#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/84/4318408.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_4318408
loop_
_publ_author_name
'David Esteban'
'Fernando Avecilla'
'Carlos Platas-Iglesias'
'Jose Mahía'
'Andrés de Blas'
'Teresa Rodríguez-Blas'
_publ_section_title
;
 Lead(II) Complexes with Macrocyclic Receptors Derived from
 4,13-Diaza-18-crown-6
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4337
_journal_page_last               4347
_journal_paper_doi               10.1021/ic0255095
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C40 H50 Cl N4 O11.5 Pb'
_chemical_formula_weight         1013.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.1290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   40.3616(6)
_cell_length_b                   10.59050(10)
_cell_length_c                   19.8960(3)
_cell_measurement_temperature    298(2)
_cell_volume                     8372.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0771
_diffrn_reflns_limit_h_max       53
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27930
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    4.159
_exptl_absorpt_correction_T_max  0.5743
_exptl_absorpt_correction_T_min  0.2870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             4072
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.044
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         10323
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0516P)²+14.4890P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1300
_reflns_number_gt                5982
_reflns_number_total             10323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255095_s2_3.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        8371.99(19)
_cod_original_formula_sum        'C40 H50 Cl N4 O11.50 Pb'
_cod_database_code               4318408
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.102834(6) 0.74262(2) 0.983693(12) 0.04419(9) Uani 1 1 d . . .
O1 O 0.07992(12) 0.5546(5) 1.0115(3) 0.0686(15) Uani 1 1 d . . .
O2 O 0.04111(12) 0.7441(4) 0.9079(3) 0.0602(12) Uani 1 1 d . . .
O3 O 0.04811(13) 0.8635(5) 1.0313(3) 0.0675(14) Uani 1 1 d . . .
O4 O 0.13708(12) 0.9151(4) 0.9149(2) 0.0563(12) Uani 1 1 d . . .
O5 O 0.16562(11) 0.8407(4) 1.0432(2) 0.0516(11) Uani 1 1 d . . .
O6 O 0.19576(12) 0.5078(5) 1.1715(3) 0.0665(14) Uani 1 1 d . . .
H6 H 0.1818 0.5444 1.1898 0.100 Uiso 1 1 calc R . .
N1 N 0.14605(13) 0.5773(5) 0.9765(3) 0.0467(13) Uani 1 1 d . . .
N2 N 0.17337(14) 0.6466(4) 1.2610(3) 0.0468(13) Uani 1 1 d . . .
N3 N 0.10034(14) 0.7004(5) 0.8509(3) 0.0477(13) Uani 1 1 d . . .
N4 N 0.11174(14) 0.8137(5) 1.1308(3) 0.0493(13) Uani 1 1 d . . .
C1 C 0.12718(17) 0.4231(6) 1.0536(3) 0.0478(16) Uani 1 1 d . . .
C2 C 0.13920(19) 0.3208(6) 1.0962(3) 0.0546(18) Uani 1 1 d . . .
H2 H 0.1615 0.2954 1.0993 0.066 Uiso 1 1 calc R . .
C3 C 0.1188(2) 0.2578(6) 1.1330(4) 0.0612(19) Uani 1 1 d . . .
H3 H 0.1273 0.1914 1.1615 0.073 Uiso 1 1 calc R . .
C4 C 0.0857(2) 0.2933(7) 1.1277(4) 0.065(2) Uani 1 1 d . . .
H4 H 0.0716 0.2499 1.1521 0.078 Uiso 1 1 calc R . .
C5 C 0.07322(19) 0.3926(6) 1.0865(4) 0.062(2) Uani 1 1 d . . .
H5 H 0.0507 0.4153 1.0834 0.074 Uiso 1 1 calc R . .
C6 C 0.09367(17) 0.4609(6) 1.0487(4) 0.0521(17) Uani 1 1 d . . .
C7 C 0.15065(17) 0.4766(6) 1.0143(3) 0.0488(17) Uani 1 1 d . . .
H7 H 0.1711 0.4348 1.0162 0.059 Uiso 1 1 calc R . .
C8 C 0.17187(18) 0.6078(6) 0.9398(4) 0.0487(17) Uani 1 1 d . . .
C9 C 0.20509(19) 0.6177(6) 0.9696(4) 0.0604(19) Uani 1 1 d . . .
H9 H 0.2113 0.6057 1.0164 0.073 Uiso 1 1 calc R . .
C10 C 0.2294(2) 0.6456(7) 0.9306(5) 0.070(2) Uani 1 1 d . . .
H10 H 0.2519 0.6506 0.9515 0.084 Uiso 1 1 calc R . .
C11 C 0.2209(2) 0.6661(7) 0.8615(5) 0.071(2) Uani 1 1 d . . .
H11 H 0.2372 0.6850 0.8353 0.085 Uiso 1 1 calc R . .
C12 C 0.1875(2) 0.6578(6) 0.8322(4) 0.063(2) Uani 1 1 d . . .
H12 H 0.1816 0.6703 0.7853 0.076 Uiso 1 1 calc R . .
C13 C 0.16230(18) 0.6317(6) 0.8694(4) 0.0510(17) Uani 1 1 d . . .
C14 C 0.12656(18) 0.6134(6) 0.8336(4) 0.0540(18) Uani 1 1 d . . .
