# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2020

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

data_dvdz007
_database_code_depnum_ccdc_archive 'CCDC 1914880'
loop_
_audit_author_name
_audit_author_address
'Kristof Van Hecke'
;Ghent University
Belgium
;
_audit_update_record             
;
2019-05-08 deposited with the CCDC.	2020-04-23 downloaded from the CCDC.
;
_audit_creation_date             2019-03-08
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C17 H16 N S2, I3 Pb, C4 H6 O2'
_chemical_formula_sum            'C21 H22 I3 N O2 Pb S2'
_chemical_formula_weight         972.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C21 H22 I3 N O2 Pb S2'
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'
I I -0.4742 1.8119 '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                   8.61360(10)
_cell_length_b                   37.1171(7)
_cell_length_c                   8.01050(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.825(2)
_cell_angle_gamma                90
_cell_volume                     2559.75(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17047
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.4540
_cell_measurement_theta_min      3.0190
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    10.391
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.523
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-12 -2 0 0.0898
10 0 -6 0.0171
0 39 8 0.1218
-9 -2 8 0.1366
2 -51 -2 0.0066
-2 51 1 0.0807
-2 7 -11 0.0923
-1 -8 11 0.1571
12 1 1 0.0399
1 -48 -5 0.0068
3 -50 2 0.0213

_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.093
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-11.9988 -1.9730 0.0025 -0.8641 0.4130 0.2469
9.9987 -0.0239 -6.0032 0.8677 -0.2963 0.3039
0.0008 39.0032 8.0053 -0.4507 -0.7130 -0.5891
-8.9988 -1.9780 8.0031 -0.8262 0.2940 -0.5010
1.9991 -51.0068 -2.0060 0.5437 0.8434 0.0040
-1.9991 51.0066 1.0059 -0.5210 -0.8403 0.0816
-2.0002 7.0023 -11.0006 0.0550 -0.0268 1.0009
-0.9995 -7.9956 11.0011 -0.2676 0.1389 -0.9404
11.9989 0.9733 0.9976 0.8483 -0.3984 -0.3349
0.9991 -48.0051 -5.0060 0.5179 0.8312 0.2892
2.9992 -50.0081 1.9945 0.5192 0.7820 -0.3569

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            29003
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.746
_diffrn_reflns_theta_min         2.429
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00  35.00   0.50   15.00    --   10.40 -38.00 -60.00  198
  2  ω    -22.00  87.00   0.50   15.00    --   10.40  77.00-150.00  218
  3  ω    -14.00  85.00   0.50   15.00    --   10.40  38.00  90.00  198
  4  ω    -83.00 -36.00   0.50   15.00    --  -11.11 149.00  23.29   94
  5  ω    -36.00  10.00   0.50   15.00    --  -11.11  38.00 150.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0731444000
_diffrn_orient_matrix_UB_12      -0.0068997000
_diffrn_orient_matrix_UB_13      -0.0226917000
_diffrn_orient_matrix_UB_21      -0.0315191000
_diffrn_orient_matrix_UB_22      -0.0176499000
_diffrn_orient_matrix_UB_23      -0.0030687000
_diffrn_orient_matrix_UB_31      -0.0209967000
_diffrn_orient_matrix_UB_32      0.0024646000
_diffrn_orient_matrix_UB_33      -0.0855976000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5812
_reflns_number_total             6474
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.549
_refine_diff_density_min         -1.813
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         6474
_refine_ls_number_restraints     390
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0305
_refine_ls_restrained_S_all      1.120
_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)+(0.0114P)²+19.4875P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0600
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.004 and
sigma for terminal atoms of 0.008
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C20(H20A,H20B), C19(H19A,
 H19B), C21(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C13(H13)
4.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_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 0.68261(2) 0.24872(2) 0.51751(2) 0.01499(5) Uani 1 1 d . U . . .
I1 I 0.43430(3) 0.21552(2) 0.77353(4) 0.01778(7) Uani 1 1 d . U . . .
I2 I 0.64979(4) 0.31743(2) 0.75864(4) 0.01947(7) Uani 1 1 d . U . . .
I3 I 0.95175(3) 0.22235(2) 0.79807(4) 0.01799(7) Uani 1 1 d . U . . .
S1 S 0.0152(2) 0.53161(4) 0.6558(3) 0.0529(5) Uani 1 1 d . U . . .
S2 S 0.3094(3) 0.48658(5) 1.0198(3) 0.0647(7) Uani 1 1 d . U . . .
N1 N 0.2210(5) 0.30172(12) 0.6436(5) 0.0230(9) Uani 1 1 d . U . . .
H1A H 0.173323 0.294337 0.546560 0.028 Uiso 1 1 calc GR . . . .
H1B H 0.254429 0.282155 0.703056 0.028 Uiso 1 1 calc GR . . . .
H1C H 0.303651 0.315920 0.620256 0.028 Uiso 1 1 calc GR . . . .
C1 C 0.1462(7) 0.56529(15) 0.7166(7) 0.0280(10) Uani 1 1 d . U . . .
C2 C 0.1494(8) 0.60026(17) 0.6547(9) 0.0383(12) Uani 1 1 d . U . . .
H2 H 0.074081 0.608088 0.573456 0.046 Uiso 1 1 calc R . . . .
C3 C 0.2641(7) 0.62341(16) 0.7135(7) 0.0310(10) Uani 1 1 d . U . . .
H3 H 0.269754 0.647156 0.669830 0.037 Uiso 1 1 calc R . . . .
C4 C 0.3710(7) 0.61225(17) 0.8356(8) 0.0335(11) Uani 1 1 d . U . . .
H4 H 0.448258 0.628595 0.876183 0.040 Uiso 1 1 calc R . . . .
