# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1838399'
_audit_update_record             
;
2018-09-20 deposited with the CCDC.
2018-09-24 downloaded from the CCDC.
;
_audit_creation_date             2018-09-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.06(C48 H32 N8 O20 Pb8)'
_chemical_formula_sum            'C12 H8 N2 O5 Pb2'
_chemical_formula_weight         674.60
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   22.4281(7)
_cell_length_b                   22.4281(7)
_cell_length_c                   11.1579(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5612.6(5)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    7180
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      3.28
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.987
_exptl_absorpt_correction_T_max  0.017
_exptl_absorpt_correction_T_min  0.008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.193
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6448
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15127
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.317
_diffrn_reflns_theta_min         3.280
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2971
_reflns_number_total             3487
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         3.324
_refine_diff_density_min         -3.217
_refine_diff_density_rms         0.326
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3487
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0387
_refine_ls_restrained_S_all      1.031
_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)+(0.0511P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0930
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C14(H14), C12(H12), C11(H11), C3(H3), C4(H4), C7(H7), C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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 0.24605(2) 0.41864(2) 0.01898(2) 0.01247(10) Uani 1 1 d . . . . .
Pb2 Pb 0.18921(2) 0.55552(2) 0.11219(2) 0.01253(10) Uani 1 1 d . . . . .
O1 O 0.1047(3) 0.4841(4) 0.1191(6) 0.0379(18) Uani 1 1 d . . . . .
O2 O 0.1372(3) 0.4214(3) -0.0225(6) 0.0271(14) Uani 1 1 d . . . . .
O3 O 0.2219(3) 0.3943(3) -0.2145(5) 0.0297(16) Uani 1 1 d . . . . .
O4 O 0.2383(2) 0.4776(2) 0.1880(4) 0.0111(11) Uani 1 1 d . . . . .
O5 O 0.2971(3) 0.6061(3) 0.0913(5) 0.0239(14) Uani 1 1 d . . . . .
C8 C 0.2974(4) 0.6314(4) 0.1902(7) 0.0173(16) Uani 1 1 d . . . . .
C9 C 0.3185(4) 0.6941(4) 0.1988(7) 0.0159(16) Uani 1 1 d . . . . .
C1 C 0.0979(4) 0.4425(4) 0.0455(8) 0.0221(18) Uani 1 1 d . . . . .
N2 N 0.3510(4) 0.7755(4) 0.3227(8) 0.044(2) Uani 1 1 d . . . . .
C10 C 0.3269(4) 0.7277(4) 0.0960(7) 0.0238(19) Uani 1 1 d . . . . .
H10 H 0.318329 0.711640 0.019142 0.029 Uiso 1 1 calc R . . . .
C14 C 0.3299(4) 0.7196(4) 0.3102(8) 0.027(2) Uani 1 1 d . . . . .
H14 H 0.322364 0.696723 0.380194 0.033 Uiso 1 1 calc R . . . .
C12 C 0.3593(6) 0.8060(5) 0.2227(10) 0.042(3) Uani 1 1 d . U . . .
H12 H 0.374220 0.845493 0.230698 0.051 Uiso 1 1 calc R . . . .
C11 C 0.3484(5) 0.7861(4) 0.1086(9) 0.034(2) Uani 1 1 d . . . . .
H11 H 0.355199 0.810859 0.040796 0.041 Uiso 1 1 calc R . . . .
C2 C 0.0365(4) 0.4146(4) 0.0357(7) 0.0188(17) Uani 1 1 d . . . . .
C3 C 0.0286(4) 0.3616(4) -0.0261(8) 0.026(2) Uani 1 1 d . . . . .
H3 H 0.061099 0.342279 -0.064303 0.031 Uiso 1 1 calc R . . . .
C4 C -0.0288(4) 0.3375(5) -0.0304(9) 0.032(2) Uani 1 1 d . . . . .
H4 H -0.035978 0.301246 -0.071768 0.038 Uiso 1 1 calc R . . . .
C7 C -0.0131(5) 0.4404(5) 0.0911(8) 0.030(2) Uani 1 1 d . . . . .
H7 H -0.007417 0.476163 0.135213 0.036 Uiso 1 1 calc R . . . .
N1 N -0.0680(4) 0.4174(4) 0.0852(8) 0.0331(19) Uani 1 1 d . . . . .
C5 C -0.0738(4) 0.3663(4) 0.0248(8) 0.029(2) Uani 1 1 d . . . . .
