# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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. 
# 
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data_1
_audit_block_doi                 10.5517/ccdc.csd.cc216y5d
_database_code_depnum_ccdc_archive 'CCDC 1883503'
_audit_update_record             
;
2018-12-06 deposited with the CCDC.
2019-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H14 N20 O11 Pb2'
_chemical_formula_sum            'C4 H14 N20 O11 Pb2'
_chemical_formula_weight         932.73

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'
'-x, -y, -z'

_cell_length_a                   6.5991(6)
_cell_length_b                   10.8137(10)
_cell_length_c                   15.2509(12)
_cell_angle_alpha                84.753(3)
_cell_angle_beta                 81.706(3)
_cell_angle_gamma                74.843(3)
_cell_volume                     1037.82(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1910
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      25.31

_exptl_crystal_description       sheet
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.985
_exptl_crystal_F_000             860
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    16.304
_shelx_estimated_absorpt_T_min   0.322
_shelx_estimated_absorpt_T_max   0.736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4957
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7852
_diffrn_reflns_av_unetI/netI     0.1282
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.224
_diffrn_reflns_theta_max         25.329
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             3721
_reflns_number_gt                2391
_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.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (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)+(0.0235P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3721
_refine_ls_number_parameters     367
_refine_ls_number_restraints     326
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.0974
_refine_ls_wR_factor_gt          0.0853
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      0.994
_refine_ls_shift/su_max          0.000
_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
C1 C 0.732(3) 0.6531(17) 0.4646(11) 0.024(4) Uani 1 1 d . . . . .
C2 C 0.738(3) 0.9665(16) 0.4994(10) 0.019(4) Uani 1 1 d . U . . .
C3 C 0.606(2) 1.1104(13) 0.0717(10) 0.019(4) Uani 1 1 d D U . . .
N1 N 0.7302(19) 0.7802(12) 0.4512(8) 0.016(3) Uani 1 1 d . U . . .
N2 N 0.725(2) 0.8395(14) 0.5207(9) 0.030(4) Uani 1 1 d . . . . .
N3 N 0.751(2) 0.5844(13) 0.3962(9) 0.017(3) Uani 1 1 d . . . . .
N4 N 0.765(2) 0.4596(14) 0.4262(9) 0.025(4) Uani 1 1 d . . . . .
N5 N 0.759(3) 0.4572(15) 0.5130(10) 0.036(4) Uani 1 1 d . . . . .
N6 N 0.740(2) 0.5746(13) 0.5400(8) 0.021(3) Uani 1 1 d . U . . .
N7 N 0.711(2) 1.0462(13) 0.5631(9) 0.020(3) Uani 1 1 d . . . . .
N8 N 0.744(2) 1.1595(13) 0.5238(10) 0.030(4) Uani 1 1 d . . . . .
N9 N 0.782(2) 1.1419(14) 0.4366(10) 0.033(4) Uani 1 1 d . . . . .
N10 N 0.782(2) 1.0240(13) 0.4190(9) 0.024(3) Uani 1 1 d . U . . .
