# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1494103'
_audit_update_record             
;
2016-08-26 deposited with the CCDC.
2016-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H19 N18 O1.50 Pb2.50'
_chemical_formula_weight         1173.61

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'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   37.7785(11)
_cell_length_b                   7.4676(2)
_cell_length_c                   29.5720(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 128.268(3)
_cell_angle_gamma                90.00
_cell_volume                     6550.0(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6456
_cell_measurement_theta_min      4.6800
_cell_measurement_theta_max      70.3860

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4336
_exptl_absorpt_coefficient_mu    25.133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2384
_exptl_absorpt_correction_T_max  0.2721
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23455
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_sigmaI/netI    0.0758
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         67.23
_reflns_number_total             5852
_reflns_number_gt                4406
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2002)'
_computing_cell_refinement       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-II (Johnson, 1976)'
_computing_publication_material  SHELXL-97

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0332P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5852
_refine_ls_number_parameters     470
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0877
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.629277(14) 0.74138(5) 0.812415(18) 0.02997(12) Uani 1 1 d . . .
Pb2 Pb 0.531161(14) 0.72691(5) 0.645203(18) 0.03122(12) Uani 1 1 d . . .
Pb3 Pb 0.5000 0.97235(8) 0.7500 0.03300(16) Uani 1 2 d S . .
N1 N 0.5983(3) 0.7465(11) 0.8670(4) 0.035(2) Uani 1 1 d . . .
N2 N 0.5578(3) 0.8020(12) 0.8480(4) 0.038(2) Uani 1 1 d . . .
N3 N 0.5520(3) 0.7562(13) 0.8860(4) 0.044(2) Uani 1 1 d . . .
N4 N 0.5884(3) 0.6769(14) 0.9315(4) 0.049(3) Uani 1 1 d . . .
N5 N 0.6862(3) 0.6022(11) 0.9374(4) 0.035(2) Uani 1 1 d . . .
N6 N 0.5812(3) 0.1670(12) 0.8070(4) 0.040(2) Uani 1 1 d . . .
N7 N 0.5805(3) 0.3416(12) 0.8133(4) 0.040(2) Uani 1 1 d . . .
N8 N 0.6107(3) 0.4190(10) 0.8083(3) 0.030(2) Uani 1 1 d . . .
N9 N 0.6118(3) 0.1266(12) 0.7988(4) 0.038(2) Uani 1 1 d . . .
N10 N 0.6848(3) 0.4652(12) 0.8107(4) 0.037(2) Uani 1 1 d . . .
N11 N 0.5280(3) 1.0491(11) 0.6503(3) 0.032(2) Uani 1 1 d . . .
N12 N 0.5158(3) 1.1524(13) 0.6759(4) 0.042(2) Uani 1 1 d . . .
N13 N 0.5240(4) 1.3230(13) 0.6727(4) 0.050(3) Uani 1 1 d . . .
N14 N 0.5422(3) 1.3310(12) 0.6448(4) 0.047(3) Uani 1 1 d . . .
N15 N 0.5485(3) 0.9340(11) 0.5812(4) 0.035(2) Uani 1 1 d . . .
N16 N 0.6133(3) 0.7475(13) 0.7091(4) 0.050(3) Uani 1 1 d . . .
N17 N 0.6298(3) 0.6576(15) 0.6931(4) 0.046(3) Uani 1 1 d . . .
N18 N 0.6458(4) 0.5660(16) 0.6778(5) 0.069(4) Uani 1 1 d . . .
O1 O 0.5501(2) 0.7603(8) 0.7369(3) 0.0296(16) Uani 1 1 d . . .
O2 O 0.5000 0.5298(13) 0.7500 0.043(3) Uani 1 2 d S . .
H2C H 0.5255 0.4862 0.7774 0.052 Uiso 0.50 1 d PR . .
H2D H 0.4909 0.5972 0.7641 0.052 Uiso 0.50 1 d PR . .
C1 C 0.6171(4) 0.6709(13) 0.9186(5) 0.032(2) Uani 1 1 d . . .
C2 C 0.6619(4) 0.5950(13) 0.9558(4) 0.035(3) Uani 1 1 d . . .
C3 C 0.6789(4) 0.5229(16) 1.0102(5) 0.047(3) Uani 1 1 d . . .
H3 H 0.6609 0.5209 1.0216 0.056 Uiso 1 1 calc R . .
