#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:37:03 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179069 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/31/4303125.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_4303125
loop_
_publ_author_name
'Eric C. Y. Tam'
'Nick C. Johnstone'
'Lorenzo Ferro'
'Peter B. Hitchcock'
'J. Robin Fulton'
_publ_section_title
;
Carbon Dioxide Activation by "Non-nucleophilic" Lead Alkoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8971
_journal_page_last               8976
_journal_paper_doi               10.1021/ic900134f
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H48 N2 O3 Pb, 0.5(C7 H8)'
_chemical_formula_sum            'C36.5 H52 N2 O3 Pb'
_chemical_formula_weight         773.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2007-02-22T11:04:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                99.649(2)
_cell_angle_beta                 106.996(2)
_cell_angle_gamma                113.105(1)
_cell_formula_units_Z            2
_cell_length_a                   11.9673(4)
_cell_length_b                   13.2339(5)
_cell_length_c                   13.5828(3)
_cell_measurement_reflns_used    22529
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     1792.09(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.81057E-2
_diffrn_orient_matrix_UB_12      0.671299E-1
_diffrn_orient_matrix_UB_13      -0.194717E-1
_diffrn_orient_matrix_UB_21      -0.575135E-1
_diffrn_orient_matrix_UB_22      -0.29564E-2
_diffrn_orient_matrix_UB_23      0.412091E-1
_diffrn_orient_matrix_UB_31      0.800296E-1
_diffrn_orient_matrix_UB_32      0.548554E-1
_diffrn_orient_matrix_UB_33      0.673054E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.066
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26307
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.47
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.742
_exptl_absorpt_correction_T_max  0.7882
_exptl_absorpt_correction_T_min  0.6946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.446
_refine_diff_density_min         -0.71
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7017
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0678P)²+4.8234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                5851
_reflns_number_total             7017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900134f_si_002_3.cif
_cod_data_source_block           (5)-feb1507
_cod_original_cell_volume        1792.09(10)
_cod_database_code               4303125
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Pb Pb 0.16430(2) 0.09969(2) 0.117610(19) 0.03516(10) Uani 1 1 d . . .
N1 N 0.3219(5) 0.1545(5) 0.2880(4) 0.0341(12) Uani 1 1 d . A .
N2 N 0.3055(5) 0.2770(5) 0.1177(4) 0.0358(12) Uani 1 1 d . A .
C1 C 0.4481(7) 0.2339(6) 0.3255(5) 0.0380(15) Uani 1 1 d . . .
C2 C 0.4994(7) 0.3113(6) 0.2702(5) 0.0383(15) Uani 1 1 d . A .
H2 H 0.5931 0.354 0.2992 0.046 Uiso 1 1 calc R . .
C3 C 0.4345(6) 0.3353(6) 0.1799(5) 0.0348(14) Uani 1 1 d . . .
C4 C 0.5437(7) 0.2482(7) 0.4354(6) 0.053(2) Uani 1 1 d . A .
H4A H 0.5103 0.2634 0.4911 0.08 Uiso 1 1 calc R . .
H4B H 0.6305 0.3135 0.4535 0.08 Uiso 1 1 calc R . .
H4C H 0.552 0.1771 0.4323 0.08 Uiso 1 1 calc R . .
C5 C 0.5221(7) 0.4368(6) 0.1559(7) 0.0480(18) Uani 1 1 d . A .
H5A H 0.5252 0.4098 0.0855 0.072 Uiso 1 1 calc R . .
H5B H 0.6115 0.4747 0.213 0.072 Uiso 1 1 calc R . .
H5C H 0.4868 0.4922 0.1537 0.072 Uiso 1 1 calc R . .
C6 C 0.2763(7) 0.0924(6) 0.3563(5) 0.0416(16) Uani 1 1 d . . .
C7 C 0.2709(7) -0.0167(7) 0.3491(6) 0.0466(18) Uani 1 1 d . A .
