# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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 1998756'
loop_
_audit_author_name
_audit_author_address
'Liu Jiao'
;NWU
China
;
_audit_update_record             
;
2020-04-26 deposited with the CCDC.	2020-06-15 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         'C28 H32 N10 O14 Zn3'
_chemical_formula_sum            'C28 H32 N10 O14 Zn3'
_chemical_formula_weight         928.74

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'
Zn Zn 0.2839 1.4301 '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 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   7.3787(9)
_cell_length_b                   15.3471(19)
_cell_length_c                   14.9299(18)
_cell_angle_alpha                90
_cell_angle_beta                 96.703(4)
_cell_angle_gamma                90
_cell_volume                     1679.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9912
_cell_measurement_theta_min      2.605
_cell_measurement_theta_max      25.362

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   0.678
_exptl_transmission_factor_max   0.750
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    2.212
_shelx_estimated_absorpt_T_min   0.654
_shelx_estimated_absorpt_T_max   0.762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ω
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19977
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.654
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2959
_reflns_number_gt                2641
_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)+(0.0590P)²+0.1540P] 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         2959
_refine_ls_number_parameters     251
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0830
_refine_ls_wR_factor_gt          0.0698
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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
Zn1 Zn 0.23411(3) 0.97464(2) 0.25151(2) 0.01027(12) Uani 1 1 d . . . . .
Zn2 Zn 1.0000 0.5000 0.5000 0.01074(13) Uani 1 2 d S . P . .
O1 O 0.3884(2) 0.87419(10) 0.23152(11) 0.0140(4) Uani 1 1 d . . . . .
O2 O 0.2281(2) 0.78455(11) 0.30982(13) 0.0194(4) Uani 1 1 d . . . . .
O3 O 1.0697(2) 0.54440(11) 0.37869(11) 0.0148(4) Uani 1 1 d . . . . .
O4 O 1.0712(2) 0.56496(10) 0.23298(11) 0.0144(4) Uani 1 1 d . . . . .
O5 O 0.1692(3) 0.98908(11) 0.37518(12) 0.0210(4) Uani 1 1 d . . . . .
O6 O 1.0982(2) 0.37638(10) 0.46730(12) 0.0173(4) Uani 1 1 d . . . . .
H6WB H 1.1007 0.3731 0.4133 0.026 Uiso 1 1 d R U . . .
H6WA H 1.0431 0.3335 0.4805 0.026 Uiso 1 1 d R U . . .
O7 O 0.8639(2) 0.25532(12) 0.51902(13) 0.0239(4) Uani 1 1 d . . . . .
H7WB H 0.7827 0.2894 0.5031 0.036 Uiso 1 1 d R U . . .
H7WA H 0.8618 0.2495 0.5728 0.036 Uiso 1 1 d R U . . .
N1 N 0.7371(3) 0.47215(12) 0.43091(14) 0.0129(5) Uani 1 1 d . . . . .
N2 N 0.6493(3) 0.39602(13) 0.44319(15) 0.0173(5) Uani 1 1 d . . . . .
N3 N 0.4986(3) 0.39242(12) 0.38887(15) 0.0160(5) Uani 1 1 d . . . . .
N4 N 0.4849(3) 0.46664(12) 0.33935(14) 0.0114(4) Uani 1 1 d . . . . .
N5 N 0.2482(3) 1.02707(13) 0.52099(16) 0.0200(5) Uani 1 1 d . . . . .
C1 C 0.3642(3) 0.80189(15) 0.27304(16) 0.0129(5) Uani 1 1 d . . . . .
C2 C 0.5224(3) 0.73939(15) 0.27657(16) 0.0114(5) Uani 1 1 d . . . . .
C3 C 0.6831(3) 0.76284(15) 0.24247(16) 0.0132(5) Uani 1 1 d . . . . .
H3 H 0.6904 0.8170 0.2123 0.016 Uiso 1 1 calc R U . . .
C4 C 0.8320(3) 0.70757(15) 0.25224(17) 0.0130(5) Uani 1 1 d . . . . .
H4 H 0.9405 0.7240 0.2280 0.016 Uiso 1 1 calc R U . . .
C5 C 0.8259(3) 0.62810(14) 0.29702(15) 0.0107(5) Uani 1 1 d . . . . .
C6 C 0.6619(3) 0.60224(14) 0.32855(16) 0.0105(5) Uani 1 1 d . . . . .
C7 C 0.5128(3) 0.65808(14) 0.31869(16) 0.0115(5) Uani 1 1 d . . . . .
H7 H 0.4026 0.6409 0.3408 0.014 Uiso 1 1 calc R U . . .
C8 C 0.6328(3) 0.51462(14) 0.36704(16) 0.0093(5) Uani 1 1 d . . . . .
C9 C 0.9990(3) 0.57483(14) 0.30516(16) 0.0110(5) Uani 1 1 d . . . . .
C10 C 0.2134(3) 1.04589(17) 0.43480(17) 0.0168(5) Uani 1 1 d . . . . .
C11 C 0.2257(4) 1.14316(16) 0.42231(18) 0.0204(6) Uani 1 1 d . . . . .
H11A H 0.1028 1.1693 0.4093 0.025 Uiso 1 1 calc R U . . .
H11B H 0.2983 1.1575 0.3726 0.025 Uiso 1 1 calc R U . . .
C12 C 0.3212(4) 1.17514(18) 0.51311(19) 0.0259(6) Uani 1 1 d . . . . .
H12A H 0.4544 1.1810 0.5113 0.031 Uiso 1 1 calc R U . . .
H12B H 0.2714 1.2320 0.5299 0.031 Uiso 1 1 calc R U . . .
C13 C 0.2790(4) 1.10361(17) 0.57889(19) 0.0269(7) Uani 1 1 d . . . . .
H13A H 0.3831 1.0944 0.6261 0.032 Uiso 1 1 calc R U . . .
H13B H 0.1690 1.1180 0.6080 0.032 Uiso 1 1 calc R U . . .
C14 C 0.2422(4) 0.94034(17) 0.55941(19) 0.0253(6) Uani 1 1 d . . . . .