H5 H -0.112402 0.349011 0.020464 0.035 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 O2 2.485(6) . ?
Pb1 O3 2.740(6) 3 ?
Pb1 O3 2.716(6) . ?
Pb1 O4 2.311(4) . ?
Pb1 O4 2.313(5) 4_454 ?
Pb2 O1 2.482(7) . ?
Pb2 O4 2.231(5) . ?
Pb2 O4 2.342(4) 4_454 ?
Pb2 O5 2.683(6) . ?
Pb2 O5 2.757(6) 3 ?
O1 C1 1.252(11) . ?
O2 C1 1.256(10) . ?
O3 C8 1.285(10) 2_564 ?
O5 C8 1.240(9) . ?
C8 C9 1.487(11) . ?
C9 C10 1.385(11) . ?
C9 C14 1.392(11) . ?
C1 C2 1.519(12) . ?
N2 C14 1.347(11) . ?
N2 C12 1.323(13) . ?
C10 C11 1.404(13) . ?
C12 C11 1.371(14) . ?
C2 C3 1.385(12) . ?
C2 C7 1.396(12) . ?
C3 C4 1.395(12) . ?
C4 C5 1.347(13) . ?
C7 N1 1.339(12) . ?
N1 C5 1.335(13) . ?

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
O2 Pb1 O3 152.0(2) . 3 ?
O2 Pb1 O3 68.3(2) . . ?
O3 Pb1 O3 109.3(2) . 3 ?
O4 Pb1 O2 93.6(2) . . ?
O4 Pb1 O2 74.27(19) 4_454 . ?
O4 Pb1 O3 78.03(19) 4_454 3 ?
O4 Pb1 O3 152.00(18) . . ?
O4 Pb1 O3 76.77(17) 4_454 . ?
O4 Pb1 O3 76.30(18) . 3 ?
O4 Pb1 O4 77.77(12) . 4_454 ?
O1 Pb2 O5 164.6(2) . . ?
O1 Pb2 O5 69.3(2) . 3 ?
O4 Pb2 O1 81.9(2) . . ?
O4 Pb2 O1 92.1(2) 4_454 . ?
O4 Pb2 O4 78.76(13) . 4_454 ?
O4 Pb2 O5 151.21(17) 4_454 3 ?
O4 Pb2 O5 76.88(17) 4_454 . ?
O4 Pb2 O5 85.35(19) . . ?
O4 Pb2 O5 77.08(17) . 3 ?
O5 Pb2 O5 116.2(2) . 3 ?
C1 O1 Pb2 123.5(6) . . ?
C1 O2 Pb1 125.9(6) . . ?
Pb1 O3 Pb1 88.34(18) . 4_454 ?
C8 O3 Pb1 101.5(5) 2_564 4_454 ?
C8 O3 Pb1 162.0(5) 2_564 . ?
Pb1 O4 Pb1 110.66(19) . 3 ?
Pb1 O4 Pb2 96.90(16) 3 3 ?
Pb1 O4 Pb2 119.9(2) . 3 ?
Pb2 O4 Pb1 100.14(17) . . ?
Pb2 O4 Pb1 117.0(2) . 3 ?
Pb2 O4 Pb2 113.3(2) . 3 ?
Pb2 O5 Pb2 89.23(17) . 4_454 ?
C8 O5 Pb2 96.9(5) . . ?
C8 O5 Pb2 173.0(5) . 4_454 ?
O3 C8 C9 118.6(7) 2_565 . ?
O5 C8 O3 121.9(8) . 2_565 ?
O5 C8 C9 119.5(7) . . ?
C10 C9 C8 120.3(7) . . ?
C10 C9 C14 119.4(8) . . ?
C14 C9 C8 120.3(7) . . ?
O1 C1 O2 126.4(8) . . ?
O1 C1 C2 117.7(8) . . ?
O2 C1 C2 116.0(8) . . ?
C12 N2 C14 116.3(8) . . ?
C9 C10 C11 118.2(8) . . ?
N2 C14 C9 122.7(9) . . ?
N2 C12 C11 126.1(10) . . ?
C12 C11 C10 117.2(9) . . ?
C3 C2 C1 120.4(8) . . ?
C3 C2 C7 118.3(8) . . ?
C7 C2 C1 121.3(8) . . ?
C2 C3 C4 117.8(9) . . ?
C5 C4 C3 119.3(9) . . ?
N1 C7 C2 123.5(10) . . ?
C5 N1 C7 116.4(8) . . ?
N1 C5 C4 124.7(8) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