H14A H 0.1263 0.6197 0.7849 0.065 Uiso 1 1 calc R . .
H14B H 0.1199 0.5279 0.8427 0.065 Uiso 1 1 calc R . .
C15 C 0.10086(18) 0.8281(6) 0.8193(4) 0.0547(18) Uani 1 1 d . . .
H15A H 0.0817 0.8756 0.8289 0.066 Uiso 1 1 calc R . .
H15B H 0.0981 0.8180 0.7702 0.066 Uiso 1 1 calc R . .
C16 C 0.13200(19) 0.9040(6) 0.8428(4) 0.0585(19) Uani 1 1 d . . .
H16A H 0.1512 0.8628 0.8291 0.070 Uiso 1 1 calc R . .
H16B H 0.1296 0.9872 0.8221 0.070 Uiso 1 1 calc R . .
C17 C 0.16980(18) 0.9580(7) 0.9445(4) 0.0597(19) Uani 1 1 d . . .
H17A H 0.1738 1.0411 0.9272 0.072 Uiso 1 1 calc R . .
H17B H 0.1867 0.9006 0.9332 0.072 Uiso 1 1 calc R . .
C18 C 0.17159(19) 0.9630(6) 1.0209(4) 0.0582(19) Uani 1 1 d . . .
H18A H 0.1936 0.9920 1.0430 0.070 Uiso 1 1 calc R . .
H18B H 0.1548 1.0209 1.0322 0.070 Uiso 1 1 calc R . .
C19 C 0.17163(19) 0.8242(7) 1.1162(4) 0.0610(19) Uani 1 1 d . . .
H19A H 0.1927 0.8648 1.1355 0.073 Uiso 1 1 calc R . .
H19B H 0.1739 0.7348 1.1266 0.073 Uiso 1 1 calc R . .
C20 C 0.14427(18) 0.8775(6) 1.1489(3) 0.0579(19) Uani 1 1 d . . .
H20A H 0.1513 0.8738 1.1980 0.069 Uiso 1 1 calc R . .
H20B H 0.1413 0.9658 1.1362 0.069 Uiso 1 1 calc R . .
C21 C 0.0840(2) 0.9041(7) 1.1358(4) 0.068(2) Uani 1 1 d . . .
H21A H 0.0840 0.9205 1.1838 0.082 Uiso 1 1 calc R . .
H21B H 0.0890 0.9832 1.1151 0.082 Uiso 1 1 calc R . .
C22 C 0.0511(2) 0.8651(9) 1.1048(4) 0.084(3) Uani 1 1 d . . .
H22A H 0.0346 0.9226 1.1177 0.100 Uiso 1 1 calc R . .
H22B H 0.0466 0.7814 1.1209 0.100 Uiso 1 1 calc R . .
C23 C 0.0168(2) 0.8156(10) 0.9991(5) 0.090(3) Uani 1 1 d . . .
H23A H -0.0011 0.8664 1.0116 0.108 Uiso 1 1 calc R . .
H23B H 0.0142 0.7298 1.0144 0.108 Uiso 1 1 calc R . .
C24 C 0.0144(2) 0.8169(9) 0.9248(4) 0.077(2) Uani 1 1 d . . .
H24A H -0.0070 0.7818 0.9031 0.093 Uiso 1 1 calc R . .
H24B H 0.0159 0.9029 0.9089 0.093 Uiso 1 1 calc R . .
C25 C 0.03712(19) 0.7124(7) 0.8375(4) 0.064(2) Uani 1 1 d . . .
H25A H 0.0350 0.7885 0.8100 0.077 Uiso 1 1 calc R . .
H25B H 0.0170 0.6620 0.8242 0.077 Uiso 1 1 calc R . .
C26 C 0.06726(18) 0.6395(7) 0.8267(4) 0.063(2) Uani 1 1 d . . .
H26A H 0.0670 0.5587 0.8495 0.076 Uiso 1 1 calc R . .
H26B H 0.0653 0.6228 0.7782 0.076 Uiso 1 1 calc R . .
C27 C 0.11028(17) 0.6952(6) 1.1717(3) 0.0492(16) Uani 1 1 d . . .
H27A H 0.1275 0.6378 1.1615 0.059 Uiso 1 1 calc R . .
H27B H 0.0887 0.6552 1.1563 0.059 Uiso 1 1 calc R . .
C28 C 0.11495(17) 0.7107(6) 1.2481(3) 0.0467(15) Uani 1 1 d . . .
C29 C 0.08787(19) 0.7443(6) 1.2791(4) 0.0603(18) Uani 1 1 d . . .
H29 H 0.0668 0.7550 1.2518 0.072 Uiso 1 1 calc R . .
C30 C 0.0910(2) 0.7621(7) 1.3473(4) 0.065(2) Uani 1 1 d . . .
H30 H 0.0723 0.7857 1.3660 0.078 Uiso 1 1 calc R . .
C31 C 0.1217(2) 0.7452(6) 1.3892(4) 0.0583(18) Uani 1 1 d . . .
H31 H 0.1238 0.7572 1.4361 0.070 Uiso 1 1 calc R . .
C32 C 0.14915(19) 0.7107(6) 1.3615(3) 0.0517(17) Uani 1 1 d . . .