C4 C 0.7209(4) 0.4576(17) 1.0452(5) 0.054(3) Uani 1 1 d . . .
H4 H 0.7317 0.4073 1.0804 0.065 Uiso 1 1 calc R . .
C5 C 0.7491(4) 0.4654(15) 1.0285(5) 0.045(3) Uani 1 1 d . . .
C6 C 0.7298(4) 0.5409(14) 0.9728(4) 0.039(3) Uani 1 1 d . . .
C7 C 0.7562(4) 0.5526(15) 0.9546(5) 0.044(3) Uani 1 1 d . . .
H7 H 0.7439 0.6014 0.9187 0.053 Uiso 1 1 calc R . .
C8 C 0.7994(4) 0.4941(17) 0.9884(6) 0.059(4) Uani 1 1 d . . .
H8 H 0.8167 0.5027 0.9759 0.071 Uiso 1 1 calc R . .
C9 C 0.8179(5) 0.4198(17) 1.0429(6) 0.069(4) Uani 1 1 d . . .
H9 H 0.8475 0.3783 1.0659 0.083 Uiso 1 1 calc R . .
C10 C 0.7937(4) 0.4077(18) 1.0624(5) 0.059(4) Uani 1 1 d . . .
H10 H 0.8070 0.3603 1.0988 0.070 Uiso 1 1 calc R . .
C11 C 0.6291(3) 0.2835(13) 0.7989(4) 0.031(2) Uani 1 1 d . . .
C12 C 0.6666(4) 0.3083(15) 0.7968(4) 0.036(3) Uani 1 1 d . . .
C13 C 0.6818(4) 0.1557(16) 0.7846(5) 0.048(3) Uani 1 1 d . . .
H13 H 0.6662 0.0476 0.7725 0.057 Uiso 1 1 calc R . .
C14 C 0.7205(5) 0.1787(18) 0.7919(6) 0.060(4) Uani 1 1 d . . .
H14 H 0.7328 0.0815 0.7863 0.072 Uiso 1 1 calc R . .
C15 C 0.7430(4) 0.344(2) 0.8078(5) 0.053(4) Uani 1 1 d . . .
C16 C 0.7224(4) 0.4891(17) 0.8143(5) 0.045(3) Uani 1 1 d . . .
C17 C 0.7435(4) 0.6559(18) 0.8282(5) 0.054(3) Uani 1 1 d . . .
H17 H 0.7300 0.7536 0.8316 0.065 Uiso 1 1 calc R . .
C18 C 0.7832(4) 0.681(2) 0.8371(6) 0.075(5) Uani 1 1 d . . .
H18 H 0.7961 0.7943 0.8467 0.090 Uiso 1 1 calc R . .
C19 C 0.8045(5) 0.543(3) 0.8323(7) 0.096(7) Uani 1 1 d . . .
H19 H 0.8316 0.5605 0.8386 0.115 Uiso 1 1 calc R . .
C20 C 0.7846(5) 0.376(3) 0.8179(7) 0.081(5) Uani 1 1 d . . .
H20 H 0.7988 0.2813 0.8147 0.097 Uiso 1 1 calc R . .
C21 C 0.5431(4) 1.1616(14) 0.6315(5) 0.034(3) Uani 1 1 d . . .
C22 C 0.5567(4) 1.1031(15) 0.5968(5) 0.038(3) Uani 1 1 d . . .
C23 C 0.5762(4) 1.2215(15) 0.5812(5) 0.049(3) Uani 1 1 d . . .
H23 H 0.5826 1.3389 0.5946 0.059 Uiso 1 1 calc R . .
C24 C 0.5855(4) 1.1631(17) 0.5465(6) 0.056(4) Uani 1 1 d . . .
H24 H 0.5983 1.2407 0.5357 0.068 Uiso 1 1 calc R . .
C25 C 0.5759(4) 0.9845(17) 0.5264(5) 0.045(3) Uani 1 1 d . . .
C26 C 0.5579(4) 0.8698(16) 0.5462(5) 0.040(3) Uani 1 1 d . . .
C27 C 0.5481(4) 0.6962(16) 0.5274(5) 0.050(3) Uani 1 1 d . . .
H27 H 0.5359 0.6215 0.5397 0.060 Uiso 1 1 calc R . .
C28 C 0.5558(4) 0.6288(18) 0.4907(5) 0.055(4) Uani 1 1 d . . .
