# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_aa
_database_code_depnum_ccdc_archive 'CCDC 1958251'
loop_
_audit_author_name
_audit_author_address
'Pengfei Hao'
;School of Chemical and Material Science, Shanxi Normal University
China
;
_audit_update_record             
;
2019-10-09 deposited with the CCDC.	2020-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H36 Bi O8 S8, Bi2 I9'
_chemical_formula_sum            'C16 H36 Bi3 I9 O8 S8'
_chemical_formula_weight         2381.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'
_space_group_name_Hall           '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.958(3)
_cell_length_b                   15.817(4)
_cell_length_c                   16.280(5)
_cell_angle_alpha                82.222(6)
_cell_angle_beta                 69.979(6)
_cell_angle_gamma                78.914(6)
_cell_volume                     2831.1(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    7407
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      28.33

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.794
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2100
_exptl_absorpt_coefficient_mu    14.531
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.100
_exptl_absorpt_correction_T_max  0.270
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21701
_diffrn_reflns_av_R_equivalents  0.0834
_diffrn_reflns_av_sigmaI/netI    0.1519
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         28.42
_reflns_number_total             14222
_reflns_number_gt                7336
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1406P)²+447.5368P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13522
_refine_ls_number_parameters     409
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.2368
_refine_ls_R_factor_gt           0.1541
_refine_ls_wR_factor_ref         0.3981
_refine_ls_wR_factor_gt          0.3401
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.034
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.17249(13) 0.82128(9) 0.26202(10) 0.0414(4) Uani 1 1 d . . .
Bi2 Bi -0.06743(13) 0.67534(9) 0.23456(10) 0.0411(4) Uani 1 1 d . . .
Bi3 Bi 0.57513(15) 0.24147(10) 0.25068(11) 0.0513(4) Uani 1 1 d . . .
I1 I 0.2615(4) 0.9700(2) 0.1422(3) 0.0874(12) Uani 1 1 d . . .
I2 I 0.1009(3) 0.9232(2) 0.4154(2) 0.0682(9) Uani 1 1 d . . .
I3 I 0.4062(3) 0.7408(2) 0.2764(3) 0.0676(9) Uani 1 1 d . . .
I4 I 0.0432(2) 0.66764(17) 0.38829(17) 0.0495(6) Uani 1 1 d . . .
I5 I 0.1996(2) 0.70753(19) 0.10632(17) 0.0517(7) Uani 1 1 d . . .
I6 I -0.1018(3) 0.87569(18) 0.2443(2) 0.0615(8) Uani 1 1 d . . .
I7 I 0.0085(3) 0.48271(19) 0.2217(3) 0.0717(9) Uani 1 1 d . . .
I8 I -0.3053(3) 0.6614(3) 0.3646(2) 0.0807(11) Uani 1 1 d . . .
I9 I -0.1618(3) 0.7088(2) 0.0827(2) 0.0628(9) Uani 1 1 d . . .
C1 C 0.658(4) 0.516(2) 0.187(2) 0.063(10) Uani 1 1 d DU . .
H1A H 0.6050 0.4997 0.2438 0.094 Uiso 1 1 calc R . .
H1B H 0.6213 0.5690 0.1638 0.094 Uiso 1 1 calc R . .
H1C H 0.7328 0.5243 0.1920 0.094 Uiso 1 1 calc R . .
C2 C 0.831(4) 0.449(3) 0.051(3) 0.060(12) Uani 1 1 d . . .
H2A H 0.8643 0.4821 0.0797 0.090 Uiso 1 1 calc R . .
H2B H 0.8286 0.4800 -0.0040 0.090 Uiso 1 1 calc R . .
H2C H 0.8807 0.3941 0.0396 0.090 Uiso 1 1 calc R . .
C3 C 0.601(4) 0.418(4) 0.443(4) 0.11(2) Uani 1 1 d D . .
H3A H 0.5238 0.4153 0.4383 0.170 Uiso 1 1 calc R . .
H3B H 0.6127 0.4769 0.4371 0.170 Uiso 1 1 calc R . .
H3C H 0.6030 0.3923 0.5000 0.170 Uiso 1 1 calc R . .
C4 C 0.822(6) 0.321(6) 0.414(4) 0.14(3) Uani 1 1 d . . .
H4A H 0.7965 0.2735 0.4550 0.211 Uiso 1 1 calc R . .