H32 H 0.1699 0.6997 1.3898 0.062 Uiso 1 1 calc R . .
C33 C 0.14639(16) 0.6920(6) 1.2911(3) 0.0439(15) Uani 1 1 d . . .
C34 C 0.20351(17) 0.6662(6) 1.2890(3) 0.0474(16) Uani 1 1 d . . .
H34 H 0.2078 0.7159 1.3281 0.057 Uiso 1 1 calc R . .
C35 C 0.23161(16) 0.6137(6) 1.2620(3) 0.0478(16) Uani 1 1 d . . .
C36 C 0.26456(18) 0.6383(6) 1.2948(4) 0.0563(18) Uani 1 1 d . . .
H36 H 0.2683 0.6891 1.3335 0.068 Uiso 1 1 calc R . .
C37 C 0.29172(19) 0.5880(7) 1.2702(4) 0.066(2) Uani 1 1 d . . .
H37 H 0.3136 0.6056 1.2918 0.079 Uiso 1 1 calc R . .
C38 C 0.2860(2) 0.5113(7) 1.2131(5) 0.070(2) Uani 1 1 d . . .
H38 H 0.3042 0.4759 1.1971 0.084 Uiso 1 1 calc R . .
C39 C 0.2545(2) 0.4864(7) 1.1799(4) 0.063(2) Uani 1 1 d . . .
H39 H 0.2513 0.4360 1.1411 0.075 Uiso 1 1 calc R . .
C40 C 0.22681(18) 0.5366(6) 1.2041(4) 0.0518(17) Uani 1 1 d . . .
Cl2 Cl 0.2500 0.2500 1.0000 0.0655(7) Uani 1 2 d SDU . .
Cl1 Cl 0.0000 0.9548(3) 1.2500 0.0763(8) Uani 1 2 d S . .
O1W O 0.01618(15) 0.4772(7) 0.9448(3) 0.114(2) Uani 1 1 d . . .
O7 O 0.02616(15) 1.0292(6) 1.2332(4) 0.109(2) Uani 1 1 d . . .
O8 O 0.0128(2) 0.8778(10) 1.3048(5) 0.210(5) Uani 1 1 d . . .
O2W O -0.0045(3) 0.3980(11) 0.8143(6) 0.085(3) Uiso 0.50 1 d P . .
O9 O 0.2588(6) 0.1581(19) 1.0472(9) 0.155(8) Uani 0.485(15) 1 d PDU . 1
O10 O 0.2602(7) 0.3625(18) 1.0276(14) 0.165(8) Uani 0.485(15) 1 d PDU . 1
O11 O 0.2749(6) 0.265(3) 1.0501(11) 0.182(8) Uani 0.515(15) 1 d PDU . 2
O12 O 0.2220(5) 0.2703(18) 1.0294(12) 0.174(9) Uani 0.515(15) 1 d PDU . 2
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
O1 Pb1 N1 73.81(18) . . ?
O1 Pb1 N3 98.41(18) . . ?
N1 Pb1 N3 74.33(17) . . ?
O1 Pb1 O2 76.52(15) . . ?
N1 Pb1 O2 124.28(16) . . ?
N3 Pb1 O2 64.74(16) . . ?
O1 Pb1 O4 159.72(18) . . ?
N1 Pb1 O4 91.11(16) . . ?
N3 Pb1 O4 63.81(15) . . ?
O2 Pb1 O4 102.25(14) . . ?
O1 Pb1 O5 126.20(14) . . ?
N1 Pb1 O5 72.21(15) . . ?
N3 Pb1 O5 110.77(15) . . ?
O2 Pb1 O5 156.85(13) . . ?
O4 Pb1 O5 58.35(13) . . ?
O1 Pb1 O3 86.62(17) . . ?
N1 Pb1 O3 157.48(17) . . ?
N3 Pb1 O3 120.54(15) . . ?
O2 Pb1 O3 59.10(15) . . ?
O4 Pb1 O3 110.39(15) . . ?
O5 Pb1 O3 112.88(14) . . ?
O1 Pb1 N4 88.10(17) . . ?
N1 Pb1 N4 105.60(16) . . ?
N3 Pb1 N4 173.11(15) . . ?
O2 Pb1 N4 119.41(15) . . ?
O4 Pb1 N4 109.38(14) . . ?
O5 Pb1 N4 63.12(14) . . ?
O3 Pb1 N4 61.82(14) . . ?
C6 O1 Pb1 130.2(4) . . ?
C24 O2 C25 113.9(5) . . ?
C24 O2 Pb1 122.8(4) . . ?
C25 O2 Pb1 119.1(4) . . ?
C23 O3 C22 111.9(7) . . ?
C23 O3 Pb1 111.8(5) . . ?
C22 O3 Pb1 114.2(4) . . ?
C16 O4 C17 113.8(5) . . ?
C16 O4 Pb1 116.5(4) . . ?
C17 O4 Pb1 120.6(4) . . ?
C18 O5 C19 114.9(5) . . ?
C18 O5 Pb1 113.7(4) . . ?
C19 O5 Pb1 111.1(4) . . ?
C7 N1 C8 116.3(6) . . ?
C7 N1 Pb1 125.0(5) . . ?
C8 N1 Pb1 117.2(4) . . ?