N13 N 0.5048(19) 1.1748(12) 0.1446(8) 0.020(3) Uani 1 1 d D . . . .
N14 N 0.3929(19) 1.2902(12) 0.1160(9) 0.022(3) Uani 1 1 d D . . . .
N15 N 0.431(2) 1.2935(13) 0.0267(9) 0.030(4) Uani 1 1 d D . . . .
N16 N 0.555(2) 1.1844(13) -0.0008(9) 0.029(4) Uani 1 1 d D . . . .
O1 O 0.7477(17) 0.6182(10) 0.3119(6) 0.017(3) Uani 1 1 d . U . . .
O2 O 0.659(2) 1.0308(13) 0.6474(8) 0.039(4) Uani 1 1 d . . . . .
O3 O 0.5237(18) 1.1359(11) 0.2269(7) 0.027(3) Uani 1 1 d . . . . .
O5 O 1.1205(17) 0.7538(10) 0.3144(7) 0.024(3) Uani 1 1 d . . . . .
H5A H 1.2176 0.7698 0.2755 0.028 Uiso 1 1 d R U . . .
H5B H 1.1371 0.7783 0.3637 0.028 Uiso 1 1 d R U . . .
O6 O 0.4508(18) 0.8171(12) 0.1886(7) 0.031(3) Uani 1 1 d . . . . .
H6A H 0.4467 0.8545 0.1372 0.037 Uiso 1 1 d R U . . .
H6B H 0.4902 0.7367 0.1825 0.037 Uiso 1 1 d R U . . .
O7 O 1.0300(18) 1.0119(11) 0.2158(7) 0.027(3) Uani 1 1 d . . . . .
H7A H 1.1542 0.9828 0.2302 0.032 Uiso 1 1 d R U . . .
H7B H 1.0001 1.0817 0.1844 0.032 Uiso 1 1 d R U . . .
O8 O 1.2406(18) 0.5031(11) 0.2742(8) 0.029(3) Uani 1 1 d . . . . .
H8A H 1.2006 0.5818 0.2858 0.035 Uiso 1 1 d R U . . .
H8B H 1.2694 0.4567 0.3210 0.035 Uiso 1 1 d R U . . .
O9 O 0.6547(17) 0.3324(10) 0.2877(6) 0.022(3) Uani 1 1 d . U . . .
H9A H 0.6209 0.2875 0.2519 0.026 Uiso 1 1 d R U . . .
H9B H 0.7016 0.2831 0.3309 0.026 Uiso 1 1 d R U . . .
O10 O 0.5906(17) 0.5565(12) 0.1480(7) 0.030(3) Uani 1 1 d . . . . .
H10A H 0.4745 0.5530 0.1794 0.036 Uiso 1 1 d R U . . .
H10B H 0.5922 0.5983 0.0980 0.036 Uiso 1 1 d R U . . .
O11 O 1.1121(18) 0.2358(12) 0.3003(8) 0.039(4) Uani 1 1 d . . . . .
H11B H 1.1118 0.2555 0.3530 0.047 Uiso 1 1 d R U . . .
H11C H 1.2384 0.2056 0.2769 0.047 Uiso 1 1 d R U . . .
Pb1 Pb 0.73998(10) 0.88633(6) 0.26856(4) 0.01649(18) Uani 1 1 d . . . . .
Pb2 Pb 0.93796(10) 0.43588(7) 0.20930(4) 0.0230(2) Uani 1 1 d . . . . .
N11 N 0.731(3) 0.9873(15) 0.0840(11) 0.023(4) Uani 0.745(15) 1 d D U P A 1
N12 N 0.829(4) 0.9356(16) 0.0153(12) 0.027(4) Uani 0.745(15) 1 d D U P A 1
C4 C 0.937(3) 0.8085(15) 0.0361(11) 0.016(4) Uani 0.745(15) 1 d D U P A 1
N17 N 1.043(3) 0.7318(14) -0.0289(9) 0.017(3) Uani 0.745(15) 1 d D U P A 1
N18 N 1.124(3) 0.6167(14) 0.0099(10) 0.019(4) Uani 0.745(15) 1 d D U P A 1
N19 N 1.068(3) 0.6279(16) 0.0977(11) 0.027(4) Uani 0.745(15) 1 d D U P A 1
N20 N 0.952(3) 0.7437(16) 0.1154(11) 0.023(4) Uani 0.745(15) 1 d D U P A 1
O4 O 1.067(2) 0.7601(15) -0.1133(9) 0.028(4) Uani 0.745(15) 1 d D U P A 1
N11' N 0.732(8) 0.987(3) 0.089(3) 0.028(7) Uiso 0.255(15) 1 d D U P A 2
N12' N 0.804(12) 0.933(4) 0.017(3) 0.028(6) Uiso 0.255(15) 1 d D U P A 2
C4' C 0.933(7) 0.810(3) 0.004(2) 0.022(5) Uiso 0.255(15) 1 d D U P A 2
N17' N 0.981(6) 0.727(4) 0.0740(19) 0.022(5) Uiso 0.255(15) 1 d D U P A 2
N18' N 1.103(9) 0.618(3) 0.040(3) 0.022(6) Uiso 0.255(15) 1 d D U P A 2
N19' N 1.131(7) 0.640(3) -0.049(3) 0.024(6) Uiso 0.255(15) 1 d D U P A 2
N20' N 1.025(8) 0.755(3) -0.072(2) 0.024(6) Uiso 0.255(15) 1 d D U P A 2
O4' O 0.946(7) 0.714(4) 0.160(2) 0.022(7) Uiso 0.255(15) 1 d D U P A 2


