#------------------------------------------------------------------------------
#$Date: 2016-07-07 05:35:11 +0300 (Thu, 07 Jul 2016) $
#$Revision: 184267 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/36/1543615.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_1543615
loop_
_publ_author_name
'Stauber, Julia'
'Mueller, Peter'
'Dai, Yizhe'
'Wu, Gang'
'Nocera, Daniel G.'
'Cummins, Christopher'
_publ_section_title
;
 Multi-electron reactivity of a cofacial di-tin(II) cryptand: Partial
 reduction of sulfur and selenium and reversible generation of
 S3●−
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C6SC01754A
_journal_year                    2016
_chemical_formula_sum            'C84 H132 K2 N12 O18 Pb2'
_chemical_formula_weight         2090.59
_chemical_name_systematic        '[K(Kryptofix-2,2,2)]2[Pb2(mBDCA-5t)]'
_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'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-26 deposited with the CCDC.
2016-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.2463(16)
_cell_length_b                   13.2463(16)
_cell_length_c                   29.783(4)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.83
_cell_measurement_theta_min      2.24
_cell_volume                     4525.7(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            113659
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.502
_diffrn_reflns_theta_min         1.367
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    3.881
_exptl_absorpt_correction_T_max  0.5282
_exptl_absorpt_correction_T_min  0.4842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2140
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         3.298
_refine_diff_density_min         -1.673
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5130
_refine_ls_number_restraints     546
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0178P)²+8.4443P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3431
_reflns_number_total             5130
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6sc01754a2.cif
_cod_data_source_block           Pb2
_cod_original_cell_volume        4525.7(12)
_cod_database_code               1543615
_shelx_shelxl_version_number     2014/7
_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   0.892
_shelx_estimated_absorpt_t_max   0.962
_solvent_exptl_crystal_recrystallization_method DMF/Et2O
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 0.0000 1.0000 0.30922(2) 0.01383(4) Uani 1 3 d S T P . .
O1 O 0.25568(17) 0.92881(17) 0.36436(6) 0.0211(4) Uani 1 1 d . . . . .
N1 N 0.18318(19) 1.04663(19) 0.34096(7) 0.0174(4) Uani 1 1 d D . . . .
N2 N 0.0000 1.0000 0.40512(12) 0.0183(6) Uani 1 3 d S T P . .
C1 C 0.2083(2) 1.1019(2) 0.38521(8) 0.0182(5) Uani 1 1 d . . . . .
H1A H 0.2099 1.1773 0.3832 0.022 Uiso 1 1 calc R U . . .
H1B H 0.2860 1.1177 0.3954 0.022 Uiso 1 1 calc R U . . .
C2 C 0.1161(2) 1.0235(2) 0.41924(8) 0.0204(5) Uani 1 1 d . . . . .
H2A H 0.1162 0.9490 0.4220 0.024 Uiso 1 1 calc R U . . .
H2B H 0.1351 1.0618 0.4490 0.024 Uiso 1 1 calc R U . . .
C3 C 0.2098(2) 0.9622(2) 0.33577(8) 0.0167(5) Uani 1 1 d D U . . .
C4 C 0.1756(9) 0.8990(13) 0.2936(5) 0.0126(16) Uani 0.385(3) 1 d D U P A -1
