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

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

data_1-p63m
_database_code_depnum_ccdc_archive 'CCDC 1436334'
loop_
_audit_author_name
_audit_author_address
'Andreas Eichhoefer'
;KIT Campus North, Institute of Nanotechnology
Germany
;
_audit_update_record             
;
2023-07-28 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT201_1-p63m              
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          1 Report
RESPONSE: The C atom of a CF3SO3- anion could not be adequately refined with anisotropic displacement parameters
;
_vrf_PLAT241_1-p63m              
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         O3 Check
RESPONSE: Two of the CF3SO3- anions display unusually large displacement parameters most probably due to strong disorder
;
# Added during the CSD deposition process: Friday 28 July 2023 02:01 PM
# end Validation Reply Form

_audit_creation_date             2023-07-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C120 H126 N48 Pb6, 12(C F3 O3 S), 3(C2 H3 N)'
_chemical_formula_sum            'C138 H135 F36 N51 O36 Pb6 S12'
_chemical_formula_weight         5395.82
_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 0.0137 0.0067 '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'
F F 0.0583 0.0400 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.4950 6.8412 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.2925 0.4295 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   21.0549(6)
_cell_length_b                   21.0549(6)
_cell_length_c                   31.7103(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     12174.1(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    40636
_cell_measurement_temperature    150
_cell_measurement_theta_max      63.98
_cell_measurement_theta_min      2.43
_shelx_estimated_absorpt_T_max   0.564
_shelx_estimated_absorpt_T_min   0.444
_exptl_absorpt_coefficient_mu    6.457
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5232
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0964
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51469
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         64.052
_diffrn_reflns_theta_min         2.108
_diffrn_ambient_temperature      150.00
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            Dectris
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5261
_reflns_number_total             9933
_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       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.144.0 (STOE, 2018)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.0.0 (STOE, 2018)
X-Area LANA 1.72.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         2.250
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         9933
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0696
_refine_ls_restrained_S_all      0.957
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1361P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1968
_refine_ls_wR_factor_ref         0.2213
_refine_special_details          'Solvent Masking'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C24-F6 = C24-F7
 1.33 with sigma of 0.02
 C22-S2
 1.85 with sigma of 0.02
 C24-S4
 1.85 with sigma of 0.02
 C22-F2
 1.33 with sigma of 0.02
 S3-C23
 1.82 with sigma of 0.02
 C23-F3 = C23-F4 = C23-F5
 1.33 with sigma of 0.02
 C22-O2
 2.578 with sigma of 0.04
 S3-O3 \\sim S3-O4 \\sim S3-O5
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F7)
Uanis(F3) = Uanis(F4) = Uanis(F5)
Uanis(O3) = Uanis(O4) = Uanis(O5)
4. Others
 Fixed Sof: F2(0.5) O2(0.5) C22(0.16666) N9(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 H25C(0.5) C26(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C10(H10), C16(H16), C17(H17), C19(H19),
 C20(H20)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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 0.54780(2) 0.82967(2) 0.56142(2) 0.06366(16) Uani 1 1 d . . . . .
S3 S 0.5829(3) 0.8706(2) 0.45238(11) 0.156(2) Uani 1 1 d D . . . .
F3 F 0.4491(10) 0.8163(9) 0.4146(4) 0.247(4) Uani 1 1 d D . . . .
F4 F 0.4954(10) 0.7522(9) 0.4130(5) 0.247(4) Uani 1 1 d D . . . .
F5 F 0.4438(10) 0.7554(9) 0.4711(5) 0.247(4) Uani 1 1 d D . . . .
O3 O 0.6023(8) 0.8306(6) 0.4802(3) 0.161(3) Uani 1 1 d D . . . .
O4 O 0.6136(8) 0.8961(6) 0.4162(3) 0.161(3) Uani 1 1 d D . . . .
O5 O 0.5595(8) 0.9168(6) 0.4749(3) 0.161(3) Uani 1 1 d D . . . .
N1 N 0.6808(5) 0.9349(5) 0.5608(2) 0.081(2) Uani 1 1 d . . . . .
N2 N 0.6537(4) 0.8013(4) 0.5793(3) 0.072(2) Uani 1 1 d . . . . .
N3 N 0.6377(3) 0.7327(4) 0.5956(2) 0.0641(17) Uani 1 1 d . . . . .
N4 N 0.5252(4) 0.6879(4) 0.5600(2) 0.0656(18) Uani 1 1 d . . . . .
N5 N 0.4366(4) 0.5612(4) 0.5604(2) 0.0685(19) Uani 1 1 d . . . . .
N6 N 0.4614(4) 0.4782(4) 0.5917(3) 0.0680(18) Uani 1 1 d . . . . .
N7 N 0.3911(4) 0.4246(4) 0.5790(2) 0.0654(17) Uani 1 1 d . . . . .
N8 N 0.5681(4) 0.8384(3) 0.6389(2) 0.0590(17) Uani 1 1 d . . . . .
C1 C 0.6925(6) 1.0019(5) 0.5526(3) 0.081(3) Uani 1 1 d . . . . .
C2 C 0.7641(7) 1.0605(6) 0.5428(4) 0.101(4) Uani 1 1 d . . . . .
H2 H 0.7724 1.1086 0.5380 0.122 Uiso 1 1 calc R U . . .
C3 C 0.8206(7) 1.0463(6) 0.5405(5) 0.128(6) Uani 1 1 d . . . . .
H3 H 0.8687 1.0844 0.5338 0.154 Uiso 1 1 calc R U . . .
C4 C 0.8071(6) 0.9744(8) 0.5482(5) 0.125(5) Uani 1 1 d . . . . .
H4 H 0.8456 0.9634 0.5457 0.151 Uiso 1 1 calc R U . . .
C5 C 0.7372(6) 0.9202(6) 0.5594(3) 0.090(4) Uani 1 1 d . . . . .
C6 C 0.7202(6) 0.8463(6) 0.5700(4) 0.087(3) Uani 1 1 d . . . . .
C7 C 0.5685(4) 0.6750(4) 0.5846(3) 0.062(2) Uani 1 1 d . . . . .
C8 C 0.5487(5) 0.6059(5) 0.5993(3) 0.077(3) Uani 1 1 d . . . . .
H8 H 0.5784 0.5976 0.6186 0.092 Uiso 1 1 calc R U . . .
C9 C 0.4804(4) 0.5471(5) 0.5836(3) 0.064(2) Uani 1 1 d . . . . .
C10 C 0.4613(5) 0.6308(5) 0.5501(3) 0.070(2) Uani 1 1 d . . . . .
H10 H 0.4292 0.6406 0.5338 0.084 Uiso 1 1 calc R U . . .
C11 C 0.3853(7) 0.3694(6) 0.5603(3) 0.083(3) Uani 1 1 d . . . . .
C12 C 0.4503(7) 0.3623(8) 0.5459(4) 0.112(4) Uani 1 1 d . . . . .
H12A H 0.4617 0.3360 0.5674 0.168 Uiso 1 1 calc R U . . .
H12B H 0.4930 0.4112 0.5417 0.168 Uiso 1 1 calc R U . . .
H12C H 0.4382 0.3350 0.5193 0.168 Uiso 1 1 calc R U . . .
C13 C 0.7816(6) 0.8297(7) 0.5713(5) 0.117(5) Uani 1 1 d . . . . .
H13A H 0.8084 0.8443 0.5445 0.176 Uiso 1 1 calc R U . . .
H13B H 0.7616 0.7770 0.5757 0.176 Uiso 1 1 calc R U . . .
H13C H 0.8151 0.8570 0.5944 0.176 Uiso 1 1 calc R U . . .
C14 C 0.6755(5) 0.7308(5) 0.6327(4) 0.078(3) Uani 1 1 d . . . . .
H14A H 0.7101 0.7144 0.6252 0.117 Uiso 1 1 calc R U . . .
H14B H 0.6399 0.6967 0.6532 0.117 Uiso 1 1 calc R U . . .
H14C H 0.7022 0.7800 0.6451 0.117 Uiso 1 1 calc R U . . .
C15 C 0.4941(6) 0.4585(5) 0.6251(4) 0.091(3) Uani 1 1 d . . . . .
H15A H 0.4618 0.4070 0.6326 0.137 Uiso 1 1 calc R U . . .
H15B H 0.5012 0.4895 0.6497 0.137 Uiso 1 1 calc R U . . .
H15C H 0.5416 0.4657 0.6157 0.137 Uiso 1 1 calc R U . . .
C16 C 0.6098(5) 0.9000(5) 0.6597(4) 0.085(3) Uani 1 1 d . . . . .
H16 H 0.6367 0.9442 0.6442 0.103 Uiso 1 1 calc R U . . .
C17 C 0.6157(5) 0.9026(5) 0.7036(3) 0.069(2) Uani 1 1 d . . . . .
H17 H 0.6438 0.9482 0.7176 0.083 Uiso 1 1 calc R U . . .
C18 C 0.5810(4) 0.8395(4) 0.7259(3) 0.0524(17) Uani 1 1 d . . . . .
C19 C 0.5419(5) 0.7739(5) 0.7041(3) 0.068(2) Uani 1 1 d . . . . .
H19 H 0.5185 0.7284 0.7186 0.082 Uiso 1 1 calc R U . . .
C20 C 0.5379(5) 0.7767(5) 0.6615(3) 0.066(2) Uani 1 1 d . . . . .
H20 H 0.5117 0.7315 0.6468 0.079 Uiso 1 1 calc R U . . .
C23 C 0.4895(10) 0.7982(11) 0.4383(7) 0.230(13) Uiso 1 1 d D . . . .
S1 S 0.3333 0.6667 0.60821(11) 0.0656(9) Uani 1 3 d S T P . .
F1 F 0.2657(3) 0.6253(3) 0.68118(16) 0.0775(13) Uani 1 1 d . . . . .
O1 O 0.4066(3) 0.7210(3) 0.59749(18) 0.0763(16) Uani 1 1 d . . . . .
C21 C 0.3333 0.6667 0.6656(5) 0.064(3) Uani 1 3 d S T P . .
S2 S 1.0000 1.0000 0.5000 0.0556(12) Uani 1 6 d DS T P . .
F2 F 0.9523(5) 0.9330(5) 0.5664(3) 0.074(3) Uani 0.5 1 d D . P A 1
O2 O 0.9429(5) 0.9257(4) 0.5142(4) 0.056(3) Uani 0.5 1 d D . P B 2
C22 C 1.0000 1.0000 0.5589(5) 0.065(7) Uani 0.5 3 d DS T P A .
S4 S 0.0169(2) 0.4156(3) 0.7500 0.1082(14) Uani 1 2 d DS T P . .
F6 F 0.1065(8) 0.5354(8) 0.7139(5) 0.278(7) Uani 1 1 d D . . . .
F7 F 0.0237(11) 0.5417(11) 0.7500 0.278(7) Uani 1 2 d DS T P . .
O6 O 0.0709(8) 0.3965(9) 0.7500 0.178(8) Uani 1 2 d S T P . .
O7 O -0.0268(7) 0.3963(7) 0.7108(4) 0.184(5) Uani 1 1 d . . . . .
C24 C 0.0698(12) 0.5164(9) 0.7500 0.172(10) Uiso 1 2 d DS . P . .
N9 N 0.3665(9) 0.2703(10) 0.6498(6) 0.091(5) Uiso 0.5 1 d . . P . .
C25 C 0.4034(15) 0.1814(14) 0.6845(9) 0.115(8) Uiso 0.5 1 d . . P . .
H25A H 0.4459 0.1848 0.6698 0.172 Uiso 0.5 1 calc R U P . .
H25B H 0.3625 0.1308 0.6831 0.172 Uiso 0.5 1 calc R U P . .
H25C H 0.4161 0.1958 0.7140 0.172 Uiso 0.5 1 calc R U P . .
C26 C 0.3818(13) 0.2305(13) 0.6642(9) 0.100(7) Uiso 0.5 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N1 2.559(8) . ?
Pb1 N2 2.643(8) . ?
Pb1 N4 2.779(8) . ?
Pb1 N7 2.698(7) 2_665 ?
Pb1 N8 2.484(7) . ?
S3 O3 1.415(11) . ?
S3 O4 1.294(11) . ?
S3 O5 1.476(9) . ?
S3 C23 1.843(17) . ?
F3 C23 1.326(17) . ?
F4 C23 1.311(17) . ?
F5 C23 1.397(16) . ?
N1 C1 1.332(13) . ?
N1 C5 1.368(13) . ?
N2 N3 1.406(10) . ?
N2 C6 1.272(12) . ?
N3 C7 1.396(11) . ?
N3 C14 1.431(13) . ?
N4 C7 1.328(11) . ?
N4 C10 1.318(12) . ?
N5 C9 1.324(11) . ?
N5 C10 1.327(12) . ?
N6 N7 1.399(10) . ?
N6 C9 1.324(11) . ?
N6 C15 1.431(13) . ?
N7 Pb1 2.698(7) 3_565 ?
N7 C11 1.256(12) . ?
N8 C16 1.323(12) . ?
N8 C20 1.335(10) . ?
C1 C2 1.424(14) . ?
C1 C11 1.492(16) 2_665 ?
C2 H2 0.9500 . ?
C2 C3 1.367(17) . ?
C3 H3 0.9500 . ?
C3 C4 1.414(18) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(14) . ?
C5 C6 1.451(14) . ?
C6 C13 1.500(15) . ?
C7 C8 1.379(12) . ?
C8 H8 0.9500 . ?
C8 C9 1.439(13) . ?
C10 H10 0.9500 . ?
C11 C1 1.492(16) 3_565 ?
C11 C12 1.520(14) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 0.9500 . ?
C16 C17 1.396(14) . ?
C17 H17 0.9500 . ?
C17 C18 1.352(11) . ?
C18 C18 1.527(16) 10_557 ?
C18 C19 1.388(11) . ?
C19 H19 0.9500 . ?
C19 C20 1.355(12) . ?
C20 H20 0.9500 . ?
S1 O1 1.428(6) 2_665 ?
S1 O1 1.428(6) 3_565 ?
S1 O1 1.428(6) . ?
S1 C21 1.821(15) . ?
F1 C21 1.338(7) . ?
C21 F1 1.338(7) 2_665 ?
C21 F1 1.338(7) 3_565 ?
S2 O2 1.489(8) 7_776 ?
S2 O2 1.489(8) 8_566 ?
S2 O2 1.489(8) 9_656 ?
S2 O2 1.489(8) . ?
S2 O2 1.489(8) 3_675 ?
S2 O2 1.489(8) 2_765 ?
S2 C22 1.869(16) . ?
S2 C22 1.869(16) 7_776 ?
F2 C22 1.280(9) . ?
O2 O2 1.682(15) 8_566 ?
O2 O2 1.682(15) 9_656 ?
C22 F2 1.280(9) 2_765 ?
C22 F2 1.280(9) 3_675 ?
S4 O6 1.383(12) . ?
S4 O7 1.478(11) . ?
S4 O7 1.478(11) 10_557 ?
S4 C24 1.839(17) . ?
F6 C24 1.327(12) . ?
F7 C24 1.319(17) . ?
C24 F6 1.327(12) 10_557 ?
N9 C26 1.13(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25 C26 1.47(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pb1 N2 61.0(2) . . ?
N1 Pb1 N4 117.1(2) . . ?
N1 Pb1 N7 61.2(2) . 2_665 ?
N2 Pb1 N4 58.1(2) . . ?
N2 Pb1 N7 116.2(2) . 2_665 ?
N7 Pb1 N4 168.7(2) 2_665 . ?
N8 Pb1 N1 82.5(2) . . ?
N8 Pb1 N2 70.8(2) . . ?
N8 Pb1 N4 91.5(2) . . ?
N8 Pb1 N7 77.2(2) . 2_665 ?
O3 S3 O5 112.5(6) . . ?
O3 S3 C23 99.5(9) . . ?
O4 S3 O3 124.5(8) . . ?
O4 S3 O5 114.7(6) . . ?
O4 S3 C23 103.5(10) . . ?
O5 S3 C23 95.3(9) . . ?
C1 N1 Pb1 117.4(7) . . ?
C1 N1 C5 120.8(8) . . ?
C5 N1 Pb1 120.1(7) . . ?
N3 N2 Pb1 120.9(5) . . ?
C6 N2 Pb1 121.3(7) . . ?
C6 N2 N3 117.4(8) . . ?
N2 N3 C14 118.7(7) . . ?
C7 N3 N2 114.3(7) . . ?
C7 N3 C14 122.2(7) . . ?
C7 N4 Pb1 116.3(6) . . ?
C10 N4 Pb1 122.1(6) . . ?
C10 N4 C7 116.6(8) . . ?
C9 N5 C10 116.9(8) . . ?
N7 N6 C15 116.6(7) . . ?
C9 N6 N7 116.5(7) . . ?
C9 N6 C15 122.4(8) . . ?
N6 N7 Pb1 123.9(5) . 3_565 ?
C11 N7 Pb1 113.7(7) . 3_565 ?
C11 N7 N6 117.2(8) . . ?
C16 N8 Pb1 124.9(6) . . ?
C16 N8 C20 116.4(8) . . ?
C20 N8 Pb1 118.7(5) . . ?
N1 C1 C2 120.9(10) . . ?
N1 C1 C11 117.4(8) . 2_665 ?
C2 C1 C11 121.0(9) . 2_665 ?
C1 C2 H2 120.5 . . ?
C3 C2 C1 118.9(10) . . ?
C3 C2 H2 120.5 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.6(10) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.2(11) . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 120.5(10) . . ?
N1 C5 C6 117.3(8) . . ?
C4 C5 C6 122.2(10) . . ?
N2 C6 C5 116.3(9) . . ?
N2 C6 C13 125.1(9) . . ?
C5 C6 C13 118.5(9) . . ?
N4 C7 N3 119.6(7) . . ?
N4 C7 C8 122.5(8) . . ?
C8 C7 N3 117.9(8) . . ?
C7 C8 H8 122.1 . . ?
C7 C8 C9 115.8(9) . . ?
C9 C8 H8 122.1 . . ?
N5 C9 N6 119.5(8) . . ?
N5 C9 C8 120.6(8) . . ?
N6 C9 C8 119.9(8) . . ?
N4 C10 N5 127.2(9) . . ?
N4 C10 H10 116.4 . . ?
N5 C10 H10 116.4 . . ?
N7 C11 C1 116.8(9) . 3_565 ?
N7 C11 C12 123.9(11) . . ?
C1 C11 C12 119.3(9) 3_565 . ?
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 . . ?
C6 C13 H13A 109.5 . . ?
C6 C13 H13B 109.5 . . ?
C6 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C14 H14A 109.5 . . ?
N3 C14 H14B 109.5 . . ?
N3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N8 C16 H16 118.7 . . ?
N8 C16 C17 122.6(9) . . ?
C17 C16 H16 118.7 . . ?
C16 C17 H17 120.3 . . ?
C18 C17 C16 119.3(8) . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C18 121.6(5) . 10_557 ?
C17 C18 C19 118.4(8) . . ?
C19 C18 C18 119.9(5) . 10_557 ?
C18 C19 H19 120.9 . . ?
C20 C19 C18 118.2(8) . . ?
C20 C19 H19 120.9 . . ?
N8 C20 C19 124.6(8) . . ?
N8 C20 H20 117.7 . . ?
C19 C20 H20 117.7 . . ?
F3 C23 S3 118.1(16) . . ?
F3 C23 F5 106.0(16) . . ?
F4 C23 S3 107.6(14) . . ?
F4 C23 F3 100.3(16) . . ?
F4 C23 F5 105.5(18) . . ?
F5 C23 S3 117.3(14) . . ?
O1 S1 O1 114.5(2) 2_665 3_565 ?
O1 S1 O1 114.5(2) . 3_565 ?
O1 S1 O1 114.5(2) 2_665 . ?
O1 S1 C21 103.8(3) 2_665 . ?
O1 S1 C21 103.8(3) . . ?
O1 S1 C21 103.8(3) 3_565 . ?
F1 C21 S1 111.6(6) 3_565 . ?
F1 C21 S1 111.6(6) 2_665 . ?
F1 C21 S1 111.6(6) . . ?
F1 C21 F1 107.2(7) 3_565 2_665 ?
F1 C21 F1 107.2(7) 3_565 . ?
F1 C21 F1 107.2(7) . 2_665 ?
O2 S2 O2 180.0(2) 8_566 2_765 ?
O2 S2 O2 111.2(4) 8_566 9_656 ?
O2 S2 O2 180.0(9) 7_776 . ?
O2 S2 O2 111.2(4) 8_566 7_776 ?
O2 S2 O2 68.8(4) 8_566 3_675 ?
O2 S2 O2 68.8(4) 8_566 . ?
O2 S2 O2 68.8(4) 7_776 3_675 ?
O2 S2 O2 68.8(4) 2_765 9_656 ?
O2 S2 O2 180.0(9) 9_656 3_675 ?
O2 S2 O2 68.8(4) 9_656 . ?
O2 S2 O2 111.2(4) 2_765 3_675 ?
O2 S2 O2 68.8(4) 2_765 7_776 ?
O2 S2 O2 111.2(4) 3_675 . ?
O2 S2 O2 111.2(4) 7_776 9_656 ?
O2 S2 O2 111.2(4) 2_765 . ?
O2 S2 C22 107.7(4) 8_566 . ?
O2 S2 C22 107.7(4) 3_675 7_776 ?
O2 S2 C22 107.7(4) 2_765 7_776 ?
O2 S2 C22 72.3(4) 9_656 7_776 ?
O2 S2 C22 72.3(4) 7_776 7_776 ?
O2 S2 C22 72.3(4) 8_566 7_776 ?
O2 S2 C22 107.7(4) 9_656 . ?
O2 S2 C22 72.3(4) 2_765 . ?
O2 S2 C22 72.3(4) 3_675 . ?
O2 S2 C22 107.7(4) . 7_776 ?
O2 S2 C22 107.7(4) 7_776 . ?
O2 S2 C22 72.3(4) . . ?
C22 S2 C22 180.0 . 7_776 ?
S2 O2 O2 55.6(2) . 8_566 ?
S2 O2 O2 55.6(2) . 9_656 ?
O2 O2 O2 93.8(9) 8_566 9_656 ?
F2 C22 S2 100.7(9) . . ?
F2 C22 S2 100.7(9) 2_765 . ?
F2 C22 S2 100.7(9) 3_675 . ?
F2 C22 F2 116.6(5) 2_765 . ?
F2 C22 F2 116.6(5) 2_765 3_675 ?
F2 C22 F2 116.6(5) . 3_675 ?
O6 S4 O7 114.2(7) . . ?
O6 S4 O7 114.2(7) . 10_557 ?
O6 S4 C24 102.9(10) . . ?
O7 S4 O7 114.7(12) . 10_557 ?
O7 S4 C24 104.6(7) . . ?
O7 S4 C24 104.6(7) 10_557 . ?
F6 C24 S4 105.9(11) . . ?
F6 C24 S4 105.9(11) 10_557 . ?
F6 C24 F6 119(3) 10_557 . ?
F7 C24 S4 108.8(16) . . ?
F7 C24 F6 108.2(12) . 10_557 ?
F7 C24 F6 108.2(12) . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
N9 C26 C25 177(3) . . ?

