# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Pb2TbL2
_database_code_depnum_ccdc_archive 'CCDC 1043820'
_audit_update_record             
;
2015-01-16 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_audit_creation_date             2013-07-04
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'0.5(C192 H144 N28 O24 Pb4 Tb2), 2(H2 O), 2(C3 H7 N O), 3(O)'
_chemical_formula_sum            'C102 H90 N16 O19 Pb2 Tb'
_chemical_formula_weight         2417.19
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.32630(10)
_cell_length_b                   20.7018(2)
_cell_length_c                   18.2517(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.6420(10)
_cell_angle_gamma                90
_cell_volume                     4655.49(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    11.259
_exptl_absorpt_correction_T_max  0.324
_exptl_absorpt_correction_T_min  0.165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2390
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.873
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22586
_diffrn_reflns_point_group_measured_fraction_full 0.873
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.481
_diffrn_reflns_theta_min         3.229
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.873
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6768
_reflns_number_total             7340
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         1.617
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         7340
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0400
_refine_ls_restrained_S_all      1.063
_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)+(0.0764P)²+4.1439P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1139
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N7-C1D
 1.25 with sigma of 0.02
 O7-C1D
 1.15 with sigma of 0.02
 N7-C1E = N7-C16
 1.45 with sigma of 0.02
3.a Free rotating group:
 O6(H6A,H6B)
3.b Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C62(H62A,H62B), C1C(H1CA,H1CB)
3.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C57(H57), C19(H19), C27(H27), C1A(H1A), C32(H32), C1B(H1B),
 C37(H37), C1D(H1D)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C1E(H1EA,H1EB,H1EC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.12668(2) 0.18888(2) 0.94536(2) 0.03602(11) Uani 1 1 d . . . . .
Tb2 Tb 0.5000 0.5000 0.5000 0.03561(14) Uani 1 2 d S . P . .
C13 C 0.4163(5) 0.1849(3) 0.9601(3) 0.0458(14) Uani 1 1 d . . . . .
N15 N 0.1740(4) 0.3196(2) 0.9191(3) 0.0446(11) Uani 1 1 d . . . . .
N20 N 0.3229(4) 0.2185(3) 0.9391(2) 0.0443(11) Uani 1 1 d . . . . .
N21 N 0.4653(4) 0.2821(3) 0.9206(2) 0.0500(12) Uani 1 1 d . . . . .
C24 C 0.2803(5) 0.3238(3) 0.8829(3) 0.0459(13) Uani 1 1 d . . . . .
C28 C 0.6237(7) 0.3103(4) 0.7925(4) 0.065(2) Uani 1 1 d . . . . .
H28 H 0.6530 0.2751 0.8178 0.078 Uiso 1 1 calc R U . . .
C29 C 0.5070(5) 0.2241(4) 0.9478(3) 0.0538(16) Uani 1 1 d . . . . .
C33 C 0.5293(6) 0.3407(5) 0.9069(3) 0.0585(19) Uani 1 1 d . . . . .
C36 C 0.6118(6) 0.2037(5) 0.9639(4) 0.069(2) Uani 1 1 d . . . . .
C39 C 0.6245(6) 0.1426(5) 0.9919(4) 0.075(2) Uani 1 1 d . . . . .
C44 C 0.5540(5) 0.3510(3) 0.8269(3) 0.0485(14) Uani 1 1 d . . . . .
C49 C 0.1832(6) 0.3569(3) 0.9892(3) 0.0526(15) Uani 1 1 d . . . . .
H49A H 0.2546 0.3502 1.0116 0.063 Uiso 1 1 calc R U . . .
H49B H 0.1750 0.4027 0.9789 0.063 Uiso 1 1 calc R U . . .
C52 C 0.5346(6) 0.1028(5) 1.0046(4) 0.0631(18) Uani 1 1 d . . . . .
C57 C 0.5106(6) 0.4015(3) 0.7889(3) 0.0546(15) Uani 1 1 d . . . . .
H57 H 0.4637 0.4296 0.8120 0.065 Uiso 1 1 calc R U . . .
C59 C 0.6511(6) 0.3209(4) 0.7208(4) 0.0577(17) Uani 1 1 d . . . . .
C62 C 0.0865(5) 0.3446(3) 0.8707(3) 0.0497(14) Uani 1 1 d . . . . .
H62A H 0.1090 0.3849 0.8486 0.060 Uiso 1 1 calc R U . . .
H62B H 0.0225 0.3531 0.8990 0.060 Uiso 1 1 calc R U . . .
C68 C 0.3562(4) 0.2754(3) 0.9155(3) 0.0429(13) Uani 1 1 d . . . . .
C73 C 0.4298(5) 0.1231(4) 0.9891(3) 0.0532(15) Uani 1 1 d . . . . .
N9 N 0.0811(5) 0.3691(3) 1.1034(3) 0.0528(12) Uani 1 1 d . . . . .
C11 C 0.6054(5) 0.3707(3) 0.6814(3) 0.0403(12) Uani 1 1 d . . . . .
C12 C 0.6328(5) 0.3793(3) 0.6019(3) 0.0433(13) Uani 1 1 d . . . . .
C1 C 0.5354(5) 0.4121(3) 0.7151(3) 0.0491(14) Uani 1 1 d . . . . .
N16 N 0.0365(4) 0.2851(3) 1.0326(3) 0.0505(12) Uani 1 1 d . . . . .
C17 C 0.0988(5) 0.3362(3) 1.0408(3) 0.0461(13) Uani 1 1 d . . . . .
O3 O 0.7032(4) 0.3434(2) 0.5761(2) 0.0543(10) Uani 1 1 d . . . . .
O4 O 0.5825(4) 0.4211(2) 0.5661(2) 0.0618(12) Uani 1 1 d . . . . .
N5 N 0.0012(5) 0.3102(2) 0.7500(3) 0.0515(13) Uani 1 1 d . . . . .
N6 N 0.0910(4) 0.2350(2) 0.8146(2) 0.0433(10) Uani 1 1 d . . . . .
C7 C 0.0523(5) 0.4168(3) 0.6997(3) 0.0456(13) Uani 1 1 d . . . . .
C8 C 0.2030(5) 0.4121(3) 1.2020(4) 0.0535(16) Uani 1 1 d . . . . .
C2 C 0.2137(5) 0.4977(3) 0.6467(3) 0.0393(12) Uani 1 1 d . . . . .
C3 C 0.0599(5) 0.2959(3) 0.8118(3) 0.0454(13) Uani 1 1 d . . . . .
O13 O 0.4033(5) 0.3216(3) 1.4214(4) 0.0840(17) Uani 1 1 d . . . . .
C14 C 0.1517(6) 0.3925(3) 0.6812(4) 0.0534(15) Uani 1 1 d . . . . .
C15 C -0.0380(5) 0.3742(3) 0.7276(4) 0.0560(16) Uani 1 1 d . . . . .
C4 C 0.0497(5) 0.2072(3) 0.7498(3) 0.0490(14) Uani 1 1 d . . . . .
C5 C -0.0060(5) 0.2546(3) 0.7085(3) 0.0507(14) Uani 1 1 d . . . . .
C18 C 0.3765(6) 0.3779(4) 1.4055(4) 0.0633(18) Uani 1 1 d . . . . .
C19 C 0.1142(5) 0.5225(3) 0.6655(3) 0.0473(13) Uani 1 1 d . . . . .
H19 H 0.1015 0.5666 0.6608 0.057 Uiso 1 1 calc R U . . .
C20 C -0.0271(5) 0.2835(3) 1.0940(3) 0.0519(14) Uani 1 1 d . . . . .
C21 C 0.0000(6) 0.3359(3) 1.1387(3) 0.0540(15) Uani 1 1 d . . . . .
C22 C 0.2322(5) 0.4317(3) 0.6543(3) 0.0490(14) Uani 1 1 d . . . . .
C23 C 0.0332(6) 0.4830(3) 0.6914(3) 0.0516(14) Uani 1 1 d . . . . .
C6 C -0.0520(7) 0.2403(5) 0.6397(4) 0.064(2) Uani 1 1 d . . . . .
C25 C 0.3165(5) 0.3899(3) 1.3350(4) 0.0568(16) Uani 1 1 d . . . . .
C26 C 0.2345(5) 0.4635(4) 1.2470(4) 0.0565(16) Uani 1 1 d . . . . .
C27 C 0.2892(5) 0.4519(4) 1.3134(4) 0.0613(18) Uani 1 1 d . . . . .
H27 H 0.3077 0.4865 1.3438 0.074 Uiso 1 1 calc R U . . .
C10 C -0.0501(7) 0.3471(4) 1.2053(4) 0.073(2) Uani 1 1 d . . . . .
C1A C -0.1079(7) 0.2408(4) 1.1145(4) 0.072(2) Uani 1 1 d . . . . .
H1A H -0.1279 0.2055 1.0855 0.086 Uiso 1 1 calc R U . . .
C31 C -0.0429(7) 0.1786(5) 0.6151(4) 0.072(2) Uani 1 1 d . . . . .
C32 C 0.0089(7) 0.1316(4) 0.6558(4) 0.075(2) Uani 1 1 d . . . . .
H32 H 0.0117 0.0898 0.6373 0.090 Uiso 1 1 calc R U . . .
C1B C 0.2337(6) 0.3510(4) 1.2231(4) 0.0627(18) Uani 1 1 d . . . . .
H1B H 0.2171 0.3164 1.1923 0.075 Uiso 1 1 calc R U . . .
C34 C 0.0572(7) 0.1444(4) 0.7239(4) 0.0657(19) Uani 1 1 d . . . . .
C35 C 0.2884(6) 0.3396(4) 1.2888(4) 0.0629(18) Uani 1 1 d . . . . .
C1C C 0.1392(7) 0.4259(4) 1.1320(4) 0.0660(18) Uani 1 1 d . . . . .
H1CA H 0.0872 0.4600 1.1409 0.079 Uiso 1 1 calc R U . . .
H1CB H 0.1883 0.4413 1.0953 0.079 Uiso 1 1 calc R U . . .
C37 C -0.1568(8) 0.2535(5) 1.1798(5) 0.091(3) Uani 1 1 d . . . . .
H37 H -0.2119 0.2261 1.1945 0.109 Uiso 1 1 calc R U . . .
C38 C -0.1280(8) 0.3052(5) 1.2251(5) 0.083(3) Uani 1 1 d . . . . .
O2 O 0.2868(4) 0.6005(2) 0.6261(2) 0.0546(10) Uani 1 1 d . . . . .
O1 O 0.3796(4) 0.5157(2) 0.5884(2) 0.0577(11) Uani 1 1 d . . . . .
