#------------------------------------------------------------------------------
#$Date: 2023-11-08 01:00:26 +0200 (Wed, 08 Nov 2023) $
#$Revision: 287473 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/23/7132312.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7132312
loop_
_publ_author_name
'Wang, Hai-Ping'
'Eichhöfer, Andreas'
'Gu, Zhi-Gang'
'Gruber, Nathalie'
'Stadler, Adrian-Mihail'
_publ_section_title
;
 Anion-encapsulating, discrete prism and extended frusta, from
 trimetallated triangular macrocycles and linkers.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc00137g
_journal_year                    2023
_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
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-09-07 deposited with the CCDC.	2023-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.0435(6)
_cell_length_b                   21.0435(6)
_cell_length_c                   58.507(3)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.20
_cell_volume                     22437.5(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       76
_diffrn_reflns_limit_l_min       -77
_diffrn_reflns_number            70808
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.911
_diffrn_reflns_theta_min         1.935
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_exptl_absorpt_coefficient_mu    3.491
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             7341
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         2.434
_refine_diff_density_min         -2.162
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         11923
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0722P)²+129.9682P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10039
_reflns_number_total             11923
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc00137g2.cif
_cod_data_source_block           3PF6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        22437.5(16)
_cod_database_code               7132312
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.514
_shelx_estimated_absorpt_t_max   0.572
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'
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 . . . . .
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'
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_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_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 . . . ?