C8 C 0.2197(9) -0.0766(8) 0.4145(7) 0.062(2) Uani 1 1 d . . .
H8 H 0.2165 -0.1499 0.4118 0.074 Uiso 1 1 calc R A .
C9 C 0.1743(10) -0.0307(9) 0.4824(8) 0.071(3) Uani 1 1 d . A .
H9 H 0.1403 -0.0727 0.5261 0.086 Uiso 1 1 calc R . .
C10 C 0.1770(9) 0.0740(9) 0.4884(7) 0.067(2) Uani 1 1 d . . .
H10 H 0.1448 0.104 0.5359 0.08 Uiso 1 1 calc R A .
C11 C 0.2268(8) 0.1376(7) 0.4252(6) 0.0492(18) Uani 1 1 d . A .
C12 C 0.3157(8) -0.0729(7) 0.2713(6) 0.0518(19) Uani 1 1 d . . .
H12 H 0.3522 -0.0161 0.2345 0.062 Uiso 1 1 calc R A .
C13 C 0.4248(10) -0.0999(9) 0.3295(8) 0.072(3) Uani 1 1 d . A .
H13A H 0.4972 -0.0299 0.388 0.107 Uiso 1 1 calc R . .
H13B H 0.458 -0.1259 0.2777 0.107 Uiso 1 1 calc R . .
H13C H 0.3895 -0.1612 0.3604 0.107 Uiso 1 1 calc R . .
C14 C 0.2001(10) -0.1827(8) 0.1827(8) 0.074(3) Uani 1 1 d . A .
H14A H 0.1602 -0.2394 0.2164 0.111 Uiso 1 1 calc R . .
H14B H 0.2322 -0.2157 0.134 0.111 Uiso 1 1 calc R . .
H14C H 0.1337 -0.1635 0.1411 0.111 Uiso 1 1 calc R . .
C15 C 0.2255(9) 0.2522(7) 0.4305(6) 0.058(2) Uani 1 1 d . . .
H15 H 0.2788 0.2907 0.3906 0.069 Uiso 1 1 calc R A .
C16 C 0.0855(10) 0.2328(8) 0.3741(8) 0.069(2) Uani 1 1 d . A .
H16A H 0.0487 0.1844 0.2981 0.103 Uiso 1 1 calc R . .
H16B H 0.0868 0.3078 0.3767 0.103 Uiso 1 1 calc R . .
H16C H 0.0306 0.1939 0.4109 0.103 Uiso 1 1 calc R . .
C17 C 0.2866(11) 0.3353(10) 0.5473(8) 0.089(3) Uani 1 1 d . A .
H17A H 0.227 0.3066 0.5841 0.133 Uiso 1 1 calc R . .
H17B H 0.2996 0.4127 0.5453 0.133 Uiso 1 1 calc R . .
H17C H 0.372 0.3396 0.587 0.133 Uiso 1 1 calc R . .
C18 C 0.2498(6) 0.3247(6) 0.0399(5) 0.0355(14) Uani 1 1 d . . .
C19 C 0.2398(7) 0.2936(6) -0.0665(5) 0.0407(16) Uani 1 1 d . A .
C20 C 0.1884(8) 0.3459(7) -0.1362(7) 0.053(2) Uani 1 1 d . . .
H20 H 0.1794 0.3254 -0.2096 0.064 Uiso 1 1 calc R A .
C21 C 0.1506(8) 0.4262(8) -0.1009(7) 0.058(2) Uani 1 1 d . A .
H21 H 0.1206 0.4637 -0.1485 0.07 Uiso 1 1 calc R . .
C22 C 0.1563(8) 0.4517(7) 0.0021(7) 0.054(2) Uani 1 1 d . . .
H22 H 0.1265 0.5048 0.0245 0.065 Uiso 1 1 calc R A .
C23 C 0.2049(7) 0.4020(6) 0.0767(6) 0.0452(17) Uani 1 1 d . A .
C24 C 0.2783(8) 0.2041(7) -0.1098(6) 0.0475(18) Uani 1 1 d . . .