O5 O 0.3958(5) 0.4251(3) 1.4458(3) 0.0822(16) Uani 1 1 d . . . . .
C9 C 0.2991(5) 0.5411(3) 0.6179(3) 0.0424(13) Uani 1 1 d . . . . .
H73 H 0.367(5) 0.096(3) 1.001(3) 0.040(15) Uiso 1 1 d . . . . .
H52 H 0.538(5) 0.062(3) 1.017(3) 0.037(16) Uiso 1 1 d . . . . .
O6 O 0.8319(8) 0.2998(4) 0.9232(5) 0.115(2) Uiso 1 1 d G . . . .
H6A H 0.8460 0.2627 0.9060 0.172 Uiso 1 1 d G U . . .
H6B H 0.8331 0.3276 0.8890 0.172 Uiso 1 1 d G U . . .
O7 O 0.3948(15) 0.4672(9) 0.9594(10) 0.211(6) Uiso 1 1 d D . . . .
O8 O -0.1788(13) 0.4227(7) 0.8839(9) 0.195(5) Uiso 1 1 d . . . . .
C16 C 0.2368(19) 0.5154(11) 0.8661(13) 0.196(9) Uiso 1 1 d D . . . .
H16A H 0.1601 0.5083 0.8692 0.295 Uiso 1 1 calc R U . . .
H16B H 0.2716 0.4760 0.8521 0.295 Uiso 1 1 calc R U . . .
H16C H 0.2499 0.5481 0.8302 0.295 Uiso 1 1 calc R U . . .
N7 N 0.282(3) 0.5370(15) 0.9396(17) 0.362(18) Uiso 1 1 d D . . . .
C1E C 0.248(2) 0.6059(13) 0.9490(16) 0.244(12) Uiso 1 1 d D . . . .
H1EA H 0.2437 0.6267 0.9020 0.365 Uiso 1 1 calc R U . . .
H1EB H 0.2995 0.6279 0.9802 0.365 Uiso 1 1 calc R U . . .
H1EC H 0.1776 0.6072 0.9706 0.365 Uiso 1 1 calc R U . . .
H23 H -0.042(7) 0.496(3) 0.701(4) 0.057(19) Uiso 1 1 d . . . . .
H24A H 0.310(5) 0.359(3) 0.884(3) 0.034(15) Uiso 1 1 d . . . . .
H33A H 0.595(7) 0.338(4) 0.937(4) 0.07(2) Uiso 1 1 d . . . . .
H15A H -0.095(6) 0.365(3) 0.690(4) 0.053(18) Uiso 1 1 d . . . . .
H6 H -0.080(7) 0.271(4) 0.623(5) 0.06(2) Uiso 1 1 d . . . . .
H10 H -0.046(8) 0.387(5) 1.230(6) 0.09(3) Uiso 1 1 d . . . . .
H33B H 0.477(6) 0.371(3) 0.915(4) 0.045(18) Uiso 1 1 d . . . . .
H15B H -0.070(6) 0.398(4) 0.773(4) 0.06(2) Uiso 1 1 d . . . . .
H35 H 0.321(7) 0.294(4) 1.306(4) 0.06(2) Uiso 1 1 d . . . . .
H34 H 0.084(5) 0.116(3) 0.756(4) 0.046(17) Uiso 1 1 d . . . . .
H14 H 0.165(6) 0.355(4) 0.685(4) 0.047(18) Uiso 1 1 d . . . . .
H31 H -0.072(7) 0.158(4) 0.567(5) 0.07(2) Uiso 1 1 d . . . . .
H38 H -0.150(8) 0.307(4) 1.277(6) 0.08(3) Uiso 1 1 d . . . . .
H26 H 0.229(6) 0.503(4) 1.230(4) 0.048(18) Uiso 1 1 d . . . . .
H22 H 0.304(5) 0.414(3) 0.634(3) 0.035(14) Uiso 1 1 d . . . . .
H36 H 0.667(7) 0.232(4) 0.958(4) 0.057(19) Uiso 1 1 d . . . . .
H39 H 0.705(6) 0.128(3) 1.015(4) 0.048(17) Uiso 1 1 d . . . . .
H59 H 0.694(7) 0.294(4) 0.705(5) 0.06(2) Uiso 1 1 d . . . . .
H24B H 0.256(7) 0.317(4) 0.822(5) 0.07(2) Uiso 1 1 d . . . . .
H1 H 0.489(9) 0.438(5) 0.674(6) 0.12(4) Uiso 1 1 d . . . . .
C1D C 0.347(3) 0.5080(14) 0.9944(16) 0.260(15) Uiso 1 1 d D . . . .
H1D H 0.3516 0.5172 1.0443 0.312 Uiso 1 1 calc R U . . .
O9 O 0.0000 0.5000 1.0000 0.222(10) Uiso 1 2 d S . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 N20 2.501(5) . ?
Pb1 O3 2.627(4) 4_566 ?
Pb1 N6 2.597(4) . ?
Pb1 O2 2.503(4) 2_546 ?
Tb2 O4 2.255(4) . ?
Tb2 O4 2.255(4) 3_666 ?
Tb2 O1 2.246(4) 3_666 ?
Tb2 O1 2.246(4) . ?
Tb2 O5 2.227(5) 3_667 ?
Tb2 O5 2.227(5) 1_554 ?
C13 N20 1.390(8) . ?
C13 C29 1.404(9) . ?
C13 C73 1.393(10) . ?
N15 C24 1.486(8) . ?
N15 C49 1.496(8) . ?
N15 C62 1.468(8) . ?
N20 C68 1.324(8) . ?
N21 C29 1.394(9) . ?
N21 C33 1.472(9) . ?
N21 C68 1.353(8) . ?
C24 C68 1.484(9) . ?
C28 C44 1.368(11) . ?
C28 C59 1.379(10) . ?
C29 C36 1.383(10) . ?
C33 C44 1.514(8) . ?
C36 C39 1.370(14) . ?
C39 C52 1.407(12) . ?
C44 C57 1.357(10) . ?
C49 C17 1.486(9) . ?
C52 C73 1.379(10) . ?
C57 C1 1.407(9) . ?
C59 C11 1.369(9) . ?
C62 C3 1.503(9) . ?
N9 C17 1.353(8) . ?
N9 C21 1.387(9) . ?
N9 C1C 1.465(9) . ?
C11 C12 1.510(8) . ?
C11 C1 1.373(9) . ?
C12 O3 1.246(7) . ?
C12 O4 1.241(7) . ?
N16 C17 1.314(8) . ?
N16 C20 1.386(8) . ?
O3 Pb1 2.627(4) 4_665 ?
N5 C3 1.355(8) . ?
N5 C15 1.465(9) . ?
N5 C5 1.378(9) . ?
N6 C3 1.318(8) . ?
N6 C4 1.399(8) . ?
C7 C14 1.375(10) . ?
C7 C15 1.520(9) . ?
C7 C23 1.399(9) . ?
C8 C26 1.393(9) . ?
C8 C1B 1.372(11) . ?
C8 C1C 1.509(11) . ?
C2 C19 1.382(9) . ?
C2 C22 1.391(9) . ?
C2 C9 1.492(8) . ?
O13 C18 1.244(10) . ?
C14 C22 1.384(10) . ?
C4 C5 1.404(9) . ?
C4 C34 1.388(10) . ?
C5 C6 1.395(9) . ?
C18 C25 1.487(11) . ?
C18 O5 1.242(9) . ?
C19 C23 1.384(9) . ?
C20 C21 1.392(10) . ?
C20 C1A 1.392(10) . ?
C21 C10 1.398(10) . ?
C6 C31 1.361(13) . ?
C25 C27 1.380(11) . ?
C25 C35 1.379(10) . ?
C26 C27 1.391(11) . ?
C10 C38 1.351(13) . ?
C1A C37 1.377(12) . ?
C31 C32 1.371(13) . ?
C32 C34 1.387(11) . ?
C1B C35 1.380(11) . ?
C37 C38 1.391(13) . ?
O2 Pb1 2.503(4) 2_556 ?
O2 C9 1.250(8) . ?
O1 C9 1.257(7) . ?
O5 Tb2 2.227(5) 1_556 ?
O7 C1D 1.223(18) . ?
C16 N7 1.506(18) . ?
N7 C1E 1.500(18) . ?
N7 C1D 1.395(19) . ?

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
N20 Pb1 O3 77.35(14) . 4_566 ?
N20 Pb1 N6 90.37(15) . . ?
N20 Pb1 O2 74.23(16) . 2_546 ?
N6 Pb1 O3 167.27(15) . 4_566 ?
O2 Pb1 O3 98.06(15) 2_546 4_566 ?
O2 Pb1 N6 81.55(15) 2_546 . ?
O4 Tb2 O4 180.0 . 3_666 ?
O1 Tb2 O4 91.03(16) . . ?
O1 Tb2 O4 88.97(16) 3_666 . ?
O1 Tb2 O4 88.97(16) . 3_666 ?
O1 Tb2 O4 91.03(16) 3_666 3_666 ?
O1 Tb2 O1 180.00(15) . 3_666 ?
O5 Tb2 O4 88.8(2) 3_667 3_666 ?
O5 Tb2 O4 91.2(2) 1_554 3_666 ?
O5 Tb2 O4 91.2(2) 3_667 . ?
O5 Tb2 O4 88.8(2) 1_554 . ?
O5 Tb2 O1 92.0(2) 1_554 . ?
O5 Tb2 O1 88.0(2) 3_667 . ?
O5 Tb2 O1 92.0(2) 3_667 3_666 ?
O5 Tb2 O1 88.0(2) 1_554 3_666 ?
O5 Tb2 O5 180.0 3_667 1_554 ?
N20 C13 C29 108.9(6) . . ?
N20 C13 C73 130.8(6) . . ?
C73 C13 C29 120.3(6) . . ?
C24 N15 C49 107.7(5) . . ?
C62 N15 C24 110.8(5) . . ?
C62 N15 C49 111.6(5) . . ?
C13 N20 Pb1 131.3(4) . . ?
C68 N20 Pb1 122.8(4) . . ?
C68 N20 C13 105.8(5) . . ?
C29 N21 C33 125.3(6) . . ?
C68 N21 C29 106.9(5) . . ?
C68 N21 C33 127.6(6) . . ?
C68 C24 N15 109.6(5) . . ?
C44 C28 C59 120.8(7) . . ?
N21 C29 C13 105.6(5) . . ?
C36 C29 C13 122.2(7) . . ?
C36 C29 N21 132.2(7) . . ?
N21 C33 C44 113.7(5) . . ?
C39 C36 C29 117.2(7) . . ?
C36 C39 C52 121.4(7) . . ?
C28 C44 C33 120.2(7) . . ?