H14A H 0.1987 0.8988 0.5119 0.038 Uiso 1 1 calc R U . . .
H14B H 0.1592 0.9402 0.6061 0.038 Uiso 1 1 calc R U . . .
H14C H 0.3649 0.9235 0.5862 0.038 Uiso 1 1 calc 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
Zn1 O1 1.9599(16) . ?
Zn1 O5 1.9732(18) . ?
Zn1 N4 1.9885(19) 2 ?
Zn1 O4 1.9904(16) 2_655 ?
Zn2 O3 2.0557(17) . ?
Zn2 O3 2.0558(17) 3_766 ?
Zn2 O6 2.1083(16) 3_766 ?
Zn2 O6 2.1083(16) . ?
Zn2 N1 2.131(2) 3_766 ?
Zn2 N1 2.131(2) . ?
O1 C1 1.293(3) . ?
O2 C1 1.228(3) . ?
O3 C9 1.250(3) . ?
O4 C9 1.266(3) . ?
O4 Zn1 1.9904(16) 2_645 ?
O5 C10 1.261(3) . ?
O6 H6WB 0.8099 . ?
O6 H6WA 0.8100 . ?
O7 H7WB 0.8100 . ?
O7 H7WA 0.8100 . ?
N1 C8 1.325(3) . ?
N1 N2 1.359(3) . ?
N2 N3 1.298(3) . ?
N3 N4 1.355(3) . ?
N4 C8 1.341(3) . ?
N4 Zn1 1.9884(19) 2_545 ?
N5 C10 1.315(3) . ?
N5 C14 1.452(3) . ?
N5 C13 1.460(3) . ?
C1 C2 1.507(3) . ?
C2 C3 1.391(3) . ?
C2 C7 1.403(3) . ?
C3 C4 1.383(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.394(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.406(3) . ?
C5 C9 1.510(3) . ?
C6 C7 1.389(3) . ?
C6 C8 1.488(3) . ?
C7 H7 0.9500 . ?
C10 C11 1.508(3) . ?
C11 C12 1.534(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.529(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

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 Zn1 O5 116.07(8) . . ?
O1 Zn1 N4 106.72(7) . 2 ?
O5 Zn1 N4 112.26(8) . 2 ?
O1 Zn1 O4 98.12(7) . 2_655 ?
O5 Zn1 O4 93.65(7) . 2_655 ?
N4 Zn1 O4 129.82(8) 2 2_655 ?
O3 Zn2 O3 180.00(4) . 3_766 ?
O3 Zn2 O6 91.93(7) . 3_766 ?
O3 Zn2 O6 88.07(7) 3_766 3_766 ?
O3 Zn2 O6 88.07(7) . . ?
O3 Zn2 O6 91.93(7) 3_766 . ?
O6 Zn2 O6 180.00(9) 3_766 . ?
O3 Zn2 N1 93.03(7) . 3_766 ?
O3 Zn2 N1 86.97(7) 3_766 3_766 ?
O6 Zn2 N1 91.45(7) 3_766 3_766 ?
O6 Zn2 N1 88.55(7) . 3_766 ?
O3 Zn2 N1 86.97(7) . . ?
O3 Zn2 N1 93.03(7) 3_766 . ?
O6 Zn2 N1 88.55(7) 3_766 . ?
O6 Zn2 N1 91.45(7) . . ?
N1 Zn2 N1 180.0 3_766 . ?
C1 O1 Zn1 119.12(15) . . ?
C9 O3 Zn2 140.93(16) . . ?
C9 O4 Zn1 110.73(14) . 2_645 ?
C10 O5 Zn1 131.84(18) . . ?
Zn2 O6 H6WB 109.6 . . ?
Zn2 O6 H6WA 118.7 . . ?
H6WB O6 H6WA 105.1 . . ?
H7WB O7 H7WA 105.2 . . ?
C8 N1 N2 105.90(18) . . ?
C8 N1 Zn2 132.00(15) . . ?
N2 N1 Zn2 121.91(15) . . ?
N3 N2 N1 109.83(19) . . ?
N2 N3 N4 108.01(18) . . ?
C8 N4 N3 106.66(18) . . ?
C8 N4 Zn1 138.03(16) . 2_545 ?
N3 N4 Zn1 115.30(14) . 2_545 ?
C10 N5 C14 125.2(2) . . ?
C10 N5 C13 113.7(2) . . ?
C14 N5 C13 120.9(2) . . ?
O2 C1 O1 124.5(2) . . ?
O2 C1 C2 121.1(2) . . ?
O1 C1 C2 114.4(2) . . ?
C3 C2 C7 119.0(2) . . ?
C3 C2 C1 120.8(2) . . ?
C7 C2 C1 120.2(2) . . ?
C4 C3 C2 120.2(2) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 121.2(2) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C4 C5 C6 119.0(2) . . ?
C4 C5 C9 116.0(2) . . ?
C6 C5 C9 125.0(2) . . ?
C7 C6 C5 119.5(2) . . ?
C7 C6 C8 116.8(2) . . ?
C5 C6 C8 123.6(2) . . ?
C6 C7 C2 121.0(2) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
N1 C8 N4 109.6(2) . . ?
N1 C8 C6 128.7(2) . . ?
N4 C8 C6 121.7(2) . . ?
O3 C9 O4 122.0(2) . . ?
O3 C9 C5 122.4(2) . . ?
O4 C9 C5 115.6(2) . . ?
O5 C10 N5 122.9(2) . . ?
O5 C10 C11 127.7(2) . . ?
N5 C10 C11 109.3(2) . . ?
C10 C11 C12 103.6(2) . . ?
C10 C11 H11A 111.0 . . ?
C12 C11 H11A 111.0 . . ?
C10 C11 H11B 111.0 . . ?
C12 C11 H11B 111.0 . . ?
H11A C11 H11B 109.0 . . ?
C13 C12 C11 103.3(2) . . ?
C13 C12 H12A 111.1 . . ?
C11 C12 H12A 111.1 . . ?
C13 C12 H12B 111.1 . . ?
C11 C12 H12B 111.1 . . ?