H28 H 0.5487 0.5108 0.4781 0.066 Uiso 1 1 calc R . .
C29 C 0.5749(5) 0.743(2) 0.4727(6) 0.065(4) Uani 1 1 d . . .
H29 H 0.5812 0.6975 0.4492 0.078 Uiso 1 1 calc R . .
C30 C 0.5841(4) 0.916(2) 0.4887(5) 0.059(4) Uani 1 1 d . . .
H30 H 0.5957 0.9892 0.4753 0.071 Uiso 1 1 calc R . .


_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 O1 2.383(7) . ?
Pb1 N8 2.489(8) . ?
Pb1 N1 2.515(8) . ?
Pb1 N16 2.722(10) . ?
Pb2 O1 2.350(6) . ?
Pb2 N11 2.418(8) . ?
Pb2 N16 2.440(10) . ?
Pb2 N3 2.679(9) 2_656 ?
Pb3 N2 2.636(9) 2_656 ?
Pb3 N2 2.636(9) . ?
Pb3 O1 2.674(6) . ?
Pb3 O1 2.674(6) 2_656 ?
N1 N2 1.326(11) . ?
N1 C1 1.344(12) . ?
N2 N3 1.317(11) . ?
N3 N4 1.326(12) . ?
N3 Pb2 2.679(9) 2_656 ?
N4 C1 1.354(12) . ?
N5 C2 1.329(12) . ?
N5 C6 1.370(12) . ?
N6 N7 1.320(11) . ?
N6 N9 1.353(11) . ?
N7 N8 1.368(10) . ?
N8 C11 1.350(11) . ?
N9 C11 1.342(12) . ?
N10 C12 1.291(13) . ?
N10 C16 1.369(12) . ?
N11 C21 1.318(12) . ?
N11 N12 1.348(10) . ?
N12 N13 1.328(13) . ?
N13 N14 1.367(11) . ?
N14 C21 1.331(13) . ?
N15 C22 1.314(13) . ?
N15 C26 1.374(12) . ?
N16 N17 1.197(12) . ?
N17 N18 1.172(12) . ?
C1 C2 1.444(14) . ?
C2 C3 1.417(13) . ?
C3 C4 1.339(15) . ?
C4 C5 1.424(15) . ?
C5 C10 1.393(15) . ?
C5 C6 1.442(14) . ?
C6 C7 1.401(13) . ?
C7 C8 1.352(15) . ?
C8 C9 1.413(17) . ?
C9 C10 1.354(16) . ?
C11 C12 1.465(13) . ?
C12 C13 1.419(14) . ?
C13 C14 1.349(16) . ?
C14 C15 1.407(17) . ?
C15 C16 1.411(15) . ?
C15 C20 1.426(17) . ?
C16 C17 1.396(16) . ?
C17 C18 1.364(15) . ?
C18 C19 1.37(2) . ?
C19 C20 1.37(2) . ?
C21 C22 1.469(13) . ?
C22 C23 1.398(14) . ?
C23 C24 1.348(15) . ?
C24 C25 1.413(16) . ?
C25 C26 1.424(15) . ?
C25 C30 1.427(14) . ?
C26 C27 1.368(15) . ?
C27 C28 1.382(14) . ?
C28 C29 1.416(17) . ?
C29 C30 1.339(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 N8 81.9(2) . . ?
O1 Pb1 N1 77.7(2) . . ?
N8 Pb1 N1 79.5(3) . . ?
O1 Pb1 N16 70.7(3) . . ?
N8 Pb1 N16 95.8(3) . . ?
N1 Pb1 N16 148.4(3) . . ?
O1 Pb2 N11 79.3(2) . . ?
O1 Pb2 N16 76.5(3) . . ?
N11 Pb2 N16 88.7(3) . . ?
O1 Pb2 N3 81.0(3) . 2_656 ?
N11 Pb2 N3 81.2(3) . 2_656 ?
N16 Pb2 N3 156.7(3) . 2_656 ?
N2 Pb3 N2 122.3(4) 2_656 . ?
N2 Pb3 O1 74.6(2) 2_656 . ?
N2 Pb3 O1 72.2(2) . . ?
N2 Pb3 O1 72.2(2) 2_656 2_656 ?
N2 Pb3 O1 74.6(2) . 2_656 ?