C57 C44 C28 118.9(6) . . ?
C57 C44 C33 120.9(7) . . ?
C17 C49 N15 110.9(5) . . ?
C73 C52 C39 121.6(8) . . ?
C44 C57 C1 121.1(6) . . ?
C11 C59 C28 120.7(7) . . ?
N15 C62 C3 109.6(5) . . ?
N20 C68 N21 112.7(5) . . ?
N20 C68 C24 122.3(5) . . ?
N21 C68 C24 124.9(5) . . ?
C52 C73 C13 117.3(7) . . ?
C17 N9 C21 106.2(5) . . ?
C17 N9 C1C 128.0(6) . . ?
C21 N9 C1C 125.6(5) . . ?
C59 C11 C12 119.5(6) . . ?
C59 C11 C1 119.3(5) . . ?
C1 C11 C12 121.2(5) . . ?
O3 C12 C11 118.1(5) . . ?
O4 C12 C11 117.8(5) . . ?
O4 C12 O3 124.1(5) . . ?
C11 C1 C57 119.2(6) . . ?
C17 N16 C20 105.6(5) . . ?
N9 C17 C49 121.5(5) . . ?
N16 C17 C49 125.3(5) . . ?
N16 C17 N9 113.2(5) . . ?
C12 O3 Pb1 105.0(4) . 4_665 ?
C12 O4 Tb2 176.8(5) . . ?
C3 N5 C15 126.4(6) . . ?
C3 N5 C5 107.5(5) . . ?
C5 N5 C15 125.9(6) . . ?
C3 N6 Pb1 115.3(4) . . ?
C3 N6 C4 105.3(5) . . ?
C4 N6 Pb1 132.4(4) . . ?
C14 C7 C15 122.4(6) . . ?
C14 C7 C23 118.7(6) . . ?
C23 C7 C15 118.8(6) . . ?
C26 C8 C1C 118.9(7) . . ?
C1B C8 C26 118.0(7) . . ?
C1B C8 C1C 123.1(6) . . ?
C19 C2 C22 119.0(6) . . ?
C19 C2 C9 120.3(5) . . ?
C22 C2 C9 120.7(5) . . ?
N5 C3 C62 123.3(6) . . ?
N6 C3 C62 123.9(5) . . ?
N6 C3 N5 112.8(5) . . ?
C7 C14 C22 121.7(6) . . ?
N5 C15 C7 112.3(5) . . ?
N6 C4 C5 109.0(6) . . ?
C34 C4 N6 130.4(6) . . ?
C34 C4 C5 120.6(6) . . ?
N5 C5 C4 105.4(5) . . ?
N5 C5 C6 133.6(7) . . ?
C6 C5 C4 120.9(7) . . ?
O13 C18 C25 118.8(7) . . ?
O5 C18 O13 123.6(8) . . ?
O5 C18 C25 117.5(8) . . ?
C2 C19 C23 121.3(6) . . ?
N16 C20 C21 108.9(6) . . ?
N16 C20 C1A 131.1(6) . . ?
C1A C20 C21 120.0(6) . . ?
N9 C21 C20 106.1(5) . . ?
N9 C21 C10 131.7(7) . . ?
C20 C21 C10 122.3(7) . . ?
C14 C22 C2 119.7(6) . . ?
C19 C23 C7 119.6(6) . . ?
C31 C6 C5 117.5(8) . . ?
C27 C25 C18 121.0(6) . . ?
C35 C25 C18 120.8(7) . . ?
C35 C25 C27 118.2(7) . . ?
C27 C26 C8 120.1(7) . . ?
C25 C27 C26 121.2(6) . . ?
C38 C10 C21 117.5(8) . . ?
C37 C1A C20 116.5(8) . . ?
C6 C31 C32 121.9(7) . . ?
C31 C32 C34 122.2(8) . . ?
C8 C1B C35 121.8(6) . . ?
C32 C34 C4 116.9(8) . . ?
C25 C35 C1B 120.6(7) . . ?
N9 C1C C8 112.7(6) . . ?
C1A C37 C38 123.4(8) . . ?
C10 C38 C37 120.4(8) . . ?
C9 O2 Pb1 127.0(4) . 2_556 ?
C9 O1 Tb2 156.0(4) . . ?
C18 O5 Tb2 155.4(6) . 1_556 ?
O2 C9 C2 117.4(5) . . ?
O2 C9 O1 124.3(6) . . ?
O1 C9 C2 118.3(5) . . ?
C1E N7 C16 107(2) . . ?
C1D N7 C16 134(3) . . ?
C1D N7 C1E 119(3) . . ?
O7 C1D N7 101(3) . . ?

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Pb2EuL2
_database_code_depnum_ccdc_archive 'CCDC 1043821'
_audit_update_record             
;
2015-01-16 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_audit_creation_date             2013-06-21
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'0.5(C192 H144 Eu2 N28 O24 Pb4), 3(O), 2(H2 O), 2(C3 H7 N O)'
_chemical_formula_sum            'C102 H90 Eu N16 O19 Pb2'
_chemical_formula_weight         2410.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.31597(16)
_cell_length_b                   20.8623(2)
_cell_length_c                   18.2267(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.6890(11)
_cell_angle_gamma                90
_cell_volume                     4681.11(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    12.278
_exptl_absorpt_correction_T_max  0.293
_exptl_absorpt_correction_T_min  0.165
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2386
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.854
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13080
_diffrn_reflns_point_group_measured_fraction_full 0.854
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         62.536
_diffrn_reflns_theta_min         3.220
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.854
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_radiation_type           'CU K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6461
_reflns_number_total             7230
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_refine_diff_density_max         1.930
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         7230
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0361
_refine_ls_restrained_S_all      0.883
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1000P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1162
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O0AA(H0AA,H0AB)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C20(H20A,H20B), C27(H27A,H27B), C31(H31A,H31B), C41(H41A,H41B),
 C57(H57A,H57B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C14(H14), C15(H15), C17(H17), C32(H32), C34(H34), C42(H42), C44(H44),
 C51(H51), C18(H18)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
H5 H 0.655(8) 0.688(4) -0.271(6) 0.07(3) Uiso 1 1 d . . . . .
H9 H 0.002(9) 0.569(5) 0.323(6) 0.09(3) Uiso 1 1 d . . . . .
H10 H -0.198(6) 0.710(3) 0.303(4) 0.042(18) Uiso 1 1 d . . . . .
H13 H 0.580(6) 0.846(4) 0.437(4) 0.05(2) Uiso 1 1 d . . . . .
H33 H -0.172(7) 0.770(4) 0.048(4) 0.05(2) Uiso 1 1 d . . . . .
H36 H 0.133(5) 0.904(3) 0.002(3) 0.029(15) Uiso 1 1 d . . . . .
H37 H -0.150(12) 0.735(7) 0.184(8) 0.14(5) Uiso 1 1 d . . . . .
H38 H 0.023(7) 0.577(4) 0.186(5) 0.06(2) Uiso 1 1 d . . . . .
H46 H -0.189(7) 0.867(4) -0.011(4) 0.05(2) Uiso 1 1 d . . . . .
H47 H -0.047(6) 0.941(4) -0.018(4) 0.048(19) Uiso 1 1 d . . . . .
H49 H 0.283(7) 0.692(3) -0.186(5) 0.06(2) Uiso 1 1 d . . . . .
H53 H 0.429(8) 0.880(5) 0.248(6) 0.07(3) Uiso 1 1 d . . . . .
H54 H 0.539(9) 0.617(5) -0.240(6) 0.09(3) Uiso 1 1 d . . . . .
H59 H 0.500(9) 0.904(5) 0.366(7) 0.10(4) Uiso 1 1 d . . . . .
H60 H 0.724(7) 0.784(4) -0.204(5) 0.07(2) Uiso 1 1 d . . . . .
C1 C 0.5049(5) 0.7462(3) 0.2941(3) 0.0444(14) Uani 1 1 d . . . . .
C2 C -0.1078(5) 0.6305(3) 0.3197(3) 0.0347(12) Uani 1 1 d . . . . .
C3 C -0.1364(5) 0.6222(3) 0.3986(3) 0.0392(13) Uani 1 1 d . . . . .
C4 C 0.5519(6) 0.7602(4) 0.3630(4) 0.0564(18) Uani 1 1 d . . . . .
H4 H 0.5865 0.7287 0.3913 0.068 Uiso 1 1 calc R U . . .
C5 C 0.6244(8) 0.6936(5) -0.2244(5) 0.073(3) Uani 1 1 d . . . . .
C6 C 0.2945(6) 0.5877(4) -0.1998(4) 0.0518(17) Uani 1 1 d . . . . .
C7 C 0.2176(5) 0.6781(3) 0.1192(3) 0.0396(13) Uani 1 1 d . . . . .
H7A H 0.1871 0.6355 0.1122 0.048 Uiso 1 1 calc R U . . .
H7B H 0.2271 0.6857 0.1714 0.048 Uiso 1 1 calc R U . . .
C8 C 0.4455(5) 0.5843(3) 0.3013(3) 0.0382(13) Uani 1 1 d . . . . .
C9 C -0.0401(6) 0.5891(3) 0.2850(4) 0.0436(14) Uani 1 1 d . . . . .
C10 C -0.1511(6) 0.6820(3) 0.2813(4) 0.0495(17) Uani 1 1 d . . . . .
C12 C 0.0842(5) 0.8171(3) 0.0412(3) 0.0404(14) Uani 1 1 d . . . . .
C13 C 0.5447(7) 0.8216(5) 0.3871(4) 0.066(2) Uani 1 1 d . . . . .
C14 C 0.2095(6) 0.6596(4) -0.2876(4) 0.0577(18) Uani 1 1 d . . . . .
H14 H 0.1894 0.7011 -0.3005 0.069 Uiso 1 1 calc R U . . .
C15 C 0.3462(6) 0.6078(3) 0.3202(4) 0.0491(16) Uani 1 1 d . . . . .
H15 H 0.3326 0.6516 0.3163 0.059 Uiso 1 1 calc R U . . .
C17 C 0.2656(5) 0.5675(3) 0.3452(3) 0.0400(13) Uani 1 1 d . . . . .
H17 H 0.1988 0.5844 0.3577 0.048 Uiso 1 1 calc R U . . .
C19 C 0.3992(5) 0.6642(3) -0.0383(3) 0.0420(14) Uani 1 1 d . . . . .
C20 C 0.5358(5) 0.6273(3) 0.2749(4) 0.0482(15) Uani 1 1 d . . . . .
H20A H 0.5904 0.6320 0.3140 0.058 Uiso 1 1 calc R U . . .
H20B H 0.5700 0.6070 0.2337 0.058 Uiso 1 1 calc R U . . .