H4B H 0.8305 0.3662 0.4446 0.211 Uiso 1 1 calc R . .
H4C H 0.8978 0.3024 0.3709 0.211 Uiso 1 1 calc R . .
C5 C 0.994(6) 0.195(6) 0.165(5) 0.13(3) Uani 1 1 d . . .
C6 C 0.954(5) 0.108(3) 0.049(3) 0.080(18) Uani 1 1 d . . .
H6A H 0.9167 0.0592 0.0805 0.120 Uiso 1 1 calc R . .
H6B H 1.0381 0.0966 0.0417 0.120 Uiso 1 1 calc R . .
H6C H 0.9426 0.1183 -0.0073 0.120 Uiso 1 1 calc R . .
C7 C 0.591(6) 0.137(4) 0.515(4) 0.093(15) Uani 1 1 d U . .
H7A H 0.6289 0.1874 0.4945 0.139 Uiso 1 1 calc R . .
H7B H 0.6148 0.1068 0.5627 0.139 Uiso 1 1 calc R . .
H7C H 0.5050 0.1535 0.5334 0.139 Uiso 1 1 calc R . .
C8 C 0.786(3) 0.078(4) 0.381(4) 0.093(16) Uani 1 1 d DU . .
H8A H 0.8013 0.0982 0.3203 0.140 Uiso 1 1 calc R . .
H8B H 0.8342 0.0230 0.3853 0.140 Uiso 1 1 calc R . .
H8C H 0.8063 0.1189 0.4103 0.140 Uiso 1 1 calc R . .
C9 C 0.529(6) -0.041(4) 0.271(4) 0.100(17) Uani 1 1 d U . .
H9A H 0.4499 -0.0188 0.2689 0.150 Uiso 1 1 calc R . .
H9B H 0.5297 -0.0399 0.3303 0.150 Uiso 1 1 calc R . .
H9C H 0.5530 -0.0987 0.2541 0.150 Uiso 1 1 calc R . .
C10 C 0.667(7) -0.019(5) 0.097(5) 0.12(2) Uani 1 1 d U . .
H10A H 0.5962 -0.0345 0.0919 0.187 Uiso 1 1 calc R . .
H10B H 0.7277 -0.0691 0.0931 0.187 Uiso 1 1 calc R . .
H10C H 0.6968 0.0240 0.0514 0.187 Uiso 1 1 calc R . .
C11 C 0.240(6) 0.167(4) 0.476(3) 0.10(2) Uani 1 1 d . . .
H11A H 0.2965 0.1378 0.5048 0.146 Uiso 1 1 calc R . .
H11B H 0.1647 0.1459 0.5027 0.146 Uiso 1 1 calc R . .
H11C H 0.2279 0.2280 0.4823 0.146 Uiso 1 1 calc R . .
C12 C 0.168(7) 0.181(5) 0.345(7) 0.17(5) Uani 1 1 d . . .
H12A H 0.1060 0.1529 0.3870 0.256 Uiso 1 1 calc R . .
H12B H 0.1781 0.1677 0.2871 0.256 Uiso 1 1 calc R . .
H12C H 0.1465 0.2427 0.3491 0.256 Uiso 1 1 calc R . .
C13 C 0.424(14) 0.363(6) 0.004(8) 0.23(7) Uani 1 1 d . . .
C14 C 0.461(12) 0.181(6) 0.018(7) 0.21(3) Uani 1 1 d DU . .
C15 C 0.248(8) 0.434(4) 0.400(5) 0.12(3) Uani 1 1 d . . .
C16 C 0.330(4) 0.514(3) 0.241(5) 0.10(2) Uani 1 1 d . . .
H16A H 0.3314 0.5514 0.2822 0.153 Uiso 1 1 calc R . .
H16B H 0.2591 0.5325 0.2244 0.153 Uiso 1 1 calc R . .
H16C H 0.4003 0.5145 0.1905 0.153 Uiso 1 1 calc R . .
O1 O 0.702(3) 0.350(2) 0.171(2) 0.062(8) Uani 1 1 d U . .
O2 O 0.666(3) 0.2814(17) 0.3565(18) 0.053(7) Uani 1 1 d . . .
O3 O 0.776(3) 0.1694(16) 0.178(2) 0.062(8) Uani 1 1 d . . .
O4 O 0.575(3) 0.117(2) 0.365(2) 0.071(9) Uani 1 1 d . . .
