#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/08/4310895.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_4310895
loop_
_publ_author_name
'Robert D. Hancock'
'Joseph H. Reibenspies'
'Hulisani Maumela'
_publ_section_title
;
 Structural Effects of the Lone Pair on Lead(II), and Parallels with the
 Coordination Geometry of Mercury(II). Does the Lone Pair on Lead(II) Form
 H-Bonds? Structures of the Lead(II) and Mercury(II) Complexes of the
 Pendant-Donor Macrocycle DOTAM
 (1,4,7,10-Tetrakis(carbamoylmethyl)-1,4,7,10-tetraazacyclododecane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2981
_journal_page_last               2987
_journal_paper_doi               10.1021/ic030277a
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C16 H41 Cl2 N8 O16.5 Pb'
_chemical_formula_weight         887.66
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL
_cell_angle_alpha                101.45(2)
_cell_angle_beta                 93.32(2)
_cell_angle_gamma                90.53(2)
_cell_formula_units_Z            4
_cell_length_a                   12.767(3)
_cell_length_b                   13.528(4)
_cell_length_c                   18.385(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3106.2(15)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11304
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    5.687
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.7
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_description       plate
_exptl_crystal_F_000             1764
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.097
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         10875
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.156
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_obs          0.0500
_refine_ls_shift/esd_max         -0.021
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s²(Fo²)+( 0.0310P)²+31.4774P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1240
_refine_ls_wR_factor_obs         0.0984
_reflns_number_observed          7755
_reflns_number_total             10932
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic030277a_s_2.cif
_cod_data_source_block           rh23
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0310P)^2^+31.4774P] where P=(Fo^2^+2Fc^2^)/3' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0310P)^2^+31.4774P]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3106.2(14)
_cod_original_formula_sum        'C16 H41 Cl2 N8 O16.50 Pb'
_cod_database_code               4310895
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Pb1 Pb 0.15745(3) 0.34829(3) 0.29096(2) 0.02301(12) Uani 1 d . .
Pb2 Pb 0.62882(3) -0.07058(3) 0.17753(2) 0.02130(11) Uani 1 d . .
Cl1 Cl 0.2333(3) 0.5911(2) -0.0138(2) 0.0439(8) Uani 1 d . .
Cl2 Cl 0.3495(2) 0.4772(2) -0.3077(2) 0.0411(7) Uani 1 d . .
Cl3 Cl 0.1097(3) 0.8165(4) 0.2405(3) 0.088(2) Uani 1 d . .
Cl4 Cl 0.3810(3) 0.8137(3) 0.5049(2) 0.0619(10) Uani 1 d D .
O1 O 0.3466(6) 0.3446(6) 0.3728(5) 0.042(2) Uani 1 d . .
O2 O 0.0562(6) 0.3552(7) 0.4291(5) 0.043(2) Uani 1 d . .
O3 O -0.0078(6) 0.2288(6) 0.2366(4) 0.036(2) Uani 1 d . .
O4 O 0.2571(5) 0.2180(5) 0.1820(4) 0.032(2) Uani 1 d . .
O5 O 0.4447(5) -0.0309(5) 0.1008(4) 0.032(2) Uani 1 d . .
O6 O 0.5592(6) 0.0823(5) 0.2809(4) 0.036(2) Uani 1 d . .
O7 O 0.8169(6) 0.0171(6) 0.2209(4) 0.036(2) Uani 1 d . .
O8 O 0.7207(6) -0.1021(6) 0.0353(4) 0.036(2) Uani 1 d . .
O9 O 0.3318(7) 0.5605(7) 0.0087(6) 0.067(3) Uani 1 d . .
O10 O 0.1916(9) 0.6502(9) 0.0573(7) 0.053(4) Uiso 0.73(2) d P .
O10' O 0.2349(30) 0.6875(31) -0.0156(25) 0.069(13) Uiso 0.27(2) d P .
O11 O 0.2255(9) 0.6537(9) -0.0675(7) 0.042(3) Uiso 0.73(2) d P .
O11' O 0.2915(27) 0.5598(26) -0.0952(20) 0.059(12) Uiso 0.27(2) d P .
O12 O 0.1617(13) 0.5044(13) -0.0372(9) 0.043(5) Uiso 0.73(2) d P .
O12' O 0.1544(35) 0.5258(35) -0.0216(26) 0.045(14) Uiso 0.27(2) d P .
O13 O 0.2793(7) 0.4051(6) -0.3537(5) 0.056(3) Uani 1 d . .
O14 O 0.4318(7) 0.4262(7) -0.2745(7) 0.068(3) Uani 1 d . .
O15 O 0.3925(8) 0.5421(7) -0.3524(6) 0.063(3) Uani 1 d . .