C34 N2 C33 120.7(6) . . ?
C26 N3 C14 107.0(5) . . ?
C26 N3 C15 109.6(5) . . ?
C14 N3 C15 113.6(5) . . ?
C26 N3 Pb1 105.6(4) . . ?
C14 N3 Pb1 115.4(4) . . ?
C15 N3 Pb1 105.3(4) . . ?
C20 N4 C21 109.8(6) . . ?
C20 N4 C27 111.8(5) . . ?
C21 N4 C27 113.6(5) . . ?
C20 N4 Pb1 107.8(4) . . ?
C21 N4 Pb1 105.4(4) . . ?
C27 N4 Pb1 108.1(4) . . ?
C6 C1 C2 119.3(6) . . ?
C6 C1 C7 124.6(6) . . ?
C2 C1 C7 116.0(6) . . ?
C3 C2 C1 121.4(7) . . ?
C2 C3 C4 119.6(7) . . ?
C5 C4 C3 120.3(8) . . ?
C4 C5 C6 121.6(7) . . ?
O1 C6 C1 124.6(6) . . ?
O1 C6 C5 117.6(6) . . ?
C1 C6 C5 117.8(6) . . ?
N1 C7 C1 126.4(6) . . ?
C9 C8 C13 119.5(7) . . ?
C9 C8 N1 123.3(7) . . ?
C13 C8 N1 117.2(6) . . ?
C8 C9 C10 120.6(8) . . ?
C11 C10 C9 121.0(8) . . ?
C12 C11 C10 118.0(8) . . ?
C11 C12 C13 122.9(8) . . ?
C12 C13 C8 117.9(7) . . ?
C12 C13 C14 120.4(7) . . ?
C8 C13 C14 121.3(6) . . ?
N3 C14 C13 118.3(5) . . ?
N3 C15 C16 115.4(5) . . ?
O4 C16 C15 108.9(6) . . ?
O4 C17 C18 107.7(6) . . ?
O5 C18 C17 107.7(5) . . ?
O5 C19 C20 112.9(6) . . ?
N4 C20 C19 114.9(6) . . ?
C22 C21 N4 116.1(7) . . ?
C21 C22 O3 110.3(7) . . ?
O3 C23 C24 110.6(8) . . ?
O2 C24 C23 108.5(7) . . ?
O2 C25 C26 108.1(6) . . ?
N3 C26 C25 116.1(6) . . ?
N4 C27 C28 116.4(5) . . ?
C29 C28 C33 117.2(6) . . ?
C29 C28 C27 120.4(6) . . ?
C33 C28 C27 122.4(6) . . ?
C30 C29 C28 122.6(7) . . ?
C29 C30 C31 120.2(7) . . ?
C32 C31 C30 119.7(7) . . ?
C31 C32 C33 120.9(7) . . ?
C32 C33 C28 119.4(6) . . ?
C32 C33 N2 122.7(6) . . ?
C28 C33 N2 117.8(6) . . ?
N2 C34 C35 122.0(6) . . ?
C40 C35 C36 118.4(7) . . ?
C40 C35 C34 121.7(6) . . ?
C36 C35 C34 119.9(6) . . ?
C37 C36 C35 120.8(7) . . ?
C38 C37 C36 119.2(7) . . ?
C39 C38 C37 121.6(8) . . ?
C38 C39 C40 119.9(8) . . ?
O6 C40 C35 121.0(6) . . ?
O6 C40 C39 118.9(7) . . ?
C35 C40 C39 120.1(7) . . ?
O11 Cl2 O11 180.0(16) . 7_557 ?
O11 Cl2 O10 55.9(11) . . ?
O11 Cl2 O10 124.1(11) 7_557 . ?
O11 Cl2 O10 124.1(11) . 7_557 ?
O11 Cl2 O10 55.9(11) 7_557 7_557 ?
O10 Cl2 O10 180.000(6) . 7_557 ?
O11 Cl2 O9 121.3(11) . 7_557 ?
O11 Cl2 O9 58.7(11) 7_557 7_557 ?
O10 Cl2 O9 70.8(15) . 7_557 ?
O10 Cl2 O9 109.2(15) 7_557 7_557 ?
O11 Cl2 O9 58.7(11) . . ?
O11 Cl2 O9 121.3(11) 7_557 . ?
O10 Cl2 O9 109.2(15) . . ?
O10 Cl2 O9 70.8(15) 7_557 . ?
O9 Cl2 O9 180.000(7) 7_557 . ?
O11 Cl2 O12 76.2(16) . 7_557 ?
O11 Cl2 O12 103.8(16) 7_557 7_557 ?
O10 Cl2 O12 95.5(12) . 7_557 ?
O10 Cl2 O12 84.5(12) 7_557 7_557 ?
O9 Cl2 O12 87.2(13) 7_557 7_557 ?
O9 Cl2 O12 92.8(13) . 7_557 ?
O11 Cl2 O12 103.8(16) . . ?
O11 Cl2 O12 76.2(16) 7_557 . ?
O10 Cl2 O12 84.5(12) . . ?
O10 Cl2 O12 95.5(12) 7_557 . ?
O9 Cl2 O12 92.8(13) 7_557 . ?
O9 Cl2 O12 87.2(13) . . ?
