(3) Uani d S 1 . .
Sb Sb1 0.62110(13) 0.02087(12) -0.046(3) 0.027(2) Uani d P 0.5 . .
Sb Sb2 0.48677(12) -0.22966(12) -0.041(4) 0.025(3) Uani d P 0.5 . .
Se Se1 0.77168(13) -0.05222(12) 0 0.0169(5) Uani d S 1 . .
Se Se2 0.64225(13) -0.29328(12) 0 0.0150(5) Uani d S 1 . .
Se Se3 0.56487(14) -0.10331(14) 0.5 0.0203(5) Uani d SP 0.93 . .
Cl Cl2 0.56487(14) -0.10331(14) 0.5 0.0203(5) Uani d SP 0.07 . .
Se Se4 0.94311(15) -0.16588(14) 0.5 0.0213(6) Uani d SP 0.87 . .
Cl Cl3 0.94311(15) -0.16588(14) 0.5 0.0213(6) Uani d SP 0.13 . .
Se Se5 0.68398(16) 0.12298(15) 0.5 0.0223(6) Uani d SP 0.75 . .
Cl Cl4 0.68398(16) 0.12298(15) 0.5 0.0223(6) Uani d SP 0.25 . .
Cl Cl1 0 0 0 0.0215(16) Uani d S 1 . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix.  The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.  An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 Se3 . 2.911(3) ?
Pb1 Se1 1_556 2.9828(18) ?
Pb1 Se1 . 2.9828(18) ?
Pb1 Se2 1_556 3.1245(18) ?
Pb1 Se2 . 3.1245(18) ?
Pb1 Se4 . 3.197(3) ?
Pb2 Cl1 1_656 3.0402(11) ?
Pb2 Cl1 1_655 3.0402(11) ?
Pb2 Se2 3_656 3.0416(18) ?
Pb2 Se2 3_655 3.0416(18) ?
Pb2 Se5 . 3.088(3) ?
Pb2 Se4 5_756 3.169(3) ?
Sb1 Sb1 6 0.38(3) ?
Sb1 Se1 . 2.607(3) ?
Sb1 Cl4 1_554 2.690(10) ?
Sb1 Se5 1_554 2.690(10) ?
Sb1 Se3 1_554 2.889(9) ?
Sb1 Cl2 1_554 2.889(9) ?
Sb1 Se5 . 2.971(10) ?
Sb2 Sb2 6 0.34(3) ?
Sb2 Se2 . 2.609(3) ?
Sb2 Cl3 7_554 2.636(12) ?
Sb2 Se4 7_554 2.636(12) ?
Sb2 Cl3 7 2.896(13) ?
Sb2 Se4 7 2.896(13) ?
Sb2 Se3 1_554 3.042(10) ?
Se1 Sb1 6 2.607(3) ?
Se1 Pb1 1_554 2.9828(18) ?
Se2 Sb2 6 2.609(3) ?
Se2 Pb2 3_645 3.0415(18) ?
Se2 Pb2 3_646 3.0415(18) ?
Se2 Pb1 1_554 3.1245(18) ?
Se3 Sb1 1_556 2.889(9) ?
Se3 Sb1 6 2.889(9) ?
Se3 Sb2 6 3.042(10) ?
Se3 Sb2 1_556 3.042(10) ?
Se4 Sb2 4_545 2.636(12) ?
Se4 Sb2 7_656 2.636(12) ?
Se4 Sb2 7_655 2.896(13) ?
Se4 Sb2 4_546 2.896(13) ?
Se4 Pb2 5_756 3.168(3) ?
Se5 Sb1 6 2.690(10) ?
Se5 Sb1 1_556 2.690(10) ?
Se5 Sb1 6_556 2.971(10) ?
Cl1 Pb2 5_656 3.0402(11) ?
Cl1 Pb2 1_454 3.0402(11) ?
Cl1 Pb2 1_455 3.0402(11) ?
Cl1 Pb2 5_655 3.0402(11) ?

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
Se3 Pb1 Se1 . 1_556 82.73(6) ?
Se3 Pb1 Se1 . . 82.73(6) ?
Se1 Pb1 Se1 1_556 . 88.86(7) ?
Se3 Pb1 Se2 . 1_556 80.15(6) ?
Se1 Pb1 Se2 1_556 1_556 91.11(5) ?
Se1 Pb1 Se2 . 1_556 162.74(7) ?
Se3 Pb1 Se2 . . 80.15(6) ?
Se1 Pb1 Se2 1_556 . 162.74(7) ?
Se1 Pb1 Se2 . . 91.11(5) ?