H12A C12 H12B 109.1 . . ?
N5 C13 C12 103.1(2) . . ?
N5 C13 H13A 111.1 . . ?
C12 C13 H13A 111.1 . . ?
N5 C13 H13B 111.1 . . ?
C12 C13 H13B 111.1 . . ?
H13A C13 H13B 109.1 . . ?
N5 C14 H14A 109.5 . . ?
N5 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N5 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

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
C8 N1 N2 N3 0.2(3) . . . . ?
Zn2 N1 N2 N3 -175.38(16) . . . . ?
N1 N2 N3 N4 0.2(3) . . . . ?
N2 N3 N4 C8 -0.5(3) . . . . ?
N2 N3 N4 Zn1 178.57(16) . . . 2_545 ?
Zn1 O1 C1 O2 16.0(3) . . . . ?
Zn1 O1 C1 C2 -161.76(14) . . . . ?
O2 C1 C2 C3 -173.7(2) . . . . ?
O1 C1 C2 C3 4.1(3) . . . . ?
O2 C1 C2 C7 3.0(3) . . . . ?
O1 C1 C2 C7 -179.2(2) . . . . ?
C7 C2 C3 C4 -1.7(4) . . . . ?
C1 C2 C3 C4 175.1(2) . . . . ?
C2 C3 C4 C5 -0.7(4) . . . . ?
C3 C4 C5 C6 3.3(4) . . . . ?
C3 C4 C5 C9 -178.5(2) . . . . ?
C4 C5 C6 C7 -3.3(3) . . . . ?
C9 C5 C6 C7 178.6(2) . . . . ?
C4 C5 C6 C8 172.3(2) . . . . ?
C9 C5 C6 C8 -5.8(4) . . . . ?
C5 C6 C7 C2 0.9(3) . . . . ?
C8 C6 C7 C2 -175.0(2) . . . . ?
C3 C2 C7 C6 1.6(3) . . . . ?
C1 C2 C7 C6 -175.2(2) . . . . ?
N2 N1 C8 N4 -0.5(3) . . . . ?
Zn2 N1 C8 N4 174.46(16) . . . . ?
N2 N1 C8 C6 178.7(2) . . . . ?
Zn2 N1 C8 C6 -6.4(4) . . . . ?
N3 N4 C8 N1 0.6(3) . . . . ?
Zn1 N4 C8 N1 -178.08(18) 2_545 . . . ?
N3 N4 C8 C6 -178.6(2) . . . . ?
Zn1 N4 C8 C6 2.7(4) 2_545 . . . ?
C7 C6 C8 N1 -134.1(3) . . . . ?
C5 C6 C8 N1 50.2(4) . . . . ?
C7 C6 C8 N4 45.0(3) . . . . ?
C5 C6 C8 N4 -130.7(2) . . . . ?
Zn2 O3 C9 O4 -152.15(18) . . . . ?
Zn2 O3 C9 C5 29.9(4) . . . . ?
Zn1 O4 C9 O3 13.5(3) 2_645 . . . ?
Zn1 O4 C9 C5 -168.39(14) 2_645 . . . ?
C4 C5 C9 O3 129.2(2) . . . . ?
C6 C5 C9 O3 -52.7(3) . . . . ?
C4 C5 C9 O4 -48.8(3) . . . . ?
C6 C5 C9 O4 129.3(2) . . . . ?
Zn1 O5 C10 N5 -141.2(2) . . . . ?
Zn1 O5 C10 C11 42.2(4) . . . . ?
C14 N5 C10 O5 0.4(4) . . . . ?
C13 N5 C10 O5 -174.3(2) . . . . ?
C14 N5 C10 C11 177.5(2) . . . . ?
C13 N5 C10 C11 2.8(3) . . . . ?
O5 C10 C11 C12 -169.1(3) . . . . ?
N5 C10 C11 C12 14.0(3) . . . . ?
C10 C11 C12 C13 -24.0(3) . . . . ?
C10 N5 C13 C12 -18.4(3) . . . . ?
C14 N5 C13 C12 166.7(2) . . . . ?
C11 C12 C13 N5 25.3(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C14 H14C O4 0.98 2.52 3.338(3) 140.4 4_576
C14 H14A O7 0.98 2.44 3.284(3) 143.7 3_666
C13 H13A O1 0.99 2.60 3.540(3) 158.6 3_676
C11 H11B O4 0.99 2.40 3.142(3) 130.8 2_655
O7 H7WA O2 0.81 2.01 2.787(3) 159.7 3_666
O7 H7WB N2 0.81 2.06 2.834(3) 160.1 .
O6 H6WA O7 0.81 1.92 2.711(2) 164.1 .
O6 H6WB O1 0.81 2.17 2.982(3) 175.9 2_645
C14 H14C O4 0.98 2.52 3.338(3) 140.4 4_576
C14 H14A O7 0.98 2.44 3.284(3) 143.7 3_666
C13 H13A O1 0.99 2.60 3.540(3) 158.6 3_676
C11 H11B O4 0.99 2.40 3.142(3) 130.8 2_655
O7 H7WA O2 0.81 2.01 2.787(3) 159.7 3_666
O7 H7WB N2 0.81 2.06 2.834(3) 160.1 .
O6 H6WA O7 0.81 1.92 2.711(2) 164.1 .
O6 H6WB O1 0.81 2.17 2.982(3) 175.9 2_645
C14 H14C O4 0.98 2.52 3.338(3) 140.4 4_576
C14 H14A O7 0.98 2.44 3.284(3) 143.7 3_666
C13 H13A O1 0.99 2.60 3.540(3) 158.6 3_676
C11 H11B O4 0.99 2.40 3.142(3) 130.8 2_655
O7 H7WA O2 0.81 2.01 2.787(3) 159.7 3_666
O7 H7WB N2 0.81 2.06 2.834(3) 160.1 .
O6 H6WA O7 0.81 1.92 2.711(2) 164.1 .
