# Supplementary Information (SI) for Organic & Biomolecular Chemistry.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 2324085'
loop_
_audit_author_name
_audit_author_address
'Chris Hawes'
;Keele University
United Kingdom
;
_audit_update_record             
;
2024-01-08 deposited with the CCDC.	2025-09-19 downloaded from the CCDC.
;
_audit_creation_date             2024-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H20 N2 S2'
_chemical_formula_sum            'C12 H20 N2 S2'
_chemical_formula_weight         256.42
_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'
N N 0.0061 0.0033 '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           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   8.4881(12)
_cell_length_b                   6.8098(9)
_cell_length_c                   12.4405(17)
_cell_angle_alpha                90
_cell_angle_beta                 103.668(4)
_cell_angle_gamma                90
_cell_volume                     698.73(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1967
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.982
_cell_measurement_theta_min      3.88
_shelx_estimated_absorpt_T_max   0.986
_shelx_estimated_absorpt_T_min   0.932
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0813 before and 0.0660 after correction.
The Ratio of minimum to maximum transmission is 0.8662.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6198
_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         26.327
_diffrn_reflns_theta_min         3.371
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                618
_reflns_number_total             778
_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       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         778
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0506
_refine_ls_restrained_S_all      1.093
_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)+(0.0175P)²+0.9594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0879
_refine_special_details          
;
The model was generated on the basis of two overlapping
orientations of the hydrogen bonded chains running in 
the b direction. Examination of the diffraction data
revealed no observable interstitial reflections to
suggest any long-range ordering in the directionality
of these chains, and so the model is presented in the
space group C2/m as a disordered overlap of both 
orientations, which allowed the heavy atoms positions
to be freely refined.
;
_olex2_refinement_description    
;
1. Restrained distances
 N1-H1
 0.88 with sigma of 0.02
2. Others
 Fixed Sof: H1(0.5) C1(0.5) C2(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5)
 H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5) H6C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   mixed
_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
S1 S 0.58752(11) 0.000000 0.37234(8) 0.0384(3) Uani 1 2 d S T P A .
N1 N 0.5652(4) 0.500000 0.3886(2) 0.0365(7) Uani 1 2 d DS T P . .
H1 H 0.544(8) 0.616(5) 0.413(5) 0.044 Uiso 0.5 1 d D U P . .
C1 C 0.5327(5) 0.1565(6) 0.4504(3) 0.0305(10) Uani 0.5 1 d . . P . .
C2 C 0.5306(7) 0.3698(7) 0.4505(4) 0.0304(12) Uani 0.5 1 d . . P A .
C3 C 0.6221(5) 0.5296(16) 0.2877(3) 0.030(2) Uani 0.5 1 d . . P A -1
H3A H 0.689022 0.415510 0.277111 0.036 Uiso 0.5 1 calc R U P A -1
H3B H 0.692232 0.647532 0.297090 0.036 Uiso 0.5 1 calc R U P A -1
C4 C 0.4882(6) 0.5547(7) 0.1863(3) 0.0434(16) Uani 0.5 1 d . . P A -1
H4A H 0.537746 0.559102 0.121803 0.052 Uiso 0.5 1 calc R U P A -1
H4B H 0.437845 0.684546 0.191057 0.052 Uiso 0.5 1 calc R U P A -1
C5 C 0.3550(6) 0.4046(7) 0.1623(4) 0.0380(11) Uani 0.5 1 d . . P A -1
H5A H 0.311904 0.387954 0.229108 0.046 Uiso 0.5 1 calc R U P A -1
H5B H 0.401089 0.277075 0.146891 0.046 Uiso 0.5 1 calc R U P A -1
C6 C 0.2161(5) 0.4575(12) 0.0654(3) 0.053(3) Uani 0.5 1 d . . P A -1
H6A H 0.256939 0.470822 -0.001619 0.079 Uiso 0.5 1 calc R U P A -1
H6B H 0.167722 0.581977 0.080678 0.079 Uiso 0.5 1 calc R U P A -1
H6C H 0.133812 0.353698 0.054517 0.079 Uiso 0.5 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.584(4) . ?
S1 C1 1.584(4) 6 ?
N1 H1 0.88(2) . ?
N1 H1 0.88(2) 6_565 ?
N1 C2 1.254(5) 6_565 ?
N1 C2 1.254(5) . ?
N1 C3 1.461(5) . ?
C1 C1 1.468(9) 2_656 ?
C1 C2 1.453(6) . ?
C2 C2 1.445(9) 2_656 ?
C2 C2 1.773(9) 6_565 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.495(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.501(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.517(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
C1 S1 C1 84.6(3) . 6 ?
H1 N1 H1 128(8) . 6_565 ?
C2 N1 H1 109(4) . . ?
C2 N1 H1 109(4) 6_565 6_565 ?
C2 N1 H1 20(4) 6_565 . ?
C2 N1 H1 20(4) . 6_565 ?
C2 N1 C2 90.0(4) . 6_565 ?
C2 N1 C3 127.1(5) 6_565 . ?
C2 N1 C3 143.0(5) . . ?
C3 N1 H1 108(4) . . ?
C3 N1 H1 124(4) . 6_565 ?
C1 C1 S1 137.70(15) 2_656 . ?
C2 C1 S1 132.8(4) . . ?
C2 C1 C1 89.5(3) . 2_656 ?
N1 C2 H1 35(5) . 6_565 ?
N1 C2 C1 134.5(4) . . ?
N1 C2 C2 135.0(2) . 2_656 ?
N1 C2 C2 45.0(2) . 6_565 ?
C1 C2 H1 100(5) . 6_565 ?
C1 C2 C2 179.3(3) . 6_565 ?
C2 C2 H1 167(7) 2_656 6_565 ?
C2 C2 H1 79(5) 6_565 6_565 ?
C2 C2 C1 90.5(3) 2_656 . ?
C2 C2 C2 89.999(1) 2_656 6_565 ?
N1 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
N1 C3 C4 113.7(3) . . ?
H3A C3 H3B 107.7 . . ?
C4 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
C3 C4 H4A 107.7 . . ?
C3 C4 H4B 107.7 . . ?
C3 C4 C5 118.4(5) . . ?
H4A C4 H4B 107.1 . . ?
C5 C4 H4A 107.7 . . ?
C5 C4 H4B 107.7 . . ?
C4 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
C4 C5 C6 113.8(4) . . ?
H5A C5 H5B 107.7 . . ?
C6 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

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
S1 C1 C2 N1 2.8(9) . . . . ?
S1 C1 C2 C2 -178.3(4) . . . 2_656 ?
N1 C3 C4 C5 -51.5(8) . . . . ?
C1 S1 C1 C1 1.6(7) 6 . . 2_656 ?
C1 S1 C1 C2 -179.3(4) 6 . . . ?
C1 C1 C2 N1 -177.8(5) 2_656 . . . ?
C1 C1 C2 C2 1.1(5) 2_656 . . 2_656 ?
C2 N1 C2 C1 -179.2(4) 6_565 . . . ?
C2 N1 C2 C2 2.4(10) 6_565 . . 2_656 ?
C2 N1 C3 C4 -86.4(7) 6_565 . . . ?
C2 N1 C3 C4 93.9(8) . . . . ?
C3 N1 C2 C1 0.6(10) . . . . ?
C3 N1 C2 C2 179.8(7) . . . 6_565 ?
C3 N1 C2 C2 -177.8(7) . . . 2_656 ?
C3 C4 C5 C6 173.1(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_3_BuNH3_SO4
_database_code_depnum_ccdc_archive 'CCDC 2324086'
loop_
_audit_author_name
_audit_author_address
'Chris Hawes'
;Keele University
United Kingdom
;
_audit_update_record             
;
2024-01-08 deposited with the CCDC.	2025-09-19 downloaded from the CCDC.
;
_audit_creation_date             2024-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '6(C12 H20 N2 S2), 3(O4 S), 6(C4 H12 N)'
_chemical_formula_sum            'C96 H192 N18 O12 S15'
_chemical_formula_weight         2271.56
_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'
N N 0.0061 0.0033 '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'

_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      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   17.4462(5)
_cell_length_b                   17.4462(5)
_cell_length_c                   40.0341(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     10552.7(8)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    7145
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      24.934
_cell_measurement_theta_min      2.744
_shelx_estimated_absorpt_T_max   0.978
_shelx_estimated_absorpt_T_min   0.946
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0758 before and 0.0693 after correction.
The Ratio of minimum to maximum transmission is 0.9148.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3690
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1262
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            57599
_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         27.130
_diffrn_reflns_theta_min         2.441
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3215
_reflns_number_total             5197
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         5197
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0624
_refine_ls_restrained_S_all      1.042
_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)+(0.0578P)²+21.3223P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1493
_refine_special_details          
;
The specimen was a single crystal isolated as a decomposition
product after extended exposure of the parent thiosquaramide
to water. As such, the structural model presented here could not
be validated with bulk-phase supporting methods, and so the 
disordered solvent present within the voids is taken as water
for the purposes of the electron count, but could equally well
contain acetonitrile. Neither outcome affects the main conclusion
of the structural study which is purely concerned with the hydrogen
bonding interactions between the thiosquaramide and the sulfate
guest.
;
_olex2_refinement_description    
;
1. Restrained distances
 N2-H2 = N1-H1 = N3-H3C = N3-H3E = N3-H3D
 0.9 with sigma of 0.02
 S4-O4 \\sim S4-O3 \\sim S3-O1 \\sim S3-O2
 with sigma of 0.02
 S4-O3 \\sim S4-O4
 with sigma of 0.01
2. Others
 Fixed Sof: O3(0.166667) O4(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   mixed
_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
S1 S 0.66657(5) 0.57920(6) 0.46836(2) 0.0397(2) Uani 1 1 d . . . . .
S2 S 0.49295(5) 0.49919(6) 0.40086(2) 0.0388(2) Uani 1 1 d . . . . .
N1 N 0.52927(16) 0.64133(16) 0.51286(6) 0.0311(6) Uani 1 1 d D . . . .