C5 C 0.2039(15) 0.9605(8) 0.2532(6) 0.0129(13) Uani 0.385(3) 1 d D U P A -1
H5 H 0.2414 1.0432 0.2535 0.015 Uiso 0.385(3) 1 calc R U P A -1
C6 C 0.177(2) 0.9005(13) 0.2122(5) 0.014(2) Uani 0.385(3) 1 d D U P A -1
C7 C 0.1179(17) 0.7782(12) 0.2128(7) 0.014(2) Uani 0.385(3) 1 d D U P A -1
H7 H 0.1003 0.7370 0.1851 0.017 Uiso 0.385(3) 1 calc R U P A -1
C8 C 0.0839(5) 0.7150(4) 0.2532(7) 0.0159(15) Uani 0.385(3) 1 d D U P A -1
C9 C 0.1164(16) 0.7781(12) 0.2930(7) 0.013(2) Uani 0.385(3) 1 d D U P A -1
H9 H 0.0975 0.7371 0.3207 0.016 Uiso 0.385(3) 1 calc R U P A -1
C10 C 0.0061(4) 0.5816(4) 0.2507(7) 0.0187(10) Uani 0.385(3) 1 d D U P A -1
C11 C 0.015(2) 0.5190(19) 0.2925(7) 0.024(3) Uani 0.385(3) 1 d D U P A -1
H11A H 0.0959 0.5377 0.2965 0.036 Uiso 0.385(3) 1 calc R U P A -1
H11B H -0.0352 0.4347 0.2888 0.036 Uiso 0.385(3) 1 calc R U P A -1
H11C H -0.0102 0.5447 0.3190 0.036 Uiso 0.385(3) 1 calc R U P A -1
C12 C -0.1214(5) 0.5542(6) 0.2549(8) 0.025(3) Uani 0.385(3) 1 d D U P A -1
H12A H -0.1737 0.4695 0.2551 0.038 Uiso 0.385(3) 1 calc R U P A -1
H12B H -0.1406 0.5882 0.2294 0.038 Uiso 0.385(3) 1 calc R U P A -1
H12C H -0.1309 0.5874 0.2829 0.038 Uiso 0.385(3) 1 calc R U P A -1
C13 C 0.0378(16) 0.5324(15) 0.2100(6) 0.022(3) Uani 0.385(3) 1 d D U P A -1
H13A H 0.1204 0.5553 0.2115 0.033 Uiso 0.385(3) 1 calc R U P A -1
H13B H 0.0231 0.5632 0.1824 0.033 Uiso 0.385(3) 1 calc R U P A -1
H13C H -0.0099 0.4472 0.2100 0.033 Uiso 0.385(3) 1 calc R U P A -1
C4A C 0.1860(17) 0.9057(18) 0.2927(8) 0.0126(16) Uani 0.115(3) 1 d D U P A -2
C5A C 0.203(5) 0.969(2) 0.2532(9) 0.0129(13) Uani 0.115(3) 1 d D U P A -2
H5A H 0.2294 1.0497 0.2545 0.015 Uiso 0.115(3) 1 calc R U P A -2
C6A C 0.180(7) 0.912(3) 0.2119(9) 0.014(2) Uani 0.115(3) 1 d D U P A -2
C7A C 0.142(5) 0.792(2) 0.2109(12) 0.014(2) Uani 0.115(3) 1 d D U P A -2
H7A H 0.1335 0.7549 0.1828 0.017 Uiso 0.115(3) 1 calc R U P A -2
C8A C 0.1179(17) 0.7273(12) 0.2506(11) 0.0159(15) Uani 0.115(3) 1 d D U P A -2
C9A C 0.147(4) 0.787(2) 0.2914(11) 0.013(2) Uani 0.115(3) 1 d D U P A -2
H9A H 0.1404 0.7464 0.3185 0.016 Uiso 0.115(3) 1 calc R U P A -2
C10A C 0.0772(13) 0.5960(12) 0.2500(12) 0.0211(19) Uani 0.115(3) 1 d D U P A -2
C11A C 0.014(5) 0.537(4) 0.2939(13) 0.024(3) Uani 0.115(3) 1 d D U P A -2
H11D H -0.0180 0.4527 0.2914 0.036 Uiso 0.115(3) 1 calc R U P A -2
H11E H -0.0487 0.5538 0.2994 0.036 Uiso 0.115(3) 1 calc R U P A -2
H11F H 0.0700 0.5673 0.3189 0.036 Uiso 0.115(3) 1 calc R U P A -2
C12A C 0.1858(13) 0.5815(15) 0.253(2) 0.025(3) Uani 0.115(3) 1 d D U P A -2
H12D H 0.2462 0.6372 0.2325 0.038 Uiso 0.115(3) 1 calc R U P A -2
H12E H 0.1644 0.5019 0.2440 0.038 Uiso 0.115(3) 1 calc R U P A -2
H12F H 0.2155 0.5960 0.2836 0.038 Uiso 0.115(3) 1 calc R U P A -2
C13A C -0.007(3) 0.535(3) 0.2112(10) 0.018(5) Uani 0.115(3) 1 d D U P A -2
H13D H 0.0318 0.5685 0.1827 0.026 Uiso 0.115(3) 1 calc R U P A -2
H13E H -0.0752 0.5457 0.2144 0.026 Uiso 0.115(3) 1 calc R U P A -2
H13F H -0.0333 0.4515 0.2118 0.026 Uiso 0.115(3) 1 calc R U P A -2
K1 K 0.3333 0.6667 0.51336(19) 0.0153(5) Uani 0.95(2) 3 d S T P B 1
K1A K 0.3333 0.6667 0.498(3) 0.0153(5) Uani 0.05(2) 3 d S T P B 2
N3 N 0.3333 0.6667 0.41238(12) 0.0161(7) Uani 1 3 d S T P B .