O16 O 0.2917(7) 0.5362(7) -0.2513(5) 0.054(2) Uani 1 d . .
O17 O 0.0569(9) 0.8981(11) 0.2230(9) 0.117(5) Uani 1 d . .
O18 O 0.1998(12) 0.8050(21) 0.2228(23) 0.326(20) Uani 1 d . .
O19 O 0.0958(29) 0.8115(19) 0.3102(12) 0.283(18) Uani 1 d . .
O20 O 0.0476(12) 0.7294(13) 0.2033(15) 0.188(10) Uani 1 d . .
O21 O 0.3459(10) 0.7890(10) 0.4247(4) 0.134(6) Uiso 1 d D .
O22 O 0.4252(18) 0.7239(11) 0.5287(11) 0.202(18) Uiso 0.57(2) d PD .
O22' O 0.4971(8) 0.7955(19) 0.5087(11) 0.102(12) Uiso 0.43(2) d PD .
O23 O 0.4512(12) 0.9004(11) 0.5244(8) 0.089(8) Uiso 0.57(2) d PD .
O23' O 0.3661(20) 0.9229(8) 0.5334(10) 0.110(13) Uiso 0.43(2) d PD .
O24 O 0.2809(9) 0.8371(15) 0.5455(8) 0.101(9) Uiso 0.57(2) d PD .
O24' O 0.3277(18) 0.7514(17) 0.5476(9) 0.138(16) Uiso 0.43(2) d PD .
O25 O 0.1112(6) 0.8470(6) 0.0311(5) 0.046(2) Uani 1 d . .
H25C H 0.1742(6) 0.8342(6) 0.0205(5) 0.050 Uiso 1 d R .
H25D H 0.1204(6) 0.9039(6) 0.0603(5) 0.050 Uiso 1 d R .
O26 O 0.0391(9) 0.8719(9) 0.5141(6) 0.089(4) Uani 1 d . .
H26A H -0.0233(9) 0.8717(9) 0.4951(6) 0.080 Uiso 1 d R .
H26B H 0.0734(9) 0.8998(9) 0.4851(6) 0.080 Uiso 1 d R .
O27 O 0.1607(7) 1.0279(6) 0.1340(5) 0.058(3) Uani 1 d . .
H27D H 0.1775(7) 1.0252(6) 0.1789(5) 0.080 Uiso 1 d R .
H27E H 0.1184(7) 0.9795(6) 0.1152(5) 0.080 Uiso 1 d R .
O28 O 1.1623(11) 0.2403(13) 0.5191(8) 0.135(6) Uani 1 d . .
H28B H 1.2092(11) 0.2141(13) 0.4908(8) 0.080 Uiso 1 d R .
H28C H 1.1902(11) 0.2855(13) 0.5538(8) 0.080 Uiso 1 d R .
O29 O 0.1857(11) 0.1196(13) 0.3534(11) 0.162(8) Uani 1 d . .
H29D H 0.1488(11) 0.0802(13) 0.3196(11) 0.050 Uiso 1 d R .
H29C H 0.1781(11) 0.1806(13) 0.3493(11) 0.050 Uiso 1 d R .
O30 O 0.1602(17) -0.0363(18) 0.4277(13) 0.235(12) Uani 1 d . .
H30A H 0.1732(17) -0.0980(18) 0.4117(13) 0.080 Uiso 1 d R .
H30B H 0.0961(17) -0.0256(18) 0.4171(13) 0.080 Uiso 1 d R .
O31 O 0.3321(23) 0.0688(28) 0.4752(14) 0.402(27) Uani 1 d . .
H31E H 0.3652(23) 0.0159(28) 0.4579(14) 0.080 Uiso 1 d R .
H31C H 0.2773(23) 0.0591(28) 0.4461(14) 0.050 Uiso 1 d R .
O32 O 0.3589(7) 0.7508(6) -0.1476(5) 0.048(2) Uiso 1 d . .
H32A H 0.3757(7) 0.6913(6) -0.1675(5) 0.080 Uiso 1 d R .
H32C H 0.2925(7) 0.7541(6) -0.1468(5) 0.080 Uiso 1 d R .
O33 O -0.3047(7) 0.2561(7) 0.2998(5) 0.053(2) Uiso 1 d . .
H33A H -0.3246(7) 0.3143(7) 0.3202(5) 0.080 Uiso 1 d R .
H33C H -0.2887(7) 0.2569(7) 0.2556(5) 0.080 Uiso 1 d R .
N1 N 0.2436(6) 0.5216(6) 0.3641(5) 0.027(2) Uani 1 d . .
N2 N 0.0122(6) 0.4824(6) 0.3319(5) 0.027(2) Uani 1 d . .