C5 C 0.3669(8) 0.57773(17) 0.8992(8) 0.0390(13) Uani 1 1 d . U . . .
H5 H 0.440133 0.570479 0.983844 0.047 Uiso 1 1 calc R . . . .
C6 C 0.2547(6) 0.55351(15) 0.8386(7) 0.0245(9) Uani 1 1 d . U . . .
C7 C 0.2256(7) 0.51647(15) 0.8782(7) 0.0258(9) Uani 1 1 d . U . . .
C8 C 0.1036(6) 0.50111(15) 0.7911(7) 0.0222(8) Uani 1 1 d . U . . .
C9 C 0.0749(6) 0.46440(14) 0.8323(6) 0.0212(8) Uani 1 1 d . U . . .
C10 C -0.0369(7) 0.44004(16) 0.7730(8) 0.0314(11) Uani 1 1 d . U . . .
H10 H -0.111927 0.447358 0.690289 0.038 Uiso 1 1 calc R . . . .
C11 C -0.0387(7) 0.40536(15) 0.8341(7) 0.0284(10) Uani 1 1 d . U . . .
H11 H -0.116250 0.389175 0.792727 0.034 Uiso 1 1 calc R . . . .
C12 C 0.0693(6) 0.39316(15) 0.9549(6) 0.0226(8) Uani 1 1 d . U . . .
C13 C 0.1785(8) 0.41765(17) 1.0161(8) 0.0353(12) Uani 1 1 d . U . . .
H13 H 0.252197 0.410414 1.100267 0.042 Uiso 1 1 calc R . . . .
C14 C 0.1808(7) 0.45233(16) 0.9560(7) 0.0292(10) Uani 1 1 d . U . . .
C15 C 0.0702(7) 0.35492(15) 1.0169(7) 0.0261(8) Uani 1 1 d . U . . .
H15A H -0.037238 0.345450 1.010864 0.031 Uiso 1 1 calc R . . . .
H15B H 0.105877 0.354680 1.135630 0.031 Uiso 1 1 calc R . . . .
C16 C 0.1752(6) 0.32989(15) 0.9172(6) 0.0232(9) Uani 1 1 d . U . . .
H16A H 0.279008 0.341067 0.909061 0.028 Uiso 1 1 calc R . . . .
H16B H 0.188161 0.306781 0.977727 0.028 Uiso 1 1 calc R . . . .
C17 C 0.1093(6) 0.32254(15) 0.7433(6) 0.0211(9) Uani 1 1 d . U . . .
H17A H 0.011303 0.308796 0.750762 0.025 Uiso 1 1 calc R . . . .
H17B H 0.085493 0.345667 0.686525 0.025 Uiso 1 1 calc R . . . .
O1 O 0.3187(6) 0.42569(13) 0.4170(6) 0.0457(10) Uani 1 1 d . U . . .
O0AA O 0.2931(6) 0.36994(13) 0.4944(6) 0.0461(11) Uani 1 1 d . U . . .
C20 C 0.5123(10) 0.4469(2) 0.5981(10) 0.0533(16) Uani 1 1 d . U . . .
H20A H 0.514117 0.463712 0.694262 0.064 Uiso 1 1 calc R . . . .
H20B H 0.617200 0.446219 0.551087 0.064 Uiso 1 1 calc R . . . .
C18 C 0.3481(7) 0.39798(17) 0.5163(8) 0.0330(10) Uani 1 1 d . U . . .
C19 C 0.4018(8) 0.45785(19) 0.4767(9) 0.0424(13) Uani 1 1 d . U . . .
H19A H 0.453460 0.469799 0.382943 0.051 Uiso 1 1 calc R . . . .
H19B H 0.328195 0.475128 0.525226 0.051 Uiso 1 1 calc R . . . .
C21 C 0.4633(10) 0.4101(2) 0.6511(10) 0.0511(15) Uani 1 1 d . U . . .
H21A H 0.414142 0.410901 0.761037 0.061 Uiso 1 1 calc R . . . .
H21B H 0.553473 0.393529 0.658451 0.061 Uiso 1 1 calc R . . . .


_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 I1 3.1447(3) 4_565 ?
Pb1 I1 3.2525(4) . ?
Pb1 I2 3.2171(4) . ?
Pb1 I2 3.2205(4) 4_565 ?
Pb1 I3 3.1427(4) 4_565 ?
Pb1 I3 3.3244(3) . ?
S1 C1 1.743(6) . ?
S1 C8 1.727(6) . ?
S2 C7 1.728(6) . ?
S2 C14 1.752(6) . ?
N1 C17 1.486(6) . ?
C1 C2 1.390(8) . ?
C1 C6 1.401(8) . ?
C2 C3 1.381(8) . ?
C3 C4 1.386(8) . ?
C4 C5 1.380(9) . ?
C5 C6 1.396(8) . ?
C6 C7 1.435(8) . ?
C7 C8 1.367(7) . ?
C8 C9 1.425(8) . ?
C9 C10 1.394(7) . ?
C9 C14 1.399(8) . ?
C10 C11 1.378(8) . ?
C11 C12 1.397(8) . ?
C12 C13 1.386(8) . ?
C12 C15 1.503(8) . ?
C13 C14 1.375(8) . ?
C15 C16 1.538(8) . ?
C16 C17 1.512(7) . ?
O1 C18 1.320(8) . ?
O1 C19 1.464(8) . ?
O0AA C18 1.154(8) . ?
C20 C19 1.400(10) . ?
C20 C21 1.498(10) . ?
C18 C21 1.511(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 Pb1 I1 95.961(10) 4_565 . ?
I1 Pb1 I2 88.144(9) 4_565 . ?