H24 H 0.3159 0.1796 -0.0479 0.057 Uiso 1 1 calc R A .
C25 C 0.3830(9) 0.2510(7) -0.1566(7) 0.057(2) Uani 1 1 d . A .
H25A H 0.3468 0.2716 -0.2202 0.085 Uiso 1 1 calc R . .
H25B H 0.4081 0.1914 -0.1784 0.085 Uiso 1 1 calc R . .
H25C H 0.461 0.3199 -0.1014 0.085 Uiso 1 1 calc R . .
C26 C 0.1548(9) 0.0971(8) -0.1952(7) 0.064(2) Uani 1 1 d . A .
H26A H 0.0907 0.0657 -0.1629 0.097 Uiso 1 1 calc R . .
H26B H 0.1792 0.0382 -0.2207 0.097 Uiso 1 1 calc R . .
H26C H 0.1152 0.1189 -0.2566 0.097 Uiso 1 1 calc R . .
C27 C 0.2036(10) 0.4280(8) 0.1886(7) 0.065(2) Uani 1 1 d . . .
H27 H 0.2151 0.3675 0.2194 0.078 Uiso 1 1 calc R A .
C28 C 0.3171(13) 0.5450(16) 0.2642(11) 0.175(9) Uani 1 1 d . A .
H28A H 0.4009 0.548 0.2663 0.263 Uiso 1 1 calc R . .
H28B H 0.3174 0.5562 0.3375 0.263 Uiso 1 1 calc R . .
H28C H 0.3064 0.6065 0.2378 0.263 Uiso 1 1 calc R . .
C29 C 0.0766(10) 0.4246(9) 0.1892(8) 0.076(3) Uani 1 1 d . A .
H29A H 0.0689 0.4901 0.1693 0.115 Uiso 1 1 calc R . .
H29B H 0.0767 0.4297 0.262 0.115 Uiso 1 1 calc R . .
H29C H 0.0017 0.3517 0.1366 0.115 Uiso 1 1 calc R . .
O1 O 0.2976(11) 0.0472(10) 0.0648(9) 0.046(3) Uiso 0.583(13) 1 d PD A 1
O2 O 0.1192(13) -0.1077(9) -0.0657(8) 0.057(3) Uiso 0.583(13) 1 d PD A 1
O3 O 0.3263(10) -0.0549(9) -0.0588(8) 0.068(3) Uiso 0.583(13) 1 d PD A 1
C30 C 0.2349(15) -0.0447(13) -0.0218(10) 0.041(3) Uiso 0.583(13) 1 d PD A 1
C31 C 0.2791(15) -0.1576(12) -0.1491(11) 0.060(4) Uiso 0.583(13) 1 d PD A 1
H31 H 0.1813 -0.1937 -0.1904 0.072 Uiso 0.583(13) 1 calc PR A 1
C32 C 0.318(2) -0.2411(15) -0.1046(16) 0.078(5) Uiso 0.583(13) 1 d PD A 1
H32A H 0.4044 -0.1977 -0.0435 0.117 Uiso 0.583(13) 1 calc PR A 1
H32B H 0.3233 -0.293 -0.1617 0.117 Uiso 0.583(13) 1 calc PR A 1
H32C H 0.2518 -0.287 -0.0797 0.117 Uiso 0.583(13) 1 calc PR A 1
C33 C 0.3528(18) -0.1150(15) -0.2188(16) 0.065(5) Uiso 0.583(13) 1 d PD A 1
H33A H 0.3246 -0.0631 -0.2499 0.098 Uiso 0.583(13) 1 calc PR A 1
H33B H 0.3337 -0.1814 -0.2776 0.098 Uiso 0.583(13) 1 calc PR A 1
H33C H 0.448 -0.073 -0.1743 0.098 Uiso 0.583(13) 1 calc PR A 1
O1A O 0.2706(12) 0.0113(12) 0.0365(11) 0.032(3) Uiso 0.417(13) 1 d PD A 2
