# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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. 
# 
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data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2182340'
loop_
_audit_author_name
_audit_author_address
'Dinesh K. Amarasinghe'
;Iowa State University
United States of America
;
_audit_update_record             
;
2022-06-27 deposited with the CCDC.	2022-09-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Bi12.89 Br2.85 S17.15'
_chemical_formula_weight         3471.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_H-M_alt        'P 63'
_space_group_name_Hall           'P 6c'

_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'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'

_cell_length_a                   15.473(3)
_cell_length_b                   15.473(3)
_cell_length_c                   4.0041(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     830.2(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12606
_cell_measurement_theta_min      2.63
_cell_measurement_theta_max      25

_exptl_crystal_description       Needle
_exptl_crystal_colour            Silver
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    6.943
_exptl_crystal_F_000             1444
_exptl_transmission_factor_min   0.43
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    72.537
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus selaed tube'
_diffrn_measurement_device_type  
'Bruker D8 Venture with a Photon100 CMOS detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12606
_diffrn_reflns_av_unetI/netI     0.1138
_diffrn_reflns_av_R_equivalents  0.2910
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         2.633
_diffrn_reflns_theta_max         24.939
_diffrn_reflns_theta_full        24.939
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             962
_reflns_number_gt                662
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.712
_reflns_Friedel_fraction_max     0.976
_reflns_Friedel_fraction_full    0.976

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0003P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.1(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         962
_refine_ls_number_parameters     35
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0499
_refine_ls_wR_factor_gt          0.0470
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_restrained_S_all      0.970
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Bi1 Bi 0.60958(7) 0.48268(6) 0.885(3) 0.0078(3) Uiso 1 1 d . . . . .
Bi2 Bi 0.70295(11) 0.75519(19) 0.378(3) 0.0054(4) Uiso 0.877(8) 1 d . . P . .
Bi22 Bi 0.7121(7) 0.7878(13) 0.359(7) 0.0054(4) Uiso 0.123(8) 1 d . . P . .
Bi3 Bi 1.000000 1.000000 1.012(6) 0.0110(18) Uiso 0.21(2) 3 d S . P . .
Bi4 Bi 1.000000 1.000000 0.726(5) 0.0110(18) Uiso 0.24(2) 3 d S . P . .
Br1 Br 0.666667 0.333333 0.372(6) 0.0055(10) Uiso 1 3 d S . P . .
S1 S 0.8331(4) 0.8142(4) 0.882(6) 0.0029(12) Uiso 1 1 d . . . . .
S2 S 0.7383(3) 0.6006(3) 0.384(6) 0.0104(14) Uiso 0.877(8) 1 d . . P . .
Br2 Br 0.7383(3) 0.6006(3) 0.384(6) 0.0104(14) Uiso 0.123(8) 1 d . . P . .
S3 S 0.5477(4) 0.6105(4) -0.128(7) 0.001(2) Uiso 0.982(12) 1 d . . P . .
Br3 Br 0.5477(4) 0.6105(4) -0.128(7) 0.001(2) Uiso 0.018(12) 1 d . . P . .

_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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Bi1 S3 2.593(5) 1_556 ?
Bi1 S2 2.765(17) 1_556 ?
Bi1 Br2 2.774(17) . ?
Bi1 S3 2.879(18) 4_666 ?
Bi1 S3 2.953(18) 4_665 ?
Bi2 S1 2.646(18) 1_554 ?
Bi2 S1 2.667(17) . ?
Bi2 Br2 2.708(5) . ?
Bi2 S1 3.027(5) 5_564 ?
Bi2 S3 3.050(17) 1_556 ?
Bi2 Br3 3.085(17) . ?
Bi22 S1 2.56(3) 1_554 ?
Bi22 S1 2.593(18) 5_564 ?
Bi22 S1 2.70(3) . ?
Bi22 Br2 3.121(17) . ?
Bi22 Br2 3.15(2) 5_564 ?
Bi3 Bi4 0.859(14) 4_775 ?
Bi3 Bi4 1.143(14) . ?
Bi3 Bi3 2.0020(5) 4_775 ?
Bi3 Bi3 2.0021(5) 4_774 ?
Bi3 S1 2.789(10) . ?
Bi3 S1 2.789(10) 2_765 ?
Bi3 S1 2.789(9) 3_675 ?
Bi3 Bi4 2.861(14) 1_556 ?
Bi3 S1 3.12(2) 4_775 ?
Bi3 S1 3.12(2) 5_565 ?
Bi3 S1 3.12(2) 6_655 ?
Bi3 Bi4 3.145(14) 4_774 ?