N3 N 0.0488(6) 0.3913(7) 0.1757(5) 0.027(2) Uani 1 d . .
N4 N 0.2790(7) 0.4244(6) 0.2058(5) 0.029(2) Uani 1 d . .
N5 N 0.4084(8) 0.4027(8) 0.4919(6) 0.054(3) Uani 1 d . .
H5C H 0.4074(8) 0.4504(8) 0.5337(6) 0.080 Uiso 1 d R .
H5D H 0.4505(8) 0.3495(8) 0.4905(6) 0.080 Uiso 1 d R .
N6 N -0.1099(7) 0.3018(7) 0.4286(5) 0.039(2) Uani 1 d . .
H6C H -0.1774(7) 0.3092(7) 0.4141(5) 0.080 Uiso 1 d R .
H6D H -0.0928(7) 0.2560(7) 0.4565(5) 0.080 Uiso 1 d R .
N7 N -0.0964(7) 0.1536(7) 0.1312(5) 0.035(2) Uani 1 d . .
H7C H -0.1081(7) 0.1487(7) 0.0818(5) 0.080 Uiso 1 d R .
H7D H -0.1291(7) 0.1105(7) 0.1544(5) 0.080 Uiso 1 d R .
N8 N 0.4222(7) 0.1931(6) 0.1444(5) 0.032(2) Uani 1 d . .
H8C H 0.4854(7) 0.2211(6) 0.1407(5) 0.080 Uiso 1 d R .
H8D H 0.4111(7) 0.1264(6) 0.1281(5) 0.080 Uiso 1 d R .
N9 N 0.5093(6) -0.2247(6) 0.1104(5) 0.028(2) Uani 1 d . .
N10 N 0.4971(6) -0.1164(6) 0.2669(5) 0.026(2) Uani 1 d . .
N11 N 0.7307(6) -0.1254(6) 0.2900(5) 0.024(2) Uani 1 d . .
N12 N 0.7438(6) -0.2324(6) 0.1328(5) 0.025(2) Uani 1 d . .
N13 N 0.3628(7) -0.0862(7) -0.0119(5) 0.035(2) Uani 1 d . .
H13C H 0.3516(7) -0.1378(7) -0.0509(5) 0.080 Uiso 1 d R .
H13D H 0.3311(7) -0.0271(7) -0.0118(5) 0.080 Uiso 1 d R .
N14 N 0.4040(8) 0.1387(7) 0.3222(6) 0.048(3) Uani 1 d . .
H14A H 0.3369(8) 0.1229(7) 0.3285(6) 0.080 Uiso 1 d R .
H14B H 0.4270(8) 0.2033(7) 0.3348(6) 0.080 Uiso 1 d R .
N15 N 0.9182(7) 0.0850(7) 0.3240(6) 0.044(3) Uani 1 d . .
H15C H 0.9299(7) 0.0913(7) 0.3735(6) 0.080 Uiso 1 d R .
H15D H 0.9580(7) 0.1205(7) 0.2989(6) 0.080 Uiso 1 d R .
N16 N 0.8921(7) -0.1055(7) 0.0100(5) 0.038(2) Uani 1 d . .
H16A H 0.9559(7) -0.1298(7) 0.0187(5) 0.080 Uiso 1 d R .
H16B H 0.8831(7) -0.0642(7) -0.0226(5) 0.080 Uiso 1 d R .
C1 C 0.1647(9) 0.6024(8) 0.3728(7) 0.039(3) Uani 1 d . .
H1A H 0.1553(9) 0.6267(8) 0.3273(7) 0.080 Uiso 1 d R .
H1B H 0.1909(9) 0.6574(8) 0.4111(7) 0.080 Uiso 1 d R .
C2 C 0.0579(8) 0.5649(8) 0.3924(6) 0.035(3) Uani 1 d . .
H2A H 0.0672(8) 0.5397(8) 0.4376(6) 0.080 Uiso 1 d R .
H2B H 0.0101(8) 0.6199(8) 0.4007(6) 0.080 Uiso 1 d R .
C3 C -0.0293(8) 0.5263(8) 0.2691(6) 0.033(3) Uani 1 d . .
H3A H 0.0192(8) 0.5765(8) 0.2600(6) 0.080 Uiso 1 d R .
H3B H -0.0939(8) 0.5587(8) 0.2824(6) 0.080 Uiso 1 d R .
C4 C -0.0488(8) 0.4464(8) 0.1989(6) 0.032(3) Uani 1 d . .
H4A H -0.1006(8) 0.3985(8) 0.2072(6) 0.080 Uiso 1 d R .
H4B H -0.0762(8) 0.4775(8) 0.1594(6) 0.080 Uiso 1 d R .
C5 C 0.1131(8) 0.4532(8) 0.1349(6) 0.032(3) Uani 1 d . .