O12 Cl2 O12 180.0(7) 7_557 . ?
O8 Cl1 O8 107.9(11) 2_557 . ?
O8 Cl1 O7 109.0(6) 2_557 2_557 ?
O8 Cl1 O7 109.5(5) . 2_557 ?
O8 Cl1 O7 109.5(5) 2_557 . ?
O8 Cl1 O7 109.0(6) . . ?
O7 Cl1 O7 111.8(6) 2_557 . ?
Cl2 O9 O10 54.3(9) . 7_557 ?
Cl2 O10 O9 54.9(9) . 7_557 ?
Cl2 O11 O12 54.2(10) . 7_557 ?
Cl2 O12 O11 49.6(8) . 7_557 ?
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 O1 2.304(5) . ?
Pb1 N1 2.493(5) . ?
Pb1 N3 2.665(5) . ?
Pb1 O2 2.675(4) . ?
Pb1 O4 2.791(4) . ?
Pb1 O5 2.801(4) . ?
Pb1 O3 2.855(5) . ?
Pb1 N4 2.982(5) . ?
O1 C6 1.302(7) . ?
O2 C24 1.412(9) . ?
O2 C25 1.422(9) . ?
O3 C23 1.406(10) . ?
O3 C22 1.446(9) . ?
O4 C16 1.417(8) . ?
O4 C17 1.423(8) . ?
O5 C18 1.403(7) . ?
O5 C19 1.441(8) . ?
O6 C40 1.342(8) . ?
N1 C7 1.299(7) . ?
N1 C8 1.411(8) . ?
N2 C34 1.263(7) . ?
N2 C33 1.416(8) . ?
N3 C26 1.484(8) . ?
N3 C14 1.487(8) . ?
N3 C15 1.493(8) . ?
N4 C20 1.464(8) . ?
N4 C21 1.488(9) . ?
N4 C27 1.503(8) . ?
C1 C6 1.397(9) . ?
C1 C2 1.408(9) . ?
C1 C7 1.447(9) . ?
C2 C3 1.369(10) . ?
C3 C4 1.374(11) . ?
C4 C5 1.372(9) . ?
C5 C6 1.410(9) . ?
C8 C9 1.372(9) . ?
C8 C13 1.409(9) . ?
C9 C10 1.387(10) . ?
C10 C11 1.375(11) . ?
C11 C12 1.373(10) . ?
C12 C13 1.388(9) . ?
C13 C14 1.504(9) . ?
C15 C16 1.496(9) . ?
C17 C18 1.511(9) . ?
C19 C20 1.488(10) . ?
C21 C22 1.426(10) . ?
C23 C24 1.464(12) . ?
C25 C26 1.488(10) . ?
C27 C28 1.507(9) . ?
C28 C29 1.392(9) . ?
C28 C33 1.415(8) . ?
C29 C30 1.355(10) . ?
C30 C31 1.379(11) . ?
C31 C32 1.371(10) . ?
C32 C33 1.398(9) . ?
C34 C35 1.448(9) . ?
C35 C40 1.397(9) . ?
C35 C36 1.399(9) . ?
C36 C37 1.383(10) . ?
C37 C38 1.383(11) . ?
C38 C39 1.348(10) . ?
C39 C40 1.399(9) . ?
Cl2 O11 1.295(12) . ?
Cl2 O11 1.295(12) 7_557 ?
Cl2 O10 1.346(12) . ?
Cl2 O10 1.346(12) 7_557 ?
Cl2 O9 1.355(11) 7_557 ?
Cl2 O9 1.355(11) . ?
Cl2 O12 1.378(13) 7_557 ?
Cl2 O12 1.378(13) . ?
Cl1 O8 1.387(8) 2_557 ?
Cl1 O8 1.387(8) . ?
Cl1 O7 1.403(6) 2_557 ?
Cl1 O7 1.403(6) . ?
O9 O10 1.57(3) 7_557 ?
O10 O9 1.57(3) 7_557 ?
O11 O12 1.65(3) 7_557 ?
O12 O11 1.65(3) 7_557 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H6 N2 0.82 1.86 2.592(7) 147.7 .
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
N1 Pb1 O1 C6 40.9(6) . . . . ?
N3 Pb1 O1 C6 111.7(6) . . . . ?
O2 Pb1 O1 C6 173.1(7) . . . . ?
O4 Pb1 O1 C6 84.2(8) . . . . ?
O5 Pb1 O1 C6 -11.8(7) . . . . ?
O3 Pb1 O1 C6 -127.9(6) . . . . ?
N4 Pb1 O1 C6 -66.0(6) . . . . ?
O1 Pb1 O2 C24 103.2(6) . . . . ?
N1 Pb1 O2 C24 162.5(6) . . . . ?
N3 Pb1 O2 C24 -150.6(6) . . . . ?
O4 Pb1 O2 C24 -97.6(6) . . . . ?
O5 Pb1 O2 C24 -66.7(7) . . . . ?
O3 Pb1 O2 C24 9.0(6) . . . . ?
N4 Pb1 O2 C24 23.2(6) . . . . ?
O1 Pb1 O2 C25 -101.2(5) . . . . ?
N1 Pb1 O2 C25 -41.9(5) . . . . ?