O2A O 0.0625(13) -0.1260(10) -0.0510(10) 0.047(4) Uiso 0.417(13) 1 d PD . 2
O3A O 0.2154(12) -0.1473(11) -0.0967(10) 0.056(4) Uiso 0.417(13) 1 d PD A 2
C30A C 0.1761(19) -0.0893(15) -0.0340(12) 0.031(4) Uiso 0.417(13) 1 d PD A 2
C31A C 0.3546(16) -0.1110(16) -0.0721(15) 0.054(5) Uiso 0.417(13) 1 d PD A 2
H31A H 0.4137 -0.0384 -0.0085 0.065 Uiso 0.417(13) 1 calc PR A 2
C32A C 0.381(3) -0.211(2) -0.055(2) 0.079(7) Uiso 0.417(13) 1 d PD A 2
H32D H 0.4326 -0.1923 0.0218 0.119 Uiso 0.417(13) 1 calc PR A 2
H32E H 0.4296 -0.2235 -0.0983 0.119 Uiso 0.417(13) 1 calc PR A 2
H32F H 0.2962 -0.2808 -0.0787 0.119 Uiso 0.417(13) 1 calc PR A 2
C33A C 0.369(4) -0.095(3) -0.176(3) 0.112(14) Uiso 0.417(13) 1 d PD A 2
H33D H 0.3041 -0.1659 -0.2374 0.168 Uiso 0.417(13) 1 calc PR A 2
H33E H 0.4586 -0.0799 -0.1704 0.168 Uiso 0.417(13) 1 calc PR A 2
H33F H 0.355 -0.0297 -0.189 0.168 Uiso 0.417(13) 1 calc PR A 2
C1S C -0.0068(14) 0.4622(10) 0.5315(11) 0.061(4) Uiso 0.5 1 d PD . 2
C2S C -0.0979(17) 0.3426(13) 0.4872(12) 0.068(5) Uiso 0.5 1 d PD . 2
C3S C -0.0049(10) 0.3840(8) 0.5943(8) 0.076(3) Uiso 1 1 d D B 2
C4S C 0.0957(17) 0.4989(12) 0.6350(13) 0.082(6) Uiso 0.5 1 d PD B 2
C5S C 0.0957(10) 0.5770(8) 0.5741(8) 0.074(3) Uiso 1 1 d D . 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 0 '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 0.006 '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 Pb N2 82.2(3) . . ?
O1 Pb N1 83.5(3) . . ?
N2 Pb N1 83.23(18) . . ?
N2 Pb O1A 90.2(3) . . ?
N1 Pb O1A 91.7(3) . . ?
N2 Pb O2A 96.3(3) . 2 ?
N1 Pb O2A 130.5(3) . 2 ?
O1A Pb O2A 137.8(4) . 2 ?
O1 Pb Pb 100.9(3) . 2 ?
N2 Pb Pb 122.31(13) . 2 ?
N1 Pb Pb 154.37(13) . 2 ?
O1A Pb Pb 90.5(3) . 2 ?
O2A Pb Pb 51.2(2) 2 2 ?
C1 N1 C6 119.2(5) . . ?
C1 N1 Pb 126.4(4) . . ?
C6 N1 Pb 114.4(4) . . ?
C3 N2 C18 118.6(5) . . ?
C3 N2 Pb 124.7(4) . . ?
C18 N2 Pb 116.6(4) . . ?
N1 C1 C2 123.5(6) . . ?
N1 C1 C4 119.5(6) . . ?
C2 C1 C4 116.9(6) . . ?
C3 C2 C1 130.8(6) . . ?
C3 C2 H2 114.6 . . ?
C1 C2 H2 114.6 . . ?
N2 C3 C2 125.5(6) . . ?
N2 C3 C5 119.7(6) . . ?
C2 C3 C5 114.8(6) . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C11 120.3(6) . . ?
C7 C6 N1 120.4(6) . . ?