I1 Pb1 I2 82.967(9) 4_565 4_565 ?
I1 Pb1 I3 171.998(10) 4_565 . ?
I1 Pb1 I3 85.445(9) . . ?
I2 Pb1 I1 81.352(9) . . ?
I2 Pb1 I1 94.079(10) 4_565 . ?
I2 Pb1 I2 169.551(12) . 4_565 ?
I2 Pb1 I3 84.274(9) . . ?
I2 Pb1 I3 104.821(9) 4_565 . ?
I3 Pb1 I1 173.589(10) 4_565 . ?
I3 Pb1 I1 90.427(9) 4_565 4_565 ?
I3 Pb1 I2 87.223(9) 4_565 4_565 ?
I3 Pb1 I2 98.364(10) 4_565 . ?
I3 Pb1 I3 88.154(10) 4_565 . ?
Pb1 I1 Pb1 77.530(8) 4_566 . ?
Pb1 I2 Pb1 76.974(7) . 4_566 ?
Pb1 I3 Pb1 76.501(7) 4_566 . ?
C8 S1 C1 91.5(3) . . ?
C7 S2 C14 91.6(3) . . ?
C2 C1 S1 126.2(5) . . ?
C2 C1 C6 121.3(5) . . ?
C6 C1 S1 112.5(4) . . ?
C3 C2 C1 118.8(6) . . ?
C2 C3 C4 120.5(6) . . ?
C5 C4 C3 120.9(6) . . ?
C4 C5 C6 119.7(6) . . ?
C1 C6 C7 109.6(5) . . ?
C5 C6 C1 118.8(5) . . ?
C5 C6 C7 131.6(5) . . ?
C6 C7 S2 133.5(4) . . ?
C8 C7 S2 111.4(4) . . ?
C8 C7 C6 115.1(5) . . ?
C7 C8 S1 111.3(4) . . ?
C7 C8 C9 114.6(5) . . ?
C9 C8 S1 134.1(4) . . ?
C10 C9 C8 131.6(5) . . ?
C10 C9 C14 117.5(5) . . ?
C14 C9 C8 110.9(5) . . ?
C11 C10 C9 120.0(5) . . ?
C10 C11 C12 122.3(5) . . ?
C11 C12 C15 122.1(5) . . ?
C13 C12 C11 117.5(5) . . ?
C13 C12 C15 120.4(5) . . ?
C14 C13 C12 120.5(6) . . ?
C9 C14 S2 111.5(4) . . ?
C13 C14 S2 126.4(5) . . ?
C13 C14 C9 122.1(5) . . ?
C12 C15 C16 113.3(5) . . ?
C17 C16 C15 112.2(4) . . ?
N1 C17 C16 111.0(4) . . ?
C18 O1 C19 110.9(5) . . ?
C19 C20 C21 105.6(6) . . ?
O1 C18 C21 108.0(6) . . ?
O0AA C18 O1 122.7(6) . . ?
O0AA C18 C21 129.3(6) . . ?
C20 C19 O1 107.8(6) . . ?
C20 C21 C18 104.7(6) . . ?

_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_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 1.829
_oxdiff_exptl_absorpt_empirical_full_min 0.729

####################################################################### 
# 
# 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_dvdz011
_database_code_depnum_ccdc_archive 'CCDC 1985268'
loop_
_audit_author_name
_audit_author_address
'Kristof Van Hecke'
;Ghent University
Belgium
;
_audit_update_record             
;
2020-02-20 deposited with the CCDC.	2020-04-23 downloaded from the CCDC.
;
_audit_creation_date             2019-10-18
_audit_creation_method           
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I10 Pb3, 4(C17 H16 N S2)'
_chemical_formula_sum            'C68 H64 I10 N4 Pb3 S8'
_chemical_formula_weight         3084.28
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C68 H64 I10 N4 Pb3 S8'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   21.7102(2)
_cell_length_b                   8.53560(10)
_cell_length_c                   45.5345(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8437.98(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    25658
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      73.5460
_cell_measurement_theta_min      2.7750
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    42.333
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.543
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.428
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5616
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 5 3 0.0966
2 -5 -3 0.0966
-14 0 -5 0.0784
14 0 5 0.0344
-3 0 29 0.0355
3 0 -29 0.0175
-8 3 -18 0.0777
9 3 -17 0.0491
-7 -3 19 0.0939
-6 -4 -13 0.0975
12 3 8 0.0571
13 -3 2 0.0591

_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.053
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.8873 5.4697 2.5407 0.2248 0.9381 -0.2633
1.8873 -5.4697 -2.5407 -0.2248 -0.9381 0.2633
-13.8806 -0.2777 -4.9110 -0.0450 -0.1919 -0.9804
13.8806 0.2777 4.9110 0.0450 0.1919 0.9804
-2.5929 0.0144 29.0514 -0.9421 0.3330 -0.0401
2.5929 -0.0144 -29.0514 0.9421 -0.3330 0.0401
-7.9998 3.0000 -18.0014 0.6388 0.2396 -0.7218
9.0002 3.0001 -16.9963 0.8303 0.3577 0.4637
-7.0002 -3.0001 18.9969 -0.8666 -0.3213 -0.3151
-5.9999 -4.0000 -13.0029 0.0875 -0.8651 -0.3738
12.0000 3.0001 8.0044 0.0874 0.6747 0.7928
12.9999 -2.9999 2.0030 -0.0727 -0.3994 0.9918

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            75572
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.123
_diffrn_reflns_theta_min         2.812
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -14.00   1.00    2.00    --  -41.68 -57.00 -60.00  101
  2  ω    -87.00  -6.00   1.00    2.00    --  -41.68 125.00-120.00   81
  3  ω    103.00 178.00   1.00   12.00    --  106.01  77.00 -90.00   75
  4  ω     74.00 158.00   1.00   12.00    --  106.01 161.00 174.00   84
  5  ω     33.00 112.00   1.00   12.00    --  106.01-125.00  60.00   79
  6  ω    103.00 178.00   1.00   12.00    --  106.01  77.00-120.00   75