O6 H6WB O1 0.81 2.17 2.982(3) 175.9 2_645
C14 H14C O4 0.98 2.52 3.338(3) 140.4 4_576
C14 H14A O7 0.98 2.44 3.284(3) 143.7 3_666
C13 H13A O1 0.99 2.60 3.540(3) 158.6 3_676
C11 H11B O4 0.99 2.40 3.142(3) 130.8 2_655
O7 H7WA O2 0.81 2.01 2.787(3) 159.7 3_666
O7 H7WB N2 0.81 2.06 2.834(3) 160.1 .
O6 H6WA O7 0.81 1.92 2.711(2) 164.1 .
O6 H6WB O1 0.81 2.17 2.982(3) 175.9 2_645
C14 H14C O4 0.98 2.52 3.338(3) 140.4 4_576
C14 H14A O7 0.98 2.44 3.284(3) 143.7 3_666
C13 H13A O1 0.99 2.60 3.540(3) 158.6 3_676
C11 H11B O4 0.99 2.40 3.142(3) 130.8 2_655
O7 H7WA O2 0.81 2.01 2.787(3) 159.7 3_666
O7 H7WB N2 0.81 2.06 2.834(3) 160.1 .
O6 H6WA O7 0.81 1.92 2.711(2) 164.1 .
O6 H6WB O1 0.81 2.17 2.982(3) 175.9 2_645
C14 H14C O4 0.98 2.52 3.338(3) 140.4 4_576
C14 H14A O7 0.98 2.44 3.284(3) 143.7 3_666
C13 H13A O1 0.99 2.60 3.540(3) 158.6 3_676
C11 H11B O4 0.99 2.40 3.142(3) 130.8 2_655
O7 H7WA O2 0.81 2.01 2.787(3) 159.7 3_666
O7 H7WB N2 0.81 2.06 2.834(3) 160.1 .
O6 H6WA O7 0.81 1.92 2.711(2) 164.1 .
O6 H6WB O1 0.81 2.17 2.982(3) 175.9 2_645
O6 H6WB O1 0.81 2.17 2.982(3) 175.9 2_645
O6 H6WA O7 0.81 1.92 2.711(2) 164.1 .
O7 H7WB N2 0.81 2.06 2.834(3) 160.1 .
O7 H7WA O2 0.81 2.01 2.787(3) 159.7 3_666
C11 H11B O4 0.99 2.40 3.142(3) 130.8 2_655
C13 H13A O1 0.99 2.60 3.540(3) 158.6 3_676
C14 H14A O7 0.98 2.44 3.284(3) 143.7 3_666
C14 H14C O4 0.98 2.52 3.338(3) 140.4 4_576
O6 H6WB O1 0.81 2.17 2.982(3) 175.9 2_645
O6 H6WA O7 0.81 1.92 2.711(2) 164.1 .
O7 H7WB N2 0.81 2.06 2.834(3) 160.1 .
O7 H7WA O2 0.81 2.01 2.787(3) 159.7 3_666
C11 H11B O4 0.99 2.40 3.142(3) 130.8 2_655
C13 H13A O1 0.99 2.60 3.540(3) 158.6 3_676
C14 H14A O7 0.98 2.44 3.284(3) 143.7 3_666
C14 H14C O4 0.98 2.52 3.338(3) 140.4 4_576
O6 H6WB O1 0.81 2.17 2.982(3) 175.9 2_645
O6 H6WA O7 0.81 1.92 2.711(2) 164.1 .
O7 H7WB N2 0.81 2.06 2.834(3) 160.1 .
O7 H7WA O2 0.81 2.01 2.787(3) 159.7 3_666
C11 H11B O4 0.99 2.40 3.142(3) 130.8 2_655
C13 H13A O1 0.99 2.60 3.540(3) 158.6 3_676
C14 H14A O7 0.98 2.44 3.284(3) 143.7 3_666
C14 H14C O4 0.98 2.52 3.338(3) 140.4 4_576
O6 H6WB O1 0.81 2.17 2.982(3) 175.9 2_645
O6 H6WA O7 0.81 1.92 2.711(2) 164.1 .
O7 H7WB N2 0.81 2.06 2.834(3) 160.1 .
O7 H7WA O2 0.81 2.01 2.787(3) 159.7 3_666
C11 H11B O4 0.99 2.40 3.142(3) 130.8 2_655
C13 H13A O1 0.99 2.60 3.540(3) 158.6 3_676
C14 H14A O7 0.98 2.44 3.284(3) 143.7 3_666
C14 H14C O4 0.98 2.52 3.338(3) 140.4 4_576
O6 H6WB O1 0.81 2.17 2.982(3) 175.9 2_645
O6 H6WA O7 0.81 1.92 2.711(2) 164.1 .
O7 H7WB N2 0.81 2.06 2.834(3) 160.1 .
O7 H7WA O2 0.81 2.01 2.787(3) 159.7 3_666
C11 H11B O4 0.99 2.40 3.142(3) 130.8 2_655
C13 H13A O1 0.99 2.60 3.540(3) 158.6 3_676
C14 H14A O7 0.98 2.44 3.284(3) 143.7 3_666
C14 H14C O4 0.98 2.52 3.338(3) 140.4 4_576

_refine_diff_density_max         0.505
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.207

####################################################################### 
# 
# 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 1998757'
loop_
_audit_author_name
_audit_author_address
'Liu Jiao'
;NWU
China
;
_audit_update_record             
;
2020-04-23 deposited with the CCDC.	2020-06-15 downloaded from the CCDC.
