# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_PhaseI
_database_code_depnum_ccdc_archive 'CCDC 2263854'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2023-05-18 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT084_PhaseI              
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.38 Report
RESPONSE: due to high, temperature induced disorder
;
_vrf_PLAT196_PhaseI              
;
PROBLEM: No TEMP record and _measurement_temperature .NE.        293 Degree
RESPONSE: the hydrogen atom were not included into refinement
;
_vrf_PLAT242_PhaseI              
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Bi1 Check 
RESPONSE: due to high, temperature induced disorder of iodide ligands
;
# end Validation Reply Form
_audit_creation_date             2022-04-27
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(Bi1 I4.5), 0.75(C4), 2(C3 S1), 0.083(S12)'
_chemical_formula_sum            'C9 Bi2 I9 S3'
_chemical_formula_weight         1764.33
_chemical_melting_point          ?
_chemical_oxdiff_formula         Bi2I9S3C9H9
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'
C C 0.0033 0.0016 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
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'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-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'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   9.7593(10)
_cell_length_b                   9.7593(10)
_cell_length_c                   23.153(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1909.8(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    734
_cell_measurement_temperature    325.01(10)
_cell_measurement_theta_max      17.6640
_cell_measurement_theta_min      2.9760
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    3.068
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1490
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5576
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.258
_diffrn_reflns_theta_min         2.565
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      325.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -1.00  51.00   1.00   35.00    --   13.31 -99.00 120.00   52
  2  ω     -7.00  66.00   1.00   35.00    --   13.31  57.00-120.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0590043000
_diffrn_orient_matrix_UB_12      0.0460542000
_diffrn_orient_matrix_UB_13      0.0206301000
_diffrn_orient_matrix_UB_21      -0.0430375000
_diffrn_orient_matrix_UB_22      -0.0575026000
_diffrn_orient_matrix_UB_23      0.0214710000
_diffrn_orient_matrix_UB_31      0.0414410000
_diffrn_orient_matrix_UB_32      -0.0402186000
_diffrn_orient_matrix_UB_33      -0.0071270000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                294
_reflns_number_total             981
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.406
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         981
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.2188
_refine_ls_R_factor_gt           0.0878
_refine_ls_restrained_S_all      3.355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1808P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2820
_refine_ls_wR_factor_ref         0.3753
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 S1-C1
 1.8 with sigma of 0.001
 S3-C1
 1.8 with sigma of 0.001
 S2-C2
 1.8 with sigma of 0.003
2. Others
 Fixed Sof: C2(0.25) C1(0.5) S1(0.08333) S3(0.08333) S2(0.08333)
3.a Everything fixed:
 C2, C1, S1, S3, S2
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.666667 0.333333 0.65806(10) 0.1489(15) Uani 1 6 d S T P . .
I1 I 0.52140(16) 0.47860(16) 0.750000 0.188(2) Uani 1 4 d S T P . .
I2 I 0.3749(5) 0.1874(3) 0.5905(2) 0.277(3) Uani 1 2 d S T P . .
C2 C -0.181150 -0.065070 0.756250 0.304 Uani 0.25 1 d D . P . .
C1 C 0.477290 0.217350 0.417830 0.304 Uani 0.5 1 d D . P . .
S1 S 0.666667 0.333333 0.374550 0.250 Uani 0.5 6 d DS T P . .
S3 S 0.666667 0.333333 0.450870 0.250 Uani 0.5 6 d DS T P . .
S2 S 0.000000 0.000000 0.712520 0.250 Uani 0.5 6 d DS T 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 I1 3.250(3) 2_655 ?
Bi1 I1 3.250(3) . ?
Bi1 I1 3.250(3) 3_665 ?
Bi1 I2 2.920(3) 2_655 ?
Bi1 I2 2.920(3) 3_665 ?
Bi1 I2 2.920(3) . ?
C2 S2 1.7114 16_557 ?
C2 S2 1.8524 . ?
C1 S1 1.8998 . ?
C1 S3 1.7861 . ?
S1 S3 1.7671 . ?
S2 S2 1.7357 16_557 ?

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 I1 81.74(7) 2_655 . ?
I1 Bi1 I1 81.74(7) 3_665 2_655 ?
I1 Bi1 I1 81.74(7) 3_665 . ?
I2 Bi1 I1 91.81(9) 2_655 2_655 ?
I2 Bi1 I1 171.45(13) 2_655 . ?
I2 Bi1 I1 171.45(13) . 3_665 ?
I2 Bi1 I1 91.81(9) 3_665 . ?
I2 Bi1 I1 91.81(9) 3_665 3_665 ?
I2 Bi1 I1 91.81(9) 2_655 3_665 ?
I2 Bi1 I1 91.81(9) . 2_655 ?
I2 Bi1 I1 171.45(13) 3_665 2_655 ?
I2 Bi1 I1 91.81(9) . . ?
I2 Bi1 I2 94.01(16) . 3_665 ?
I2 Bi1 I2 94.01(16) 2_655 . ?
I2 Bi1 I2 94.01(16) 2_655 3_665 ?
Bi1 I1 Bi1 81.85(9) . 16_557 ?



_olex2_date_sample_data_collection 2021-04-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 324.231
_oxdiff_exptl_absorpt_empirical_full_min 0.187
####################################################################### 
# 
# 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_PhaseII
_database_code_depnum_ccdc_archive 'CCDC 2263856'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2023-05-18 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT315_PhaseII             
;
PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing).       C4AA Check 
RESPONSE: carbon atom from disordered molecule
;
_vrf_PLAT910_PhaseII             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         15 Note  
RESPONSE: large monoclinic unit cell, refinement on dominating twin domain 
;
# end Validation Reply Form
_audit_creation_date             2023-05-16
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Bi2 I9.008, 0.5(C3 H9 S), 0.5(C3 H9 S0.8), 0.5(C3 H9 S0.7), 0.25(C S), 0.25(C6 S2), 0.5(C3 H9 S0.45), 0.525(S), 0.5(C2.5 H7.5 S0.5)'
_chemical_formula_sum            'C9 H21.75 Bi2 I9 S3'
_chemical_formula_weight         1786.57
_chemical_melting_point          ?
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'
Bi Bi -4.1077 10.2566 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.0052(4)
_cell_length_b                   33.1993(8)
_cell_length_c                   22.8970(6)
_cell_angle_alpha                90
_cell_angle_beta                 91.878(2)
_cell_angle_gamma                90
_cell_volume                     14439.3(6)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    16550
_cell_measurement_temperature    199.8(4)
_cell_measurement_theta_max      27.6490
_cell_measurement_theta_min      2.7360
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    17.608
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    3.287
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?

_exptl_crystal_F_000             12270
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            49649
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.602
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00  84.20   0.80   35.00    --   13.31  77.00  60.00  134
  2  ω     -1.00  94.20   0.80   35.00    --   13.31  77.00 -90.00  119
  3  ω    -47.00  57.00   0.80   35.00    --  -14.40  77.00 150.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0278542000
_diffrn_orient_matrix_UB_12      -0.0033681000
_diffrn_orient_matrix_UB_13      0.0208137000
_diffrn_orient_matrix_UB_21      -0.0248630000
_diffrn_orient_matrix_UB_22      -0.0035596000
_diffrn_orient_matrix_UB_23      0.0218311000
_diffrn_orient_matrix_UB_31      -0.0002565000
_diffrn_orient_matrix_UB_32      -0.0208006000
_diffrn_orient_matrix_UB_33      -0.0071114000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10712
_reflns_number_total             13689
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.808
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.287
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         13689
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0484
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0215P)²+456.2979P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1004
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 S11-C8A \\sim S11-C7A \\sim S11-C5A
 with sigma of 0.02
 S12-C8A \\sim S12-C7A \\sim S12-C5A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C8A) = Uiso(C7A) = Uiso(C5A)
4. Others
 Fixed Sof: S2(0.8) S3(0.7) S4(0.5) S5(0.5) S6(0.45) S7(0.3) S8(0.5) S9(0.2)
 C2AA(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5) S10(0.55) C5AA(0.5) S11(0.25)
 S12(0.25) C8A(0.5) C1(0.5) C5AB(0.5) C7A(0.5) C5A(0.5)
5.a Me refined with riding coordinates:
 C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C012(H01M,H01N,H01O), C013(H01G,
 H01H,H01I), C015(H01J,H01K,H01L), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,
 H9C), C10(H10A,H10B,H10C), C2(H2A,H2B,H2C), C2AA(H2AA,H2AB,H2AC), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.26096(3) 0.58848(2) 0.83275(2) 0.02971(13) Uani 1 1 d . . . . .
Bi2 Bi 0.49379(3) 0.32754(2) 0.65714(2) 0.03029(13) Uani 1 1 d . . . . .
Bi3 Bi 0.25069(3) 0.57799(2) 0.64666(2) 0.03197(13) Uani 1 1 d . . . . .
Bi4 Bi 0.48277(3) 0.16253(2) 0.34144(2) 0.03125(13) Uani 1 1 d . . . . .
I1 I 0.35148(5) 0.63172(3) 0.73268(4) 0.0340(2) Uani 1 1 d . . . . .
I2 I 0.12839(5) 0.60415(3) 0.73984(4) 0.0353(2) Uani 1 1 d . . . . .
I3 I 0.58409(5) 0.19319(3) 0.43217(4) 0.0397(2) Uani 1 1 d . . . . .
I4 I 0.500000 0.25732(4) 0.750000 0.0388(3) Uani 1 2 d S T P . .
I5 I 0.61167(5) 0.12651(3) 0.26832(4) 0.0397(2) Uani 1 1 d . . . . .
I6 I 0.25194(5) 0.66924(3) 0.88609(4) 0.0388(2) Uani 1 1 d . . . . .
I7 I 0.50116(5) 0.39327(3) 0.56881(4) 0.0398(2) Uani 1 1 d . . . . .
I8 I 0.60637(5) 0.37376(3) 0.74650(4) 0.0408(2) Uani 1 1 d . . . . .
I9 I 0.35940(5) 0.20373(3) 0.38890(5) 0.0430(2) Uani 1 1 d . . . . .
I10 I 0.38744(5) 0.56481(3) 0.90229(4) 0.0434(2) Uani 1 1 d . . . . .
I11 I 0.59882(5) 0.27990(3) 0.59433(4) 0.0428(2) Uani 1 1 d . . . . .
I12 I 0.37124(5) 0.28565(3) 0.60292(4) 0.0428(2) Uani 1 1 d . . . . .
I13 I 0.15761(5) 0.52347(3) 0.57791(4) 0.0423(2) Uani 1 1 d . . . . .
I14 I 0.46334(5) 0.08658(3) 0.40594(5) 0.0422(2) Uani 1 1 d . . . . .
I15 I 0.21477(5) 0.64939(3) 0.57497(4) 0.0435(2) Uani 1 1 d . . . . .
I16 I 0.2778(3) 0.50922(5) 0.74832(9) 0.0405(9) Uani 0.930(19) 1 d . . . . .
I17 I 0.16726(5) 0.54905(3) 0.91640(5) 0.0461(3) Uani 1 1 d . . . . .
I18 I 0.37895(5) 0.55867(3) 0.58354(5) 0.0472(3) Uani 1 1 d . . . . .
I19 I 0.500000 0.23688(4) 0.250000 0.0495(4) Uani 1 2 d S T P . .
S1 S 0.7713(2) 0.24156(12) 0.74385(17) 0.0424(9) Uani 1 1 d . . . . .
S2 S 0.3098(2) 0.39993(14) 0.6040(2) 0.0373(11) Uiso 0.8 1 d . . P A 1
S3 S 0.5081(3) 0.29643(17) 0.3993(2) 0.0434(14) Uani 0.7 1 d . . P B 1
S4 S 0.0514(3) 0.63999(17) 0.8969(3) 0.0182(12) Uiso 0.5 1 d . . P C -1
S5 S 0.4690(4) 0.5006(3) 0.7454(6) 0.074(3) Uani 0.5 1 d . . P . .
S6 S 0.2455(5) 0.5802(3) 0.3764(4) 0.050(2) Uiso 0.45 1 d . . P D 1
S7 S 0.5003(6) 0.3401(4) 0.4232(5) 0.038(3) Uani 0.3 1 d . . P B -1
S8 S -0.0089(8) 0.6648(5) 0.9181(7) 0.117(5) Uiso 0.5 1 d . . P C 1
C010 C 0.7365(9) 0.2902(5) 0.7471(7) 0.059(5) Uani 1 1 d . . . . .
H01A H 0.774898 0.309696 0.752741 0.088 Uiso 1 1 calc R U . . .
H01B H 0.710275 0.296241 0.710605 0.088 Uiso 1 1 calc R U . . .
H01C H 0.704767 0.292070 0.779936 0.088 Uiso 1 1 calc R U . . .
C011 C 0.6932(8) 0.2129(5) 0.7338(7) 0.051(4) Uani 1 1 d . . . . .
H01D H 0.705172 0.184290 0.731210 0.077 Uiso 1 1 calc R U . . .