_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 N3 1.31(2) . ?
C1 N6 1.37(2) . ?
C1 N1 1.37(2) . ?
C2 N7 1.32(2) . ?
C2 N10 1.351(18) . ?
C2 N2 1.40(2) . ?
C3 N16 1.334(16) . ?
C3 N13 1.360(17) . ?
C3 N11 1.384(16) . ?
C3 N11' 1.39(2) . ?
N1 N2 1.280(19) . ?
N3 O1 1.305(15) . ?
N3 N4 1.368(18) . ?
N4 N5 1.318(19) . ?
N5 N6 1.339(19) . ?
N7 O2 1.289(16) . ?
N7 N8 1.370(18) . ?
N8 N9 1.339(19) . ?
N9 N10 1.326(19) . ?
N13 O3 1.299(15) . ?
N13 N14 1.343(15) . ?
N14 N15 1.347(16) . ?
N15 N16 1.314(16) . ?
O1 Pb2 2.572(10) . ?
O2 Pb1 2.716(12) 2_676 ?
O5 Pb1 2.700(11) . ?
O5 H5A 0.8500 . ?
O5 H5B 0.8500 . ?
O6 Pb1 2.697(12) . ?
O6 H6A 0.8501 . ?
O6 H6B 0.8500 . ?
O7 Pb1 2.621(10) . ?
O7 H7A 0.8500 . ?
O7 H7B 0.8500 . ?
O8 Pb2 2.638(12) . ?
O8 H8A 0.8500 . ?
O8 H8B 0.8499 . ?
O9 Pb2 2.526(10) . ?
O9 H9A 0.8500 . ?
O9 H9B 0.8500 . ?
O10 Pb2 2.581(11) . ?
O10 H10A 0.8499 . ?
O10 H10B 0.8501 . ?
O11 Pb2 2.557(12) . ?
O11 H11B 0.8500 . ?
O11 H11C 0.8500 . ?
Pb1 O4' 2.58(4) . ?
Pb1 O2 2.716(12) 2_676 ?
Pb2 O4 2.693(17) 2_765 ?
Pb2 N19' 2.79(4) 2_765 ?
Pb2 N19 2.794(16) . ?
N11 N12 1.247(16) . ?
N12 C4 1.403(17) . ?
C4 N20 1.344(19) . ?
C4 N17 1.346(18) . ?
N17 O4 1.293(15) . ?
N17 N18 1.339(17) . ?
N18 N19 1.345(18) . ?
N19 N20 1.314(18) . ?
O4 Pb2 2.693(17) 2_765 ?
N11' N12' 1.26(2) . ?
N12' C4' 1.388(19) . ?
C4' N20' 1.34(2) . ?
C4' N17' 1.35(2) . ?
N17' O4' 1.30(2) . ?
N17' N18' 1.34(2) . ?
N18' N19' 1.35(2) . ?
N19' N20' 1.30(2) . ?
N19' Pb2 2.79(4) 2_765 ?