H5A H 0.1117(8) 0.5230(8) 0.1587(6) 0.080 Uiso 1 d R .
H5B H 0.0822(8) 0.4466(8) 0.0853(6) 0.080 Uiso 1 d R .
C6 C 0.2253(8) 0.4192(8) 0.1311(6) 0.029(2) Uani 1 d . .
H6A H 0.2268(8) 0.3507(8) 0.1043(6) 0.080 Uiso 1 d R .
H6B H 0.2634(8) 0.4605(8) 0.1044(6) 0.080 Uiso 1 d R .
C7 C 0.3074(9) 0.5316(8) 0.2403(7) 0.035(3) Uani 1 d . .
H7A H 0.2505(9) 0.5741(8) 0.2308(7) 0.080 Uiso 1 d R .
H7B H 0.3675(9) 0.5515(8) 0.2172(7) 0.080 Uiso 1 d R .
C8 C 0.3333(8) 0.5488(8) 0.3225(6) 0.033(3) Uani 1 d . .
H8A H 0.3918(8) 0.5079(8) 0.3317(6) 0.080 Uiso 1 d R .
H8B H 0.3537(8) 0.6180(8) 0.3412(6) 0.080 Uiso 1 d R .
C9 C 0.2808(8) 0.5021(8) 0.4369(6) 0.032(3) Uani 1 d . .
H9A H 0.2212(8) 0.4920(8) 0.4643(6) 0.080 Uiso 1 d R .
H9B H 0.3195(8) 0.5603(8) 0.4641(6) 0.080 Uiso 1 d R .
C10 C 0.3495(9) 0.4091(9) 0.4306(7) 0.036(3) Uani 1 d . .
C11 C -0.0741(8) 0.4320(9) 0.3609(6) 0.033(3) Uani 1 d . .
H11A H -0.1193(8) 0.3971(9) 0.3202(6) 0.080 Uiso 1 d R .
H11B H -0.1146(8) 0.4826(9) 0.3905(6) 0.080 Uiso 1 d R .
C12 C -0.0374(9) 0.3589(9) 0.4093(6) 0.034(3) Uani 1 d . .
C13 C 0.0198(9) 0.2937(8) 0.1267(6) 0.031(3) Uani 1 d . .
H13A H 0.0811(9) 0.2626(8) 0.1053(6) 0.080 Uiso 1 d R .
H13B H -0.0282(9) 0.3045(8) 0.0870(6) 0.080 Uiso 1 d R .
C14 C -0.0312(8) 0.2241(8) 0.1699(6) 0.030(3) Uani 1 d . .
C15 C 0.3743(8) 0.3629(8) 0.1988(6) 0.029(3) Uani 1 d . .
H15A H 0.4130(8) 0.3734(8) 0.2461(6) 0.080 Uiso 1 d R .
H15B H 0.4183(8) 0.3835(8) 0.1637(6) 0.080 Uiso 1 d R .
C16 C 0.3464(8) 0.2511(8) 0.1733(5) 0.025(2) Uani 1 d . .
C17 C 0.4166(7) -0.2334(8) 0.1551(6) 0.027(2) Uani 1 d . .
H17A H 0.3834(7) -0.2986(8) 0.1383(6) 0.080 Uiso 1 d R .
H17B H 0.3668(7) -0.1831(8) 0.1475(6) 0.080 Uiso 1 d R .
C18 C 0.4484(8) -0.2178(7) 0.2377(6) 0.029(2) Uani 1 d . .
H18A H 0.3883(8) -0.2254(7) 0.2653(6) 0.080 Uiso 1 d R .
H18B H 0.4981(8) -0.2680(7) 0.2455(6) 0.080 Uiso 1 d R .
C19 C 0.5530(8) -0.1158(9) 0.3416(6) 0.031(3) Uani 1 d . .
H19A H 0.5084(8) -0.1476(9) 0.3709(6) 0.080 Uiso 1 d R .
H19B H 0.5660(8) -0.0472(9) 0.3669(6) 0.080 Uiso 1 d R .
C20 C 0.6558(8) -0.1699(9) 0.3340(6) 0.033(3) Uani 1 d . .
H20A H 0.6878(8) -0.1695(9) 0.3826(6) 0.080 Uiso 1 d R .
H20B H 0.6417(8) -0.2390(9) 0.3102(6) 0.080 Uiso 1 d R .
C21 C 0.8130(8) -0.1984(8) 0.2642(6) 0.027(2) Uani 1 d . .
H21A H 0.8355(8) -0.2310(8) 0.3041(6) 0.080 Uiso 1 d R .
H21B H 0.8722(8) -0.1620(8) 0.2520(6) 0.080 Uiso 1 d R .