C22 C 0.1993(5) 0.4579(3) 0.3791(3) 0.0367(13) Uani 1 1 d . . . . .
C23 C 0.1425(5) 0.7269(3) 0.0862(3) 0.0366(13) Uani 1 1 d . . . . .
C24 C 0.2841(5) 0.5027(3) 0.3517(3) 0.0341(12) Uani 1 1 d . . . . .
C25 C -0.0559(5) 0.6523(3) 0.1741(3) 0.0408(14) Uani 1 1 d . . . . .
C27 C -0.0313(6) 0.6629(4) 0.0944(3) 0.0494(16) Uani 1 1 d . . . . .
H27A H 0.0083 0.6261 0.0768 0.059 Uiso 1 1 calc R U . . .
H27B H -0.0993 0.6654 0.0664 0.059 Uiso 1 1 calc R U . . .
C28 C -0.0079(5) 0.7784(3) 0.0529(3) 0.0409(14) Uani 1 1 d . . . . .
C29 C 0.5244(5) 0.7156(3) -0.0932(4) 0.0463(15) Uani 1 1 d . . . . .
C31 C 0.3144(6) 0.6448(3) 0.0137(4) 0.0483(15) Uani 1 1 d . . . . .
H31A H 0.3217 0.5995 0.0246 0.058 Uiso 1 1 calc R U . . .
H31B H 0.2431 0.6518 -0.0089 0.058 Uiso 1 1 calc R U . . .
C32 C 0.3860(5) 0.4781(3) 0.3337(3) 0.0406(13) Uani 1 1 d . . . . .
H32 H 0.4000 0.4345 0.3387 0.049 Uiso 1 1 calc R U . . .
C33 C -0.1139(6) 0.7988(5) 0.0372(4) 0.058(2) Uani 1 1 d . . . . .
C34 C 0.4654(5) 0.5187(3) 0.3086(3) 0.0412(14) Uani 1 1 d . . . . .
H34 H 0.5327 0.5022 0.2965 0.049 Uiso 1 1 calc R U . . .
C35 C 0.4390(5) 0.7053(3) 0.1903(3) 0.0370(13) Uani 1 1 d . . . . .
C36 C 0.0706(6) 0.8785(4) 0.0122(3) 0.0459(15) Uani 1 1 d . . . . .
C37 C -0.1252(6) 0.6935(4) 0.2095(4) 0.0555(19) Uani 1 1 d . . . . .
C38 C -0.0149(6) 0.6001(3) 0.2120(4) 0.0467(15) Uani 1 1 d . . . . .
C39 C 0.4967(6) 0.6638(4) -0.1377(4) 0.0489(15) Uani 1 1 d . . . . .
C40 C 0.1842(5) 0.6092(4) -0.3354(4) 0.0511(16) Uani 1 1 d . . . . .
C41 C 0.4116(5) 0.6572(3) 0.1320(4) 0.0422(14) Uani 1 1 d . . . . .
H41A H 0.4754 0.6482 0.1038 0.051 Uiso 1 1 calc R U . . .
H41B H 0.3881 0.6176 0.1544 0.051 Uiso 1 1 calc R U . . .
C42 C 0.2659(6) 0.5365(4) -0.2465(4) 0.0527(17) Uani 1 1 d . . . . .
H42 H 0.2829 0.4947 -0.2326 0.063 Uiso 1 1 calc R U . . .
C43 C 0.1277(6) 0.6201(4) -0.4057(4) 0.0573(19) Uani 1 1 d . . . . .
C44 C 0.2125(6) 0.5477(4) -0.3130(4) 0.0529(17) Uani 1 1 d . . . . .
H44 H 0.1952 0.5133 -0.3435 0.064 Uiso 1 1 calc R U . . .
C45 C 0.4512(5) 0.7933(3) 0.2521(3) 0.0430(14) Uani 1 1 d . . . . .
C46 C -0.1248(6) 0.8596(5) 0.0084(4) 0.063(2) Uani 1 1 d . . . . .
C47 C -0.0351(6) 0.8991(4) -0.0043(4) 0.0546(18) Uani 1 1 d . . . . .
C49 C 0.2639(6) 0.6487(4) -0.2215(4) 0.0549(17) Uani 1 1 d . . . . .
C51 C 0.6055(7) 0.7582(4) -0.1146(4) 0.063(2) Uani 1 1 d . . . . .
H51 H 0.6252 0.7935 -0.0860 0.075 Uiso 1 1 calc R U . . .
C53 C 0.4445(8) 0.8559(4) 0.2772(4) 0.059(2) Uani 1 1 d . . . . .
C54 C 0.5461(7) 0.6516(4) -0.2042(4) 0.062(2) Uani 1 1 d . . . . .
C57 C 0.3569(7) 0.5744(3) -0.1298(4) 0.0548(17) Uani 1 1 d . . . . .
H57A H 0.3070 0.5598 -0.0932 0.066 Uiso 1 1 calc R U . . .
H57B H 0.4084 0.5402 -0.1381 0.066 Uiso 1 1 calc R U . . .
C59 C 0.4925(8) 0.8685(5) 0.3453(5) 0.067(2) Uani 1 1 d . . . . .
C60 C 0.6549(8) 0.7451(5) -0.1800(5) 0.080(3) Uani 1 1 d . . . . .
N1 N 0.3244(4) 0.6823(2) 0.0831(3) 0.0371(11) Uani 1 1 d . . . . .
N2 N 0.4972(5) 0.6907(2) 0.2527(3) 0.0441(13) Uani 1 1 d . . . . .
N6 N 0.1760(4) 0.7836(2) 0.0626(3) 0.0360(10) Uani 1 1 d . . . . .
N9 N 0.4095(4) 0.7659(2) 0.1876(3) 0.0375(11) Uani 1 1 d . . . . .
N13 N 0.0321(4) 0.7208(3) 0.0805(3) 0.0423(12) Uani 1 1 d . . . . .
N14 N 0.4157(5) 0.6310(3) -0.1017(3) 0.0486(13) Uani 1 1 d . . . . .
N26 N 0.4622(4) 0.7149(3) -0.0315(3) 0.0435(12) Uani 1 1 d . . . . .
O1 O 0.1166(4) 0.4822(2) 0.4071(2) 0.0478(10) Uani 1 1 d . . . . .
O2 O 0.2143(4) 0.3988(2) 0.3711(3) 0.0467(11) Uani 1 1 d . . . . .
O3 O -0.2059(4) 0.6576(2) 0.4254(2) 0.0471(10) Uani 1 1 d . . . . .
O4 O -0.0864(4) 0.5792(2) 0.4344(2) 0.0543(12) Uani 1 1 d . . . . .
O5 O 0.1095(4) 0.5740(3) -0.4485(3) 0.0663(14) Uani 1 1 d . . . . .
O8 O 0.0970(5) 0.6765(3) -0.4221(4) 0.0748(17) Uani 1 1 d . . . . .
Eu2 Eu 0.0000 0.5000 0.5000 0.03067(14) Uani 1 2 d S . P . .
Pb1 Pb 0.12776(2) 0.31163(2) 0.44359(2) 0.03105(11) Uani 1 1 d . . . . .
O6 O 0.5000 0.5000 0.0000 0.186(8) Uiso 1 2 d S . P . .
O10 O 0.6718(13) 0.5774(6) 0.1193(9) 0.188(6) Uani 1 1 d . . . . .
O0AA O -0.3336(6) 0.7017(4) 0.0783(5) 0.093(2) Uani 1 1 d G . . . .
H0AA H -0.2762 0.6969 0.0542 0.140 Uiso 1 1 d G U . . .
H0AB H -0.3382 0.7404 0.0925 0.140 Uiso 1 1 d G U . . .
C11 C 0.2502(12) 0.3974(8) 0.0570(8) 0.132(6) Uani 1 1 d . . . . .
H11A H 0.2194 0.3860 0.0098 0.198 Uiso 1 1 calc R U . . .
H11B H 0.2311 0.3655 0.0925 0.198 Uiso 1 1 calc R U . . .
H11C H 0.3279 0.3996 0.0543 0.198 Uiso 1 1 calc R U . . .
C16 C 0.2569(15) 0.4839(7) 0.1441(8) 0.128(5) Uani 1 1 d . . . . .
H16A H 0.3316 0.4945 0.1366 0.193 Uiso 1 1 calc R U . . .
H16B H 0.2526 0.4534 0.1834 0.193 Uiso 1 1 calc R U . . .
H16C H 0.2178 0.5220 0.1566 0.193 Uiso 1 1 calc R U . . .
C18 C 0.1466(12) 0.4928(7) 0.0229(9) 0.113(4) Uiso 1 1 d . . . . .
H18 H 0.1349 0.4784 -0.0249 0.136 Uiso 1 1 calc R U . . .
N7 N 0.2101(11) 0.4567(5) 0.0781(7) 0.127(4) Uani 1 1 d . . . . .
O7 O 0.1105(8) 0.5430(5) 0.0447(7) 0.134(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C1 C4 1.399(10) . ?
C1 C45 1.398(10) . ?
C1 N2 1.384(9) . ?
C2 C3 1.500(8) . ?
C2 C9 1.368(9) . ?
C2 C10 1.380(9) . ?
C3 O3 1.240(8) . ?
C3 O4 1.261(8) . ?
C4 C13 1.357(12) . ?
C5 C54 1.364(13) . ?
C5 C60 1.390(13) . ?
C6 C42 1.405(10) . ?
C6 C49 1.382(11) . ?
C6 C57 1.495(11) . ?
C7 C23 1.491(9) . ?
C7 N1 1.491(8) . ?
C8 C15 1.372(10) . ?
C8 C20 1.518(9) . ?
C8 C34 1.395(9) . ?
C9 C38 1.394(9) . ?
C10 C37 1.376(10) . ?
C12 C28 1.413(9) . ?
C12 C36 1.395(10) . ?
C12 N6 1.375(9) . ?
C13 C59 1.387(13) . ?
C14 C40 1.394(10) . ?
C14 C49 1.381(11) . ?
C15 C17 1.388(10) . ?
C17 C24 1.376(9) . ?
C19 C31 1.487(10) . ?
C19 N14 1.366(8) . ?
C19 N26 1.315(9) . ?
C20 N2 1.460(8) . ?
C22 C24 1.499(8) . ?
C22 O1 1.260(8) . ?
C22 O2 1.255(8) . ?
C23 N6 1.329(8) . ?
C23 N13 1.367(8) . ?
C24 C32 1.402(9) . ?
C25 C27 1.509(8) . ?
C25 C37 1.384(11) . ?
C25 C38 1.377(10) . ?
C27 N13 1.465(9) . ?
C28 C33 1.395(10) . ?