N3 Pb1 O2 C25 5.0(4) . . . . ?
O4 Pb1 O2 C25 58.0(5) . . . . ?
O5 Pb1 O2 C25 88.9(6) . . . . ?
O3 Pb1 O2 C25 164.6(5) . . . . ?
N4 Pb1 O2 C25 178.8(4) . . . . ?
O1 Pb1 O3 C23 -53.9(6) . . . . ?
N1 Pb1 O3 C23 -83.2(7) . . . . ?
N3 Pb1 O3 C23 43.9(6) . . . . ?
O2 Pb1 O3 C23 22.5(5) . . . . ?
O4 Pb1 O3 C23 114.8(5) . . . . ?
O5 Pb1 O3 C23 178.0(5) . . . . ?
N4 Pb1 O3 C23 -143.5(6) . . . . ?
O1 Pb1 O3 C22 74.5(6) . . . . ?
N1 Pb1 O3 C22 45.1(8) . . . . ?
N3 Pb1 O3 C22 172.3(5) . . . . ?
O2 Pb1 O3 C22 150.8(6) . . . . ?
O4 Pb1 O3 C22 -116.8(5) . . . . ?
O5 Pb1 O3 C22 -53.6(6) . . . . ?
N4 Pb1 O3 C22 -15.1(5) . . . . ?
O1 Pb1 O4 C16 39.3(7) . . . . ?
N1 Pb1 O4 C16 80.6(4) . . . . ?
N3 Pb1 O4 C16 8.7(4) . . . . ?
O2 Pb1 O4 C16 -44.9(4) . . . . ?
O5 Pb1 O4 C16 148.8(5) . . . . ?
O3 Pb1 O4 C16 -106.2(4) . . . . ?
N4 Pb1 O4 C16 -172.5(4) . . . . ?
O1 Pb1 O4 C17 -105.8(6) . . . . ?
N1 Pb1 O4 C17 -64.5(5) . . . . ?
N3 Pb1 O4 C17 -136.4(5) . . . . ?
O2 Pb1 O4 C17 170.0(5) . . . . ?
O5 Pb1 O4 C17 3.7(4) . . . . ?
O3 Pb1 O4 C17 108.6(5) . . . . ?
N4 Pb1 O4 C17 42.4(5) . . . . ?
O1 Pb1 O5 C18 -173.9(4) . . . . ?
N1 Pb1 O5 C18 132.8(4) . . . . ?
N3 Pb1 O5 C18 67.9(4) . . . . ?
O2 Pb1 O5 C18 -6.2(6) . . . . ?
O4 Pb1 O5 C18 30.0(4) . . . . ?
O3 Pb1 O5 C18 -70.6(4) . . . . ?
N4 Pb1 O5 C18 -108.6(4) . . . . ?
O1 Pb1 O5 C19 -42.4(5) . . . . ?
N1 Pb1 O5 C19 -95.7(4) . . . . ?
N3 Pb1 O5 C19 -160.5(4) . . . . ?
O2 Pb1 O5 C19 125.4(5) . . . . ?
O4 Pb1 O5 C19 161.5(4) . . . . ?
O3 Pb1 O5 C19 60.9(4) . . . . ?
N4 Pb1 O5 C19 23.0(4) . . . . ?
O1 Pb1 N1 C7 -32.1(5) . . . . ?
N3 Pb1 N1 C7 -136.0(5) . . . . ?
O2 Pb1 N1 C7 -92.7(5) . . . . ?
O4 Pb1 N1 C7 161.6(5) . . . . ?
O5 Pb1 N1 C7 105.5(5) . . . . ?
O3 Pb1 N1 C7 -1.5(8) . . . . ?
N4 Pb1 N1 C7 51.1(5) . . . . ?
O1 Pb1 N1 C8 162.2(5) . . . . ?
N3 Pb1 N1 C8 58.4(4) . . . . ?
O2 Pb1 N1 C8 101.7(5) . . . . ?
O4 Pb1 N1 C8 -4.0(4) . . . . ?
O5 Pb1 N1 C8 -60.1(4) . . . . ?
O3 Pb1 N1 C8 -167.1(4) . . . . ?
N4 Pb1 N1 C8 -114.5(4) . . . . ?
O1 Pb1 N3 C26 41.6(4) . . . . ?
N1 Pb1 N3 C26 112.0(4) . . . . ?
O2 Pb1 N3 C26 -29.2(4) . . . . ?
O4 Pb1 N3 C26 -148.7(4) . . . . ?
O5 Pb1 N3 C26 175.6(4) . . . . ?
O3 Pb1 N3 C26 -49.5(4) . . . . ?
N4 Pb1 N3 C26 -157.6(11) . . . . ?
O1 Pb1 N3 C14 -76.4(4) . . . . ?
N1 Pb1 N3 C14 -5.9(4) . . . . ?
O2 Pb1 N3 C14 -147.1(5) . . . . ?
O4 Pb1 N3 C14 93.3(4) . . . . ?
O5 Pb1 N3 C14 57.6(4) . . . . ?
O3 Pb1 N3 C14 -167.4(4) . . . . ?
N4 Pb1 N3 C14 84.4(13) . . . . ?
O1 Pb1 N3 C15 157.5(4) . . . . ?