H1 H 0.4865(16) 0.651(2) 0.5212(8) 0.037 Uiso 1 1 d D U . . .
N2 N 0.37397(16) 0.56493(16) 0.45648(6) 0.0303(6) Uani 1 1 d D . . . .
H2 H 0.359(2) 0.5890(19) 0.4731(6) 0.036 Uiso 1 1 d D U . . .
C1 C 0.8274(3) 0.9007(3) 0.53603(13) 0.0818(16) Uani 1 1 d . . . . .
H1A H 0.841792 0.909826 0.512168 0.123 Uiso 1 1 calc R U . . .
H1B H 0.881851 0.920365 0.548941 0.123 Uiso 1 1 calc R U . . .
H1C H 0.799393 0.934927 0.542742 0.123 Uiso 1 1 calc R U . . .
C2 C 0.7639(2) 0.8024(2) 0.54262(10) 0.0509(9) Uani 1 1 d . . . . .
H2A H 0.792587 0.767978 0.536041 0.061 Uiso 1 1 calc R U . . .
H2B H 0.750607 0.793087 0.566804 0.061 Uiso 1 1 calc R U . . .
C3 C 0.6786(2) 0.7693(2) 0.52331(9) 0.0393(8) Uani 1 1 d . . . . .
H3A H 0.653205 0.807743 0.528119 0.047 Uiso 1 1 calc R U . . .
H3B H 0.691301 0.773002 0.499077 0.047 Uiso 1 1 calc R U . . .
C4 C 0.61183(19) 0.6750(2) 0.53225(8) 0.0340(7) Uani 1 1 d . . . . .
H4A H 0.637929 0.636923 0.528061 0.041 Uiso 1 1 calc R U . . .
H4B H 0.597950 0.671702 0.556369 0.041 Uiso 1 1 calc R U . . .
C5 C 0.51891(19) 0.60232(18) 0.48423(7) 0.0277(6) Uani 1 1 d . . . . .
C6 C 0.57126(19) 0.57612(18) 0.46405(8) 0.0297(7) Uani 1 1 d . . . . .
C7 C 0.50277(18) 0.54388(18) 0.43821(7) 0.0284(7) Uani 1 1 d . . . . .
C8 C 0.45114(19) 0.56866(18) 0.45890(7) 0.0267(6) Uani 1 1 d . . . . .
C9 C 0.3155(2) 0.5278(2) 0.42753(8) 0.0338(7) Uani 1 1 d . . . . .
H9A H 0.350766 0.527598 0.408197 0.041 Uiso 1 1 calc R U . . .
H9B H 0.290959 0.566503 0.421844 0.041 Uiso 1 1 calc R U . . .
C10 C 0.2398(2) 0.4349(2) 0.43307(8) 0.0360(7) Uani 1 1 d . . . . .
H10A H 0.205883 0.433910 0.453033 0.043 Uiso 1 1 calc R U . . .
H10B H 0.263775 0.394926 0.437322 0.043 Uiso 1 1 calc R U . . .
C11 C 0.1784(2) 0.4015(2) 0.40305(9) 0.0459(9) Uani 1 1 d . . . . .
H11A H 0.212544 0.401840 0.383227 0.055 Uiso 1 1 calc R U . . .
H11B H 0.155848 0.442458 0.398571 0.055 Uiso 1 1 calc R U . . .
C12 C 0.1004(3) 0.3086(3) 0.40796(12) 0.0701(13) Uani 1 1 d . . . . .
H12A H 0.063389 0.290294 0.387854 0.105 Uiso 1 1 calc R U . . .
H12B H 0.065223 0.308089 0.427140 0.105 Uiso 1 1 calc R U . . .
H12C H 0.122210 0.267430 0.412066 0.105 Uiso 1 1 calc R U . . .
S3 S 0.333333 0.666667 0.53897(3) 0.0247(3) Uani 1 3 d DS T P . .
O1 O 0.41622(12) 0.67366(13) 0.55093(5) 0.0294(5) Uani 1 1 d D . . . .
O2 O 0.333333 0.666667 0.50179(8) 0.0305(8) Uani 1 3 d DS T P . .
S4 S 0.333333 0.666667 0.666667 0.0266(4) Uani 1 6 d DS T P . .
O3 O 0.333333 0.666667 0.63102(13) 0.0284(15) Uani 0.5 3 d DS T P A 1
O4 O 0.4236(2) 0.7253(3) 0.68055(10) 0.0337(10) Uani 0.5 1 d D . P A -2
N3 N 0.48699(17) 0.80681(17) 0.60269(7) 0.0329(6) Uani 1 1 d D . . . .
H3C H 0.469(2) 0.7724(18) 0.5846(6) 0.039 Uiso 1 1 d D U . . .
H3D H 0.486(2) 0.8556(15) 0.5960(8) 0.039 Uiso 1 1 d D U . . .
H3E H 0.4453(17) 0.7778(19) 0.6182(7) 0.039 Uiso 1 1 d D U . . .
C13 C 0.5738(3) 0.8335(3) 0.61773(11) 0.0613(11) Uani 1 1 d . . . . .
H13A H 0.620753 0.875040 0.602365 0.074 Uiso 1 1 calc R U . . .
H13B H 0.579416 0.865689 0.638774 0.074 Uiso 1 1 calc R U . . .
C14 C 0.5886(3) 0.7607(3) 0.62485(11) 0.0631(11) Uani 1 1 d . . . . .
H14A H 0.582008 0.727656 0.603937 0.076 Uiso 1 1 calc R U . . .
H14B H 0.542774 0.719809 0.640691 0.076 Uiso 1 1 calc R U . . .
C15 C 0.6809(3) 0.7909(4) 0.63985(11) 0.0827(15) Uani 1 1 d . . . . .
H15A H 0.726479 0.834651 0.624618 0.099 Uiso 1 1 calc R U . . .
H15B H 0.685999 0.820916 0.661401 0.099 Uiso 1 1 calc R U . . .
C16 C 0.6991(3) 0.7181(4) 0.64546(14) 0.0924(17) Uani 1 1 d . . . . .
H16A H 0.694825 0.688271 0.624213 0.139 Uiso 1 1 calc R U . . .
H16B H 0.655784 0.675588 0.661253 0.139 Uiso 1 1 calc R U . . .
H16C H 0.758834 0.741917 0.654634 0.139 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
S1 C6 1.646(3) . ?
S2 C7 1.655(3) . ?
N1 H1 0.910(17) . ?
N1 C4 1.475(4) . ?
N1 C5 1.299(4) . ?
N2 H2 0.896(17) . ?
N2 C8 1.319(4) . ?
N2 C9 1.464(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.529(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.513(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.508(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.454(4) . ?
C5 C8 1.441(4) . ?
C6 C7 1.463(4) . ?
C7 C8 1.440(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.509(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.519(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.521(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
S3 O1 1.4692(19) . ?
S3 O1 1.4693(19) 3_565 ?
S3 O1 1.4693(19) 2_665 ?
S3 O2 1.489(3) . ?
S4 O3 1.427(5) 13_566 ?
S4 O3 1.427(5) . ?
S4 O4 1.491(4) . ?
S4 O4 1.491(4) 15_556 ?
N3 H3C 0.891(18) . ?
N3 H3D 0.900(17) . ?
N3 H3E 0.896(18) . ?
N3 C13 1.473(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.445(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.544(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.473(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

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
C4 N1 H1 117(2) . . ?
C5 N1 H1 121(2) . . ?
C5 N1 C4 121.7(3) . . ?
C8 N2 H2 117(2) . . ?
C8 N2 C9 123.3(3) . . ?
C9 N2 H2 119(2) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C3 C2 C1 111.3(3) . . ?
C3 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 . . ?
C2 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 C2 111.8(3) . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
N1 C4 C3 112.2(3) . . ?
N1 C4 H4A 109.2 . . ?
N1 C4 H4B 109.2 . . ?
C3 C4 H4A 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N1 C5 C6 135.3(3) . . ?
N1 C5 C8 134.9(3) . . ?
C8 C5 C6 89.8(2) . . ?
C5 C6 S1 135.6(2) . . ?
C5 C6 C7 89.6(2) . . ?
C7 C6 S1 134.8(2) . . ?
C6 C7 S2 133.8(2) . . ?
C8 C7 S2 136.7(2) . . ?
C8 C7 C6 89.5(2) . . ?
N2 C8 C5 133.0(3) . . ?
N2 C8 C7 136.0(3) . . ?
C7 C8 C5 91.0(2) . . ?
N2 C9 H9A 108.8 . . ?
N2 C9 H9B 108.8 . . ?
N2 C9 C10 113.6(3) . . ?
H9A C9 H9B 107.7 . . ?
C10 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
C9 C10 H10A 109.3 . . ?
C9 C10 H10B 109.3 . . ?
C9 C10 C11 111.4(3) . . ?
H10A C10 H10B 108.0 . . ?
C11 C10 H10A 109.3 . . ?
C11 C10 H10B 109.3 . . ?
C10 C11 H11A 109.0 . . ?
C10 C11 H11B 109.0 . . ?
C10 C11 C12 113.0(3) . . ?
H11A C11 H11B 107.8 . . ?
C12 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 S3 O1 109.93(9) . 3_565 ?
O1 S3 O1 109.93(9) 2_665 . ?
O1 S3 O1 109.92(9) 2_665 3_565 ?
O1 S3 O2 109.02(9) 2_665 . ?
O1 S3 O2 109.02(9) 3_565 . ?
O1 S3 O2 109.01(9) . . ?
O3 S4 O3 180.0 13_566 . ?
O3 S4 O4 68.12(16) . 15_556 ?
O3 S4 O4 111.88(16) 13_566 15_556 ?
H3C N3 H3D 103(3) . . ?
H3C N3 H3E 106(3) . . ?
H3D N3 H3E 110(3) . . ?
C13 N3 H3C 120(2) . . ?
C13 N3 H3D 109(2) . . ?
C13 N3 H3E 108(2) . . ?
N3 C13 H13A 108.7 . . ?