C11 C6 N1 119.2(6) . . ?
C8 C7 C6 118.1(7) . . ?
C8 C7 C12 119.3(7) . . ?
C6 C7 C12 122.5(6) . . ?
C9 C8 C7 120.9(8) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C10 C9 C8 121.3(7) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 120.5(9) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C10 C11 C6 118.9(8) . . ?
C10 C11 C15 119.8(8) . . ?
C6 C11 C15 121.3(7) . . ?
C13 C12 C7 112.8(7) . . ?
C13 C12 C14 109.8(8) . . ?
C7 C12 C14 111.8(7) . . ?
C13 C12 H12 107.4 . . ?
C7 C12 H12 107.4 . . ?
C14 C12 H12 107.4 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 C16 110.6(7) . . ?
C11 C15 C17 113.2(8) . . ?
C16 C15 C17 109.4(8) . . ?
C11 C15 H15 107.8 . . ?
C16 C15 H15 107.8 . . ?
C17 C15 H15 107.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C23 122.0(6) . . ?
C19 C18 N2 120.8(6) . . ?
C23 C18 N2 117.2(6) . . ?
C18 C19 C20 117.5(7) . . ?
C18 C19 C24 122.9(6) . . ?
C20 C19 C24 119.6(6) . . ?
C21 C20 C19 121.7(8) . . ?
C21 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
C22 C21 C20 119.7(7) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C23 122.2(8) . . ?
C21 C22 H22 118.9 . . ?
C23 C22 H22 118.9 . . ?
C22 C23 C18 116.8(7) . . ?
C22 C23 C27 120.5(7) . . ?
C18 C23 C27 122.6(7) . . ?
C19 C24 C26 109.6(7) . . ?
C19 C24 C25 113.4(6) . . ?
C26 C24 C25 110.4(7) . . ?
C19 C24 H24 107.8 . . ?
C26 C24 H24 107.8 . . ?
C25 C24 H24 107.8 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C29 C27 C23 113.7(7) . . ?
C29 C27 C28 108.4(9) . . ?
C23 C27 C28 111.8(10) . . ?
C29 C27 H27 107.6 . . ?
C23 C27 H27 107.6 . . ?
C28 C27 H27 107.6 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 O1 Pb 113.5(8) . . ?
C30 O3 C31 117.0(11) . . ?
O2 C30 O1 127.9(12) . . ?
O2 C30 O3 124.1(13) . . ?
O1 C30 O3 107.9(12) . . ?
O3 C31 C32 108.1(12) . . ?
O3 C31 C33 104.6(12) . . ?
C32 C31 C33 109.7(13) . . ?
O3 C31 H31 111.4 . . ?
C32 C31 H31 111.4 . . ?
C33 C31 H31 111.4 . . ?
C30A O1A Pb 106.2(9) . . ?
C30A O2A Pb 148.4(11) . 2 ?
C30A O3A C31A 121.3(13) . . ?
O2A C30A O1A 125.1(13) . . ?
O2A C30A O3A 119.8(16) . . ?
O1A C30A O3A 114.9(16) . . ?
O3A C31A C32A 108.0(15) . . ?
O3A C31A C33A 103.8(18) . . ?
C32A C31A C33A 107.3(18) . . ?
O3A C31A H31A 112.4 . . ?
C32A C31A H31A 112.4 . . ?
C33A C31A H31A 112.4 . . ?
C31A C32A H32D 109.5 . . ?
C31A C32A H32E 109.5 . . ?
H32D C32A H32E 109.5 . . ?
C31A C32A H32F 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
C31A C33A H33D 109.5 . . ?
C31A C33A H33E 109.5 . . ?
H33D C33A H33E 109.5 . . ?
C31A C33A H33F 109.5 . . ?
H33D C33A H33F 109.5 . . ?
H33E C33A H33F 109.5 . . ?
C5S C1S C5S 118.9(10) 2_566 . ?
C1S C1S C2S 123.0(14) 2_566 . ?
