# Supplementary Information (SI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_Pb1
_database_code_depnum_ccdc_archive 'CCDC 2360850'
loop_
_audit_author_name
_audit_author_address
'Yuan-Chun He'
;Qufu Normal University
China
;
_audit_update_record             
;
2024-07-26 deposited with the CCDC.	2024-08-02 downloaded from the CCDC.
;
_audit_creation_date             2024-07-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H4 N22 O2 Pb3'
_chemical_formula_sum            'C8 H4 N22 O2 Pb3'
_chemical_formula_weight         1061.90
_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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   7.3616(4)
_cell_length_b                   14.2632(6)
_cell_length_c                   19.3471(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2031.44(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5418
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      31.99
_cell_measurement_theta_min      2.86
_shelx_estimated_absorpt_T_max   0.182
_shelx_estimated_absorpt_T_min   0.118
_exptl_absorpt_coefficient_mu    24.867
_exptl_absorpt_correction_T_max  0.0725
_exptl_absorpt_correction_T_min  0.0228
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1482 before and 0.0636 after correction.
The Ratio of minimum to maximum transmission is 0.3145.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.472
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 -1.00 0.0070
1.00 0.00 0.00 0.0020
1.00 -1.00 -1.00 0.0290
-1.00 -1.00 1.00 0.1120
-1.00 0.00 -1.00 0.0920
-1.00 1.00 -1.00 0.0710
-1.00 1.00 1.00 0.1050
0.00 1.00 0.00 0.0350
0.00 -1.00 -1.00 0.0350
1.00 0.00 1.00 0.0510
1.00 -1.00 0.00 0.0370
0.00 -1.00 1.00 0.0780
-1.00 0.00 1.00 0.1560
0.00 0.00 1.00 0.0860

_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.104
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20783
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.105
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1315
_reflns_number_total             1785
_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       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         3.452
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.322
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         1785
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0523
_refine_ls_restrained_S_all      1.103
_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)+(0.0702P)²+119.9979P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1696
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Pb2-N9 \\sim Pb3-N9
 with sigma of 0.02
 Pb2-N8 \\sim Pb3-N8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Pb3) = Uanis(Pb2)
4. Others
 Sof(Pb3)=0.5*(1-FVAR(2))
 Sof(Pb2)=0.5*FVAR(2)
5.a Free rotating group:
 O1W(H1WA,H1WB)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.08251(11) 0.41354(5) 0.59274(3) 0.0347(3) Uani 1 1 d . . . . .
N1 N 0.179(2) 0.2435(11) 0.5573(8) 0.035(4) Uani 1 1 d . . . . .
C1 C 0.249(3) 0.2330(11) 0.4932(7) 0.024(4) Uani 1 1 d . . . . .
Pb2 Pb 0.0977(5) 0.42709(14) 0.22476(11) 0.0214(6) Uani 0.356(3) 1 d D . P A 1
N2 N 0.211(2) 0.1605(10) 0.5904(8) 0.038(4) Uani 1 1 d . . . . .
C2 C 0.236(3) 0.3061(13) 0.4413(9) 0.030(4) Uani 1 1 d . . . . .
Pb3 Pb 0.1799(11) 0.4347(4) 0.2278(3) 0.0214(6) Uani 0.144(3) 1 d D . P A 2
N3 N 0.289(2) 0.1023(11) 0.5447(9) 0.042(4) Uani 1 1 d . . . . .
C3 C 0.240(3) 0.3109(12) 0.3713(9) 0.032(4) Uani 1 1 d . . . . .
N4 N 0.319(2) 0.1456(11) 0.4849(8) 0.036(4) Uani 1 1 d . . . . .
C4 C 0.257(3) 0.2379(13) 0.3167(8) 0.031(4) Uani 1 1 d . . . . .
N5 N 0.325(3) 0.1534(11) 0.3251(8) 0.038(4) Uani 1 1 d . . . . .
N6 N 0.319(3) 0.1127(12) 0.2611(8) 0.046(5) Uani 1 1 d . . . . .
N7 N 0.240(3) 0.1690(12) 0.2193(9) 0.052(5) Uani 1 1 d . . . . .
N8 N 0.204(3) 0.2559(12) 0.2527(9) 0.051(5) Uani 1 1 d D . . . .
N9 N 0.197(3) 0.3969(12) 0.3518(8) 0.045(4) Uani 1 1 d D . . . .