N3 C13 H13B 108.7 . . ?
H13A C13 H13B 107.6 . . ?
C14 C13 N3 114.2(3) . . ?
C14 C13 H13A 108.7 . . ?
C14 C13 H13B 108.7 . . ?
C13 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C13 C14 C15 113.0(4) . . ?
H14A C14 H14B 107.8 . . ?
C15 C14 H14A 109.0 . . ?
C15 C14 H14B 109.0 . . ?
C14 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C16 C15 C14 113.8(4) . . ?
C16 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 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
N1 H1 O1 0.910(17) 1.88(2) 2.765(3) 162(3) . yes
N2 H2 O2 0.896(17) 1.987(19) 2.864(3) 166(3) . yes
N3 H3C O1 0.891(18) 2.012(19) 2.889(3) 168(3) . yes
N3 H3E O3 0.896(18) 2.01(2) 2.810(3) 148(3) . yes
N3 H3E O4 0.896(18) 1.87(2) 2.731(5) 160(3) 15_556 yes

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
S1 C6 C7 S2 -2.8(5) . . . . ?
S1 C6 C7 C8 177.9(3) . . . . ?
S2 C7 C8 N2 0.7(6) . . . . ?
S2 C7 C8 C5 -178.2(3) . . . . ?
N1 C5 C6 S1 3.3(6) . . . . ?
N1 C5 C6 C7 -177.7(3) . . . . ?
N1 C5 C8 N2 -1.2(6) . . . . ?
N1 C5 C8 C7 177.7(3) . . . . ?
N2 C9 C10 C11 176.8(3) . . . . ?
C1 C2 C3 C4 -174.2(3) . . . . ?
C2 C3 C4 N1 -178.4(3) . . . . ?
C4 N1 C5 C6 3.5(5) . . . . ?
C4 N1 C5 C8 -174.9(3) . . . . ?
C5 N1 C4 C3 89.5(3) . . . . ?
C5 C6 C7 S2 178.2(3) . . . . ?
C5 C6 C7 C8 -1.1(2) . . . . ?
C6 C5 C8 N2 179.9(3) . . . . ?
C6 C5 C8 C7 -1.1(2) . . . . ?
C6 C7 C8 N2 180.0(3) . . . . ?
C6 C7 C8 C5 1.1(2) . . . . ?
C8 N2 C9 C10 100.9(3) . . . . ?
C8 C5 C6 S1 -177.9(3) . . . . ?
C8 C5 C6 C7 1.1(2) . . . . ?
C9 N2 C8 C5 179.3(3) . . . . ?
C9 N2 C8 C7 0.8(5) . . . . ?
C9 C10 C11 C12 -178.9(3) . . . . ?
N3 C13 C14 C15 178.7(3) . . . . ?
C13 C14 C15 C16 -176.6(4) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 135 electrons were 
found in a volume of 1635Å³ in 2 voids per unit cell. 
This is consistent with the presence of 
5[H2O] per Formula Unit 
which account for 150 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.187 -0.305 0.333 536.1 44.7 '5 H2O'
2 0.000 0.000 0.500 8.9 0.0 ?
3 0.368 0.163 0.667 536.1 44.7 '5 H2O'
4 -0.531 0.556 0.000 536.1 44.7 '5 H2O'
5 0.333 0.667 0.167 8.9 0.0 ?
6 0.667 0.333 0.833 8.9 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# 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_4_Pb
_database_code_depnum_ccdc_archive 'CCDC 2324087'
loop_
_audit_author_name
_audit_author_address
'Chris Hawes'
;Keele University
United Kingdom
;
_audit_update_record             
;
2024-01-08 deposited with the CCDC.	2025-09-19 downloaded from the CCDC.
;
_audit_creation_date             2024-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H24 N4 Pb S4, 2(Cl O4)'
_chemical_formula_sum            'C32 H24 Cl2 N4 O8 Pb S4'
_chemical_formula_weight         998.88
_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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Pb Pb -3.3944 10.1111 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.8074(18)
_cell_length_b                   19.4115(17)
_cell_length_c                   21.364(2)
_cell_angle_alpha                90
_cell_angle_beta                 107.795(3)
_cell_angle_gamma                90
_cell_volume                     7031.4(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7475
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      23.794
_cell_measurement_theta_min      2.616
_shelx_estimated_absorpt_T_max   0.949
_shelx_estimated_absorpt_T_min   0.507
_exptl_absorpt_coefficient_mu    5.246
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0896 before and 0.0723 after correction.
The Ratio of minimum to maximum transmission is 0.7962.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             3904
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1719
_diffrn_reflns_av_unetI/netI     0.1386
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            77976
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.412
_diffrn_reflns_theta_min         2.402
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7084
_reflns_number_total             12890
_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       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.964
_refine_diff_density_min         -1.270
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     985
_refine_ls_number_reflns         12890
_refine_ls_number_restraints     317
_refine_ls_R_factor_all          0.1409
_refine_ls_R_factor_gt           0.0581
_refine_ls_restrained_S_all      1.013
_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)+(0.0418P)²+9.0763P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1207
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 Cl4-O13 \\sim Cl4-O13A \\sim Cl4-O15 \\sim Cl4-O14 \\sim Cl4-O14A \\sim
Cl4-O15A \\sim Cl4-O16 \\sim Cl4-
 O16A
 with sigma of 0.01
 C13A-C14 \\sim C13-C14 \\sim C13-C12 \\sim C12A-C13A \\sim C12A-C11 \\sim
C12-C11 \\sim C16A-C11 ~
 C16-C11 \\sim C16A-C15A \\sim C15-C16 \\sim C15A-C14 \\sim C15-C14
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C12A)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C15A)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.02
Uanis(O16) = Uanis(O16A)
3. Rigid body (RIGU) restrains
 N7, C49, C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 Cl4, O13, O14, O15, O16, O13A, O14A, O15A, O16A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C11, C14, C12, C13, C15, C16, C12A, C13A, C15A, C16A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: H14(0.5) H14A(0.5) C12(0.5) H12(0.5) C13(0.5) H13(0.5) C15(0.5)
 H15(0.5) C16(0.5) H16(0.5) C12A(0.5) H12A(0.5) C13A(0.5) H13A(0.5) C15A(0.5)
 H15A(0.5) C16A(0.5) H16A(0.5) O13(0.6667) O14(0.6667) O15(0.6667) O16(0.6667)
 O13A(0.3333) O14A(0.3333) O15A(0.3333) O16A(0.3333)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C1(H1A), C2(H2A), C3(H3A), C4(H4A), C5(H5),
 C14(H14), C14(H14A), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
 C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C12(H12), C13(H13), C15(H15),
  C16(H16), C12A(H12A), C13A(H13A), C15A(H15A), C16A(H16A), N5(H5A), N6(H6),
 N7(H7), N8(H8), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C44(H44),
 C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
  C53(H53), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64)
;
_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
Pb1 Pb 0.66154(3) 0.58940(2) 0.54587(2) 0.03884(14) Uani 1 1 d . . . . .
S1 S 0.68770(18) 0.50185(14) 0.66783(14) 0.0393(7) Uani 1 1 d . . . . .
S2 S 0.8216(2) 0.5509(2) 0.57862(18) 0.0780(12) Uani 1 1 d . . . . .
S3 S 0.66775(19) 0.69863(14) 0.63163(13) 0.0416(8) Uani 1 1 d . . . . .
S4 S 0.74146(19) 0.69459(16) 0.49143(14) 0.0489(8) Uani 1 1 d . . . . .
N1 N 0.8425(6) 0.3806(5) 0.7597(4) 0.047(3) Uani 1 1 d . . . . .
H1 H 0.879993 0.349577 0.765225 0.056 Uiso 1 1 calc R U . . .
N2 N 0.9583(6) 0.4179(5) 0.6786(5) 0.058(3) Uani 1 1 d . . . . .
H2 H 0.974725 0.384948 0.707869 0.069 Uiso 1 1 calc R U . . .
N3 N 0.7655(6) 0.8657(4) 0.6713(4) 0.046(3) Uani 1 1 d . . . . .
H3 H 0.791663 0.903437 0.668398 0.055 Uiso 1 1 calc R U . . .
N4 N 0.8319(5) 0.8657(4) 0.5502(4) 0.042(2) Uani 1 1 d . . . . .
H4 H 0.846897 0.901356 0.576489 0.051 Uiso 1 1 calc R U . . .
C1 C 0.7716(8) 0.4320(6) 0.8285(6) 0.061(4) Uani 1 1 d . . . . .
H1A H 0.781475 0.476653 0.814664 0.073 Uiso 1 1 calc R U . . .
C2 C 0.7327(8) 0.4250(6) 0.8748(6) 0.058(4) Uani 1 1 d . . . . .
H2A H 0.715858 0.465371 0.891715 0.070 Uiso 1 1 calc R U . . .
C3 C 0.7176(8) 0.3641(6) 0.8967(6) 0.055(4) Uani 1 1 d . . . . .
H3A H 0.692189 0.360866 0.929722 0.066 Uiso 1 1 calc R U . . .
C4 C 0.7405(8) 0.3043(7) 0.8696(6) 0.059(4) Uani 1 1 d . . . . .
H4A H 0.729317 0.260022 0.883501 0.070 Uiso 1 1 calc R U . . .
C5 C 0.7796(8) 0.3105(7) 0.8222(6) 0.061(4) Uani 1 1 d . . . . .
H5 H 0.795145 0.270792 0.803270 0.074 Uiso 1 1 calc R U . . .
C6 C 0.7955(7) 0.3768(6) 0.8032(5) 0.047(3) Uani 1 1 d . . . . .
C7 C 0.8357(7) 0.4255(6) 0.7128(6) 0.045(3) Uani 1 1 d . . . . .
C8 C 0.7786(7) 0.4756(6) 0.6759(5) 0.043(3) Uani 1 1 d . . . . .
C9 C 0.8311(8) 0.4943(6) 0.6384(6) 0.052(3) Uani 1 1 d . . . . .
C10 C 0.8878(8) 0.4442(7) 0.6745(6) 0.054(3) Uani 1 1 d . . . . .