C22 C 0.7746(9) -0.2778(8) 0.1962(6) 0.033(3) Uani 1 d . .
H22A H 0.8309(9) -0.3228(8) 0.1823(6) 0.080 Uiso 1 d R .
H22B H 0.7171(9) -0.3165(8) 0.2084(6) 0.080 Uiso 1 d R .
C23 C 0.6792(9) -0.3050(8) 0.0763(7) 0.035(3) Uani 1 d . .
H23A H 0.7128(9) -0.3691(8) 0.0680(7) 0.080 Uiso 1 d R .
H23B H 0.6752(9) -0.2817(8) 0.0302(7) 0.080 Uiso 1 d R .
C24 C 0.5694(8) -0.3190(7) 0.0989(6) 0.026(2) Uani 1 d . .
H24A H 0.5319(8) -0.3690(7) 0.0620(6) 0.080 Uiso 1 d R .
H24B H 0.5740(8) -0.3435(7) 0.1445(6) 0.080 Uiso 1 d R .
C25 C 0.4740(9) -0.2021(8) 0.0370(6) 0.030(3) Uani 1 d . .
H25A H 0.4222(9) -0.2519(8) 0.0134(6) 0.080 Uiso 1 d R .
H25B H 0.5322(9) -0.2059(8) 0.0058(6) 0.080 Uiso 1 d R .
C26 C 0.4246(8) -0.0983(8) 0.0458(6) 0.025(2) Uani 1 d . .
C27 C 0.4183(8) -0.0386(8) 0.2762(6) 0.029(3) Uani 1 d . .
H27A H 0.3753(8) -0.0478(8) 0.3155(6) 0.080 Uiso 1 d R .
H27B H 0.3740(8) -0.0453(8) 0.2314(6) 0.080 Uiso 1 d R .
C28 C 0.4677(9) 0.0680(8) 0.2946(6) 0.034(3) Uani 1 d . .
C29 C 0.7801(9) -0.0331(9) 0.3343(6) 0.035(3) Uani 1 d . .
H29A H 0.8262(9) -0.0498(9) 0.3731(6) 0.080 Uiso 1 d R .
H29B H 0.7269(9) 0.0100(9) 0.3573(6) 0.080 Uiso 1 d R .
C30 C 0.8425(9) 0.0245(8) 0.2874(6) 0.032(3) Uani 1 d . .
C31 C 0.8366(8) -0.2014(9) 0.0987(6) 0.033(3) Uani 1 d . .
H31A H 0.8695(8) -0.2603(9) 0.0723(6) 0.080 Uiso 1 d R .
H31B H 0.8857(8) -0.1678(9) 0.1375(6) 0.080 Uiso 1 d R .
C32 C 0.8095(9) -0.1312(8) 0.0451(6) 0.028(2) Uani 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N4 Pb1 N3 69.1(3) . . ?
N4 Pb1 N2 107.0(3) . . ?
N3 Pb1 N2 68.2(3) . . ?
N4 Pb1 N1 69.7(3) . . ?
N3 Pb1 N1 105.9(3) . . ?
N2 Pb1 N1 69.0(3) . . ?
N4 Pb1 O3 122.4(3) . . ?
N3 Pb1 O3 63.0(3) . . ?
N2 Pb1 O3 83.3(2) . . ?
N1 Pb1 O3 152.3(2) . . ?
N4 Pb1 O4 61.4(2) . . ?
N3 Pb1 O4 82.8(2) . . ?
N2 Pb1 O4 151.0(2) . . ?
N1 Pb1 O4 123.0(2) . . ?
O3 Pb1 O4 82.3(2) . . ?
N4 Pb1 O1 81.4(3) . . ?
N3 Pb1 O1 150.6(3) . . ?
N2 Pb1 O1 122.6(2) . . ?
N1 Pb1 O1 61.3(2) . . ?
O3 Pb1 O1 140.1(2) . . ?
O4 Pb1 O1 83.6(2) . . ?
N4 Pb1 O2 152.4(3) . . ?
N3 Pb1 O2 119.3(2) . . ?
N2 Pb1 O2 59.4(3) . . ?
N1 Pb1 O2 82.7(3) . . ?
O3 Pb1 O2 81.9(2) . . ?
O4 Pb1 O2 142.0(2) . . ?
O1 Pb1 O2 86.8(2) . . ?
N4 Pb1 O29 127.9(3) . . ?
N3 Pb1 O29 130.9(4) . . ?
N2 Pb1 O29 124.9(3) . . ?
N1 Pb1 O29 123.1(4) . . ?
O3 Pb1 O29 71.7(3) . . ?
O4 Pb1 O29 73.4(3) . . ?
O1 Pb1 O29 68.6(3) . . ?
O2 Pb1 O29 68.8(3) . . ?
