#------------------------------------------------------------------------------
#$Date: 2023-11-08 01:00:26 +0200 (Wed, 08 Nov 2023) $
#$Revision: 287473 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/23/7132310.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_7132310
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         '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
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-28 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            2
_cell_length_a                   21.0549(6)
_cell_length_b                   21.0549(6)
_cell_length_c                   31.7103(14)
_cell_measurement_reflns_used    40636
_cell_measurement_temperature    150
_cell_measurement_theta_max      63.98
_cell_measurement_theta_min      2.43
_cell_volume                     12174.1(7)
_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)'
_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_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
_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_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
_refine_diff_density_max         2.250
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.170
_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_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0696
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5261
_reflns_number_total             9933
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3cc00137g2.cif
_cod_data_source_block           1-p63m
_cod_original_cell_volume        12174.1(9)
_cod_database_code               7132310
_shelxl_version_number           2014-3
_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_max   0.564
_shelx_estimated_absorpt_t_min   0.444
_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)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
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'
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 . .
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'
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_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_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 . . . ?
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 ?