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 N1 C1 C2 -166.6(9) . . . . ?
Pb1 N1 C1 C11 22.5(12) . . . 2_665 ?
Pb1 N1 C5 C4 163.2(10) . . . . ?
Pb1 N1 C5 C6 -16.8(13) . . . . ?
Pb1 N2 N3 C7 26.5(9) . . . . ?
Pb1 N2 N3 C14 -129.6(7) . . . . ?
Pb1 N2 C6 C5 15.1(14) . . . . ?
Pb1 N2 C6 C13 -167.8(10) . . . . ?
Pb1 N4 C7 N3 -25.8(9) . . . . ?
Pb1 N4 C7 C8 155.7(7) . . . . ?
Pb1 N4 C10 N5 -157.5(7) . . . . ?
Pb1 N7 C11 C1 -33.2(12) 3_565 . . 3_565 ?
Pb1 N7 C11 C12 147.6(10) 3_565 . . . ?
Pb1 N8 C16 C17 175.8(7) . . . . ?
Pb1 N8 C20 C19 -176.8(7) . . . . ?
O3 S3 C23 F3 174.4(16) . . . . ?
O3 S3 C23 F4 -73.2(16) . . . . ?
O3 S3 C23 F5 45.5(16) . . . . ?
O4 S3 C23 F3 -56.5(18) . . . . ?
O4 S3 C23 F4 55.9(17) . . . . ?
O4 S3 C23 F5 174.6(14) . . . . ?
O5 S3 C23 F3 60.5(18) . . . . ?
O5 S3 C23 F4 172.9(15) . . . . ?
O5 S3 C23 F5 -68.4(16) . . . . ?
N1 C1 C2 C3 2(2) . . . . ?
N1 C5 C6 N2 0.9(16) . . . . ?
N1 C5 C6 C13 -176.4(11) . . . . ?
N2 N3 C7 N4 1.2(11) . . . . ?
N2 N3 C7 C8 179.8(8) . . . . ?
N3 N2 C6 C5 -170.9(9) . . . . ?
N3 N2 C6 C13 6.1(18) . . . . ?
N3 C7 C8 C9 -173.8(8) . . . . ?
N4 C7 C8 C9 4.7(13) . . . . ?
N6 N7 C11 C1 171.1(9) . . . 3_565 ?
N6 N7 C11 C12 -8.0(16) . . . . ?
N7 N6 C9 N5 -7.5(12) . . . . ?
N7 N6 C9 C8 173.8(8) . . . . ?
N8 C16 C17 C18 3.7(16) . . . . ?
C1 N1 C5 C4 -1.7(17) . . . . ?
C1 N1 C5 C6 178.2(10) . . . . ?
C1 C2 C3 C4 -1(2) . . . . ?
C2 C3 C4 C5 -2(3) . . . . ?
C3 C4 C5 N1 3(2) . . . . ?
C3 C4 C5 C6 -176.5(14) . . . . ?
C4 C5 C6 N2 -179.1(13) . . . . ?
C4 C5 C6 C13 3.6(19) . . . . ?
C5 N1 C1 C2 -1.2(16) . . . . ?
C5 N1 C1 C11 -172.2(10) . . . 2_665 ?
C6 N2 N3 C7 -147.5(10) . . . . ?
C6 N2 N3 C14 56.5(12) . . . . ?
C7 N4 C10 N5 -3.4(13) . . . . ?
C7 C8 C9 N5 -7.2(13) . . . . ?
C7 C8 C9 N6 171.5(8) . . . . ?
C9 N5 C10 N4 1.0(13) . . . . ?
C9 N6 N7 Pb1 -18.7(10) . . . 3_565 ?
C9 N6 N7 C11 134.2(9) . . . . ?
C10 N4 C7 N3 178.6(7) . . . . ?
C10 N4 C7 C8 0.2(12) . . . . ?
C10 N5 C9 N6 -174.2(8) . . . . ?
C10 N5 C9 C8 4.5(12) . . . . ?
C11 C1 C2 C3 173.0(13) 2_665 . . . ?
C14 N3 C7 N4 156.3(8) . . . . ?
C14 N3 C7 C8 -25.1(12) . . . . ?
C15 N6 N7 Pb1 137.9(7) . . . 3_565 ?
C15 N6 N7 C11 -69.2(12) . . . . ?
C15 N6 C9 N5 -162.6(9) . . . . ?
C15 N6 C9 C8 18.7(13) . . . . ?
C16 N8 C20 C19 6.0(13) . . . . ?
C16 C17 C18 C18 -175.5(7) . . . 10_557 ?
C16 C17 C18 C19 1.4(13) . . . . ?
C17 C18 C19 C20 -2.6(12) . . . . ?
C18 C18 C19 C20 174.4(6) 10_557 . . . ?
C18 C19 C20 N8 -1.1(14) . . . . ?
C20 N8 C16 C17 -7.2(14) . . . . ?
O1 S1 C21 F1 51.9(4) 3_565 . . 2_665 ?
O1 S1 C21 F1 171.9(4) 3_565 . . 3_565 ?
O1 S1 C21 F1 -68.1(4) . . . 2_665 ?
O1 S1 C21 F1 -68.1(4) 2_665 . . 3_565 ?
O1 S1 C21 F1 171.9(4) 2_665 . . 2_665 ?
O1 S1 C21 F1 51.9(4) . . . 3_565 ?
O1 S1 C21 F1 51.8(4) 2_665 . . . ?
O1 S1 C21 F1 171.8(4) . . . . ?
O1 S1 C21 F1 -68.2(4) 3_565 . . . ?
O2 S2 O2 O2 -124.5(11) 9_656 . . 8_566 ?
O2 S2 O2 O2 124.5(11) 8_566 . . 9_656 ?
O2 S2 O2 O2 55.5(11) 3_675 . . 8_566 ?
O2 S2 O2 O2 180.000(1) 2_765 . . 8_566 ?
O2 S2 O2 O2 -55.5(11) 2_765 . . 9_656 ?
O2 S2 O2 O2 180.000(1) 3_675 . . 9_656 ?
O2 S2 C22 F2 -116.6(6) 3_675 . . 2_765 ?
O2 S2 C22 F2 -176.6(6) 7_776 . . . ?
O2 S2 C22 F2 -116.6(6) 2_765 . . . ?
O2 S2 C22 F2 123.4(5) . . . 2_765 ?
O2 S2 C22 F2 3.4(5) 2_765 . . 2_765 ?
O2 S2 C22 F2 63.4(6) 8_566 . . . ?
O2 S2 C22 F2 123.4(6) 3_675 . . . ?
O2 S2 C22 F2 -176.6(5) 8_566 . . 2_765 ?
O2 S2 C22 F2 -56.6(6) 8_566 . . 3_675 ?
O2 S2 C22 F2 123.4(6) 2_765 . . 3_675 ?
O2 S2 C22 F2 63.4(6) 7_776 . . 3_675 ?
O2 S2 C22 F2 -56.6(5) 7_776 . . 2_765 ?
O2 S2 C22 F2 3.4(6) 3_675 . . 3_675 ?
O2 S2 C22 F2 3.4(6) . . . . ?
O2 S2 C22 F2 -56.6(6) 9_656 . . . ?
O2 S2 C22 F2 63.4(6) 9_656 . . 2_765 ?
O2 S2 C22 F2 -176.6(6) 9_656 . . 3_675 ?
O2 S2 C22 F2 -116.6(6) . . . 3_675 ?
C22 S2 O2 O2 62.3(6) 7_776 . . 9_656 ?
C22 S2 O2 O2 -62.3(6) 7_776 . . 8_566 ?
C22 S2 O2 O2 -117.7(6) . . . 9_656 ?
C22 S2 O2 O2 117.7(6) . . . 8_566 ?
O6 S4 C24 F6 63.9(14) . . . . ?
O6 S4 C24 F6 -63.9(14) . . . 10_557 ?
O6 S4 C24 F7 180.0 . . . . ?
O7 S4 C24 F6 55.7(17) 10_557 . . 10_557 ?
O7 S4 C24 F6 176.6(15) . . . 10_557 ?
O7 S4 C24 F6 -176.6(15) 10_557 . . . ?
O7 S4 C24 F6 -55.7(17) . . . . ?
O7 S4 C24 F7 60.4(6) . . . . ?
O7 S4 C24 F7 -60.4(6) 10_557 . . . ?

_smtbx_masks_special_details     ?
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 -0.652 -0.847 0.250 1528.7 225.1 ?
2 -0.292 -0.742 0.750 1528.7 222.5 ?

_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).
# 
# 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-r-3
_database_code_depnum_ccdc_archive 'CCDC 2285239'
loop_
_audit_author_name
_audit_author_address
'Andreas Eichhoefer'
;KIT Campus North, Institute of Nanotechnology
Germany
;
_audit_update_record             
;
2023-07-28 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT201_3-r-3               
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          2 Report
RESPONSE: Part of the atoms of the CF3SO3- anions display very large displacement parameters and could not be refined with anisotropic ones
;
_vrf_PLAT230_3-r-3               
;
PROBLEM: Hirshfeld Test Diff for    S3       --O3       .        9.3 s.u.
RESPONSE: Part of the atoms of the CF3SO3- anions display very large displacement parameters most probably due to severe disorder
;
_vrf_PLAT230_3-r-3_2             
;
PROBLEM: Hirshfeld Test Diff for    S3       --O4       .       13.7 s.u.
RESPONSE: Part of the atoms of the CF3SO3- anions display very large displacement parameters most probably due to severe disorder
;
_vrf_PLAT230_3-r-3_3             
;
PROBLEM: Hirshfeld Test Diff for    S3       --C26      .        7.1 s.u.
RESPONSE: Part of the atoms of the CF3SO3- anions display very large displacement parameters most probably due to severe disorder
;
# Added during the CSD deposition process: Friday 28 July 2023 03:10 PM
# end Validation Reply Form

_audit_creation_date             2023-07-28
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C138 H138 N48 Pb6, 9(C F3 O3 S), 3(C2 H3 N)'
_chemical_formula_sum            'C153 H147 F27 N51 O27 Pb6 S9'
_chemical_formula_weight         5176.89
_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'
F F 0.0171 0.0103 '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      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                   21.0331(2)
_cell_length_b                   21.0331(2)
_cell_length_c                   58.2510(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     22317.2(6)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    70615
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      1.32
_shelx_estimated_absorpt_T_max   0.570
_shelx_estimated_absorpt_T_min   0.474
_exptl_absorpt_coefficient_mu    3.513
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.4
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7551
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0939
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       82
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            107507
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.501
_diffrn_reflns_theta_min         1.319
_diffrn_ambient_temperature      150.0(2)
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            'EIGER 2R 1M CDTE'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8067
_reflns_number_total             14376
_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       
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)
;
_computing_data_reduction        
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_refine_diff_density_max         1.305
_refine_diff_density_min         -1.543
_refine_diff_density_rms         0.119
_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     399
_refine_ls_number_reflns         14376
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0515
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0931P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1623
_refine_special_details          'Use of Solvent Masking'
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C21-C22 = C21-C23 = C21-C22A = C21-C23A
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O4) = Uanis(O5)
Uanis(F3) = Uanis(F4) = Uanis(F5)
4. Others
 Fixed Sof: C22(0.7) H22(0.7) C23(0.7) H23(0.7) C22A(0.3) H22A(0.3) C23A(0.3)
 H23A(0.3) N8(0.5) C00D(0.5) H00A(0.5) H00B(0.5) H00C(0.5) C29(0.5) O2(0.5)
 C24(0.16666) F2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C6(H6), C7(H7), C11(H11), C16(H16), C17(H17), C19(H19),
 C20(H20), C22(H22), C23(H23), C22A(H22A), C23A(H23A)
5.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C00D(H00A,H00B,H00C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.71357(2) 0.54495(2) 0.53420(2) 0.04933(9) Uani 1 1 d . . . . .
S3 S 0.70735(12) 0.57792(16) 0.47481(3) 0.1047(8) Uani 1 1 d . . . . .
F3 F 0.6974(5) 0.4454(6) 0.48644(16) 0.234(3) Uani 1 1 d . . . . .
F4 F 0.7564(5) 0.5045(6) 0.45322(14) 0.234(3) Uani 1 1 d . . . . .
F5 F 0.6404(5) 0.4473(6) 0.45425(13) 0.234(3) Uani 1 1 d . . . . .
O3 O 0.7668(3) 0.6000(4) 0.48974(10) 0.1188(12) Uani 1 1 d . . . . .
O4 O 0.7115(3) 0.6054(4) 0.45463(10) 0.1188(12) Uani 1 1 d . . . . .
O5 O 0.6373(3) 0.5515(4) 0.48548(10) 0.1188(12) Uani 1 1 d . . . . .
N1 N 0.8332(2) 0.5270(3) 0.53333(7) 0.0531(11) Uani 1 1 d . . . . .
N2 N 0.9020(3) 0.6411(3) 0.55158(8) 0.0623(12) Uani 1 1 d . . . . .
N3 N 0.8482(3) 0.6547(3) 0.54285(8) 0.0627(12) Uani 1 1 d . . . . .
N4 N 0.7385(3) 0.6779(3) 0.53289(8) 0.0652(13) Uani 1 1 d . . . . .
N5 N 0.6045(3) 0.5726(3) 0.54345(8) 0.0615(12) Uani 1 1 d . . . . .
N6 N 0.5323(3) 0.5176(3) 0.54960(10) 0.0710(14) Uani 1 1 d . . . . .
N7 N 0.5604(2) 0.4349(2) 0.53359(7) 0.0503(10) Uani 1 1 d . . . . .
N9 N 0.7287(2) 0.5669(3) 0.57658(7) 0.0545(11) Uani 1 1 d . . . . .
C1 C 0.9427(3) 0.5533(3) 0.55319(10) 0.0646(15) Uani 1 1 d . . . . .
H1 H 0.9828 0.5845 0.5628 0.077 Uiso 1 1 calc R U . . .
C2 C 0.8924(3) 0.5727(3) 0.54610(10) 0.0595(14) Uani 1 1 d . . . . .
C3 C 0.8688(4) 0.7219(3) 0.53783(10) 0.0676(16) Uani 1 1 d . . . . .
C4 C 0.8092(4) 0.7363(4) 0.53200(10) 0.0726(18) Uani 1 1 d . . . . .
C5 C 0.8223(5) 0.8055(4) 0.52590(13) 0.098(3) Uani 1 1 d . . . . .
H5 H 0.8710 0.8460 0.5254 0.118 Uiso 1 1 calc R U . . .
C6 C 0.7637(7) 0.8142(5) 0.52062(15) 0.118(4) Uani 1 1 d . . . . .
H6 H 0.7725 0.8615 0.5163 0.142 Uiso 1 1 calc R U . . .
C7 C 0.6927(6) 0.7569(5) 0.52134(12) 0.099(3) Uani 1 1 d . . . . .
H7 H 0.6524 0.7636 0.5177 0.119 Uiso 1 1 calc R U . . .
C8 C 0.6822(4) 0.6875(4) 0.52780(10) 0.0721(18) Uani 1 1 d . . . . .
C9 C 0.6085(4) 0.6256(4) 0.53154(10) 0.0715(18) Uani 1 1 d . . . . .
C10 C 0.5135(3) 0.4461(3) 0.54571(10) 0.0570(14) Uani 1 1 d . . . . .
C11 C 0.5379(3) 0.3656(3) 0.52858(8) 0.0524(13) Uani 1 1 d . . . . .
H11 H 0.5721 0.3567 0.5206 0.063 Uiso 1 1 calc R U . . .
C12 C 0.9425(3) 0.6790(3) 0.57182(10) 0.0747(18) Uani 1 1 d . . . . .
H12A H 0.9338 0.6433 0.5839 0.112 Uiso 1 1 calc R U . . .
H12B H 0.9263 0.7129 0.5771 0.112 Uiso 1 1 calc R U . . .
H12C H 0.9951 0.7067 0.5682 0.112 Uiso 1 1 calc R U . . .
C13 C 0.9450(4) 0.7843(3) 0.53780(15) 0.091(2) Uani 1 1 d . . . . .
H13A H 0.9511 0.8181 0.5503 0.137 Uiso 1 1 calc R U . . .
H13B H 0.9552 0.8102 0.5231 0.137 Uiso 1 1 calc R U . . .
H13C H 0.9792 0.7659 0.5400 0.137 Uiso 1 1 calc R U . . .
C14 C 0.5423(5) 0.6266(5) 0.52205(16) 0.126(4) Uani 1 1 d . . . . .
H14A H 0.5219 0.6446 0.5339 0.189 Uiso 1 1 calc R U . . .
H14B H 0.5051 0.5769 0.5175 0.189 Uiso 1 1 calc R U . . .
H14C H 0.5569 0.6592 0.5087 0.189 Uiso 1 1 calc R U . . .
C15 C 0.4972(4) 0.5391(4) 0.56727(16) 0.109(3) Uani 1 1 d . . . . .
H15A H 0.4460 0.5217 0.5630 0.164 Uiso 1 1 calc R U . . .
H15B H 0.5234 0.5927 0.5687 0.164 Uiso 1 1 calc R U . . .
H15C H 0.4986 0.5173 0.5820 0.164 Uiso 1 1 calc R U . . .
C16 C 0.7658(3) 0.5412(3) 0.58845(9) 0.0581(14) Uani 1 1 d . . . . .
H16 H 0.7758 0.5065 0.5814 0.070 Uiso 1 1 calc R U . . .
C17 C 0.7898(3) 0.5634(3) 0.61053(9) 0.0640(15) Uani 1 1 d . . . . .
H17 H 0.8143 0.5424 0.6184 0.077 Uiso 1 1 calc R U . . .
C18 C 0.7793(3) 0.6139(3) 0.62113(9) 0.0553(13) Uani 1 1 d . . . . .
C19 C 0.7397(4) 0.6403(4) 0.60899(9) 0.0682(16) Uani 1 1 d . . . . .
H19 H 0.7295 0.6752 0.6158 0.082 Uiso 1 1 calc R U . . .
C20 C 0.7156(4) 0.6150(3) 0.58693(9) 0.0658(16) Uani 1 1 d . . . . .
H20 H 0.6885 0.6330 0.5789 0.079 Uiso 1 1 calc R U . . .
C21 C 0.8055(3) 0.6404(3) 0.64446(9) 0.0597(14) Uani 1 1 d D . . . .
C26 C 0.6934(8) 0.4811(11) 0.4670(3) 0.221(9) Uani 1 1 d . . . . .
C22 C 0.8715(4) 0.6459(5) 0.65163(15) 0.068(2) Uiso 0.7 1 d D . P A 1
H22 H 0.8977 0.6316 0.6416 0.081 Uiso 0.7 1 calc R U P A 1
C23 C 0.7675(5) 0.6608(5) 0.65969(15) 0.074(2) Uiso 0.7 1 d D . P A 1
H23 H 0.7222 0.6567 0.6551 0.089 Uiso 0.7 1 calc R U P A 1
C22A C 0.8137(12) 0.5951(10) 0.6597(3) 0.072(5) Uiso 0.3 1 d D . P A 2
H22A H 0.8031 0.5472 0.6554 0.086 Uiso 0.3 1 calc R U P A 2
C23A C 0.8285(12) 0.7117(7) 0.6516(4) 0.076(6) Uiso 0.3 1 d D . P A 2
H23A H 0.8276 0.7447 0.6407 0.091 Uiso 0.3 1 calc R U P A 2
S1 S 0.6667 0.3333 0.56062(3) 0.0461(5) Uani 1 3 d S T P . .
F1 F 0.6237(2) 0.3581(2) 0.60022(5) 0.0760(10) Uani 1 1 d . . . . .
O1 O 0.59263(19) 0.2775(2) 0.55480(6) 0.0536(9) Uani 1 1 d . . . . .
C28 C 0.6667 0.3333 0.59235(15) 0.059(2) Uani 1 3 d S T P . .
N8 N 0.6306(7) 0.7211(7) 0.5823(2) 0.087(3) Uiso 0.5 1 d . . P . .
C00D C 0.7341(10) 0.8554(10) 0.5798(3) 0.118(6) Uiso 0.5 1 d . . P . .
H00A H 0.7306 0.8777 0.5654 0.177 Uiso 0.5 1 calc R U P . .
H00B H 0.7815 0.8569 0.5803 0.177 Uiso 0.5 1 calc R U P . .
H00C H 0.7303 0.8826 0.5928 0.177 Uiso 0.5 1 calc R U P . .
C29 C 0.6712(10) 0.7748(11) 0.5809(3) 0.108(5) Uiso 0.5 1 d . . P . .
S2 S 1.0000 1.0000 0.5000 0.0450(7) Uani 1 6 d S T P . .
O2 O 0.9467(3) 0.9256(3) 0.49518(14) 0.0537(18) Uani 0.5 1 d . . P . .
C24 C 1.0000 1.0000 0.4682(4) 0.058(5) Uani 0.5 3 d S T P . .
F2 F 0.9756(4) 1.0424(4) 0.45913(13) 0.074(2) Uani 0.5 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N1 2.726(4) . ?
Pb1 N3 2.658(5) . ?
Pb1 N4 2.575(5) . ?
Pb1 N5 2.688(5) . ?
Pb1 N9 2.502(4) . ?
S3 O3 1.398(6) . ?
S3 O4 1.293(6) . ?
S3 O5 1.430(6) . ?
S3 C26 1.960(19) . ?
F3 C26 1.39(2) . ?
F4 C26 1.411(15) . ?
F5 C26 1.227(13) . ?
N1 C2 1.353(7) . ?
N1 C11 1.340(7) 3_665 ?
N2 N3 1.393(7) . ?
N2 C2 1.385(7) . ?
N2 C12 1.440(7) . ?
N3 C3 1.289(7) . ?
N4 C4 1.378(9) . ?
N4 C8 1.330(8) . ?
N5 N6 1.420(7) . ?
N5 C9 1.279(8) . ?
N6 C10 1.370(7) . ?
N6 C15 1.464(8) . ?
N7 C10 1.326(7) . ?
N7 C11 1.320(7) . ?
N9 C16 1.342(7) . ?
N9 C20 1.318(7) . ?
C1 H1 0.9500 . ?
C1 C2 1.376(8) . ?
C1 C10 1.382(8) 3_665 ?
C3 C4 1.470(9) . ?
C3 C13 1.478(9) . ?
C4 C5 1.384(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.369(13) . ?
C6 H6 0.9500 . ?
C6 C7 1.374(13) . ?
C7 H7 0.9500 . ?
C7 C8 1.414(9) . ?
C8 C9 1.458(10) . ?
C9 C14 1.508(9) . ?
C10 C1 1.382(8) 2_655 ?
C11 N1 1.340(7) 2_655 ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 0.9500 . ?
C16 C17 1.375(7) . ?
C17 H17 0.9500 . ?
C17 C18 1.340(8) . ?
C18 C19 1.400(8) . ?
C18 C21 1.467(7) . ?
C19 H19 0.9500 . ?
C19 C20 1.387(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.399(7) . ?
C21 C23 1.398(7) . ?
C21 C22A 1.377(9) . ?
C21 C23A 1.390(9) . ?
C22 H22 0.9500 . ?
C22 C23 1.404(11) 13_666 ?
C23 C22 1.404(11) 13_666 ?
C23 H23 0.9500 . ?
C22A H22A 0.9500 . ?
C22A C23A 1.39(3) 13_666 ?
C23A C22A 1.39(3) 13_666 ?
C23A H23A 0.9500 . ?
S1 O1 1.446(3) 2_655 ?
S1 O1 1.446(4) . ?
S1 O1 1.446(3) 3_665 ?
S1 C28 1.848(9) . ?
F1 C28 1.331(4) . ?
C28 F1 1.331(4) 3_665 ?
C28 F1 1.331(4) 2_655 ?
N8 C29 1.02(2) . ?
C00D H00A 0.9800 . ?
C00D H00B 0.9800 . ?
C00D H00C 0.9800 . ?
C00D C29 1.54(2) . ?
S2 O2 1.424(6) 3_675 ?
S2 O2 1.425(6) 11_566 ?
S2 O2 1.425(6) 2_765 ?
S2 O2 1.424(6) . ?
S2 O2 1.425(6) 10_776 ?
S2 O2 1.424(6) 12_656 ?
S2 C24 1.85(2) . ?
S2 C24 1.85(2) 10_776 ?
O2 O2 1.505(8) 12_656 ?
O2 O2 1.505(8) 11_566 ?
C24 F2 1.341(10) 2_765 ?
C24 F2 1.341(10) . ?
C24 F2 1.341(10) 3_675 ?