H01E H 0.662854 0.217245 0.767064 0.077 Uiso 1 1 calc R U . . .
H01F H 0.668362 0.221416 0.697733 0.077 Uiso 1 1 calc R U . . .
C012 C 0.1696(8) 0.5748(6) 0.4202(8) 0.067(5) Uani 1 1 d . . . D 1
H01M H 0.132188 0.592725 0.405345 0.101 Uiso 1 1 calc R U . D 1
H01N H 0.153123 0.546826 0.418335 0.101 Uiso 1 1 calc R U . D 1
H01O H 0.182054 0.581818 0.460771 0.101 Uiso 1 1 calc R U . D 1
C013 C 0.2715(10) 0.3823(6) 0.5388(7) 0.069(5) Uani 1 1 d . . . A 1
H01G H 0.308279 0.377630 0.510496 0.103 Uiso 1 1 calc R U . A 1
H01H H 0.246830 0.356921 0.546036 0.103 Uiso 1 1 calc R U . A 1
H01I H 0.238002 0.402244 0.523152 0.103 Uiso 1 1 calc R U . A 1
S9 S 0.2383(9) 0.4215(5) 0.5708(8) 0.031(4) Uiso 0.2 1 d . . P A -1
C015 C 0.4515(9) 0.2980(6) 0.4591(7) 0.061(5) Uani 1 1 d . . . B 1
H01J H 0.469237 0.279635 0.489746 0.091 Uiso 1 1 calc R U . B 1
H01K H 0.449966 0.325462 0.474587 0.091 Uiso 1 1 calc R U . B 1
H01L H 0.404083 0.289658 0.446113 0.091 Uiso 1 1 calc R U . B 1
C6 C 0.0762(10) 0.6651(6) 0.9638(8) 0.081(6) Uani 1 1 d . . . C 1
H6A H 0.065367 0.663562 1.005319 0.121 Uiso 1 1 calc R U . C 1
H6B H 0.105039 0.641959 0.953288 0.121 Uiso 1 1 calc R U . C 1
H6C H 0.102049 0.690079 0.956510 0.121 Uiso 1 1 calc R U . C 1
C7 C 0.5827(9) 0.3231(6) 0.4285(8) 0.075(6) Uani 1 1 d . . . B 1
H7A H 0.608211 0.306000 0.457032 0.112 Uiso 1 1 calc R U . B 1
H7B H 0.613934 0.330112 0.396853 0.112 Uiso 1 1 calc R U . B 1
H7C H 0.567082 0.347693 0.447775 0.112 Uiso 1 1 calc R U . B 1
C9 C -0.0174(8) 0.6087(5) 0.9226(9) 0.066(6) Uani 1 1 d . . . C 1
H9A H -0.037001 0.601367 0.960214 0.099 Uiso 1 1 calc R U . C 1
H9B H -0.048747 0.599138 0.890760 0.099 Uiso 1 1 calc R U . C 1
H9C H 0.029101 0.596340 0.919294 0.099 Uiso 1 1 calc R U . C 1
C10 C 0.8017(9) 0.2430(6) 0.6703(8) 0.065(5) Uani 1 1 d . . . . .
H10A H 0.823457 0.217156 0.660836 0.098 Uiso 1 1 calc R U . . .
H10B H 0.761748 0.248046 0.643086 0.098 Uiso 1 1 calc R U . . .
H10C H 0.836420 0.264629 0.666786 0.098 Uiso 1 1 calc R U . . .
C12 C 0.2373(9) 0.4062(6) 0.6478(8) 0.065(5) Uani 1 1 d . . . A 1
H12A H 0.200294 0.420889 0.625921 0.097 Uiso 1 1 calc R U . A 1
H12B H 0.251407 0.421456 0.682867 0.097 Uiso 1 1 calc R U . A 1
H12C H 0.219458 0.379727 0.659157 0.097 Uiso 1 1 calc R U . A 1
C2 C 0.2757(10) 0.6279(6) 0.4057(11) 0.095(8) Uani 1 1 d . . . D 1
H2A H 0.244727 0.649515 0.391082 0.142 Uiso 1 1 calc R U . D 1
H2B H 0.274969 0.627145 0.448504 0.142 Uiso 1 1 calc R U . D 1
H2C H 0.323874 0.632995 0.393557 0.142 Uiso 1 1 calc R U . D 1
C2AA C 0.024(2) 0.6677(12) 0.8520(17) 0.068(11) Uiso 0.5 1 d . . P C 1
H2AA H 0.032582 0.696003 0.842062 0.102 Uiso 0.5 1 calc R U P C 1
H2AB H 0.069176 0.652997 0.851726 0.102 Uiso 0.5 1 calc R U P C 1
H2AC H -0.008672 0.655795 0.823191 0.102 Uiso 0.5 1 calc R U P C 1
S10 S 0.2558(4) 0.5825(2) 0.4457(3) 0.0413(16) Uiso 0.55 1 d . . P D -1
C3 C 0.3245(9) 0.4508(5) 0.5831(10) 0.085(7) Uani 1 1 d . . . A 1
H3A H 0.346576 0.465485 0.616035 0.127 Uiso 1 1 calc R U . A 1
H3B H 0.355631 0.451425 0.549851 0.127 Uiso 1 1 calc R U . A 1
H3C H 0.279477 0.463469 0.572044 0.127 Uiso 1 1 calc R U . A 1
C4 C 0.3074(9) 0.5466(6) 0.4078(11) 0.091(8) Uani 1 1 d . . . D 1
H4A H 0.350975 0.547775 0.386100 0.137 Uiso 1 1 calc R U . D 1
H4B H 0.317369 0.554167 0.448604 0.137 Uiso 1 1 calc R U . D 1
H4C H 0.288438 0.519175 0.406168 0.137 Uiso 1 1 calc R U . D 1
C5AA C 0.5196(19) 0.4777(10) 0.6883(15) 0.048(9) Uiso 0.5 1 d . . P E 1
C8 C 0.4695(10) 0.3298(6) 0.3507(8) 0.079(6) Uani 1 1 d . . . B 1
H8A H 0.497238 0.331221 0.315409 0.118 Uiso 1 1 calc R U . B 1
H8B H 0.421636 0.320770 0.340218 0.118 Uiso 1 1 calc R U . B 1
H8C H 0.467518 0.356573 0.368692 0.118 Uiso 1 1 calc R U . B 1
C4AA C 0.500000 0.5491(6) 0.750000 0.062(7) Uani 1 2 d S T P E .
S11 S 0.000000 0.5179(4) 0.750000 0.061(3) Uiso 0.5 2 d DS . P . .
S12 S 0.000000 0.4752(4) 0.750000 0.055(3) Uiso 0.5 2 d DS . P F .
C8A C -0.008(4) 0.4960(11) 0.6821(14) 0.150(14) Uiso 0.5 1 d D . P F 1
I1A I 0.250(3) 0.5070(7) 0.7525(10) 0.048(7) Uiso 0.079(18) 1 d . . . . .
C1 C -0.004(2) 0.6804(11) 0.8639(17) 0.059(10) Uiso 0.5 1 d . . P C -1
C5AB C 0.484(2) 0.4767(12) 0.6866(18) 0.062(11) Uiso 0.5 1 d . . P E 2
C7A C -0.0791(18) 0.4918(11) 0.731(3) 0.150(14) Uiso 0.5 1 d D . P F 2
C5A C -0.077(2) 0.4913(11) 0.770(3) 0.150(14) Uiso 0.5 1 d D . P F 2


_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 3.2448(10) . ?
Bi1 I2 3.2852(10) . ?
Bi1 I6 2.9534(10) . ?
Bi1 I10 2.9463(11) . ?
Bi1 I16 3.2870(16) . ?
Bi1 I17 2.9626(11) . ?
Bi1 I1A 3.27(2) . ?
Bi2 I4 3.1550(11) . ?
Bi2 I7 2.9816(11) . ?
Bi2 I8 3.3349(11) 2_656 ?
Bi2 I8 3.2913(11) . ?
Bi2 I11 2.9567(11) . ?
Bi2 I12 2.9514(11) . ?
Bi3 I1 3.2378(10) . ?
Bi3 I2 3.3217(11) . ?
Bi3 I13 2.9497(11) . ?
Bi3 I15 2.9508(11) . ?
Bi3 I16 3.2890(17) . ?
Bi3 I18 2.9449(11) . ?
Bi3 I1A 3.38(2) . ?
Bi4 I3 2.9660(11) . ?
Bi4 I5 3.2667(11) 2_655 ?
Bi4 I5 3.2409(11) . ?
Bi4 I9 2.9523(11) . ?
Bi4 I14 2.9515(11) . ?
Bi4 I19 3.2603(12) . ?
I16 I1A 0.54(5) . ?
S1 C010 1.749(17) . ?
S1 C011 1.771(14) . ?
S1 C10 1.800(16) . ?
S2 C013 1.741(17) . ?
S2 S9 1.694(17) . ?
S2 C12 1.743(17) . ?
S2 C3 1.779(17) . ?
S3 S7 1.559(13) . ?
S3 C015 1.770(16) . ?
S3 C7 1.783(17) . ?
S3 C8 1.718(18) . ?
S4 S8 1.505(16) . ?
S4 C6 1.79(2) . ?
S4 C9 1.784(16) . ?
S4 C2AA 1.46(4) . ?
S4 C1 1.85(4) . ?
S5 S5 1.189(17) 2_656 ?
S5 C5AA 1.71(4) 2_656 ?
S5 C5AA 1.82(4) . ?
S5 C4AA 1.72(2) . ?
S5 C5AB 1.60(4) . ?
S5 C5AB 1.94(4) 2_656 ?
S6 C012 1.791(19) . ?
S6 C2 1.81(2) . ?
S6 S10 1.594(12) . ?
S6 C4 1.76(2) . ?
S7 C015 1.88(2) . ?
S7 C7 1.67(2) . ?
S7 C8 1.78(2) . ?
S8 C6 1.90(2) . ?
S8 C9 1.87(2) . ?
S8 C2AA 1.66(4) . ?
S8 C1 1.35(4) . ?
C010 H01A 0.9800 . ?
C010 H01B 0.9800 . ?
C010 H01C 0.9800 . ?
C011 H01D 0.9800 . ?
C011 H01E 0.9800 . ?
C011 H01F 0.9800 . ?
C012 H01M 0.9800 . ?
C012 H01N 0.9800 . ?
C012 H01O 0.9800 . ?
C012 S10 1.739(18) . ?
C013 H01G 0.9800 . ?
C013 H01H 0.9800 . ?
C013 H01I 0.9800 . ?
C013 S9 1.63(2) . ?
S9 C12 1.84(2) . ?
S9 C3 1.92(2) . ?
C015 H01J 0.9800 . ?
C015 H01K 0.9800 . ?
C015 H01L 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2 S10 1.81(2) . ?
C2AA H2AA 0.9800 . ?
C2AA H2AB 0.9800 . ?
C2AA H2AC 0.9800 . ?
C2AA C1 0.74(5) . ?
S10 C4 1.79(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
S11 S12 1.416(18) . ?
S11 C8A 1.72(3) 2_556 ?
S11 C8A 1.72(3) . ?
S11 C7A 1.78(3) 2_556 ?
S11 C7A 1.78(3) . ?
S11 C5A 1.79(3) . ?
S11 C5A 1.79(3) 2_556 ?
S12 C8A 1.70(3) 2_556 ?
S12 C8A 1.70(3) . ?
S12 C7A 1.64(3) . ?
S12 C7A 1.64(3) 2_556 ?
S12 C5A 1.64(3) . ?
S12 C5A 1.64(3) 2_556 ?
C7A C5A 0.89(9) . ?

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 83.44(3) . . ?
I1 Bi1 I16 82.81(8) . . ?
I1 Bi1 I1A 89.7(7) . . ?
I2 Bi1 I16 80.39(7) . . ?
I6 Bi1 I1 85.97(3) . . ?
I6 Bi1 I2 94.03(3) . . ?
I6 Bi1 I16 167.96(6) . . ?
I6 Bi1 I17 95.14(3) . . ?
I6 Bi1 I1A 168.3(6) . . ?
I10 Bi1 I1 93.30(3) . . ?
I10 Bi1 I2 170.76(3) . . ?
I10 Bi1 I6 94.36(3) . . ?
I10 Bi1 I16 90.64(7) . . ?
I10 Bi1 I17 91.71(3) . . ?
I10 Bi1 I1A 96.8(7) . . ?
I17 Bi1 I1 174.77(3) . . ?
I17 Bi1 I2 91.38(3) . . ?
I17 Bi1 I16 95.65(9) . . ?
I17 Bi1 I1A 88.3(7) . . ?
I1A Bi1 I2 74.6(7) . . ?
I1A Bi1 I16 9.4(9) . . ?
I4 Bi2 I8 85.20(2) . . ?
I4 Bi2 I8 84.47(2) . 2_656 ?
I7 Bi2 I4 175.13(3) . . ?
I7 Bi2 I8 92.09(3) . . ?