;
_audit_creation_date             2020-04-22
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H10 N8 O9 Pb2, H2 O'
_chemical_formula_sum            'C18 H11 N8 O10 Pb2'
_chemical_formula_weight         913.73
_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      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                   7.0192(10)
_cell_length_b                   12.1615(18)
_cell_length_c                   14.3322(19)
_cell_angle_alpha                66.712(4)
_cell_angle_beta                 85.198(4)
_cell_angle_gamma                89.169(5)
_cell_volume                     1119.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5581
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.82
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    15.094
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.2975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1551 before and 0.0889 after correction. The Ratio of minimum to maximum transmission is 0.3992. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    2.710
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             838
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1223
_diffrn_reflns_av_unetI/netI     0.0938
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19780
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.421
_diffrn_reflns_theta_min         2.825
_diffrn_ambient_temperature      149.98
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_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                2936
_reflns_number_total             4102
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.588
_refine_diff_density_min         -2.609
_refine_diff_density_rms         0.411
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4102
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0564
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0835P)²+10.1997P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1657
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1-O10_$1
 2.85 with sigma of 0.02
 O9-H9A = O9-H9B
 0.87 with sigma of 0.02
 H9A-H9B
 1.38 with sigma of 0.04
 Pb1-H9A \\sim Pb1-H9B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O4) = Uanis(O5)
Uanis(C9) = Uanis(C13) = Uanis(C12) = Uanis(C17) = Uanis(C16) = Uanis(C15) =
Uanis(C14)
Uanis(C9) = Uanis(C6) = Uanis(C7) = Uanis(C2) = Uanis(C3) = Uanis(C4) =
Uanis(C5)
Uanis(C5) = Uanis(C11)
4.a Rotating group:
 O10(H10A,H10B)
4.b :
 N1(N2,N3,N4,C8), N6(N5,C11,N8,N7)
4.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N8(H8), C7(H7), C3(H3), C4(H4), C17(H17), C15(H15), C14(H14)
4.d Fitted hexagon refined as free rotating group:
 C6(C7,C2,C3,C4,C5), C13(C12,C17,C16,C15,C14)
;
_atom_sites_solution_hydrogens   mixed
_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
Pb2 Pb 0.04189(8) 0.35315(5) 0.74791(4) 0.0202(2) Uani 1 1 d . . . . .
Pb1 Pb 0.49526(9) 0.11342(5) 0.84036(4) 0.0212(2) Uani 1 1 d D . . . .
O10 O 0.5987(17) 0.1162(10) 1.0123(7) 0.030(3) Uani 1 1 d D . . . .
H10A H 0.7220 0.1275 1.0072 0.045 Uiso 1 1 d GR . . . .
H10B H 0.5785 0.0454 1.0609 0.045 Uiso 1 1 d GR . . . .
O6 O 0.1829(16) 0.1548(10) 0.7568(8) 0.025(3) Uani 1 1 d . . . . .
O3 O 0.3989(15) 0.3263(9) 0.7870(9) 0.026(3) Uani 1 1 d . . . . .
O4 O 0.6954(16) 0.3205(11) 0.8273(9) 0.031(2) Uani 1 1 d . . . . .
O1 O 0.4924(17) 0.9095(10) 0.7885(8) 0.031(3) Uani 1 1 d D . . . .
O8 O 0.1195(18) -0.2845(10) 0.5503(9) 0.035(3) Uani 1 1 d . . . . .
O5 O -0.1111(16) 0.1810(11) 0.7131(9) 0.031(2) Uani 1 1 d . . . . .
O7 O 0.0791(19) -0.4084(11) 0.7159(10) 0.038(3) Uani 1 1 d . . . . .
O2 O 0.5796(14) 0.9567(9) 0.6263(8) 0.020(2) Uani 1 1 d . . . . .
N1 N 0.7537(15) 0.4620(8) 0.5955(6) 0.022(3) Uani 1 1 d . . . . .
H1 H 0.7720 0.4011 0.6529 0.026 Uiso 1 1 calc R . . . .
N2 N 0.7996(14) 0.4670(8) 0.5018(6) 0.023(3) Uani 1 1 d G . . . .
N3 N 0.7493(14) 0.5735(8) 0.4356(6) 0.024(3) Uani 1 1 d G . . . .
N4 N 0.6724(15) 0.6344(8) 0.4884(6) 0.023(3) Uani 1 1 d G U . . .
C8 C 0.6751(15) 0.5655(8) 0.5872(7) 0.019(3) Uani 1 1 d G . . . .
N6 N -0.0679(15) -0.1964(10) 1.0596(7) 0.033(4) Uani 1 1 d . . . . .
N5 N 0.0231(15) -0.2021(9) 0.9778(7) 0.032(4) Uani 1 1 d G . . . .
C11 C -0.0510(15) -0.1232(10) 0.8976(7) 0.0210(10) Uani 1 1 d G . . . .
N8 N -0.1881(15) -0.0688(10) 0.9299(7) 0.032(4) Uani 1 1 d G . . . .
H8 H -0.2602 -0.0121 0.8913 0.038 Uiso 1 1 calc R . . . .
N7 N -0.1985(15) -0.1141(10) 1.0300(7) 0.037(4) Uani 1 1 d G . . . .
C10 C 0.038(2) 0.1213(15) 0.7292(12) 0.025(4) Uani 1 1 d . . . . .
C6 C 0.6041(15) 0.5963(8) 0.6714(6) 0.0210(10) Uani 1 1 d . . . . .
C7 C 0.6012(15) 0.7171(7) 0.6543(5) 0.0210(10) Uani 1 1 d G . . . .
H7 H 0.6402 0.7758 0.5886 0.025 Uiso 1 1 calc R . . . .
C2 C 0.5411(15) 0.7519(6) 0.7333(7) 0.0210(10) Uani 1 1 d G . . . .
C3 C 0.4840(15) 0.6659(8) 0.8294(6) 0.0210(10) Uani 1 1 d G . . . .
H3 H 0.4430 0.6897 0.8834 0.025 Uiso 1 1 calc R . . . .
C4 C 0.4870(14) 0.5452(7) 0.8465(5) 0.0210(10) Uani 1 1 d G . . . .
H4 H 0.4480 0.4864 0.9122 0.025 Uiso 1 1 calc R . . . .
C5 C 0.5471(15) 0.5104(6) 0.7675(7) 0.0210(10) Uani 1 1 d G . . . .
C9 C 0.555(2) 0.3773(14) 0.7956(12) 0.0210(10) Uani 1 1 d . . . . .
C13 C 0.0474(15) 0.0065(7) 0.7144(7) 0.0210(10) Uani 1 1 d . . . . .
C12 C 0.0035(15) -0.1060(8) 0.7904(5) 0.0210(10) Uani 1 1 d G . . . .
C17 C 0.0200(15) -0.2072(7) 0.7681(6) 0.0210(10) Uani 1 1 d G . . . .