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
N3 C1 N6 109.1(15) . . ?
N3 C1 N1 119.6(16) . . ?
N6 C1 N1 131.0(16) . . ?
N7 C2 N10 111.0(15) . . ?
N7 C2 N2 119.9(14) . . ?
N10 C2 N2 129.1(16) . . ?
N16 C3 N13 108.9(12) . . ?
N16 C3 N11 132.7(13) . . ?
N13 C3 N11 118.4(12) . . ?
N16 C3 N11' 135(2) . . ?
N13 C3 N11' 116(2) . . ?
N2 N1 C1 116.2(14) . . ?
N1 N2 C2 111.7(14) . . ?
O1 N3 C1 130.7(15) . . ?
O1 N3 N4 120.7(13) . . ?
C1 N3 N4 108.5(14) . . ?
N5 N4 N3 106.2(14) . . ?
N4 N5 N6 111.0(13) . . ?
N5 N6 C1 105.3(13) . . ?
O2 N7 C2 130.5(14) . . ?
O2 N7 N8 122.4(14) . . ?
C2 N7 N8 107.2(14) . . ?
N9 N8 N7 105.4(13) . . ?
N10 N9 N8 112.0(12) . . ?
N9 N10 C2 104.4(14) . . ?
O3 N13 N14 126.0(12) . . ?
O3 N13 C3 126.5(12) . . ?
N14 N13 C3 107.4(11) . . ?
N13 N14 N15 106.1(11) . . ?
N16 N15 N14 111.0(12) . . ?
N15 N16 C3 106.6(12) . . ?
N3 O1 Pb2 113.6(8) . . ?
N7 O2 Pb1 124.2(10) . 2_676 ?
Pb1 O5 H5A 109.3 . . ?
Pb1 O5 H5B 109.2 . . ?
H5A O5 H5B 108.0 . . ?
Pb1 O6 H6A 108.8 . . ?
Pb1 O6 H6B 108.7 . . ?
H6A O6 H6B 107.9 . . ?
Pb1 O7 H7A 120.0 . . ?
Pb1 O7 H7B 120.1 . . ?
H7A O7 H7B 119.9 . . ?
Pb2 O8 H8A 109.9 . . ?
Pb2 O8 H8B 109.0 . . ?
H8A O8 H8B 110.1 . . ?
Pb2 O9 H9A 109.7 . . ?
Pb2 O9 H9B 109.7 . . ?
H9A O9 H9B 108.3 . . ?
Pb2 O10 H10A 117.9 . . ?
Pb2 O10 H10B 121.0 . . ?
H10A O10 H10B 121.1 . . ?
Pb2 O11 H11B 109.3 . . ?
Pb2 O11 H11C 109.8 . . ?
H11B O11 H11C 109.9 . . ?
O4' Pb1 O7 87.7(10) . . ?
O4' Pb1 O6 73.2(11) . . ?
O7 Pb1 O6 134.5(3) . . ?
O4' Pb1 O5 66.0(10) . . ?
O7 Pb1 O5 68.7(3) . . ?
O6 Pb1 O5 132.0(4) . . ?
O4' Pb1 O2 138.5(11) . 2_676 ?