Bi4 Bi4 2.0020(5) 4_774 ?
Bi4 Bi4 2.0021(5) 4_775 ?
Bi4 S1 2.810(10) . ?
Bi4 S1 2.810(10) 2_765 ?
Bi4 S1 2.810(10) 3_675 ?
Bi4 S1 3.068(18) 5_564 ?
Bi4 S1 3.068(18) 6_654 ?
Bi4 S1 3.068(18) 4_774 ?

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
S3 Bi1 S2 86.0(4) 1_556 1_556 ?
S3 Bi1 Br2 84.3(4) 1_556 . ?
S2 Bi1 Br2 92.58(14) 1_556 . ?
S3 Bi1 S3 81.6(3) 1_556 4_666 ?
S2 Bi1 S3 89.5(5) 1_556 4_666 ?
Br2 Bi1 S3 165.6(2) . 4_666 ?
S3 Bi1 S3 80.2(4) 1_556 4_665 ?
S2 Bi1 S3 166.09(17) 1_556 4_665 ?
Br2 Bi1 S3 87.9(5) . 4_665 ?
S3 Bi1 S3 86.70(14) 4_666 4_665 ?
S1 Bi2 S1 97.80(17) 1_554 . ?
S1 Bi2 Br2 81.7(4) 1_554 . ?
S1 Bi2 Br2 81.1(4) . . ?
S1 Bi2 S1 73.1(3) 1_554 5_564 ?
S1 Bi2 S1 72.9(3) . 5_564 ?
Br2 Bi2 S1 140.41(14) . 5_564 ?
S1 Bi2 S3 157.5(3) 1_554 1_556 ?
S1 Bi2 S3 86.8(5) . 1_556 ?
Br2 Bi2 S3 77.3(3) . 1_556 ?
S1 Bi2 S3 129.0(5) 5_564 1_556 ?
S1 Bi2 Br3 86.5(5) 1_554 . ?
S1 Bi2 Br3 157.8(3) . . ?
Br2 Bi2 Br3 78.0(4) . . ?
S1 Bi2 Br3 128.9(5) 5_564 . ?
S3 Bi2 Br3 81.47(13) 1_556 . ?
S1 Bi22 S1 82.4(6) 1_554 5_564 ?
S1 Bi22 S1 99.1(4) 1_554 . ?
S1 Bi22 S1 79.7(6) 5_564 . ?
S1 Bi22 Br2 75.4(6) 1_554 . ?
S1 Bi22 Br2 141.5(4) 5_564 . ?
S1 Bi22 Br2 73.4(5) . . ?
S1 Bi22 Br2 89.0(9) 1_554 5_564 ?
S1 Bi22 Br2 74.3(6) 5_564 5_564 ?
S1 Bi22 Br2 151.5(8) . 5_564 ?
Br2 Bi22 Br2 135.1(10) . 5_564 ?
Bi4 Bi3 Bi4 180.00(8) 4_775 . ?
Bi4 Bi3 Bi3 0.00(5) 4_775 4_775 ?
Bi4 Bi3 Bi3 180.00(6) . 4_775 ?
Bi4 Bi3 Bi3 180.00(8) 4_775 4_774 ?
Bi4 Bi3 Bi3 0.00(3) . 4_774 ?
Bi3 Bi3 Bi3 180.00(5) 4_775 4_774 ?
Bi4 Bi3 S1 100.8(9) 4_775 . ?
Bi4 Bi3 S1 79.2(9) . . ?
Bi3 Bi3 S1 100.8(9) 4_775 . ?
Bi3 Bi3 S1 79.2(9) 4_774 . ?
Bi4 Bi3 S1 100.8(9) 4_775 2_765 ?
Bi4 Bi3 S1 79.2(9) . 2_765 ?
Bi3 Bi3 S1 100.8(9) 4_775 2_765 ?
Bi3 Bi3 S1 79.2(9) 4_774 2_765 ?
S1 Bi3 S1 116.6(5) . 2_765 ?
Bi4 Bi3 S1 100.8(9) 4_775 3_675 ?
Bi4 Bi3 S1 79.2(9) . 3_675 ?
Bi3 Bi3 S1 100.8(9) 4_775 3_675 ?
Bi3 Bi3 S1 79.2(9) 4_774 3_675 ?
S1 Bi3 S1 116.6(5) . 3_675 ?
S1 Bi3 S1 116.6(5) 2_765 3_675 ?
Bi4 Bi3 Bi4 0.00(5) 4_775 1_556 ?
Bi4 Bi3 Bi4 180.00(5) . 1_556 ?
Bi3 Bi3 Bi4 0.00(2) 4_775 1_556 ?