I7 Bi2 I8 98.77(3) . 2_656 ?
I8 Bi2 I8 75.39(3) . 2_656 ?
I11 Bi2 I4 85.50(3) . . ?
I11 Bi2 I7 90.81(3) . . ?
I11 Bi2 I8 96.68(3) . . ?
I11 Bi2 I8 167.69(3) . 2_656 ?
I12 Bi2 I4 86.95(3) . . ?
I12 Bi2 I7 96.52(3) . . ?
I12 Bi2 I8 92.03(3) . 2_656 ?
I12 Bi2 I8 165.74(3) . . ?
I12 Bi2 I11 94.55(3) . . ?
I1 Bi3 I2 82.97(3) . . ?
I1 Bi3 I16 82.89(6) . . ?
I1 Bi3 I1A 87.9(6) . . ?
I2 Bi3 I1A 72.8(7) . . ?
I13 Bi3 I1 174.38(3) . . ?
I13 Bi3 I2 94.77(3) . . ?
I13 Bi3 I15 94.14(3) . . ?
I13 Bi3 I16 91.66(7) . . ?
I13 Bi3 I1A 86.5(6) . . ?
I15 Bi3 I1 90.99(3) . . ?
I15 Bi3 I2 89.61(3) . . ?
I15 Bi3 I16 168.35(6) . . ?
I15 Bi3 I1A 162.3(8) . . ?
I16 Bi3 I2 79.83(9) . . ?
I16 Bi3 I1A 9.2(8) . . ?
I18 Bi3 I1 86.32(3) . . ?
I18 Bi3 I2 168.52(3) . . ?
I18 Bi3 I13 95.51(3) . . ?
I18 Bi3 I15 94.71(3) . . ?
I18 Bi3 I16 94.78(10) . . ?
I18 Bi3 I1A 102.8(8) . . ?
I3 Bi4 I5 90.23(3) . . ?
I3 Bi4 I5 172.82(3) . 2_655 ?
I3 Bi4 I19 96.51(3) . . ?
I5 Bi4 I5 82.71(3) . 2_655 ?
I5 Bi4 I19 81.61(2) . . ?
I9 Bi4 I3 95.08(3) . . ?
I9 Bi4 I5 169.72(3) . . ?
I9 Bi4 I5 91.71(3) . 2_655 ?
I9 Bi4 I19 89.04(3) . . ?
I14 Bi4 I3 91.82(3) . . ?
I14 Bi4 I5 93.00(3) . . ?
I14 Bi4 I5 89.86(3) . 2_655 ?
I14 Bi4 I9 95.61(3) . . ?
I14 Bi4 I19 170.07(3) . . ?
I19 Bi4 I5 81.22(2) . 2_655 ?
Bi3 I1 Bi1 82.48(2) . . ?
Bi1 I2 Bi3 80.60(2) . . ?
Bi2 I4 Bi2 84.72(4) 2_656 . ?
Bi4 I5 Bi4 81.77(3) . 2_655 ?
Bi2 I8 Bi2 79.82(3) . 2_656 ?
Bi1 I16 Bi3 81.06(3) . . ?
I1A I16 Bi1 84(2) . . ?
I1A I16 Bi3 95(3) . . ?
Bi4 I19 Bi4 81.58(4) 2_655 . ?
C010 S1 C011 100.6(8) . . ?
C010 S1 C10 98.6(8) . . ?
C011 S1 C10 100.8(8) . . ?
C013 S2 C12 102.6(9) . . ?
C013 S2 C3 98.9(10) . . ?
S9 S2 C013 56.7(9) . . ?
S9 S2 C12 64.6(8) . . ?
S9 S2 C3 67.0(9) . . ?
C12 S2 C3 100.1(9) . . ?
S7 S3 C015 68.5(8) . . ?
S7 S3 C7 59.4(8) . . ?
S7 S3 C8 65.4(9) . . ?
C015 S3 C7 101.0(8) . . ?
C8 S3 C015 103.0(9) . . ?
C8 S3 C7 104.0(11) . . ?
S8 S4 C6 69.6(9) . . ?
S8 S4 C9 68.8(9) . . ?
S8 S4 C1 46.0(13) . . ?
C6 S4 C1 98.1(14) . . ?
C9 S4 C6 99.4(9) . . ?
C9 S4 C1 98.3(13) . . ?
C2AA S4 S8 68.2(17) . . ?
C2AA S4 C6 112.6(18) . . ?
C2AA S4 C9 110.8(17) . . ?
C2AA S4 C1 22.2(18) . . ?
S5 S5 C5AA 75.3(16) 2_656 2_656 ?
S5 S5 C5AA 65.3(14) 2_656 . ?
S5 S5 C4AA 69.7(4) 2_656 . ?
S5 S5 C5AB 87.0(18) 2_656 . ?
S5 S5 C5AB 55.3(14) 2_656 2_656 ?
C5AA S5 C5AA 113(2) 2_656 . ?
C5AA S5 C4AA 109.4(14) 2_656 . ?
C5AA S5 C5AB 20.2(15) 2_656 2_656 ?
C5AA S5 C5AB 99.5(14) . 2_656 ?
C4AA S5 C5AA 104.4(12) . . ?
C4AA S5 C5AB 100.8(13) . 2_656 ?
C5AB S5 C4AA 116.7(16) . . ?
C012 S6 C2 97.6(10) . . ?
S10 S6 C012 61.5(7) . . ?
S10 S6 C2 63.9(9) . . ?
S10 S6 C4 64.2(9) . . ?
C4 S6 C012 104.3(11) . . ?
C4 S6 C2 101.7(11) . . ?
S3 S7 C015 61.1(7) . . ?
S3 S7 C7 67.0(8) . . ?
S3 S7 C8 61.6(8) . . ?
C7 S7 C015 101.0(11) . . ?
C7 S7 C8 106.4(11) . . ?
C8 S7 C015 96.5(10) . . ?
S4 S8 C6 62.4(9) . . ?
S4 S8 C9 62.7(8) . . ?
S4 S8 C2AA 54.7(16) . . ?
C9 S8 C6 92.8(11) . . ?
C2AA S8 C6 99.2(17) . . ?
C2AA S8 C9 98.3(17) . . ?
C1 S8 S4 80.7(19) . . ?
C1 S8 C6 115(2) . . ?
C1 S8 C9 116(2) . . ?
C1 S8 C2AA 26(2) . . ?
S1 C010 H01A 109.5 . . ?
S1 C010 H01B 109.5 . . ?
S1 C010 H01C 109.5 . . ?
H01A C010 H01B 109.5 . . ?
H01A C010 H01C 109.5 . . ?
H01B C010 H01C 109.5 . . ?
S1 C011 H01D 109.5 . . ?
S1 C011 H01E 109.5 . . ?
S1 C011 H01F 109.5 . . ?
H01D C011 H01E 109.5 . . ?
H01D C011 H01F 109.5 . . ?
H01E C011 H01F 109.5 . . ?
S6 C012 H01M 109.5 . . ?
S6 C012 H01N 109.5 . . ?
S6 C012 H01O 109.5 . . ?
H01M C012 H01N 109.5 . . ?
H01M C012 H01O 109.5 . . ?
H01N C012 H01O 109.5 . . ?
S10 C012 S6 53.6(6) . . ?
S10 C012 H01M 133.7 . . ?
S10 C012 H01N 116.8 . . ?
S10 C012 H01O 56.7 . . ?
S2 C013 H01G 109.5 . . ?
S2 C013 H01H 109.5 . . ?
S2 C013 H01I 109.5 . . ?
H01G C013 H01H 109.5 . . ?
H01G C013 H01I 109.5 . . ?
H01H C013 H01I 109.5 . . ?
S9 C013 S2 60.2(9) . . ?
S9 C013 H01G 135.7 . . ?
S9 C013 H01H 114.5 . . ?
S9 C013 H01I 50.7 . . ?
S2 S9 C12 59.0(8) . . ?
S2 S9 C3 58.6(8) . . ?
C013 S9 S2 63.1(9) . . ?
C013 S9 C12 103.1(12) . . ?
C013 S9 C3 97.5(12) . . ?
C12 S9 C3 92.0(12) . . ?
S3 C015 S7 50.4(6) . . ?
S3 C015 H01J 109.5 . . ?
S3 C015 H01K 109.5 . . ?
S3 C015 H01L 109.5 . . ?
S7 C015 H01J 127.7 . . ?
S7 C015 H01K 59.1 . . ?
S7 C015 H01L 122.6 . . ?
H01J C015 H01K 109.5 . . ?
H01J C015 H01L 109.5 . . ?
H01K C015 H01L 109.5 . . ?
S4 C6 S8 48.0(7) . . ?
S4 C6 H6A 138.2 . . ?
S4 C6 H6B 63.7 . . ?
S4 C6 H6C 111.5 . . ?
S8 C6 H6A 109.5 . . ?
S8 C6 H6B 109.5 . . ?
S8 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
S3 C7 H7A 109.5 . . ?
S3 C7 H7B 109.5 . . ?
S3 C7 H7C 109.5 . . ?
S7 C7 S3 53.6(7) . . ?
S7 C7 H7A 133.4 . . ?
S7 C7 H7B 117.1 . . ?
S7 C7 H7C 56.7 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
S4 C9 S8 48.5(6) . . ?
S4 C9 H9A 137.6 . . ?
S4 C9 H9B 112.2 . . ?
S4 C9 H9C 63.0 . . ?
S8 C9 H9A 109.5 . . ?
S8 C9 H9B 109.5 . . ?
S8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
S1 C10 H10A 109.5 . . ?
S1 C10 H10B 109.5 . . ?
S1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
S2 C12 S9 56.4(8) . . ?
S2 C12 H12A 109.5 . . ?
S2 C12 H12B 109.5 . . ?
S2 C12 H12C 109.5 . . ?
S9 C12 H12A 53.2 . . ?
S9 C12 H12B 129.3 . . ?
S9 C12 H12C 121.2 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
S6 C2 H2A 109.5 . . ?
S6 C2 H2B 109.5 . . ?
S6 C2 H2C 109.5 . . ?
S6 C2 S10 52.3(6) . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
S10 C2 H2A 130.5 . . ?
S10 C2 H2B 57.5 . . ?
S10 C2 H2C 120.0 . . ?
S4 C2AA S8 57.2(15) . . ?
S4 C2AA H2AA 135.5 . . ?
S4 C2AA H2AB 53.6 . . ?
S4 C2AA H2AC 115.0 . . ?
S8 C2AA H2AA 109.5 . . ?
S8 C2AA H2AB 109.5 . . ?
S8 C2AA H2AC 109.5 . . ?
H2AA C2AA H2AB 109.5 . . ?
H2AA C2AA H2AC 109.5 . . ?
H2AB C2AA H2AC 109.5 . . ?
C1 C2AA S4 110(5) . . ?
C1 C2AA S8 53(4) . . ?
C1 C2AA H2AA 70.2 . . ?
C1 C2AA H2AB 157.5 . . ?
C1 C2AA H2AC 91.1 . . ?
S6 S10 C012 64.8(7) . . ?
S6 S10 C2 63.8(9) . . ?
S6 S10 C4 62.4(8) . . ?
C012 S10 C2 99.4(10) . . ?
C012 S10 C4 105.3(10) . . ?
C4 S10 C2 100.5(11) . . ?
S2 C3 S9 54.4(7) . . ?
S2 C3 H3A 109.5 . . ?
S2 C3 H3B 109.5 . . ?
S2 C3 H3C 109.5 . . ?
S9 C3 H3A 135.0 . . ?
S9 C3 H3B 115.5 . . ?
S9 C3 H3C 56.3 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
S6 C4 S10 53.4(6) . . ?
S6 C4 H4A 109.5 . . ?
S6 C4 H4B 109.5 . . ?
S6 C4 H4C 109.5 . . ?
S10 C4 H4A 134.9 . . ?
S10 C4 H4B 57.2 . . ?
S10 C4 H4C 115.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
S5 C5AA S5 39.3(10) 2_656 . ?
S3 C8 S7 53.0(7) . . ?
S3 C8 H8A 109.5 . . ?
S3 C8 H8B 109.5 . . ?
S3 C8 H8C 109.5 . . ?
S7 C8 H8A 126.3 . . ?
S7 C8 H8B 124.2 . . ?
S7 C8 H8C 56.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
S5 C4AA S5 40.5(8) . 2_656 ?
S12 S11 C8A 65.0(13) . 2_556 ?
S12 S11 C8A 65.0(13) . . ?
S12 S11 C7A 60.8(12) . 2_556 ?
S12 S11 C7A 60.8(13) . . ?
S12 S11 C5A 60.4(12) . 2_556 ?
S12 S11 C5A 60.4(12) . . ?
C8A S11 C8A 130(3) 2_556 . ?
C8A S11 C7A 62(3) 2_556 2_556 ?
C8A S11 C7A 94(3) . 2_556 ?
C8A S11 C5A 88(3) 2_556 2_556 ?
C8A S11 C5A 67(3) . 2_556 ?