O7 Pb1 O2 130.1(4) . 2_676 ?
O6 Pb1 O2 67.7(4) . 2_676 ?
O5 Pb1 O2 136.7(3) . 2_676 ?
O9 Pb2 O11 71.0(3) . . ?
O9 Pb2 O1 82.7(3) . . ?
O11 Pb2 O1 110.3(4) . . ?
O9 Pb2 O10 73.6(3) . . ?
O11 Pb2 O10 143.8(4) . . ?
O1 Pb2 O10 72.0(4) . . ?
O9 Pb2 O8 129.6(3) . . ?
O11 Pb2 O8 75.9(4) . . ?
O1 Pb2 O8 74.5(3) . . ?
O10 Pb2 O8 135.4(4) . . ?
O9 Pb2 O4 72.6(4) . 2_765 ?
O11 Pb2 O4 76.0(4) . 2_765 ?
O1 Pb2 O4 151.0(4) . 2_765 ?
O10 Pb2 O4 86.4(4) . 2_765 ?
O8 Pb2 O4 133.5(4) . 2_765 ?
O9 Pb2 N19' 89.0(10) . 2_765 ?
O11 Pb2 N19' 108.4(7) . 2_765 ?
O1 Pb2 N19' 135.0(7) . 2_765 ?
O10 Pb2 N19' 63.2(7) . 2_765 ?
O8 Pb2 N19' 137.9(9) . 2_765 ?
O9 Pb2 N19 151.8(4) . . ?
O11 Pb2 N19 137.1(4) . . ?
O1 Pb2 N19 85.2(4) . . ?
O10 Pb2 N19 78.5(4) . . ?
O8 Pb2 N19 70.2(5) . . ?
O4 Pb2 N19 109.8(4) 2_765 . ?
N12 N11 C3 115.7(15) . . ?
N11 N12 C4 109.9(16) . . ?
N20 C4 N17 109.9(13) . . ?
N20 C4 N12 129.9(15) . . ?
N17 C4 N12 120.2(13) . . ?
O4 N17 N18 124.8(15) . . ?
O4 N17 C4 128.1(14) . . ?
N18 N17 C4 107.1(12) . . ?
N17 N18 N19 106.3(13) . . ?
N20 N19 N18 111.4(14) . . ?
N20 N19 Pb2 112.9(11) . . ?
N18 N19 Pb2 122.7(12) . . ?
N19 N20 C4 105.3(15) . . ?
N17 O4 Pb2 112.4(11) . 2_765 ?
N12' N11' C3 110(2) . . ?
N11' N12' C4' 129(3) . . ?
N20' C4' N17' 110.2(18) . . ?
N20' C4' N12' 129(2) . . ?
N17' C4' N12' 120.7(19) . . ?
O4' N17' N18' 111(4) . . ?
O4' N17' C4' 143(4) . . ?
N18' N17' C4' 106.2(18) . . ?
N17' N18' N19' 106.7(19) . . ?
N20' N19' N18' 111(2) . . ?
N20' N19' Pb2 87(2) . 2_765 ?
N18' N19' Pb2 144(3) . 2_765 ?
N19' N20' C4' 105(2) . . ?
N17' O4' Pb1 128(3) . . ?