C11 C 1.0116(8) 0.4358(6) 0.6420(6) 0.063(3) Uani 1 1 d D . . . .
C14 C 1.1205(9) 0.4645(8) 0.5788(8) 0.092(5) Uani 1 1 d D . . . .
H14 H 1.161911 0.478283 0.562181 0.110 Uiso 0.5 1 calc R U P A 1
H14A H 1.157130 0.474122 0.555660 0.110 Uiso 0.5 1 calc R U P B 2
C17 C 0.6995(8) 0.9220(6) 0.7400(5) 0.052(4) Uani 1 1 d . . . . .
H17 H 0.700813 0.963475 0.716681 0.062 Uiso 1 1 calc R U . . .
C18 C 0.6638(7) 0.9210(6) 0.7902(5) 0.053(3) Uani 1 1 d . . . . .
H18 H 0.639541 0.961241 0.800307 0.063 Uiso 1 1 calc R U . . .
C19 C 0.6644(8) 0.8604(6) 0.8248(5) 0.051(4) Uani 1 1 d . . . . .
H19 H 0.640138 0.858722 0.858694 0.062 Uiso 1 1 calc R U . . .
C20 C 0.7001(8) 0.8031(6) 0.8097(5) 0.053(4) Uani 1 1 d . . . . .
H20 H 0.700840 0.761875 0.833838 0.063 Uiso 1 1 calc R U . . .
C21 C 0.7349(7) 0.8038(5) 0.7608(5) 0.042(3) Uani 1 1 d . . . . .
H21 H 0.760634 0.763856 0.751662 0.050 Uiso 1 1 calc R U . . .
C22 C 0.7320(7) 0.8635(5) 0.7249(5) 0.037(3) Uani 1 1 d . . . . .
C23 C 0.7619(7) 0.8189(5) 0.6264(5) 0.042(3) Uani 1 1 d . . . . .
C24 C 0.7254(6) 0.7538(5) 0.6077(5) 0.029(3) Uani 1 1 d . . . . .
C25 C 0.7546(6) 0.7515(5) 0.5515(5) 0.035(3) Uani 1 1 d . . . . .
C26 C 0.7909(7) 0.8189(5) 0.5708(5) 0.038(3) Uani 1 1 d . . . . .
C27 C 0.8560(7) 0.8679(6) 0.4919(6) 0.043(3) Uani 1 1 d . . . . .
C28 C 0.8767(8) 0.9316(6) 0.4745(6) 0.059(4) Uani 1 1 d . . . . .
H28 H 0.875342 0.970548 0.501064 0.071 Uiso 1 1 calc R U . . .
C29 C 0.8993(9) 0.9395(7) 0.4186(7) 0.073(4) Uani 1 1 d . . . . .
H29 H 0.913129 0.983689 0.406533 0.088 Uiso 1 1 calc R U . . .
C30 C 0.9018(7) 0.8829(7) 0.3804(6) 0.054(3) Uani 1 1 d . . . . .
H30 H 0.915228 0.887973 0.340861 0.065 Uiso 1 1 calc R U . . .
C31 C 0.8845(8) 0.8184(7) 0.4003(6) 0.064(4) Uani 1 1 d . . . . .
H31 H 0.889247 0.778786 0.375668 0.077 Uiso 1 1 calc R U . . .
C32 C 0.8602(7) 0.8109(7) 0.4562(5) 0.053(4) Uani 1 1 d . . . . .
H32 H 0.846826 0.766855 0.468937 0.063 Uiso 1 1 calc R U . . .
C12 C 0.9992(18) 0.4853(14) 0.5929(13) 0.086(8) Uani 0.5 1 d D U P C 1
H12 H 0.952684 0.512323 0.584190 0.104 Uiso 0.5 1 calc R U P C 1
C13 C 1.0493(13) 0.4988(17) 0.5553(14) 0.094(8) Uani 0.5 1 d D U P C 1
H13 H 1.036042 0.528108 0.517894 0.112 Uiso 0.5 1 calc R U P C 1
C15 C 1.1360(18) 0.4124(13) 0.6237(12) 0.070(7) Uani 0.5 1 d D U P C 1
H15 H 1.180684 0.383363 0.630524 0.084 Uiso 0.5 1 calc R U P C 1
C16 C 1.0836(12) 0.4045(16) 0.6585(15) 0.078(8) Uani 0.5 1 d D U P C 1
H16 H 1.098077 0.375557 0.696181 0.094 Uiso 0.5 1 calc R U P C 1
C12A C 1.0221(18) 0.5044(10) 0.6307(15) 0.077(7) Uani 0.5 1 d D U P C 2
H12A H 0.995644 0.540376 0.645551 0.093 Uiso 0.5 1 calc R U P C 2
C13A C 1.0753(17) 0.5162(14) 0.5955(16) 0.095(8) Uani 0.5 1 d D U P C 2
H13A H 1.081109 0.561994 0.582097 0.114 Uiso 0.5 1 calc R U P C 2
C15A C 1.1084(19) 0.3985(11) 0.5979(16) 0.084(8) Uani 0.5 1 d D U P C 2
H15A H 1.134707 0.361811 0.583930 0.101 Uiso 0.5 1 calc R U P C 2
C16A C 1.0607(14) 0.3824(13) 0.6360(13) 0.057(6) Uani 0.5 1 d D U P C 2
H16A H 1.061501 0.338711 0.656322 0.069 Uiso 0.5 1 calc R U P C 2
Pb2 Pb 0.39114(3) 0.62510(2) 0.44633(2) 0.03058(12) Uani 1 1 d . . . . .
S5 S 0.41817(19) 0.72512(14) 0.54683(13) 0.0407(8) Uani 1 1 d . . . . .
S6 S 0.52545(17) 0.69825(13) 0.42728(13) 0.0331(7) Uani 1 1 d . . . . .
S7 S 0.23517(19) 0.65746(15) 0.46407(13) 0.0418(8) Uani 1 1 d . . . . .
S8 S 0.32905(18) 0.72112(15) 0.34491(13) 0.0408(8) Uani 1 1 d . . . . .
N5 N 0.5311(5) 0.8885(4) 0.5879(4) 0.036(2) Uani 1 1 d . . . . .
H5A H 0.556907 0.925711 0.582792 0.044 Uiso 1 1 calc R U . . .
N6 N 0.5900(5) 0.8765(4) 0.4598(4) 0.040(2) Uani 1 1 d . . . . .
H6 H 0.611398 0.913027 0.482787 0.048 Uiso 1 1 calc R U . . .
N7 N 0.1159(6) 0.8177(5) 0.4269(4) 0.047(2) Uani 1 1 d . . . . .
H7 H 0.100343 0.859187 0.411982 0.057 Uiso 1 1 calc R U . . .
N8 N 0.1795(6) 0.8542(4) 0.3053(4) 0.041(2) Uani 1 1 d . . . . .
H8 H 0.139322 0.881173 0.304221 0.050 Uiso 1 1 calc R U . . .
C33 C 0.4809(7) 0.9495(5) 0.6653(5) 0.047(3) Uani 1 1 d . . . . .
H33 H 0.484789 0.990984 0.642891 0.056 Uiso 1 1 calc R U . . .
C34 C 0.4540(7) 0.9514(6) 0.7177(5) 0.045(3) Uani 1 1 d . U . . .
H34 H 0.439903 0.994181 0.732548 0.054 Uiso 1 1 calc R U . . .
C35 C 0.4468(7) 0.8913(5) 0.7498(5) 0.045(3) Uani 1 1 d . . . . .
H35 H 0.425512 0.892636 0.785540 0.055 Uiso 1 1 calc R U . . .
C36 C 0.4700(7) 0.8302(5) 0.7307(5) 0.044(3) Uani 1 1 d . . . . .
H36 H 0.466506 0.789335 0.754164 0.053 Uiso 1 1 calc R U . . .
C37 C 0.4987(7) 0.8269(5) 0.6775(5) 0.042(3) Uani 1 1 d . . . . .
H37 H 0.515037 0.784140 0.664305 0.050 Uiso 1 1 calc R U . . .
C38 C 0.5031(7) 0.8870(5) 0.6437(5) 0.037(3) Uani 1 1 d . . . . .
C39 C 0.5221(7) 0.8394(5) 0.5430(5) 0.037(3) Uani 1 1 d . . . . .
C40 C 0.4828(6) 0.7731(5) 0.5262(5) 0.029(3) Uani 1 1 d . . . . .
C41 C 0.5199(6) 0.7651(5) 0.4739(5) 0.027(2) Uani 1 1 d . . . . .
C42 C 0.5520(7) 0.8333(5) 0.4868(5) 0.033(3) Uani 1 1 d . . . . .
C43 C 0.5993(7) 0.8688(5) 0.3955(5) 0.037(3) Uani 1 1 d . . . . .
C44 C 0.5362(7) 0.8462(5) 0.3439(5) 0.040(3) Uani 1 1 d . . . . .
H44 H 0.488721 0.831843 0.351395 0.048 Uiso 1 1 calc R U . . .
C45 C 0.5433(9) 0.8447(6) 0.2803(6) 0.059(4) Uani 1 1 d . . . . .
H45 H 0.500495 0.829351 0.244323 0.071 Uiso 1 1 calc R U . . .
C46 C 0.6114(11) 0.8653(6) 0.2707(8) 0.069(5) Uani 1 1 d . . . . .
H46 H 0.616090 0.864164 0.227649 0.083 Uiso 1 1 calc R U . . .
C47 C 0.6745(10) 0.8879(7) 0.3224(9) 0.077(5) Uani 1 1 d . . . . .
H47 H 0.722320 0.901921 0.315340 0.092 Uiso 1 1 calc R U . . .
C48 C 0.6660(8) 0.8896(6) 0.3853(7) 0.057(4) Uani 1 1 d . . . . .
H48 H 0.708295 0.905877 0.421244 0.068 Uiso 1 1 calc R U . . .
C49 C 0.0709(8) 0.8368(9) 0.5219(6) 0.080(4) Uani 1 1 d . . . . .