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
N3 Pb1 N1 57.79(14) . . ?
N3 Pb1 N5 115.38(14) . . ?
N4 Pb1 N1 116.71(15) . . ?
N4 Pb1 N3 60.88(16) . . ?
N4 Pb1 N5 60.22(17) . . ?
N5 Pb1 N1 168.74(13) . . ?
N9 Pb1 N1 90.17(14) . . ?
N9 Pb1 N3 70.77(15) . . ?
N9 Pb1 N4 83.72(15) . . ?
N9 Pb1 N5 78.81(14) . . ?
O3 S3 O5 115.8(4) . . ?
O3 S3 C26 97.8(5) . . ?
O4 S3 O3 124.6(4) . . ?
O4 S3 O5 113.3(4) . . ?
O4 S3 C26 101.2(7) . . ?
O5 S3 C26 96.1(6) . . ?
C2 N1 Pb1 118.4(4) . . ?
C11 N1 Pb1 122.0(3) 3_665 . ?
C11 N1 C2 114.8(5) 3_665 . ?
N3 N2 C12 120.1(5) . . ?
C2 N2 N3 114.6(4) . . ?
C2 N2 C12 120.1(5) . . ?
N2 N3 Pb1 120.9(3) . . ?
C3 N3 Pb1 122.5(4) . . ?
C3 N3 N2 116.5(5) . . ?
C4 N4 Pb1 120.8(4) . . ?
C8 N4 Pb1 117.3(5) . . ?
C8 N4 C4 120.2(6) . . ?
N6 N5 Pb1 123.7(3) . . ?
C9 N5 Pb1 112.9(5) . . ?
C9 N5 N6 115.1(5) . . ?
N5 N6 C15 115.2(5) . . ?
C10 N6 N5 117.1(5) . . ?
C10 N6 C15 122.9(6) . . ?
C11 N7 C10 115.2(5) . . ?
C16 N9 Pb1 118.7(4) . . ?
C20 N9 Pb1 122.5(4) . . ?
C20 N9 C16 117.4(5) . . ?
C2 C1 H1 121.4 . . ?
C2 C1 C10 117.2(5) . 3_665 ?
C10 C1 H1 121.4 3_665 . ?
N1 C2 N2 118.0(5) . . ?
N1 C2 C1 121.6(6) . . ?
C1 C2 N2 120.3(5) . . ?
N3 C3 C4 115.2(6) . . ?
N3 C3 C13 126.5(7) . . ?
C4 C3 C13 118.3(6) . . ?
N4 C4 C3 117.4(5) . . ?
N4 C4 C5 120.4(7) . . ?
C5 C4 C3 122.3(7) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 C4 118.6(9) . . ?
C6 C5 H5 120.7 . . ?
C5 C6 H6 118.9 . . ?
C5 C6 C7 122.1(8) . . ?
C7 C6 H6 118.9 . . ?
C6 C7 H7 121.5 . . ?
C6 C7 C8 117.1(8) . . ?
C8 C7 H7 121.5 . . ?
N4 C8 C7 121.6(8) . . ?
N4 C8 C9 117.4(6) . . ?
C7 C8 C9 120.6(7) . . ?
N5 C9 C8 115.9(5) . . ?
N5 C9 C14 123.5(8) . . ?
C8 C9 C14 120.6(6) . . ?
N6 C10 C1 120.3(5) . 2_655 ?
N7 C10 N6 116.9(5) . . ?
N7 C10 C1 122.7(5) . 2_655 ?
N1 C11 H11 115.9 2_655 . ?
N7 C11 N1 128.2(5) . 2_655 ?
N7 C11 H11 115.9 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C3 C13 H13A 109.5 . . ?
C3 C13 H13B 109.5 . . ?
C3 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 H15A 109.5 . . ?
N6 C15 H15B 109.5 . . ?
N6 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N9 C16 H16 118.8 . . ?
N9 C16 C17 122.3(5) . . ?
C17 C16 H16 118.8 . . ?
C16 C17 H17 119.3 . . ?
C18 C17 C16 121.5(6) . . ?
C18 C17 H17 119.3 . . ?
C17 C18 C19 116.6(5) . . ?
C17 C18 C21 123.3(5) . . ?
C19 C18 C21 120.2(5) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 C18 119.5(6) . . ?
C20 C19 H19 120.3 . . ?
N9 C20 C19 122.8(6) . . ?
N9 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
C22 C21 C18 118.5(6) . . ?
C23 C21 C18 122.7(6) . . ?
C23 C21 C22 118.8(6) . . ?
C22A C21 C18 119.3(10) . . ?
C22A C21 C23A 117.2(13) . . ?
C23A C21 C18 123.3(10) . . ?
F3 C26 S3 110.8(8) . . ?
F3 C26 F4 110.6(14) . . ?
F4 C26 S3 98.2(12) . . ?
F5 C26 S3 111.3(15) . . ?
F5 C26 F3 117.7(18) . . ?
F5 C26 F4 106.3(11) . . ?
C21 C22 H22 119.9 . . ?
C21 C22 C23 120.2(7) . 13_666 ?
C23 C22 H22 119.9 13_666 . ?
C21 C23 C22 121.1(8) . 13_666 ?
C21 C23 H23 119.5 . . ?
C22 C23 H23 119.5 13_666 . ?
C21 C22A H22A 121.1 . . ?
C21 C22A C23A 117.9(16) . 13_666 ?
C23A C22A H22A 121.1 13_666 . ?
C21 C23A H23A 117.7 . . ?
C22A C23A C21 124.6(17) 13_666 . ?
C22A C23A H23A 117.7 13_666 . ?
O1 S1 O1 114.69(12) 2_655 . ?
O1 S1 O1 114.69(12) 2_655 3_665 ?
O1 S1 O1 114.68(12) . 3_665 ?
O1 S1 C28 103.55(15) 2_655 . ?
O1 S1 C28 103.55(15) . . ?
O1 S1 C28 103.55(15) 3_665 . ?
F1 C28 S1 110.1(4) . . ?
F1 C28 S1 110.1(4) 3_665 . ?
F1 C28 S1 110.1(4) 2_655 . ?
F1 C28 F1 108.8(4) 2_655 . ?
F1 C28 F1 108.8(4) 2_655 3_665 ?
F1 C28 F1 108.8(4) 3_665 . ?
H00A C00D H00B 109.5 . . ?
H00A C00D H00C 109.5 . . ?
H00B C00D H00C 109.5 . . ?
C29 C00D H00A 109.5 . . ?
C29 C00D H00B 109.5 . . ?
C29 C00D H00C 109.5 . . ?
N8 C29 C00D 177(2) . . ?
O2 S2 O2 116.2(2) 3_675 2_765 ?
O2 S2 O2 63.8(2) 3_675 10_776 ?
O2 S2 O2 63.8(2) 12_656 2_765 ?
O2 S2 O2 63.8(2) 10_776 2_765 ?
O2 S2 O2 180.0(4) . 10_776 ?
O2 S2 O2 63.8(2) 3_675 11_566 ?
O2 S2 O2 116.2(2) 10_776 11_566 ?
O2 S2 O2 116.2(2) . 2_765 ?
O2 S2 O2 180.0(6) 12_656 3_675 ?
O2 S2 O2 116.2(2) 12_656 11_566 ?
O2 S2 O2 63.8(2) 12_656 . ?
O2 S2 O2 63.8(2) . 11_566 ?
O2 S2 O2 116.2(2) 3_675 . ?
O2 S2 O2 116.2(2) 12_656 10_776 ?
O2 S2 O2 180.0(6) 2_765 11_566 ?
O2 S2 C24 101.4(3) 12_656 . ?
O2 S2 C24 101.4(3) . 10_776 ?
O2 S2 C24 78.6(3) 12_656 10_776 ?
O2 S2 C24 78.6(3) 3_675 . ?
O2 S2 C24 78.6(3) 11_566 10_776 ?
O2 S2 C24 78.6(3) . . ?
O2 S2 C24 101.4(3) 3_675 10_776 ?
O2 S2 C24 101.4(3) 10_776 . ?
O2 S2 C24 78.6(3) 10_776 10_776 ?
O2 S2 C24 78.6(3) 2_765 . ?
O2 S2 C24 101.4(3) 11_566 . ?
O2 S2 C24 101.4(3) 2_765 10_776 ?
C24 S2 C24 180.0 . 10_776 ?
S2 O2 O2 58.11(10) . 12_656 ?
S2 O2 O2 58.11(10) . 11_566 ?
O2 O2 O2 106.9(6) 12_656 11_566 ?
F2 C24 S2 113.3(9) 2_765 . ?
F2 C24 S2 113.3(9) 3_675 . ?
F2 C24 S2 113.3(9) . . ?
F2 C24 F2 105.4(10) 2_765 . ?
F2 C24 F2 105.4(10) 3_675 . ?
F2 C24 F2 105.4(10) 2_765 3_675 ?

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 N1 C2 N2 -24.6(6) . . . . ?
Pb1 N1 C2 C1 156.7(4) . . . . ?
Pb1 N3 C3 C4 13.5(7) . . . . ?
Pb1 N3 C3 C13 -167.5(5) . . . . ?
Pb1 N4 C4 C3 -15.5(7) . . . . ?
Pb1 N4 C4 C5 164.7(5) . . . . ?
Pb1 N4 C8 C7 -164.8(5) . . . . ?
Pb1 N4 C8 C9 21.7(7) . . . . ?
Pb1 N5 N6 C10 -14.7(7) . . . . ?
Pb1 N5 N6 C15 141.4(5) . . . . ?
Pb1 N5 C9 C8 -38.7(6) . . . . ?
Pb1 N5 C9 C14 142.5(6) . . . . ?
Pb1 N9 C16 C17 166.2(5) . . . . ?
Pb1 N9 C20 C19 -164.3(5) . . . . ?
N2 N3 C3 C4 -171.1(5) . . . . ?
N2 N3 C3 C13 7.8(9) . . . . ?
N3 N2 C2 N1 -0.4(7) . . . . ?
N3 N2 C2 C1 178.3(5) . . . . ?
N3 C3 C4 N4 1.1(8) . . . . ?
N3 C3 C4 C5 -179.1(6) . . . . ?
N4 C4 C5 C6 -0.5(11) . . . . ?
N4 C8 C9 N5 13.0(8) . . . . ?
N4 C8 C9 C14 -168.1(6) . . . . ?
N5 N6 C10 N7 -9.4(7) . . . . ?
N5 N6 C10 C1 174.0(5) . . . 2_655 ?
N6 N5 C9 C8 171.7(5) . . . . ?
N6 N5 C9 C14 -7.2(9) . . . . ?
N9 C16 C17 C18 -2.2(10) . . . . ?
C2 N2 N3 Pb1 26.7(6) . . . . ?
C2 N2 N3 C3 -148.7(5) . . . . ?
C3 C4 C5 C6 179.7(7) . . . . ?
C4 N4 C8 C7 0.2(9) . . . . ?
C4 N4 C8 C9 -173.3(5) . . . . ?
C4 C5 C6 C7 0.5(13) . . . . ?
C5 C6 C7 C8 -0.1(13) . . . . ?
C6 C7 C8 N4 -0.2(11) . . . . ?
C6 C7 C8 C9 173.0(7) . . . . ?
C7 C8 C9 N5 -160.5(6) . . . . ?
C7 C8 C9 C14 18.4(10) . . . . ?
C8 N4 C4 C3 -180.0(5) . . . . ?
C8 N4 C4 C5 0.2(9) . . . . ?
C9 N5 N6 C10 131.2(6) . . . . ?
C9 N5 N6 C15 -72.6(7) . . . . ?
C10 N7 C11 N1 3.1(8) . . . 2_655 ?
C10 C1 C2 N1 3.3(9) 3_665 . . . ?
C10 C1 C2 N2 -175.4(5) 3_665 . . . ?
C11 N1 C2 N2 179.6(5) 3_665 . . . ?
C11 N1 C2 C1 0.8(8) 3_665 . . . ?
C11 N7 C10 N6 -174.7(5) . . . . ?
C11 N7 C10 C1 1.8(7) . . . 2_655 ?
C12 N2 N3 Pb1 -128.0(4) . . . . ?
C12 N2 N3 C3 56.6(7) . . . . ?
C12 N2 C2 N1 154.3(5) . . . . ?
C12 N2 C2 C1 -27.0(8) . . . . ?
C13 C3 C4 N4 -177.9(6) . . . . ?
C13 C3 C4 C5 1.9(9) . . . . ?
C15 N6 C10 N7 -163.6(6) . . . . ?
C15 N6 C10 C1 19.8(9) . . . 2_655 ?
C16 N9 C20 C19 1.4(9) . . . . ?
C16 C17 C18 C19 2.9(9) . . . . ?
C16 C17 C18 C21 -178.5(6) . . . . ?
C17 C18 C19 C20 -1.7(9) . . . . ?
C17 C18 C21 C22 34.1(9) . . . . ?
C17 C18 C21 C23 -146.5(7) . . . . ?
C17 C18 C21 C22A -27.4(13) . . . . ?
C17 C18 C21 C23A 147.0(12) . . . . ?
C18 C19 C20 N9 -0.5(10) . . . . ?
C18 C21 C22 C23 178.6(7) . . . 13_666 ?
C18 C21 C23 C22 -178.6(7) . . . 13_666 ?
C18 C21 C22A C23A -179.5(15) . . . 13_666 ?
C18 C21 C23A C22A 179.3(16) . . . 13_666 ?
C19 C18 C21 C22 -147.4(7) . . . . ?
C19 C18 C21 C23 32.0(9) . . . . ?
C19 C18 C21 C22A 151.1(11) . . . . ?
C19 C18 C21 C23A -34.4(14) . . . . ?
C20 N9 C16 C17 -0.1(9) . . . . ?
C21 C18 C19 C20 179.7(6) . . . . ?
C22 C21 C23 C22 0.9(14) . . . 13_666 ?
C22 C21 C22A C23A 75.2(19) . . . 13_666 ?
C22 C21 C23A C22A -55(2) . . . 13_666 ?
C23 C21 C22 C23 -0.9(14) . . . 13_666 ?
C23 C21 C22A C23A -47(2) . . . 13_666 ?
C23 C21 C23A C22A 70(2) . . . 13_666 ?
C22A C21 C22 C23 -74.6(14) . . . 13_666 ?
C22A C21 C23 C22 51.4(13) . . . 13_666 ?
C22A C21 C23A C22A -6(3) . . . 13_666 ?
C23A C21 C22 C23 49.0(13) . . . 13_666 ?
C23A C21 C23 C22 -68.4(14) . . . 13_666 ?
C23A C21 C22A C23A 6(3) . . . 13_666 ?
O1 S1 C28 F1 52.4(2) 3_665 . . . ?
O1 S1 C28 F1 -67.6(2) 2_655 . . 2_655 ?
O1 S1 C28 F1 52.4(2) . . . 2_655 ?
O1 S1 C28 F1 -67.6(2) 3_665 . . 3_665 ?
O1 S1 C28 F1 172.4(2) 2_655 . . . ?
O1 S1 C28 F1 -67.6(2) . . . . ?
O1 S1 C28 F1 172.4(2) 3_665 . . 2_655 ?
O1 S1 C28 F1 172.4(2) . . . 3_665 ?
O1 S1 C28 F1 52.4(2) 2_655 . . 3_665 ?
O2 S2 O2 O2 180.000(2) 3_675 . . 12_656 ?
O2 S2 O2 O2 -37.7(10) 3_675 . . 11_566 ?
O2 S2 O2 O2 142.3(10) 12_656 . . 11_566 ?
O2 S2 O2 O2 37.7(10) 2_765 . . 12_656 ?
O2 S2 O2 O2 -142.3(10) 11_566 . . 12_656 ?
O2 S2 O2 O2 180.000(0) 2_765 . . 11_566 ?
O2 S2 C24 F2 -65.2(4) 12_656 . . 3_675 ?
O2 S2 C24 F2 114.8(4) . . . . ?
O2 S2 C24 F2 174.8(4) 12_656 . . . ?
O2 S2 C24 F2 -125.2(4) . . . 3_675 ?
O2 S2 C24 F2 -125.2(4) 2_765 . . . ?
O2 S2 C24 F2 -5.2(4) 2_765 . . 3_675 ?
O2 S2 C24 F2 114.8(4) 3_675 . . 3_675 ?
O2 S2 C24 F2 54.8(4) 12_656 . . 2_765 ?
O2 S2 C24 F2 54.8(4) 10_776 . . 3_675 ?
O2 S2 C24 F2 -125.2(4) 3_675 . . 2_765 ?
O2 S2 C24 F2 174.8(4) 11_566 . . 3_675 ?
O2 S2 C24 F2 -5.2(4) . . . 2_765 ?
O2 S2 C24 F2 -5.2(4) 3_675 . . . ?
O2 S2 C24 F2 54.8(4) 11_566 . . . ?
O2 S2 C24 F2 -65.2(4) 10_776 . . . ?
O2 S2 C24 F2 114.8(4) 2_765 . . 2_765 ?
O2 S2 C24 F2 -65.2(4) 11_566 . . 2_765 ?
O2 S2 C24 F2 174.8(4) 10_776 . . 2_765 ?
C24 S2 O2 O2 -108.8(5) . . . 11_566 ?
C24 S2 O2 O2 -71.2(5) 10_776 . . 12_656 ?
C24 S2 O2 O2 108.8(5) . . . 12_656 ?
C24 S2 O2 O2 71.2(5) 10_776 . . 11_566 ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 2367 electrons were 
found in a volume of 9246Å³ in 1 void per unit cell. 
This is consistent with the presence of 
3[(CF3SO3)], 18[(CH3CN)] per Formula Unit 
which account for 2367 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 -0.782 -0.596 0.000 3082.1 789.4 '3 (CF3SO3),18 (CH3CN)'
2 -0.130 -0.297 0.333 3082.1 789.4 '3 (CF3SO3),18 (CH3CN)'
3 -0.859 -0.589 0.667 3082.1 789.4 '3 (CF3SO3),18 (CH3CN)'

_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).
# 
# 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_3PF6
_database_code_depnum_ccdc_archive 'CCDC 2293673'
loop_
_audit_author_name
_audit_author_address
'Nathalie Gruber'
;Universite de Strasbourg
France
;
_audit_update_record             
;
2023-09-07 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C73 H69 F12 N24 O12 Pb3 S4), F6 P,solvent'
_chemical_formula_sum            'C146 H138 F30 N48 O24 P Pb6 S8'
_chemical_formula_weight         5049.63

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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+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                   21.0435(6)
_cell_length_b                   21.0435(6)
_cell_length_c                   58.507(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     22437.5(16)
_cell_formula_units_Z            3
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9914
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      27.80

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_F_000             7341
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    3.491
_shelx_estimated_absorpt_T_min   0.514
_shelx_estimated_absorpt_T_max   0.572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6231
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            70808
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -77
_diffrn_reflns_limit_l_max       76
_diffrn_reflns_theta_min         1.935
_diffrn_reflns_theta_max         27.911
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11923
_reflns_number_gt                10039
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.