C7A S11 C7A 122(2) 2_556 . ?
C7A S11 C5A 29(3) 2_556 2_556 ?
C7A S11 C5A 113(2) . 2_556 ?
C7A S11 C5A 113(2) 2_556 . ?
C7A S11 C5A 29(3) . . ?
C5A S11 C5A 121(2) . 2_556 ?
S11 S12 C8A 66.1(13) . . ?
S11 S12 C8A 66.1(13) . 2_556 ?
S11 S12 C7A 70.5(14) . 2_556 ?
S11 S12 C7A 70.5(14) . . ?
S11 S12 C5A 71.0(14) . . ?
S11 S12 C5A 71.0(14) . 2_556 ?
C8A S12 C8A 132(3) . 2_556 ?
C5A S12 C7A 31(3) . . ?
C5A S12 C7A 130(3) 2_556 . ?
C5A S12 C5A 142(3) 2_556 . ?
S12 C8A S11 48.9(11) . . ?
Bi1 I1A Bi3 79.9(5) . . ?
I16 I1A Bi1 87(3) . . ?
I16 I1A Bi3 76(2) . . ?
S8 C1 S4 53.3(15) . . ?
C2AA C1 S4 48(4) . . ?
C2AA C1 S8 101(5) . . ?
S5 C5AB S5 37.7(10) . 2_656 ?
S12 C7A S11 48.7(11) . . ?
C5A C7A S11 76(2) . . ?
C5A C7A S12 74(2) . . ?
S12 C5A S11 48.6(11) . . ?
C7A C5A S11 74.9(19) . . ?
C7A C5A S12 74(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Bi1 I16 I1A Bi3 80.4(4) . . . . ?
Bi3 I16 I1A Bi1 -80.4(4) . . . . ?
S2 C013 S9 C12 -44.7(9) . . . . ?
S2 C013 S9 C3 49.1(9) . . . . ?
S4 S8 C2AA C1 -176(6) . . . . ?
S4 S8 C1 C2AA 3(5) . . . . ?
S4 C2AA C1 S8 -3(6) . . . . ?
S6 C012 S10 C2 55.1(9) . . . . ?
S6 C012 S10 C4 -48.7(10) . . . . ?
S6 C2 S10 C012 -55.8(9) . . . . ?
S6 C2 S10 C4 51.9(9) . . . . ?
S8 S4 C2AA C1 3(5) . . . . ?
S8 S4 C1 C2AA -176(7) . . . . ?
S8 C2AA C1 S4 3(6) . . . . ?
C012 S6 C2 S10 53.1(8) . . . . ?
C012 S6 S10 C2 -115.6(11) . . . . ?
C012 S6 S10 C4 125.1(11) . . . . ?
C012 S6 C4 S10 -47.9(9) . . . . ?
C012 S10 C4 S6 50.1(9) . . . . ?
C013 S2 S9 C12 126.9(12) . . . . ?
C013 S2 S9 C3 -118.7(12) . . . . ?
C013 S2 C12 S9 -43.2(10) . . . . ?
C013 S2 C3 S9 47.9(10) . . . . ?
C013 S9 C12 S2 47.0(10) . . . . ?
C015 S3 S7 C7 118.1(10) . . . . ?
C015 S3 S7 C8 -116.5(10) . . . . ?
C015 S3 C7 S7 -56.7(10) . . . . ?
C015 S3 C8 S7 58.7(9) . . . . ?
C015 S7 C7 S3 51.8(8) . . . . ?
C015 S7 C8 S3 -52.0(8) . . . . ?
C6 S4 S8 C9 -109.4(10) . . . . ?
C6 S4 S8 C2AA 126.2(19) . . . . ?
C6 S4 S8 C1 124.6(19) . . . . ?
C6 S4 C9 S8 63.7(10) . . . . ?
C6 S4 C2AA S8 -55.0(15) . . . . ?
C6 S4 C2AA C1 -52(6) . . . . ?
C6 S4 C1 S8 -51.2(16) . . . . ?
C6 S4 C1 C2AA 133(6) . . . . ?
C6 S8 C9 S4 -56.8(8) . . . . ?
C6 S8 C2AA S4 46.4(14) . . . . ?
C6 S8 C2AA C1 -130(5) . . . . ?
C6 S8 C1 S4 53.5(14) . . . . ?
C6 S8 C1 C2AA 57(6) . . . . ?
C7 S3 S7 C015 -118.1(10) . . . . ?
C7 S3 S7 C8 125.4(11) . . . . ?
C7 S3 C015 S7 50.6(9) . . . . ?
C7 S3 C8 S7 -46.3(9) . . . . ?
C7 S7 C015 S3 -55.8(9) . . . . ?
C7 S7 C8 S3 51.5(10) . . . . ?
C9 S4 S8 C6 109.4(10) . . . . ?
C9 S4 S8 C2AA -124.4(19) . . . . ?
C9 S4 S8 C1 -126.1(19) . . . . ?
C9 S4 C6 S8 -63.1(9) . . . . ?
C9 S4 C2AA S8 55.4(15) . . . . ?
C9 S4 C2AA C1 59(6) . . . . ?
C9 S4 C1 S8 49.6(17) . . . . ?
C9 S4 C1 C2AA -126(6) . . . . ?
C9 S8 C6 S4 57.0(9) . . . . ?
C9 S8 C2AA S4 -47.8(13) . . . . ?
C9 S8 C2AA C1 136(5) . . . . ?
C9 S8 C1 S4 -53.2(13) . . . . ?
C9 S8 C1 C2AA -50(6) . . . . ?
C12 S2 C013 S9 47.7(11) . . . . ?
C12 S2 S9 C013 -126.9(12) . . . . ?
C12 S2 S9 C3 114.4(11) . . . . ?
C12 S2 C3 S9 -56.7(10) . . . . ?
C2 S6 C012 S10 -54.8(9) . . . . ?
C2 S6 S10 C012 115.6(11) . . . . ?
C2 S6 S10 C4 -119.2(11) . . . . ?
C2 S6 C4 S10 53.2(9) . . . . ?
C2 S10 C4 S6 -52.8(9) . . . . ?
C2AA S4 S8 C6 -126.2(19) . . . . ?
C2AA S4 S8 C9 124.4(19) . . . . ?
C2AA S4 S8 C1 -2(3) . . . . ?
C2AA S4 C6 S8 54.2(18) . . . . ?
C2AA S4 C9 S8 -55.0(19) . . . . ?
C2AA S4 C1 S8 176(7) . . . . ?
C2AA S8 C6 S4 -41.8(16) . . . . ?
C2AA S8 C9 S4 42.9(16) . . . . ?
C2AA S8 C1 S4 -3(5) . . . . ?
C3 S2 C013 S9 -54.8(10) . . . . ?
C3 S2 S9 C013 118.7(12) . . . . ?
C3 S2 S9 C12 -114.4(11) . . . . ?
C3 S2 C12 S9 58.4(11) . . . . ?
C3 S9 C12 S2 -51.1(7) . . . . ?
C4 S6 C012 S10 49.4(9) . . . . ?
C4 S6 C2 S10 -53.4(10) . . . . ?
C4 S6 S10 C012 -125.1(11) . . . . ?
C4 S6 S10 C2 119.2(11) . . . . ?
C5AA S5 C5AA S5 -59.8(19) 2_656 . . 2_656 ?
C5AA S5 C4AA S5 65.4(16) 2_656 . . 2_656 ?
C5AA S5 C4AA S5 -56.3(14) . . . 2_656 ?
C8 S3 S7 C015 116.5(10) . . . . ?
C8 S3 S7 C7 -125.4(11) . . . . ?
C8 S3 C015 S7 -56.6(10) . . . . ?
C8 S3 C7 S7 49.8(10) . . . . ?
C8 S7 C015 S3 52.4(8) . . . . ?
C8 S7 C7 S3 -48.4(10) . . . . ?
C4AA S5 C5AA S5 59.2(9) . . . 2_656 ?
C4AA S5 C5AB S5 65.5(10) . . . 2_656 ?
S11 S12 C7A C5A -85(2) . . . . ?
S11 S12 C5A C7A 83(2) . . . . ?
S11 C7A C5A S12 -50.5(12) . . . . ?
S12 S11 C7A C5A 81(2) . . . . ?
S12 S11 C5A C7A -82(2) . . . . ?
S12 C7A C5A S11 50.5(12) . . . . ?
C8A S11 S12 C8A 179.998(17) . . . 2_556 ?
C8A S11 S12 C8A 180.002(16) 2_556 . . . ?
C8A S11 C8A S12 0.003(3) 2_556 . . . ?
C8A S12 C8A S11 -0.003(3) 2_556 . . . ?
C1 S4 S8 C6 -124.6(19) . . . . ?
C1 S4 S8 C9 126.1(19) . . . . ?
C1 S4 S8 C2AA 2(3) . . . . ?
C1 S4 C6 S8 36.8(13) . . . . ?
C1 S4 C9 S8 -36.0(14) . . . . ?
C1 S4 C2AA S8 -3(5) . . . . ?
C1 S8 C6 S4 -64(2) . . . . ?
C1 S8 C9 S4 63(2) . . . . ?
C1 S8 C2AA S4 176(6) . . . . ?
C5AB S5 C4AA S5 -75.7(19) . . . 2_656 ?
C5AB S5 C4AA S5 46.5(14) 2_656 . . 2_656 ?
C5AB S5 C5AB S5 -50.2(14) 2_656 . . 2_656 ?
C7A S11 S12 C7A 179.999(3) 2_556 . . . ?
C7A S11 S12 C7A 180.001(3) . . . 2_556 ?
C7A S11 S12 C5A -33(3) . . . . ?
C7A S11 S12 C5A 147(3) 2_556 . . . ?
C7A S11 S12 C5A -33(3) 2_556 . . 2_556 ?
C7A S11 S12 C5A 147(3) . . . 2_556 ?
C7A S11 C7A S12 -0.001(2) 2_556 . . . ?
C7A S11 C7A C5A 81(2) 2_556 . . . ?
C7A S11 C5A S12 -31(3) 2_556 . . . ?
C7A S11 C5A S12 82(2) . . . . ?
C7A S11 C5A C7A -114(3) 2_556 . . . ?
C7A S12 C7A S11 0.002(2) 2_556 . . . ?
C7A S12 C7A C5A -85(2) 2_556 . . . ?
C7A S12 C5A S11 -83(2) . . . . ?
C7A S12 C5A S11 42(4) 2_556 . . . ?
C7A S12 C5A C7A 126(4) 2_556 . . . ?
C5A S11 S12 C7A 33(3) . . . . ?
C5A S11 S12 C7A -147(3) 2_556 . . . ?
C5A S11 S12 C7A 33(3) 2_556 . . 2_556 ?
C5A S11 S12 C7A -147(3) . . . 2_556 ?
C5A S11 S12 C5A 179.997(4) 2_556 . . . ?
C5A S11 S12 C5A 180.003(6) . . . 2_556 ?
C5A S11 C7A S12 31(3) 2_556 . . . ?
C5A S11 C7A S12 -81(2) . . . . ?
C5A S11 C7A C5A 112(3) 2_556 . . . ?
C5A S11 C5A S12 -0.003(3) 2_556 . . . ?
C5A S11 C5A C7A -82(2) 2_556 . . . ?
C5A S12 C7A S11 -42(4) 2_556 . . . ?
C5A S12 C7A S11 85(2) . . . . ?
C5A S12 C7A C5A -128(4) 2_556 . . . ?
C5A S12 C5A S11 0.004(4) 2_556 . . . ?
C5A S12 C5A C7A 83(2) 2_556 . . . ?

_olex2_date_sample_data_collection 2021-04-27
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.565
_oxdiff_exptl_absorpt_empirical_full_min 0.471
####################################################################### 
# 
# 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_PhaseIII
_database_code_depnum_ccdc_archive 'CCDC 2263855'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2023-05-18 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT971_PhaseIII            
;
PROBLEM: Check Calcd Resid. Dens.  0.91Ang From Bi4             6.45 eA-3  
RESPONSE: LT polimorph, large unit cell refinement on dominating twin domain
;
_vrf_PLAT972_PhaseIII            
;
PROBLEM: Check Calcd Resid. Dens.  1.07Ang From Bi4            -4.60 eA-3  
RESPONSE: LT polimorph, large unit cell refinement on dominating twin domain
;
_vrf_PLAT196_PhaseIII            
;
PROBLEM: No TEMP record and _measurement_temperature .NE.        293 Degree
RESPONSE: no influence on structural parameters as the diffracted intensities
come mainly form heavy atoms as Bi and I, no HBs reported
;
_vrf_PLAT910_PhaseIII            
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         28 Note  
RESPONSE: large unit cell refinement on dominating twin domain
;
_vrf_PLAT934_PhaseIII            
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          2 Check 
RESPONSE: intensity disturbed due to twinning
;
_vrf_PLAT977_PhaseIII            
;
PROBLEM: Check Negative Difference Density on H32B      .      -1.80 eA-3  
RESPONSE: large unit cell refinement on dominating twin domain
;
# end Validation Reply Form
_audit_creation_date             2022-11-30
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'Bi2 I9, 2.25(C3 H9 S), 0.25(C3 H9 S0.8), 0.375(S), 0.25(C3 H9 S0.5), 0.25(C3 H9 S0.2)'
_chemical_formula_sum            'C9 H27 Bi2 I9 S3'
_chemical_formula_weight         1791.54
_chemical_melting_point          ?