O1 Pb3 O1 107.4(3) . 2_656 ?
N2 N1 C1 105.9(8) . . ?
N2 N1 Pb1 127.2(6) . . ?
C1 N1 Pb1 126.3(7) . . ?
N3 N2 N1 108.3(9) . . ?
N3 N2 Pb3 126.9(7) . . ?
N1 N2 Pb3 124.7(6) . . ?
N2 N3 N4 111.3(9) . . ?
N2 N3 Pb2 120.5(7) . 2_656 ?
N4 N3 Pb2 124.9(7) . 2_656 ?
N3 N4 C1 103.8(9) . . ?
C2 N5 C6 118.9(9) . . ?
N7 N6 N9 110.0(8) . . ?
N6 N7 N8 108.0(8) . . ?
C11 N8 N7 106.0(8) . . ?
C11 N8 Pb1 124.7(7) . . ?
N7 N8 Pb1 129.2(6) . . ?
C11 N9 N6 105.9(8) . . ?
C12 N10 C16 117.9(10) . . ?
C21 N11 N12 105.2(9) . . ?
C21 N11 Pb2 123.8(7) . . ?
N12 N11 Pb2 130.7(7) . . ?
N13 N12 N11 109.4(8) . . ?
N12 N13 N14 108.2(8) . . ?
C21 N14 N13 104.6(9) . . ?
C22 N15 C26 119.0(10) . . ?
N17 N16 Pb2 112.4(8) . . ?
N17 N16 Pb1 128.9(8) . . ?
Pb2 N16 Pb1 99.2(3) . . ?
N18 N17 N16 178.4(13) . . ?
Pb2 O1 Pb1 112.6(2) . . ?
Pb2 O1 Pb3 119.5(2) . . ?
Pb1 O1 Pb3 119.3(2) . . ?
N1 C1 N4 110.6(10) . . ?
N1 C1 C2 125.3(9) . . ?
N4 C1 C2 124.2(10) . . ?
N5 C2 C3 122.5(10) . . ?
N5 C2 C1 116.9(9) . . ?
C3 C2 C1 120.6(10) . . ?
C4 C3 C2 120.2(11) . . ?
C3 C4 C5 119.9(11) . . ?
C10 C5 C4 124.7(12) . . ?
C10 C5 C6 118.3(11) . . ?
C4 C5 C6 117.0(11) . . ?
N5 C6 C7 119.5(10) . . ?
N5 C6 C5 121.4(10) . . ?
C7 C6 C5 119.1(10) . . ?
C8 C7 C6 121.2(11) . . ?
C7 C8 C9 119.2(12) . . ?
C10 C9 C8 121.6(13) . . ?
C9 C10 C5 120.6(13) . . ?
N9 C11 N8 110.0(9) . . ?
N9 C11 C12 126.3(10) . . ?
N8 C11 C12 123.2(9) . . ?
N10 C12 C13 126.0(11) . . ?
N10 C12 C11 116.1(9) . . ?
C13 C12 C11 117.6(11) . . ?
C14 C13 C12 115.2(12) . . ?
C13 C14 C15 122.4(12) . . ?
C14 C15 C16 116.7(11) . . ?
C14 C15 C20 125.2(14) . . ?
C16 C15 C20 118.0(14) . . ?
N10 C16 C17 121.0(11) . . ?
N10 C16 C15 121.4(12) . . ?
C17 C16 C15 117.5(11) . . ?
C18 C17 C16 122.4(14) . . ?
C17 C18 C19 121.5(16) . . ?
C20 C19 C18 117.9(15) . . ?
C19 C20 C15 122.5(15) . . ?
N11 C21 N14 112.6(9) . . ?
N11 C21 C22 122.4(9) . . ?
N14 C21 C22 124.9(10) . . ?
N15 C22 C23 123.4(10) . . ?
N15 C22 C21 114.9(10) . . ?
C23 C22 C21 121.7(10) . . ?
C24 C23 C22 119.0(12) . . ?
C23 C24 C25 120.3(11) . . ?
C24 C25 C26 117.3(11) . . ?
C24 C25 C30 123.0(12) . . ?
C26 C25 C30 119.6(12) . . ?
C27 C26 N15 120.3(11) . . ?
C27 C26 C25 118.8(11) . . ?
N15 C26 C25 120.8(11) . . ?
C26 C27 C28 121.9(12) . . ?