H17 H -0.0100 -0.2842 0.8201 0.025 Uiso 1 1 calc R . . . .
C16 C 0.0805(15) -0.1959(7) 0.6698(7) 0.0210(10) Uani 1 1 d G . . . .
C15 C 0.1245(15) -0.0834(8) 0.5938(5) 0.0210(10) Uani 1 1 d G . . . .
H15 H 0.1658 -0.0757 0.5266 0.025 Uiso 1 1 calc R . . . .
C14 C 0.1079(15) 0.0178(7) 0.6161(6) 0.0210(10) Uani 1 1 d G . . . .
H14 H 0.1380 0.0948 0.5642 0.025 Uiso 1 1 calc R . . . .
C1 C 0.534(2) 0.8772(14) 0.7210(12) 0.018(3) Uani 1 1 d . . . . .
C18 C 0.095(2) -0.3081(14) 0.6463(13) 0.020(3) Uani 1 1 d . . . . .
O9 O 0.5569(15) 0.1748(10) 0.6268(8) 0.023(3) Uani 1 1 d D . . . .
H9A H 0.634(11) 0.197(14) 0.660(6) 0.034 Uiso 1 1 d DR . . . .
H9B H 0.444(5) 0.167(15) 0.658(6) 0.034 Uiso 1 1 d DR . . . .


_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
Pb2 O6 2.554(11) . ?
Pb2 O3 2.602(11) . ?
Pb2 O4 2.564(11) 1_455 ?
Pb2 O5 2.601(12) . ?
Pb2 N3 2.72(3) 2_666 ?
Pb2 N6 2.683(9) 2_557 ?
Pb1 O10 2.640(10) . ?
Pb1 O6 2.535(11) . ?
Pb1 O3 2.493(10) . ?
Pb1 N7 2.68(4) 2_557 ?
O10 H10A 0.8707 . ?
O10 H10B 0.8708 . ?
O6 C10 1.249(19) . ?
O3 C9 1.301(19) . ?
O4 Pb2 2.564(11) 1_655 ?
O4 C9 1.212(18) . ?
O1 C1 1.194(17) . ?
O8 C18 1.287(19) . ?
O5 C10 1.251(19) . ?
O7 C18 1.232(19) . ?
O2 C1 1.333(18) . ?
N1 H1 0.8800 . ?
N1 N2 1.332(7) . ?
N1 C8 1.332(7) . ?
N2 N3 1.332(7) . ?
N3 Pb2 2.720(9) 2_666 ?
N3 N4 1.332(7) . ?
N4 C8 1.332(7) . ?
C8 C6 1.449(10) . ?
N6 Pb2 2.683(9) 2_557 ?
N6 N5 1.313(7) . ?
N6 N7 1.314(7) . ?
N5 C11 1.313(7) . ?
C11 N8 1.313(7) . ?
C11 C12 1.484(11) . ?
N8 H8 0.8800 . ?
N8 N7 1.313(7) . ?
N7 Pb1 2.675(9) 2_557 ?
C10 C13 1.492(17) . ?
C6 C7 1.3900 . ?
C6 C5 1.3900 . ?
C7 H7 0.9500 . ?
C7 C2 1.3900 . ?
C2 C3 1.3900 . ?
C2 C1 1.464(16) . ?
C3 H3 0.9500 . ?
C3 C4 1.3900 . ?
C4 H4 0.9500 . ?
C4 C5 1.3900 . ?
C5 C9 1.507(17) . ?
C13 C12 1.3900 . ?
C13 C14 1.3900 . ?
C12 C17 1.3900 . ?
C17 H17 0.9500 . ?
C17 C16 1.3900 . ?
C16 C15 1.3900 . ?
C16 C18 1.530(17) . ?
C15 H15 0.9500 . ?
C15 C14 1.3900 . ?
C14 H14 0.9500 . ?
O9 H9A 0.87(2) . ?
O9 H9B 0.86(2) . ?

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
O6 Pb2 O3 65.4(3) . . ?
O6 Pb2 O4 110.2(4) . 1_455 ?
O6 Pb2 O5 50.2(3) . . ?
O6 Pb2 N3 79.4(6) . 2_666 ?
O6 Pb2 N6 67.7(3) . 2_557 ?
O3 Pb2 N3 73.7(6) . 2_666 ?
O3 Pb2 N6 70.2(3) . 2_557 ?
O4 Pb2 O3 144.6(4) 1_455 . ?
O4 Pb2 O5 71.7(4) 1_455 . ?
O4 Pb2 N3 141.6(6) 1_455 2_666 ?
O4 Pb2 N6 75.8(3) 1_455 2_557 ?
O5 Pb2 O3 115.5(3) . . ?
O5 Pb2 N3 90.1(6) . 2_666 ?
O5 Pb2 N6 87.7(4) . 2_557 ?
N6 Pb2 N3 138.6(6) 2_557 2_666 ?
O10 Pb1 N7 66.8(7) . 2_557 ?
O6 Pb1 O10 133.1(3) . . ?
O6 Pb1 N7 67.8(7) . 2_557 ?
O3 Pb1 O10 89.4(4) . . ?
O3 Pb1 O6 67.3(4) . . ?
O3 Pb1 N7 73.8(7) . 2_557 ?
Pb1 O10 H10A 109.3 . . ?
Pb1 O10 H10B 109.3 . . ?
H10A O10 H10B 104.5 . . ?
Pb1 O6 Pb2 111.8(4) . . ?
C10 O6 Pb2 94.9(9) . . ?
C10 O6 Pb1 151.8(10) . . ?
Pb1 O3 Pb2 111.6(4) . . ?
C9 O3 Pb2 146.4(9) . . ?
C9 O3 Pb1 101.9(9) . . ?
C9 O4 Pb2 129.5(11) . 1_655 ?
C10 O5 Pb2 92.6(10) . . ?
N2 N1 H1 126.0 . . ?
C8 N1 H1 126.0 . . ?
C8 N1 N2 108.0 . . ?
N3 N2 N1 108.0 . . ?