O5 O 0.551(3) 0.1123(18) 0.1905(17) 0.057(7) Uani 1 1 d . . .
O6 O 0.362(3) 0.226(2) 0.327(2) 0.083(11) Uani 1 1 d . . .
O7 O 0.497(3) 0.2937(19) 0.1327(18) 0.057(8) Uani 1 1 d . . .
O8 O 0.456(3) 0.3812(15) 0.297(2) 0.055(7) Uani 1 1 d . . .
S1 S 0.6848(11) 0.4353(7) 0.1172(8) 0.057(3) Uani 1 1 d DU . .
S2 S 0.7140(12) 0.3610(8) 0.3621(8) 0.066(3) Uani 1 1 d D . .
S3 S 0.8888(10) 0.1964(7) 0.1066(8) 0.056(3) Uani 1 1 d . . .
S4 S 0.6345(16) 0.0693(10) 0.4295(10) 0.088(5) Uani 1 1 d D . .
S5 S 0.6298(11) 0.0237(6) 0.2012(8) 0.058(3) Uani 1 1 d . . .
S6 S 0.2964(12) 0.1483(8) 0.3661(10) 0.078(4) Uani 1 1 d . . .
S7 S 0.440(4) 0.2651(19) 0.082(2) 0.25(2) Uani 1 1 d D . .
S8 S 0.3270(11) 0.4108(7) 0.2896(10) 0.069(3) Uani 1 1 d . . .


_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 I3 2.913(3) . ?
Bi1 I2 2.943(3) . ?
Bi1 I1 2.962(3) . ?
Bi1 I5 3.196(3) . ?
Bi1 I4 3.231(3) . ?
Bi1 I6 3.329(3) . ?
Bi2 I8 2.934(3) . ?
Bi2 I9 3.000(3) . ?
Bi2 I7 3.022(3) . ?
Bi2 I6 3.135(3) . ?
Bi2 I4 3.186(3) . ?
Bi2 I5 3.253(3) . ?
Bi3 O7 2.40(2) . ?
Bi3 O3 2.42(3) . ?
Bi3 O8 2.45(3) . ?
Bi3 O1 2.45(3) . ?
Bi3 O6 2.47(3) . ?
Bi3 O5 2.48(3) . ?
Bi3 O4 2.53(3) . ?
Bi3 O2 2.53(3) . ?
C1 S1 1.735(19) . ?
C2 S1 1.75(4) . ?
C3 S2 1.738(19) . ?
C4 S2 1.75(7) . ?
C5 S3 1.82(7) . ?
C6 S3 1.69(5) . ?
C7 S4 1.74(6) . ?
C8 S4 1.737(19) . ?
C9 S5 1.73(6) . ?
C10 S5 1.78(8) . ?
C11 S6 1.73(5) . ?
C12 S6 1.65(7) . ?
C13 S7 1.88(8) . ?
C14 S7 1.74(2) . ?
C15 S8 1.77(8) . ?
C16 S8 1.71(5) . ?
O1 S1 1.52(3) . ?
O2 S2 1.51(3) . ?
O3 S3 1.53(3) . ?
O4 S4 1.50(3) . ?
O5 S5 1.55(3) . ?
O6 S6 1.54(3) . ?
O7 S7 1.40(3) . ?
O8 S8 1.57(3) . ?

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
I3 Bi1 I2 95.66(11) . . ?
I3 Bi1 I1 95.61(12) . . ?
I2 Bi1 I1 91.27(12) . . ?
I3 Bi1 I5 92.85(10) . . ?
I2 Bi1 I5 169.59(10) . . ?
I1 Bi1 I5 93.88(11) . . ?
I3 Bi1 I4 91.60(9) . . ?
I2 Bi1 I4 89.02(10) . . ?
I1 Bi1 I4 172.73(11) . . ?
I5 Bi1 I4 84.73(8) . . ?
I3 Bi1 I6 169.29(9) . . ?
I2 Bi1 I6 91.02(10) . . ?
I1 Bi1 I6 92.60(11) . . ?
I5 Bi1 I6 79.72(8) . . ?
I4 Bi1 I6 80.13(8) . . ?
I8 Bi2 I9 93.69(10) . . ?
I8 Bi2 I7 94.73(12) . . ?
I9 Bi2 I7 96.65(10) . . ?
I8 Bi2 I6 92.86(12) . . ?
I9 Bi2 I6 88.43(9) . . ?
I7 Bi2 I6 170.58(9) . . ?