C27 C28 C29 118.6(13) . . ?
C30 C29 C28 122.0(12) . . ?
C29 C30 C25 119.1(13) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        67.23
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.631
_refine_diff_density_min         -1.680
_refine_diff_density_rms         0.205
####################################################################### 
# 
# 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_r-3_sq
_database_code_depnum_ccdc_archive 'CCDC 1494104'
_audit_update_record             
;
2016-09-09 deposited with the CCDC.
2016-09-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H18 N17.89 O2 Pb2'
_chemical_formula_weight         1027.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0192 0.0096 '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'
Pb Pb -4.0816 8.6988 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0330 0.0189 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0517 0.0336 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   33.2975(17)
_cell_length_b                   33.2975(17)
_cell_length_c                   9.6334(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9249.9(11)
_cell_formula_units_Z            9
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3157
_cell_measurement_theta_min      4.5970
_cell_measurement_theta_max      62.0070

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_F_000             4313
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    15.392
_shelx_estimated_absorpt_T_min   0.372
_shelx_estimated_absorpt_T_max   0.412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3588
_exptl_absorpt_correction_T_max  0.3983
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19919
_diffrn_reflns_av_unetI/netI     0.1194
_diffrn_reflns_av_R_equivalents  0.1729
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.654
_diffrn_reflns_theta_max         72.672
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4022
_reflns_number_gt                2386
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1160P)²+533.3143P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4022
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0834
_refine_ls_wR_factor_ref         0.2604
_refine_ls_wR_factor_gt          0.2108
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_restrained_S_all      0.967
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.59858(2) 0.61885(3) 0.33369(9) 0.0555(3) Uani 1 1 d . . . . .
N1 N 0.5216(6) 0.5462(5) 0.227(2) 0.067(5) Uani 0.9444 1 d . . P . .
N2 N 0.5703(5) 0.5353(6) 0.4422(19) 0.062(4) Uani 1 1 d . . . . .
N3 N 0.6430(5) 0.6149(5) 0.5495(17) 0.054(4) Uani 1 1 d . . . . .
N4 N 0.6750(5) 0.6443(5) 0.635(2) 0.061(4) Uani 1 1 d . . . . .
N5 N 0.6825(6) 0.6203(5) 0.732(2) 0.062(4) Uani 1 1 d . . . . .
N6 N 0.6566(6) 0.5755(6) 0.712(2) 0.065(5) Uani 1 1 d . . . . .
N7 N 0.6407(6) 0.5902(6) 0.206(2) 0.068(5) Uani 1 1 d . . . . .
N8 N 0.6313(6) 0.5506(7) 0.202(2) 0.067(5) Uani 1 1 d . . . . .
N9 N 0.6243(9) 0.5126(7) 0.201(3) 0.110(9) Uani 1 1 d . . . . .
C1 C 0.4964(8) 0.5522(8) 0.130(3) 0.079(7) Uani 1 1 d . . . . .
H1 H 0.5052 0.5821 0.1002 0.095 Uiso 1 1 calc R U . . .
C2 C 0.4569(8) 0.5146(9) 0.071(3) 0.087(8) Uani 1 1 d . . . . .
H2 H 0.4393 0.5200 0.0066 0.104 Uiso 1 1 calc R U . . .
C3 C 0.4442(8) 0.4709(10) 0.106(3) 0.089(8) Uani 1 1 d . . . . .
H3 H 0.4191 0.4463 0.0624 0.107 Uiso 1 1 calc R U . . .
C4 C 0.4694(7) 0.4621(8) 0.212(2) 0.077(7) Uani 1 1 d . . . . .
C5 C 0.5081(7) 0.5022(7) 0.271(3) 0.073(7) Uani 1 1 d . . . . .
C6 C 0.4576(8) 0.4178(8) 0.259(3) 0.095(9) Uani 1 1 d . . . . .
H6 H 0.4317 0.3919 0.2226 0.114 Uiso 1 1 calc R U . . .
C7 C 0.4849(7) 0.4123(6) 0.360(3) 0.082(8) Uani 1 1 d . . . . .
H7 H 0.4778 0.3826 0.3872 0.098 Uiso 1 1 calc R U . . .
C8 C 0.5236(7) 0.4518(7) 0.423(3) 0.071(6) Uani 1 1 d . . . . .
C9 C 0.5350(6) 0.4965(6) 0.381(3) 0.068(6) Uani 1 1 d . . . . .