N10 N 0.187(3) 0.4491(12) 0.4091(8) 0.044(4) Uani 1 1 d . . . . .
N11 N 0.204(2) 0.3958(10) 0.4641(8) 0.035(4) Uani 1 1 d . . . . .
O1W O 0.468(3) 0.4378(18) 0.6048(12) 0.084(6) Uani 1 1 d G . . . .
H1WA H 0.475826 0.461480 0.645055 0.127 Uiso 1 1 d G U . . .
H1WB H 0.462488 0.379037 0.611750 0.127 Uiso 1 1 d G 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 N1 2.617(16) . ?
Pb1 N4 2.592(15) 4_456 ?
Pb1 N5 2.652(17) 4_456 ?
Pb1 N10 2.789(18) 5_566 ?
Pb1 N11 2.656(15) . ?
N1 C1 1.35(2) . ?
N1 N2 1.37(2) . ?
C1 C2 1.45(2) . ?
C1 N4 1.36(2) . ?
Pb2 N8 2.620(17) . ?
Pb2 N9 2.601(16) . ?
N2 N3 1.34(2) . ?
C2 C3 1.36(3) . ?
C2 N11 1.37(2) . ?
Pb3 N6 2.618(18) 8_665 ?
Pb3 N8 2.602(18) . ?
Pb3 N9 2.462(17) . ?
N3 N4 1.33(2) . ?
C3 C4 1.49(3) . ?
C3 N9 1.32(2) . ?
C4 N5 1.31(2) . ?
C4 N8 1.32(2) . ?
N5 N6 1.37(2) . ?
N6 N7 1.28(2) . ?
N7 N8 1.42(2) . ?
N9 N10 1.34(2) . ?
N10 N11 1.31(2) . ?
O1W H1WA 0.8503 . ?
O1W H1WB 0.8501 . ?

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
N1 Pb1 N5 91.0(5) . 4_456 ?
N1 Pb1 N10 147.1(5) . 5_566 ?
N1 Pb1 N11 64.9(4) . . ?
N4 Pb1 N1 75.5(5) 4_456 . ?
N4 Pb1 N5 72.3(5) 4_456 4_456 ?
N4 Pb1 N10 71.9(5) 4_456 5_566 ?
N4 Pb1 N11 71.1(5) 4_456 . ?
N5 Pb1 N10 75.6(5) 4_456 5_566 ?
N5 Pb1 N11 140.1(5) 4_456 . ?
N11 Pb1 N10 107.1(5) . 5_566 ?
C1 N1 Pb1 116.5(11) . . ?
C1 N1 N2 105.5(14) . . ?
N2 N1 Pb1 136.7(11) . . ?
N1 C1 C2 122.0(16) . . ?
N1 C1 N4 110.8(14) . . ?
N4 C1 C2 127.1(15) . . ?
N9 Pb2 N8 64.3(5) . . ?
N3 N2 N1 107.5(13) . . ?
C3 C2 C1 136.6(17) . . ?
C3 C2 N11 106.1(16) . . ?
N11 C2 C1 117.3(15) . . ?
N8 Pb3 N6 154.8(6) . 8_665 ?
N9 Pb3 N6 88.4(6) . 8_665 ?
N9 Pb3 N8 66.5(6) . . ?
N4 N3 N2 111.0(14) . . ?
C2 C3 C4 132.4(16) . . ?
N9 C3 C2 109.1(17) . . ?
N9 C3 C4 117.9(16) . . ?
C1 N4 Pb1 130.7(12) . 4_556 ?
N3 N4 Pb1 118.5(12) . 4_556 ?
N3 N4 C1 105.1(14) . . ?
N5 C4 C3 125.9(15) . . ?
N5 C4 N8 113.9(16) . . ?
N8 C4 C3 120.1(16) . . ?
C4 N5 Pb1 132.5(12) . 4_556 ?
C4 N5 N6 105.3(15) . . ?
N6 N5 Pb1 114.4(12) . 4_556 ?
N5 N6 Pb3 129.3(12) . 8_655 ?
N7 N6 Pb3 117.1(12) . 8_655 ?
N7 N6 N5 108.7(16) . . ?
N6 N7 N8 110.2(16) . . ?
C4 N8 Pb2 117.5(12) . . ?
C4 N8 Pb3 112.6(12) . . ?