  7  ω     97.00 178.00   1.00   12.00    --  106.01 125.00-120.00   81
  8  ω    103.00 178.00   1.00   12.00    --  106.01  77.00 -60.00   75
  9  ω     30.00 134.00   1.00   12.00    --  106.01 -30.00 -60.00  104
 10  ω   -115.00 -14.00   1.00    2.00    --  -41.68 -57.00 150.00  101
 11  ω   -116.00 -17.00   1.00    2.00    --  -41.68 -38.00  30.00   99
 12  ω     33.00 132.00   1.00   12.00    --  106.01 -45.00-180.00   99
 13  ω     77.00 178.00   1.00   12.00    --  106.01  61.00   0.00  101
 14  ω     78.00 178.00   1.00   12.00    --  106.01  30.00-150.00  100
 15  ω     53.00 178.00   1.00   12.00    --  106.01  15.00 120.00  125
 16  ω   -115.00 -78.00   1.00    2.00    --  -41.68 -57.00-150.00   37
 17  ω    -87.00  -6.00   1.00    2.00    --  -41.68 125.00  60.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0131108000
_diffrn_orient_matrix_UB_12      0.0601584000
_diffrn_orient_matrix_UB_13      -0.0312879000
_diffrn_orient_matrix_UB_21      0.0062355000
_diffrn_orient_matrix_UB_22      0.1681239000
_diffrn_orient_matrix_UB_23      0.0119344000
_diffrn_orient_matrix_UB_31      0.0694498000
_diffrn_orient_matrix_UB_32      -0.0264277000
_diffrn_orient_matrix_UB_33      0.0048306000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7760
_reflns_number_total             8475
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.987
_refine_diff_density_min         -2.470
_refine_diff_density_rms         0.296
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         8475
_refine_ls_number_restraints     105
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0698
_refine_ls_restrained_S_all      1.047
_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)+(0.0689P)²+313.9139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1725
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C10-C15
 1.508 with sigma of 0.01
 C15-C16A
 1.529 with sigma of 0.01
 C16A-C17A
 1.517 with sigma of 0.01
 C17A-N1A
 1.484 with sigma of 0.01
 C15-C16B
 1.529 with sigma of 0.01
 C16B-C17B
 1.517 with sigma of 0.01
 C17B-N1B
 1.484 with sigma of 0.01
 C27-C32A = C27-C32B
 1.508 with sigma of 0.01
 C32A-C33A = C32B-C33B
 1.529 with sigma of 0.01
 C33A-C34A = C33B-C34B
 1.517 with sigma of 0.01
 C34A-N2A = C34B-N2B
 1.484 with sigma of 0.01
 C10-C16A = C10-C16B
 2.538 with sigma of 0.02
 C15-C17A = C15-C17B
 2.529 with sigma of 0.02
 C16A-N1A = C16B-N1B
 2.482 with sigma of 0.02
 C27-C33A = C27-C33B
 2.538 with sigma of 0.02
 C32A-C34A = C32B-C34B
 2.529 with sigma of 0.02
 C33A-N2A = C33B-N2B
 2.482 with sigma of 0.02
 C26-C32A = C26-C32B
 2.52 with sigma of 0.02
 C28-C32A = C28-C32B
 2.52 with sigma of 0.02
3. Restrained planarity
 C26, C27, C28, C32A
 with sigma of 0.1
 C26, C27, C28, C32B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C16A) = Uanis(C16B)
Uanis(C17A) = Uanis(C17B)
Uanis(N1A) = Uanis(N1B)
Uanis(C32A) = Uanis(C32B)
Uanis(C33A) = Uanis(C33B)
Uanis(C34A) = Uanis(C34B)
Uanis(N2A) = Uanis(N2B)
5. Rigid body (RIGU) restrains
 C27, C32A, C33A, C34A, N2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C27, C32B, C33B, C34B, N2B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C15, C16A, C17A, N1A, C16B, C17B, N1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(H15C)=Sof(H15D)=Sof(C16B)=Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=
 Sof(H17D)=Sof(N1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(N2B)=Sof(H2BA)=Sof(H2BB)=
 Sof(H2BC)=Sof(C34B)=Sof(H34C)=Sof(H34D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=
 Sof(C33B)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C17A)=Sof(H17A)=Sof(H17B)=
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H15A)=Sof(H15B)=Sof(C34A)=Sof(H34A)=
 Sof(H34B)=Sof(N2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C33A)=Sof(H33A)=Sof(H33B)=
 Sof(C32A)=Sof(H32A)=Sof(H32B)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C17A(H17A,H17B), C16A(H16A,H16B), C15(H15A,H15B), C15(H15C,H15D), C34A(H34A,
 H34B), C33A(H33A,H33B), C32A(H32A,H32B), C16B(H16C,H16D), C17B(H17C,H17D),
 C34B(H34C,H34D), C32B(H32C,H32D), C33B(H33C,H33D)
7.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12), C11(H11), C22(H22), C29(H29), C5(H5), C19(H19), C21(H21),
 C26(H26), C2(H2), C20(H20), C3(H3), C4(H4), C28(H28)
7.c Idealised Me refined as rotating group:
 N1A(H1AA,H1AB,H1AC), N2A(H2AA,H2AB,H2AC), N1B(H1BA,H1BB,H1BC), N2B(H2BA,H2BB,
 H2BC)
;
_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
Pb2 Pb 0.500000 0.500000 0.500000 0.02958(17) Uani 1 2 d S T P . .