C1S C1S C4S 118.5(12) 2_566 . ?
C2S C1S C4S 116.5(10) . . ?
C5S C1S C3S 121.4(10) 2_566 . ?
C5S C1S C3S 119.1(9) . . ?
C3S C2S C5S 119.2(11) . 2_566 ?
C4S C3S C2S 118.7(9) . . ?
C3S C4S C5S 121.0(10) . . ?
C1S C5S C4S 120.7(10) 2_566 . ?
C1S C5S C2S 120.6(10) . 2_566 ?
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
Pb O1 2.217(10) . ?
Pb N2 2.291(5) . ?
Pb N1 2.292(5) . ?
Pb O1A 2.399(13) . ?
Pb O2A 2.777(13) 2 ?
Pb Pb 3.7842(5) 2 ?
N1 C1 1.331(8) . ?
N1 C6 1.425(8) . ?
N2 C3 1.333(8) . ?
N2 C18 1.449(8) . ?
C1 C2 1.423(9) . ?
C1 C4 1.519(9) . ?
C2 C3 1.406(9) . ?
C2 H2 0.95 . ?
C3 C5 1.500(9) . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 C7 1.406(10) . ?
C6 C11 1.414(11) . ?
C7 C8 1.402(10) . ?
C7 C12 1.528(11) . ?
C8 C9 1.370(13) . ?
C8 H8 0.95 . ?
C9 C10 1.361(13) . ?
C9 H9 0.95 . ?
C10 C11 1.395(11) . ?
C10 H10 0.95 . ?
C11 C15 1.512(12) . ?
C12 C13 1.522(12) . ?
C12 C14 1.529(12) . ?
C12 H12 1 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 C16 1.520(13) . ?
C15 C17 1.539(12) . ?
C15 H15 1 . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 C19 1.390(9) . ?
C18 C23 1.414(10) . ?
C19 C20 1.404(10) . ?
C19 C24 1.520(10) . ?
C20 C21 1.378(12) . ?
C20 H20 0.95 . ?
C21 C22 1.358(11) . ?
C21 H21 0.95 . ?
C22 C23 1.406(10) . ?
C22 H22 0.95 . ?
C23 C27 1.507(11) . ?
C24 C26 1.529(11) . ?
C24 C25 1.532(10) . ?
C24 H24 1 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C27 C29 1.505(13) . ?
C27 C28 1.516(16) . ?
C27 H27 1 . ?
C28 H28A 0.98 . ?
C28 H28B 0.98 . ?
C28 H28C 0.98 . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
O1 C30 1.309(16) . ?
O2 C30 1.188(17) . ?
O3 C30 1.372(14) . ?
O3 C31 1.451(15) . ?
C31 C32 1.505(18) . ?
C31 C33 1.506(19) . ?
C31 H31 1 . ?
C32 H32A 0.98 . ?
C32 H32B 0.98 . ?
C32 H32C 0.98 . ?
C33 H33A 0.98 . ?
C33 H33B 0.98 . ?
C33 H33C 0.98 . ?
O1A C30A 1.314(18) . ?
O2A C30A 1.18(2) . ?
O2A Pb 2.777(13) 2 ?
O3A C30A 1.355(15) . ?
O3A C31A 1.453(16) . ?
C31A C32A 1.50(2) . ?
C31A C33A 1.52(2) . ?
C31A H31A 1 . ?
C32A H32D 0.98 . ?
C32A H32E 0.98 . ?
C32A H32F 0.98 . ?
C33A H33D 0.98 . ?
C33A H33E 0.98 . ?
C33A H33F 0.98 . ?
C1S C5S 1.373(16) 2_566 ?
C1S C5S 1.406(12) . ?
C1S C2S 1.414(14) . ?
C1S C3S 1.450(13) . ?
C2S C3S 1.400(14) . ?
C2S C5S 1.454(18) 2_566 ?
C3S C4S 1.400(13) . ?
C4S C5S 1.428(13) . ?