C28 N13 1.387(9) . ?
C29 C39 1.387(10) . ?
C29 C51 1.400(11) . ?
C29 N26 1.381(9) . ?
C31 N1 1.489(8) . ?
C32 C34 1.383(9) . ?
C33 C46 1.378(13) . ?
C35 C41 1.494(9) . ?
C35 N2 1.361(8) . ?
C35 N9 1.316(8) . ?
C36 C47 1.395(10) . ?
C39 C54 1.395(10) . ?
C39 N14 1.390(9) . ?
C40 C43 1.457(11) . ?
C40 C44 1.388(11) . ?
C41 N1 1.471(8) . ?
C42 C44 1.381(11) . ?
C43 O5 1.255(10) . ?
C43 O8 1.269(11) . ?
C45 C53 1.388(11) . ?
C45 N9 1.391(8) . ?
C46 C47 1.403(12) . ?
C51 C60 1.382(12) . ?
C53 C59 1.385(12) . ?
C57 N14 1.471(9) . ?
N6 Pb1 2.492(4) 2 ?
N9 Pb1 2.603(5) 2 ?
O1 Eu2 2.282(4) . ?
O2 Pb1 2.505(4) . ?
O3 Pb1 2.628(4) 3_566 ?
O4 Eu2 2.283(5) . ?
O5 Eu2 2.238(5) 1_554 ?
Eu2 O1 2.282(4) 3_566 ?
Eu2 O4 2.283(5) 3_566 ?
Eu2 O5 2.238(5) 3_565 ?
Eu2 O5 2.238(5) 1_556 ?
Pb1 N6 2.492(4) 2_545 ?
Pb1 N9 2.603(5) 2_545 ?
Pb1 O3 2.628(4) 3_566 ?
C11 N7 1.392(17) . ?
C16 N7 1.435(18) . ?
C18 N7 1.47(2) . ?
C18 O7 1.207(16) . ?

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
C45 C1 C4 121.5(7) . . ?
N2 C1 C4 133.2(6) . . ?
N2 C1 C45 105.4(5) . . ?
C9 C2 C3 122.2(5) . . ?
C9 C2 C10 119.2(6) . . ?
C10 C2 C3 118.5(6) . . ?
O3 C3 C2 119.5(5) . . ?
O3 C3 O4 123.5(6) . . ?
O4 C3 C2 117.0(6) . . ?
C13 C4 C1 117.2(7) . . ?
C54 C5 C60 121.4(8) . . ?
C42 C6 C57 119.3(7) . . ?
C49 C6 C42 117.8(7) . . ?
C49 C6 C57 122.9(6) . . ?
C23 C7 N1 109.1(5) . . ?
C15 C8 C20 122.3(6) . . ?
C15 C8 C34 118.9(6) . . ?
C34 C8 C20 118.8(6) . . ?
C2 C9 C38 119.5(6) . . ?
C37 C10 C2 121.4(7) . . ?
C36 C12 C28 119.6(6) . . ?
N6 C12 C28 109.0(5) . . ?
N6 C12 C36 131.4(6) . . ?
C4 C13 C59 121.5(7) . . ?
C49 C14 C40 121.0(8) . . ?
C8 C15 C17 121.1(6) . . ?
C24 C17 C15 120.4(6) . . ?
N14 C19 C31 121.7(6) . . ?
N26 C19 C31 125.5(6) . . ?
N26 C19 N14 112.7(6) . . ?
N2 C20 C8 112.9(5) . . ?
O1 C22 C24 117.6(5) . . ?
O2 C22 C24 117.8(5) . . ?
O2 C22 O1 124.5(6) . . ?
N6 C23 C7 123.0(5) . . ?
N6 C23 N13 112.1(5) . . ?
N13 C23 C7 124.8(5) . . ?
C17 C24 C22 121.7(5) . . ?
C17 C24 C32 119.1(6) . . ?
C32 C24 C22 119.1(5) . . ?
C37 C25 C27 120.1(6) . . ?
C38 C25 C27 121.2(6) . . ?
C38 C25 C37 118.7(6) . . ?
N13 C27 C25 114.3(6) . . ?
C33 C28 C12 123.1(7) . . ?
N13 C28 C12 105.7(5) . . ?
N13 C28 C33 131.2(6) . . ?
C39 C29 C51 119.8(6) . . ?
N26 C29 C39 109.6(6) . . ?
N26 C29 C51 130.6(6) . . ?
C19 C31 N1 110.9(5) . . ?
C34 C32 C24 120.0(6) . . ?
C46 C33 C28 116.0(7) . . ?
C32 C34 C8 120.5(6) . . ?
N2 C35 C41 123.2(6) . . ?
N9 C35 C41 124.3(5) . . ?
N9 C35 N2 112.6(6) . . ?
C47 C36 C12 117.7(7) . . ?
C10 C37 C25 119.8(6) . . ?
C25 C38 C9 121.4(7) . . ?
C29 C39 C54 123.0(7) . . ?
C29 C39 N14 105.9(6) . . ?
N14 C39 C54 131.1(7) . . ?
C14 C40 C43 121.6(7) . . ?
C44 C40 C14 117.5(7) . . ?
C44 C40 C43 120.9(7) . . ?
N1 C41 C35 109.7(5) . . ?
C44 C42 C6 120.4(7) . . ?
O5 C43 C40 119.9(8) . . ?
O5 C43 O8 121.2(8) . . ?
O8 C43 C40 118.9(7) . . ?
C42 C44 C40 121.7(6) . . ?
C53 C45 C1 120.8(6) . . ?
C53 C45 N9 129.8(7) . . ?
N9 C45 C1 109.4(6) . . ?
C33 C46 C47 122.4(7) . . ?
C36 C47 C46 121.2(7) . . ?
C14 C49 C6 121.5(7) . . ?
C60 C51 C29 116.7(7) . . ?
C59 C53 C45 116.5(8) . . ?
C5 C54 C39 116.6(8) . . ?
N14 C57 C6 112.6(6) . . ?
C53 C59 C13 122.4(8) . . ?
C51 C60 C5 122.5(8) . . ?
C31 N1 C7 106.9(5) . . ?
C41 N1 C7 110.5(5) . . ?
C41 N1 C31 111.6(5) . . ?
C1 N2 C20 126.2(6) . . ?
C35 N2 C1 107.1(5) . . ?
C35 N2 C20 126.5(6) . . ?
C12 N6 Pb1 131.2(4) . 2 ?
C23 N6 C12 106.4(5) . . ?
C23 N6 Pb1 122.3(4) . 2 ?
C35 N9 C45 105.5(5) . . ?
C35 N9 Pb1 115.2(4) . 2 ?
C45 N9 Pb1 132.6(4) . 2 ?
C23 N13 C27 126.7(6) . . ?
C23 N13 C28 106.8(5) . . ?
C28 N13 C27 126.3(5) . . ?
C19 N14 C39 106.1(5) . . ?
C19 N14 C57 128.2(6) . . ?
C39 N14 C57 125.7(6) . . ?
C19 N26 C29 105.7(5) . . ?
C22 O1 Eu2 154.2(4) . . ?
C22 O2 Pb1 125.8(4) . . ?
C3 O3 Pb1 105.4(4) . 3_566 ?
C3 O4 Eu2 178.5(5) . . ?
C43 O5 Eu2 152.2(5) . 1_554 ?
O1 Eu2 O1 180.0 3_566 . ?
O1 Eu2 O4 88.70(16) . 3_566 ?
O1 Eu2 O4 91.30(16) 3_566 3_566 ?
O1 Eu2 O4 91.30(16) . . ?
O1 Eu2 O4 88.70(16) 3_566 . ?
O4 Eu2 O4 180.0(2) 3_566 . ?
O5 Eu2 O1 87.76(19) 3_565 . ?
O5 Eu2 O1 87.76(19) 1_556 3_566 ?
O5 Eu2 O1 92.24(19) 3_565 3_566 ?
O5 Eu2 O1 92.24(19) 1_556 . ?
O5 Eu2 O4 89.2(2) 1_556 . ?
O5 Eu2 O4 89.2(2) 3_565 3_566 ?
O5 Eu2 O4 90.8(2) 1_556 3_566 ?
O5 Eu2 O4 90.8(2) 3_565 . ?
O5 Eu2 O5 180.0(2) 3_565 1_556 ?
N6 Pb1 N9 91.03(16) 2_545 2_545 ?
N6 Pb1 O2 73.62(16) 2_545 . ?
N6 Pb1 O3 76.63(15) 2_545 3_566 ?
N9 Pb1 O3 167.04(15) 2_545 3_566 ?
O2 Pb1 N9 81.22(15) . 2_545 ?
O2 Pb1 O3 98.73(15) . 3_566 ?
O7 C18 N7 114.5(15) . . ?
C11 N7 C16 116.5(13) . . ?
C11 N7 C18 117.1(12) . . ?
C16 N7 C18 124.4(12) . . ?

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_PbTb2L2
_database_code_depnum_ccdc_archive 'CCDC 1043822'
_audit_update_record             
;
2015-01-16 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_audit_creation_date             2013-07-04
_audit_creation_method           
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C96 H72 N16 O18 Pb Tb2, 4(C3 H7 N O), 6(O)'
_chemical_formula_sum            'C108 H100 N20 O28 Pb Tb2'
_chemical_formula_weight         2651.10
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7061(5)
_cell_length_b                   13.0527(4)
_cell_length_c                   17.9550(8)
_cell_angle_alpha                87.730(3)
_cell_angle_beta                 88.010(4)
_cell_angle_gamma                89.886(3)
_cell_volume                     2739.65(19)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    9.890
_exptl_absorpt_correction_T_max  0.372
_exptl_absorpt_correction_T_min  0.211
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.864
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14657
_diffrn_reflns_point_group_measured_fraction_full 0.864
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         62.557
_diffrn_reflns_theta_min         3.389
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.864
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7731
_reflns_number_total             8548
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_refine_diff_density_max         1.683
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         8548
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0410
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.076
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0608P)²+4.4657P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1119
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O4 \\sim N2 \\sim O5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
: with sigma of 0.1 and sigma for terminal atoms of 0.2
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C22(H22A,H22B), C29(H29A,H29B), C35(H35A,H35B)
3.b Aromatic/amide H refined with riding coordinates:
 C1F(H1F), C1G(H1G), C1I(H1I), C1J(H1J), C17(H17), C34(H34), C36(H36),
 C39(H39), C40(H40), C42(H42), C50(H50), C53(H53), C62(H62), C64(H64), C12(H12),
  C11(H11)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
C1 C -0.0788(5) 1.2823(4) 1.5141(3) 0.0299(12) Uani 1 1 d . . . . .