_chemical_oxdiff_formula         Bi2I9C9S3H27
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'
Bi Bi -4.1077 10.2566 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   18.8536(5)
_cell_length_b                   18.9933(4)
_cell_length_c                   22.6857(6)
_cell_angle_alpha                89.063(2)
_cell_angle_beta                 88.081(2)
_cell_angle_gamma                60.273(2)
_cell_volume                     7050.5(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    15557
_cell_measurement_temperature    99.9(10)
_cell_measurement_theta_max      29.1360
_cell_measurement_theta_min      2.7700
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    18.028
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    3.376
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             6176
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.1126
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48474
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.490
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00  84.20   0.80   35.00    --   13.31  77.00  60.00  134
  2  ω     -1.00  94.20   0.80   35.00    --   13.31  77.00 -90.00  119
  3  ω    -47.00  57.00   0.80   35.00    --  -14.40  77.00 150.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0315183000
_diffrn_orient_matrix_UB_12      0.0069353000
_diffrn_orient_matrix_UB_13      0.0210103000
_diffrn_orient_matrix_UB_21      0.0216720000
_diffrn_orient_matrix_UB_22      0.0068478000
_diffrn_orient_matrix_UB_23      0.0220715000
_diffrn_orient_matrix_UB_31      -0.0203809000
_diffrn_orient_matrix_UB_32      0.0418852000
_diffrn_orient_matrix_UB_33      -0.0070780000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                20438
_reflns_number_total             26743
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         5.884
_refine_diff_density_min         -4.095
_refine_diff_density_rms         0.604
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         26743
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1320
_refine_ls_R_factor_gt           0.1016
_refine_ls_restrained_S_all      1.173
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0384P)²+1164.6615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2139
_refine_ls_wR_factor_ref         0.2290
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C37-C36 = C37-C35 = C36-C35
 2.8 with sigma of 0.005
 S12-C37 = S12-C36 = S12-C35
 1.7 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uiso(C36) = Uiso(C35) = Uiso(C37)
4. Others
 Fixed Sof: S9(0.8) S3A(0.8) S2A(0.5) S5(0.5) S2(0.2) S1A(0.2)
5.a Fixed occupancy and ADP/Uiso:
 C37, C36, C35
5.b Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C33(H33A,H33B,H33C), C14(H14A,H14B,H14C), C23(H23A,H23B,
 H23C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C31(H31A,
 H31B,H31C), C18(H18A,H18B,H18C), C5(H5A,H5B,H5C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C4(H4A,H4B,H4C),
  C28(H28A,H28B,H28C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C22(H22A,H22B,H22C),
 C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C29(H29A,H29B,H29C), C3(H3A,H3B,H3C),
  C2(H2A,H2B,H2C), C27(H27A,H27B,H27C), C17(H17A,H17B,H17C), C16(H16A,H16B,
 H16C), C12(H12A,H12B,H12C), C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C32(H32A,
 H32B,H32C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C)
5.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.17639(7) 0.65823(7) 0.65640(6) 0.0170(3) Uani 1 1 d . . . . .
Bi2 Bi 0.16547(7) 0.65822(7) 0.84356(6) 0.0171(3) Uani 1 1 d . . . . .
I28 I 0.34275(13) 0.57177(13) 0.60141(10) 0.0221(5) Uani 1 1 d . . . . .
I29 I 0.10311(13) 0.78783(13) 0.56479(10) 0.0219(5) Uani 1 1 d . . . . .
I30 I 0.11866(14) 0.56066(13) 0.59471(10) 0.0226(5) Uani 1 1 d . . . . .
I31 I 0.01774(13) 0.75148(13) 0.74549(10) 0.0231(5) Uani 1 1 d . . . . .
I32 I 0.24099(13) 0.51811(12) 0.75014(10) 0.0212(5) Uani 1 1 d . . . . .
I33 I 0.23084(14) 0.75166(13) 0.75455(10) 0.0232(5) Uani 1 1 d . . . . .
I34 I 0.32081(13) 0.56050(13) 0.90528(10) 0.0218(5) Uani 1 1 d . . . . .
I35 I 0.10900(13) 0.78801(13) 0.93496(10) 0.0215(5) Uani 1 1 d . . . . .
I36 I 0.08540(13) 0.57176(13) 0.89848(10) 0.0225(5) Uani 1 1 d . . . . .
Bi3 Bi 0.35449(8) 0.32515(7) 0.34208(6) 0.0181(3) Uani 1 1 d . . . . .
Bi4 Bi 0.32020(8) 0.32506(7) 0.15804(6) 0.0180(3) Uani 1 1 d . . . . .
I1 I 0.22224(13) 0.38546(13) 0.43469(10) 0.0225(5) Uani 1 1 d . . . . .
I2 I 0.45128(13) 0.17160(13) 0.40666(10) 0.0225(5) Uani 1 1 d . . . . .
I3 I 0.43868(13) 0.40771(13) 0.38943(10) 0.0231(5) Uani 1 1 d . . . . .
I4 I 0.26179(14) 0.25227(14) 0.26824(10) 0.0242(5) Uani 1 1 d . . . . .
I5 I 0.48591(13) 0.25219(14) 0.23188(10) 0.0245(5) Uani 1 1 d . . . . .
I6 I 0.26251(15) 0.47534(13) 0.25000(10) 0.0250(5) Uani 1 1 d . . . . .
I7 I 0.37708(13) 0.17156(13) 0.09325(10) 0.0232(5) Uani 1 1 d . . . . .
I8 I 0.15360(13) 0.40781(13) 0.11050(10) 0.0224(5) Uani 1 1 d . . . . .
I9 I 0.39239(13) 0.38536(13) 0.06558(10) 0.0218(5) Uani 1 1 d . . . . .
Bi5 Bi 0.67163(7) 0.17605(7) 0.66587(6) 0.0172(3) Uani 1 1 d . . . . .
Bi6 Bi 0.67038(8) 0.15688(8) 0.85258(6) 0.0191(3) Uani 1 1 d . . . . .
I10 I 0.82447(13) 0.12686(14) 0.59682(11) 0.0253(5) Uani 1 1 d . . . . .
I11 I 0.61787(14) 0.09661(13) 0.58078(11) 0.0259(5) Uani 1 1 d . . . . .
I12 I 0.58338(13) 0.33935(13) 0.61211(10) 0.0212(5) Uani 1 1 d . . . . .
I13 I 0.76655(19) 0.01691(14) 0.75153(12) 0.0443(8) Uani 1 1 d . . . . .
I14 I 0.71889(13) 0.26423(13) 0.76634(10) 0.0200(5) Uani 1 1 d . . . . .
I15 I 0.52055(13) 0.20913(13) 0.75801(10) 0.0202(5) Uani 1 1 d . . . . .
I16 I 0.81920(14) 0.11889(14) 0.91602(11) 0.0266(5) Uani 1 1 d . . . . .
I17 I 0.63302(14) 0.04684(13) 0.92345(11) 0.0251(5) Uani 1 1 d . . . . .
I18 I 0.56125(13) 0.30184(14) 0.92356(10) 0.0240(5) Uani 1 1 d . . . . .
Bi7 Bi 0.15244(7) 0.17606(7) 0.83412(6) 0.0173(3) Uani 1 1 d . . . . .
Bi8 Bi 0.17288(8) 0.15671(8) 0.64747(6) 0.0188(3) Uani 1 1 d . . . . .
I19 I 0.32008(13) 0.04664(13) 0.57641(10) 0.0240(5) Uani 1 1 d . . . . .
I20 I 0.13689(14) 0.30182(13) 0.57641(10) 0.0237(5) Uani 1 1 d . . . . .
I21 I 0.27038(13) 0.20907(13) 0.74201(10) 0.0203(5) Uani 1 1 d . . . . .
I22 I 0.06189(14) 0.11850(14) 0.58429(11) 0.0264(5) Uani 1 1 d . . . . .
I23 I 0.01742(13) 0.26393(13) 0.73375(10) 0.0205(5) Uani 1 1 d . . . . .
I24 I 0.2172(2) 0.01672(14) 0.74872(12) 0.0451(8) Uani 1 1 d . . . . .
I25 I 0.07736(13) 0.33942(13) 0.88819(10) 0.0216(5) Uani 1 1 d . . . . .
I26 I 0.28561(13) 0.09661(13) 0.91942(11) 0.0251(5) Uani 1 1 d . . . . .
I27 I 0.04883(14) 0.12671(14) 0.90336(11) 0.0255(5) Uani 1 1 d . . . . .
S1 S 0.9127(5) 0.8004(5) 0.8959(4) 0.0214(18) Uiso 1 1 d . . . . .
C2 C 0.894(2) 0.766(2) 0.9633(18) 0.037(10) Uiso 1 1 d . . . . .
H2A H 0.933582 0.759764 0.990974 0.055 Uiso 1 1 calc R U . . .
H2B H 0.840010 0.804363 0.978226 0.055 Uiso 1 1 calc R U . . .
H2C H 0.896477 0.714506 0.957518 0.055 Uiso 1 1 calc R U . . .
C3 C 0.836(2) 0.808(3) 0.8522(19) 0.040(10) Uiso 1 1 d . . . . .
H3A H 0.841326 0.826602 0.813655 0.059 Uiso 1 1 calc R U . . .
H3B H 0.840228 0.755474 0.848942 0.059 Uiso 1 1 calc R U . . .
H3C H 0.783761 0.845331 0.869649 0.059 Uiso 1 1 calc R U . . .
C20 C 0.877(3) 0.903(2) 0.9170(19) 0.040(10) Uiso 1 1 d . . . . .
H20A H 0.916765 0.905343 0.941778 0.060 Uiso 1 1 calc R U . . .
H20B H 0.870802 0.935510 0.882346 0.060 Uiso 1 1 calc R U . . .
H20C H 0.826060 0.924351 0.938176 0.060 Uiso 1 1 calc R U . . .
S1A S -0.172(3) 0.836(3) 0.628(2) 0.027(10) Uiso 0.2 1 d . . P A 1
S2 S 0.335(2) 0.840(2) 0.8749(17) 0.012(7) Uiso 0.2 1 d . . P D 1
C4 C 0.411(2) 0.846(2) 0.9215(15) 0.021(7) Uiso 1 1 d . . . D 1
H4A H 0.465105 0.810082 0.906127 0.031 Uiso 1 1 calc R U . D 1
H4B H 0.401844 0.900701 0.921178 0.031 Uiso 1 1 calc R U . D 1
H4C H 0.405685 0.830923 0.961241 0.031 Uiso 1 1 calc R U . D 1
C5 C 0.350(3) 0.744(3) 0.9091(19) 0.042(10) Uiso 1 1 d . . . D 1
H5A H 0.401182 0.700189 0.895749 0.062 Uiso 1 1 calc R U . D 1
H5B H 0.348944 0.748591 0.951255 0.062 Uiso 1 1 calc R U . D 1
H5C H 0.306400 0.734851 0.897934 0.062 Uiso 1 1 calc R U . D 1
C6 C 0.240(3) 0.907(3) 0.9059(19) 0.042(10) Uiso 1 1 d . . . D 1
H6A H 0.223313 0.960994 0.892149 0.063 Uiso 1 1 calc R U . D 1
H6B H 0.200879 0.891784 0.894787 0.063 Uiso 1 1 calc R U . D 1
H6C H 0.243423 0.905525 0.948108 0.063 Uiso 1 1 calc R U . D 1
S2A S 0.9652(14) 0.0045(13) 0.7541(10) 0.041(5) Uiso 0.5 1 d . . P C -1
S3 S 0.2865(5) 0.8011(5) 0.6044(4) 0.0212(18) Uiso 1 1 d . . . . .
C7 C 0.343(3) 0.764(3) 0.5375(18) 0.039(10) Uiso 1 1 d . . . . .
H7A H 0.310352 0.757277 0.509291 0.059 Uiso 1 1 calc R U . . .
H7B H 0.359025 0.802092 0.522487 0.059 Uiso 1 1 calc R U . . .
H7C H 0.391292 0.712904 0.544407 0.059 Uiso 1 1 calc R U . . .
C8 C 0.220(3) 0.903(3) 0.584(2) 0.051(12) Uiso 1 1 d . . . . .
H8A H 0.178475 0.904928 0.559135 0.076 Uiso 1 1 calc R U . . .
H8B H 0.194541 0.934834 0.618606 0.076 Uiso 1 1 calc R U . . .
H8C H 0.250273 0.923819 0.562702 0.076 Uiso 1 1 calc R U . . .