Some atoms were left in isotrope due to high thermal agitation
C24F1F2F3 C24AF1AF2AF3A
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0722P)²+129.9682P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11923
_refine_ls_number_parameters     376
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.1220
_refine_ls_wR_factor_gt          0.1171
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.004

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 0.82815(2) 0.28328(2) 0.53461(2) 0.03665(7) Uani 1 1 d . . . . .
N1 N 0.9350(2) 0.2549(2) 0.53312(7) 0.0484(9) Uani 1 1 d . . . . .
C1 C 0.9225(3) 0.1856(3) 0.53263(10) 0.0510(11) Uani 1 1 d . . . . .
C2 C 0.9775(3) 0.1696(3) 0.52717(12) 0.0647(15) Uani 1 1 d . . . . .
H2 H 0.967824 0.120411 0.527153 0.078 Uiso 1 1 calc R U . . .
C3 C 1.0460(3) 0.2266(4) 0.52181(13) 0.0718(18) Uani 1 1 d . . . . .
H3 H 1.084097 0.216778 0.518011 0.086 Uiso 1 1 calc R U . . .
C4 C 1.0600(3) 0.2978(4) 0.52189(11) 0.0658(15) Uani 1 1 d . . . . .
H4 H 1.106974 0.337497 0.517957 0.079 Uiso 1 1 calc R U . . .
C5 C 1.0023(3) 0.3098(3) 0.52797(10) 0.0528(12) Uani 1 1 d . . . . .
C6 C 1.0159(3) 0.3858(3) 0.53116(10) 0.0546(13) Uani 1 1 d . . . . .
C7 C 1.0835(4) 0.4487(4) 0.52079(17) 0.099(3) Uani 1 1 d . . . . .
H7A H 1.075695 0.490473 0.518577 0.148 Uiso 1 1 calc R U . . .
H7B H 1.093596 0.433687 0.506004 0.148 Uiso 1 1 calc R U . . .
H7C H 1.125404 0.463072 0.531034 0.148 Uiso 1 1 calc R U . . .
N2 N 0.9674(2) 0.3916(2) 0.54301(7) 0.0458(9) Uani 1 1 d . . . . .
N3 N 0.9864(2) 0.4636(2) 0.54883(9) 0.0524(10) Uani 1 1 d . . . . .
C8 C 1.0452(3) 0.5015(4) 0.56565(16) 0.092(3) Uani 1 1 d . . . . .
H8A H 1.080742 0.550306 0.559895 0.138 Uiso 1 1 calc R U . . .
H8B H 1.069936 0.473069 0.568220 0.138 Uiso 1 1 calc R U . . .
H8C H 1.024314 0.506273 0.580066 0.138 Uiso 1 1 calc R U . . .
C9 C 0.9346(2) 0.4837(2) 0.54571(8) 0.0426(10) Uani 1 1 d . . . . .
N4 N 0.87473(19) 0.4366(2) 0.53363(6) 0.0383(7) Uani 1 1 d . . . . .
C10 C 0.8278(2) 0.4599(2) 0.52903(7) 0.0391(9) Uani 1 1 d . . . . .
H10 H 0.784527 0.426635 0.520994 0.047 Uiso 1 1 calc R U . . .
N5 N 0.8344(2) 0.52435(19) 0.53435(7) 0.0395(8) Uani 1 1 d . . . . .
C11 C 0.8943(2) 0.5700(2) 0.54681(8) 0.0393(9) Uani 1 1 d . . . . .
C12 C 0.9455(2) 0.5505(3) 0.55359(9) 0.0473(10) Uani 1 1 d . . . . .
H12 H 0.985909 0.581306 0.563120 0.057 Uiso 1 1 calc R U . . .
N6 N 0.9045(2) 0.6383(2) 0.55201(7) 0.0455(9) Uani 1 1 d . . . . .
C13 C 0.9478(3) 0.6777(3) 0.57221(10) 0.0534(12) Uani 1 1 d . . . . .
H13A H 0.945460 0.642281 0.583534 0.080 Uiso 1 1 calc R U . . .
H13B H 0.927785 0.706793 0.578857 0.080 Uiso 1 1 calc R U . . .
H13C H 0.998935 0.710313 0.567718 0.080 Uiso 1 1 calc R U . . .
N7 N 0.8524(2) 0.6539(2) 0.54374(7) 0.0449(9) Uani 1 1 d . . . . .
C14 C 0.8735(3) 0.7209(2) 0.53868(10) 0.0505(11) Uani 1 1 d . . . . .
C15 C 0.9520(3) 0.7816(3) 0.53806(13) 0.0629(15) Uani 1 1 d . . . . .
H15A H 0.963880 0.809637 0.552339 0.094 Uiso 1 1 calc R U . . .
H15B H 0.959110 0.814212 0.525142 0.094 Uiso 1 1 calc R U . . .
H15C H 0.984146 0.760750 0.536286 0.094 Uiso 1 1 calc R U . . .
N8 N 0.8349(2) 0.2689(2) 0.57670(7) 0.0457(9) Uani 1 1 d . . . . .
C16 C 0.8976(3) 0.2821(3) 0.58724(9) 0.0555(13) Uani 1 1 d . . . . .
H16 H 0.942515 0.308788 0.579156 0.067 Uiso 1 1 calc R U . . .
C17 C 0.8995(3) 0.2591(4) 0.60892(9) 0.0595(13) Uani 1 1 d . . . . .
H17 H 0.944941 0.269579 0.615535 0.071 Uiso 1 1 calc R U . . .
C18 C 0.8344(3) 0.2201(3) 0.62139(8) 0.0511(11) Uani 1 1 d . . . . .
C19 C 0.7701(3) 0.2075(3) 0.61053(8) 0.0482(11) Uani 1 1 d . . . . .
H19 H 0.724556 0.181750 0.618339 0.058 Uiso 1 1 calc R U . . .
C20 C 0.7721(3) 0.2319(3) 0.58874(8) 0.0453(10) Uani 1 1 d . . . . .
H20 H 0.727424 0.222279 0.581785 0.054 Uiso 1 1 calc R U . . .
C21 C 0.8335(3) 0.1928(3) 0.64465(9) 0.0536(12) Uani 1 1 d . . . . .
C22 C 0.8934(3) 0.2320(4) 0.65931(10) 0.0658(15) Uani 1 1 d . . . . .
H22 H 0.934534 0.276645 0.654373 0.079 Uiso 1 1 calc R U . . .
C23 C 0.8921(3) 0.2050(4) 0.68120(10) 0.0678(16) Uani 1 1 d . . . . .
H23 H 0.932690 0.231777 0.691111 0.081 Uiso 1 1 calc R U . . .
S1 S 0.86852(11) 0.28223(13) 0.47450(3) 0.0959(8) Uani 1 1 d D . . . .
O2 O 0.9181(4) 0.3519(4) 0.48582(11) 0.1277(14) Uani 1 1 d D . . . .
O1 O 0.8282(4) 0.2286(4) 0.49105(11) 0.1277(14) Uani 1 1 d D . . . .
O3 O 0.8991(4) 0.2385(4) 0.46183(11) 0.1277(14) Uani 1 1 d D . . . .
C24 C 0.7974(8) 0.3074(8) 0.4714(3) 0.145 Uani 0.5 1 d D . P A 1
F3 F 0.7461(7) 0.2505(6) 0.45680(19) 0.145 Uani 0.5 1 d D . P A 1
F1 F 0.7502(7) 0.3087(6) 0.48739(18) 0.145 Uani 0.5 1 d D . P A 1
F2 F 0.8170(7) 0.3683(6) 0.45704(19) 0.145 Uani 0.5 1 d D . P A 1
C24A C 0.8286(9) 0.2818(9) 0.4502(3) 0.145 Uani 0.5 1 d D . P A 2
F1A F 0.7750(7) 0.2142(5) 0.4430(2) 0.145 Uani 0.5 1 d D . P A 2
F2A F 0.7890(7) 0.3183(6) 0.4547(2) 0.145 Uani 0.5 1 d D . P A 2
F3A F 0.8736(6) 0.3144(6) 0.43369(18) 0.145 Uani 0.5 1 d D . P A 2
S2 S 0.666667 0.333333 0.56118(3) 0.0347(3) Uani 1 3 d S T P . .
O4 O 0.72281(16) 0.31555(17) 0.55551(5) 0.0414(7) Uani 1 1 d . . . . .
C25 C 0.666667 0.333333 0.59237(14) 0.0474(18) Uani 1 3 d S T P . .
F4 F 0.62449(19) 0.35846(19) 0.60057(5) 0.0632(8) Uani 1 1 d . . . . .
P1 P 0.000000 1.000000 0.500000 0.0478(8) Uani 1 6 d S T P . .
F5 F 0.01755(15) 0.94825(15) 0.51544(7) 0.0707(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N8 2.494(4) . ?
Pb1 N1 2.601(4) . ?
Pb1 N7 2.674(4) 3_665 ?
Pb1 N2 2.711(4) . ?
Pb1 N5 2.718(4) 3_665 ?
N1 C5 1.340(6) . ?
N1 C1 1.346(6) . ?
C1 C2 1.394(7) . ?
C1 C14 1.485(7) 3_665 ?
C2 C3 1.373(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.375(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.402(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.488(8) . ?
C6 N2 1.289(6) . ?
C6 C7 1.505(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N2 N3 1.402(6) . ?
N3 C9 1.364(6) . ?
N3 C8 1.465(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.349(6) . ?
C9 C12 1.385(7) . ?
N4 C10 1.333(6) . ?
C10 N5 1.329(6) . ?
C10 H10 0.9500 . ?
N5 C11 1.354(6) . ?
C11 N6 1.376(6) . ?
C11 C12 1.390(6) . ?
C12 H12 0.9500 . ?
N6 N7 1.380(5) . ?
N6 C13 1.470(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N7 C14 1.283(6) . ?
C14 C15 1.500(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N8 C20 1.348(6) . ?
N8 C16 1.353(6) . ?
C16 C17 1.365(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.400(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.394(7) . ?
C18 C21 1.474(7) . ?
C19 C20 1.366(7) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C23 1.374(8) 13_656 ?
C21 C22 1.402(8) . ?
C22 C23 1.396(8) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
S1 O1 1.405(7) . ?
S1 O2 1.465(6) . ?
S1 O3 1.551(7) . ?
S1 C24A 1.652(15) . ?
S1 C24 1.829(15) . ?
C24 F1 1.376(15) . ?
C24 F2 1.409(15) . ?
C24 F3 1.427(16) . ?
C24A F3A 1.282(14) . ?
C24A F1A 1.366(14) . ?
C24A F2A 1.411(16) . ?
S2 O4 1.445(3) . ?
S2 O4 1.445(3) 3_665 ?
S2 O4 1.445(3) 2_655 ?
S2 C25 1.825(8) . ?
C25 F4 1.329(4) 2_655 ?
C25 F4 1.329(4) 3_665 ?
C25 F4 1.329(4) . ?
P1 F5 1.594(3) 11_456 ?
P1 F5 1.594(3) 2_675 ?
P1 F5 1.594(3) 10_576 ?
P1 F5 1.594(3) 12_666 ?
P1 F5 1.594(3) 3_465 ?
P1 F5 1.594(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Pb1 N1 84.10(13) . . ?
N8 Pb1 N7 70.57(13) . 3_665 ?
N1 Pb1 N7 60.35(12) . 3_665 ?
N8 Pb1 N2 79.63(13) . . ?
N1 Pb1 N2 60.27(12) . . ?
N7 Pb1 N2 115.04(11) 3_665 . ?
N8 Pb1 N5 89.69(12) . 3_665 ?
N1 Pb1 N5 116.40(12) . 3_665 ?
N7 Pb1 N5 58.04(11) 3_665 3_665 ?
N2 Pb1 N5 169.01(12) . 3_665 ?
C5 N1 C1 118.6(4) . . ?
C5 N1 Pb1 118.1(3) . . ?
C1 N1 Pb1 121.8(3) . . ?
N1 C1 C2 122.0(5) . . ?
N1 C1 C14 116.9(4) . 3_665 ?
C2 C1 C14 121.1(5) . 3_665 ?
C3 C2 C1 118.4(5) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 120.7(5) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C3 C4 C5 117.6(5) . . ?
C3 C4 H4 121.2 . . ?
C5 C4 H4 121.2 . . ?
N1 C5 C4 122.6(5) . . ?
N1 C5 C6 116.8(4) . . ?
C4 C5 C6 120.4(5) . . ?
N2 C6 C5 115.7(4) . . ?
N2 C6 C7 125.3(5) . . ?
C5 C6 C7 119.0(5) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 N2 N3 115.0(4) . . ?
C6 N2 Pb1 113.3(4) . . ?
N3 N2 Pb1 123.9(3) . . ?
C9 N3 N2 117.5(4) . . ?
C9 N3 C8 120.7(5) . . ?
N2 N3 C8 117.2(4) . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 N3 116.1(4) . . ?
N4 C9 C12 122.7(4) . . ?
N3 C9 C12 121.1(4) . . ?
C10 N4 C9 115.3(4) . . ?
N5 C10 N4 127.6(4) . . ?
N5 C10 H10 116.2 . . ?
N4 C10 H10 116.2 . . ?
C10 N5 C11 115.8(4) . . ?
C10 N5 Pb1 121.6(3) . 2_655 ?
C11 N5 Pb1 118.9(3) . 2_655 ?
N5 C11 N6 117.6(4) . . ?
N5 C11 C12 121.9(4) . . ?
N6 C11 C12 120.5(4) . . ?
C9 C12 C11 116.5(4) . . ?
C9 C12 H12 121.8 . . ?
C11 C12 H12 121.7 . . ?
C11 N6 N7 116.3(4) . . ?
C11 N6 C13 119.7(4) . . ?
N7 N6 C13 119.3(4) . . ?
N6 C13 H13A 109.5 . . ?
N6 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N6 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 N7 N6 117.6(4) . . ?
C14 N7 Pb1 122.1(3) . 2_655 ?
N6 N7 Pb1 120.0(3) . 2_655 ?
N7 C14 C1 115.8(4) . 2_655 ?
N7 C14 C15 124.8(5) . . ?
C1 C14 C15 119.4(4) 2_655 . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C20 N8 C16 116.9(4) . . ?
C20 N8 Pb1 119.2(3) . . ?
C16 N8 Pb1 122.3(3) . . ?
N8 C16 C17 123.3(5) . . ?
N8 C16 H16 118.3 . . ?
C17 C16 H16 118.4 . . ?
C16 C17 C18 119.9(5) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C19 C18 C17 116.5(4) . . ?
C19 C18 C21 121.6(5) . . ?
C17 C18 C21 121.8(5) . . ?
C20 C19 C18 120.6(5) . . ?
C20 C19 H19 119.7 . . ?
C18 C19 H19 119.7 . . ?
N8 C20 C19 122.8(4) . . ?
N8 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
C23 C21 C22 119.2(5) 13_656 . ?
C23 C21 C18 120.6(5) 13_656 . ?
C22 C21 C18 120.2(5) . . ?
C23 C22 C21 119.5(6) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C21 C23 C22 121.2(6) 13_656 . ?
C21 C23 H23 119.4 13_656 . ?
C22 C23 H23 119.4 . . ?
O1 S1 O2 109.5(4) . . ?
O1 S1 O3 96.7(4) . . ?
O2 S1 O3 120.7(4) . . ?
O1 S1 C24A 119.3(6) . . ?
O2 S1 C24A 120.1(7) . . ?
O3 S1 C24A 86.9(7) . . ?
O1 S1 C24 92.8(6) . . ?
O2 S1 C24 91.8(6) . . ?
O3 S1 C24 140.1(6) . . ?
F1 C24 F2 105.8(12) . . ?
F1 C24 F3 100.0(11) . . ?
F2 C24 F3 99.3(12) . . ?
F1 C24 S1 129.9(13) . . ?
F2 C24 S1 114.4(11) . . ?
F3 C24 S1 101.6(11) . . ?
F3A C24A F1A 109.3(13) . . ?
F3A C24A F2A 109.4(13) . . ?
F1A C24A F2A 102.7(12) . . ?
F3A C24A S1 114.0(12) . . ?
F1A C24A S1 114.9(11) . . ?
F2A C24A S1 105.7(12) . . ?
O4 S2 O4 114.89(10) . 3_665 ?
O4 S2 O4 114.90(11) . 2_655 ?
O4 S2 O4 114.90(10) 3_665 2_655 ?
O4 S2 C25 103.27(14) . . ?
O4 S2 C25 103.27(14) 3_665 . ?
O4 S2 C25 103.27(14) 2_655 . ?
F4 C25 F4 107.7(4) 2_655 3_665 ?
F4 C25 F4 107.7(4) 2_655 . ?
F4 C25 F4 107.7(4) 3_665 . ?
F4 C25 S2 111.2(4) 2_655 . ?
F4 C25 S2 111.2(4) 3_665 . ?
F4 C25 S2 111.2(4) . . ?
F5 P1 F5 180.0(3) 11_456 2_675 ?
F5 P1 F5 91.0(2) 11_456 10_576 ?
F5 P1 F5 89.0(2) 2_675 10_576 ?
F5 P1 F5 91.0(2) 11_456 12_666 ?
F5 P1 F5 89.0(2) 2_675 12_666 ?
F5 P1 F5 91.0(2) 10_576 12_666 ?
F5 P1 F5 89.0(2) 11_456 3_465 ?
F5 P1 F5 91.0(2) 2_675 3_465 ?
F5 P1 F5 89.0(2) 10_576 3_465 ?
F5 P1 F5 180.0(3) 12_666 3_465 ?
F5 P1 F5 89.0(2) 11_456 . ?
F5 P1 F5 91.0(2) 2_675 . ?
F5 P1 F5 180.00(19) 10_576 . ?
F5 P1 F5 89.0(2) 12_666 . ?
F5 P1 F5 91.0(2) 3_465 . ?