O12 O 0.14070(16) 0.65579(16) 0.46618(6) 0.0183(4) Uani 1 1 d . . . . .
O13 O 0.15398(16) 0.67644(17) 0.56024(6) 0.0205(4) Uani 1 1 d . . . . .
N4 N 0.3333 0.6667 0.61566(13) 0.0181(7) Uani 1 3 d S T P . .
C21 C 0.2176(2) 0.6390(2) 0.39559(8) 0.0189(5) Uani 1 1 d . . . . .
H21A H 0.1645 0.5537 0.3974 0.023 Uiso 1 1 calc R U . B 2
H21B H 0.2247 0.6616 0.3636 0.023 Uiso 1 1 calc R U . B 2
C22 C 0.1643(2) 0.6991(2) 0.42095(9) 0.0203(5) Uani 1 1 d . . . . .
H22A H 0.2187 0.7843 0.4211 0.024 Uiso 1 1 calc R U . B 2
H22B H 0.0911 0.6838 0.4062 0.024 Uiso 1 1 calc R U . B 2
C23 C 0.0816(2) 0.7026(2) 0.49087(9) 0.0223(6) Uani 1 1 d . . . . .
H23A H 0.0104 0.6882 0.4746 0.027 Uiso 1 1 calc R U . . .
H23B H 0.1327 0.7878 0.4945 0.027 Uiso 1 1 calc R U . . .
C24 C 0.0494(2) 0.6450(2) 0.53601(9) 0.0207(5) Uani 1 1 d . . . . .
H24A H 0.0015 0.6707 0.5527 0.025 Uiso 1 1 calc R U . . .
H24B H 0.0033 0.5593 0.5324 0.025 Uiso 1 1 calc R U . . .
C25 C 0.1290(2) 0.6179(2) 0.60269(9) 0.0212(5) Uani 1 1 d . . . . .
H25A H 0.1086 0.5357 0.5984 0.025 Uiso 1 1 calc R U . . .
H25B H 0.0622 0.6189 0.6172 0.025 Uiso 1 1 calc R U . . .
C26 C 0.2363(2) 0.6809(3) 0.63162(9) 0.0218(5) Uani 1 1 d . . . . .
H26A H 0.2614 0.7649 0.6322 0.026 Uiso 1 1 calc R U . . .
H26B H 0.2165 0.6510 0.6627 0.026 Uiso 1 1 calc R U . . .
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'
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'
K K 0.2009 0.2494 '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'
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
N1 Pb1 N1 105.26(6) . 3_465
N1 Pb1 N1 105.26(6) . 2_675
N1 Pb1 N1 105.26(6) 3_465 2_675
N1 Pb1 Pb1 113.41(5) . 10_556
N1 Pb1 Pb1 113.41(5) 3_465 10_556
N1 Pb1 Pb1 113.41(5) 2_675 10_556
C3 N1 C1 115.7(2) . .
C3 N1 Pb1 113.42(16) . .
C1 N1 Pb1 115.80(16) . .
C2 N2 C2 112.17(15) . 3_465
C2 N2 C2 112.17(15) . 2_675
C2 N2 C2 112.17(15) 3_465 2_675
N1 C1 C2 110.7(2) . .
N1 C1 H1A 109.5 . .
C2 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 108.1 . .
N2 C2 C1 110.5(2) . .
N2 C2 H2A 109.5 . .
C1 C2 H2A 109.5 . .
N2 C2 H2B 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 108.1 . .
O1 C3 N1 126.5(2) . .
O1 C3 C4A 116.3(9) . .
N1 C3 C4A 117.2(9) . .
O1 C3 C4 116.9(5) . .
N1 C3 C4 116.5(5) . .
C9 C4 C5 119.6(12) . .
C9 C4 C3 120.7(12) . .
C5 C4 C3 119.6(11) . .
C4 C5 C6 120.2(6) . .
C4 C5 H5 119.9 . .
C6 C5 H5 119.9 . .
C7 C6 C5 118.7(12) . .
C6 C7 C8 121.7(12) . .
C6 C7 H7 119.1 . .
C8 C7 H7 119.1 . .
C9 C8 C7 117.5(5) . .
C9 C8 C10 124.0(11) . .
C7 C8 C10 118.3(11) . .
C4 C9 C8 122.1(13) . .
C4 C9 H9 118.9 . .
C8 C9 H9 118.9 . .