C9 C 0.357(2) 0.809(2) 0.6489(17) 0.030(9) Uiso 1 1 d . . . . .
H9A H 0.332558 0.829033 0.687122 0.046 Uiso 1 1 calc R U . . .
H9B H 0.404760 0.756650 0.652794 0.046 Uiso 1 1 calc R U . . .
H9C H 0.372493 0.845837 0.630875 0.046 Uiso 1 1 calc R U . . .
S3A S 0.6707(7) 0.1645(7) 0.0499(5) 0.026(2) Uiso 0.8 1 d . . P B -1
S4 S 0.5289(5) 0.4842(5) 0.7546(4) 0.0198(18) Uiso 1 1 d . . . . .
C10 C 0.443(2) 0.585(2) 0.7511(17) 0.031(9) Uiso 1 1 d . . . . .
H10A H 0.461125 0.623215 0.746704 0.047 Uiso 1 1 calc R U . . .
H10B H 0.410331 0.588468 0.718053 0.047 Uiso 1 1 calc R U . . .
H10C H 0.409881 0.595785 0.786813 0.047 Uiso 1 1 calc R U . . .
C11 C 0.479(2) 0.427(2) 0.7625(18) 0.033(9) Uiso 1 1 d . . . . .
H11A H 0.519318 0.370522 0.764925 0.050 Uiso 1 1 calc R U . . .
H11B H 0.445550 0.443281 0.797777 0.050 Uiso 1 1 calc R U . . .
H11C H 0.446001 0.435964 0.729017 0.050 Uiso 1 1 calc R U . . .
C12 C 0.558(2) 0.489(2) 0.8298(16) 0.030(9) Uiso 1 1 d . . . . .
H12A H 0.586194 0.519218 0.830285 0.046 Uiso 1 1 calc R U . . .
H12B H 0.510042 0.514416 0.854972 0.046 Uiso 1 1 calc R U . . .
H12C H 0.593528 0.434675 0.843763 0.046 Uiso 1 1 calc R U . . .
S5 S 1.0298(12) 0.0044(12) 0.7463(9) 0.031(4) Uiso 0.5 1 d . . P C 1
C13 C 1.024(3) -0.044(3) 0.687(2) 0.057(13) Uiso 1 1 d . . . C 1
H13A H 1.070018 -0.097964 0.686132 0.085 Uiso 1 1 calc R U . C 1
H13B H 0.974414 -0.046454 0.690215 0.085 Uiso 1 1 calc R U . C 1
H13C H 1.024384 -0.015328 0.652320 0.085 Uiso 1 1 calc R U . C 1
C14 C 1.026(3) -0.044(3) 0.8124(18) 0.039(10) Uiso 1 1 d . . . C 1
H14A H 1.029927 -0.014365 0.845259 0.059 Uiso 1 1 calc R U . C 1
H14B H 0.976088 -0.044692 0.815463 0.059 Uiso 1 1 calc R U . C 1
H14C H 1.071574 -0.098156 0.812628 0.059 Uiso 1 1 calc R U . C 1
C15 C 0.949(2) 0.102(2) 0.7511(17) 0.027(8) Uiso 1 1 d . . . C 1
H15A H 0.954163 0.127693 0.785258 0.041 Uiso 1 1 calc R U . C 1
H15B H 0.948763 0.131353 0.716369 0.041 Uiso 1 1 calc R U . C 1
H15C H 0.898792 0.100227 0.754263 0.041 Uiso 1 1 calc R U . C 1
S6 S 0.6929(5) 0.7209(5) 0.1027(4) 0.0248(19) Uiso 1 1 d . . . . .
C16 C 0.680(3) 0.643(3) 0.134(2) 0.049(12) Uiso 1 1 d . . . . .
H16A H 0.732031 0.601063 0.147956 0.073 Uiso 1 1 calc R U . . .
H16B H 0.642025 0.664300 0.167122 0.073 Uiso 1 1 calc R U . . .
H16C H 0.660338 0.621487 0.105555 0.073 Uiso 1 1 calc R U . . .
C17 C 0.745(3) 0.677(3) 0.0319(19) 0.042(10) Uiso 1 1 d . . . . .
H17A H 0.754606 0.715649 0.010603 0.063 Uiso 1 1 calc R U . . .
H17B H 0.795860 0.628853 0.038751 0.063 Uiso 1 1 calc R U . . .
H17C H 0.710965 0.663738 0.009146 0.063 Uiso 1 1 calc R U . . .
C18 C 0.591(2) 0.788(2) 0.0824(17) 0.031(9) Uiso 1 1 d . . . . .
H18A H 0.588130 0.834935 0.063829 0.046 Uiso 1 1 calc R U . . .
H18B H 0.574207 0.760957 0.055405 0.046 Uiso 1 1 calc R U . . .
H18C H 0.555894 0.803770 0.116972 0.046 Uiso 1 1 calc R U . . .
S7 S 0.2141(6) 0.5903(6) 0.1012(4) 0.027(2) Uiso 1 1 d . . . . .
C19 C 0.137(3) 0.667(3) 0.150(2) 0.054(13) Uiso 1 1 d . . . . .
H19A H 0.104405 0.646334 0.168209 0.082 Uiso 1 1 calc R U . . .
H19B H 0.163128 0.680646 0.179604 0.082 Uiso 1 1 calc R U . . .
H19C H 0.102634 0.714527 0.127355 0.082 Uiso 1 1 calc R U . . .
C21 C 0.157(2) 0.592(2) 0.0374(17) 0.031(9) Uiso 1 1 d . . . . .
H21A H 0.126367 0.565095 0.046897 0.046 Uiso 1 1 calc R U . . .
H21B H 0.119479 0.647607 0.026898 0.046 Uiso 1 1 calc R U . . .
H21C H 0.193764 0.565524 0.004748 0.046 Uiso 1 1 calc R U . . .
C22 C 0.265(3) 0.644(3) 0.0735(19) 0.042(10) Uiso 1 1 d . . . . .
H22A H 0.308163 0.609444 0.046498 0.063 Uiso 1 1 calc R U . . .
H22B H 0.226179 0.691875 0.053546 0.063 Uiso 1 1 calc R U . . .
H22C H 0.286674 0.657994 0.105795 0.063 Uiso 1 1 calc R U . . .
S8 S 0.1957(6) 0.5899(6) 0.3984(4) 0.027(2) Uiso 1 1 d . . . . .
C23 C 0.253(2) 0.588(2) 0.4626(18) 0.036(9) Uiso 1 1 d . . . . .
H23A H 0.257401 0.547343 0.489760 0.054 Uiso 1 1 calc R U . . .
H23B H 0.307092 0.576857 0.449888 0.054 Uiso 1 1 calc R U . . .
H23C H 0.225525 0.640336 0.481792 0.054 Uiso 1 1 calc R U . . .
C24 C 0.194(3) 0.668(3) 0.353(2) 0.056(13) Uiso 1 1 d . . . . .
H24A H 0.246725 0.649723 0.334999 0.084 Uiso 1 1 calc R U . . .
H24B H 0.154164 0.682085 0.323158 0.084 Uiso 1 1 calc R U . . .
H24C H 0.179135 0.715096 0.376904 0.084 Uiso 1 1 calc R U . . .
C25 C 0.091(3) 0.643(3) 0.425(2) 0.055(13) Uiso 1 1 d . . . . .
H25A H 0.080682 0.607866 0.450920 0.083 Uiso 1 1 calc R U . . .
H25B H 0.080011 0.690605 0.445812 0.083 Uiso 1 1 calc R U . . .
H25C H 0.055040 0.657594 0.392066 0.083 Uiso 1 1 calc R U . . .
S9 S -0.1643(7) 0.8351(7) 0.5508(5) 0.024(2) Uiso 0.8 1 d . . P A -1
C26 C -0.091(2) 0.743(2) 0.5873(18) 0.037(10) Uiso 1 1 d . . . A -1
H26A H -0.036951 0.730338 0.575663 0.055 Uiso 1 1 calc R U . A -1
H26B H -0.098665 0.750787 0.629297 0.055 Uiso 1 1 calc R U . A -1
H26C H -0.100120 0.699371 0.576472 0.055 Uiso 1 1 calc R U . A -1
C27 C -0.149(3) 0.909(3) 0.5873(19) 0.043(11) Uiso 1 1 d . . . A -1
H27A H -0.097973 0.905077 0.573176 0.064 Uiso 1 1 calc R U . A -1
H27B H -0.192767 0.962556 0.579073 0.064 Uiso 1 1 calc R U . A -1
H27C H -0.146393 0.899824 0.629031 0.064 Uiso 1 1 calc R U . A -1
C28 C -0.258(3) 0.846(3) 0.5785(19) 0.042(10) Uiso 1 1 d . . . A -1
H28A H -0.267979 0.807099 0.559849 0.063 Uiso 1 1 calc R U . A -1
H28B H -0.254620 0.837005 0.620306 0.063 Uiso 1 1 calc R U . A -1
H28C H -0.300995 0.899737 0.570347 0.063 Uiso 1 1 calc R U . A -1
S10 S 0.4136(5) 0.2792(5) 0.6029(4) 0.0241(19) Uiso 1 1 d . . . . .
C29 C 0.330(3) 0.355(3) 0.638(2) 0.048(11) Uiso 1 1 d . . . . .
H29A H 0.342344 0.395177 0.651764 0.071 Uiso 1 1 calc R U . . .
H29B H 0.285524 0.380022 0.611204 0.071 Uiso 1 1 calc R U . . .
H29C H 0.313764 0.333335 0.671111 0.071 Uiso 1 1 calc R U . . .
C30 C 0.380(3) 0.210(3) 0.5804(19) 0.041(10) Uiso 1 1 d . . . . .
H30A H 0.423853 0.165218 0.560029 0.062 Uiso 1 1 calc R U . . .
H30B H 0.362915 0.191407 0.614590 0.062 Uiso 1 1 calc R U . . .
H30C H 0.334676 0.238093 0.554683 0.062 Uiso 1 1 calc R U . . .
C31 C 0.420(2) 0.325(2) 0.5318(17) 0.034(9) Uiso 1 1 d . . . . .
H31A H 0.466121 0.285421 0.508919 0.050 Uiso 1 1 calc R U . . .
H31B H 0.370875 0.341064 0.510630 0.050 Uiso 1 1 calc R U . . .
H31C H 0.426037 0.371002 0.538845 0.050 Uiso 1 1 calc R U . . .
S11 S -0.0130(5) 0.4841(5) 0.7449(4) 0.0210(18) Uiso 1 1 d . . . . .
C32 C -0.044(3) 0.490(3) 0.6691(19) 0.043(11) Uiso 1 1 d . . . . .
H32A H -0.041018 0.439146 0.658616 0.065 Uiso 1 1 calc R U . . .
H32B H -0.099716 0.532771 0.665573 0.065 Uiso 1 1 calc R U . . .
H32C H -0.009123 0.499545 0.643151 0.065 Uiso 1 1 calc R U . . .
C33 C 0.095(2) 0.426(2) 0.7352(16) 0.027(8) Uiso 1 1 d . . . . .
H33A H 0.110579 0.369125 0.732855 0.040 Uiso 1 1 calc R U . . .
H33B H 0.111348 0.441662 0.699449 0.040 Uiso 1 1 calc R U . . .
H33C H 0.120323 0.434030 0.768051 0.040 Uiso 1 1 calc R U . . .
C34 C -0.027(2) 0.582(2) 0.7479(18) 0.033(9) Uiso 1 1 d . . . . .
H34A H -0.083842 0.620657 0.753145 0.050 Uiso 1 1 calc R U . . .
H34B H 0.002554 0.585994 0.780334 0.050 Uiso 1 1 calc R U . . .
H34C H -0.006420 0.593626 0.711732 0.050 Uiso 1 1 calc R U . . .
S12 S 0.4757(7) 0.0490(7) 0.2492(5) 0.047(3) Uiso 1 1 d D . . . .
C35 C 0.441(2) 0.017(2) 0.3086(10) 0.055 Uiso 1 1 d D . . . .
H35A H 0.394315 0.013649 0.297968 0.083 Uiso 1 1 calc R U . . .
H35B H 0.426476 0.055378 0.340279 0.083 Uiso 1 1 calc R U . . .
H35C H 0.483564 -0.034983 0.320935 0.083 Uiso 1 1 calc R U . . .
C36 C 0.5651(14) 0.046(2) 0.2642(14) 0.055 Uiso 1 1 d D . . . .
H36A H 0.608568 -0.009531 0.263871 0.083 Uiso 1 1 calc R U . . .
H36B H 0.560568 0.069047 0.302324 0.083 Uiso 1 1 calc R U . . .
H36C H 0.576544 0.075995 0.234785 0.083 Uiso 1 1 calc R U . . .
C37 C 0.488(2) -0.009(2) 0.1890(10) 0.055 Uiso 1 1 d D . . . .
H37A H 0.458080 0.025360 0.156941 0.083 Uiso 1 1 calc R U . . .
H37B H 0.467881 -0.045577 0.198407 0.083 Uiso 1 1 calc R U . . .