N10 Pb2 N11 70.5(3) . . ?
N10 Pb2 N9 69.7(3) . . ?
N11 Pb2 N9 107.2(3) . . ?
N10 Pb2 N12 107.8(3) . . ?
N11 Pb2 N12 68.7(3) . . ?
N9 Pb2 N12 69.2(3) . . ?
N10 Pb2 O7 124.2(3) . . ?
N11 Pb2 O7 63.0(2) . . ?
N9 Pb2 O7 151.8(3) . . ?
N12 Pb2 O7 82.8(2) . . ?
N10 Pb2 O6 62.8(2) . . ?
N11 Pb2 O6 85.1(2) . . ?
N9 Pb2 O6 123.1(2) . . ?
N12 Pb2 O6 153.8(3) . . ?
O7 Pb2 O6 83.7(2) . . ?
N10 Pb2 O5 81.7(3) . . ?
N11 Pb2 O5 152.2(2) . . ?
N9 Pb2 O5 62.1(2) . . ?
N12 Pb2 O5 123.0(2) . . ?
O7 Pb2 O5 138.4(2) . . ?
O6 Pb2 O5 81.4(2) . . ?
N10 Pb2 O8 152.0(2) . . ?
N11 Pb2 O8 119.4(2) . . ?
N9 Pb2 O8 82.3(3) . . ?
N12 Pb2 O8 59.4(2) . . ?
O7 Pb2 O8 81.0(2) . . ?
O6 Pb2 O8 139.6(2) . . ?
O5 Pb2 O8 85.8(2) . . ?
O10' Cl1 O12' 130.8(26) . . ?
O10' Cl1 O9 110.9(18) . . ?
O12' Cl1 O9 117.9(20) . . ?
O10' Cl1 O11 41.4(18) . . ?
O12' Cl1 O11 112.2(20) . . ?
O9 Cl1 O11 119.3(7) . . ?
O10' Cl1 O12 137.9(19) . . ?
O12' Cl1 O12 14.7(22) . . ?
O9 Cl1 O12 110.7(8) . . ?
O11 Cl1 O12 109.3(8) . . ?
O10' Cl1 O10 70.7(19) . . ?
O12' Cl1 O10 90.8(21) . . ?
O9 Cl1 O10 104.0(7) . . ?
O11 Cl1 O10 107.3(7) . . ?
O12 Cl1 O10 105.3(9) . . ?
O10' Cl1 O11' 92.8(22) . . ?
O12' Cl1 O11' 103.4(24) . . ?
O9 Cl1 O11' 77.7(13) . . ?
O11 Cl1 O11' 58.9(13) . . ?
O12 Cl1 O11' 89.6(14) . . ?
O10 Cl1 O11' 163.0(13) . . ?
O16 Cl2 O13 108.4(5) . . ?
O16 Cl2 O14 110.0(7) . . ?
O13 Cl2 O14 109.8(6) . . ?
O16 Cl2 O15 109.2(6) . . ?
O13 Cl2 O15 108.9(6) . . ?
O14 Cl2 O15 110.5(6) . . ?
O18 Cl3 O19 114.5(21) . . ?
O18 Cl3 O17 117.9(17) . . ?
O19 Cl3 O17 109.4(15) . . ?
O18 Cl3 O20 108.6(17) . . ?
O19 Cl3 O20 99.6(16) . . ?
O17 Cl3 O20 104.9(10) . . ?
O23 Cl4 O24' 133.9(10) . . ?
O23 Cl4 O22 112.3(7) . . ?
O24' Cl4 O22 54.8(11) . . ?
O23 Cl4 O23' 45.9(10) . . ?
O24' Cl4 O23' 112.1(8) . . ?
O22 Cl4 O23' 140.7(10) . . ?
O23 Cl4 O21 113.7(7) . . ?
O24' Cl4 O21 112.0(7) . . ?
O22 Cl4 O21 110.4(7) . . ?
O23' Cl4 O21 108.7(7) . . ?
O23 Cl4 O22' 62.1(10) . . ?
O24' Cl4 O22' 110.1(7) . . ?
O22 Cl4 O22' 57.8(11) . . ?
O23' Cl4 O22' 107.4(7) . . ?
O21 Cl4 O22' 106.2(7) . . ?
O23 Cl4 O24 108.6(7) . . ?
O24' Cl4 O24 52.5(11) . . ?
O22 Cl4 O24 106.4(7) . . ?
O23' Cl4 O24 66.1(10) . . ?
O21 Cl4 O24 104.9(6) . . ?
O22' Cl4 O24 148.6(9) . . ?
C10 O1 Pb1 111.0(7) . . ?
C12 O2 Pb1 102.2(7) . . ?
C14 O3 Pb1 114.8(7) . . ?