I8 Bi2 I4 90.09(10) . . ?
I9 Bi2 I4 171.55(8) . . ?
I7 Bi2 I4 90.56(9) . . ?
I6 Bi2 I4 83.84(8) . . ?
I8 Bi2 I5 172.77(11) . . ?
I9 Bi2 I5 91.02(9) . . ?
I7 Bi2 I5 90.17(9) . . ?
I6 Bi2 I5 81.78(9) . . ?
I4 Bi2 I5 84.53(8) . . ?
O7 Bi3 O3 103.5(11) . . ?
O7 Bi3 O8 77.3(11) . . ?
O3 Bi3 O8 143.8(9) . . ?
O7 Bi3 O1 77.6(10) . . ?
O3 Bi3 O1 71.0(9) . . ?
O8 Bi3 O1 74.0(10) . . ?
O7 Bi3 O6 81.3(11) . . ?
O3 Bi3 O6 146.6(11) . . ?
O8 Bi3 O6 69.7(11) . . ?
O1 Bi3 O6 141.1(11) . . ?
O7 Bi3 O5 73.4(10) . . ?
O3 Bi3 O5 73.5(10) . . ?
O8 Bi3 O5 137.9(10) . . ?
O1 Bi3 O5 126.4(10) . . ?
O6 Bi3 O5 76.5(12) . . ?
O7 Bi3 O4 141.4(11) . . ?
O3 Bi3 O4 83.5(11) . . ?
O8 Bi3 O4 118.8(11) . . ?
O1 Bi3 O4 138.7(11) . . ?
O6 Bi3 O4 73.8(12) . . ?
O5 Bi3 O4 72.5(9) . . ?
O7 Bi3 O2 145.3(9) . . ?
O3 Bi3 O2 85.2(11) . . ?
O8 Bi3 O2 76.3(10) . . ?
O1 Bi3 O2 73.7(9) . . ?
O6 Bi3 O2 109.9(12) . . ?
O5 Bi3 O2 140.5(9) . . ?
O4 Bi3 O2 72.3(9) . . ?
Bi2 I4 Bi1 81.27(7) . . ?
Bi1 I5 Bi2 80.77(7) . . ?
Bi2 I6 Bi1 80.51(7) . . ?
S1 O1 Bi3 135.5(18) . . ?
S2 O2 Bi3 132.7(15) . . ?
S3 O3 Bi3 135.3(15) . . ?
S4 O4 Bi3 146(2) . . ?
S5 O5 Bi3 120.1(16) . . ?
S6 O6 Bi3 134(2) . . ?
S7 O7 Bi3 140(2) . . ?
S8 O8 Bi3 122.0(15) . . ?
O1 S1 C1 106(2) . . ?
O1 S1 C2 104(2) . . ?
C1 S1 C2 98.4(19) . . ?
O2 S2 C3 105(2) . . ?
O2 S2 C4 103(3) . . ?
C3 S2 C4 102(4) . . ?
O3 S3 C6 104.7(19) . . ?
O3 S3 C5 104(3) . . ?
C6 S3 C5 100(4) . . ?
O4 S4 C8 105(3) . . ?
O4 S4 C7 105(3) . . ?
C8 S4 C7 102(3) . . ?
O5 S5 C9 105(3) . . ?
O5 S5 C10 103(3) . . ?
C9 S5 C10 103(3) . . ?
O6 S6 C12 101(3) . . ?
O6 S6 C11 101(3) . . ?
C12 S6 C11 97(5) . . ?
O7 S7 C14 140(6) . . ?
O7 S7 C13 102(3) . . ?
C14 S7 C13 102(6) . . ?
O8 S8 C16 104(2) . . ?
O8 S8 C15 99(3) . . ?
C16 S8 C15 100(3) . . ?