N1 Pb1 N3 C15 -132.0(4) . . . . ?
O2 Pb1 N3 C15 86.8(4) . . . . ?
O4 Pb1 N3 C15 -32.8(4) . . . . ?
O5 Pb1 N3 C15 -68.5(4) . . . . ?
O3 Pb1 N3 C15 66.5(4) . . . . ?
N4 Pb1 N3 C15 -41.7(14) . . . . ?
O1 Pb1 N4 C20 140.2(4) . . . . ?
N1 Pb1 N4 C20 67.5(4) . . . . ?
N3 Pb1 N4 C20 -20.9(14) . . . . ?
O2 Pb1 N4 C20 -146.5(4) . . . . ?
O4 Pb1 N4 C20 -29.3(4) . . . . ?
O5 Pb1 N4 C20 7.4(4) . . . . ?
O3 Pb1 N4 C20 -132.7(4) . . . . ?
O1 Pb1 N4 C21 -102.6(4) . . . . ?
N1 Pb1 N4 C21 -175.2(4) . . . . ?
N3 Pb1 N4 C21 96.3(13) . . . . ?
O2 Pb1 N4 C21 -29.3(5) . . . . ?
O4 Pb1 N4 C21 87.9(4) . . . . ?
O5 Pb1 N4 C21 124.6(5) . . . . ?
O3 Pb1 N4 C21 -15.4(4) . . . . ?
O1 Pb1 N4 C27 19.1(4) . . . . ?
N1 Pb1 N4 C27 -53.5(4) . . . . ?
N3 Pb1 N4 C27 -141.9(11) . . . . ?
O2 Pb1 N4 C27 92.5(4) . . . . ?
O4 Pb1 N4 C27 -150.3(3) . . . . ?
O5 Pb1 N4 C27 -113.7(4) . . . . ?
O3 Pb1 N4 C27 106.3(4) . . . . ?
C6 C1 C2 C3 -0.3(10) . . . . ?
C7 C1 C2 C3 -176.3(6) . . . . ?
C1 C2 C3 C4 1.2(11) . . . . ?
C2 C3 C4 C5 -1.0(11) . . . . ?
C3 C4 C5 C6 -0.1(12) . . . . ?
Pb1 O1 C6 C1 -32.9(10) . . . . ?
Pb1 O1 C6 C5 147.4(5) . . . . ?
C2 C1 C6 O1 179.5(6) . . . . ?
C7 C1 C6 O1 -4.8(11) . . . . ?
C2 C1 C6 C5 -0.8(9) . . . . ?
C7 C1 C6 C5 174.9(6) . . . . ?
C4 C5 C6 O1 -179.3(7) . . . . ?
C4 C5 C6 C1 1.0(11) . . . . ?
C8 N1 C7 C1 -176.7(6) . . . . ?
Pb1 N1 C7 C1 17.6(9) . . . . ?
C6 C1 C7 N1 10.4(10) . . . . ?
C2 C1 C7 N1 -173.7(6) . . . . ?
C7 N1 C8 C9 -52.2(9) . . . . ?
Pb1 N1 C8 C9 114.7(6) . . . . ?
C7 N1 C8 C13 129.4(6) . . . . ?
Pb1 N1 C8 C13 -63.7(6) . . . . ?
C13 C8 C9 C10 -2.8(10) . . . . ?
N1 C8 C9 C10 178.8(6) . . . . ?
C8 C9 C10 C11 1.1(11) . . . . ?
C9 C10 C11 C12 -0.1(11) . . . . ?
C10 C11 C12 C13 0.9(11) . . . . ?
C11 C12 C13 C8 -2.6(10) . . . . ?
C11 C12 C13 C14 -175.0(6) . . . . ?
C9 C8 C13 C12 3.5(9) . . . . ?
N1 C8 C13 C12 -178.0(5) . . . . ?
C9 C8 C13 C14 175.8(6) . . . . ?
N1 C8 C13 C14 -5.7(9) . . . . ?
C26 N3 C14 C13 -162.6(6) . . . . ?
C15 N3 C14 C13 76.3(7) . . . . ?
Pb1 N3 C14 C13 -45.4(7) . . . . ?
C12 C13 C14 N3 -119.9(7) . . . . ?
C8 C13 C14 N3 68.0(8) . . . . ?
C26 N3 C15 C16 176.2(6) . . . . ?
C14 N3 C15 C16 -64.2(7) . . . . ?
Pb1 N3 C15 C16 63.0(6) . . . . ?
C17 O4 C16 C15 165.5(5) . . . . ?
Pb1 O4 C16 C15 18.0(6) . . . . ?
N3 C15 C16 O4 -55.9(8) . . . . ?
C16 O4 C17 C18 -179.1(5) . . . . ?
Pb1 O4 C17 C18 -33.1(7) . . . . ?
C19 O5 C18 C17 170.6(6) . . . . ?
Pb1 O5 C18 C17 -59.7(6) . . . . ?
O4 C17 C18 O5 59.9(7) . . . . ?
C18 O5 C19 C20 76.5(7) . . . . ?
Pb1 O5 C19 C20 -54.4(6) . . . . ?
C21 N4 C20 C19 -152.2(6) . . . . ?
C27 N4 C20 C19 80.9(7) . . . . ?