C1A C -0.2224(5) 1.4289(4) 1.8528(3) 0.0301(12) Uani 1 1 d . . . . .
C1B C -0.2528(5) 0.9752(4) 1.8438(3) 0.0312(12) Uani 1 1 d . . . . .
C1C C -0.1893(6) 1.3920(5) 1.4367(4) 0.0405(14) Uani 1 1 d . . . . .
C1D C 0.3985(5) 0.9038(4) 1.5461(3) 0.0274(11) Uani 1 1 d . . . . .
C1E C -0.3189(5) 1.0291(4) 1.7923(3) 0.0319(12) Uani 1 1 d . . . . .
C1F C -0.1244(6) 1.3202(5) 1.7677(4) 0.0464(17) Uani 1 1 d . . . . .
H1F H -0.1135 1.2552 1.7493 0.056 Uiso 1 1 calc R U . . .
C1G C -0.1551(6) 1.5087(5) 1.8256(4) 0.0471(17) Uani 1 1 d . . . . .
H1G H -0.1641 1.5731 1.8454 0.056 Uiso 1 1 calc R U . . .
C1I C -0.0742(6) 1.4944(5) 1.7691(4) 0.0474(17) Uani 1 1 d . . . . .
H1I H -0.0309 1.5500 1.7504 0.057 Uiso 1 1 calc R U . . .
C1J C -0.2084(6) 1.3345(5) 1.8224(4) 0.0423(15) Uani 1 1 d . . . . .
H1J H -0.2556 1.2802 1.8385 0.051 Uiso 1 1 calc R U . . .
C2 C 0.4152(5) 0.6605(4) 1.8242(3) 0.0307(12) Uani 1 1 d . . . . .
C3 C -0.1186(5) 1.4575(4) 1.5509(4) 0.0367(13) Uani 1 1 d . . . . .
C6 C 0.0292(4) 1.2269(4) 1.6029(3) 0.0246(11) Uani 1 1 d . . . . .
C7 C -0.1560(5) 0.9042(4) 1.8217(3) 0.0331(12) Uani 1 1 d . . . . .
H7A H -0.0844 0.9331 1.8366 0.040 Uiso 1 1 calc R U . . .
H7B H -0.1665 0.8388 1.8486 0.040 Uiso 1 1 calc R U . . .
C10 C -0.4025(5) 1.0969(4) 1.8166(3) 0.0321(12) Uani 1 1 d . . . . .
C13 C 0.4213(5) 0.9329(4) 1.6833(3) 0.0306(12) Uani 1 1 d . . . . .
C14 C 0.4195(5) 0.5664(4) 1.8744(3) 0.0274(11) Uani 1 1 d . . . . .
C15 C -0.1397(6) 1.2972(5) 1.4500(4) 0.0378(14) Uani 1 1 d . . . . .
C16 C 0.3091(5) 0.9194(4) 1.4977(3) 0.0262(11) Uani 1 1 d . . . . .
C17 C -0.3569(6) 1.0555(5) 1.9433(3) 0.0397(14) Uani 1 1 d . . . . .
H17 H -0.3699 1.0639 1.9941 0.048 Uiso 1 1 calc R U . . .
C18 C 0.2449(4) 0.9619(4) 1.6063(3) 0.0243(10) Uani 1 1 d . . . . .
C19 C -0.3152(5) 1.4461(4) 1.9118(3) 0.0303(12) Uani 1 1 d . . . . .
C21 C -0.0892(4) 0.9420(4) 1.6873(3) 0.0256(11) Uani 1 1 d . . . . .
C22 C 0.1101(5) 1.1597(4) 1.6457(3) 0.0287(11) Uani 1 1 d . . . . .
H22A H 0.1858 1.1645 1.6222 0.034 Uiso 1 1 calc R U . . .
H22B H 0.1146 1.1834 1.6961 0.034 Uiso 1 1 calc R U . . .
C23 C -0.4212(5) 1.1115(4) 1.8923(3) 0.0321(12) Uani 1 1 d . . . . .
C24 C -0.0566(5) 1.3998(4) 1.7399(3) 0.0311(12) Uani 1 1 d . . . . .
C25 C -0.1730(5) 0.8224(4) 1.6304(3) 0.0299(12) Uani 1 1 d . . . . .
C26 C 0.3826(5) 0.6543(5) 1.7513(3) 0.0334(12) Uani 1 1 d . . . . .
C27 C 0.3244(6) 0.8960(5) 1.4232(3) 0.0356(13) Uani 1 1 d . . . . .
C28 C -0.1789(5) 1.4705(5) 1.4868(4) 0.0406(15) Uani 1 1 d . . . . .
C29 C 0.1667(5) 0.9845(4) 1.6711(3) 0.0278(11) Uani 1 1 d . . . . .
H29A H 0.1356 0.9208 1.6927 0.033 Uiso 1 1 calc R U . . .
H29B H 0.2097 1.0169 1.7089 0.033 Uiso 1 1 calc R U . . .
C30 C -0.5014(5) 1.1931(4) 1.9184(3) 0.0335(13) Uani 1 1 d . . . . .
C31 C -0.2045(5) 0.8097(4) 1.7061(3) 0.0306(12) Uani 1 1 d . . . . .
C32 C 0.5042(5) 0.8640(4) 1.5236(4) 0.0352(13) Uani 1 1 d . . . . .
C33 C -0.0676(5) 1.3627(4) 1.5633(3) 0.0294(12) Uani 1 1 d . . . . .
C34 C -0.2747(6) 0.9883(5) 1.9198(3) 0.0425(15) Uani 1 1 d . . . . .
H34 H -0.2330 0.9510 1.9547 0.051 Uiso 1 1 calc R U . . .
C35 C 0.0383(5) 1.3848(4) 1.6816(3) 0.0326(12) Uani 1 1 d . . . . .
H35A H 0.0646 1.4514 1.6623 0.039 Uiso 1 1 calc R U . . .
H35B H 0.1021 1.3504 1.7050 0.039 Uiso 1 1 calc R U . . .
C36 C 0.4281(6) 0.8562(5) 1.4003(4) 0.0419(15) Uani 1 1 d . . . . .
H36 H 0.4394 0.8390 1.3508 0.050 Uiso 1 1 calc R U . . .
C37 C 0.3822(6) 0.7422(4) 1.7048(3) 0.0342(13) Uani 1 1 d . . . . .
C39 C 0.4435(8) 0.7539(5) 1.8504(4) 0.054(2) Uani 1 1 d . . . . .
H39 H 0.4646 0.7588 1.8996 0.065 Uiso 1 1 calc R U . . .
C40 C 0.5168(5) 0.8410(5) 1.4496(4) 0.0415(15) Uani 1 1 d . . . . .
H40 H 0.5861 0.8148 1.4320 0.050 Uiso 1 1 calc R U . . .
C41 C 0.4125(5) 0.8362(4) 1.7314(3) 0.0288(11) Uani 1 1 d . . . . .
C42 C -0.2156(5) 0.7567(4) 1.5796(4) 0.0361(13) Uani 1 1 d . . . . .
H42 H -0.1953 0.7634 1.5291 0.043 Uiso 1 1 calc R U . . .
C45 C -0.0246(6) 1.0378(5) 1.7020(3) 0.0314(13) Uani 1 1 d . . . . .
C50 C -0.2781(6) 0.7331(5) 1.7339(4) 0.0438(15) Uani 1 1 d . . . . .
H50 H -0.2979 0.7251 1.7844 0.053 Uiso 1 1 calc R U . . .
C53 C 0.4409(8) 0.8408(5) 1.8041(4) 0.0518(19) Uani 1 1 d . . . . .
H53 H 0.4590 0.9039 1.8229 0.062 Uiso 1 1 calc R U . . .
C62 C -0.3197(6) 0.6702(5) 1.6821(4) 0.0485(17) Uani 1 1 d . . . . .
H62 H -0.3702 0.6183 1.6981 0.058 Uiso 1 1 calc R U . . .
C64 C -0.2898(5) 0.6805(5) 1.6069(4) 0.0426(15) Uani 1 1 d . . . . .
H64 H -0.3202 0.6354 1.5741 0.051 Uiso 1 1 calc R U . . .
N1H N -0.1483(4) 0.8869(3) 1.7420(3) 0.0295(10) Uani 1 1 d . . . . .
N2 N -0.2062(17) 1.7166(14) 1.9957(10) 0.165(6) Uiso 1 1 d . U . . .
N4 N 0.3567(4) 0.9327(3) 1.6149(2) 0.0257(9) Uani 1 1 d . . . . .
N5 N 0.2138(4) 0.9567(3) 1.5368(2) 0.0259(9) Uani 1 1 d . . . . .
N8 N -0.0170(4) 1.1975(3) 1.5407(3) 0.0296(10) Uani 1 1 d . . . . .
N9 N 0.0018(4) 1.3244(3) 1.6193(2) 0.0269(9) Uani 1 1 d . . . . .
N11 N -0.1006(4) 0.9064(3) 1.6205(2) 0.0282(10) Uani 1 1 d . . . . .
N12 N 0.0721(4) 1.0524(3) 1.6486(2) 0.0242(9) Uani 1 1 d . . . . .
O1 O 0.3763(4) 0.4836(3) 1.8556(2) 0.0364(9) Uani 1 1 d . . . . .
O2 O -0.2231(4) 1.6630(4) 2.0627(3) 0.0526(12) Uani 1 1 d . . . . .
O3 O 0.4665(3) 0.5721(3) 1.9366(2) 0.0303(8) Uani 1 1 d . . . . .
O4 O -0.2987(6) 1.7275(4) 1.9386(3) 0.0743(18) Uani 1 1 d . U . . .
O5 O -0.1122(18) 1.7602(15) 1.9976(11) 0.224(7) Uiso 1 1 d . U . . .
O6 O -0.4023(3) 1.3907(3) 1.9097(2) 0.0326(9) Uani 1 1 d . . . . .
O7 O -0.4994(5) 1.2152(3) 1.9859(2) 0.0468(12) Uani 1 1 d . . . . .
O8 O -0.2982(4) 1.5151(3) 1.9571(2) 0.0377(9) Uani 1 1 d . . . . .
O9 O -0.5650(4) 1.2405(3) 1.8736(2) 0.0361(9) Uani 1 1 d . . . . .
Tb2 Tb -0.41291(3) 1.61869(2) 2.03264(2) 0.02461(11) Uani 1 1 d . . . . .
Pb1 Pb 0.0000 1.0000 1.5000 0.02085(10) Uani 1 2 d S . P . .
C8 C 0.1087(15) 0.5862(12) 1.9209(9) 0.132(5) Uiso 1 1 d . . . . .
H8A H 0.1805 0.5517 1.9268 0.198 Uiso 1 1 calc R U . . .
