#------------------------------------------------------------------------------
#$Date: 2023-11-08 01:00:26 +0200 (Wed, 08 Nov 2023) $
#$Revision: 287473 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/23/7132315.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_7132315
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(C67 H66 F12 N24 O12 Pb3 S4), F6 P [+ solvent]'
_chemical_formula_sum            'C134 H132 F30 N48 O24 P Pb6 S8 en lv so t'
_chemical_formula_weight         4899.46
_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                   21.1133(6)
_cell_length_b                   21.1133(6)
_cell_length_c                   51.250(3)
_cell_measurement_reflns_used    9800
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.27
_cell_volume                     19785.0(14)
_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 0.995
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            117507
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.947
_diffrn_reflns_theta_min         1.929
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_exptl_absorpt_coefficient_mu    3.957
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             7107
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_refine_diff_density_max         2.522
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         10519
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0649P)²+121.8275P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8716
_reflns_number_total             10519
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc00137g2.cif
_cod_data_source_block           2PF6
_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        19784.9(15)
_cod_original_formula_sum        'C134 H132 F30 N48 O24 P Pb6 S8,solvent'
_cod_database_code               7132315
_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   0.536
_shelx_estimated_absorpt_t_max   0.607
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 0.49479(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 . . . . .
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 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_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_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) . . . . ?