H37C H 0.544918 -0.039517 0.177921 0.083 Uiso 1 1 calc R 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 I28 2.964(2) . ?
Bi1 I29 2.990(3) . ?
Bi1 I30 2.961(3) . ?
Bi1 I31 3.260(2) . ?
Bi1 I32 3.140(2) . ?
Bi1 I33 3.354(3) . ?
Bi2 I31 3.352(3) . ?
Bi2 I32 3.135(2) . ?
Bi2 I33 3.261(2) . ?
Bi2 I34 2.963(3) . ?
Bi2 I35 2.988(2) . ?
Bi2 I36 2.965(2) . ?
Bi3 I1 2.973(2) . ?
Bi3 I2 2.957(3) . ?
Bi3 I3 2.961(3) . ?
Bi3 I4 3.232(3) . ?
Bi3 I5 3.256(3) . ?
Bi3 I6 3.263(3) . ?
Bi4 I4 3.254(3) . ?
Bi4 I5 3.236(3) . ?
Bi4 I6 3.263(2) . ?
Bi4 I7 2.957(2) . ?
Bi4 I8 2.962(3) . ?
Bi4 I9 2.973(3) . ?
Bi5 I10 2.951(2) . ?
Bi5 I11 2.962(3) . ?
Bi5 I12 2.961(2) . ?
Bi5 I13 3.285(3) . ?
Bi5 I14 3.246(2) . ?
Bi5 I15 3.278(2) . ?
Bi6 I13 3.279(3) . ?
Bi6 I14 3.228(2) . ?
Bi6 I15 3.335(3) . ?
Bi6 I16 2.948(3) . ?
Bi6 I17 2.954(3) . ?
Bi6 I18 2.951(2) . ?
Bi7 I21 3.276(2) . ?
Bi7 I23 3.240(3) . ?
Bi7 I24 3.282(3) . ?
Bi7 I25 2.965(2) . ?
Bi7 I26 2.966(3) . ?
Bi7 I27 2.954(3) . ?
Bi8 I19 2.954(2) . ?
Bi8 I20 2.954(3) . ?
Bi8 I21 3.334(3) . ?
Bi8 I22 2.950(3) . ?
Bi8 I23 3.224(2) . ?
Bi8 I24 3.282(3) . ?
S1 C2 1.75(4) . ?
S1 C3 1.73(4) . ?
S1 C20 1.79(4) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
S2 C6 1.73(5) . ?
C4 S2 1.86(5) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 S2 1.86(5) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
S2A S5 1.23(3) . ?
S2A C13 1.81(5) . ?
S2A C14 1.71(5) . ?
S2A C15 1.72(4) . ?
S3 C7 1.77(4) . ?
S3 C8 1.77(5) . ?
S3 C9 1.76(4) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
S4 C10 1.79(4) . ?
S4 C11 1.75(4) . ?
S4 C12 1.83(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
S5 C13 1.67(5) . ?
S5 C14 1.76(4) . ?
S5 C15 1.72(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
S6 C16 1.75(4) . ?
S6 C17 1.83(4) . ?
S6 C18 1.77(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
S7 C19 1.82(5) . ?
S7 C21 1.83(4) . ?
S7 C22 1.80(4) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
S8 C23 1.84(4) . ?
S8 C24 1.78(5) . ?
S8 C25 1.81(5) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
S9 S1A 1.74(5) . ?
S9 C26 1.81(4) . ?
S9 C27 1.80(4) . ?
S9 C28 1.76(4) . ?
C26 S1A 1.89(6) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 S1A 1.87(6) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 S1A 1.93(6) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
S10 C29 1.71(4) . ?
S10 C30 1.80(4) . ?
S10 C31 1.85(4) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
S11 C32 1.82(4) . ?
S11 C33 1.77(4) . ?
S11 C34 1.75(4) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 S12 1.703(5) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 S12 1.702(5) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 S12 1.705(5) . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?

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
I28 Bi1 I29 96.38(7) . . ?
I28 Bi1 I31 165.95(8) . . ?
I28 Bi1 I32 86.45(7) . . ?
I28 Bi1 I33 92.61(7) . . ?
I29 Bi1 I31 92.57(7) . . ?
I29 Bi1 I32 174.78(8) . . ?
I29 Bi1 I33 100.25(7) . . ?
I30 Bi1 I28 94.23(7) . . ?
I30 Bi1 I29 90.40(7) . . ?
I30 Bi1 I31 96.53(7) . . ?
I30 Bi1 I32 85.01(7) . . ?
I30 Bi1 I33 166.63(7) . . ?
I31 Bi1 I33 75.10(6) . . ?
I32 Bi1 I31 85.51(6) . . ?
I32 Bi1 I33 83.96(6) . . ?
I32 Bi2 I31 84.06(6) . . ?
I32 Bi2 I33 85.62(6) . . ?
I33 Bi2 I31 75.11(6) . . ?
I34 Bi2 I31 166.62(7) . . ?
I34 Bi2 I32 84.88(7) . . ?
I34 Bi2 I33 96.58(7) . . ?
I34 Bi2 I35 90.54(7) . . ?
I34 Bi2 I36 94.23(7) . . ?
I35 Bi2 I31 100.15(7) . . ?
I35 Bi2 I32 174.79(7) . . ?
I35 Bi2 I33 92.46(7) . . ?
I36 Bi2 I31 92.55(7) . . ?
I36 Bi2 I32 86.41(7) . . ?
I36 Bi2 I33 165.93(8) . . ?
I36 Bi2 I35 96.42(7) . . ?
Bi1 I31 Bi2 79.85(6) . . ?
Bi2 I32 Bi1 85.12(6) . . ?
Bi2 I33 Bi1 79.81(6) . . ?
I1 Bi3 I4 90.54(7) . . ?
I1 Bi3 I5 173.00(7) . . ?
I1 Bi3 I6 97.09(7) . . ?
I2 Bi3 I1 91.54(7) . . ?
I2 Bi3 I3 95.57(7) . . ?
I2 Bi3 I4 92.84(7) . . ?
I2 Bi3 I5 89.30(7) . . ?
I2 Bi3 I6 169.90(7) . . ?
I3 Bi3 I1 95.51(7) . . ?
I3 Bi3 I4 169.50(8) . . ?
I3 Bi3 I5 91.32(7) . . ?
I3 Bi3 I6 88.83(7) . . ?
I4 Bi3 I5 82.48(6) . . ?
I4 Bi3 I6 81.89(7) . . ?
I5 Bi3 I6 81.50(6) . . ?
I4 Bi4 I6 81.57(6) . . ?
I5 Bi4 I4 82.46(6) . . ?
I5 Bi4 I6 81.82(6) . . ?
I7 Bi4 I4 89.46(7) . . ?
I7 Bi4 I5 92.81(7) . . ?
I7 Bi4 I6 170.06(8) . . ?
I7 Bi4 I8 95.63(7) . . ?
I7 Bi4 I9 91.47(7) . . ?
I8 Bi4 I4 91.48(7) . . ?
I8 Bi4 I5 169.57(7) . . ?
I8 Bi4 I6 88.92(7) . . ?
I8 Bi4 I9 95.47(7) . . ?
I9 Bi4 I4 172.87(7) . . ?
I9 Bi4 I5 90.42(7) . . ?
I9 Bi4 I6 96.91(7) . . ?
Bi3 I4 Bi4 81.79(6) . . ?
Bi4 I5 Bi3 81.71(6) . . ?
Bi4 I6 Bi3 81.18(6) . . ?
I10 Bi5 I11 91.56(7) . . ?
I10 Bi5 I12 94.40(7) . . ?
I10 Bi5 I13 90.42(8) . . ?
I10 Bi5 I14 92.94(7) . . ?
I10 Bi5 I15 170.83(8) . . ?
I11 Bi5 I13 95.65(8) . . ?
I11 Bi5 I14 175.37(7) . . ?
I11 Bi5 I15 91.40(7) . . ?
I12 Bi5 I11 95.70(7) . . ?
I12 Bi5 I13 167.53(8) . . ?
I12 Bi5 I14 84.99(7) . . ?
I12 Bi5 I15 93.94(7) . . ?
I14 Bi5 I13 83.28(7) . . ?
I14 Bi5 I15 83.98(6) . . ?
I15 Bi5 I13 80.65(7) . . ?
I13 Bi6 I15 79.90(7) . . ?
I14 Bi6 I13 83.65(7) . . ?
I14 Bi6 I15 83.35(6) . . ?
I16 Bi6 I13 94.77(8) . . ?
I16 Bi6 I14 85.66(7) . . ?
I16 Bi6 I15 168.24(8) . . ?
I16 Bi6 I17 95.02(7) . . ?
I16 Bi6 I18 95.13(7) . . ?
I17 Bi6 I13 91.17(7) . . ?
I17 Bi6 I14 174.81(7) . . ?
I17 Bi6 I15 95.56(7) . . ?
I18 Bi6 I13 168.14(8) . . ?
I18 Bi6 I14 90.60(7) . . ?
I18 Bi6 I15 89.15(7) . . ?
I18 Bi6 I17 94.46(7) . . ?
Bi6 I13 Bi5 80.61(6) . . ?
Bi6 I14 Bi5 81.96(6) . . ?
Bi5 I15 Bi6 79.87(6) . . ?
I21 Bi7 I24 80.57(7) . . ?
I23 Bi7 I21 83.94(6) . . ?
I23 Bi7 I24 83.44(7) . . ?
I25 Bi7 I21 94.06(7) . . ?
I25 Bi7 I23 85.09(6) . . ?
I25 Bi7 I24 167.78(8) . . ?
I25 Bi7 I26 95.62(7) . . ?
I26 Bi7 I21 91.48(7) . . ?
I26 Bi7 I23 175.40(7) . . ?
I26 Bi7 I24 95.48(8) . . ?
I27 Bi7 I21 170.83(8) . . ?
I27 Bi7 I23 93.05(7) . . ?
I27 Bi7 I24 90.50(8) . . ?
I27 Bi7 I25 94.31(7) . . ?
I27 Bi7 I26 91.43(7) . . ?
I19 Bi8 I21 95.66(7) . . ?
I19 Bi8 I23 174.82(8) . . ?
I19 Bi8 I24 91.13(7) . . ?
I20 Bi8 I19 94.47(7) . . ?
I20 Bi8 I21 89.21(7) . . ?
I20 Bi8 I23 90.58(7) . . ?
I20 Bi8 I24 168.05(8) . . ?
I22 Bi8 I19 95.01(7) . . ?
I22 Bi8 I20 95.17(8) . . ?
I22 Bi8 I21 168.11(7) . . ?
I22 Bi8 I23 85.64(7) . . ?
I22 Bi8 I24 94.85(8) . . ?
I23 Bi8 I21 83.27(6) . . ?
I23 Bi8 I24 83.70(7) . . ?
I24 Bi8 I21 79.72(7) . . ?
Bi7 I21 Bi8 79.89(6) . . ?
Bi8 I23 Bi7 82.07(6) . . ?
Bi8 I24 Bi7 80.58(6) . . ?
C2 S1 C20 98(2) . . ?
C3 S1 C2 103(2) . . ?
C3 S1 C20 103(2) . . ?
S1 C2 H2A 109.5 . . ?
S1 C2 H2B 109.5 . . ?
S1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
S1 C3 H3A 109.5 . . ?
S1 C3 H3B 109.5 . . ?
S1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
S1 C20 H20A 109.5 . . ?
S1 C20 H20B 109.5 . . ?
S1 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
S9 S1A C26 59.6(19) . . ?
S9 S1A C27 60(2) . . ?
S9 S1A C28 57.1(19) . . ?
C26 S1A C28 93(3) . . ?
C27 S1A C26 96(3) . . ?
C27 S1A C28 98(3) . . ?
C5 S2 C4 94(2) . . ?
C6 S2 C4 106(3) . . ?
C6 S2 C5 99(3) . . ?
S2 C4 H4A 109.5 . . ?
S2 C4 H4B 109.5 . . ?
S2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
S2 C5 H5A 109.5 . . ?
S2 C5 H5B 109.5 . . ?
S2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
S2 C6 H6A 109.5 . . ?
S2 C6 H6B 109.5 . . ?
S2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
S5 S2A C13 63(2) . . ?
S5 S2A C14 71(2) . . ?
S5 S2A C15 69.2(18) . . ?
C14 S2A C13 107(2) . . ?
C14 S2A C15 108(2) . . ?
C15 S2A C13 105(2) . . ?
C7 S3 C8 100(2) . . ?
C9 S3 C7 101.9(19) . . ?
C9 S3 C8 103(2) . . ?
S3 C7 H7A 109.5 . . ?
S3 C7 H7B 109.5 . . ?
S3 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
S3 C8 H8A 109.5 . . ?
S3 C8 H8B 109.5 . . ?
S3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
S3 C9 H9A 109.5 . . ?
S3 C9 H9B 109.5 . . ?
S3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C10 S4 C12 98.1(18) . . ?