C16 O4 Pb1 111.3(6) . . ?
C26 O5 Pb2 110.8(6) . . ?
C28 O6 Pb2 112.0(7) . . ?
C30 O7 Pb2 114.9(7) . . ?
C32 O8 Pb2 106.7(7) . . ?
O30 O29 Pb1 163.0(7) . . ?
O31 O30 O29 68.5(9) . . ?
C9 N1 C1 110.7(9) . . ?
C9 N1 C8 110.8(8) . . ?
C1 N1 C8 110.7(8) . . ?
C9 N1 Pb1 105.2(6) . . ?
C1 N1 Pb1 110.5(6) . . ?
C8 N1 Pb1 108.8(6) . . ?
C11 N2 C3 109.1(8) . . ?
C11 N2 C2 108.8(8) . . ?
C3 N2 C2 109.3(8) . . ?
C11 N2 Pb1 108.5(6) . . ?
C3 N2 Pb1 111.6(6) . . ?
C2 N2 Pb1 109.5(6) . . ?
C13 N3 C4 109.3(8) . . ?
C13 N3 C5 109.6(8) . . ?
C4 N3 C5 109.5(8) . . ?
C13 N3 Pb1 106.1(6) . . ?
C4 N3 Pb1 111.2(6) . . ?
C5 N3 Pb1 111.2(6) . . ?
C15 N4 C6 109.7(8) . . ?
C15 N4 C7 110.1(8) . . ?
C6 N4 C7 109.8(9) . . ?
C15 N4 Pb1 106.9(6) . . ?
C6 N4 Pb1 110.2(6) . . ?
C7 N4 Pb1 110.0(6) . . ?
C24 N9 C25 109.4(8) . . ?
C24 N9 C17 111.0(8) . . ?
C25 N9 C17 110.0(8) . . ?
C24 N9 Pb2 110.8(6) . . ?
C25 N9 Pb2 106.0(6) . . ?
C17 N9 Pb2 109.5(6) . . ?
C27 N10 C18 111.3(8) . . ?
C27 N10 C19 108.5(8) . . ?
C18 N10 C19 109.1(8) . . ?
C27 N10 Pb2 107.4(6) . . ?
C18 N10 Pb2 111.1(6) . . ?
C19 N10 Pb2 109.4(6) . . ?
C29 N11 C21 109.3(8) . . ?
C29 N11 C20 110.8(8) . . ?
C21 N11 C20 110.5(8) . . ?
C29 N11 Pb2 105.8(6) . . ?
C21 N11 Pb2 110.9(6) . . ?
C20 N11 Pb2 109.5(6) . . ?
C22 N12 C31 110.7(8) . . ?
C22 N12 C23 110.3(8) . . ?
C31 N12 C23 109.3(8) . . ?
C22 N12 Pb2 109.6(6) . . ?
C31 N12 Pb2 108.8(6) . . ?
C23 N12 Pb2 108.0(6) . . ?
N1 C1 C2 112.1(9) . . ?
N2 C2 C1 111.2(9) . . ?
N2 C3 C4 111.7(9) . . ?
N3 C4 C3 112.2(8) . . ?
N3 C5 C6 111.9(9) . . ?
N4 C6 C5 112.9(9) . . ?
N4 C7 C8 113.7(9) . . ?
N1 C8 C7 112.5(8) . . ?
N1 C9 C10 112.7(9) . . ?
O1 C10 N5 124.0(11) . . ?
O1 C10 C9 120.7(10) . . ?
N5 C10 C9 115.3(10) . . ?
N2 C11 C12 113.6(9) . . ?
O2 C12 N6 122.8(12) . . ?
O2 C12 C11 120.7(11) . . ?
N6 C12 C11 116.5(10) . . ?
N3 C13 C14 110.5(9) . . ?
O3 C14 N7 122.0(10) . . ?
O3 C14 C13 121.5(9) . . ?
N7 C14 C13 116.4(10) . . ?
N4 C15 C16 111.2(8) . . ?
O4 C16 N8 123.3(10) . . ?
O4 C16 C15 120.5(9) . . ?
N8 C16 C15 116.1(9) . . ?
N9 C17 C18 111.4(8) . . ?
N10 C18 C17 112.0(8) . . ?
C20 C19 N10 111.8(9) . . ?
N11 C20 C19 113.6(9) . . ?
N11 C21 C22 112.3(8) . . ?
N12 C22 C21 111.9(9) . . ?
N12 C23 C24 113.0(9) . . ?
N9 C24 C23 113.1(8) . . ?
N9 C25 C26 111.2(8) . . ?
O5 C26 N13 123.5(10) . . ?
O5 C26 C25 122.4(9) . . ?
N13 C26 C25 114.1(9) . . ?