Se2 Pb1 Se2 1_556 . 83.87(6) ?
Se3 Pb1 Se4 . . 150.77(7) ?
Se1 Pb1 Se4 1_556 . 76.53(5) ?
Se1 Pb1 Se4 . . 76.53(5) ?
Se2 Pb1 Se4 1_556 . 120.19(5) ?
Se2 Pb1 Se4 . . 120.19(5) ?
Cl1 Pb2 Cl1 1_656 1_655 86.75(4) ?
Cl1 Pb2 Se2 1_656 3_656 81.83(4) ?
Cl1 Pb2 Se2 1_655 3_656 143.21(5) ?
Cl1 Pb2 Se2 1_656 3_655 143.21(5) ?
Cl1 Pb2 Se2 1_655 3_655 81.83(4) ?
Se2 Pb2 Se2 3_656 3_655 86.71(7) ?
Cl1 Pb2 Se5 1_656 . 134.59(3) ?
Cl1 Pb2 Se5 1_655 . 134.59(3) ?
Se2 Pb2 Se5 3_656 . 73.14(5) ?
Se2 Pb2 Se5 3_655 . 73.14(5) ?
Cl1 Pb2 Se4 1_656 5_756 68.60(4) ?
Cl1 Pb2 Se4 1_655 5_756 68.60(4) ?
Se2 Pb2 Se4 3_656 5_756 74.67(5) ?
Se2 Pb2 Se4 3_655 5_756 74.67(5) ?
Se5 Pb2 Se4 . 5_756 135.16(7) ?
Sb1 Sb1 Se1 6 . 85.8(3) ?
Sb1 Sb1 Cl4 6 1_554 134.8(2) ?
Se1 Sb1 Cl4 . 1_554 90.4(2) ?
Sb1 Sb1 Se5 6 1_554 134.8(2) ?
Se1 Sb1 Se5 . 1_554 90.4(2) ?
Cl4 Sb1 Se5 1_554 1_554 0.00(13) ?
Sb1 Sb1 Se3 6 1_554 131.1(2) ?
Se1 Sb1 Se3 . 1_554 90.14(18) ?
Cl4 Sb1 Se3 1_554 1_554 93.8(4) ?
Se5 Sb1 Se3 1_554 1_554 93.8(4) ?
Sb1 Sb1 Cl2 6 1_554 131.1(2) ?
Se1 Sb1 Cl2 . 1_554 90.14(18) ?
Cl4 Sb1 Cl2 1_554 1_554 93.8(4) ?
Se5 Sb1 Cl2 1_554 1_554 93.8(4) ?
Se3 Sb1 Cl2 1_554 1_554 0.00(11) ?
Sb1 Sb1 Se5 6 . 39.93(17) ?
Se1 Sb1 Se5 . . 84.5(2) ?
Cl4 Sb1 Se5 1_554 . 94.92(10) ?
Se5 Sb1 Se5 1_554 . 94.92(10) ?
Se3 Sb1 Se5 1_554 . 169.7(3) ?
Cl2 Sb1 Se5 1_554 . 169.7(3) ?
Sb2 Sb2 Se2 6 . 86.2(4) ?
Sb2 Sb2 Cl3 6 7_554 136.6(2) ?
Se2 Sb2 Cl3 . 7_554 91.8(3) ?
Sb2 Sb2 Se4 6 7_554 136.6(2) ?
Se2 Sb2 Se4 . 7_554 91.8(3) ?
Cl3 Sb2 Se4 7_554 7_554 0.00(7) ?
Sb2 Sb2 Cl3 6 7 38.7(2) ?
Se2 Sb2 Cl3 . 7 86.2(3) ?
Cl3 Sb2 Cl3 7_554 7 97.92(10) ?
Se4 Sb2 Cl3 7_554 7 97.92(10) ?
Sb2 Sb2 Se4 6 7 38.7(2) ?
Se2 Sb2 Se4 . 7 86.2(3) ?
Cl3 Sb2 Se4 7_554 7 97.92(10) ?
Se4 Sb2 Se4 7_554 7 97.92(10) ?
Cl3 Sb2 Se4 7 7 0.00(7) ?
Sb2 Sb2 Se3 6 1_554 129.1(3) ?
Se2 Sb2 Se3 . 1_554 86.6(2) ?
Cl3 Sb2 Se3 7_554 1_554 94.0(5) ?
Se4 Sb2 Se3 7_554 1_554 94.0(5) ?
Cl3 Sb2 Se3 7 1_554 166.3(4) ?
Se4 Sb2 Se3 7 1_554 166.3(4) ?
Sb1 Se1 Sb1 . 6 8.4(6) ?