C10 C 0.5962(7) 0.5293(7) 0.534(3) 0.069(6) Uani 1 1 d . . . . .
C11 C 0.5872(8) 0.4859(8) 0.584(3) 0.076(6) Uani 1 1 d . . . . .
H11 H 0.6053 0.4834 0.6532 0.091 Uiso 1 1 calc R U . . .
C12 C 0.5499(9) 0.4468(8) 0.525(3) 0.082(7) Uani 1 1 d . . . . .
H12 H 0.5428 0.4173 0.5538 0.098 Uiso 1 1 calc R U . . .
C13 C 0.6318(6) 0.5721(7) 0.594(2) 0.060(5) Uani 1 1 d . . . . .
O1 O 0.5187(12) 0.6552(11) 0.265(4) 0.221(17) Uani 1 1 d . . . . .
H1C H 0.5397 0.6626 0.2041 0.266 Uiso 1 1 d R U . . .
H1D H 0.5310 0.6712 0.3376 0.266 Uiso 1 1 d R U . . .


_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 N7 2.392(19) . ?
Pb1 N3 2.591(16) . ?
Pb1 N2 2.665(16) . ?
Pb1 N1 2.699(18) . ?
Pb1 N5 2.768(19) 6_564 ?
N1 C1 1.34(3) . ?
N1 C5 1.37(3) . ?
N2 C10 1.32(3) . ?
N2 C9 1.37(3) . ?
N3 N4 1.31(2) . ?
N3 C13 1.35(2) . ?
N4 N5 1.33(2) . ?
N5 N6 1.31(2) . ?
N5 Pb1 2.768(19) 8_655 ?
N6 C13 1.38(3) . ?
N7 N8 1.20(2) . ?
N8 N9 1.16(3) . ?
C1 C2 1.40(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.34(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.44(4) . ?
C3 H3 0.9300 . ?
C4 C6 1.40(4) . ?
C4 C5 1.43(3) . ?
C5 C9 1.46(3) . ?
C6 C7 1.41(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.43(3) . ?
C7 H7 0.9300 . ?
C8 C12 1.38(3) . ?
C8 C9 1.40(3) . ?
C10 C11 1.41(3) . ?
C10 C13 1.44(3) . ?
C11 C12 1.40(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
O1 H1C 0.8501 . ?
O1 H1D 0.8499 . ?

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
N7 Pb1 N3 86.0(6) . . ?
N7 Pb1 N2 75.9(5) . . ?
N3 Pb1 N2 62.9(5) . . ?
N7 Pb1 N1 85.9(6) . . ?
N3 Pb1 N1 124.8(6) . . ?
N2 Pb1 N1 62.1(6) . . ?
N7 Pb1 N5 74.3(5) . 6_564 ?
N3 Pb1 N5 146.8(5) . 6_564 ?
N2 Pb1 N5 133.5(5) . 6_564 ?
N1 Pb1 N5 80.9(6) . 6_564 ?
C1 N1 C5 119(2) . . ?
C1 N1 Pb1 121.2(14) . . ?
C5 N1 Pb1 119.9(16) . . ?
C10 N2 C9 117.8(18) . . ?
C10 N2 Pb1 120.3(13) . . ?
C9 N2 Pb1 120.2(14) . . ?
N4 N3 C13 106.4(16) . . ?
N4 N3 Pb1 137.3(12) . . ?
C13 N3 Pb1 116.3(12) . . ?
N3 N4 N5 108.5(14) . . ?
N6 N5 N4 111.6(17) . . ?
N6 N5 Pb1 114.9(13) . 8_655 ?
N4 N5 Pb1 128.8(12) . 8_655 ?
N5 N6 C13 103.7(17) . . ?
N8 N7 Pb1 125.1(14) . . ?
N9 N8 N7 177(2) . . ?
N1 C1 C2 122(2) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C3 C2 C1 121(3) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C2 C3 C4 120(2) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C6 C4 C5 120(3) . . ?
C6 C4 C3 124(2) . . ?
C5 C4 C3 116(2) . . ?
N1 C5 C4 123(3) . . ?
N1 C5 C9 118.0(19) . . ?
C4 C5 C9 119(2) . . ?
C4 C6 C7 120(2) . . ?
C4 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C8 121(2) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C12 C8 C9 119(2) . . ?