Pb1 Pb 0.34664(2) 0.57330(6) 0.44976(2) 0.02990(14) Uani 1 1 d . . . . .
I3 I 0.47823(3) 0.77433(9) 0.45307(2) 0.03140(18) Uani 1 1 d . . . . .
I5 I 0.43321(4) 0.26612(10) 0.45440(2) 0.0395(2) Uani 1 1 d . . . . .
I4 I 0.63665(4) 0.42007(12) 0.47762(2) 0.0416(2) Uani 1 1 d . . . . .
I1 I 0.21814(4) 0.40602(12) 0.45164(3) 0.0606(3) Uani 1 1 d . . . . .
I2 I 0.34341(6) 0.58066(15) 0.38155(2) 0.0600(3) Uani 1 1 d . . . . .
S4 S 0.3651(2) 0.6963(6) 0.72134(10) 0.0602(11) Uani 1 1 d . . . . .
S3 S 0.5172(2) 0.5032(6) 0.67783(12) 0.0658(12) Uani 1 1 d . . . . .
S2 S 0.2439(2) -0.0135(7) 0.67771(13) 0.0770(15) Uani 1 1 d . . . . .
S1 S 0.3859(2) 0.2315(7) 0.71867(16) 0.0826(17) Uani 1 1 d . . . . .
N1A N 0.3888(8) -0.004(3) 0.5074(4) 0.043(4) Uani 0.654(12) 1 d D U . A 1
H1AA H 0.385580 0.006934 0.487550 0.052 Uiso 0.654(12) 1 calc GR . . A 1
H1AB H 0.386182 -0.107254 0.512184 0.052 Uiso 0.654(12) 1 calc GR . . A 1
H1AC H 0.425707 0.034718 0.513471 0.052 Uiso 0.654(12) 1 calc GR . . A 1
C17A C 0.3382(10) 0.083(3) 0.5219(3) 0.055(4) Uani 0.654(12) 1 d D U . A 1
H17A H 0.298139 0.043016 0.514792 0.065 Uiso 0.654(12) 1 calc R . . A 1
H17B H 0.340975 0.195499 0.516480 0.065 Uiso 0.654(12) 1 calc R . . A 1
C10 C 0.3071(7) 0.172(2) 0.6025(3) 0.059(5) Uani 1 1 d D . . . .
C13 C 0.3357(7) 0.1667(19) 0.6618(5) 0.055(4) Uani 1 1 d . . . . .
C8 C 0.2856(7) 0.082(2) 0.6511(5) 0.055(4) Uani 1 1 d . . . . .
C25 C 0.4114(8) 0.613(2) 0.7489(4) 0.056(4) Uani 1 1 d . . . . .
C9 C 0.2708(7) 0.085(2) 0.6200(5) 0.067(6) Uani 1 1 d . . . . .
H9 H 0.237045 0.027072 0.612305 0.081 Uiso 1 1 calc R . . . .
C16A C 0.3412(9) 0.068(3) 0.5549(3) 0.052(4) Uani 0.654(12) 1 d D U . A 1
H16A H 0.383093 0.094794 0.561786 0.062 Uiso 0.654(12) 1 calc R . . A 1
H16B H 0.332840 -0.042467 0.560503 0.062 Uiso 0.654(12) 1 calc R . . A 1
C12 C 0.3722(8) 0.253(2) 0.6418(6) 0.070(6) Uani 1 1 d . . . . .
H12 H 0.407032 0.309500 0.648565 0.084 Uiso 1 1 calc R . . . .
C11 C 0.3571(8) 0.254(2) 0.6129(5) 0.069(6) Uani 1 1 d . . . . .
H11 H 0.381647 0.312707 0.599589 0.083 Uiso 1 1 calc R . . . .
C15 C 0.2935(7) 0.176(2) 0.5701(3) 0.065(4) Uani 1 1 d D U . . .
H15A H 0.297344 0.284801 0.562528 0.078 Uiso 0.654(12) 1 calc R . . A 1
H15B H 0.251092 0.139038 0.566250 0.078 Uiso 0.654(12) 1 calc R . . A 1
H15C H 0.271874 0.276297 0.566030 0.078 Uiso 0.346(12) 1 calc R . . A 2
H15D H 0.263952 0.091025 0.565889 0.078 Uiso 0.346(12) 1 calc R . . A 2
C31 C 0.4659(7) 0.5621(19) 0.7053(4) 0.049(4) Uani 1 1 d . . . . .
C30 C 0.4646(9) 0.5418(18) 0.7365(5) 0.062(5) Uani 1 1 d . . . . .
C23 C 0.4172(7) 0.661(2) 0.6631(4) 0.051(4) Uani 1 1 d . . . . .
C14 C 0.3382(7) 0.153(2) 0.6928(5) 0.058(5) Uani 1 1 d . . . . .
C22 C 0.3756(8) 0.729(3) 0.6444(4) 0.065(5) Uani 1 1 d . . . . .
H22 H 0.339650 0.777540 0.652097 0.078 Uiso 1 1 calc R . . . .
C29 C 0.5066(9) 0.464(2) 0.7536(5) 0.069(5) Uani 1 1 d . . . . .
H29 H 0.542841 0.417286 0.745886 0.083 Uiso 1 1 calc R . . . .
C7 C 0.2926(7) 0.061(2) 0.7046(6) 0.067(6) Uani 1 1 d . . . . .
C6 C 0.2940(8) 0.050(2) 0.7365(5) 0.060(5) Uani 1 1 d . . . . .