_diffrn_measured_fraction_theta_max 0.950
_diffrn_reflns_theta_full        28.42
_diffrn_measured_fraction_theta_full 0.950
_refine_diff_density_max         5.872
_refine_diff_density_min         -5.024
_refine_diff_density_rms         0.579
_chemical_properties_physical    Heat-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_aa_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1958253'
loop_
_audit_author_name
_audit_author_address
'Pengfei Hao'
;School of Chemical and Material Science, Shanxi Normal University
China
;
_audit_update_record             
;
2019-10-09 deposited with the CCDC.	2020-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H45 La O8 S8, Bi2 I9'
_chemical_formula_sum            'C16 H45 Bi2 I9 La O8 S8'
_chemical_formula_weight         2320.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '
_symmetry_space_group_name_Hall  '-P 1 '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.0219(14)
_cell_length_b                   15.8042(19)
_cell_length_c                   16.282(2)
_cell_angle_alpha                82.124(3)
_cell_angle_beta                 69.973(3)
_cell_angle_gamma                78.890(3)
_cell_volume                     2843.5(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    273(2)
_cell_measurement_reflns_used    9893
_cell_measurement_theta_min      2.41
_cell_measurement_theta_max      27.01

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.028
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2066
_exptl_absorpt_coefficient_mu    12.119
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.376
_exptl_absorpt_correction_T_max  0.712
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      273(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            40936
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         28.36
_reflns_number_total             14207
_reflns_number_gt                9369
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1018P)²+9.2322P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14002
_refine_ls_number_parameters     412
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1928
_refine_ls_wR_factor_gt          0.1663
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.32667(4) 0.18053(3) 0.23775(3) 0.04540(14) Uani 1 1 d . . .
Bi2 Bi 0.56715(4) 0.32498(3) 0.26526(3) 0.04545(14) Uani 1 1 d . . .
I1 I 0.09519(9) 0.26172(7) 0.22155(8) 0.0728(3) Uani 1 1 d . . .
I2 I 0.39879(10) 0.07836(7) 0.08437(7) 0.0734(3) Uani 1 1 d . . .
I3 I 0.23630(14) 0.03276(9) 0.35710(9) 0.0979(4) Uani 1 1 d . . .
I4 I 0.45767(8) 0.33350(6) 0.11088(6) 0.0555(2) Uani 1 1 d . . .
I5 I 0.29986(8) 0.29508(6) 0.39299(6) 0.0584(2) Uani 1 1 d . . .
I6 I 0.59705(9) 0.12438(6) 0.25644(8) 0.0667(3) Uani 1 1 d . . .
I7 I 0.49472(11) 0.51737(7) 0.27674(9) 0.0792(3) Uani 1 1 d . . .
I8 I 0.80543(10) 0.33575(10) 0.13597(8) 0.0895(4) Uani 1 1 d . . .
I9 I 0.65984(9) 0.29134(7) 0.41750(7) 0.0650(3) Uani 1 1 d . . .
La1 La 0.92465(6) 0.75981(4) 0.24894(4) 0.03710(16) Uani 1 1 d . . .
C1 C 0.8382(15) 0.4815(9) 0.3133(12) 0.079(5) Uani 1 1 d . . .
H1A H 0.7707 0.4876 0.2929 0.118 Uiso 1 1 calc R . .
H1B H 0.8477 0.4255 0.3438 0.118 Uiso 1 1 calc R . .
H1C H 0.9093 0.4873 0.2642 0.118 Uiso 1 1 calc R . .
C2 C 0.6679(14) 0.5492(9) 0.4505(9) 0.065(4) Uani 1 1 d . . .
H2A H 0.6305 0.5987 0.4838 0.098 Uiso 1 1 calc R . .
H2B H 0.6705 0.4982 0.4899 0.098 Uiso 1 1 calc R . .
H2C H 0.6227 0.5431 0.4138 0.098 Uiso 1 1 calc R . .
C3 C 0.509(2) 0.811(2) 0.3357(16) 0.162(13) Uani 1 1 d . . .
H3A H 0.5528 0.7991 0.2758 0.243 Uiso 1 1 calc R . .
H3B H 0.4637 0.8679 0.3377 0.243 Uiso 1 1 calc R . .
H3C H 0.4558 0.7693 0.3619 0.243 Uiso 1 1 calc R . .
C4 C 0.5411(19) 0.8952(11) 0.4516(14) 0.108(8) Uani 1 1 d . . .
H4A H 0.5734 0.8945 0.4981 0.162 Uiso 1 1 calc R . .
H4B H 0.4563 0.8951 0.4759 0.162 Uiso 1 1 calc R . .
H4C H 0.5563 0.9464 0.4129 0.162 Uiso 1 1 calc R . .
C5 C 0.900(3) 0.584(2) 0.057(2) 0.22(2) Uani 1 1 d . . .
H5A H 0.9686 0.6128 0.0382 0.330 Uiso 1 1 calc R . .
H5B H 0.8732 0.5822 0.0080 0.330 Uiso 1 1 calc R . .