Sb1 Se1 Pb1 . . 101.5(2) ?
Sb1 Se1 Pb1 6 . 95.5(2) ?
Sb1 Se1 Pb1 . 1_554 95.5(2) ?
Sb1 Se1 Pb1 6 1_554 101.5(2) ?
Pb1 Se1 Pb1 . 1_554 88.86(7) ?
Sb2 Se2 Sb2 6 . 7.6(7) ?
Sb2 Se2 Pb2 6 3_645 103.8(3) ?
Sb2 Se2 Pb2 . 3_645 98.6(3) ?
Sb2 Se2 Pb2 6 3_646 98.6(3) ?
Sb2 Se2 Pb2 . 3_646 103.8(3) ?
Pb2 Se2 Pb2 3_645 3_646 86.71(7) ?
Sb2 Se2 Pb1 6 1_554 103.9(3) ?
Sb2 Se2 Pb1 . 1_554 98.7(3) ?
Pb2 Se2 Pb1 3_645 1_554 90.34(4) ?
Pb2 Se2 Pb1 3_646 1_554 157.44(8) ?
Sb2 Se2 Pb1 6 . 98.7(3) ?
Sb2 Se2 Pb1 . . 103.9(3) ?
Pb2 Se2 Pb1 3_645 . 157.44(8) ?
Pb2 Se2 Pb1 3_646 . 90.34(4) ?
Pb1 Se2 Pb1 1_554 . 83.87(6) ?
Sb1 Se3 Sb1 1_556 6 82.1(4) ?
Sb1 Se3 Pb1 1_556 . 91.28(7) ?
Sb1 Se3 Pb1 6 . 91.28(7) ?
Sb1 Se3 Sb2 1_556 6 174.15(14) ?
Sb1 Se3 Sb2 6 6 99.6(3) ?
Pb1 Se3 Sb2 . 6 94.25(7) ?
Sb1 Se3 Sb2 1_556 1_556 99.6(3) ?
Sb1 Se3 Sb2 6 1_556 174.15(14) ?
Pb1 Se3 Sb2 . 1_556 94.25(7) ?
Sb2 Se3 Sb2 6 1_556 78.1(5) ?
Sb2 Se4 Sb2 4_545 7_656 93.2(5) ?
Sb2 Se4 Sb2 4_545 7_655 4.7(4) ?
Sb2 Se4 Sb2 7_656 7_655 97.92(10) ?
Sb2 Se4 Sb2 4_545 4_546 97.92(10) ?
Sb2 Se4 Sb2 7_656 4_546 4.7(4) ?
Sb2 Se4 Sb2 7_655 4_546 102.6(4) ?
Sb2 Se4 Pb2 4_545 5_756 94.92(8) ?
Sb2 Se4 Pb2 7_656 5_756 94.92(8) ?
Sb2 Se4 Pb2 7_655 5_756 94.48(7) ?
Sb2 Se4 Pb2 4_546 5_756 94.48(7) ?
Sb2 Se4 Pb1 4_545 . 102.04(9) ?
Sb2 Se4 Pb1 7_656 . 102.04(9) ?
Sb2 Se4 Pb1 7_655 . 100.95(8) ?
Sb2 Se4 Pb1 4_546 . 100.95(8) ?
Pb2 Se4 Pb1 5_756 . 155.14(8) ?
Sb1 Se5 Sb1 6 1_556 89.7(4) ?
Sb1 Se5 Sb1 6 6_556 94.92(10) ?
Sb1 Se5 Sb1 1_556 6_556 5.2(4) ?
Sb1 Se5 Sb1 6 . 5.2(4) ?
Sb1 Se5 Sb1 1_556 . 94.92(10) ?
Sb1 Se5 Sb1 6_556 . 100.1(3) ?
Sb1 Se5 Pb2 6 . 100.32(9) ?
Sb1 Se5 Pb2 1_556 . 100.32(9) ?
Sb1 Se5 Pb2 6_556 . 99.34(8) ?
Sb1 Se5 Pb2 . . 99.34(8) ?
Pb2 Cl1 Pb2 5_656 1_454 180.00(4) ?
Pb2 Cl1 Pb2 5_656 1_455 93.25(4) ?
Pb2 Cl1 Pb2 1_454 1_455 86.75(4) ?
Pb2 Cl1 Pb2 5_656 5_655 86.75(4) ?
Pb2 Cl1 Pb2 1_454 5_655 93.25(4) ?
Pb2 Cl1 Pb2 1_455 5_655 180.00(3) ?

_exptl_crystal_recrystallization_method 'Solid State Reaction'