H49 H 0.085419 0.883938 0.521833 0.095 Uiso 1 1 calc R U . . .
C50 C 0.0366(9) 0.8105(11) 0.5680(7) 0.104(5) Uani 1 1 d . . . . .
H50 H 0.027817 0.839039 0.601191 0.125 Uiso 1 1 calc R U . . .
C51 C 0.0153(11) 0.7388(11) 0.5634(8) 0.116(6) Uani 1 1 d . . . . .
H51 H -0.009887 0.720613 0.593087 0.140 Uiso 1 1 calc R U . . .
C52 C 0.0291(10) 0.6983(10) 0.5202(9) 0.116(6) Uani 1 1 d . . . . .
H52 H 0.015847 0.650842 0.519877 0.139 Uiso 1 1 calc R U . . .
C53 C 0.0629(9) 0.7230(7) 0.4743(7) 0.082(4) Uani 1 1 d . . . . .
H53 H 0.071877 0.693038 0.442237 0.098 Uiso 1 1 calc R U . . .
C54 C 0.0827(7) 0.7894(7) 0.4756(6) 0.060(3) Uani 1 1 d . . . . .
C55 C 0.1673(7) 0.7869(6) 0.4030(5) 0.041(3) Uani 1 1 d . . . . .
C56 C 0.2190(6) 0.7268(5) 0.4170(5) 0.035(3) Uani 1 1 d . . . . .
C57 C 0.2530(6) 0.7505(5) 0.3678(5) 0.030(3) Uani 1 1 d . . . . .
C58 C 0.1978(7) 0.8068(5) 0.3507(5) 0.036(3) Uani 1 1 d . . . . .
C59 C 0.2189(8) 0.8664(6) 0.2570(6) 0.049(3) Uani 1 1 d . . . . .
C60 C 0.1743(8) 0.8696(7) 0.1930(6) 0.064(4) Uani 1 1 d . . . . .
H60 H 0.118583 0.865161 0.181017 0.077 Uiso 1 1 calc R U . . .
C61 C 0.2123(10) 0.8795(7) 0.1443(6) 0.081(5) Uani 1 1 d . . . . .
H61 H 0.182587 0.879781 0.098985 0.098 Uiso 1 1 calc R U . . .
C62 C 0.2923(9) 0.8887(6) 0.1634(6) 0.061(4) Uani 1 1 d . . . . .
H62 H 0.318591 0.893846 0.131109 0.074 Uiso 1 1 calc R U . . .
C63 C 0.3329(8) 0.8904(6) 0.2260(6) 0.051(3) Uani 1 1 d . . . . .
H63 H 0.387969 0.899157 0.238743 0.061 Uiso 1 1 calc R U . . .
C64 C 0.2959(9) 0.8795(5) 0.2737(6) 0.050(3) Uani 1 1 d . . . . .
H64 H 0.325941 0.881448 0.318847 0.060 Uiso 1 1 calc R U . . .
Cl1 Cl 0.46006(17) 0.52762(12) 0.59386(12) 0.0323(7) Uani 1 1 d . . . . .
O1 O 0.5109(5) 0.5616(4) 0.5620(4) 0.059(2) Uani 1 1 d . . . . .
O2 O 0.4698(5) 0.5562(4) 0.6570(3) 0.057(2) Uani 1 1 d . . . . .
O3 O 0.3791(4) 0.5376(3) 0.5526(3) 0.0383(19) Uani 1 1 d . . . . .
O4 O 0.4788(5) 0.4563(3) 0.6002(4) 0.057(2) Uani 1 1 d . . . . .
Cl2 Cl 0.9456(2) 1.00257(15) 0.66886(15) 0.0478(8) Uani 1 1 d . . . . .
O5 O 0.8917(7) 0.9511(6) 0.6702(6) 0.133(5) Uani 1 1 d . . . . .
O6 O 0.9187(7) 1.0378(6) 0.6074(5) 0.116(4) Uani 1 1 d . . . . .
O7 O 0.9513(7) 1.0483(5) 0.7190(5) 0.113(4) Uani 1 1 d . . . . .
O8 O 1.0219(6) 0.9724(5) 0.6768(5) 0.087(3) Uani 1 1 d . . . . .
Cl3 Cl -0.0209(2) 0.7527(2) 0.23822(16) 0.0624(10) Uani 1 1 d . . . . .
O9 O -0.0034(11) 0.7628(8) 0.3052(6) 0.192(7) Uani 1 1 d . . . . .
O10 O 0.0008(13) 0.8102(8) 0.2089(8) 0.239(10) Uani 1 1 d . . . . .
O11 O -0.0958(8) 0.7508(10) 0.2121(11) 0.263(11) Uani 1 1 d . . . . .
O12 O 0.0087(11) 0.6901(8) 0.2258(7) 0.205(9) Uani 1 1 d . . . . .
Cl4 Cl 0.6572(2) 1.03820(15) 0.55116(14) 0.0551(9) Uani 1 1 d D . . . .
O13 O 0.5896(8) 1.0195(8) 0.5675(10) 0.108(5) Uani 0.6667 1 d D . P D 1
O14 O 0.7213(8) 1.0091(8) 0.6001(7) 0.100(5) Uani 0.6667 1 d D . P D 1
O15 O 0.6674(9) 1.1094(4) 0.5498(6) 0.060(4) Uani 0.6667 1 d D . P D 1
O16 O 0.6566(14) 1.0068(9) 0.4915(5) 0.101(5) Uani 0.6667 1 d D . P D 1
O13A O 0.5939(15) 1.0688(19) 0.5671(17) 0.108(9) Uani 0.3333 1 d D . P D 2
O14A O 0.7253(14) 1.0789(17) 0.5659(15) 0.113(11) Uani 0.3333 1 d D . P D 2
O15A O 0.6642(19) 0.9725(8) 0.5794(13) 0.080(7) Uani 0.3333 1 d D . P D 2
O16A O 0.622(3) 1.030(2) 0.4828(6) 0.101(5) Uani 0.3333 1 d D . P D 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
Pb1 S1 3.025(3) . ?
Pb1 S2 2.821(4) . ?
Pb1 S3 2.782(3) . ?
Pb1 S4 2.926(3) . ?
S1 C8 1.655(12) . ?
S2 C9 1.654(12) . ?
S3 C24 1.668(10) . ?
S4 C25 1.654(10) . ?
N1 H1 0.8800 . ?
N1 C6 1.430(13) . ?
N1 C7 1.305(13) . ?
N2 H2 0.8800 . ?
N2 C10 1.332(14) . ?
N2 C11 1.445(15) . ?
N3 H3 0.8800 . ?
N3 C22 1.444(12) . ?
N3 C23 1.309(12) . ?
N4 H4 0.8800 . ?
N4 C26 1.323(12) . ?
N4 C27 1.436(13) . ?
C1 H1A 0.9500 . ?
C1 C2 1.376(16) . ?
C1 C6 1.327(14) . ?
C2 H2A 0.9500 . ?
C2 C3 1.329(15) . ?
C3 H3A 0.9500 . ?
C3 C4 1.411(15) . ?
C4 H4A 0.9500 . ?
C4 C5 1.400(16) . ?
C5 H5 0.9500 . ?
C5 C6 1.404(15) . ?
C7 C8 1.454(15) . ?
C7 C10 1.459(16) . ?
C8 C9 1.450(15) . ?
C9 C10 1.444(16) . ?
C11 C12 1.389(14) . ?
C11 C16 1.365(14) . ?
C11 C12A 1.375(14) . ?
C11 C16A 1.388(14) . ?
C14 H14 0.9500 . ?
C14 H14A 0.9500 . ?
C14 C13 1.383(14) . ?
C14 C15 1.362(14) . ?
C14 C13A 1.399(14) . ?
C14 C15A 1.380(14) . ?
C17 H17 0.9500 . ?
C17 C18 1.403(14) . ?
C17 C22 1.359(14) . ?
C18 H18 0.9500 . ?
C18 C19 1.388(14) . ?
C19 H19 0.9500 . ?
C19 C20 1.367(14) . ?
C20 H20 0.9500 . ?
C20 C21 1.369(14) . ?
C21 H21 0.9500 . ?
C21 C22 1.383(13) . ?
C23 C24 1.421(13) . ?
C23 C25 2.040(14) . ?
C23 C26 1.433(14) . ?
C24 C25 1.447(12) . ?
C24 C26 2.035(14) . ?
C25 C26 1.462(14) . ?
C27 C28 1.373(14) . ?
C27 C32 1.360(14) . ?
C28 H28 0.9500 . ?
C28 C29 1.381(16) . ?
C29 H29 0.9500 . ?
C29 C30 1.377(16) . ?
C30 H30 0.9500 . ?
C30 C31 1.388(15) . ?
C31 H31 0.9500 . ?
C31 C32 1.395(15) . ?
C32 H32 0.9500 . ?
C12 H12 0.9500 . ?
C12 C13 1.395(15) . ?
C13 H13 0.9500 . ?
C15 H15 0.9500 . ?
C15 C16 1.368(14) . ?
C16 H16 0.9500 . ?
C12A H12A 0.9500 . ?
C12A C13A 1.397(15) . ?
C13A H13A 0.9500 . ?
C15A H15A 0.9500 . ?
C15A C16A 1.380(14) . ?
C16A H16A 0.9500 . ?
Pb2 S5 2.825(3) . ?
Pb2 S6 2.915(3) . ?
Pb2 S7 2.982(3) . ?
Pb2 S8 2.815(3) . ?
S5 C40 1.642(10) . ?
S6 C41 1.657(9) . ?
S7 C56 1.652(10) . ?
S8 C57 1.673(10) . ?
N5 H5A 0.8800 . ?
N5 C38 1.424(12) . ?
N5 C39 1.327(12) . ?
N6 H6 0.8800 . ?
N6 C42 1.317(12) . ?
N6 C43 1.439(12) . ?
N7 H7 0.8800 . ?
N7 C54 1.452(14) . ?
N7 C55 1.320(12) . ?