C11 C10 C13 107.6(6) . .
C11 C10 C8 113.2(12) . .
C13 C10 C8 110.9(10) . .
C11 C10 C12 100.2(17) . .
C13 C10 C12 117.6(15) . .
C8 C10 C12 107.0(5) . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C10 C13 H13A 109.5 . .
C10 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C10 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C9A C4A C5A 121(2) . .
C9A C4A C3 118.2(18) . .
C5A C4A C3 120.9(18) . .
C4A C5A C6A 119.7(18) . .
C4A C5A H5A 120.1 . .
C6A C5A H5A 120.1 . .
C5A C6A C7A 119(2) . .
C6A C7A C8A 121(2) . .
C6A C7A H7A 119.4 . .
C8A C7A H7A 119.4 . .
C9A C8A C7A 118.2(14) . .
C9A C8A C10A 119.4(16) . .
C7A C8A C10A 121.7(17) . .
C4A C9A C8A 120.4(18) . .
C4A C9A H9A 119.8 . .
C8A C9A H9A 119.8 . .
C13A C10A C11A 108(2) . .
C13A C10A C8A 110.8(14) . .
C11A C10A C8A 111.0(18) . .
C13A C10A C12A 117(2) . .
C11A C10A C12A 101(3) . .
C8A C10A C12A 108.5(12) . .
C10A C11A H11D 109.5 . .
C10A C11A H11E 109.5 . .
H11D C11A H11E 109.5 . .
C10A C11A H11F 109.5 . .
H11D C11A H11F 109.5 . .
H11E C11A H11F 109.5 . .
C10A C12A H12D 109.5 . .
C10A C12A H12E 109.5 . .
H12D C12A H12E 109.5 . .
C10A C12A H12F 109.5 . .
H12D C12A H12F 109.5 . .
H12E C12A H12F 109.5 . .
C10A C13A H13D 109.5 . .
C10A C13A H13E 109.5 . .
H13D C13A H13E 109.5 . .
C10A C13A H13F 109.5 . .
H13D C13A H13F 109.5 . .
H13E C13A H13F 109.5 . .
O13 K1 O13 97.51(14) 3_565 .
O13 K1 O13 97.51(14) 3_565 2_665
O13 K1 O13 97.51(14) . 2_665
O13 K1 O12 59.49(5) 3_565 3_565
O13 K1 O12 123.89(5) . 3_565
O13 K1 O12 133.10(5) 2_665 3_565
O13 K1 O12 123.89(5) 3_565 2_665
O13 K1 O12 133.10(5) . 2_665
O13 K1 O12 59.49(5) 2_665 2_665
O12 K1 O12 97.82(14) 3_565 2_665
O13 K1 O12 133.10(5) 3_565 .
O13 K1 O12 59.49(5) . .
O13 K1 O12 123.89(5) 2_665 .
O12 K1 O12 97.82(14) 3_565 .
O12 K1 O12 97.82(14) 2_665 .
O13 K1 N3 119.75(11) 3_565 .
O13 K1 N3 119.75(11) . .
O13 K1 N3 119.75(11) 2_665 .
O12 K1 N3 60.49(11) 3_565 .
O12 K1 N3 60.49(11) 2_665 .
O12 K1 N3 60.49(11) . .
O13 K1 N4 60.25(11) 3_565 .
O13 K1 N4 60.25(11) . .
O13 K1 N4 60.25(11) 2_665 .
O12 K1 N4 119.51(11) 3_565 .
O12 K1 N4 119.51(11) 2_665 .
O12 K1 N4 119.51(11) . .
N3 K1 N4 180.0 . .
N3 K1A O12 69.0(16) . 3_565
N3 K1A O12 69.0(16) . 2_665
O12 K1A O12 107.9(17) 3_565 2_665
N3 K1A O12 69.0(16) . .
O12 K1A O12 107.9(17) 3_565 .
O12 K1A O12 107.9(17) 2_665 .
N3 K1A O13 127.1(12) . 3_565
O12 K1A O13 58.3(4) 3_565 3_565
O12 K1A O13 121.7(8) 2_665 3_565
O12 K1A O13 130.5(9) . 3_565
N3 K1A O13 127.1(12) . 2_665
O12 K1A O13 130.5(9) 3_565 2_665
O12 K1A O13 58.3(4) 2_665 2_665
O12 K1A O13 121.7(8) . 2_665
O13 K1A O13 87.4(18) 3_565 2_665
N3 K1A O13 127.1(12) . .