Pb1 N4 C20 C19 -37.8(6) . . . . ?
O5 C19 C20 N4 66.0(8) . . . . ?
C20 N4 C21 C22 165.8(7) . . . . ?
C27 N4 C21 C22 -68.2(8) . . . . ?
Pb1 N4 C21 C22 50.0(8) . . . . ?
N4 C21 C22 O3 -69.3(9) . . . . ?
C23 O3 C22 C21 175.1(7) . . . . ?
Pb1 O3 C22 C21 46.8(8) . . . . ?
C22 O3 C23 C24 179.2(7) . . . . ?
Pb1 O3 C23 C24 -51.3(8) . . . . ?
C25 O2 C24 C23 165.6(7) . . . . ?
Pb1 O2 C24 C23 -37.7(9) . . . . ?
O3 C23 C24 O2 58.3(10) . . . . ?
C24 O2 C25 C26 178.3(6) . . . . ?
Pb1 O2 C25 C26 20.6(7) . . . . ?
C14 N3 C26 C25 -178.7(6) . . . . ?
C15 N3 C26 C25 -55.1(8) . . . . ?
Pb1 N3 C26 C25 57.9(7) . . . . ?
O2 C25 C26 N3 -54.3(8) . . . . ?
C20 N4 C27 C28 60.4(7) . . . . ?
C21 N4 C27 C28 -64.5(7) . . . . ?
Pb1 N4 C27 C28 178.9(4) . . . . ?
N4 C27 C28 C29 83.3(8) . . . . ?
N4 C27 C28 C33 -96.9(7) . . . . ?
C33 C28 C29 C30 1.6(10) . . . . ?
C27 C28 C29 C30 -178.6(6) . . . . ?
C28 C29 C30 C31 -0.9(11) . . . . ?
C29 C30 C31 C32 0.2(11) . . . . ?
C30 C31 C32 C33 -0.2(10) . . . . ?
C31 C32 C33 C28 1.0(9) . . . . ?
C31 C32 C33 N2 -174.8(6) . . . . ?
C29 C28 C33 C32 -1.6(9) . . . . ?
C27 C28 C33 C32 178.6(6) . . . . ?
C29 C28 C33 N2 174.3(6) . . . . ?
C27 C28 C33 N2 -5.5(9) . . . . ?
C34 N2 C33 C32 -27.7(9) . . . . ?
C34 N2 C33 C28 156.5(6) . . . . ?
C33 N2 C34 C35 175.6(6) . . . . ?
N2 C34 C35 C40 -1.1(10) . . . . ?
N2 C34 C35 C36 179.9(6) . . . . ?
C40 C35 C36 C37 0.3(10) . . . . ?
C34 C35 C36 C37 179.4(6) . . . . ?
C35 C36 C37 C38 -0.9(11) . . . . ?
C36 C37 C38 C39 1.5(12) . . . . ?
C37 C38 C39 C40 -1.4(11) . . . . ?
C36 C35 C40 O6 178.7(6) . . . . ?
C34 C35 C40 O6 -0.4(10) . . . . ?
C36 C35 C40 C39 -0.3(10) . . . . ?
C34 C35 C40 C39 -179.4(6) . . . . ?
C38 C39 C40 O6 -178.2(7) . . . . ?
C38 C39 C40 C35 0.8(11) . . . . ?
O11 Cl2 O9 O10 -155(2) . . . 7_557 ?
O11 Cl2 O9 O10 25(2) 7_557 . . 7_557 ?
O10 Cl2 O9 O10 180.000(9) . . . 7_557 ?
O9 Cl2 O9 O10 -9(100) 7_557 . . 7_557 ?
O12 Cl2 O9 O10 -83.1(14) 7_557 . . 7_557 ?
O12 Cl2 O9 O10 96.9(14) . . . 7_557 ?
O11 Cl2 O10 O9 154(2) . . . 7_557 ?
O11 Cl2 O10 O9 -26(2) 7_557 . . 7_557 ?
O10 Cl2 O10 O9 114(43) 7_557 . . 7_557 ?
O9 Cl2 O10 O9 180.000(8) . . . 7_557 ?
O12 Cl2 O10 O9 85.1(15) 7_557 . . 7_557 ?
O12 Cl2 O10 O9 -94.9(15) . . . 7_557 ?
O11 Cl2 O11 O12 43(100) 7_557 . . 7_557 ?
O10 Cl2 O11 O12 -106.7(19) . . . 7_557 ?
O10 Cl2 O11 O12 73.3(19) 7_557 . . 7_557 ?
O9 Cl2 O11 O12 -77.9(18) 7_557 . . 7_557 ?
O9 Cl2 O11 O12 102.1(18) . . . 7_557 ?
O12 Cl2 O11 O12 180.000(12) . . . 7_557 ?
O11 Cl2 O12 O11 180.000(14) . . . 7_557 ?
O10 Cl2 O12 O11 127.2(13) . . . 7_557 ?
O10 Cl2 O12 O11 -52.8(13) 7_557 . . 7_557 ?
O9 Cl2 O12 O11 56.8(12) 7_557 . . 7_557 ?
O9 Cl2 O12 O11 -123.2(12) . . . 7_557 ?
O12 Cl2 O12 O11 -57(86) 7_557 . . 7_557 ?