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
C5 N1 C1 C2 0.6(8) . . . . ?
Pb1 N1 C1 C2 166.6(5) . . . . ?
C5 N1 C1 C14 179.4(5) . . . 3_665 ?
Pb1 N1 C1 C14 -14.6(7) . . . 3_665 ?
N1 C1 C2 C3 -1.0(10) . . . . ?
C14 C1 C2 C3 -179.7(6) 3_665 . . . ?
C1 C2 C3 C4 0.1(11) . . . . ?
C2 C3 C4 C5 1.0(11) . . . . ?
C1 N1 C5 C4 0.7(9) . . . . ?
Pb1 N1 C5 C4 -165.8(5) . . . . ?
C1 N1 C5 C6 -173.5(5) . . . . ?
Pb1 N1 C5 C6 19.9(7) . . . . ?
C3 C4 C5 N1 -1.5(10) . . . . ?
C3 C4 C5 C6 172.5(6) . . . . ?
N1 C5 C6 N2 14.2(8) . . . . ?
C4 C5 C6 N2 -160.1(6) . . . . ?
N1 C5 C6 C7 -166.2(6) . . . . ?
C4 C5 C6 C7 19.5(9) . . . . ?
C5 C6 N2 N3 170.6(5) . . . . ?
C7 C6 N2 N3 -8.9(9) . . . . ?
C5 C6 N2 Pb1 -38.8(6) . . . . ?
C7 C6 N2 Pb1 141.6(6) . . . . ?
C6 N2 N3 C9 133.7(5) . . . . ?
Pb1 N2 N3 C9 -13.4(6) . . . . ?
C6 N2 N3 C8 -70.2(7) . . . . ?
Pb1 N2 N3 C8 142.8(5) . . . . ?
N2 N3 C9 N4 -11.2(7) . . . . ?
C8 N3 C9 N4 -166.4(6) . . . . ?
N2 N3 C9 C12 172.0(4) . . . . ?
C8 N3 C9 C12 16.7(8) . . . . ?
N3 C9 N4 C10 -174.3(4) . . . . ?
C12 C9 N4 C10 2.4(6) . . . . ?
C9 N4 C10 N5 2.1(7) . . . . ?
N4 C10 N5 C11 -3.3(7) . . . . ?
N4 C10 N5 Pb1 -161.5(3) . . . 2_655 ?
C10 N5 C11 N6 177.8(4) . . . . ?
Pb1 N5 C11 N6 -23.3(5) 2_655 . . . ?
C10 N5 C11 C12 0.0(6) . . . . ?
Pb1 N5 C11 C12 158.8(4) 2_655 . . . ?
N4 C9 C12 C11 -5.2(7) . . . . ?
N3 C9 C12 C11 171.4(4) . . . . ?
N5 C11 C12 C9 4.0(7) . . . . ?
N6 C11 C12 C9 -173.8(4) . . . . ?
N5 C11 N6 N7 -0.6(6) . . . . ?
C12 C11 N6 N7 177.3(4) . . . . ?
N5 C11 N6 C13 155.2(4) . . . . ?
C12 C11 N6 C13 -27.0(7) . . . . ?
C11 N6 N7 C14 -148.6(5) . . . . ?
C13 N6 N7 C14 55.5(6) . . . . ?
C11 N6 N7 Pb1 24.9(5) . . . 2_655 ?
C13 N6 N7 Pb1 -130.9(4) . . . 2_655 ?
N6 N7 C14 C1 -172.6(5) . . . 2_655 ?
Pb1 N7 C14 C1 14.0(7) 2_655 . . 2_655 ?
N6 N7 C14 C15 8.7(8) . . . . ?
Pb1 N7 C14 C15 -164.7(5) 2_655 . . . ?
C20 N8 C16 C17 0.9(8) . . . . ?
Pb1 N8 C16 C17 -164.4(5) . . . . ?
N8 C16 C17 C18 -0.4(10) . . . . ?
C16 C17 C18 C19 -0.4(9) . . . . ?
C16 C17 C18 C21 178.7(6) . . . . ?
C17 C18 C19 C20 0.7(8) . . . . ?
C21 C18 C19 C20 -178.4(5) . . . . ?
C16 N8 C20 C19 -0.6(7) . . . . ?
Pb1 N8 C20 C19 165.2(4) . . . . ?
C18 C19 C20 N8 -0.2(8) . . . . ?
C19 C18 C21 C23 32.3(9) . . . 13_656 ?
C17 C18 C21 C23 -146.8(6) . . . 13_656 ?
C19 C18 C21 C22 -148.6(6) . . . . ?
C17 C18 C21 C22 32.3(9) . . . . ?
C23 C21 C22 C23 -0.2(11) 13_656 . . . ?
C18 C21 C22 C23 -179.3(6) . . . . ?
C21 C22 C23 C21 0.2(11) . . . 13_656 ?
O1 S1 C24 F1 33.8(14) . . . . ?
O2 S1 C24 F1 -75.8(14) . . . . ?
O3 S1 C24 F1 137.6(12) . . . . ?
O1 S1 C24 F2 174.2(12) . . . . ?
O2 S1 C24 F2 64.5(12) . . . . ?
O3 S1 C24 F2 -82.0(14) . . . . ?
O1 S1 C24 F3 -79.9(9) . . . . ?
O2 S1 C24 F3 170.5(9) . . . . ?
O3 S1 C24 F3 23.9(14) . . . . ?
O1 S1 C24A F3A -157.4(11) . . . . ?
O2 S1 C24A F3A 62.6(16) . . . . ?
O3 S1 C24A F3A -61.5(13) . . . . ?
O1 S1 C24A F1A -30.1(17) . . . . ?
O2 S1 C24A F1A -170.1(10) . . . . ?
O3 S1 C24A F1A 65.9(13) . . . . ?
O1 S1 C24A F2A 82.5(11) . . . . ?
O2 S1 C24A F2A -57.6(11) . . . . ?
O3 S1 C24A F2A 178.4(10) . . . . ?
O4 S2 C25 F4 -68.4(2) . . . 2_655 ?
O4 S2 C25 F4 51.6(2) 3_665 . . 2_655 ?
O4 S2 C25 F4 171.6(2) 2_655 . . 2_655 ?
O4 S2 C25 F4 51.6(2) . . . 3_665 ?
O4 S2 C25 F4 171.6(2) 3_665 . . 3_665 ?
O4 S2 C25 F4 -68.4(2) 2_655 . . 3_665 ?
O4 S2 C25 F4 171.6(2) . . . . ?
O4 S2 C25 F4 -68.4(2) 3_665 . . . ?
O4 S2 C25 F4 51.6(2) 2_655 . . . ?

_refine_diff_density_max         2.434
_refine_diff_density_min         -2.162
_refine_diff_density_rms         0.112



####################################################################### 
# 
# 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_2c
_database_code_depnum_ccdc_archive 'CCDC 2285236'
loop_
_audit_author_name
_audit_author_address
'Andreas Eichhoefer'
;Institute of Nanotechnology, KIT
Germany
;
_audit_update_record             
;
2023-11-02 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/3
_shelx_SHELXL_version_number     2019/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C126 H132 N48 Pb6, 9(C F3 O3 S), 6(C F1.5 O1.5 S0.5)'
_chemical_formula_sum            'C141 H132 F36 N48 O36 Pb6 S12'
_chemical_formula_weight         5386.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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'
F F 0.0600 0.0411 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.2612 7.2060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.2924 0.4248 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+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                   21.1054(2)
_cell_length_b                   21.1054(2)
_cell_length_c                   51.1319(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     19724.7(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    61587
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      62.14

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_F_000             7830
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    6.185
_shelx_estimated_absorpt_T_min   0.524
_shelx_estimated_absorpt_T_max   0.577
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_T_max  0.577
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.34143
_diffrn_radiation_type           GaK\a
_diffrn_source                   ?
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            93267
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_theta_min         2.233
_diffrn_reflns_theta_max         64.473
_diffrn_reflns_theta_full        53.597
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11021
_reflns_number_gt                7300
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/3(Sheldrick, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11021
_refine_ls_number_parameters     409
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0800
_refine_ls_wR_factor_ref         0.2730
_refine_ls_wR_factor_gt          0.2498
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.54415(2) 0.83128(2) 0.46221(2) 0.06291(16) Uani 1 1 d . . . A 43
N1 N 0.6787(5) 0.9370(4) 0.46378(14) 0.0754(19) Uani 1 1 d . . . A 43
N2 N 0.6526(4) 0.8022(4) 0.45175(16) 0.0759(19) Uani 1 1 d . . . A 43
N3 N 0.6369(4) 0.7342(4) 0.44222(16) 0.0748(19) Uani 1 1 d . . . A 43
N5 N 0.4372(4) 0.5650(4) 0.46242(14) 0.0669(17) Uani 1 1 d . . . B 43
N6 N 0.4651(4) 0.4817(4) 0.44484(17) 0.0743(19) Uani 1 1 d . . . C 43
N7 N 0.3934(4) 0.4260(4) 0.45262(16) 0.077(2) Uani 1 1 d . . . C 43
C16A C 0.6201(11) 0.9152(10) 0.4033(4) 0.0675(12) Uiso 0.5 1 d . . P D 1
H16A H 0.632356 0.957095 0.413708 0.081 Uiso 0.5 1 calc R U P D 1
N8A N 0.5688(11) 0.8492(10) 0.4125(4) 0.0675(12) Uiso 0.5 1 d . . P D 1
C20A C 0.5519(11) 0.7939(10) 0.4000(4) 0.0675(12) Uiso 0.5 1 d . . P D 1
H20A H 0.517611 0.748049 0.407365 0.081 Uiso 0.5 1 calc R U P D 1
C19A C 0.5829(10) 0.7952(10) 0.3736(3) 0.0675(12) Uiso 0.5 1 d D . P D 1
H19A H 0.567525 0.752796 0.363054 0.081 Uiso 0.5 1 calc R U P D 1
C18A C 0.6314(10) 0.8581(10) 0.3667(3) 0.0675(12) Uiso 0.5 1 d D . P D 1
C17A C 0.6554(10) 0.9255(10) 0.3799(4) 0.0675(12) Uiso 0.5 1 d . . P D 1
H17A H 0.691237 0.971800 0.373261 0.081 Uiso 0.5 1 calc R U P D 1
C1 C 0.6331(9) 1.0867(7) 0.4756(4) 0.135(6) Uani 1 1 d . . . . .
H1A H 0.663108 1.127591 0.463846 0.203 Uiso 1 1 calc R U . . .
H1B H 0.655618 1.096988 0.492993 0.203 Uiso 1 1 calc R U . . .
H1C H 0.583976 1.080588 0.476885 0.203 Uiso 1 1 calc R U . . .
C2 C 0.6276(6) 1.0165(5) 0.4648(2) 0.084(3) Uani 1 1 d . . . . .
C3 C 0.6879(6) 1.0019(6) 0.46837(19) 0.083(3) Uani 1 1 d . . . . .
C4 C 0.7599(6) 1.0646(6) 0.4761(2) 0.096(3) Uani 1 1 d . . . . .
H4 H 0.766748 1.110865 0.481192 0.115 Uiso 1 1 calc R U . . .
C5 C 0.8202(8) 1.0476(7) 0.4749(3) 0.122(5) Uani 1 1 d . . . . .
H5 H 0.869120 1.085300 0.477904 0.146 Uiso 1 1 calc R U . . .
C6 C 0.8066(6) 0.9810(7) 0.4698(2) 0.099(3) Uani 1 1 d . . . . .
H6 H 0.845768 0.971041 0.469915 0.118 Uiso 1 1 calc R U . . .
C7 C 0.7351(5) 0.9236(6) 0.46398(18) 0.081(2) Uani 1 1 d . . . . .
C8 C 0.7221(5) 0.8499(6) 0.45701(19) 0.081(3) Uani 1 1 d . . . . .
C9 C 0.5708(5) 0.6783(5) 0.44841(18) 0.072(2) Uani 1 1 d . . . . .
C10 C 0.5519(5) 0.6091(5) 0.4408(2) 0.079(2) Uani 1 1 d . . . . .
H10 H 0.583611 0.600115 0.430208 0.095 Uiso 1 1 calc R U . . .
C11 C 0.4836(5) 0.5514(5) 0.4490(2) 0.075(2) Uani 1 1 d . . . . .
N12 N 0.5255(4) 0.6920(4) 0.46247(15) 0.0732(18) Uani 1 1 d . . . . .
C13 C 0.4990(7) 0.4570(6) 0.4266(3) 0.120(5) Uani 1 1 d . . . . .
H13A H 0.472002 0.403412 0.426022 0.180 Uiso 1 1 calc R U . C 43
H13B H 0.549598 0.474161 0.432045 0.180 Uiso 1 1 calc R U . C 43
H13C H 0.498888 0.476445 0.409223 0.180 Uiso 1 1 calc R U . C 43
C14 C 0.7800(6) 0.8297(7) 0.4577(3) 0.096(3) Uani 1 1 d . . . . .
H14A H 0.800275 0.837084 0.475374 0.143 Uiso 1 1 calc R U . . .
H14B H 0.818899 0.860465 0.445349 0.143 Uiso 1 1 calc R U . . .
H14C H 0.758998 0.778187 0.452736 0.143 Uiso 1 1 calc R U . . .
C15 C 0.6765(6) 0.7326(6) 0.4192(2) 0.089(3) Uani 1 1 d . . . . .
H15A H 0.642071 0.696915 0.406677 0.133 Uiso 1 1 calc R U . A 43
H15B H 0.712559 0.718507 0.424366 0.133 Uiso 1 1 calc R U . A 43
H15C H 0.701715 0.781178 0.411154 0.133 Uiso 1 1 calc R U . A 43
C21 C 0.6422(15) 0.8157(16) 0.3377(4) 0.148(10) Uiso 0.65 1 d D . P E 2
H21 H 0.608059 0.772952 0.328511 0.177 Uiso 0.65 1 calc R U P E 2
S1 S 0.333333 0.666667 0.43017(8) 0.0742(9) Uani 1 3 d S T P . .
F1 F 0.2671(4) 0.6218(4) 0.38519(14) 0.114(2) Uani 1 1 d . . . . .
O1 O 0.4070(3) 0.7228(4) 0.43695(14) 0.0812(17) Uani 1 1 d . . . . .
C22 C 0.333333 0.666667 0.3953(4) 0.093(5) Uani 1 3 d S T P . .
S2 S 1.000000 1.000000 0.500000 0.0545(10) Uani 1 6 d S T P . .
F2 F 0.9546(5) 0.9344(5) 0.4529(2) 0.080(3) Uani 0.5 1 d . . P . .
O2 O 0.9445(5) 0.9256(5) 0.4948(2) 0.063(3) Uani 0.5 1 d . . P . .
C23 C 1.000000 1.000000 0.4618(6) 0.062(6) Uani 0.5 3 d S T P . .
S3 S 0.29378(17) 0.4290(2) 0.52981(5) 0.1044(10) Uani 1 1 d . . . . .
F3 F 0.2457(5) 0.5037(7) 0.5538(2) 0.181(5) Uani 1 1 d . . . . .
F4 F 0.3590(6) 0.5546(8) 0.5527(2) 0.195(6) Uani 1 1 d . . . . .
F5 F 0.3007(7) 0.5542(6) 0.5175(3) 0.177(4) Uani 1 1 d . . . . .
O3 O 0.3620(4) 0.4529(6) 0.51582(17) 0.1125(16) Uani 1 1 d . . . . .
O4 O 0.2313(4) 0.4023(6) 0.51377(16) 0.1125(16) Uani 1 1 d . . . . .
O5 O 0.2916(4) 0.4001(6) 0.55433(17) 0.1125(16) Uani 1 1 d . . . . .
C24 C 0.3027(8) 0.5195(10) 0.5400(3) 0.125(5) Uani 1 1 d . . . . .
S25 S 0.5352(6) 0.5709(5) 0.34593(17) 0.149(3) Uani 0.5 1 d D . P . .
F6 F 0.414(3) 0.525(3) 0.3740(7) 0.234(10) Uiso 0.25 1 d D . P . .
F7 F 0.395(3) 0.469(2) 0.3374(10) 0.234(10) Uiso 0.25 1 d D . P . .
F8 F 0.410(3) 0.578(3) 0.3388(10) 0.234(10) Uiso 0.25 1 d D . P . .
F9 F 0.668(3) 0.6847(19) 0.3444(10) 0.234(10) Uiso 0.25 1 d D . P . .
F10 F 0.657(4) 0.594(3) 0.3685(7) 0.234(10) Uiso 0.25 1 d D . P . .
F11 F 0.665(3) 0.590(3) 0.3260(8) 0.234(10) Uiso 0.25 1 d D . P . .
O6 O 0.5497(15) 0.6154(15) 0.3687(6) 0.195(6) Uiso 0.5 1 d D . P . .
O7 O 0.5219(15) 0.4902(15) 0.3456(7) 0.195(6) Uiso 0.5 1 d D . P . .
O8 O 0.5345(14) 0.5978(17) 0.3173(6) 0.195(6) Uiso 0.5 1 d D . P . .
C25 C 0.6396(10) 0.6124(17) 0.3459(7) 0.179(11) Uiso 0.5 1 d D . P . .
C26 C 0.4329(11) 0.5341(18) 0.3494(7) 0.179(11) Uiso 0.5 1 d D . P . .
C21A C 0.6644(9) 0.8048(6) 0.3266(2) 0.040(3) Uiso 0.35 1 d D . P F 1
H21A H 0.635499 0.757641 0.334098 0.048 Uiso 0.35 1 calc R U P F 1
C12 C 0.4600(4) 0.6338(5) 0.46785(16) 0.0637(18) Uani 1 1 d . . . . .
H12 H 0.426151 0.643561 0.476651 0.076 Uiso 1 1 calc R U . B 43
C19 C 0.5618(10) 0.7639(10) 0.3772(4) 0.0675(12) Uiso 0.5 1 d . . P E 2
H19 H 0.540070 0.718605 0.368092 0.081 Uiso 0.5 1 calc R U P E 2
C17 C 0.6429(10) 0.8910(11) 0.3798(4) 0.0675(12) Uiso 0.5 1 d . . P E 2
H17 H 0.676744 0.936505 0.372055 0.081 Uiso 0.5 1 calc R U P E 2
C20 C 0.5389(11) 0.7690(10) 0.4009(4) 0.0675(12) Uiso 0.5 1 d . . P E 2
H20 H 0.499941 0.726103 0.408515 0.081 Uiso 0.5 1 calc R U P E 2
C18 C 0.6220(11) 0.8307(10) 0.3656(3) 0.0675(12) Uiso 0.5 1 d D . P E 2
N8 N 0.5688(11) 0.8338(9) 0.4153(4) 0.0675(12) Uiso 0.5 1 d . . P E 2
C16 C 0.6192(11) 0.8920(10) 0.4043(4) 0.0675(12) Uiso 0.5 1 d . . P E 2
H16 H 0.640476 0.936985 0.413618 0.081 Uiso 0.5 1 calc R U P E 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 N1 2.590(8) . ?
Pb1 N7 2.661(8) 2_665 ?
Pb1 N2 2.703(8) . ?
Pb1 N12 2.763(8) . ?
N1 C3 1.305(13) . ?
N1 C7 1.353(13) . ?
N2 C8 1.327(12) . ?
N2 N3 1.389(10) . ?
N3 C9 1.339(12) . ?
N3 C15 1.452(12) . ?
N5 C12 1.310(11) . ?
N5 C11 1.341(10) . ?
N6 C11 1.336(11) . ?
N6 C13 1.424(12) . ?
N6 N7 1.432(11) . ?
N7 C2 1.254(13) 3_565 ?
C16A N8A 1.35(3) . ?
C16A C17A 1.37(3) . ?
C16A H16A 0.9500 . ?
N8A C20A 1.22(3) . ?
C20A C19A 1.50(3) . ?
C20A H20A 0.9500 . ?
C19A C18A 1.25(2) . ?
C19A H19A 0.9500 . ?
C18A C17A 1.42(2) . ?
C18A C21A 1.558(9) 16_665 ?
C17A H17A 0.9500 . ?
C1 C2 1.531(14) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.463(16) . ?
C3 C4 1.484(15) . ?
C4 C5 1.49(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.312(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.415(14) . ?
C6 H6 0.9500 . ?
C7 C8 1.482(15) . ?
C8 C14 1.482(15) . ?
C9 N12 1.340(11) . ?
C9 C10 1.365(12) . ?
C10 C11 1.407(14) . ?
C10 H10 0.9500 . ?
N12 C12 1.341(11) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C21 C21 1.02(5) 16_665 ?
C21 C18 1.569(10) . ?
C21 H21 0.9500 . ?
S1 O1 1.449(6) 2_665 ?
S1 O1 1.449(6) 3_565 ?
S1 O1 1.449(6) . ?
S1 C22 1.78(2) . ?
F1 C22 1.340(10) . ?
S2 O2 1.439(9) 10_776 ?
S2 O2 1.439(9) 11_566 ?
S2 O2 1.439(9) 2_765 ?
S2 O2 1.439(9) 12_656 ?
S2 O2 1.439(9) 3_675 ?
S2 O2 1.439(9) . ?
S2 C23 1.95(3) 10_776 ?
S2 C23 1.95(3) . ?
F2 C23 1.310(14) . ?
O2 O2 1.511(12) 11_566 ?
O2 O2 1.511(12) 12_656 ?
S3 O5 1.385(9) . ?
S3 O4 1.410(9) . ?
S3 O3 1.453(8) . ?
S3 C24 1.896(17) . ?
F3 C24 1.287(18) . ?
F4 C24 1.226(16) . ?
F5 C24 1.37(2) . ?
S25 O6 1.43(3) . ?
S25 O8 1.57(3) . ?
S25 O7 1.58(3) . ?
S25 C26 1.902(17) . ?
S25 C25 1.920(17) . ?
F6 C26 1.306(19) . ?
F7 C26 1.34(2) . ?
F8 C26 1.342(19) . ?
F9 C25 1.333(19) . ?
F10 C25 1.327(19) . ?
F11 C25 1.343(19) . ?
C21A C21A 1.349(17) 16_665 ?
C21A H21A 0.9500 . ?
C12 H12 0.9500 . ?
C19 C20 1.33(3) . ?
C19 C18 1.47(3) . ?
C19 H19 0.9500 . ?
C17 C18 1.33(3) . ?
C17 C16 1.35(3) . ?
C17 H17 0.9500 . ?
C20 N8 1.39(3) . ?
C20 H20 0.9500 . ?
N8 C16 1.28(3) . ?
C16 H16 0.9500 . ?