N8 H8 0.8800 . ?
N8 C58 1.304(11) . ?
N8 C59 1.435(13) . ?
C33 H33 0.9500 . ?
C33 C34 1.345(14) . ?
C33 C38 1.399(13) . ?
C34 H34 0.9500 . ?
C34 C35 1.379(14) . ?
C35 H35 0.9500 . ?
C35 C36 1.360(13) . ?
C36 H36 0.9500 . ?
C36 C37 1.383(13) . ?
C37 H37 0.9500 . ?
C37 C38 1.387(13) . ?
C39 C40 1.457(13) . ?
C39 C42 1.460(13) . ?
C40 C41 1.470(12) . ?
C41 C42 1.435(13) . ?
C43 C44 1.384(14) . ?
C43 C48 1.335(15) . ?
C44 H44 0.9500 . ?
C44 C45 1.401(14) . ?
C45 H45 0.9500 . ?
C45 C46 1.351(18) . ?
C46 H46 0.9500 . ?
C46 C47 1.38(2) . ?
C47 H47 0.9500 . ?
C47 C48 1.397(17) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C49 C50 1.406(19) . ?
C49 C54 1.413(17) . ?
C50 H50 0.9500 . ?
C50 C51 1.44(2) . ?
C51 H51 0.9500 . ?
C51 C52 1.29(2) . ?
C52 H52 0.9500 . ?
C52 C53 1.382(18) . ?
C53 H53 0.9500 . ?
C53 C54 1.335(17) . ?
C55 C56 1.460(14) . ?
C55 C57 2.024(14) . ?
C55 C58 1.435(13) . ?
C56 C57 1.440(13) . ?
C57 C58 1.442(14) . ?
C59 C60 1.356(16) . ?
C59 C64 1.333(16) . ?
C60 H60 0.9500 . ?
C60 C61 1.416(17) . ?
C61 H61 0.9500 . ?
C61 C62 1.369(18) . ?
C62 H62 0.9500 . ?
C62 C63 1.312(16) . ?
C63 H63 0.9500 . ?
C63 C64 1.388(15) . ?
C64 H64 0.9500 . ?
Cl1 O1 1.447(8) . ?
Cl1 O2 1.418(7) . ?
Cl1 O3 1.455(7) . ?
Cl1 O4 1.420(7) . ?
Cl2 O5 1.391(9) . ?
Cl2 O6 1.426(10) . ?
Cl2 O7 1.371(9) . ?
Cl2 O8 1.441(8) . ?
Cl3 O9 1.381(11) . ?
Cl3 O10 1.391(13) . ?
Cl3 O11 1.280(13) . ?
Cl3 O12 1.382(11) . ?
Cl4 O13 1.400(8) . ?
Cl4 O14 1.409(8) . ?
Cl4 O15 1.395(7) . ?
Cl4 O16 1.410(8) . ?
Cl4 O13A 1.406(9) . ?
Cl4 O14A 1.400(9) . ?
Cl4 O15A 1.399(9) . ?
Cl4 O16A 1.412(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
S2 Pb1 S1 76.10(9) . . ?
S2 Pb1 S4 72.89(10) . . ?
S3 Pb1 S1 84.05(8) . . ?
S3 Pb1 S2 101.81(11) . . ?
S3 Pb1 S4 78.68(8) . . ?
S4 Pb1 S1 140.26(9) . . ?
C8 S1 Pb1 98.7(4) . . ?
C9 S2 Pb1 102.9(5) . . ?
C24 S3 Pb1 101.0(3) . . ?
C25 S4 Pb1 97.4(4) . . ?
C6 N1 H1 116.6 . . ?
C7 N1 H1 116.6 . . ?
C7 N1 C6 126.7(10) . . ?
C10 N2 H2 115.4 . . ?
C10 N2 C11 129.3(11) . . ?
C11 N2 H2 115.4 . . ?
C22 N3 H3 115.8 . . ?
C23 N3 H3 115.8 . . ?
C23 N3 C22 128.4(9) . . ?
C26 N4 H4 114.7 . . ?
C26 N4 C27 130.6(9) . . ?
C27 N4 H4 114.7 . . ?
C2 C1 H1A 119.7 . . ?
C6 C1 H1A 119.7 . . ?
C6 C1 C2 120.5(12) . . ?
C1 C2 H2A 118.6 . . ?
C3 C2 C1 122.8(12) . . ?
C3 C2 H2A 118.6 . . ?
C2 C3 H3A 120.9 . . ?
C2 C3 C4 118.2(12) . . ?
C4 C3 H3A 120.9 . . ?
C3 C4 H4A 120.1 . . ?
C5 C4 C3 119.7(12) . . ?
C5 C4 H4A 120.1 . . ?
C4 C5 H5 120.8 . . ?
C4 C5 C6 118.5(12) . . ?
C6 C5 H5 120.8 . . ?
C1 C6 N1 123.2(11) . . ?
C1 C6 C5 120.2(11) . . ?
C5 C6 N1 116.4(11) . . ?
N1 C7 C8 138.5(11) . . ?
N1 C7 C10 132.2(12) . . ?
C8 C7 C10 89.3(10) . . ?
C7 C8 S1 139.7(10) . . ?
C9 C8 S1 129.8(10) . . ?
C9 C8 C7 90.3(10) . . ?
C8 C9 S2 131.4(11) . . ?
C10 C9 S2 138.5(10) . . ?
C10 C9 C8 90.1(9) . . ?
N2 C10 C7 128.0(12) . . ?
N2 C10 C9 141.7(12) . . ?
C9 C10 C7 90.3(10) . . ?
C12 C11 N2 126.6(15) . . ?
C16 C11 N2 118.3(17) . . ?
C16 C11 C12 115(2) . . ?
C12A C11 N2 118.3(14) . . ?
C12A C11 C16A 126(2) . . ?
C16A C11 N2 114.0(15) . . ?
C13 C14 H14 117.3 . . ?
C15 C14 H14 117.3 . . ?
C15 C14 C13 125(2) . . ?
C13A C14 H14A 122.1 . . ?
C15A C14 H14A 122.1 . . ?
C15A C14 C13A 116(2) . . ?
C18 C17 H17 120.2 . . ?
C22 C17 H17 120.2 . . ?
C22 C17 C18 119.6(10) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 C17 119.3(11) . . ?
C19 C18 H18 120.4 . . ?
C18 C19 H19 120.3 . . ?
C20 C19 C18 119.4(10) . . ?
C20 C19 H19 120.3 . . ?
C19 C20 H20 119.2 . . ?
C19 C20 C21 121.6(10) . . ?
C21 C20 H20 119.2 . . ?
C20 C21 H21 120.6 . . ?
C20 C21 C22 118.9(10) . . ?
C22 C21 H21 120.6 . . ?
C17 C22 N3 118.2(9) . . ?
C17 C22 C21 121.1(10) . . ?
C21 C22 N3 120.7(9) . . ?
N3 C23 C24 137.7(10) . . ?
N3 C23 C25 175.8(9) . . ?
N3 C23 C26 131.1(10) . . ?
C24 C23 C25 45.2(5) . . ?
C24 C23 C26 91.0(8) . . ?
C26 C23 C25 45.8(6) . . ?
S3 C24 C26 175.4(7) . . ?
C23 C24 S3 139.1(8) . . ?
C23 C24 C25 90.6(8) . . ?
C23 C24 C26 44.7(5) . . ?
C25 C24 S3 130.2(8) . . ?
C25 C24 C26 45.9(6) . . ?
S4 C25 C23 175.2(7) . . ?
C24 C25 S4 131.5(8) . . ?
C24 C25 C23 44.2(5) . . ?
C24 C25 C26 88.8(8) . . ?
C26 C25 S4 139.6(8) . . ?
C26 C25 C23 44.6(6) . . ?
N4 C26 C23 130.7(10) . . ?
N4 C26 C24 174.7(9) . . ?
N4 C26 C25 139.7(10) . . ?
C23 C26 C24 44.3(6) . . ?
C23 C26 C25 89.6(8) . . ?
C25 C26 C24 45.3(5) . . ?
C28 C27 N4 116.0(10) . . ?
C32 C27 N4 123.0(10) . . ?
C32 C27 C28 121.0(11) . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.5(12) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 H29 120.1 . . ?
C30 C29 C28 119.7(12) . . ?
C30 C29 H29 120.1 . . ?
C29 C30 H30 120.4 . . ?
C29 C30 C31 119.1(12) . . ?
C31 C30 H30 120.4 . . ?
C30 C31 H31 119.6 . . ?
C30 C31 C32 120.8(12) . . ?
C32 C31 H31 119.6 . . ?
C27 C32 C31 118.7(11) . . ?
C27 C32 H32 120.6 . . ?
C31 C32 H32 120.6 . . ?
C11 C12 H12 117.2 . . ?
C11 C12 C13 126(2) . . ?
C13 C12 H12 117.2 . . ?
C14 C13 C12 112(2) . . ?
C14 C13 H13 123.9 . . ?
C12 C13 H13 123.9 . . ?
C14 C15 H15 121.9 . . ?
C14 C15 C16 116(3) . . ?
C16 C15 H15 121.9 . . ?
C11 C16 C15 124(3) . . ?
C11 C16 H16 118.2 . . ?
C15 C16 H16 118.2 . . ?
C11 C12A H12A 123.1 . . ?
C11 C12A C13A 114(2) . . ?
C13A C12A H12A 123.1 . . ?
C14 C13A H13A 118.1 . . ?
C12A C13A C14 124(3) . . ?
C12A C13A H13A 118.1 . . ?
C14 C15A H15A 117.8 . . ?
C14 C15A C16A 124(3) . . ?
C16A C15A H15A 117.8 . . ?
C11 C16A H16A 123.1 . . ?
C15A C16A C11 114(3) . . ?
C15A C16A H16A 123.1 . . ?
S5 Pb2 S6 79.33(8) . . ?
S5 Pb2 S7 73.00(9) . . ?
S6 Pb2 S7 138.66(8) . . ?