H5C H 0.9204 0.5261 0.0799 0.330 Uiso 1 1 calc R . .
C6 C 0.681(2) 0.6756(16) 0.0773(17) 0.121(8) Uani 1 1 d . . .
H6A H 0.6111 0.7105 0.1125 0.181 Uiso 1 1 calc R . .
H6B H 0.6590 0.6261 0.0624 0.181 Uiso 1 1 calc R . .
H6C H 0.7191 0.7090 0.0247 0.181 Uiso 1 1 calc R . .
C7 C 0.904(2) 0.8667(14) -0.0203(11) 0.106(7) Uani 1 1 d . . .
H7A H 0.9896 0.8584 -0.0481 0.160 Uiso 1 1 calc R . .
H7B H 0.8659 0.8955 -0.0617 0.160 Uiso 1 1 calc R . .
H7C H 0.8783 0.8116 0.0003 0.160 Uiso 1 1 calc R . .
C8 C 0.713(2) 0.9222(12) 0.1152(13) 0.101(7) Uani 1 1 d . . .
H8A H 0.7049 0.8628 0.1346 0.151 Uiso 1 1 calc R . .
H8B H 0.6748 0.9412 0.0714 0.151 Uiso 1 1 calc R . .
H8C H 0.6757 0.9572 0.1641 0.151 Uiso 1 1 calc R . .
C9 C 0.842(3) 1.0247(15) 0.3990(17) 0.178(15) Uani 1 1 d . . .
H9A H 0.7801 0.9994 0.4448 0.266 Uiso 1 1 calc R . .
H9B H 0.8171 1.0859 0.3919 0.266 Uiso 1 1 calc R . .
H9C H 0.9142 1.0137 0.4140 0.266 Uiso 1 1 calc R . .
C10 C 0.961(2) 1.0469(12) 0.2370(15) 0.107(7) Uani 1 1 d . . .
H10A H 1.0161 1.0549 0.2652 0.161 Uiso 1 1 calc R . .
H10B H 0.9151 1.1018 0.2269 0.161 Uiso 1 1 calc R . .
H10C H 1.0049 1.0225 0.1820 0.161 Uiso 1 1 calc R . .
C11 C 1.268(2) 0.8350(17) 0.0184(15) 0.128(9) Uani 1 1 d . . .
H11A H 1.2865 0.7738 0.0124 0.192 Uiso 1 1 calc R . .
H11B H 1.3400 0.8602 -0.0071 0.192 Uiso 1 1 calc R . .
H11C H 1.2115 0.8606 -0.0112 0.192 Uiso 1 1 calc R . .
C12 C 1.343(3) 0.820(3) 0.152(3) 0.22(2) Uani 1 1 d . . .
C13 C 1.081(4) 0.643(2) 0.494(2) 0.24(2) Uani 1 1 d . . .
H13A H 1.0699 0.6635 0.5490 0.353 Uiso 1 1 calc R . .
H13B H 1.1583 0.6078 0.4735 0.353 Uiso 1 1 calc R . .
H13C H 1.0198 0.6087 0.5003 0.353 Uiso 1 1 calc R . .
C14 C 1.020(4) 0.8072(17) 0.488(2) 0.34(3) Uani 1 1 d DU . .
H14A H 1.0241 0.8625 0.4556 0.512 Uiso 1 1 calc R . .
H14B H 1.0676 0.8004 0.5260 0.512 Uiso 1 1 calc R . .
H14C H 0.9379 0.8036 0.5230 0.512 Uiso 1 1 calc R . .
C15 C 1.261(3) 0.5623(18) 0.1027(18) 0.150(10) Uani 1 1 d U . .
H15A H 1.2128 0.5410 0.0762 0.224 Uiso 1 1 calc R . .
H15B H 1.3263 0.5179 0.1064 0.224 Uiso 1 1 calc R . .
H15C H 1.2919 0.6118 0.0677 0.224 Uiso 1 1 calc R . .
C16 C 1.1760(18) 0.4911(12) 0.2671(16) 0.105(7) Uani 1 1 d . . .
H16A H 1.1095 0.4955 0.3206 0.157 Uiso 1 1 calc R . .
H16B H 1.2495 0.4757 0.2804 0.157 Uiso 1 1 calc R . .
H16C H 1.1689 0.4474 0.2343 0.157 Uiso 1 1 calc R . .