C12 C8 C7 121(2) . . ?
C9 C8 C7 120(2) . . ?
N2 C9 C8 122(2) . . ?
N2 C9 C5 118.9(18) . . ?
C8 C9 C5 119(2) . . ?
N2 C10 C11 124(2) . . ?
N2 C10 C13 113(2) . . ?
C11 C10 C13 122(2) . . ?
C12 C11 C10 117(2) . . ?
C12 C11 H11 121.6 . . ?
C10 C11 H11 121.6 . . ?
C8 C12 C11 120(2) . . ?
C8 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
N3 C13 N6 109.8(17) . . ?
N3 C13 C10 125(2) . . ?
N6 C13 C10 124.9(19) . . ?
H1C O1 H1D 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 N3 N4 N5 -2(2) . . . . ?
Pb1 N3 N4 N5 177.5(13) . . . . ?
N3 N4 N5 N6 1(2) . . . . ?
N3 N4 N5 Pb1 -153.3(12) . . . 8_655 ?
N4 N5 N6 C13 0(2) . . . . ?
Pb1 N5 N6 C13 158.5(12) 8_655 . . . ?
C5 N1 C1 C2 -1(4) . . . . ?
Pb1 N1 C1 C2 178.5(17) . . . . ?
N1 C1 C2 C3 -3(4) . . . . ?
C1 C2 C3 C4 4(4) . . . . ?
C2 C3 C4 C6 178(2) . . . . ?
C2 C3 C4 C5 -1(3) . . . . ?
C1 N1 C5 C4 3(3) . . . . ?
Pb1 N1 C5 C4 -176.0(15) . . . . ?
C1 N1 C5 C9 -178(2) . . . . ?
Pb1 N1 C5 C9 3(2) . . . . ?
C6 C4 C5 N1 179(2) . . . . ?
C3 C4 C5 N1 -2(3) . . . . ?
C6 C4 C5 C9 -1(3) . . . . ?
C3 C4 C5 C9 179(2) . . . . ?
C5 C4 C6 C7 -2(4) . . . . ?
C3 C4 C6 C7 178(2) . . . . ?
C4 C6 C7 C8 3(4) . . . . ?
C6 C7 C8 C12 179(2) . . . . ?
C6 C7 C8 C9 -1(4) . . . . ?
C10 N2 C9 C8 6(3) . . . . ?
Pb1 N2 C9 C8 170.9(15) . . . . ?
C10 N2 C9 C5 -175.3(19) . . . . ?
Pb1 N2 C9 C5 -10(2) . . . . ?
C12 C8 C9 N2 -3(3) . . . . ?
C7 C8 C9 N2 177(2) . . . . ?
C12 C8 C9 C5 178(2) . . . . ?
C7 C8 C9 C5 -2(3) . . . . ?
N1 C5 C9 N2 5(3) . . . . ?
C4 C5 C9 N2 -176.2(18) . . . . ?
N1 C5 C9 C8 -176.5(19) . . . . ?
C4 C5 C9 C8 3(3) . . . . ?
C9 N2 C10 C11 -6(3) . . . . ?
Pb1 N2 C10 C11 -171.5(16) . . . . ?
C9 N2 C10 C13 -179.1(18) . . . . ?
Pb1 N2 C10 C13 16(2) . . . . ?
N2 C10 C11 C12 4(3) . . . . ?
C13 C10 C11 C12 176(2) . . . . ?
C9 C8 C12 C11 0(4) . . . . ?
C7 C8 C12 C11 -180(2) . . . . ?
C10 C11 C12 C8 0(4) . . . . ?
N4 N3 C13 N6 2(2) . . . . ?
Pb1 N3 C13 N6 -177.4(12) . . . . ?
N4 N3 C13 C10 176.7(19) . . . . ?
Pb1 N3 C13 C10 -3(3) . . . . ?
N5 N6 C13 N3 -2(2) . . . . ?
N5 N6 C13 C10 -176.1(18) . . . . ?
N2 C10 C13 N3 -9(3) . . . . ?
C11 C10 C13 N3 178(2) . . . . ?
N2 C10 C13 N6 165.0(19) . . . . ?
C11 C10 C13 N6 -8(3) . . . . ?

_refine_diff_density_max         2.975
_refine_diff_density_min         -2.100
_refine_diff_density_rms         0.274

_shelxl_version_number           2014/6