C5 C 0.2572(11) -0.030(3) 0.7552(6) 0.083(7) Uani 1 1 d . . . . .
H5 H 0.222896 -0.089099 0.748314 0.100 Uiso 1 1 calc R . . . .
C18 C 0.4701(8) 0.585(2) 0.6512(5) 0.062(5) Uani 1 1 d . . . . .
C19 C 0.4807(9) 0.582(3) 0.6211(5) 0.072(6) Uani 1 1 d . . . . .
H19 H 0.516001 0.532940 0.612867 0.086 Uiso 1 1 calc R . . . .
C21 C 0.3853(10) 0.727(3) 0.6149(5) 0.083(7) Uani 1 1 d . . . . .
H21 H 0.356688 0.775720 0.601993 0.100 Uiso 1 1 calc R . . . .
C1 C 0.3429(8) 0.138(2) 0.7469(5) 0.068(6) Uani 1 1 d . . . . .
C24 C 0.4165(8) 0.640(2) 0.6943(5) 0.061(5) Uani 1 1 d . . . . .
C26 C 0.3979(11) 0.602(3) 0.7781(4) 0.080(6) Uani 1 1 d D . . . .
H26 H 0.360841 0.646071 0.785512 0.096 Uiso 1 1 calc R . . . .
C2 C 0.3568(11) 0.149(3) 0.7758(6) 0.089(8) Uani 1 1 d . . . . .
H2 H 0.390855 0.209389 0.782359 0.107 Uiso 1 1 calc R . . . .
C20 C 0.4362(9) 0.654(3) 0.6038(5) 0.082(7) Uani 1 1 d . . . . .
H20 H 0.441555 0.652288 0.583100 0.098 Uiso 1 1 calc R . . . .
C3 C 0.3190(11) 0.068(3) 0.7956(6) 0.083(7) Uani 1 1 d . . . . .
H3 H 0.325723 0.074349 0.816201 0.100 Uiso 1 1 calc R . . . .
C27 C 0.4383(11) 0.527(2) 0.7967(3) 0.088(6) Uani 1 1 d D U . . .
C4 C 0.2715(10) -0.023(3) 0.7842(6) 0.090(8) Uani 1 1 d . . . . .
H4 H 0.247564 -0.082955 0.797498 0.108 Uiso 1 1 calc R . . . .
C28 C 0.4908(10) 0.461(3) 0.7844(5) 0.105(10) Uani 1 1 d D . . . .
H28 H 0.518630 0.409598 0.797364 0.126 Uiso 1 1 calc R . . . .
C34A C 0.4676(9) 0.496(3) 0.8796(4) 0.067(4) Uani 0.654(12) 1 d D U . A 1
H34A H 0.477785 0.383130 0.879492 0.080 Uiso 0.654(12) 1 calc R . . A 1
H34B H 0.497763 0.550201 0.892384 0.080 Uiso 0.654(12) 1 calc R . . A 1
N2A N 0.4046(9) 0.519(2) 0.8916(3) 0.049(3) Uani 0.654(12) 1 d D U . A 1
H2AA H 0.388251 0.608751 0.884264 0.059 Uiso 0.654(12) 1 calc GR . . A 1
H2AB H 0.406430 0.524787 0.911508 0.059 Uiso 0.654(12) 1 calc GR . . A 1
H2AC H 0.380458 0.436126 0.886298 0.059 Uiso 0.654(12) 1 calc GR . . A 1
C33A C 0.4726(11) 0.560(4) 0.8487(3) 0.080(5) Uani 0.654(12) 1 d D U . A 1
H33A H 0.513634 0.533598 0.840604 0.095 Uiso 0.654(12) 1 calc R . . A 1
H33B H 0.469151 0.675746 0.849314 0.095 Uiso 0.654(12) 1 calc R . . A 1
C32A C 0.4228(10) 0.494(4) 0.8285(3) 0.097(6) Uani 0.654(12) 1 d D U . A 1
H32A H 0.418988 0.380101 0.831581 0.116 Uiso 0.654(12) 1 calc R . . A 1
H32B H 0.382669 0.543301 0.833319 0.116 Uiso 0.654(12) 1 calc R . . A 1
C16B C 0.3456(14) 0.163(3) 0.5481(6) 0.052(4) Uani 0.346(12) 1 d D U . A 2
H16C H 0.383794 0.205744 0.556772 0.062 Uiso 0.346(12) 1 calc R . . A 2
H16D H 0.335556 0.224529 0.530367 0.062 Uiso 0.346(12) 1 calc R . . A 2
C17B C 0.3559(19) -0.007(3) 0.5396(10) 0.055(4) Uani 0.346(12) 1 d D U . A 2
H17C H 0.368098 -0.067813 0.557180 0.065 Uiso 0.346(12) 1 calc R . . A 2
H17D H 0.316941 -0.051936 0.532005 0.065 Uiso 0.346(12) 1 calc R . . A 2
N1B N 0.4044(16) -0.021(5) 0.5169(8) 0.043(4) Uani 0.346(12) 1 d D U . A 2
H1BA H 0.387257 -0.009686 0.498762 0.052 Uiso 0.346(12) 1 calc GR . . A 2
H1BB H 0.422321 -0.117580 0.518165 0.052 Uiso 0.346(12) 1 calc GR . . A 2
H1BC H 0.433355 0.054040 0.519720 0.052 Uiso 0.346(12) 1 calc GR . . A 2
N2B N 0.3136(14) 0.325(4) 0.8733(7) 0.049(3) Uani 0.346(12) 1 d D U . A 2
H2BA H 0.282267 0.371641 0.863355 0.059 Uiso 0.346(12) 1 calc GR . . A 2
H2BB H 0.302103 0.309316 0.892322 0.059 Uiso 0.346(12) 1 calc GR . . A 2
H2BC H 0.322404 0.230842 0.864846 0.059 Uiso 0.346(12) 1 calc GR . . A 2
C34B C 0.3691(19) 0.427(5) 0.8724(6) 0.067(4) Uani 0.346(12) 1 d D U . A 2
H34C H 0.395137 0.406434 0.889820 0.080 Uiso 0.346(12) 1 calc R . . A 2
H34D H 0.356427 0.538218 0.872789 0.080 Uiso 0.346(12) 1 calc R . . A 2
C32B C 0.4307(16) 0.539(4) 0.8296(3) 0.097(6) Uani 0.346(12) 1 d D U . A 2
H32C H 0.402735 0.628196 0.833881 0.116 Uiso 0.346(12) 1 calc R . . A 2
H32D H 0.471255 0.564530 0.838366 0.116 Uiso 0.346(12) 1 calc R . . A 2
C33B C 0.405(2) 0.394(4) 0.8446(7) 0.080(5) Uani 0.346(12) 1 d D U . A 2
H33C H 0.378535 0.337338 0.830572 0.095 Uiso 0.346(12) 1 calc R . . A 2
H33D H 0.440266 0.323540 0.849513 0.095 Uiso 0.346(12) 1 calc R . . A 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
Pb2 I3 3.2050(8) 5_666 ?