O1 O 0.8027(8) 0.6481(5) 0.3344(6) 0.055(2) Uani 1 1 d . . .
O2 O 0.7184(8) 0.8299(6) 0.3230(7) 0.069(3) Uani 1 1 d . . .
O3 O 0.8309(9) 0.7193(6) 0.1447(6) 0.061(2) Uani 1 1 d . . .
O4 O 0.9204(11) 0.8824(6) 0.1348(7) 0.073(3) Uani 1 1 d . . .
O5 O 0.9412(9) 0.8931(5) 0.3080(6) 0.058(2) Uani 1 1 d . . .
O6 O 1.1355(9) 0.7824(7) 0.1722(8) 0.078(3) Uani 1 1 d . . .
O7 O 1.0078(10) 0.7093(6) 0.3681(7) 0.066(3) Uani 1 1 d . . .
O8 O 1.0489(9) 0.6196(6) 0.1984(9) 0.080(3) Uani 1 1 d . . .
S1 S 0.8136(3) 0.5627(2) 0.3854(3) 0.0585(9) Uani 1 1 d . . .
S2 S 0.6094(3) 0.8035(2) 0.3930(3) 0.0614(9) Uani 1 1 d . . .
S3 S 0.7848(5) 0.6401(3) 0.1384(3) 0.0758(12) Uani 1 1 d . . .
S4 S 0.8647(6) 0.9317(3) 0.0707(3) 0.0945(16) Uani 1 1 d . . .
S5 S 0.8678(4) 0.9794(2) 0.3018(3) 0.0671(10) Uani 1 1 d . . .
S6 S 1.2051(4) 0.8541(3) 0.1311(3) 0.0800(13) Uani 1 1 d . . .
S7 S 1.0712(14) 0.7287(7) 0.4188(8) 0.250(8) Uani 1 1 d DU . .
S8 S 1.1759(4) 0.5908(3) 0.2048(3) 0.0835(12) Uani 1 1 d U . .


_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 I1 2.9144(11) . ?
Bi1 I2 2.9459(10) . ?
Bi1 I3 2.9493(13) . ?
Bi1 I5 3.2002(10) . ?
Bi1 I4 3.2345(11) . ?
Bi1 I6 3.3072(11) . ?
Bi2 I8 2.9369(12) . ?
Bi2 I9 2.9951(10) . ?
Bi2 I7 3.0104(12) . ?
Bi2 I6 3.1386(11) . ?
Bi2 I4 3.1895(10) . ?
Bi2 I5 3.2577(11) . ?
La1 O7 2.448(9) . ?
La1 O2 2.468(9) . ?
La1 O1 2.476(8) . ?
La1 O6 2.484(10) . ?
La1 O8 2.490(9) . ?
La1 O5 2.500(8) . ?
La1 O4 2.501(9) . ?
La1 O3 2.540(9) . ?
C1 S1 1.773(16) . ?
C2 S1 1.746(15) . ?
C3 S2 1.74(2) . ?
C4 S2 1.751(17) . ?
C5 S3 1.75(2) . ?
C6 S3 1.81(2) . ?
C7 S4 1.795(19) . ?
C8 S4 1.75(2) . ?
C9 S5 1.73(2) . ?
C10 S5 1.69(2) . ?
C11 S6 1.77(2) . ?
C12 S6 1.78(3) . ?
C13 S7 1.71(3) . ?
C14 S7 1.676(18) . ?
C15 S8 1.70(3) . ?
C16 S8 1.753(19) . ?
O1 S1 1.493(9) . ?
O2 S2 1.500(10) . ?
O3 S3 1.491(10) . ?
O4 S4 1.482(9) . ?
O5 S5 1.486(9) . ?
O6 S6 1.486(10) . ?
O7 S7 1.396(11) . ?
O8 S8 1.542(11) . ?

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
I1 Bi1 I2 95.52(3) . . ?
I1 Bi1 I3 95.54(4) . . ?
I2 Bi1 I3 91.32(4) . . ?
I1 Bi1 I5 93.06(3) . . ?
I2 Bi1 I5 169.34(3) . . ?
I3 Bi1 I5 94.14(4) . . ?
I1 Bi1 I4 91.62(3) . . ?
I2 Bi1 I4 88.78(3) . . ?
I3 Bi1 I4 172.79(4) . . ?
I5 Bi1 I4 84.66(3) . . ?
I1 Bi1 I6 169.69(3) . . ?