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
N1 Pb1 N2 60.9(2) . . ?
N7 Pb1 N2 116.0(2) 2_665 . ?
N1 Pb1 N12 115.3(2) . . ?
N7 Pb1 N12 168.5(2) 2_665 . ?
N2 Pb1 N12 56.4(2) . . ?
C3 N1 C7 122.1(9) . . ?
C3 N1 Pb1 115.7(7) . . ?
C7 N1 Pb1 121.4(6) . . ?
C8 N2 N3 117.2(8) . . ?
C8 N2 Pb1 121.8(7) . . ?
N3 N2 Pb1 120.8(5) . . ?
C9 N3 N2 115.6(7) . . ?
C9 N3 C15 121.9(8) . . ?
N2 N3 C15 117.8(8) . . ?
C12 N5 C11 116.3(8) . . ?
C11 N6 C13 125.7(9) . . ?
C11 N6 N7 117.8(7) . . ?
C13 N6 N7 113.6(8) . . ?
C2 N7 N6 116.8(8) 3_565 . ?
C2 N7 Pb1 115.4(8) 3_565 3_565 ?
N8A C16A C17A 124.0(18) . . ?
N8A C16A H16A 118.0 . . ?
C17A C16A H16A 118.0 . . ?
C20A N8A C16A 120(2) . . ?
N8A C20A C19A 122.8(18) . . ?
N8A C20A H20A 118.6 . . ?
C19A C20A H20A 118.6 . . ?
C18A C19A C20A 112.8(16) . . ?
C18A C19A H19A 123.6 . . ?
C20A C19A H19A 123.6 . . ?
C19A C18A C17A 128.5(15) . . ?
C19A C18A C21A 115.0(15) . 16_665 ?
C17A C18A C21A 116.5(13) . 16_665 ?
C16A C17A C18A 111.3(16) . . ?
C16A C17A H17A 124.4 . . ?
C18A C17A H17A 124.4 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N7 C2 C3 114.1(9) 2_665 . ?
N7 C2 C1 125.4(12) 2_665 . ?
C3 C2 C1 120.5(11) . . ?
N1 C3 C2 120.6(9) . . ?
N1 C3 C4 122.2(11) . . ?
C2 C3 C4 117.1(10) . . ?
C3 C4 C5 113.1(10) . . ?
C3 C4 H4 123.5 . . ?
C5 C4 H4 123.5 . . ?
C6 C5 C4 120.8(11) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 121.8(13) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
N1 C7 C6 119.7(11) . . ?
N1 C7 C8 119.8(8) . . ?
C6 C7 C8 120.4(11) . . ?
N2 C8 C14 122.9(10) . . ?
N2 C8 C7 113.6(9) . . ?
C14 C8 C7 123.4(9) . . ?
N3 C9 N12 118.6(8) . . ?
N3 C9 C10 119.6(8) . . ?
N12 C9 C10 121.8(9) . . ?
C9 C10 C11 117.8(8) . . ?
C9 C10 H10 121.1 . . ?
C11 C10 H10 121.1 . . ?
N6 C11 N5 118.4(9) . . ?
N6 C11 C10 120.9(8) . . ?
N5 C11 C10 120.6(8) . . ?
C9 N12 C12 115.6(7) . . ?
C9 N12 Pb1 119.4(6) . . ?
C12 N12 Pb1 120.7(5) . . ?
N6 C13 H13A 109.5 . . ?
N6 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N6 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C8 C14 H14A 109.5 . . ?
C8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 C21 C18 122(4) 16_665 . ?
C21 C21 H21 119.2 16_665 . ?
C18 C21 H21 119.2 . . ?
O1 S1 O1 114.5(2) 2_665 3_565 ?
O1 S1 O1 114.5(2) 2_665 . ?
O1 S1 O1 114.5(2) 3_565 . ?
O1 S1 C22 103.8(3) 2_665 . ?
O1 S1 C22 103.8(3) 3_565 . ?
O1 S1 C22 103.8(3) . . ?
F1 C22 F1 106.0(9) . 3_565 ?
F1 C22 F1 106.0(9) . 2_665 ?
F1 C22 F1 106.0(9) 3_565 2_665 ?
F1 C22 S1 112.8(8) . . ?
F1 C22 S1 112.8(8) 3_565 . ?
F1 C22 S1 112.8(8) 2_665 . ?
O2 S2 O2 116.7(3) 10_776 11_566 ?
O2 S2 O2 63.3(3) 10_776 2_765 ?
O2 S2 O2 180.0(10) 11_566 2_765 ?
O2 S2 O2 116.7(3) 10_776 12_656 ?
O2 S2 O2 116.7(3) 11_566 12_656 ?
O2 S2 O2 63.3(3) 2_765 12_656 ?
O2 S2 O2 63.3(3) 10_776 3_675 ?
O2 S2 O2 63.3(3) 11_566 3_675 ?
O2 S2 O2 116.7(3) 2_765 3_675 ?
O2 S2 O2 180.0(10) 12_656 3_675 ?
O2 S2 O2 180.0(8) 10_776 . ?
O2 S2 O2 63.3(3) 11_566 . ?
O2 S2 O2 116.7(3) 2_765 . ?
O2 S2 O2 63.4(3) 12_656 . ?
O2 S2 O2 116.6(3) 3_675 . ?
O2 S2 C23 79.3(5) 10_776 10_776 ?
O2 S2 C23 79.3(5) 11_566 10_776 ?
O2 S2 C23 100.7(5) 2_765 10_776 ?
O2 S2 C23 79.3(5) 12_656 10_776 ?
O2 S2 C23 100.7(5) 3_675 10_776 ?
O2 S2 C23 100.7(5) . 10_776 ?
O2 S2 C23 100.7(5) 10_776 . ?
O2 S2 C23 100.7(5) 11_566 . ?
O2 S2 C23 79.3(5) 2_765 . ?
O2 S2 C23 100.7(5) 12_656 . ?
O2 S2 C23 79.3(5) 3_675 . ?
O2 S2 C23 79.3(5) . . ?
C23 S2 C23 180.000(14) 10_776 . ?
S2 O2 O2 58.33(15) . 11_566 ?
S2 O2 O2 58.32(15) . 12_656 ?
O2 O2 O2 108.3(9) 11_566 12_656 ?
F2 C23 F2 108.6(15) . 2_765 ?
F2 C23 F2 108.6(15) . 3_675 ?
F2 C23 F2 108.6(15) 2_765 3_675 ?
F2 C23 S2 110.4(14) . . ?
F2 C23 S2 110.4(14) 2_765 . ?
F2 C23 S2 110.4(14) 3_675 . ?
O5 S3 O4 122.2(6) . . ?
O5 S3 O3 114.0(5) . . ?
O4 S3 O3 114.8(5) . . ?
O5 S3 C24 99.2(7) . . ?
O4 S3 C24 99.4(7) . . ?
O3 S3 C24 101.8(7) . . ?
F4 C24 F3 111.2(14) . . ?
F4 C24 F5 113.7(18) . . ?
F3 C24 F5 108.8(14) . . ?
F4 C24 S3 109.4(13) . . ?
F3 C24 S3 106.3(13) . . ?
F5 C24 S3 107.1(10) . . ?
O6 S25 O8 123.8(19) . . ?
O6 S25 O7 125.6(18) . . ?
O8 S25 O7 110.5(19) . . ?
O6 S25 C26 91.1(14) . . ?
O8 S25 C26 91.1(13) . . ?
O7 S25 C26 90.4(13) . . ?
O6 S25 C25 83.1(13) . . ?
O8 S25 C25 92.9(13) . . ?
O7 S25 C25 92.2(13) . . ?
C26 S25 C25 174.1(15) . . ?
F10 C25 F9 111(2) . . ?
F10 C25 F11 110(2) . . ?
F9 C25 F11 109(2) . . ?
F10 C25 S25 107(3) . . ?
F9 C25 S25 106(3) . . ?
F11 C25 S25 114(4) . . ?
F6 C26 F7 108(2) . . ?
F6 C26 F8 108(2) . . ?
F7 C26 F8 106(2) . . ?
F6 C26 S25 111(4) . . ?
F7 C26 S25 111(4) . . ?
F8 C26 S25 114(4) . . ?
C21A C21A C18A 126.4(17) 16_665 16_665 ?
C21A C21A H21A 116.8 16_665 . ?
C18A C21A H21A 116.8 16_665 . ?
N5 C12 N12 127.7(7) . . ?
N5 C12 H12 116.1 . . ?
N12 C12 H12 116.1 . . ?
C20 C19 C18 117.7(17) . . ?
C20 C19 H19 121.2 . . ?
C18 C19 H19 121.2 . . ?
C18 C17 C16 124.7(18) . . ?
C18 C17 H17 117.6 . . ?
C16 C17 H17 117.6 . . ?
C19 C20 N8 123.7(18) . . ?
C19 C20 H20 118.1 . . ?
N8 C20 H20 118.1 . . ?
C17 C18 C19 114.3(16) . . ?
C17 C18 C21 134(2) . . ?
C19 C18 C21 111.5(16) . . ?
C16 N8 C20 117.4(19) . . ?
N8 C16 C17 121.7(19) . . ?
N8 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?

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
C8 N2 N3 C9 149.7(9) . . . . ?
Pb1 N2 N3 C9 -26.1(11) . . . . ?
C8 N2 N3 C15 -54.1(12) . . . . ?
Pb1 N2 N3 C15 130.1(7) . . . . ?
C11 N6 N7 C2 -134.3(9) . . . 3_565 ?
C13 N6 N7 C2 63.9(13) . . . 3_565 ?
C11 N6 N7 Pb1 17.2(11) . . . 3_565 ?
C13 N6 N7 Pb1 -144.5(9) . . . 3_565 ?
C17A C16A N8A C20A 1(3) . . . . ?
C16A N8A C20A C19A -3(3) . . . . ?
N8A C20A C19A C18A 5(3) . . . . ?
C20A C19A C18A C17A -5(3) . . . . ?
C20A C19A C18A C21A 176.5(16) . . . 16_665 ?
N8A C16A C17A C18A 0(3) . . . . ?
C19A C18A C17A C16A 3(3) . . . . ?
C21A C18A C17A C16A -178.4(16) 16_665 . . . ?
C7 N1 C3 C2 172.4(9) . . . . ?
Pb1 N1 C3 C2 -17.8(12) . . . . ?
C7 N1 C3 C4 -4.6(15) . . . . ?
Pb1 N1 C3 C4 165.2(8) . . . . ?
N7 C2 C3 N1 -13.1(14) 2_665 . . . ?
C1 C2 C3 N1 166.9(11) . . . . ?
N7 C2 C3 C4 164.0(9) 2_665 . . . ?
C1 C2 C3 C4 -16.0(16) . . . . ?
N1 C3 C4 C5 6.6(15) . . . . ?
C2 C3 C4 C5 -170.5(10) . . . . ?
C3 C4 C5 C6 -5.7(18) . . . . ?
C4 C5 C6 C7 3(2) . . . . ?
C3 N1 C7 C6 1.1(14) . . . . ?
Pb1 N1 C7 C6 -168.2(7) . . . . ?
C3 N1 C7 C8 -176.2(8) . . . . ?
Pb1 N1 C7 C8 14.5(12) . . . . ?
C5 C6 C7 N1 -0.2(18) . . . . ?
C5 C6 C7 C8 177.0(12) . . . . ?
N3 N2 C8 C14 -11.1(14) . . . . ?
Pb1 N2 C8 C14 164.6(8) . . . . ?
N3 N2 C8 C7 173.0(8) . . . . ?
Pb1 N2 C8 C7 -11.3(11) . . . . ?
N1 C7 C8 N2 -1.8(13) . . . . ?
C6 C7 C8 N2 -179.1(9) . . . . ?
N1 C7 C8 C14 -177.6(10) . . . . ?
C6 C7 C8 C14 5.1(16) . . . . ?
N2 N3 C9 N12 1.4(13) . . . . ?
C15 N3 C9 N12 -153.7(9) . . . . ?
N2 N3 C9 C10 -177.4(9) . . . . ?
C15 N3 C9 C10 27.5(14) . . . . ?
N3 C9 C10 C11 176.2(9) . . . . ?
N12 C9 C10 C11 -2.5(15) . . . . ?
C13 N6 C11 N5 165.6(11) . . . . ?
N7 N6 C11 N5 6.3(13) . . . . ?
C13 N6 C11 C10 -17.6(16) . . . . ?
N7 N6 C11 C10 -176.9(9) . . . . ?
C12 N5 C11 N6 174.8(8) . . . . ?
C12 N5 C11 C10 -2.0(13) . . . . ?
C9 C10 C11 N6 -172.2(9) . . . . ?
C9 C10 C11 N5 4.5(14) . . . . ?
N3 C9 N12 C12 179.6(9) . . . . ?
C10 C9 N12 C12 -1.7(13) . . . . ?
N3 C9 N12 Pb1 22.9(11) . . . . ?
C10 C9 N12 Pb1 -158.3(8) . . . . ?
O1 S1 C22 F1 -54.8(5) 2_665 . . . ?
O1 S1 C22 F1 65.2(5) 3_565 . . . ?
O1 S1 C22 F1 -174.8(5) . . . . ?
O1 S1 C22 F1 65.2(5) 2_665 . . 3_565 ?
O1 S1 C22 F1 -174.8(5) 3_565 . . 3_565 ?
O1 S1 C22 F1 -54.8(5) . . . 3_565 ?
O1 S1 C22 F1 -174.8(5) 2_665 . . 2_665 ?
O1 S1 C22 F1 -54.8(5) 3_565 . . 2_665 ?
O1 S1 C22 F1 65.2(5) . . . 2_665 ?
O2 S2 O2 O2 180.000(1) 2_765 . . 11_566 ?
O2 S2 O2 O2 144.4(15) 12_656 . . 11_566 ?
O2 S2 O2 O2 -35.6(15) 3_675 . . 11_566 ?
C23 S2 O2 O2 72.2(8) 10_776 . . 11_566 ?
C23 S2 O2 O2 -107.8(8) . . . 11_566 ?
O2 S2 O2 O2 -144.4(15) 11_566 . . 12_656 ?
O2 S2 O2 O2 35.6(15) 2_765 . . 12_656 ?
O2 S2 O2 O2 180.000(2) 3_675 . . 12_656 ?
C23 S2 O2 O2 -72.2(8) 10_776 . . 12_656 ?
C23 S2 O2 O2 107.8(8) . . . 12_656 ?
O5 S3 C24 F4 60.4(15) . . . . ?
O4 S3 C24 F4 -174.6(14) . . . . ?
O3 S3 C24 F4 -56.7(16) . . . . ?
O5 S3 C24 F3 -59.7(12) . . . . ?
O4 S3 C24 F3 65.3(12) . . . . ?
O3 S3 C24 F3 -176.8(10) . . . . ?
O5 S3 C24 F5 -176.0(10) . . . . ?
O4 S3 C24 F5 -51.0(11) . . . . ?
O3 S3 C24 F5 66.9(11) . . . . ?
C11 N5 C12 N12 -2.7(14) . . . . ?
C9 N12 C12 N5 4.6(14) . . . . ?
Pb1 N12 C12 N5 161.0(7) . . . . ?
C18 C19 C20 N8 0(3) . . . . ?
C16 C17 C18 C19 9(3) . . . . ?
C16 C17 C18 C21 -179(2) . . . . ?
C20 C19 C18 C17 -5(3) . . . . ?
C20 C19 C18 C21 -179(2) . . . . ?
C21 C21 C18 C17 25(6) 16_665 . . . ?
C21 C21 C18 C19 -162(5) 16_665 . . . ?
C19 C20 N8 C16 3(3) . . . . ?
C20 N8 C16 C17 0(3) . . . . ?
C18 C17 C16 N8 -6(3) . . . . ?

_refine_diff_density_max         3.155
_refine_diff_density_min         -3.416
_refine_diff_density_rms         0.221

####################################################################### 
# 
# 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_1PF6
_database_code_depnum_ccdc_archive 'CCDC 2293672'
loop_
_audit_author_name
_audit_author_address
'Nathalie Gruber'
;Univ Strasbourg
France
;
_audit_update_record             
;
2023-09-07 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C128 H126 F24 N48 O24 Pb6 S8, 3(C F3 O3 S), F6 P,solvent'
_chemical_formula_sum            'C131 H126 F39 N48 O33 P Pb6 S11, solvent'
_chemical_formula_weight         5268.56

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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   21.0367(9)
_cell_length_b                   21.0367(9)
_cell_length_c                   31.8231(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     12196.3(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9884
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      26.64

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_F_000             5092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    4.317
_shelx_estimated_absorpt_T_min   0.583
_shelx_estimated_absorpt_T_max   0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6033
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            216465
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.936
_diffrn_reflns_theta_max         27.908
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9913
_reflns_number_gt                7225
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0615P)²+190.2079P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9913
_refine_ls_number_parameters     365
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0789
_refine_ls_wR_factor_ref         0.2101
_refine_ls_wR_factor_gt          0.1945
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.003