Bi3 Bi3 Bi4 180.00(3) 4_774 1_556 ?
S1 Bi3 Bi4 100.8(9) . 1_556 ?
S1 Bi3 Bi4 100.8(9) 2_765 1_556 ?
S1 Bi3 Bi4 100.8(9) 3_675 1_556 ?
Bi4 Bi3 S1 61.6(7) 4_775 4_775 ?
Bi4 Bi3 S1 118.4(7) . 4_775 ?
Bi3 Bi3 S1 61.6(7) 4_775 4_775 ?
Bi3 Bi3 S1 118.4(7) 4_774 4_775 ?
S1 Bi3 S1 162.4(15) . 4_775 ?
S1 Bi3 S1 69.9(2) 2_765 4_775 ?
S1 Bi3 S1 69.9(2) 3_675 4_775 ?
Bi4 Bi3 S1 61.6(7) 1_556 4_775 ?
Bi4 Bi3 S1 61.6(7) 4_775 5_565 ?
Bi4 Bi3 S1 118.4(7) . 5_565 ?
Bi3 Bi3 S1 61.6(7) 4_775 5_565 ?
Bi3 Bi3 S1 118.4(7) 4_774 5_565 ?
S1 Bi3 S1 69.9(2) . 5_565 ?
S1 Bi3 S1 162.4(15) 2_765 5_565 ?
S1 Bi3 S1 69.9(2) 3_675 5_565 ?
Bi4 Bi3 S1 61.6(7) 1_556 5_565 ?
S1 Bi3 S1 99.3(9) 4_775 5_565 ?
Bi4 Bi3 S1 61.6(7) 4_775 6_655 ?
Bi4 Bi3 S1 118.4(7) . 6_655 ?
Bi3 Bi3 S1 61.6(7) 4_775 6_655 ?
Bi3 Bi3 S1 118.4(7) 4_774 6_655 ?
S1 Bi3 S1 69.9(2) . 6_655 ?
S1 Bi3 S1 69.9(2) 2_765 6_655 ?
S1 Bi3 S1 162.4(15) 3_675 6_655 ?
Bi4 Bi3 S1 61.6(7) 1_556 6_655 ?
S1 Bi3 S1 99.3(9) 4_775 6_655 ?
S1 Bi3 S1 99.3(9) 5_565 6_655 ?
Bi4 Bi3 Bi4 180.00(6) 4_775 4_774 ?
Bi4 Bi3 Bi4 0.00(3) . 4_774 ?
Bi3 Bi3 Bi4 180.00(4) 4_775 4_774 ?
Bi3 Bi3 Bi4 0.000(17) 4_774 4_774 ?
S1 Bi3 Bi4 79.2(9) . 4_774 ?
S1 Bi3 Bi4 79.2(9) 2_765 4_774 ?
S1 Bi3 Bi4 79.2(9) 3_675 4_774 ?
Bi4 Bi3 Bi4 180.00(3) 1_556 4_774 ?
S1 Bi3 Bi4 118.4(7) 4_775 4_774 ?
S1 Bi3 Bi4 118.4(7) 5_565 4_774 ?
S1 Bi3 Bi4 118.4(7) 6_655 4_774 ?
Bi3 Bi4 Bi3 180.00(9) 4_774 . ?
Bi3 Bi4 Bi4 0.00(4) 4_774 4_774 ?
Bi3 Bi4 Bi4 180.00(5) . 4_774 ?
Bi3 Bi4 Bi4 180.00(6) 4_774 4_775 ?
Bi3 Bi4 Bi4 0.00(3) . 4_775 ?
Bi4 Bi4 Bi4 180.00(3) 4_774 4_775 ?
Bi3 Bi4 S1 102.8(8) 4_774 . ?
Bi3 Bi4 S1 77.2(8) . . ?
Bi4 Bi4 S1 102.8(8) 4_774 . ?
Bi4 Bi4 S1 77.2(8) 4_775 . ?
Bi3 Bi4 S1 102.8(8) 4_774 2_765 ?
Bi3 Bi4 S1 77.2(8) . 2_765 ?
Bi4 Bi4 S1 102.8(8) 4_774 2_765 ?
Bi4 Bi4 S1 77.2(8) 4_775 2_765 ?
S1 Bi4 S1 115.2(5) . 2_765 ?
Bi3 Bi4 S1 102.8(8) 4_774 3_675 ?
Bi3 Bi4 S1 77.2(8) . 3_675 ?
Bi4 Bi4 S1 102.8(8) 4_774 3_675 ?
Bi4 Bi4 S1 77.2(8) 4_775 3_675 ?