I2 Bi1 I6 90.71(3) . . ?
I3 Bi1 I6 92.52(4) . . ?
I5 Bi1 I6 79.92(3) . . ?
I4 Bi1 I6 80.28(3) . . ?
I8 Bi2 I9 93.48(4) . . ?
I8 Bi2 I7 95.07(4) . . ?
I9 Bi2 I7 96.56(3) . . ?
I8 Bi2 I6 92.71(4) . . ?
I9 Bi2 I6 88.80(3) . . ?
I7 Bi2 I6 170.26(3) . . ?
I8 Bi2 I4 90.24(3) . . ?
I9 Bi2 I4 171.68(3) . . ?
I7 Bi2 I4 90.52(3) . . ?
I6 Bi2 I4 83.58(3) . . ?
I8 Bi2 I5 172.60(3) . . ?
I9 Bi2 I5 91.13(3) . . ?
I7 Bi2 I5 90.14(3) . . ?
I6 Bi2 I5 81.60(3) . . ?
I4 Bi2 I5 84.45(3) . . ?
Bi2 I4 Bi1 81.21(2) . . ?
Bi1 I5 Bi2 80.69(2) . . ?
Bi2 I6 Bi1 80.83(2) . . ?
O7 La1 O2 104.4(4) . . ?
O7 La1 O1 76.6(3) . . ?
O2 La1 O1 70.7(3) . . ?
O7 La1 O6 80.6(4) . . ?
O2 La1 O6 145.5(3) . . ?
O1 La1 O6 141.9(3) . . ?
O7 La1 O8 78.5(4) . . ?
O2 La1 O8 143.6(3) . . ?
O1 La1 O8 75.0(3) . . ?
O6 La1 O8 70.9(3) . . ?
O7 La1 O5 74.1(3) . . ?
O2 La1 O5 73.1(3) . . ?
O1 La1 O5 125.1(3) . . ?
O6 La1 O5 75.7(4) . . ?
O8 La1 O5 139.5(3) . . ?
O7 La1 O4 141.2(3) . . ?
O2 La1 O4 83.6(4) . . ?
O1 La1 O4 139.9(3) . . ?
O6 La1 O4 73.0(4) . . ?
O8 La1 O4 117.3(4) . . ?
O5 La1 O4 72.2(3) . . ?
O7 La1 O3 146.3(3) . . ?
O2 La1 O3 83.4(4) . . ?
O1 La1 O3 75.3(3) . . ?
O6 La1 O3 111.6(4) . . ?
O8 La1 O3 76.6(4) . . ?
O5 La1 O3 138.4(3) . . ?
O4 La1 O3 71.5(3) . . ?
S1 O1 La1 140.9(5) . . ?
S2 O2 La1 136.3(6) . . ?
S3 O3 La1 133.4(5) . . ?
S4 O4 La1 149.5(7) . . ?
S5 O5 La1 125.3(6) . . ?
S6 O6 La1 139.5(6) . . ?
S7 O7 La1 146.2(7) . . ?
S8 O8 La1 122.5(6) . . ?
O1 S1 C2 106.0(7) . . ?
O1 S1 C1 107.3(7) . . ?
C2 S1 C1 97.5(7) . . ?
O2 S2 C3 102.3(9) . . ?
O2 S2 C4 105.0(7) . . ?
C3 S2 C4 97.4(14) . . ?
O3 S3 C5 105.3(10) . . ?
O3 S3 C6 105.5(9) . . ?
C5 S3 C6 97.7(16) . . ?
O4 S4 C8 105.2(8) . . ?
O4 S4 C7 107.3(9) . . ?
C8 S4 C7 98.5(10) . . ?
O5 S5 C10 107.5(9) . . ?
O5 S5 C9 105.9(10) . . ?
C10 S5 C9 96.3(13) . . ?
O6 S6 C11 104.9(10) . . ?
O6 S6 C12 104.1(12) . . ?
C11 S6 C12 94.1(17) . . ?
O7 S7 C14 123.6(18) . . ?
O7 S7 C13 107.9(12) . . ?
C14 S7 C13 98.1(19) . . ?
O8 S8 C15 104.1(12) . . ?
O8 S8 C16 107.3(8) . . ?
C15 S8 C16 102.3(13) . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         3.395
_refine_diff_density_min         -3.578
_refine_diff_density_rms         0.540
_chemical_properties_physical    Heat-sensitive