_refine_diff_density_max         1.705
_refine_diff_density_min         -2.300
_refine_diff_density_rms         0.350

####################################################################### 
# 
# 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_CCDC1
_audit_block_doi                 10.5517/ccdc.csd.cc1zyrj6
_database_code_depnum_ccdc_archive 'CCDC 1845849'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2019-01-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H4 N10 O5 Pb2, H2 O'
_chemical_formula_sum            'C2 H6 N10 O6 Pb2'
_chemical_formula_weight         680.55

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

_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'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   11.4741(12)
_cell_length_b                   17.026(2)
_cell_length_c                   5.9443(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1161.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1313
_cell_measurement_theta_min      3.55
_cell_measurement_theta_max      25.37

_exptl_crystal_description       needle
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.893
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    29.009
_shelx_estimated_absorpt_T_min   0.068
_shelx_estimated_absorpt_T_max   0.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4660
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4516
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.551
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             1061
_reflns_number_gt                745
_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.
 
 _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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (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)+(0.0327P)²+1.3495P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1061
_refine_ls_number_parameters     92
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0923
_refine_ls_wR_factor_gt          0.0813
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_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
C1 C 0.5792(12) -0.0150(8) 0.246(3) 0.009(3) Uani 1 1 d . U . . .
N1 N 0.5242(11) 0.0243(7) 0.068(2) 0.014(3) Uani 1 1 d . U . . .
N2 N 0.6369(12) 0.0290(7) 0.397(2) 0.015(3) Uani 1 1 d . . . . .
N3 N 0.6813(10) -0.0187(7) 0.554(2) 0.015(3) Uani 1 1 d . . . . .
N4 N 0.6506(12) -0.0899(7) 0.493(2) 0.017(3) Uani 1 1 d . U . . .
N5 N 0.5864(11) -0.0886(7) 0.302(3) 0.017(3) Uani 1 1 d . . . . .
O1 O 0.7500 0.2500 0.591(2) 0.005(3) Uani 1 2 d S TU P . .
O2 O 0.6535(9) 0.1063(5) 0.4007(18) 0.012(2) Uani 1 1 d . . . . .
O3 O 1.0029(9) 0.2820(6) 0.2190(19) 0.022(3) Uani 1 1 d . . . . .
H3A H 0.9787 0.3291 0.2095 0.027 Uiso 1 1 d R U . . .
H3B H 1.0734 0.2706 0.1893 0.027 Uiso 1 1 d R U . . .
O4 O 0.7500 0.7500 0.384(3) 0.044(5) Uani 1 2 d S T P . .
H4B H 0.7722 0.7142 0.4745 0.052 Uiso 1 1 d R U . . .
Pb1 Pb 0.85478(4) 0.17246(3) 0.34247(9) 0.0087(2) 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 N5 1.301(18) . ?
C1 N2 1.345(19) . ?
C1 N1 1.40(2) . ?
N1 N1 1.29(2) 5_655 ?
N2 O2 1.332(15) . ?
N2 N3 1.334(18) . ?
N3 N4 1.314(17) . ?
N4 N5 1.352(19) . ?
O1 Pb1 2.317(9) 2_655 ?
O1 Pb1 2.317(9) . ?
O1 Pb1 2.329(9) 7_566 ?
O1 Pb1 2.329(9) 8_756 ?
O2 Pb1 2.592(10) . ?
O3 Pb1 2.628(10) . ?
O3 H3A 0.8500 . ?
O3 H3B 0.8500 . ?
O4 H4B 0.8500 . ?
Pb1 O1 2.329(9) 7_565 ?
Pb1 Pb1 3.5712(11) 2_655 ?

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
N5 C1 N2 109.4(14) . . ?
N5 C1 N1 133.2(14) . . ?
N2 C1 N1 117.4(13) . . ?
N1 N1 C1 111.3(16) 5_655 . ?
O2 N2 N3 122.4(12) . . ?
O2 N2 C1 129.1(13) . . ?
N3 N2 C1 108.5(12) . . ?
N4 N3 N2 105.5(12) . . ?
N3 N4 N5 111.2(12) . . ?
C1 N5 N4 105.4(12) . . ?
Pb1 O1 Pb1 100.8(5) 2_655 . ?
Pb1 O1 Pb1 110.74(2) 2_655 7_566 ?
Pb1 O1 Pb1 117.66(2) . 7_566 ?
Pb1 O1 Pb1 117.66(2) 2_655 8_756 ?
Pb1 O1 Pb1 110.74(2) . 8_756 ?
Pb1 O1 Pb1 100.1(5) 7_566 8_756 ?
N2 O2 Pb1 123.7(8) . . ?
Pb1 O3 H3A 118.5 . . ?
Pb1 O3 H3B 120.7 . . ?
H3A O3 H3B 120.8 . . ?
O1 Pb1 O1 79.537(18) . 7_565 ?
O1 Pb1 O2 72.6(2) . . ?
O1 Pb1 O2 82.6(2) 7_565 . ?
O1 Pb1 O3 96.3(3) . . ?
O1 Pb1 O3 75.7(2) 7_565 . ?
O2 Pb1 O3 157.2(3) . . ?
O1 Pb1 Pb1 39.6(3) . 2_655 ?
O1 Pb1 Pb1 40.0(3) 7_565 2_655 ?
O2 Pb1 Pb1 73.8(2) . 2_655 ?
O3 Pb1 Pb1 84.9(2) . 2_655 ?

_refine_diff_density_max         2.002
_refine_diff_density_min         -1.864
_refine_diff_density_rms         0.412