H8B H 0.0710 0.5598 1.8791 0.198 Uiso 1 1 calc R U . . .
H8C H 0.0615 0.5750 1.9653 0.198 Uiso 1 1 calc R U . . .
C9 C 0.1647(19) 0.7678(16) 1.9688(11) 0.169(8) Uiso 1 1 d . . . . .
H9A H 0.1413 0.7400 2.0172 0.254 Uiso 1 1 calc R U . . .
H9B H 0.1291 0.8333 1.9604 0.254 Uiso 1 1 calc R U . . .
H9C H 0.2463 0.7757 1.9662 0.254 Uiso 1 1 calc R U . . .
C12 C 0.1030(10) 0.7326(9) 1.8395(6) 0.086(3) Uiso 1 1 d . . . . .
H12 H 0.0731 0.6889 1.8054 0.103 Uiso 1 1 calc R U . . .
N10 N 0.1283(9) 0.6938(8) 1.9083(6) 0.094(3) Uiso 1 1 d . . . . .
O11 O 0.1182(10) 0.8245(8) 1.8200(6) 0.130(3) Uiso 1 1 d . . . . .
C4 C 0.5533(8) 1.3842(6) 1.7196(4) 0.060(2) Uani 1 1 d . . . . .
H4A H 0.6233 1.3545 1.7012 0.090 Uiso 1 1 calc R U . . .
H4B H 0.5243 1.3440 1.7621 0.090 Uiso 1 1 calc R U . . .
H4C H 0.5673 1.4530 1.7340 0.090 Uiso 1 1 calc R U . . .
C5 C 0.5036(7) 1.4306(7) 1.5894(4) 0.062(2) Uani 1 1 d . . . . .
H5A H 0.4966 1.5038 1.5902 0.093 Uiso 1 1 calc R U . . .
H5B H 0.4546 1.4050 1.5526 0.093 Uiso 1 1 calc R U . . .
H5C H 0.5814 1.4126 1.5772 0.093 Uiso 1 1 calc R U . . .
C11 C 0.3670(7) 1.3473(5) 1.6739(4) 0.0515(18) Uani 1 1 d . . . . .
H11 H 0.3484 1.3216 1.7218 0.062 Uiso 1 1 calc R U . . .
N1 N 0.4707(5) 1.3858(4) 1.6620(3) 0.0448(13) Uani 1 1 d . . . . .
O10 O 0.2924(4) 1.3425(4) 1.6269(4) 0.0626(14) Uani 1 1 d . . . . .
O12 O -0.7090(7) 1.1211(6) 1.7968(4) 0.097(2) Uani 1 1 d . . . . .
H45A H 0.011(6) 1.039(5) 1.755(4) 0.038(17) Uiso 1 1 d . . . . .
H27 H 0.267(6) 0.908(4) 1.396(4) 0.024(15) Uiso 1 1 d . . . . .
H1C H -0.225(5) 1.406(4) 1.387(3) 0.021(13) Uiso 1 1 d . . . . .
H10 H -0.450(5) 1.139(4) 1.779(3) 0.023(14) Uiso 1 1 d . . . . .
H1E H -0.311(6) 1.013(5) 1.738(4) 0.040(17) Uiso 1 1 d . . . . .
H45B H -0.062(5) 1.077(5) 1.701(3) 0.011(16) Uiso 1 1 d . . . . .
H37 H 0.354(7) 0.747(6) 1.663(5) 0.05(2) Uiso 1 1 d . . . . .
H15 H -0.144(5) 1.252(5) 1.416(4) 0.030(16) Uiso 1 1 d . . . . .
H26 H 0.357(5) 0.592(5) 1.736(3) 0.025(14) Uiso 1 1 d . . . . .
H32 H 0.564(6) 0.856(5) 1.554(4) 0.035(17) Uiso 1 1 d . . . . .
H3 H -0.103(6) 1.512(5) 1.593(4) 0.036(16) Uiso 1 1 d . . . . .
H13A H 0.398(6) 0.990(5) 1.710(4) 0.034(17) Uiso 1 1 d . . . . .
H28 H -0.209(5) 1.530(5) 1.473(3) 0.028(15) Uiso 1 1 d . . . . .
H13B H 0.499(7) 0.944(5) 1.665(4) 0.044(18) Uiso 1 1 d . . . . .
O15 O 0.1271(14) 1.0042(12) 1.8845(9) 0.190(6) Uiso 1 1 d . . . . .
O13 O 0.136(2) 1.2484(17) 1.8285(12) 0.259(9) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
C1 C15 1.383(9) . ?
C1 C33 1.407(8) . ?
C1 N8 1.398(7) . ?
C1A C1G 1.370(9) . ?
C1A C1J 1.376(8) . ?
C1A C19 1.514(8) . ?
C1B C1E 1.394(9) . ?
C1B C7 1.516(8) . ?
C1B C34 1.396(8) . ?
C1C C15 1.382(9) . ?
C1C C28 1.399(10) . ?
C1D C16 1.393(8) . ?
C1D C32 1.394(8) . ?
C1D N4 1.379(7) . ?
C1E C10 1.389(8) . ?
C1F C1J 1.382(9) . ?
C1F C24 1.376(9) . ?
C1G C1I 1.382(9) . ?
C1I C24 1.373(8) . ?
C2 C14 1.496(8) . ?
C2 C26 1.383(8) . ?
C2 C39 1.369(9) . ?
C3 C28 1.375(10) . ?
C3 C33 1.386(8) . ?
C6 C22 1.500(8) . ?
C6 N8 1.328(7) . ?
C6 N9 1.353(7) . ?
C7 N1H 1.458(7) . ?
C10 C23 1.389(8) . ?
C13 C41 1.502(8) . ?
C13 N4 1.465(7) . ?
C14 O1 1.257(7) . ?
C14 O3 1.267(7) . ?
C14 Tb2 2.881(5) 2_579 ?
C16 C27 1.390(8) . ?
C16 N5 1.395(7) . ?
C17 C23 1.391(9) . ?
C17 C34 1.368(9) . ?
C18 C29 1.494(8) . ?
C18 N4 1.375(7) . ?
C18 N5 1.315(7) . ?
C19 O6 1.253(7) . ?
C19 O8 1.257(7) . ?
C21 C45 1.500(8) . ?
C21 N1H 1.363(7) . ?
C21 N11 1.315(7) . ?
C22 N12 1.469(7) . ?
C23 C30 1.498(8) . ?
C24 C35 1.518(8) . ?
C25 C31 1.400(8) . ?
C25 C42 1.383(8) . ?
C25 N11 1.389(7) . ?
C26 C37 1.391(8) . ?
C27 C36 1.376(9) . ?
C29 N12 1.475(7) . ?
C30 O7 1.257(7) . ?
C30 O9 1.259(8) . ?
C30 Tb2 2.813(6) 2_489 ?
C31 C50 1.388(9) . ?
C31 N1H 1.396(8) . ?
C32 C40 1.377(10) . ?
C33 N9 1.392(8) . ?
C35 N9 1.469(7) . ?
C36 C40 1.395(10) . ?
C37 C41 1.385(8) . ?
C39 C53 1.381(9) . ?
C41 C53 1.361(9) . ?
C42 C64 1.385(9) . ?
C45 N12 1.466(8) . ?
C50 C62 1.367(10) . ?
C62 C64 1.385(11) . ?
N2 O2 1.377(19) . ?
N2 O4 1.52(2) . ?
N2 O5 1.24(2) . ?
N2 Tb2 2.79(2) . ?
N5 Pb1 2.665(4) . ?
N8 Pb1 2.713(4) . ?
N11 Pb1 2.679(4) . ?
O1 Tb2 2.416(4) 2_579 ?
O2 Tb2 2.383(5) . ?
O3 Tb2 2.364(4) 1_645 ?
O3 Tb2 2.603(4) 2_579 ?
O4 Tb2 2.513(5) . ?
O6 Tb2 2.367(4) 2_489 ?
O7 Tb2 2.413(4) 2_489 ?
O8 Tb2 2.342(4) . ?
O9 Tb2 2.549(4) 2_489 ?
Tb2 C14 2.881(5) 2_579 ?
Tb2 C30 2.813(6) 2_489 ?
Tb2 O1 2.415(4) 2_579 ?
Tb2 O3 2.603(4) 2_579 ?
Tb2 O3 2.364(4) 1_465 ?
Tb2 O6 2.367(4) 2_489 ?
Tb2 O7 2.413(4) 2_489 ?
Tb2 O9 2.549(4) 2_489 ?
Pb1 N5 2.665(4) 2_578 ?
Pb1 N8 2.713(4) 2_578 ?
Pb1 N11 2.679(4) 2_578 ?
C8 N10 1.431(17) . ?
C9 N10 1.55(2) . ?
C12 N10 1.359(14) . ?
C12 O11 1.248(14) . ?
C4 N1 1.440(10) . ?
C5 N1 1.448(9) . ?
C11 N1 1.321(10) . ?
C11 O10 1.239(10) . ?

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
C15 C1 C33 120.1(5) . . ?
C15 C1 N8 130.9(5) . . ?
N8 C1 C33 108.9(5) . . ?
C1G C1A C1J 118.7(5) . . ?
C1G C1A C19 120.6(5) . . ?
C1J C1A C19 120.6(5) . . ?
C1E C1B C7 123.3(5) . . ?
C1E C1B C34 118.9(5) . . ?
C34 C1B C7 117.7(5) . . ?
C15 C1C C28 121.1(6) . . ?
C16 C1D C32 122.9(5) . . ?
N4 C1D C16 105.7(5) . . ?
N4 C1D C32 131.4(5) . . ?
C10 C1E C1B 120.2(5) . . ?
C24 C1F C1J 121.6(6) . . ?
C1A C1G C1I 120.7(5) . . ?
C24 C1I C1G 121.2(6) . . ?
C1A C1J C1F 120.0(5) . . ?
C26 C2 C14 120.6(5) . . ?
C39 C2 C14 120.1(5) . . ?
C39 C2 C26 119.3(5) . . ?
C28 C3 C33 116.7(6) . . ?
N8 C6 C22 122.1(5) . . ?
N8 C6 N9 112.9(5) . . ?
N9 C6 C22 124.9(5) . . ?
N1H C7 C1B 113.4(5) . . ?
C1E C10 C23 120.4(6) . . ?
N4 C13 C41 115.1(5) . . ?
C2 C14 Tb2 176.1(4) . 2_579 ?
O1 C14 C2 120.7(5) . . ?
O1 C14 O3 120.6(5) . . ?
O1 C14 Tb2 56.0(3) . 2_579 ?
O3 C14 C2 118.6(5) . . ?