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 0.82875(2) 0.28173(2) 0.56153(2) 0.04695(14) Uani 1 1 d . . . . .
N1 N 0.6877(5) 0.1638(5) 0.5604(3) 0.053(2) Uani 1 1 d . . . . .
N2 N 0.7313(5) 0.0951(5) 0.5940(3) 0.052(2) Uani 1 1 d . . . . .
N3 N 0.7991(5) 0.1468(5) 0.5792(3) 0.049(2) Uani 1 1 d . . . . .
N4 N 0.9332(5) 0.2516(5) 0.5597(3) 0.054(2) Uani 1 1 d . . . . .
N5 N 0.9661(5) 0.3888(5) 0.5775(3) 0.052(2) Uani 1 1 d . . . . .
N6 N 0.9860(5) 0.4613(5) 0.5892(4) 0.060(2) Uani 1 1 d . . . . .
N7 N 0.8740(5) 0.4349(5) 0.5588(3) 0.051(2) Uani 1 1 d . . . . .
N8 N 0.8381(5) 0.2732(5) 0.6392(3) 0.055(2) Uani 1 1 d . . . . .
C1 C 0.6306(6) 0.1716(6) 0.5504(3) 0.051(2) Uani 1 1 d . . . . .
H1 H 0.641280 0.215090 0.535639 0.061 Uiso 1 1 calc R U . . .
C2 C 0.6738(6) 0.1056(6) 0.5842(4) 0.052(2) Uani 1 1 d . . . . .
C3 C 0.8447(6) 0.1238(6) 0.5714(4) 0.056(3) Uani 1 1 d . . . . .
C4 C 0.9204(6) 0.1824(7) 0.5598(4) 0.058(3) Uani 1 1 d . . . . .
C5 C 0.9751(7) 0.1658(7) 0.5504(5) 0.076(4) Uani 1 1 d . . . . .
H5 H 0.964695 0.116338 0.550085 0.091 Uiso 1 1 calc R U . . .
C6 C 1.0445(8) 0.2226(9) 0.5417(6) 0.095(5) Uani 1 1 d . . . . .
H6 H 1.082645 0.212392 0.535311 0.114 Uiso 1 1 calc R U . . .
C7 C 1.0591(7) 0.2943(8) 0.5421(5) 0.081(4) Uani 1 1 d . . . . .
H7 H 1.106765 0.333905 0.536000 0.097 Uiso 1 1 calc R U . . .
C8 C 1.0024(6) 0.3064(7) 0.5516(4) 0.059(3) Uani 1 1 d . . . . .
C9 C 1.0161(6) 0.3836(7) 0.5577(4) 0.064(3) Uani 1 1 d . . . . .
C10 C 0.9341(6) 0.4812(6) 0.5825(4) 0.052(2) Uani 1 1 d . . . . .
C11 C 0.9449(6) 0.5487(6) 0.5972(4) 0.059(3) Uani 1 1 d . . . . .
H11 H 0.984868 0.579357 0.615001 0.070 Uiso 1 1 calc R U . . .
C12 C 0.7276(6) 0.0535(6) 0.6326(4) 0.062(3) Uani 1 1 d . . . . .
H12A H 0.702806 0.064982 0.654926 0.092 Uiso 1 1 calc R U . . .
H12B H 0.777432 0.067529 0.641678 0.092 Uiso 1 1 calc R U . . .
H12C H 0.700138 0.000785 0.626647 0.092 Uiso 1 1 calc R U . . .
C13 C 0.8257(8) 0.0447(7) 0.5708(5) 0.079(4) Uani 1 1 d . . . . .
H13A H 0.843930 0.034688 0.544675 0.118 Uiso 1 1 calc R U . . .
H13B H 0.772334 0.012976 0.572283 0.118 Uiso 1 1 calc R U . . .
H13C H 0.848579 0.034999 0.594875 0.118 Uiso 1 1 calc R U . . .
C14 C 1.0874(8) 0.4462(9) 0.5417(6) 0.099(6) Uani 1 1 d . . . . .
H14A H 1.126649 0.456600 0.561917 0.149 Uiso 1 1 calc R U . . .
H14B H 1.082673 0.489965 0.538332 0.149 Uiso 1 1 calc R U . . .
H14C H 1.099396 0.432855 0.514580 0.149 Uiso 1 1 calc R U . . .
C15 C 1.0403(7) 0.4960(7) 0.6220(6) 0.087(5) Uani 1 1 d . . . . .
H15A H 1.015929 0.495521 0.648344 0.130 Uiso 1 1 calc R U . . .
H15B H 1.075111 0.546780 0.614053 0.130 Uiso 1 1 calc R U . . .
H15C H 1.066797 0.469045 0.625908 0.130 Uiso 1 1 calc R U . . .
C16 C 0.8957(8) 0.2917(11) 0.6606(5) 0.100(6) Uani 1 1 d . . . . .
H16 H 0.940193 0.307684 0.645606 0.120 Uiso 1 1 calc R U . . .
C17 C 0.8989(8) 0.2906(12) 0.7028(5) 0.117(7) Uani 1 1 d . . . . .
H17 H 0.945395 0.310560 0.716128 0.141 Uiso 1 1 calc R U . . .
C18 C 0.8381(5) 0.2622(7) 0.7266(4) 0.059(3) Uani 1 1 d . . . . .
C19 C 0.7716(8) 0.2289(8) 0.7047(4) 0.077(4) Uani 1 1 d . . . . .
H19 H 0.726297 0.201523 0.719075 0.092 Uiso 1 1 calc R U . . .
C20 C 0.7736(7) 0.2370(7) 0.6607(4) 0.068(3) Uani 1 1 d . . . . .
H20 H 0.728722 0.216686 0.645645 0.081 Uiso 1 1 calc R U . . .
P1 P 1.000000 1.000000 0.500000 0.0492(18) Uani 1 6 d S T P . .
F1 F 0.9312(3) 0.9822(3) 0.5285(3) 0.076(2) Uani 1 1 d . U . . .
S1 S 0.8664(5) 0.2960(6) 0.4533(3) 0.076(3) Uiso 0.5 1 d D . P A 1
S1A S 0.8659(6) 0.2800(7) 0.4489(4) 0.098(5) Uiso 0.5 1 d D . P A 2
O1 O 0.9107(8) 0.3584(7) 0.4757(4) 0.094(4) Uiso 0.7 1 d D . P A 1
O1A O 0.9397(10) 0.3230(17) 0.4650(11) 0.086(9) Uiso 0.3 1 d D . P A 2
O2 O 0.8882(12) 0.2888(11) 0.4133(5) 0.150(8) Uiso 0.7 1 d D . P A 1
O2A O 0.8943(18) 0.2376(17) 0.4286(10) 0.086(9) Uiso 0.3 1 d D . P A 2
F2 F 0.7522(12) 0.2475(10) 0.4135(6) 0.257(9) Uiso 1 1 d D . . . .
F3 F 0.8138(14) 0.3728(11) 0.4182(8) 0.349(12) Uiso 1 1 d D . . . .
F4 F 0.7515(11) 0.3069(10) 0.4743(5) 0.252(8) Uiso 1 1 d D . . . .
O3 O 0.8288(5) 0.2288(5) 0.4795(3) 0.076(2) Uiso 1 1 d D . . . .
C21 C 0.7960(10) 0.3067(13) 0.4395(8) 0.250(16) Uiso 1 1 d D . . . .
S2 S 0.666667 0.333333 0.60939(15) 0.0539(11) Uani 1 3 d S T P . .
F5 F 0.6407(4) 0.2653(4) 0.6819(2) 0.077(2) Uani 1 1 d . . . . .
O4 O 0.7226(4) 0.3146(5) 0.5991(3) 0.062(2) Uani 1 1 d . . . . .
C22 C 0.666667 0.333333 0.6653(7) 0.061(5) Uani 1 3 d S T P . .
S3 S 0.5940(5) 0.0188(5) 0.750000 0.129(3) Uiso 1 2 d DS . P . .
O6 O 0.6745(11) 0.0674(14) 0.750000 0.189(11) Uiso 1 2 d DS . P . .
O5 O 0.5749(13) -0.0252(12) 0.7108(6) 0.244(10) Uiso 1 1 d D . . . .
C23 C 0.550(2) 0.0707(19) 0.750000 0.40(4) Uiso 1 2 d DS . P . .
F6 F 0.5732(17) 0.1104(15) 0.7140(9) 0.475(18) Uiso 1 1 d D . . . .
F7 F 0.4767(16) 0.022(3) 0.750000 0.43(2) Uiso 1 2 d DS . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N8 2.493(9) . ?
Pb1 N4 2.574(9) . ?
Pb1 N3 2.644(9) . ?
Pb1 N5 2.678(9) . ?
Pb1 N1 2.757(9) . ?
N1 C1 1.331(13) . ?
N1 C2 1.342(14) . ?
N2 C2 1.371(13) . ?
N2 N3 1.374(12) . ?
N2 C12 1.487(15) . ?
N3 C3 1.297(13) . ?
N4 C4 1.342(14) . ?
N4 C8 1.356(14) . ?
N5 C9 1.276(13) . ?
N5 N6 1.415(12) . ?
N6 C10 1.369(13) . ?
N6 C15 1.448(17) . ?
N7 C1 1.316(13) 2_655 ?
N7 C10 1.373(14) . ?
N8 C16 1.270(16) . ?
N8 C20 1.363(15) . ?
C2 C11 1.379(15) 3_665 ?
C3 C4 1.492(16) . ?
C3 C13 1.504(16) . ?
C4 C5 1.392(16) . ?
C5 C6 1.376(19) . ?
C6 C7 1.381(19) . ?
C7 C8 1.371(16) . ?
C8 C9 1.514(17) . ?
C9 C14 1.507(17) . ?
C10 C11 1.400(15) . ?
C16 C17 1.35(2) . ?
C17 C18 1.342(16) . ?
C18 C19 1.397(17) . ?
C18 C18 1.49(2) 10_557 ?
C19 C20 1.407(18) . ?
P1 F1 1.585(6) . ?
P1 F1 1.585(6) 9_656 ?
P1 F1 1.585(6) 3_675 ?
P1 F1 1.585(6) 7_776 ?
P1 F1 1.585(6) 8_566 ?
P1 F1 1.585(6) 2_765 ?
S1 O1 1.369(12) . ?
S1 O2 1.389(14) . ?
S1 O3 1.484(12) . ?
S1 C21 1.663(9) . ?
S1A O3 1.370(16) . ?
S1A O1A 1.445(10) . ?
S1A O2A 1.451(10) . ?
S1A C21 1.841(9) . ?
F2 C21 1.391(17) . ?
F3 C21 1.417(17) . ?
F4 C21 1.452(16) . ?
S2 O4 1.452(8) 3_665 ?
S2 O4 1.452(8) 2_655 ?
S2 O4 1.452(8) . ?
S2 C22 1.78(2) . ?
F5 C22 1.359(11) . ?
S3 O6 1.477(17) . ?
S3 O5 1.484(16) . ?
S3 O5 1.484(16) 10_557 ?
S3 C23 1.75(2) . ?
C23 F6 1.357(18) . ?
C23 F6 1.357(18) 10_557 ?
C23 F7 1.36(2) . ?

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
N8 Pb1 N4 84.0(3) . . ?
N8 Pb1 N3 72.4(3) . . ?
N4 Pb1 N3 60.8(3) . . ?
N8 Pb1 N5 77.4(3) . . ?
N4 Pb1 N5 61.1(3) . . ?
N3 Pb1 N5 116.0(3) . . ?
N8 Pb1 N1 92.1(3) . . ?
N4 Pb1 N1 116.4(3) . . ?
N3 Pb1 N1 57.8(3) . . ?
N5 Pb1 N1 169.3(3) . . ?
C1 N1 C2 116.7(9) . . ?
C1 N1 Pb1 121.6(7) . . ?
C2 N1 Pb1 117.4(7) . . ?
C2 N2 N3 116.4(9) . . ?
C2 N2 C12 119.4(9) . . ?
N3 N2 C12 118.5(8) . . ?
C3 N3 N2 116.0(9) . . ?
C3 N3 Pb1 122.6(7) . . ?
N2 N3 Pb1 121.2(6) . . ?
C4 N4 C8 118.1(10) . . ?
C4 N4 Pb1 122.3(7) . . ?
C8 N4 Pb1 118.8(7) . . ?
C9 N5 N6 114.2(9) . . ?
C9 N5 Pb1 115.1(8) . . ?
N6 N5 Pb1 124.8(6) . . ?
C10 N6 N5 115.9(9) . . ?
C10 N6 C15 120.6(10) . . ?
N5 N6 C15 117.9(9) . . ?
C1 N7 C10 115.4(9) 2_655 . ?
C16 N8 C20 115.6(12) . . ?
C16 N8 Pb1 127.4(9) . . ?
C20 N8 Pb1 116.5(8) . . ?
N7 C1 N1 127.3(11) 3_665 . ?
N1 C2 N2 117.9(10) . . ?
N1 C2 C11 122.3(10) . 3_665 ?
N2 C2 C11 119.8(10) . 3_665 ?
N3 C3 C4 114.9(10) . . ?
N3 C3 C13 125.3(11) . . ?
C4 C3 C13 119.6(9) . . ?
N4 C4 C5 121.9(11) . . ?
N4 C4 C3 116.7(9) . . ?
C5 C4 C3 121.3(11) . . ?
C6 C5 C4 118.5(12) . . ?
C5 C6 C7 120.4(12) . . ?
C8 C7 C6 117.8(12) . . ?
N4 C8 C7 123.2(12) . . ?
N4 C8 C9 115.7(10) . . ?
C7 C8 C9 120.8(11) . . ?
N5 C9 C14 126.5(12) . . ?
N5 C9 C8 115.7(10) . . ?
C14 C9 C8 117.8(10) . . ?
N6 C10 N7 117.5(10) . . ?
N6 C10 C11 120.5(11) . . ?
N7 C10 C11 121.9(10) . . ?
C2 C11 C10 116.3(11) 2_655 . ?
N8 C16 C17 125.4(13) . . ?
C18 C17 C16 121.7(14) . . ?
C17 C18 C19 115.7(13) . . ?
C17 C18 C18 124.3(9) . 10_557 ?
C19 C18 C18 119.9(8) . 10_557 ?
C18 C19 C20 118.3(13) . . ?
N8 C20 C19 121.9(12) . . ?
F1 P1 F1 89.5(5) . 9_656 ?
F1 P1 F1 90.5(5) . 3_675 ?
F1 P1 F1 180.0(4) 9_656 3_675 ?
F1 P1 F1 180.0 . 7_776 ?
F1 P1 F1 90.5(5) 9_656 7_776 ?
F1 P1 F1 89.5(5) 3_675 7_776 ?
F1 P1 F1 89.5(5) . 8_566 ?
F1 P1 F1 90.5(5) 9_656 8_566 ?
F1 P1 F1 89.5(5) 3_675 8_566 ?
F1 P1 F1 90.5(5) 7_776 8_566 ?
F1 P1 F1 90.5(5) . 2_765 ?
F1 P1 F1 89.5(5) 9_656 2_765 ?
F1 P1 F1 90.5(5) 3_675 2_765 ?
F1 P1 F1 89.5(5) 7_776 2_765 ?
F1 P1 F1 180.0(5) 8_566 2_765 ?
O1 S1 O2 118.6(12) . . ?
O1 S1 O3 113.8(9) . . ?
O2 S1 O3 117.3(11) . . ?
O1 S1 C21 103.5(13) . . ?
O2 S1 C21 97.9(14) . . ?
O3 S1 C21 101.0(11) . . ?
O3 S1A O1A 104.5(16) . . ?
O3 S1A O2A 94.6(17) . . ?
O1A S1A O2A 84(2) . . ?
O3 S1A C21 97.3(11) . . ?
O1A S1A C21 129.7(18) . . ?
O2A S1A C21 138.8(18) . . ?
F2 C21 F3 109.0(15) . . ?
F2 C21 F4 108.5(15) . . ?
F3 C21 F4 102.5(13) . . ?
F2 C21 S1 105.8(15) . . ?
F3 C21 S1 116(2) . . ?
F4 C21 S1 114.6(17) . . ?
F2 C21 S1A 95.5(15) . . ?
F3 C21 S1A 121.1(19) . . ?
F4 C21 S1A 119.4(16) . . ?
O4 S2 O4 115.0(3) 3_665 2_655 ?
O4 S2 O4 115.0(3) 3_665 . ?
O4 S2 O4 115.0(3) 2_655 . ?
O4 S2 C22 103.1(4) 3_665 . ?
O4 S2 C22 103.1(4) 2_655 . ?
O4 S2 C22 103.1(4) . . ?
F5 C22 F5 105.8(11) 3_665 . ?
F5 C22 F5 105.8(11) 3_665 2_655 ?
F5 C22 F5 105.8(11) . 2_655 ?
F5 C22 S2 112.9(10) 3_665 . ?
F5 C22 S2 112.9(10) . . ?
F5 C22 S2 112.9(10) 2_655 . ?
O6 S3 O5 106.8(12) . . ?
O6 S3 O5 106.8(12) . 10_557 ?
O5 S3 O5 114(2) . 10_557 ?
O6 S3 C23 110.5(18) . . ?
O5 S3 C23 109.1(12) . . ?
O5 S3 C23 109.1(12) 10_557 . ?
F6 C23 F6 115(4) . 10_557 ?
F6 C23 F7 113(2) . . ?
F6 C23 F7 113(2) 10_557 . ?
F6 C23 S3 104.0(15) . . ?
F6 C23 S3 104.0(15) 10_557 . ?
F7 C23 S3 106.1(18) . . ?

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
C2 N2 N3 C3 -150.5(11) . . . . ?
C12 N2 N3 C3 56.2(14) . . . . ?
C2 N2 N3 Pb1 24.3(12) . . . . ?
C12 N2 N3 Pb1 -129.1(8) . . . . ?
C9 N5 N6 C10 135.9(12) . . . . ?
Pb1 N5 N6 C10 -15.4(14) . . . . ?
C9 N5 N6 C15 -70.4(15) . . . . ?
Pb1 N5 N6 C15 138.3(10) . . . . ?
C2 N1 C1 N7 -5.2(16) . . . 3_665 ?
Pb1 N1 C1 N7 -161.1(8) . . . 3_665 ?
C1 N1 C2 N2 178.2(10) . . . . ?
Pb1 N1 C2 N2 -24.8(12) . . . . ?
C1 N1 C2 C11 1.5(16) . . . 3_665 ?
Pb1 N1 C2 C11 158.4(9) . . . 3_665 ?
N3 N2 C2 N1 1.7(15) . . . . ?
C12 N2 C2 N1 154.8(10) . . . . ?
N3 N2 C2 C11 178.5(10) . . . 3_665 ?
C12 N2 C2 C11 -28.4(16) . . . 3_665 ?
N2 N3 C3 C4 -173.7(10) . . . . ?
Pb1 N3 C3 C4 11.6(14) . . . . ?
N2 N3 C3 C13 10.1(18) . . . . ?
Pb1 N3 C3 C13 -164.5(11) . . . . ?
C8 N4 C4 C5 -2.2(18) . . . . ?
Pb1 N4 C4 C5 166.9(10) . . . . ?
C8 N4 C4 C3 176.4(11) . . . . ?
Pb1 N4 C4 C3 -14.5(14) . . . . ?
N3 C3 C4 N4 1.6(17) . . . . ?
C13 C3 C4 N4 178.0(12) . . . . ?
N3 C3 C4 C5 -179.7(12) . . . . ?
C13 C3 C4 C5 -3(2) . . . . ?
N4 C4 C5 C6 1(2) . . . . ?
C3 C4 C5 C6 -177.3(15) . . . . ?
C4 C5 C6 C7 0(3) . . . . ?
C5 C6 C7 C8 0(3) . . . . ?
C4 N4 C8 C7 2.3(19) . . . . ?
Pb1 N4 C8 C7 -167.2(11) . . . . ?
C4 N4 C8 C9 -172.0(11) . . . . ?
Pb1 N4 C8 C9 18.5(14) . . . . ?
C6 C7 C8 N4 -1(2) . . . . ?
C6 C7 C8 C9 172.8(15) . . . . ?
N6 N5 C9 C14 -8(2) . . . . ?
Pb1 N5 C9 C14 146.0(13) . . . . ?
N6 N5 C9 C8 169.3(10) . . . . ?
Pb1 N5 C9 C8 -36.6(14) . . . . ?
N4 C8 C9 N5 13.2(17) . . . . ?
C7 C8 C9 N5 -161.2(14) . . . . ?
N4 C8 C9 C14 -169.1(13) . . . . ?
C7 C8 C9 C14 16(2) . . . . ?
N5 N6 C10 N7 -11.1(15) . . . . ?
C15 N6 C10 N7 -164.0(11) . . . . ?
N5 N6 C10 C11 173.0(10) . . . . ?
C15 N6 C10 C11 20.1(17) . . . . ?
C1 N7 C10 N6 -174.9(10) 2_655 . . . ?
C1 N7 C10 C11 0.9(15) 2_655 . . . ?
N6 C10 C11 C2 171.8(11) . . . 2_655 ?
N7 C10 C11 C2 -3.9(17) . . . 2_655 ?
C20 N8 C16 C17 -13(3) . . . . ?
Pb1 N8 C16 C17 175.4(17) . . . . ?
N8 C16 C17 C18 7(4) . . . . ?
C16 C17 C18 C19 5(3) . . . . ?
C16 C17 C18 C18 -177.3(15) . . . 10_557 ?
C17 C18 C19 C20 -9(2) . . . . ?
C18 C18 C19 C20 173.1(10) 10_557 . . . ?
C16 N8 C20 C19 8(2) . . . . ?
Pb1 N8 C20 C19 -179.6(11) . . . . ?
C18 C19 C20 N8 3(2) . . . . ?
O1 S1 C21 F2 175.0(15) . . . . ?
O2 S1 C21 F2 52.9(18) . . . . ?
O3 S1 C21 F2 -67.0(16) . . . . ?
O1 S1 C21 F3 53.9(19) . . . . ?
O2 S1 C21 F3 -68.2(19) . . . . ?
O3 S1 C21 F3 171.9(16) . . . . ?
O1 S1 C21 F4 -65.5(19) . . . . ?
O2 S1 C21 F4 172.5(17) . . . . ?
O3 S1 C21 F4 52.5(18) . . . . ?
O3 S1A C21 F2 -81.0(15) . . . . ?
O1A S1A C21 F2 163(2) . . . . ?
O2A S1A C21 F2 25(3) . . . . ?
O3 S1A C21 F3 162.9(17) . . . . ?
O1A S1A C21 F3 47(3) . . . . ?
O2A S1A C21 F3 -91(3) . . . . ?
O3 S1A C21 F4 34(2) . . . . ?
O1A S1A C21 F4 -82(3) . . . . ?
O2A S1A C21 F4 140(3) . . . . ?
O4 S2 C22 F5 -68.3(5) 3_665 . . 3_665 ?
O4 S2 C22 F5 51.7(5) 2_655 . . 3_665 ?
O4 S2 C22 F5 171.7(5) . . . 3_665 ?
O4 S2 C22 F5 51.7(5) 3_665 . . . ?
O4 S2 C22 F5 171.7(5) 2_655 . . . ?
O4 S2 C22 F5 -68.3(5) . . . . ?
O4 S2 C22 F5 171.7(5) 3_665 . . 2_655 ?
O4 S2 C22 F5 -68.3(5) 2_655 . . 2_655 ?
O4 S2 C22 F5 51.7(5) . . . 2_655 ?
O6 S3 C23 F6 61(2) . . . . ?
O5 S3 C23 F6 -57(3) . . . . ?
O5 S3 C23 F6 178(2) 10_557 . . . ?
O6 S3 C23 F6 -61(2) . . . 10_557 ?
O5 S3 C23 F6 -178(2) . . . 10_557 ?
O5 S3 C23 F6 57(3) 10_557 . . 10_557 ?
O6 S3 C23 F7 180.000(2) . . . . ?
O5 S3 C23 F7 62.8(12) . . . . ?
O5 S3 C23 F7 -62.8(12) 10_557 . . . ?