C11 S4 C10 100.4(18) . . ?
C11 S4 C12 102.9(18) . . ?
S4 C10 H10A 109.5 . . ?
S4 C10 H10B 109.5 . . ?
S4 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
S4 C11 H11A 109.5 . . ?
S4 C11 H11B 109.5 . . ?
S4 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
S4 C12 H12A 109.5 . . ?
S4 C12 H12B 109.5 . . ?
S4 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
S2A S5 C13 76(2) . . ?
S2A S5 C14 67.4(19) . . ?
S2A S5 C15 69.0(18) . . ?
C13 S5 C14 112(2) . . ?
C13 S5 C15 112(2) . . ?
C15 S5 C14 106(2) . . ?
S2A C13 H13A 124.0 . . ?
S2A C13 H13B 68.5 . . ?
S2A C13 H13C 124.2 . . ?
S5 C13 S2A 41.0(15) . . ?
S5 C13 H13A 109.5 . . ?
S5 C13 H13B 109.5 . . ?
S5 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
S2A C14 S5 41.3(14) . . ?
S2A C14 H14A 122.1 . . ?
S2A C14 H14B 68.2 . . ?
S2A C14 H14C 126.2 . . ?
S5 C14 H14A 109.5 . . ?
S5 C14 H14B 109.5 . . ?
S5 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
S2A C15 S5 41.8(13) . . ?
S2A C15 H15A 121.5 . . ?
S2A C15 H15B 127.0 . . ?
S2A C15 H15C 67.7 . . ?
S5 C15 H15A 109.5 . . ?
S5 C15 H15B 109.5 . . ?
S5 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 S6 C17 103(2) . . ?
C16 S6 C18 100(2) . . ?
C18 S6 C17 102.9(19) . . ?
S6 C16 H16A 109.5 . . ?
S6 C16 H16B 109.5 . . ?
S6 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
S6 C17 H17A 109.5 . . ?
S6 C17 H17B 109.5 . . ?
S6 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
S6 C18 H18A 109.5 . . ?
S6 C18 H18B 109.5 . . ?
S6 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C19 S7 C21 104(2) . . ?
C22 S7 C19 100(2) . . ?
C22 S7 C21 101.6(19) . . ?
S7 C19 H19A 109.5 . . ?
S7 C19 H19B 109.5 . . ?
S7 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
S7 C21 H21A 109.5 . . ?
S7 C21 H21B 109.5 . . ?
S7 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
S7 C22 H22A 109.5 . . ?
S7 C22 H22B 109.5 . . ?
S7 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 S8 C23 104(2) . . ?
C24 S8 C25 98(2) . . ?
C25 S8 C23 104(2) . . ?
S8 C23 H23A 109.5 . . ?
S8 C23 H23B 109.5 . . ?
S8 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
S8 C24 H24A 109.5 . . ?
S8 C24 H24B 109.5 . . ?
S8 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
S8 C25 H25A 109.5 . . ?
S8 C25 H25B 109.5 . . ?
S8 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
S1A S9 C26 64(2) . . ?
S1A S9 C27 64(2) . . ?
S1A S9 C28 67(2) . . ?
C27 S9 C26 101(2) . . ?
C28 S9 C26 101(2) . . ?
C28 S9 C27 107(2) . . ?
S1A C26 H26A 127.8 . . ?
S1A C26 H26B 53.4 . . ?
S1A C26 H26C 122.8 . . ?
S9 C26 S1A 56.2(19) . . ?
S9 C26 H26A 109.5 . . ?
S9 C26 H26B 109.5 . . ?
S9 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
S1A C27 H27A 132.0 . . ?
S1A C27 H27B 118.5 . . ?
S1A C27 H27C 53.2 . . ?
S9 C27 S1A 56.8(19) . . ?
S9 C27 H27A 109.5 . . ?
S9 C27 H27B 109.5 . . ?
S9 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
S1A C28 H28A 133.4 . . ?
S1A C28 H28B 54.1 . . ?
S1A C28 H28C 117.1 . . ?
S9 C28 S1A 56.2(19) . . ?
S9 C28 H28A 109.5 . . ?
S9 C28 H28B 109.5 . . ?
S9 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C29 S10 C30 104(2) . . ?
C29 S10 C31 104(2) . . ?
C30 S10 C31 101.6(19) . . ?
S10 C29 H29A 109.5 . . ?
S10 C29 H29B 109.5 . . ?
S10 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
S10 C30 H30A 109.5 . . ?
S10 C30 H30B 109.5 . . ?
S10 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
S10 C31 H31A 109.5 . . ?
S10 C31 H31B 109.5 . . ?
S10 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C33 S11 C32 100.5(19) . . ?
C34 S11 C32 97(2) . . ?
C34 S11 C33 101.0(18) . . ?
S11 C32 H32A 109.5 . . ?
S11 C32 H32B 109.5 . . ?
S11 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
S11 C33 H33A 109.5 . . ?
S11 C33 H33B 109.5 . . ?
S11 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
S11 C34 H34A 109.5 . . ?
S11 C34 H34B 109.5 . . ?
S11 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 S12 C37 110.4(4) . . ?
C36 S12 C35 110.6(4) . . ?
C36 S12 C37 110.4(4) . . ?
S12 C35 H35A 109.5 . . ?
S12 C35 H35B 109.5 . . ?
S12 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
S12 C36 H36A 109.5 . . ?
S12 C36 H36B 109.5 . . ?
S12 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
S12 C37 H37A 109.5 . . ?
S12 C37 H37B 109.5 . . ?
S12 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C2 H2B I26 0.96 3.15 4.02(4) 152.8 2_667 yes
C2 H2C I8 0.96 3.33 4.20(4) 152.8 2_666 yes
C3 H3A I31 0.96 3.24 3.83(4) 121.0 1_655 yes
C3 H3B I8 0.96 3.17 4.08(4) 158.7 2_666 yes
C3 H3C I7 0.96 3.29 3.99(4) 132.1 2_666 yes
C20 H20A I35 0.96 3.18 3.82(4) 126.3 1_655 yes
C20 H20B I16 0.96 3.22 3.67(4) 111.3 1_565 yes
C20 H20C I17 0.96 3.23 4.03(4) 141.5 1_565 yes
C4 H4A I5 0.96 3.30 3.94(3) 125.9 2_666 yes
C4 H4A I7 0.96 3.16 3.84(3) 129.1 2_666 yes
C4 H4B I26 0.96 3.25 4.13(3) 153.2 1_565 yes
C4 H4C I17 0.96 3.34 3.94(3) 122.8 2_667 yes
C5 H5B I18 0.96 3.24 4.11(4) 151.6 2_667 yes
C5 H5C I34 0.96 3.19 3.79(4) 122.8 . yes
C6 H6A I26 0.96 3.39 4.11(4) 133.6 1_565 yes
C6 H6C I16 0.96 3.37 4.24(4) 151.7 2_667 yes
C7 H7A I12 0.96 3.33 3.81(4) 112.7 2_666 yes
C7 H7B I11 0.96 3.16 4.04(4) 152.3 2_666 yes
C7 H7C I3 0.96 3.27 4.16(4) 154.0 2_666 yes
C8 H8A I29 0.96 3.18 3.83(5) 126.7 . yes
C8 H8B I22 0.96 3.23 3.68(5) 110.9 1_565 yes
C8 H8C I19 0.96 3.22 4.02(5) 141.8 1_565 yes
C9 H9A I24 0.96 3.41 4.15(4) 135.0 1_565 yes
C9 H9B I3 0.96 3.19 4.09(4) 157.1 2_666 yes
C9 H9B I5 0.96 3.34 3.80(4) 112.1 2_666 yes
C9 H9C I2 0.96 3.26 3.97(4) 132.7 2_666 yes
C10 H10A I5 0.96 3.04 3.98(4) 164.7 2_666 yes
C10 H10B I28 0.96 3.06 4.01(4) 167.6 . yes
C11 H11A I14 0.96 3.27 4.02(4) 135.8 . yes
C11 H11A I15 0.96 3.06 3.82(4) 136.6 . yes
C11 H11B I34 0.96 3.32 4.24(4) 160.3 . yes
C12 H12A I9 0.96 3.16 3.84(4) 130.0 2_666 yes
C13 H13C I22 0.96 3.31 4.17(5) 150.1 1_655 yes
C14 H14A I27 0.96 3.18 4.07(4) 153.6 1_655 yes
C14 H14C I33 0.96 3.20 4.08(4) 153.1 1_645 yes
C15 H15A I27 0.96 3.26 4.13(4) 151.6 1_655 yes
C15 H15C I14 0.96 3.28 3.89(4) 123.0 . yes
C16 H16A I32 0.96 3.08 3.73(5) 126.6 2_666 yes
C16 H16B I15 0.96 3.25 4.15(5) 158.2 2_666 yes
C16 H16C I34 0.96 3.31 4.00(4) 130.5 2_666 yes
C17 H17B I25 0.96 3.25 3.74(4) 113.7 2_666 yes
C17 H17C I9 0.96 3.10 4.06(4) 177.8 2_665 yes
C18 H18A I26 0.96 3.26 3.91(4) 126.2 2_666 yes
C18 H18B I18 0.96 3.33 4.01(4) 129.2 2_666 yes
C18 H18C I15 0.96 3.20 4.11(4) 159.7 2_666 yes
C19 H19A I23 0.96 3.00 3.60(5) 121.7 2_566 yes
C19 H19B I14 0.96 3.18 4.08(5) 158.0 2_666 yes
C19 H19C I27 0.96 3.04 3.95(5) 158.0 2_566 yes
C21 H21A I8 0.96 3.11 3.88(4) 138.5 . yes
C21 H21B I35 0.96 3.29 4.07(4) 139.6 1_554 yes
C21 H21C I34 0.96 3.20 4.06(4) 150.1 1_554 yes
C22 H22A I34 0.96 3.32 4.06(4) 135.2 1_554 yes
C22 H22B I16 0.96 3.33 3.98(4) 126.4 2_666 yes
C22 H22C I14 0.96 3.25 4.14(4) 155.5 2_666 yes
C23 H23B I3 0.96 3.22 3.83(4) 123.0 . yes
C23 H23C I29 0.96 3.19 4.12(4) 162.1 . yes
C24 H24A I14 0.96 3.03 3.66(5) 124.1 2_666 yes
C24 H24B I23 0.96 3.18 4.09(5) 158.7 2_566 yes
C24 H24C I10 0.96 3.04 3.92(5) 153.2 2_666 yes
C25 H25C I23 0.96 3.22 4.12(5) 157.1 2_566 yes
C26 H26A I29 0.96 3.32 4.17(4) 148.4 . yes
C26 H26A I30 0.96 3.14 3.76(4) 124.1 . yes
C27 H27A I29 0.96 3.31 4.14(4) 145.3 . yes
C27 H27B I10 0.96 3.33 3.91(4) 121.5 1_465 yes
C27 H27B I11 0.96 3.20 4.07(4) 152.4 1_465 yes
C28 H28A I1 0.96 3.32 4.12(4) 142.6 2_566 yes
C28 H28B I4 0.96 3.06 3.94(4) 152.9 2_566 yes
C28 H28C I11 0.96 3.27 4.13(4) 150.3 1_465 yes
C29 H29A I32 0.96 3.09 3.70(4) 122.7 . yes
C29 H29C I21 0.96 3.24 4.15(5) 157.3 . yes
C30 H30A I11 0.96 3.27 3.90(4) 125.1 . yes
C30 H30B I21 0.96 3.26 4.15(4) 155.4 . yes
C31 H31A I2 0.96 3.31 3.91(4) 122.9 . yes
C31 H31B I1 0.96 3.08 4.03(4) 175.5 . yes
C31 H31C I12 0.96 3.23 3.76(4) 116.5 . yes
C32 H32B I1 0.96 3.10 3.86(4) 137.0 2_566 yes
C32 H32C I30 0.96 3.30 4.22(4) 160.8 . yes
C33 H33A I21 0.96 3.05 3.80(3) 135.6 . yes
C33 H33A I23 0.96 3.25 4.00(4) 136.2 . yes
C33 H33B I30 0.96 3.30 4.21(4) 159.5 . yes
C34 H34A I4 0.96 3.06 3.99(4) 163.6 2_566 yes
C34 H34B I36 0.96 3.09 4.03(4) 166.9 . yes
C35 H35B I2 0.96 2.92 3.79(3) 151.0 . yes
C36 H36A I21 0.96 3.32 4.26(4) 168.6 2_656 yes
C36 H36B I2 0.96 3.08 3.93(3) 148.8 . yes
C36 H36C I5 0.96 2.91 3.51(4) 121.7 . yes
C37 H37A I7 0.96 2.82 3.72(4) 156.0 . yes
C37 H37A I17 0.96 3.28 3.78(2) 114.4 2_656 yes
C37 H37B I15 0.96 3.15 4.04(3) 155.9 2_656 yes

_olex2_date_sample_data_collection 2021-04-27
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.947
_oxdiff_exptl_absorpt_empirical_full_min 0.527