S1 Bi4 S1 115.2(6) . 3_675 ?
S1 Bi4 S1 115.2(5) 2_765 3_675 ?
Bi3 Bi4 Bi3 0.00(5) 4_774 1_554 ?
Bi3 Bi4 Bi3 180.00(6) . 1_554 ?
Bi4 Bi4 Bi3 0.000(12) 4_774 1_554 ?
Bi4 Bi4 Bi3 180.00(4) 4_775 1_554 ?
S1 Bi4 Bi3 102.8(7) . 1_554 ?
S1 Bi4 Bi3 102.8(8) 2_765 1_554 ?
S1 Bi4 Bi3 102.8(8) 3_675 1_554 ?
Bi3 Bi4 S1 63.3(6) 4_774 5_564 ?
Bi3 Bi4 S1 116.7(7) . 5_564 ?
Bi4 Bi4 S1 63.3(6) 4_774 5_564 ?
Bi4 Bi4 S1 116.7(7) 4_775 5_564 ?
S1 Bi4 S1 70.37(15) . 5_564 ?
S1 Bi4 S1 166.1(14) 2_765 5_564 ?
S1 Bi4 S1 70.37(16) 3_675 5_564 ?
Bi3 Bi4 S1 63.3(6) 1_554 5_564 ?
Bi3 Bi4 S1 63.3(6) 4_774 6_654 ?
Bi3 Bi4 S1 116.7(6) . 6_654 ?
Bi4 Bi4 S1 63.3(6) 4_774 6_654 ?
Bi4 Bi4 S1 116.7(6) 4_775 6_654 ?
S1 Bi4 S1 70.37(15) . 6_654 ?
S1 Bi4 S1 70.37(15) 2_765 6_654 ?
S1 Bi4 S1 166.1(14) 3_675 6_654 ?
Bi3 Bi4 S1 63.3(6) 1_554 6_654 ?
S1 Bi4 S1 101.4(8) 5_564 6_654 ?
Bi3 Bi4 S1 63.3(7) 4_774 4_774 ?
Bi3 Bi4 S1 116.7(6) . 4_774 ?
Bi4 Bi4 S1 63.3(6) 4_774 4_774 ?
Bi4 Bi4 S1 116.7(6) 4_775 4_774 ?
S1 Bi4 S1 166.1(14) . 4_774 ?
S1 Bi4 S1 70.37(15) 2_765 4_774 ?
S1 Bi4 S1 70.37(16) 3_675 4_774 ?
Bi3 Bi4 S1 63.3(6) 1_554 4_774 ?
S1 Bi4 S1 101.4(8) 5_564 4_774 ?
S1 Bi4 S1 101.4(8) 6_654 4_774 ?
Bi3 Bi4 Bi3 180.00(7) 4_774 4_775 ?
Bi3 Bi4 Bi3 0.00(4) . 4_775 ?
Bi4 Bi4 Bi3 180.00(3) 4_774 4_775 ?
Bi4 Bi4 Bi3 0.000(17) 4_775 4_775 ?
S1 Bi4 Bi3 77.2(8) . 4_775 ?
S1 Bi4 Bi3 77.2(8) 2_765 4_775 ?
S1 Bi4 Bi3 77.2(8) 3_675 4_775 ?
Bi3 Bi4 Bi3 180.00(2) 1_554 4_775 ?
S1 Bi4 Bi3 116.7(6) 5_564 4_775 ?
S1 Bi4 Bi3 116.7(6) 6_654 4_775 ?
S1 Bi4 Bi3 116.7(6) 4_774 4_775 ?
Bi22 S1 Bi22 120.4(10) 1_556 6_655 ?
Bi22 S1 Bi2 9.9(4) 1_556 1_556 ?
Bi22 S1 Bi2 111.6(7) 6_655 1_556 ?
Bi22 S1 Bi2 98.2(5) 1_556 . ?
Bi22 S1 Bi2 108.2(8) 6_655 . ?
Bi2 S1 Bi2 97.80(17) 1_556 . ?
Bi22 S1 Bi22 99.1(4) 1_556 . ?
Bi22 S1 Bi22 115.3(10) 6_655 . ?
Bi2 S1 Bi22 100.4(5) 1_556 . ?
Bi2 S1 Bi22 9.8(3) . . ?
Bi22 S1 Bi3 104.6(9) 1_556 . ?
Bi22 S1 Bi3 97.4(3) 6_655 . ?
Bi2 S1 Bi3 111.6(9) 1_556 . ?
Bi2 S1 Bi3 130.2(8) . . ?