O12 K1A O13 121.7(8) 3_565 .
O12 K1A O13 130.5(9) 2_665 .
O12 K1A O13 58.3(4) . .
O13 K1A O13 87.4(18) 3_565 .
O13 K1A O13 87.4(18) 2_665 .
N3 K1A C21 24.4(6) . 3_565
O12 K1A C21 45.1(11) 3_565 3_565
O12 K1A C21 86(2) 2_665 3_565
O12 K1A C21 78.6(18) . 3_565
O13 K1A C21 103.4(7) 3_565 3_565
O13 K1A C21 141.8(13) 2_665 3_565
O13 K1A C21 129.0(10) . 3_565
N3 K1A C21 24.4(6) . 2_665
O12 K1A C21 78.6(18) 3_565 2_665
O12 K1A C21 45.1(11) 2_665 2_665
O12 K1A C21 86(2) . 2_665
O13 K1A C21 129.0(10) 3_565 2_665
O13 K1A C21 103.4(7) 2_665 2_665
O13 K1A C21 141.8(13) . 2_665
C21 K1A C21 41.9(10) 3_565 2_665
N3 K1A C21 24.4(6) . .
O12 K1A C21 86(2) 3_565 .
O12 K1A C21 78.6(18) 2_665 .
O12 K1A C21 45.1(11) . .
O13 K1A C21 141.8(13) 3_565 .
O13 K1A C21 129.0(10) 2_665 .
O13 K1A C21 103.4(7) . .
C21 K1A C21 41.9(10) 3_565 .
C21 K1A C21 41.9(10) 2_665 .
N3 K1A C22 47.1(10) . 3_565
O12 K1A C22 23.8(6) 3_565 3_565
O12 K1A C22 88.5(16) 2_665 3_565
O12 K1A C22 102(2) . 3_565
O13 K1A C22 80.1(2) 3_565 3_565
O13 K1A C22 130.4(3) 2_665 3_565
O13 K1A C22 138.9(3) . 3_565
C21 K1A C22 25.8(5) 3_565 3_565
C21 K1A C22 54.8(11) 2_665 3_565
C21 K1A C22 67.6(15) . 3_565
N3 K1A C22 47.1(10) . 2_665
O12 K1A C22 102(2) 3_565 2_665
O12 K1A C22 23.8(6) 2_665 2_665
O12 K1A C22 88.5(16) . 2_665
O13 K1A C22 138.9(3) 3_565 2_665
O13 K1A C22 80.1(2) 2_665 2_665
O13 K1A C22 130.4(3) . 2_665
C21 K1A C22 67.6(15) 3_565 2_665
C21 K1A C22 25.8(5) 2_665 2_665
C21 K1A C22 54.8(11) . 2_665
C22 K1A C22 78.8(15) 3_565 2_665
C21 N3 C21 109.10(17) . 3_565
C21 N3 C21 109.11(17) . 2_665
C21 N3 C21 109.11(17) 3_565 2_665
C21 N3 K1A 109.84(16) . .
C21 N3 K1A 109.83(16) 3_565 .
C21 N3 K1A 109.83(16) 2_665 .
C21 N3 K1 109.84(16) . .
C21 N3 K1 109.83(16) 3_565 .
C21 N3 K1 109.83(16) 2_665 .
C23 O12 C22 111.63(19) . .
C23 O12 K1A 120.9(14) . .
C22 O12 K1A 107.7(15) . .
C23 O12 K1 113.38(17) . .
C22 O12 K1 115.52(17) . .
C24 O13 C25 111.1(2) . .
C24 O13 K1 117.02(17) . .
C25 O13 K1 112.64(17) . .
C24 O13 K1A 110.1(12) . .
C25 O13 K1A 118.9(10) . .
C26 N4 C26 110.05(17) 3_565 2_665
C26 N4 C26 110.05(17) 3_565 .
C26 N4 C26 110.05(17) 2_665 .
C26 N4 K1 108.89(17) 3_565 .
C26 N4 K1 108.89(17) 2_665 .
C26 N4 K1 108.89(17) . .
N3 C21 C22 113.8(2) . .
N3 C21 K1A 45.8(6) . .
C22 C21 K1A 78.1(5) . .
N3 C21 H21A 108.8 . .
C22 C21 H21A 108.8 . .
K1A C21 H21A 95.7 . .
N3 C21 H21B 108.8 . .
C22 C21 H21B 108.8 . .
K1A C21 H21B 151.1 . .
H21A C21 H21B 107.7 . .