N2 N3 Pb2 113.4(5) . 2_666 ?
N2 N3 N4 108.0 . . ?
N4 N3 Pb2 131.5(5) . 2_666 ?
C8 N4 N3 108.0 . . ?
N1 C8 C6 125.5(7) . . ?
N4 C8 N1 108.1 . . ?
N4 C8 C6 126.4(7) . . ?
N5 N6 Pb2 125.9(5) . 2_557 ?
N5 N6 N7 108.0 . . ?
N7 N6 Pb2 125.1(5) . 2_557 ?
N6 N5 C11 108.0 . . ?
N5 C11 N8 108.0 . . ?
N5 C11 C12 125.2(7) . . ?
N8 C11 C12 126.7(7) . . ?
C11 N8 H8 126.0 . . ?
N7 N8 C11 108.0 . . ?
N7 N8 H8 126.0 . . ?
N6 N7 Pb1 120.1(5) . 2_557 ?
N8 N7 Pb1 128.1(5) . 2_557 ?
N8 N7 N6 108.0 . . ?
O6 C10 O5 122.2(15) . . ?
O6 C10 C13 118.0(13) . . ?
O5 C10 C13 119.8(15) . . ?
C7 C6 C8 117.4(7) . . ?
C7 C6 C5 120.0 . . ?
C5 C6 C8 122.6(7) . . ?
C6 C7 H7 120.0 . . ?
C6 C7 C2 120.0 . . ?
C2 C7 H7 120.0 . . ?
C7 C2 C1 123.1(8) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 116.9(8) . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C9 124.2(8) . . ?
C4 C5 C6 120.0 . . ?
C4 C5 C9 115.7(8) . . ?
O3 C9 C5 116.1(12) . . ?
O4 C9 O3 122.0(15) . . ?
O4 C9 C5 121.8(14) . . ?
C12 C13 C10 125.0(9) . . ?
C12 C13 C14 120.0 . . ?
C14 C13 C10 115.0(9) . . ?
C13 C12 C11 121.9(7) . . ?
C17 C12 C11 118.0(7) . . ?
C17 C12 C13 120.0 . . ?
C12 C17 H17 120.0 . . ?
C12 C17 C16 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C16 C15 120.0 . . ?
C17 C16 C18 119.3(8) . . ?
C15 C16 C18 120.7(8) . . ?
C16 C15 H15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C14 C15 H15 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
O1 C1 O2 120.7(14) . . ?
O1 C1 C2 124.6(14) . . ?
O2 C1 C2 114.8(11) . . ?
O8 C18 C16 113.2(12) . . ?
O7 C18 O8 126.4(15) . . ?
O7 C18 C16 120.4(14) . . ?
H9A O9 H9B 107(5) . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 76 21 ' '

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1998758'
loop_
_audit_author_name
_audit_author_address
'Liu Jiao'
;NWU
China
;
_audit_update_record             
;
2020-04-23 deposited with the CCDC.	2020-06-15 downloaded from the CCDC.
;
_audit_creation_date             2020-04-16
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H5 N4 O5 Pb Zn0.5'
_chemical_formula_sum            'C9 H5 N4 O5 Pb Zn0.50'
_chemical_formula_weight         489.04
_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'
Zn Zn 0.2839 1.4301 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_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                   20.796(4)
_cell_length_b                   22.171(4)
_cell_length_c                   6.8392(12)
_cell_angle_alpha                90
_cell_angle_beta                 105.035(5)
_cell_angle_gamma                90
_cell_volume                     3045.4(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9136
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      25.396
_cell_measurement_theta_min      2.737
_shelx_estimated_absorpt_T_max   0.383
_shelx_estimated_absorpt_T_min   0.155
_exptl_absorpt_coefficient_mu    11.868
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1181 before and 0.0907 after correction. The Ratio of minimum to maximum transmission is 0.7540. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0915
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            22431
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.737
_diffrn_ambient_temperature      158.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  ω
_diffrn_measurement_method       ?
_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                2319
_reflns_number_total             2677
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         3.105
_refine_diff_density_min         -3.412
_refine_diff_density_rms         0.311
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2677
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0566
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0731P)²+127.1940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1470
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C3)
Uanis(C6) = Uanis(C4)
Uanis(C7) = Uanis(C6) = Uanis(C5) = Uanis(C4)
Uanis(C8) = Uanis(C5) = Uanis(C3) = Uanis(C6)
3.a Rotating group:
 O5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_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 0.20402(2) 0.79414(2) 0.20756(7) 0.0259(2) Uani 1 1 d . . . . .
Zn1 Zn 0.5000 0.61869(9) 0.2500 0.0185(4) Uani 1 2 d S T P . .
O5 O 0.1107(5) 0.7381(5) -0.0039(15) 0.043(3) Uani 1 1 d . . . . .
H5A H 0.1197 0.7258 -0.1198 0.064 Uiso 1 1 d GR . . . .
H5B H 0.0750 0.7623 -0.0483 0.064 Uiso 1 1 d GR . . . .
O4 O 0.2179(5) 0.6854(4) 0.3896(14) 0.032(2) Uani 1 1 d . . . . .
N3 N 0.4312(6) 0.7478(5) 0.5669(17) 0.029(3) Uani 1 1 d . . . . .
O2 O 0.3559(5) 0.3883(4) 0.4241(15) 0.036(2) Uani 1 1 d . . . . .
N4 N 0.3820(6) 0.7077(5) 0.5631(16) 0.025(2) Uani 1 1 d . . . . .
N2 N 0.4744(5) 0.7266(5) 0.4784(15) 0.025(2) Uani 1 1 d . . . . .
O1 O 0.4473(4) 0.4401(4) 0.5689(14) 0.027(2) Uani 1 1 d . . . . .
N1 N 0.4521(5) 0.6700(4) 0.4038(14) 0.020(2) Uani 1 1 d . . . . .
O3 O 0.2646(6) 0.6969(4) 0.1379(15) 0.039(3) Uani 1 1 d . . . . .
C6 C 0.2510(6) 0.5536(6) 0.2915(17) 0.0226(11) Uani 1 1 d . . . . .