Pb2 I3 3.2051(8) . ?
Pb2 I5 3.2247(8) 5_666 ?
Pb2 I5 3.2247(8) . ?
Pb2 I4 3.2101(9) 5_666 ?
Pb2 I4 3.2101(9) . ?
Pb1 I3 3.3358(9) . ?
Pb1 I5 3.2328(10) . ?
Pb1 I4 3.3268(10) 5_666 ?
Pb1 I1 3.1351(10) . ?
Pb1 I1 3.1703(10) 8_665 ?
Pb1 I2 3.1074(11) . ?
S4 C25 1.757(17) . ?
S4 C24 1.73(2) . ?
S3 C31 1.748(18) . ?
S3 C18 1.73(2) . ?
S2 C8 1.720(19) . ?
S2 C7 1.74(2) . ?
S1 C14 1.706(19) . ?
S1 C1 1.78(2) . ?
N1A C17A 1.483(10) . ?
C17A C16A 1.512(10) . ?
C10 C9 1.35(3) . ?
C10 C11 1.38(2) . ?
C10 C15 1.505(9) . ?
C13 C8 1.39(2) . ?
C13 C12 1.41(3) . ?
C13 C14 1.42(3) . ?
C8 C9 1.45(3) . ?
C25 C30 1.42(3) . ?
C25 C26 1.36(3) . ?
C16A C15 1.553(9) . ?
C12 C11 1.35(3) . ?
C15 C16B 1.514(10) . ?
C31 C30 1.43(3) . ?
C31 C24 1.36(2) . ?
C30 C29 1.37(3) . ?
C23 C22 1.37(2) . ?
C23 C18 1.43(3) . ?
C23 C24 1.43(3) . ?
C14 C7 1.37(3) . ?
C22 C21 1.36(3) . ?
C29 C28 1.45(3) . ?
C7 C6 1.45(3) . ?
C6 C5 1.35(3) . ?
C6 C1 1.38(3) . ?
C5 C4 1.36(4) . ?
C18 C19 1.39(3) . ?
C19 C20 1.39(3) . ?
C21 C20 1.37(3) . ?
C1 C2 1.35(3) . ?
C26 C27 1.38(3) . ?
C2 C3 1.40(4) . ?
C3 C4 1.39(4) . ?
C27 C28 1.39(3) . ?
C27 C32A 1.511(9) . ?
C27 C32B 1.513(9) . ?
C34A N2A 1.486(10) . ?
C34A C33A 1.512(10) . ?
C33A C32A 1.528(10) . ?
C16B C17B 1.517(10) . ?
C17B N1B 1.481(10) . ?
N2B C34B 1.487(10) . ?
C34B C33B 1.519(10) . ?
C32B C33B 1.521(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I3 Pb2 I3 180.0 5_666 . ?
I3 Pb2 I5 92.48(2) . 5_666 ?
I3 Pb2 I5 87.52(2) 5_666 5_666 ?
I3 Pb2 I5 87.52(2) . . ?
I3 Pb2 I5 92.48(2) 5_666 . ?
I3 Pb2 I4 94.58(2) 5_666 5_666 ?
I3 Pb2 I4 85.42(2) 5_666 . ?
I3 Pb2 I4 94.58(2) . . ?
I3 Pb2 I4 85.41(2) . 5_666 ?
I5 Pb2 I5 180.00(2) 5_666 . ?
I4 Pb2 I5 85.44(2) . 5_666 ?
I4 Pb2 I5 85.43(2) 5_666 . ?
I4 Pb2 I5 94.57(2) 5_666 5_666 ?
I4 Pb2 I5 94.57(2) . . ?
I4 Pb2 I4 180.0 5_666 . ?
I5 Pb1 I3 85.21(2) . . ?
I5 Pb1 I4 83.42(3) . 5_666 ?
I4 Pb1 I3 81.55(2) 5_666 . ?
I1 Pb1 I3 85.29(3) 8_665 . ?
I1 Pb1 I3 174.31(3) . . ?
I1 Pb1 I5 169.32(3) 8_665 . ?
I1 Pb1 I5 98.40(3) . . ?
I1 Pb1 I4 90.36(3) 8_665 5_666 ?
I1 Pb1 I4 94.45(3) . 5_666 ?
I1 Pb1 I1 90.714(16) . 8_665 ?