_refine_diff_density_max         1.899
_refine_diff_density_min         -2.086
_refine_diff_density_rms         0.175



####################################################################### 
# 
# 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_2PF6
_database_code_depnum_ccdc_archive 'CCDC 2293677'
loop_
_audit_author_name
_audit_author_address
'Nathalie Gruber'
;Universite de Strasbourg
France
;
_audit_update_record             
;
2023-09-07 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C67 H66 F12 N24 O12 Pb3 S4), F6 P [+ solvent]'
_chemical_formula_sum            'C134 H132 F30 N48 O24 P Pb6 S8,solvent'
_chemical_formula_weight         4899.46

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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+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                   21.1133(6)
_cell_length_b                   21.1133(6)
_cell_length_c                   51.250(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     19784.9(15)
_cell_formula_units_Z            3
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9800
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      27.74

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_F_000             7107
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    3.957
_shelx_estimated_absorpt_T_min   0.536
_shelx_estimated_absorpt_T_max   0.607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5895
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            117507
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_theta_min         1.929
_diffrn_reflns_theta_max         27.947
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10519
_reflns_number_gt                8716
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0649P)²+121.8275P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10519
_refine_ls_number_parameters     370
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.1158
_refine_ls_wR_factor_gt          0.1097
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.004

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 0.49479(2) 0.61722(2) 0.37138(2) 0.03803(7) Uani 1 1 d . . . . .
N1 N 0.5993(2) 0.5854(2) 0.36997(8) 0.0461(9) Uani 1 1 d . . . . .
C1 C 0.6673(3) 0.6402(3) 0.36472(11) 0.0503(12) Uani 1 1 d . . . . .
C2 C 0.7249(3) 0.6268(4) 0.35917(13) 0.0623(15) Uani 1 1 d . . . . .
H2 H 0.772591 0.665829 0.355296 0.075 Uiso 1 1 calc R U . . .
C3 C 0.7100(3) 0.5554(3) 0.35953(15) 0.0667(17) Uani 1 1 d . . . . .
H3 H 0.748157 0.544921 0.356244 0.080 Uiso 1 1 calc R U . . .
C4 C 0.6405(3) 0.4991(3) 0.36459(13) 0.0584(14) Uani 1 1 d . . . . .
H4 H 0.629754 0.449675 0.364498 0.070 Uiso 1 1 calc R U . . .
C5 C 0.5860(3) 0.5166(3) 0.36987(11) 0.0483(11) Uani 1 1 d . . . . .
C6 C 0.5105(3) 0.4580(3) 0.37656(11) 0.0492(11) Uani 1 1 d . . . . .
C7 C 0.4919(3) 0.3792(3) 0.37575(15) 0.0617(15) Uani 1 1 d . . . . .
H7A H 0.510806 0.367909 0.391460 0.093 Uiso 1 1 calc R U . . .
H7B H 0.514113 0.371053 0.360262 0.093 Uiso 1 1 calc R U . . .
H7C H 0.438677 0.347476 0.374986 0.093 Uiso 1 1 calc R U . . .
N2 N 0.4654(2) 0.4805(2) 0.38246(9) 0.0478(9) Uani 1 1 d . . . . .
N3 N 0.3972(2) 0.4286(2) 0.39180(9) 0.0499(10) Uani 1 1 d . . . . .
C8 C 0.3921(3) 0.3835(3) 0.41460(12) 0.0575(14) Uani 1 1 d . . . . .
H8A H 0.361391 0.387774 0.428016 0.086 Uiso 1 1 calc R U . . .
H8B H 0.441153 0.400524 0.421664 0.086 Uiso 1 1 calc R U . . .
H8C H 0.370429 0.332254 0.409230 0.086 Uiso 1 1 calc R U . . .
C9 C 0.3401(3) 0.4395(3) 0.38573(11) 0.0475(11) Uani 1 1 d . . . . .
N4 N 0.3556(2) 0.5002(2) 0.37175(9) 0.0464(9) Uani 1 1 d . . . . .
C10 C 0.2979(3) 0.5068(3) 0.36578(10) 0.0456(11) Uani 1 1 d . . . . .
H10 H 0.308356 0.550495 0.356938 0.055 Uiso 1 1 calc R U . . .
N5 N 0.2282(2) 0.4609(2) 0.37047(8) 0.0440(9) Uani 1 1 d . . . . .
C11 C 0.2138(3) 0.3998(3) 0.38422(12) 0.0495(12) Uani 1 1 d . . . . .
C12 C 0.2698(3) 0.3885(3) 0.39283(13) 0.0576(14) Uani 1 1 d . . . . .
H12 H 0.259991 0.347237 0.403186 0.069 Uiso 1 1 calc R U . . .
N6 N 0.1429(2) 0.3485(2) 0.38743(12) 0.0619(13) Uani 1 1 d . . . . .
C13 C 0.1217(3) 0.2914(4) 0.4073(2) 0.103(3) Uani 1 1 d . . . . .
H13A H 0.122400 0.249222 0.399614 0.154 Uiso 1 1 calc R U . . .
H13B H 0.072320 0.276300 0.413572 0.154 Uiso 1 1 calc R U . . .
H13C H 0.156218 0.310494 0.421873 0.154 Uiso 1 1 calc R U . . .
N7 N 0.0903(2) 0.3678(2) 0.38026(9) 0.0494(10) Uani 1 1 d . . . . .
C14 C 0.0345(3) 0.3180(3) 0.36790(13) 0.0585(14) Uani 1 1 d . . . . .
C15 C 0.0261(4) 0.2478(4) 0.3577(2) 0.099(3) Uani 1 1 d . . . . .
H15A H 0.073431 0.256180 0.351260 0.148 Uiso 1 1 calc R U . . .
H15B H -0.009380 0.229975 0.343326 0.148 Uiso 1 1 calc R U . . .
H15C H 0.008768 0.211374 0.371666 0.148 Uiso 1 1 calc R U . . .
N8 N 0.5056(3) 0.6050(3) 0.41898(9) 0.0577(11) Uani 1 1 d . . . . .
C16 C 0.5680(5) 0.6165(4) 0.42971(12) 0.0759(19) Uani 1 1 d . . . . .
H16 H 0.611974 0.644884 0.420182 0.091 Uiso 1 1 calc R U . . .
C17 C 0.5728(6) 0.5900(5) 0.45365(14) 0.094(3) Uani 1 1 d . . . . .
H17 H 0.619080 0.600436 0.460220 0.113 Uiso 1 1 calc R U . . .
C18 C 0.5113(7) 0.5489(5) 0.46795(14) 0.099(3) Uani 1 1 d . . . . .
C19 C 0.4466(5) 0.5376(4) 0.45748(14) 0.089(3) Uani 1 1 d . . . . .
H19 H 0.402568 0.510155 0.467076 0.106 Uiso 1 1 calc R U . . .
C20 C 0.4439(4) 0.5658(3) 0.43286(12) 0.0661(16) Uani 1 1 d . . . . .
H20 H 0.398366 0.557206 0.426049 0.079 Uiso 1 1 calc R U . . .
C21 C 0.5268(5) 0.5241(4) 0.49286(16) 0.123(4) Uani 1 1 d D . . . .
H21 H 0.575923 0.543389 0.498506 0.148 Uiso 1 1 calc R U . . .
S1 S 0.53117(11) 0.61556(14) 0.30254(4) 0.1067(8) Uani 1 1 d D . . . .
O1 O 0.4912(3) 0.5606(2) 0.32146(9) 0.0768(13) Uani 1 1 d . U . . .
O2 O 0.5825(5) 0.6794(4) 0.31574(15) 0.200(5) Uani 1 1 d . U . . .
O3 O 0.5585(5) 0.5775(7) 0.28423(17) 0.233(5) Uani 1 1 d . U . . .
C22 C 0.4872(10) 0.6321(11) 0.2774(3) 0.183 Uiso 0.5 1 d D U P A 1
F1 F 0.5407(8) 0.6589(9) 0.2606(3) 0.183 Uiso 0.5 1 d D U P A 1
F2 F 0.4323(9) 0.5628(8) 0.2728(4) 0.183 Uiso 0.5 1 d D U P A 1
F3 F 0.4544(9) 0.6737(9) 0.2820(4) 0.183 Uiso 0.5 1 d D U P A 1
C22A C 0.4597(9) 0.6362(12) 0.2991(4) 0.183 Uiso 0.5 1 d D U P A 2
F2A F 0.4108(9) 0.6369(9) 0.3176(3) 0.183 Uiso 0.5 1 d D U P A 2
F1A F 0.4065(10) 0.5847(8) 0.2809(3) 0.183 Uiso 0.5 1 d D U P A 2
F3A F 0.4816(9) 0.7031(8) 0.2865(4) 0.183 Uiso 0.5 1 d D U P A 2
O4 O 0.3895(2) 0.6495(2) 0.39700(8) 0.0572(9) Uani 1 1 d . . . . .
S2 S 0.333333 0.666667 0.40345(5) 0.0506(5) Uani 1 3 d DS T P . .
C23 C 0.333333 0.666667 0.43830(15) 0.068(3) Uani 1 3 d DS T P . .
F4 F 0.3997(2) 0.7111(2) 0.44854(7) 0.0846(12) Uani 1 1 d . . . . .
P1 P 0.666667 0.333333 0.333333 0.0442(7) Uani 1 6 d S T P . .
F5 F 0.71851(16) 0.40185(16) 0.35111(9) 0.0689(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N8 2.476(5) . ?
Pb1 N1 2.610(4) . ?
Pb1 N7 2.667(4) 2_665 ?
Pb1 N2 2.693(4) . ?
Pb1 N4 2.735(4) . ?
N1 C5 1.334(6) . ?
N1 C1 1.346(6) . ?
C1 C2 1.409(7) . ?
C1 C14 1.490(8) 2_665 ?
C2 C3 1.379(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.374(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.400(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.489(7) . ?
C6 N2 1.295(6) . ?
C6 C7 1.506(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N2 N3 1.388(5) . ?
N3 C9 1.370(6) . ?
N3 C8 1.477(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N4 1.358(6) . ?
C9 C12 1.378(7) . ?
N4 C10 1.328(6) . ?
C10 N5 1.319(6) . ?
C10 H10 0.9500 . ?
N5 C11 1.363(6) . ?
C11 N6 1.350(6) . ?
C11 C12 1.390(7) . ?
C12 H12 0.9500 . ?
N6 N7 1.408(6) . ?
N6 C13 1.466(8) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
N7 C14 1.286(7) . ?
C14 C15 1.496(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N8 C16 1.333(8) . ?
N8 C20 1.346(8) . ?
C16 C17 1.373(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.360(13) . ?
C17 H17 0.9500 . ?
C18 C19 1.375(13) . ?
C18 C21 1.477(11) . ?
C19 C20 1.408(9) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C21 1.304(9) 10_666 ?
C21 H21 0.9500 . ?
S1 O2 1.410(7) . ?
S1 O1 1.421(5) . ?
S1 O3 1.524(12) . ?
S1 C22 1.724(10) . ?
S1 C22A 1.776(9) . ?
C22 F1 1.300(16) . ?
C22 F2 1.357(16) . ?
C22 F3 1.384(16) . ?
C22A F3A 1.405(17) . ?
C22A F2A 1.410(15) . ?
C22A F1A 1.448(17) . ?
O4 S2 1.441(4) . ?
S2 C23 1.786(8) . ?
C23 F4 1.343(5) 2_665 ?
C23 F4 1.343(5) 3_565 ?
C23 F4 1.343(5) . ?
P1 F5 1.593(3) 3_665 ?
P1 F5 1.593(3) 18_545 ?
P1 F5 1.593(3) 2_655 ?
P1 F5 1.593(3) . ?
P1 F5 1.593(3) 16_655 ?
P1 F5 1.593(3) 17 ?

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
N8 Pb1 N1 82.33(15) . . ?
N8 Pb1 N7 78.48(16) . 2_665 ?
N1 Pb1 N7 60.79(13) . 2_665 ?
N8 Pb1 N2 70.38(15) . . ?
N1 Pb1 N2 60.06(12) . . ?
N7 Pb1 N2 115.41(12) 2_665 . ?
N8 Pb1 N4 90.71(15) . . ?
N1 Pb1 N4 115.65(12) . . ?
N7 Pb1 N4 168.90(13) 2_665 . ?
N2 Pb1 N4 57.50(12) . . ?
C5 N1 C1 119.3(4) . . ?
C5 N1 Pb1 122.4(3) . . ?
C1 N1 Pb1 117.3(3) . . ?
N1 C1 C2 121.6(5) . . ?
N1 C1 C14 117.7(4) . 2_665 ?
C2 C1 C14 120.4(5) . 2_665 ?
C3 C2 C1 118.0(5) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C4 C3 C2 120.6(5) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 118.1(5) . . ?
C3 C4 H4 120.9 . . ?
C5 C4 H4 121.0 . . ?
N1 C5 C4 122.3(5) . . ?
N1 C5 C6 117.3(4) . . ?
C4 C5 C6 120.3(5) . . ?
N2 C6 C5 115.3(4) . . ?
N2 C6 C7 125.3(5) . . ?
C5 C6 C7 119.4(4) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 N2 N3 117.1(4) . . ?
C6 N2 Pb1 121.8(3) . . ?
N3 N2 Pb1 120.7(3) . . ?
C9 N3 N2 116.2(4) . . ?
C9 N3 C8 120.1(4) . . ?
N2 N3 C8 119.6(4) . . ?
N3 C8 H8A 109.4 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 N3 117.5(4) . . ?
N4 C9 C12 122.3(5) . . ?
N3 C9 C12 120.1(4) . . ?
C10 N4 C9 114.8(4) . . ?
C10 N4 Pb1 122.1(3) . . ?
C9 N4 Pb1 119.9(3) . . ?
N5 C10 N4 128.8(5) . . ?
N5 C10 H10 115.6 . . ?
N4 C10 H10 115.6 . . ?
C10 N5 C11 115.3(4) . . ?
N6 C11 N5 117.0(5) . . ?
N6 C11 C12 121.4(5) . . ?
N5 C11 C12 121.4(4) . . ?
C9 C12 C11 117.3(5) . . ?
C9 C12 H12 121.4 . . ?
C11 C12 H12 121.4 . . ?
C11 N6 N7 117.1(4) . . ?
C11 N6 C13 120.3(5) . . ?
N7 N6 C13 117.3(4) . . ?
N6 C13 H13A 109.4 . . ?
N6 C13 H13B 109.4 . . ?
H13A C13 H13B 109.5 . . ?
N6 C13 H13C 109.6 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 N7 N6 115.1(4) . . ?
C14 N7 Pb1 115.8(4) . 3_565 ?
N6 N7 Pb1 123.4(3) . 3_565 ?
N7 C14 C1 114.9(4) . 3_565 ?
N7 C14 C15 126.1(6) . . ?
C1 C14 C15 118.9(5) 3_565 . ?
C14 C15 H15A 109.4 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 N8 C20 117.4(5) . . ?
C16 N8 Pb1 121.4(4) . . ?
C20 N8 Pb1 118.3(4) . . ?
N8 C16 C17 124.1(8) . . ?
N8 C16 H16 117.9 . . ?
C17 C16 H16 117.9 . . ?
C18 C17 C16 120.1(9) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 116.7(6) . . ?
C17 C18 C21 112.5(9) . . ?
C19 C18 C21 130.8(9) . . ?
C18 C19 C20 121.6(8) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.1 . . ?
N8 C20 C19 120.1(7) . . ?
N8 C20 H20 119.9 . . ?
C19 C20 H20 120.0 . . ?
C21 C21 C18 120.1(13) 10_666 . ?
C21 C21 H21 120.0 10_666 . ?
C18 C21 H21 119.9 . . ?
O2 S1 O1 108.1(4) . . ?
O2 S1 O3 119.1(6) . . ?
O1 S1 O3 102.5(5) . . ?
O2 S1 C22 113.6(8) . . ?
O1 S1 C22 121.1(7) . . ?
O3 S1 C22 91.7(8) . . ?
O2 S1 C22A 98.9(9) . . ?
O1 S1 C22A 92.1(8) . . ?
O3 S1 C22A 131.3(8) . . ?
F1 C22 F2 116.4(17) . . ?
F1 C22 F3 116.0(15) . . ?
F2 C22 F3 106.5(13) . . ?
F1 C22 S1 98.2(11) . . ?
F2 C22 S1 99.6(13) . . ?
F3 C22 S1 119.5(16) . . ?
F3A C22A F2A 100.0(12) . . ?
F3A C22A F1A 101.6(14) . . ?
F2A C22A F1A 98.3(12) . . ?
F3A C22A S1 113.6(14) . . ?
F2A C22A S1 130.7(16) . . ?
F1A C22A S1 108.4(13) . . ?
O4 S2 O4 114.90(14) 2_665 3_565 ?
O4 S2 O4 114.90(14) 2_665 . ?
O4 S2 O4 114.90(14) 3_565 . ?
O4 S2 C23 103.26(18) 2_665 . ?
O4 S2 C23 103.26(18) 3_565 . ?
O4 S2 C23 103.27(18) . . ?
F4 C23 F4 105.7(4) 2_665 3_565 ?
F4 C23 F4 105.7(4) 2_665 . ?
F4 C23 F4 105.7(4) 3_565 . ?
F4 C23 S2 113.0(4) 2_665 . ?
F4 C23 S2 113.0(4) 3_565 . ?
F4 C23 S2 113.0(4) . . ?
F5 P1 F5 180.0 3_665 18_545 ?
F5 P1 F5 90.5(2) 3_665 2_655 ?
F5 P1 F5 89.5(2) 18_545 2_655 ?
F5 P1 F5 90.5(2) 3_665 . ?
F5 P1 F5 89.5(2) 18_545 . ?
F5 P1 F5 90.5(2) 2_655 . ?
F5 P1 F5 89.5(2) 3_665 16_655 ?
F5 P1 F5 90.5(2) 18_545 16_655 ?
F5 P1 F5 89.5(2) 2_655 16_655 ?
F5 P1 F5 180.0 . 16_655 ?
F5 P1 F5 89.5(2) 3_665 17 ?
F5 P1 F5 90.5(2) 18_545 17 ?
F5 P1 F5 180.0(3) 2_655 17 ?
F5 P1 F5 89.5(2) . 17 ?
F5 P1 F5 90.5(2) 16_655 17 ?

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
C5 N1 C1 C2 -0.2(8) . . . . ?
Pb1 N1 C1 C2 -169.1(4) . . . . ?
C5 N1 C1 C14 -173.4(5) . . . 2_665 ?
Pb1 N1 C1 C14 17.7(6) . . . 2_665 ?
N1 C1 C2 C3 -0.7(9) . . . . ?
C14 C1 C2 C3 172.3(6) 2_665 . . . ?
C1 C2 C3 C4 1.4(11) . . . . ?
C2 C3 C4 C5 -1.3(10) . . . . ?
C1 N1 C5 C4 0.3(8) . . . . ?
Pb1 N1 C5 C4 168.6(4) . . . . ?
C1 N1 C5 C6 178.3(5) . . . . ?
Pb1 N1 C5 C6 -13.4(7) . . . . ?
C3 C4 C5 N1 0.4(9) . . . . ?
C3 C4 C5 C6 -177.5(6) . . . . ?
N1 C5 C6 N2 -1.6(8) . . . . ?
C4 C5 C6 N2 176.4(5) . . . . ?
N1 C5 C6 C7 177.7(5) . . . . ?
C4 C5 C6 C7 -4.3(9) . . . . ?
C5 C6 N2 N3 -172.5(5) . . . . ?
C7 C6 N2 N3 8.2(9) . . . . ?
C5 C6 N2 Pb1 15.3(7) . . . . ?
C7 C6 N2 Pb1 -163.9(5) . . . . ?
C6 N2 N3 C9 -148.0(5) . . . . ?
Pb1 N2 N3 C9 24.3(6) . . . . ?
C6 N2 N3 C8 54.7(7) . . . . ?
Pb1 N2 N3 C8 -133.0(4) . . . . ?
N2 N3 C9 N4 -1.3(7) . . . . ?
C8 N3 C9 N4 155.8(5) . . . . ?
N2 N3 C9 C12 176.0(5) . . . . ?
C8 N3 C9 C12 -26.8(8) . . . . ?
N3 C9 N4 C10 178.1(5) . . . . ?
C12 C9 N4 C10 0.8(8) . . . . ?
N3 C9 N4 Pb1 -21.6(6) . . . . ?
C12 C9 N4 Pb1 161.1(4) . . . . ?
C9 N4 C10 N5 -3.7(8) . . . . ?
Pb1 N4 C10 N5 -163.5(4) . . . . ?
N4 C10 N5 C11 2.9(8) . . . . ?
C10 N5 C11 N6 -174.4(5) . . . . ?
C10 N5 C11 C12 0.9(8) . . . . ?
N4 C9 C12 C11 2.4(9) . . . . ?
N3 C9 C12 C11 -174.8(5) . . . . ?
N6 C11 C12 C9 171.7(6) . . . . ?
N5 C11 C12 C9 -3.3(9) . . . . ?
N5 C11 N6 N7 -10.5(8) . . . . ?
C12 C11 N6 N7 174.2(5) . . . . ?
N5 C11 N6 C13 -164.0(6) . . . . ?
C12 C11 N6 C13 20.8(9) . . . . ?
C11 N6 N7 C14 137.9(6) . . . . ?
C13 N6 N7 C14 -67.9(8) . . . . ?
C11 N6 N7 Pb1 -14.3(7) . . . 3_565 ?
C13 N6 N7 Pb1 139.9(6) . . . 3_565 ?
N6 N7 C14 C1 169.1(5) . . . 3_565 ?
Pb1 N7 C14 C1 -36.6(6) 3_565 . . 3_565 ?
N6 N7 C14 C15 -8.8(9) . . . . ?
Pb1 N7 C14 C15 145.6(6) 3_565 . . . ?
C20 N8 C16 C17 1.1(10) . . . . ?
Pb1 N8 C16 C17 -159.1(6) . . . . ?
N8 C16 C17 C18 0.3(12) . . . . ?
C16 C17 C18 C19 -1.6(11) . . . . ?
C16 C17 C18 C21 178.9(7) . . . . ?
C17 C18 C19 C20 1.5(11) . . . . ?
C21 C18 C19 C20 -179.1(7) . . . . ?
C16 N8 C20 C19 -1.2(9) . . . . ?
Pb1 N8 C20 C19 159.7(5) . . . . ?
C18 C19 C20 N8 -0.1(10) . . . . ?
C17 C18 C21 C21 -170.3(11) . . . 10_666 ?
C19 C18 C21 C21 10.3(17) . . . 10_666 ?
O2 S1 C22 F1 74.5(14) . . . . ?
O1 S1 C22 F1 -154.2(10) . . . . ?
O3 S1 C22 F1 -48.5(13) . . . . ?
O2 S1 C22 F2 -166.8(11) . . . . ?
O1 S1 C22 F2 -35.6(15) . . . . ?
O3 S1 C22 F2 70.2(12) . . . . ?
O2 S1 C22 F3 -51.6(17) . . . . ?
O1 S1 C22 F3 79.6(17) . . . . ?
O3 S1 C22 F3 -174.6(15) . . . . ?
O2 S1 C22A F3A 55.6(16) . . . . ?
O1 S1 C22A F3A 164.4(15) . . . . ?
O3 S1 C22A F3A -86.8(18) . . . . ?
O2 S1 C22A F2A -73(2) . . . . ?
O1 S1 C22A F2A 35.6(19) . . . . ?
O3 S1 C22A F2A 144.4(16) . . . . ?
O2 S1 C22A F1A 167.7(13) . . . . ?
O1 S1 C22A F1A -83.6(13) . . . . ?
O3 S1 C22A F1A 25.2(19) . . . . ?
O4 S2 C23 F4 54.0(3) 2_665 . . 2_665 ?
O4 S2 C23 F4 -66.0(3) 3_565 . . 2_665 ?
O4 S2 C23 F4 174.0(3) . . . 2_665 ?
O4 S2 C23 F4 174.0(3) 2_665 . . 3_565 ?
O4 S2 C23 F4 54.0(3) 3_565 . . 3_565 ?
O4 S2 C23 F4 -66.0(3) . . . 3_565 ?
O4 S2 C23 F4 -66.0(3) 2_665 . . . ?
O4 S2 C23 F4 174.0(3) 3_565 . . . ?
O4 S2 C23 F4 54.0(3) . . . . ?

_refine_diff_density_max         2.522
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.107