S8 Pb2 S5 93.76(8) . . ?
S8 Pb2 S6 73.50(8) . . ?
S8 Pb2 S7 78.25(8) . . ?
C40 S5 Pb2 99.0(3) . . ?
C41 S6 Pb2 95.5(4) . . ?
C56 S7 Pb2 95.2(4) . . ?
C57 S8 Pb2 99.4(3) . . ?
C38 N5 H5A 116.8 . . ?
C39 N5 H5A 116.8 . . ?
C39 N5 C38 126.4(9) . . ?
C42 N6 H6 117.4 . . ?
C42 N6 C43 125.2(9) . . ?
C43 N6 H6 117.4 . . ?
C54 N7 H7 116.9 . . ?
C55 N7 H7 116.9 . . ?
C55 N7 C54 126.1(10) . . ?
C58 N8 H8 117.1 . . ?
C58 N8 C59 125.9(10) . . ?
C59 N8 H8 117.1 . . ?
C34 C33 H33 119.8 . . ?
C34 C33 C38 120.5(10) . . ?
C38 C33 H33 119.8 . . ?
C33 C34 H34 119.9 . . ?
C33 C34 C35 120.2(10) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 119.8 . . ?
C36 C35 C34 120.3(10) . . ?
C36 C35 H35 119.8 . . ?
C35 C36 H36 119.7 . . ?
C35 C36 C37 120.7(10) . . ?
C37 C36 H36 119.7 . . ?
C36 C37 H37 120.5 . . ?
C36 C37 C38 118.9(9) . . ?
C38 C37 H37 120.5 . . ?
C33 C38 N5 117.7(9) . . ?
C37 C38 N5 122.9(9) . . ?
C37 C38 C33 119.4(10) . . ?
N5 C39 C40 139.1(10) . . ?
N5 C39 C42 131.2(10) . . ?
C40 C39 C42 89.7(8) . . ?
C39 C40 S5 139.3(8) . . ?
C39 C40 C41 89.3(8) . . ?
C41 C40 S5 131.2(7) . . ?
C40 C41 S6 131.5(7) . . ?
C42 C41 S6 138.1(8) . . ?
C42 C41 C40 90.1(7) . . ?
N6 C42 C39 132.4(9) . . ?
N6 C42 C41 137.0(9) . . ?
C41 C42 C39 90.5(8) . . ?
C44 C43 N6 119.5(10) . . ?
C48 C43 N6 119.5(11) . . ?
C48 C43 C44 120.8(11) . . ?
C43 C44 H44 120.4 . . ?
C43 C44 C45 119.2(12) . . ?
C45 C44 H44 120.4 . . ?
C44 C45 H45 120.3 . . ?
C46 C45 C44 119.4(14) . . ?
C46 C45 H45 120.3 . . ?
C45 C46 H46 119.3 . . ?
C45 C46 C47 121.3(13) . . ?
C47 C46 H46 119.3 . . ?
C46 C47 H47 120.8 . . ?
C46 C47 C48 118.4(14) . . ?
C48 C47 H47 120.8 . . ?
C43 C48 C47 120.9(14) . . ?
C43 C48 H48 119.6 . . ?
C47 C48 H48 119.6 . . ?
C50 C49 H49 121.9 . . ?
C50 C49 C54 116.3(16) . . ?
C54 C49 H49 121.9 . . ?
C49 C50 H50 121.1 . . ?
C49 C50 C51 117.8(17) . . ?
C51 C50 H50 121.1 . . ?
C50 C51 H51 118.8 . . ?
C52 C51 C50 122.3(18) . . ?
C52 C51 H51 118.8 . . ?
C51 C52 H52 119.6 . . ?
C51 C52 C53 121(2) . . ?
C53 C52 H52 119.6 . . ?
C52 C53 H53 120.3 . . ?
C54 C53 C52 119.5(16) . . ?
C54 C53 H53 120.3 . . ?
C49 C54 N7 115.8(13) . . ?
C53 C54 N7 120.9(12) . . ?
C53 C54 C49 123.2(13) . . ?
N7 C55 C56 138.6(10) . . ?
N7 C55 C57 173.2(10) . . ?
N7 C55 C58 130.6(10) . . ?
C56 C55 C57 45.3(5) . . ?
C58 C55 C56 90.6(8) . . ?
C58 C55 C57 45.4(6) . . ?
C55 C56 S7 139.3(8) . . ?
C57 C56 S7 132.1(8) . . ?
C57 C56 C55 88.5(8) . . ?
S8 C57 C55 175.3(7) . . ?
C56 C57 S8 131.5(8) . . ?
C56 C57 C55 46.1(6) . . ?
C56 C57 C58 91.1(8) . . ?
C58 C57 S8 137.3(8) . . ?
C58 C57 C55 45.1(5) . . ?
N8 C58 C55 134.5(10) . . ?
N8 C58 C57 136.0(9) . . ?
C55 C58 C57 89.4(8) . . ?
C60 C59 N8 118.0(12) . . ?
C64 C59 N8 121.9(11) . . ?
C64 C59 C60 119.9(11) . . ?
C59 C60 H60 120.5 . . ?
C59 C60 C61 118.9(13) . . ?
C61 C60 H60 120.5 . . ?
C60 C61 H61 120.5 . . ?
C62 C61 C60 119.0(12) . . ?
C62 C61 H61 120.5 . . ?
C61 C62 H62 119.8 . . ?
C63 C62 C61 120.4(12) . . ?
C63 C62 H62 119.8 . . ?
C62 C63 H63 119.7 . . ?
C62 C63 C64 120.5(13) . . ?
C64 C63 H63 119.7 . . ?
C59 C64 C63 120.8(12) . . ?
C59 C64 H64 119.6 . . ?
C63 C64 H64 119.6 . . ?
O1 Cl1 O3 107.5(4) . . ?
O2 Cl1 O1 110.9(5) . . ?
O2 Cl1 O3 109.5(4) . . ?
O2 Cl1 O4 109.4(4) . . ?
O4 Cl1 O1 109.1(5) . . ?
O4 Cl1 O3 110.4(5) . . ?
O5 Cl2 O6 108.9(7) . . ?
O5 Cl2 O8 109.7(7) . . ?
O6 Cl2 O8 109.9(6) . . ?
O7 Cl2 O5 109.7(8) . . ?
O7 Cl2 O6 109.5(7) . . ?
O7 Cl2 O8 109.2(7) . . ?
O9 Cl3 O10 110.3(10) . . ?
O9 Cl3 O12 110.1(9) . . ?
O11 Cl3 O9 109.4(13) . . ?
O11 Cl3 O10 102.8(13) . . ?
O11 Cl3 O12 107.4(12) . . ?
O12 Cl3 O10 116.4(10) . . ?
O13 Cl4 O14 106.0(11) . . ?
O13 Cl4 O16 110.0(14) . . ?
O14 Cl4 O16 106.2(11) . . ?
O15 Cl4 O13 112.9(9) . . ?
O15 Cl4 O14 109.3(9) . . ?
O15 Cl4 O16 112.0(10) . . ?
O13A Cl4 O16A 99(2) . . ?
O14A Cl4 O13A 114(2) . . ?
O14A Cl4 O16A 112(3) . . ?
O15A Cl4 O13A 105(2) . . ?
O15A Cl4 O14A 117.4(19) . . ?
O15A Cl4 O16A 107(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
Pb1 S1 C8 C7 -168.3(12) . . . . ?
Pb1 S1 C8 C9 4.4(11) . . . . ?
Pb1 S2 C9 C8 -10.7(12) . . . . ?
Pb1 S2 C9 C10 168.5(13) . . . . ?
Pb1 S3 C24 C23 -175.4(12) . . . . ?
Pb1 S3 C24 C25 8.6(11) . . . . ?
Pb1 S4 C25 C24 -8.6(11) . . . . ?
Pb1 S4 C25 C26 177.2(13) . . . . ?
S1 C8 C9 S2 4.6(18) . . . . ?
S1 C8 C9 C10 -174.9(10) . . . . ?
S2 C9 C10 N2 -1(3) . . . . ?
S2 C9 C10 C7 -179.8(12) . . . . ?
S3 C24 C25 S4 0.4(17) . . . . ?
S3 C24 C25 C23 177.4(14) . . . . ?
S3 C24 C25 C26 176.6(9) . . . . ?
S4 C25 C26 N4 -2(3) . . . . ?
S4 C25 C26 C23 176.4(12) . . . . ?
S4 C25 C26 C24 175.7(17) . . . . ?
N1 C7 C8 S1 -5(2) . . . . ?
N1 C7 C8 C9 -179.8(15) . . . . ?
N1 C7 C10 N2 1(2) . . . . ?
N1 C7 C10 C9 179.8(13) . . . . ?
N2 C11 C12 C13 -176(3) . . . . ?
N2 C11 C16 C15 174(3) . . . . ?
N2 C11 C12A C13A 179(2) . . . . ?
N2 C11 C16A C15A 177(2) . . . . ?
N3 C23 C24 S3 -1(2) . . . . ?
N3 C23 C24 C25 175.6(15) . . . . ?
N3 C23 C24 C26 175(2) . . . . ?
N3 C23 C26 N4 2(2) . . . . ?
N3 C23 C26 C24 -175.4(18) . . . . ?
N3 C23 C26 C25 -176.2(13) . . . . ?
N4 C27 C28 C29 -178.8(12) . . . . ?
N4 C27 C32 C31 -179.8(11) . . . . ?
C1 C2 C3 C4 -2(2) . . . . ?
C2 C1 C6 N1 -173.9(12) . . . . ?
C2 C1 C6 C5 1(2) . . . . ?
C2 C3 C4 C5 1.6(19) . . . . ?
C3 C4 C5 C6 0.4(19) . . . . ?
C4 C5 C6 N1 173.8(11) . . . . ?
C4 C5 C6 C1 -1.9(19) . . . . ?
C6 N1 C7 C8 -15(2) . . . . ?
C6 N1 C7 C10 165.5(12) . . . . ?
C6 C1 C2 C3 1(2) . . . . ?