I2 Pb1 I3 93.10(3) . . ?
I2 Pb1 I5 95.44(3) . . ?
I2 Pb1 I4 174.60(3) . 5_666 ?
I2 Pb1 I1 89.93(4) . 8_665 ?
I2 Pb1 I1 90.94(4) . . ?
Pb2 I3 Pb1 77.326(18) . . ?
Pb2 I5 Pb1 78.54(2) . . ?
Pb2 I4 Pb1 77.386(19) . 5_666 ?
Pb1 I1 Pb1 143.33(4) . 8_655 ?
C24 S4 C25 91.5(9) . . ?
C18 S3 C31 90.5(9) . . ?
C8 S2 C7 90.2(10) . . ?
C14 S1 C1 90.2(10) . . ?
N1A C17A C16A 111.6(12) . . ?
C9 C10 C11 122.6(17) . . ?
C9 C10 C15 118.6(15) . . ?
C11 C10 C15 118.8(17) . . ?
C8 C13 C12 119(2) . . ?
C8 C13 C14 109.4(17) . . ?
C12 C13 C14 131.6(17) . . ?
C13 C8 S2 114.3(16) . . ?
C13 C8 C9 120.4(17) . . ?
C9 C8 S2 125.3(12) . . ?
C30 C25 S4 110.8(14) . . ?
C26 C25 S4 126.8(16) . . ?
C26 C25 C30 122.2(18) . . ?
C10 C9 C8 117.1(15) . . ?
C17A C16A C15 111.2(11) . . ?
C11 C12 C13 119.6(17) . . ?
C12 C11 C10 121(2) . . ?
C10 C15 C16A 106.8(10) . . ?
C10 C15 C16B 119.9(15) . . ?
C30 C31 S3 133.4(13) . . ?
C24 C31 S3 112.5(14) . . ?
C24 C31 C30 114.2(17) . . ?
C25 C30 C31 111.0(15) . . ?
C29 C30 C25 121(2) . . ?
C29 C30 C31 128(2) . . ?
C22 C23 C18 119.1(17) . . ?
C22 C23 C24 131.5(17) . . ?
C18 C23 C24 109.3(15) . . ?
C13 C14 S1 132.6(15) . . ?
C7 C14 S1 113.1(18) . . ?
C7 C14 C13 114.3(17) . . ?
C21 C22 C23 120(2) . . ?
C30 C29 C28 114(2) . . ?
C14 C7 S2 111.8(18) . . ?
C14 C7 C6 114.5(18) . . ?
C6 C7 S2 133.7(15) . . ?
C5 C6 C7 130(2) . . ?
C5 C6 C1 121(2) . . ?
C1 C6 C7 108.8(19) . . ?
C6 C5 C4 117(2) . . ?
C23 C18 S3 113.1(15) . . ?
C19 C18 S3 125.7(17) . . ?
C19 C18 C23 121.2(18) . . ?
C18 C19 C20 116(2) . . ?
C22 C21 C20 120(2) . . ?
C6 C1 S1 113.4(18) . . ?
C2 C1 S1 123.6(17) . . ?
C2 C1 C6 123(2) . . ?
C31 C24 S4 112.5(15) . . ?
C31 C24 C23 114.7(17) . . ?
C23 C24 S4 132.8(13) . . ?
C25 C26 C27 120(2) . . ?
C1 C2 C3 117(2) . . ?
C21 C20 C19 124(2) . . ?
C4 C3 C2 118(2) . . ?
C26 C27 C28 117.7(15) . . ?
C26 C27 C32A 122(2) . . ?
C26 C27 C32B 120(2) . . ?
C28 C27 C32A 119.7(19) . . ?
C28 C27 C32B 121(2) . . ?
C5 C4 C3 124(3) . . ?
C27 C28 C29 125.2(19) . . ?
N2A C34A C33A 111.2(12) . . ?
C34A C33A C32A 112.2(13) . . ?
C27 C32A C33A 110.7(12) . . ?
C15 C16B C17B 110.8(13) . . ?
N1B C17B C16B 111.3(15) . . ?
N2B C34B C33B 109.6(15) . . ?
C27 C32B C33B 115.1(15) . . ?
C34B C33B C32B 114.1(15) . . ?

# end Validation Reply Form
_olex2_exptl_crystal_mounting_method 'mounted on a LithoLoop'
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.678
_oxdiff_exptl_absorpt_empirical_full_min 0.505
# start Validation Reply Form
_vrf_PLAT924_dvdz011             
;
PROBLEM: The Reported and Calculated Rho(min) Differ by .       3.20 eA-3  
RESPONSE: Because of low crystal diffraction quality, 
Cu-radiation had to be used, consequently leading to 
severe absorption peaks in close viccinity of the heavy atoms 
;
_vrf_PLAT925_dvdz011             
;
PROBLEM: The Reported and Calculated Rho(max) Differ by .       3.21 eA-3  
RESPONSE: Because of low crystal diffraction quality, 
Cu-radiation had to be used, consequently leading to 
severe absorption peaks in close viccinity of the heavy atoms
;
_vrf_PLAT971_dvdz011             
;
PROBLEM: Check Calcd Resid. Dens.  0.73A   From I1              6.20 eA-3  
RESPONSE: Because of low crystal diffraction quality, 
Cu-radiation had to be used, consequently leading to 
severe absorption peaks in close viccinity of the heavy atoms
;
_vrf_PLAT972_dvdz011             
;
PROBLEM: Check Calcd Resid. Dens.  0.78A   From I1             -5.67 eA-3  
RESPONSE: Because of low crystal diffraction quality, 
Cu-radiation had to be used, consequently leading to 
severe absorption peaks in close viccinity of the heavy atoms
;