Bi22 S1 Bi3 121.0(9) . . ?
Bi22 S1 Bi4 123.6(8) 1_556 . ?
Bi22 S1 Bi4 96.5(3) 6_655 . ?
Bi2 S1 Bi4 132.1(8) 1_556 . ?
Bi2 S1 Bi4 109.5(8) . . ?
Bi22 S1 Bi4 101.3(9) . . ?
Bi3 S1 Bi4 23.6(3) . . ?
Bi22 S1 Bi2 120.2(7) 1_556 6_655 ?
Bi22 S1 Bi2 3.0(4) 6_655 6_655 ?
Bi2 S1 Bi2 111.6(5) 1_556 6_655 ?
Bi2 S1 Bi2 111.0(5) . 6_655 ?
Bi22 S1 Bi2 118.0(7) . 6_655 ?
Bi3 S1 Bi2 94.77(17) . 6_655 ?
Bi4 S1 Bi2 94.62(18) . 6_655 ?
Bi22 S1 Bi4 91.1(8) 1_556 4_775 ?
Bi22 S1 Bi4 97.3(5) 6_655 4_775 ?
Bi2 S1 Bi4 97.1(8) 1_556 4_775 ?
Bi2 S1 Bi4 143.0(6) . 4_775 ?
Bi22 S1 Bi4 133.3(6) . 4_775 ?
Bi3 S1 Bi4 16.0(3) . 4_775 ?
Bi4 S1 Bi4 39.52(13) . 4_775 ?
Bi2 S1 Bi4 94.4(2) 6_655 4_775 ?
Bi22 S1 Bi3 134.8(6) 1_556 4_774 ?
Bi22 S1 Bi3 95.3(5) 6_655 4_774 ?
Bi2 S1 Bi3 144.3(6) 1_556 4_774 ?
Bi2 S1 Bi3 95.3(8) . 4_774 ?
Bi22 S1 Bi3 87.9(8) . 4_774 ?
Bi3 S1 Bi3 39.15(18) . 4_774 ?
Bi4 S1 Bi3 15.6(2) . 4_774 ?
Bi2 S1 Bi3 94.1(3) 6_655 4_774 ?
Bi4 S1 Bi3 55.1(2) 4_775 4_774 ?
Bi2 Br2 Bi1 100.4(4) . 1_554 ?
Bi2 Br2 Bi1 101.0(4) . . ?
Bi1 Br2 Bi1 92.58(14) 1_554 . ?
Bi2 Br2 Bi22 3.9(3) . . ?
Bi1 Br2 Bi22 101.8(6) 1_554 . ?
Bi1 Br2 Bi22 104.5(6) . . ?
Bi2 Br2 Bi22 93.1(4) . 6_655 ?
Bi1 Br2 Bi22 163.2(5) 1_554 6_655 ?
Bi1 Br2 Bi22 94.7(8) . 6_655 ?
Bi22 Br2 Bi22 91.0(6) . 6_655 ?
Bi1 Br3 Bi1 100.0(4) 1_554 4_663 ?
Bi1 Br3 Bi1 98.1(5) 1_554 4_664 ?
Bi1 Br3 Bi1 86.70(13) 4_663 4_664 ?
Bi1 Br3 Bi2 96.8(4) 1_554 1_554 ?
Bi1 Br3 Bi2 95.0(7) 4_663 1_554 ?
Bi1 Br3 Bi2 164.5(2) 4_664 1_554 ?
Bi1 Br3 Bi2 95.1(4) 1_554 . ?
Bi1 Br3 Bi2 164.7(2) 4_663 . ?
Bi1 Br3 Bi2 92.8(7) 4_664 . ?
Bi2 Br3 Bi2 81.47(13) 1_554 . ?

_refine_diff_density_max         2.086
_refine_diff_density_min         -2.241
_refine_diff_density_rms         0.582

# start Validation Reply Form
_vrf_ATOM007_shelx               
;
PROBLEM: _atom_site_aniso_label is missing
RESPONSE: Due to severe disorder all atoms were refined isostropically.
;
_vrf_RINTA01_shelx               
;
PROBLEM: The value of Rint is greater than 0.25
RESPONSE: Multiple crystals were tested, all resulted in similar
or higher Rints. An integration and solutions in either P1 or 
P2(1) resulted in no improvements of the disorder and comparable
Rint values.
;
_vrf_PLAT973_shelx               
;
PROBLEM: Check Calcd Positive Resid. Density on      Bi22       1.65 eA-3  
RESPONSE: Difference peaks of ~2% of total Bi electron density 
are common in disordered Bi compounds.
;
# end Validation Reply Form