N10 C27 C28 112.2(8) . . ?
O6 C28 N14 125.0(11) . . ?
O6 C28 C27 120.5(9) . . ?
N14 C28 C27 114.5(10) . . ?
N11 C29 C30 112.1(9) . . ?
O7 C30 N15 124.6(11) . . ?
O7 C30 C29 119.8(9) . . ?
N15 C30 C29 115.5(10) . . ?
N12 C31 C32 112.3(8) . . ?
O8 C32 N16 123.8(10) . . ?
O8 C32 C31 122.4(10) . . ?
N16 C32 C31 113.8(9) . . ?
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 N4 2.610(9) . ?
Pb1 N3 2.629(9) . ?
Pb1 N2 2.641(8) . ?
Pb1 N1 2.654(8) . ?
Pb1 O3 2.667(7) . ?
Pb1 O4 2.770(7) . ?
Pb1 O1 2.777(8) . ?
Pb1 O2 2.902(8) . ?
Pb1 O29 3.52(2) . ?
Pb2 N10 2.572(9) . ?
Pb2 N11 2.614(8) . ?
Pb2 N9 2.627(8) . ?
Pb2 N12 2.666(8) . ?
Pb2 O7 2.675(7) . ?
Pb2 O6 2.711(7) . ?
Pb2 O5 2.783(7) . ?
Pb2 O8 2.883(8) . ?
Cl1 O10' 1.31(4) . ?
Cl1 O12' 1.32(5) . ?
Cl1 O9 1.393(9) . ?
Cl1 O11 1.421(12) . ?
Cl1 O12 1.46(2) . ?
Cl1 O10 1.518(13) . ?
Cl1 O11' 1.69(4) . ?
Cl2 O16 1.423(9) . ?
Cl2 O13 1.428(9) . ?
Cl2 O14 1.435(9) . ?
Cl2 O15 1.441(9) . ?
Cl3 O18 1.22(2) . ?
Cl3 O19 1.32(2) . ?
Cl3 O17 1.381(13) . ?
Cl3 O20 1.44(2) . ?
Cl4 O23 1.444(8) . ?
Cl4 O24' 1.450(8) . ?
Cl4 O22 1.477(8) . ?
Cl4 O23' 1.484(8) . ?
Cl4 O21 1.488(7) . ?
Cl4 O22' 1.504(8) . ?
Cl4 O24 1.522(8) . ?
O1 C10 1.232(13) . ?
O2 C12 1.234(13) . ?
O3 C14 1.235(13) . ?
O4 C16 1.252(12) . ?
O5 C26 1.231(12) . ?
O6 C28 1.230(13) . ?
O7 C30 1.230(13) . ?
O8 C32 1.219(12) . ?
O29 O30 2.76(2) . ?
O30 O31 2.61(3) . ?
N1 C9 1.468(14) . ?
N1 C1 1.484(13) . ?
N1 C8 1.497(14) . ?
N2 C11 1.471(13) . ?
N2 C3 1.475(14) . ?
N2 C2 1.498(13) . ?
N3 C13 1.474(13) . ?
N3 C4 1.498(12) . ?
N3 C5 1.499(13) . ?
N4 C15 1.477(13) . ?
N4 C6 1.487(13) . ?
N4 C7 1.495(13) . ?
N5 C10 1.335(14) . ?
N6 C12 1.308(14) . ?
N7 C14 1.326(13) . ?
N8 C16 1.320(13) . ?
N9 C24 1.480(12) . ?
N9 C25 1.488(13) . ?
N9 C17 1.495(13) . ?
N10 C27 1.454(13) . ?
N10 C18 1.486(12) . ?
N10 C19 1.510(13) . ?
N11 C29 1.464(13) . ?
N11 C21 1.482(13) . ?
N11 C20 1.484(13) . ?
N12 C22 1.458(13) . ?
N12 C31 1.467(13) . ?
N12 C23 1.485(13) . ?
N13 C26 1.322(13) . ?
N14 C28 1.306(14) . ?
N15 C30 1.322(13) . ?
N16 C32 1.345(14) . ?
C1 C2 1.537(15) . ?
C3 C4 1.516(15) . ?
C5 C6 1.509(15) . ?
C7 C8 1.50(2) . ?
C9 C10 1.53(2) . ?
C11 C12 1.52(2) . ?
C13 C14 1.512(15) . ?
C15 C16 1.524(14) . ?
C17 C18 1.522(15) . ?
C19 C20 1.509(15) . ?
C21 C22 1.531(15) . ?
C23 C24 1.505(15) . ?
C25 C26 1.528(14) . ?
C27 C28 1.535(15) . ?
C29 C30 1.52(2) . ?
C31 C32 1.527(15) . ?