O3 C14 Tb2 64.6(3) . 2_579 ?
C1C C15 C1 118.0(6) . . ?
C1D C16 N5 109.6(5) . . ?
C27 C16 C1D 119.7(5) . . ?
C27 C16 N5 130.7(5) . . ?
C34 C17 C23 120.8(5) . . ?
N4 C18 C29 122.3(4) . . ?
N5 C18 C29 125.1(5) . . ?
N5 C18 N4 112.2(5) . . ?
O6 C19 C1A 116.2(5) . . ?
O6 C19 O8 126.7(5) . . ?
O8 C19 C1A 117.1(5) . . ?
N1H C21 C45 122.7(5) . . ?
N11 C21 C45 123.8(5) . . ?
N11 C21 N1H 113.4(5) . . ?
N12 C22 C6 111.0(4) . . ?
C10 C23 C17 119.1(5) . . ?
C10 C23 C30 120.6(5) . . ?
C17 C23 C30 120.1(5) . . ?
C1F C24 C35 122.3(5) . . ?
C1I C24 C1F 117.7(5) . . ?
C1I C24 C35 120.0(5) . . ?
C42 C25 C31 119.9(5) . . ?
C42 C25 N11 131.0(5) . . ?
N11 C25 C31 109.1(5) . . ?
C2 C26 C37 119.8(6) . . ?
C36 C27 C16 118.0(6) . . ?
C3 C28 C1C 121.9(6) . . ?
N12 C29 C18 111.5(4) . . ?
C23 C30 Tb2 161.9(4) . 2_489 ?
O7 C30 C23 117.6(6) . . ?
O7 C30 O9 121.5(5) . . ?
O7 C30 Tb2 58.7(3) . 2_489 ?
O9 C30 C23 120.9(5) . . ?
O9 C30 Tb2 64.9(3) . 2_489 ?
C50 C31 C25 123.1(6) . . ?
C50 C31 N1H 131.0(6) . . ?
N1H C31 C25 105.9(5) . . ?
C40 C32 C1D 116.2(6) . . ?
C3 C33 C1 122.1(6) . . ?
C3 C33 N9 132.3(5) . . ?
N9 C33 C1 105.6(5) . . ?
C17 C34 C1B 120.6(6) . . ?
N9 C35 C24 112.8(5) . . ?
C27 C36 C40 121.6(6) . . ?
C41 C37 C26 120.5(5) . . ?
C2 C39 C53 120.3(6) . . ?
C32 C40 C36 121.6(6) . . ?
C37 C41 C13 123.5(5) . . ?
C53 C41 C13 117.9(5) . . ?
C53 C41 C37 118.5(5) . . ?
C25 C42 C64 117.3(6) . . ?
N12 C45 C21 110.9(5) . . ?
C62 C50 C31 115.6(6) . . ?
C41 C53 C39 121.5(6) . . ?
C50 C62 C64 122.7(6) . . ?
C62 C64 C42 121.4(6) . . ?
C21 N1H C7 128.5(5) . . ?
C21 N1H C31 105.9(4) . . ?
C31 N1H C7 125.6(5) . . ?
O2 N2 O4 122.4(14) . . ?
O2 N2 Tb2 58.8(7) . . ?
O4 N2 Tb2 63.7(7) . . ?
O5 N2 O2 107.2(18) . . ?
O5 N2 O4 129.9(19) . . ?
O5 N2 Tb2 164.7(17) . . ?
C1D N4 C13 125.7(5) . . ?
C18 N4 C1D 107.0(4) . . ?
C18 N4 C13 127.3(5) . . ?
C16 N5 Pb1 133.7(3) . . ?
C18 N5 C16 105.5(4) . . ?
C18 N5 Pb1 120.7(3) . . ?
C1 N8 Pb1 133.5(4) . . ?
C6 N8 C1 105.5(4) . . ?
C6 N8 Pb1 120.6(3) . . ?
C6 N9 C33 107.2(4) . . ?
C6 N9 C35 129.1(5) . . ?
C33 N9 C35 123.7(5) . . ?
C21 N11 C25 105.6(4) . . ?
C21 N11 Pb1 121.0(3) . . ?
C25 N11 Pb1 133.3(4) . . ?
C22 N12 C29 110.0(4) . . ?
C45 N12 C22 110.5(4) . . ?
C45 N12 C29 109.2(4) . . ?
C14 O1 Tb2 98.4(3) . 2_579 ?
N2 O2 Tb2 91.6(9) . . ?
C14 O3 Tb2 89.3(3) . 2_579 ?
C14 O3 Tb2 163.2(4) . 1_645 ?
Tb2 O3 Tb2 105.30(13) 1_645 2_579 ?
N2 O4 Tb2 83.5(8) . . ?
C19 O6 Tb2 137.7(3) . 2_489 ?
C30 O7 Tb2 94.8(4) . 2_489 ?
C19 O8 Tb2 135.9(4) . . ?
C30 O9 Tb2 88.5(3) . 2_489 ?
C30 Tb2 C14 122.62(15) 2_489 2_579 ?
N2 Tb2 C14 120.7(4) . 2_579 ?
N2 Tb2 C30 88.4(4) . 2_489 ?
O1 Tb2 C14 25.57(15) 2_579 2_579 ?
O1 Tb2 C30 105.81(15) 2_579 2_489 ?
O1 Tb2 N2 104.7(4) 2_579 . ?
O1 Tb2 O3 51.66(12) 2_579 2_579 ?
O1 Tb2 O4 137.1(2) 2_579 . ?
O1 Tb2 O9 81.79(13) 2_579 2_489 ?
O2 Tb2 C14 94.70(17) . 2_579 ?
O2 Tb2 C30 91.74(18) . 2_489 ?
O2 Tb2 N2 29.6(4) . . ?
O2 Tb2 O1 75.52(17) . 2_579 ?
O2 Tb2 O3 114.35(15) . 2_579 ?
O2 Tb2 O4 62.4(2) . . ?
O2 Tb2 O7 102.10(18) . 2_489 ?
O2 Tb2 O9 74.64(15) . 2_489 ?
O3 Tb2 C14 100.54(14) 1_465 2_579 ?
O3 Tb2 C14 26.10(14) 2_579 2_579 ?
O3 Tb2 C30 105.43(16) 1_465 2_489 ?
O3 Tb2 C30 133.86(14) 2_579 2_489 ?
O3 Tb2 N2 132.8(4) 2_579 . ?
O3 Tb2 N2 119.5(4) 1_465 . ?
O3 Tb2 O1 125.66(13) 1_465 2_579 ?
O3 Tb2 O2 145.39(16) 1_465 . ?
O3 Tb2 O3 74.70(13) 1_465 2_579 ?
O3 Tb2 O4 89.00(19) 1_465 . ?
O3 Tb2 O6 75.42(14) 1_465 2_489 ?
O3 Tb2 O7 83.59(15) 1_465 2_489 ?
O3 Tb2 O9 130.25(13) 1_465 2_489 ?
O4 Tb2 C14 146.27(18) . 2_579 ?
O4 Tb2 C30 84.71(17) . 2_489 ?
O4 Tb2 N2 32.8(4) . . ?
O4 Tb2 O3 140.61(15) . 2_579 ?
O4 Tb2 O9 94.57(17) . 2_489 ?
O6 Tb2 C14 73.24(15) 2_489 2_579 ?
O6 Tb2 C30 65.48(15) 2_489 2_489 ?
O6 Tb2 N2 153.3(4) 2_489 . ?
O6 Tb2 O1 78.71(15) 2_489 2_579 ?
O6 Tb2 O2 139.07(16) 2_489 . ?
O6 Tb2 O3 70.31(13) 2_489 2_579 ?
O6 Tb2 O4 140.34(18) 2_489 . ?
O6 Tb2 O7 72.89(15) 2_489 2_489 ?
O6 Tb2 O9 70.62(13) 2_489 2_489 ?
O7 Tb2 C14 143.55(15) 2_489 2_579 ?
O7 Tb2 C30 26.43(16) 2_489 2_489 ?
O7 Tb2 N2 86.3(4) 2_489 . ?
O7 Tb2 O1 131.77(13) 2_489 2_579 ?
O7 Tb2 O3 140.83(16) 2_489 2_579 ?
O7 Tb2 O4 69.22(18) 2_489 . ?
O7 Tb2 O9 52.42(14) 2_489 2_489 ?
O8 Tb2 C14 81.35(15) . 2_579 ?
O8 Tb2 C30 154.44(15) . 2_489 ?
O8 Tb2 N2 69.9(4) . . ?
O8 Tb2 O1 93.12(15) . 2_579 ?
O8 Tb2 O2 76.27(16) . . ?
O8 Tb2 O3 75.57(14) . 1_465 ?
O8 Tb2 O3 71.52(13) . 2_579 ?
O8 Tb2 O4 69.73(17) . . ?
O8 Tb2 O6 136.74(14) . 2_489 ?
O8 Tb2 O7 133.88(14) . 2_489 ?
O8 Tb2 O9 150.82(14) . 2_489 ?
O9 Tb2 C14 103.14(14) 2_489 2_579 ?
O9 Tb2 C30 26.58(16) 2_489 2_489 ?
O9 Tb2 N2 83.5(4) 2_489 . ?
O9 Tb2 O3 123.45(12) 2_489 2_579 ?
N5 Pb1 N5 180.00(6) . 2_578 ?
N5 Pb1 N8 100.74(14) . . ?
N5 Pb1 N8 79.26(14) 2_578 . ?
N5 Pb1 N8 79.26(14) . 2_578 ?
N5 Pb1 N8 100.74(14) 2_578 2_578 ?
N5 Pb1 N11 96.04(14) . . ?
N5 Pb1 N11 83.96(14) 2_578 . ?
N5 Pb1 N11 96.04(14) 2_578 2_578 ?
N5 Pb1 N11 83.96(14) . 2_578 ?
N8 Pb1 N8 180.0 . 2_578 ?
N11 Pb1 N8 99.50(13) 2_578 2_578 ?
N11 Pb1 N8 80.50(13) . 2_578 ?
N11 Pb1 N8 99.50(13) . . ?
N11 Pb1 N8 80.50(13) 2_578 . ?
N11 Pb1 N11 180.00(17) . 2_578 ?
O11 C12 N10 122.7(12) . . ?
C8 N10 C9 124.7(13) . . ?
C12 N10 C8 115.7(11) . . ?
C12 N10 C9 119.4(12) . . ?
O10 C11 N1 125.9(7) . . ?
C4 N1 C5 118.4(6) . . ?
C11 N1 C4 121.8(6) . . ?
C11 N1 C5 119.8(6) . . ?

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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.
;
_shelxl_version_number           2013-2