C7 N1 C6 C1 -39.5(19) . . . . ?
C7 N1 C6 C5 144.9(12) . . . . ?
C7 C8 C9 S2 179.8(10) . . . . ?
C7 C8 C9 C10 0.4(9) . . . . ?
C8 C7 C10 N2 -178.8(13) . . . . ?
C8 C7 C10 C9 0.4(9) . . . . ?
C8 C9 C10 N2 178.6(17) . . . . ?
C8 C9 C10 C7 -0.4(9) . . . . ?
C10 N2 C11 C12 -1(3) . . . . ?
C10 N2 C11 C16 175.4(19) . . . . ?
C10 N2 C11 C12A 42(2) . . . . ?
C10 N2 C11 C16A -153.0(17) . . . . ?
C10 C7 C8 S1 174.0(12) . . . . ?
C10 C7 C8 C9 -0.4(9) . . . . ?
C11 N2 C10 C7 -179.3(12) . . . . ?
C11 N2 C10 C9 2(3) . . . . ?
C11 C12 C13 C14 -9(5) . . . . ?
C11 C12A C13A C14 -6(5) . . . . ?
C14 C15 C16 C11 13(5) . . . . ?
C14 C15A C16A C11 14(4) . . . . ?
C17 C18 C19 C20 0.5(19) . . . . ?
C18 C17 C22 N3 177.6(11) . . . . ?
C18 C17 C22 C21 -4.0(19) . . . . ?
C18 C19 C20 C21 -0.6(19) . . . . ?
C19 C20 C21 C22 -1.5(18) . . . . ?
C20 C21 C22 N3 -177.8(10) . . . . ?
C20 C21 C22 C17 3.8(18) . . . . ?
C22 N3 C23 C24 4(2) . . . . ?
C22 N3 C23 C26 177.3(12) . . . . ?
C22 C17 C18 C19 1.8(19) . . . . ?
C23 N3 C22 C17 -140.5(13) . . . . ?
C23 N3 C22 C21 41.1(18) . . . . ?
C23 C24 C25 S4 -177.0(10) . . . . ?
C23 C24 C25 C26 -0.8(9) . . . . ?
C23 C25 C26 N4 -178(2) . . . . ?
C23 C25 C26 C24 -0.8(9) . . . . ?
C24 C23 C26 N4 177.8(12) . . . . ?
C24 C23 C26 C25 -0.8(9) . . . . ?
C24 C25 C26 N4 -177.5(15) . . . . ?
C24 C25 C26 C23 0.8(9) . . . . ?
C25 C23 C24 S3 -177.0(16) . . . . ?
C25 C23 C24 C26 -0.8(9) . . . . ?
C25 C23 C26 N4 178.6(17) . . . . ?
C25 C23 C26 C24 0.8(9) . . . . ?
C26 N4 C27 C28 160.8(12) . . . . ?
C26 N4 C27 C32 -21(2) . . . . ?
C26 C23 C24 S3 -176.2(11) . . . . ?
C26 C23 C24 C25 0.8(9) . . . . ?
C26 C24 C25 S4 -176.3(14) . . . . ?
C26 C24 C25 C23 0.8(9) . . . . ?
C27 N4 C26 C23 -174.8(12) . . . . ?
C27 N4 C26 C25 3(2) . . . . ?
C27 C28 C29 C30 -1(2) . . . . ?
C28 C27 C32 C31 -1.2(19) . . . . ?
C28 C29 C30 C31 -3(2) . . . . ?
C29 C30 C31 C32 4(2) . . . . ?
C30 C31 C32 C27 -2(2) . . . . ?
C32 C27 C28 C29 2(2) . . . . ?
C12 C11 C16 C15 -10(4) . . . . ?
C13 C14 C15 C16 -15(4) . . . . ?
C15 C14 C13 C12 13(4) . . . . ?
C16 C11 C12 C13 8(4) . . . . ?
C12A C11 C16A C15A -20(4) . . . . ?
C13A C14 C15A C16A -5(5) . . . . ?
C15A C14 C13A C12A 2(5) . . . . ?
C16A C11 C12A C13A 16(4) . . . . ?
Pb2 S5 C40 C39 169.8(12) . . . . ?
Pb2 S5 C40 C41 -3.3(10) . . . . ?
Pb2 S6 C41 C40 20.9(10) . . . . ?
Pb2 S6 C41 C42 -167.0(11) . . . . ?
Pb2 S7 C56 C55 -165.0(13) . . . . ?
Pb2 S7 C56 C57 18.2(11) . . . . ?
Pb2 S8 C57 C56 -9.9(11) . . . . ?
Pb2 S8 C57 C58 167.9(11) . . . . ?
S5 C40 C41 S6 -15.0(17) . . . . ?
S5 C40 C41 C42 170.3(9) . . . . ?
S6 C41 C42 N6 14(2) . . . . ?
S6 C41 C42 C39 -168.9(11) . . . . ?
S7 C56 C57 S8 -7.6(18) . . . . ?
S7 C56 C57 C55 177.9(15) . . . . ?
S7 C56 C57 C58 173.8(10) . . . . ?
S8 C57 C58 N8 9(2) . . . . ?
S8 C57 C58 C55 -174.2(11) . . . . ?
N5 C39 C40 S5 10(2) . . . . ?
N5 C39 C40 C41 -175.1(14) . . . . ?
N5 C39 C42 N6 -8(2) . . . . ?
N5 C39 C42 C41 174.9(12) . . . . ?
N6 C43 C44 C45 174.2(9) . . . . ?
N6 C43 C48 C47 -174.9(10) . . . . ?
N7 C55 C56 S7 10(2) . . . . ?
N7 C55 C56 C57 -172.0(15) . . . . ?
N7 C55 C58 N8 -10(2) . . . . ?
N7 C55 C58 C57 172.6(13) . . . . ?
N8 C59 C60 C61 -178.1(11) . . . . ?
N8 C59 C64 C63 179.3(10) . . . . ?
C33 C34 C35 C36 2.9(19) . . . . ?
C34 C33 C38 N5 -180.0(11) . . . . ?
C34 C33 C38 C37 -1.3(18) . . . . ?
C34 C35 C36 C37 -2.2(18) . . . . ?
C35 C36 C37 C38 -0.2(18) . . . . ?
C36 C37 C38 N5 -179.4(11) . . . . ?
C36 C37 C38 C33 1.9(17) . . . . ?
C38 N5 C39 C40 5(2) . . . . ?
C38 N5 C39 C42 -175.6(11) . . . . ?
C38 C33 C34 C35 -1.1(19) . . . . ?
C39 N5 C38 C33 -147.8(11) . . . . ?
C39 N5 C38 C37 33.5(17) . . . . ?
C39 C40 C41 S6 169.5(9) . . . . ?
C39 C40 C41 C42 -5.2(8) . . . . ?
C40 C39 C42 N6 172.2(12) . . . . ?
C40 C39 C42 C41 -5.3(8) . . . . ?
C40 C41 C42 N6 -172.1(13) . . . . ?
C40 C41 C42 C39 5.2(8) . . . . ?
C42 N6 C43 C44 41.2(15) . . . . ?
C42 N6 C43 C48 -145.1(11) . . . . ?
C42 C39 C40 S5 -169.6(11) . . . . ?
C42 C39 C40 C41 5.1(8) . . . . ?
C43 N6 C42 C39 -164.5(11) . . . . ?
C43 N6 C42 C41 12(2) . . . . ?
C43 C44 C45 C46 0.1(16) . . . . ?
C44 C43 C48 C47 -1.3(17) . . . . ?
C44 C45 C46 C47 -0.1(19) . . . . ?
C45 C46 C47 C48 -1(2) . . . . ?
C46 C47 C48 C43 1.2(19) . . . . ?
C48 C43 C44 C45 0.6(16) . . . . ?
C49 C50 C51 C52 2(3) . . . . ?
C50 C49 C54 N7 178.2(11) . . . . ?
C50 C49 C54 C53 0(2) . . . . ?
C50 C51 C52 C53 -2(3) . . . . ?
C51 C52 C53 C54 1(3) . . . . ?
C52 C53 C54 N7 -178.0(13) . . . . ?
C52 C53 C54 C49 0(2) . . . . ?
C54 N7 C55 C56 -12(2) . . . . ?
C54 N7 C55 C58 173.0(12) . . . . ?
C54 C49 C50 C51 -1(2) . . . . ?
C55 N7 C54 C49 142.6(12) . . . . ?
C55 N7 C54 C53 -39.2(19) . . . . ?
C55 C56 C57 S8 174.5(9) . . . . ?
C55 C56 C57 C58 -4.1(9) . . . . ?
C55 C57 C58 N8 -177.0(18) . . . . ?
C56 C55 C58 N8 173.0(13) . . . . ?
C56 C55 C58 C57 -4.1(9) . . . . ?
C56 C57 C58 N8 -172.8(13) . . . . ?
C56 C57 C58 C55 4.2(9) . . . . ?
C57 C55 C56 S7 -177.7(17) . . . . ?
C57 C55 C58 N8 177.1(18) . . . . ?
C58 N8 C59 C60 128.2(13) . . . . ?
C58 N8 C59 C64 -56.7(17) . . . . ?
C58 C55 C56 S7 -173.5(12) . . . . ?
C58 C55 C56 C57 4.1(9) . . . . ?
C59 N8 C58 C55 179.2(12) . . . . ?
C59 N8 C58 C57 -5(2) . . . . ?
C59 C60 C61 C62 -3(2) . . . . ?
C60 C59 C64 C63 -5.8(19) . . . . ?
C60 C61 C62 C63 -2(2) . . . . ?
C61 C62 C63 C64 3(2) . . . . ?
C62 C63 C64 C59 0.7(18) . . . . ?
C64 C59 C60 C61 7(2) . . . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT910_4_Pb                
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         11 Note  
RESPONSE: We have examined the individual frames for the positions of these
reflections, due to the relatively large unit cell even at d = 69.83 mm 
these 11 reflectons are either fully or partly (see OMITs) obscured by 
the beamstop.
;