H6 H 0.2041 0.5554 0.2386 0.027 Uiso 1 1 calc R . . . .
C5 C 0.2884(6) 0.6069(6) 0.3318(17) 0.0226(11) Uani 1 1 d . . . . .
C4 C 0.3573(6) 0.6046(6) 0.4165(17) 0.0226(11) Uani 1 1 d . . . . .
C9 C 0.3966(6) 0.6601(5) 0.4607(16) 0.016(2) Uani 1 1 d . . . . .
C8 C 0.2548(6) 0.6664(6) 0.2784(17) 0.0226(11) Uani 1 1 d . . . . .
C7 C 0.2824(6) 0.4987(6) 0.3288(18) 0.0226(11) Uani 1 1 d . . . . .
H7 H 0.2575 0.4625 0.2950 0.027 Uiso 1 1 calc R . . . .
C2 C 0.3513(6) 0.4959(5) 0.4168(17) 0.018(2) Uani 1 1 d . . . . .
C3 C 0.3879(6) 0.5490(6) 0.4619(17) 0.0226(11) Uani 1 1 d . . . . .
H3 H 0.4343 0.5470 0.5244 0.027 Uiso 1 1 calc R . . . .
C1 C 0.3866(6) 0.4356(5) 0.4761(18) 0.022(3) 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
Pb1 O5 2.438(11) . ?
Pb1 O4 2.694(9) . ?
Pb1 O2 2.478(10) 4 ?
Pb1 N4 2.668(10) 7_566 ?
Pb1 O3 2.602(10) . ?
Pb1 O3 2.617(10) 7_565 ?
Zn1 O1 1.931(9) 6_565 ?
Zn1 O1 1.931(9) 5_666 ?
Zn1 N1 1.984(10) . ?
Zn1 N1 1.984(10) 2_655 ?
O4 C8 1.283(15) . ?
N3 N4 1.350(16) . ?
N3 N2 1.295(15) . ?
O2 Pb1 2.478(10) 4_545 ?
O2 C1 1.231(15) . ?
N4 Pb1 2.668(10) 7_566 ?
N4 C9 1.345(15) . ?
N2 N1 1.390(15) . ?
O1 Zn1 1.931(9) 5_666 ?
O1 C1 1.261(15) . ?
N1 C9 1.327(15) . ?
O3 Pb1 2.617(9) 7_565 ?
O3 C8 1.234(15) . ?
C6 C5 1.404(18) . ?
C6 C7 1.374(18) . ?
C5 C4 1.399(17) . ?
C5 C8 1.493(18) . ?
C4 C9 1.466(17) . ?
C4 C3 1.385(17) . ?
C7 C2 1.403(17) . ?
C2 C3 1.391(17) . ?
C2 C1 1.529(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
O5 Pb1 O4 78.0(3) . . ?
O5 Pb1 O2 88.0(3) . 4 ?
O5 Pb1 N4 77.8(3) . 7_566 ?
O5 Pb1 O3 81.4(4) . 7_565 ?
O5 Pb1 O3 79.5(4) . . ?
O2 Pb1 O4 154.8(3) 4 . ?
O2 Pb1 N4 82.9(3) 4 7_566 ?
O2 Pb1 O3 80.1(3) 4 7_565 ?
O2 Pb1 O3 148.6(3) 4 . ?
N4 Pb1 O4 73.9(3) 7_566 . ?
O3 Pb1 O4 49.0(3) . . ?
O3 Pb1 O4 117.6(3) 7_565 . ?
O3 Pb1 N4 153.4(4) 7_565 7_566 ?
O3 Pb1 N4 121.6(3) . 7_566 ?
O3 Pb1 O3 69.6(3) . 7_565 ?
O1 Zn1 O1 95.1(5) 6_565 5_666 ?
O1 Zn1 N1 109.0(4) 5_666 . ?
O1 Zn1 N1 109.0(4) 6_565 2_655 ?
O1 Zn1 N1 116.5(4) 6_565 . ?
O1 Zn1 N1 116.5(4) 5_666 2_655 ?
N1 Zn1 N1 110.1(6) . 2_655 ?
C8 O4 Pb1 91.7(7) . . ?
N2 N3 N4 111.5(10) . . ?
C1 O2 Pb1 175.4(9) . 4_545 ?
N3 N4 Pb1 128.2(8) . 7_566 ?
C9 N4 Pb1 124.8(8) . 7_566 ?
C9 N4 N3 104.8(10) . . ?
N3 N2 N1 107.0(10) . . ?
C1 O1 Zn1 126.7(8) . 5_666 ?
N2 N1 Zn1 123.1(8) . . ?
C9 N1 Zn1 130.9(8) . . ?
C9 N1 N2 105.9(9) . . ?
Pb1 O3 Pb1 110.4(3) . 7_565 ?
C8 O3 Pb1 97.2(8) . . ?
C8 O3 Pb1 151.0(9) . 7_565 ?
C7 C6 C5 119.8(12) . . ?
C6 C5 C8 119.7(11) . . ?
C4 C5 C6 120.3(12) . . ?
C4 C5 C8 119.9(11) . . ?
C5 C4 C9 120.7(11) . . ?
C3 C4 C5 119.2(12) . . ?
C3 C4 C9 120.1(11) . . ?
N4 C9 C4 125.3(11) . . ?
N1 C9 N4 110.7(10) . . ?
N1 C9 C4 124.0(10) . . ?
O4 C8 C5 117.4(10) . . ?
O3 C8 O4 121.7(12) . . ?
O3 C8 C5 120.8(11) . . ?
C6 C7 C2 120.1(12) . . ?
C7 C2 C1 121.2(11) . . ?
C3 C2 C7 119.8(11) . . ?
C3 C2 C1 118.9(10) . . ?
C4 C3 C2 120.6(11) . . ?
O2 C1 O1 126.0(12) . . ?
O2 C1 C2 119.5(11) . . ?
O1 C1 C2 114.4(10) . . ?

_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 -0.036 472 49 ' '
2 0.500 0.000 0.074 472 49 ' '

_olex2_submission_special_instructions 'No special instructions were received'