O12 C22 C21 109.0(2) . .
O12 C22 K1A 48.5(9) . .
C21 C22 K1A 76.1(10) . .
O12 C22 H22A 109.9 . .
C21 C22 H22A 109.9 . .
K1A C22 H22A 89.5 . .
O12 C22 H22B 109.9 . .
C21 C22 H22B 109.9 . .
K1A C22 H22B 156.9 . .
H22A C22 H22B 108.3 . .
O12 C23 C24 108.7(2) . .
O12 C23 H23A 110.0 . .
C24 C23 H23A 110.0 . .
O12 C23 H23B 110.0 . .
C24 C23 H23B 110.0 . .
H23A C23 H23B 108.3 . .
O13 C24 C23 108.5(2) . .
O13 C24 H24A 110.0 . .
C23 C24 H24A 110.0 . .
O13 C24 H24B 110.0 . .
C23 C24 H24B 110.0 . .
H24A C24 H24B 108.4 . .
O13 C25 C26 107.8(2) . .
O13 C25 H25A 110.1 . .
C26 C25 H25A 110.1 . .
O13 C25 H25B 110.1 . .
C26 C25 H25B 110.1 . .
H25A C25 H25B 108.5 . .
N4 C26 C25 112.8(2) . .
N4 C26 H26A 109.0 . .
C25 C26 H26A 109.0 . .
N4 C26 H26B 109.0 . .
C25 C26 H26B 109.0 . .
H26A C26 H26B 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 N1 2.380(2) .
Pb1 N1 2.380(2) 3_465
Pb1 N1 2.380(2) 2_675
Pb1 Pb1 3.5274(5) 10_556
O1 C3 1.248(3) .
N1 C3 1.340(3) .
N1 C1 1.463(3) .
N2 C2 1.470(3) .
N2 C2 1.470(3) 3_465
N2 C2 1.470(3) 2_675
C1 C2 1.526(4) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4A 1.44(2) .
C3 C4 1.450(16) .
C4 C9 1.387(12) .
C4 C5 1.395(11) .
C5 C6 1.403(11) .
C5 H5 0.9500 .
C6 C7 1.403(12) .
C7 C8 1.405(11) .
C7 H7 0.9500 .
C8 C9 1.390(11) .
C8 C10 1.539(7) .
C9 H9 0.9500 .
C10 C11 1.532(12) .
C10 C13 1.533(11) .
C10 C12 1.544(7) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C4A C9A 1.387(16) .
C4A C5A 1.392(15) .
C5A C6A 1.395(16) .
C5A H5A 0.9500 .
C6A C7A 1.401(16) .
C7A C8A 1.404(16) .
C7A H7A 0.9500 .
C8A C9A 1.396(16) .
C8A C10A 1.542(14) .
C9A H9A 0.9500 .
C10A C13A 1.530(14) .
C10A C11A 1.536(15) .
C10A C12A 1.546(13) .
C11A H11D 0.9800 .
C11A H11E 0.9800 .
C11A H11F 0.9800 .
C12A H12D 0.9800 .
C12A H12E 0.9800 .
C12A H12F 0.9800 .
C13A H13D 0.9800 .
C13A H13E 0.9800 .
C13A H13F 0.9800 .
K1 O13 2.814(3) 3_565
K1 O13 2.814(3) .
K1 O13 2.814(3) 2_665
K1 O12 2.853(3) 3_565
K1 O12 2.853(3) 2_665
K1 O12 2.853(3) .
K1 N3 3.008(7) .
K1 N4 3.047(7) .
K1A N3 2.56(8) .
K1A O12 2.66(3) 3_565
K1A O12 2.66(3) 2_665
K1A O12 2.66(3) .
K1A O13 3.06(5) 3_565
K1A O13 3.06(5) 2_665
K1A O13 3.06(5) .
K1A C21 3.36(7) 3_565
K1A C21 3.36(7) 2_665
K1A C21 3.36(7) .
K1A C22 3.38(6) 3_565
K1A C22 3.38(6) 2_665
N3 C21 1.474(3) .
N3 C21 1.474(3) 3_565
N3 C21 1.474(3) 2_665
O12 C23 1.423(3) .
O12 C22 1.436(3) .
O13 C24 1.427(3) .
O13 C25 1.433(3) .
N4 C26 1.468(3) 3_565
N4 C26 1.468(3) 2_665
N4 C26 1.468(3) .
C21 C22 1.504(4) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 C24 1.499(4) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C25 C26 1.507(4) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