C4 N8 N7 101.6(15) . . ?
N7 N8 Pb2 140.6(12) . . ?
N7 N8 Pb3 141.5(12) . . ?
C3 N9 Pb2 119.3(13) . . ?
C3 N9 Pb3 119.6(13) . . ?
C3 N9 N10 107.1(16) . . ?
N10 N9 Pb2 132.5(12) . . ?
N10 N9 Pb3 133.1(12) . . ?
N9 N10 Pb1 114.8(13) . 5_566 ?
N11 N10 Pb1 118.9(12) . 5_566 ?
N11 N10 N9 110.1(15) . . ?
C2 N11 Pb1 116.6(11) . . ?
N10 N11 Pb1 132.3(12) . . ?
N10 N11 C2 107.2(15) . . ?
H1WA O1W H1WB 104.5 . . ?

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
Pb1 N1 C1 C2 -13(2) . . . . ?
Pb1 N1 C1 N4 170.4(12) . . . . ?
Pb1 N1 N2 N3 -168.6(14) . . . . ?
Pb1 N5 N6 Pb3 49(2) 4_556 . . 8_655 ?
Pb1 N5 N6 N7 -157.6(15) 4_556 . . . ?
Pb1 N10 N11 Pb1 -17(2) 5_566 . . . ?
Pb1 N10 N11 C2 138.8(13) 5_566 . . . ?
N1 C1 C2 C3 -156(2) . . . . ?
N1 C1 C2 N11 20(3) . . . . ?
N1 C1 N4 Pb1 -151.2(13) . . . 4_556 ?
N1 C1 N4 N3 1(2) . . . . ?
N1 N2 N3 N4 4(2) . . . . ?
C1 N1 N2 N3 -3(2) . . . . ?
C1 C2 C3 C4 1(4) . . . . ?
C1 C2 C3 N9 172(2) . . . . ?
C1 C2 N11 Pb1 -16(2) . . . . ?
C1 C2 N11 N10 -176.7(18) . . . . ?
Pb2 N9 N10 Pb1 24(2) . . . 5_566 ?
Pb2 N9 N10 N11 161.0(14) . . . . ?
N2 N1 C1 C2 177.9(17) . . . . ?
N2 N1 C1 N4 1(2) . . . . ?
N2 N3 N4 Pb1 153.4(13) . . . 4_556 ?
N2 N3 N4 C1 -3(2) . . . . ?
C2 C1 N4 Pb1 32(3) . . . 4_556 ?
C2 C1 N4 N3 -175.6(19) . . . . ?
C2 C3 C4 N5 -21(4) . . . . ?
C2 C3 C4 N8 160(2) . . . . ?
C2 C3 N9 Pb2 -162.5(14) . . . . ?
C2 C3 N9 Pb3 -178.2(14) . . . . ?
C2 C3 N9 N10 7(3) . . . . ?
Pb3 N6 N7 N8 163.2(14) 8_655 . . . ?
Pb3 N9 N10 Pb1 42(2) . . . 5_566 ?
Pb3 N9 N10 N11 179.7(14) . . . . ?
C3 C2 N11 Pb1 161.3(13) . . . . ?
C3 C2 N11 N10 1(2) . . . . ?
C3 C4 N5 Pb1 -32(3) . . . 4_556 ?
C3 C4 N5 N6 -178.2(19) . . . . ?
C3 C4 N8 Pb2 6(3) . . . . ?
C3 C4 N8 Pb3 20(2) . . . . ?
C3 C4 N8 N7 -178.6(18) . . . . ?
C3 N9 N10 Pb1 -143.8(14) . . . 5_566 ?
C3 N9 N10 N11 -6(2) . . . . ?
N4 C1 C2 C3 20(4) . . . . ?
N4 C1 C2 N11 -163.7(19) . . . . ?
C4 C3 N9 Pb2 10(3) . . . . ?
C4 C3 N9 Pb3 -6(3) . . . . ?
C4 C3 N9 N10 179.3(18) . . . . ?
C4 N5 N6 Pb3 -158.1(15) . . . 8_655 ?
C4 N5 N6 N7 -4(2) . . . . ?
N5 C4 N8 Pb2 -173.7(14) . . . . ?
N5 C4 N8 Pb3 -159.7(14) . . . . ?
N5 C4 N8 N7 2(3) . . . . ?
N5 N6 N7 N8 6(3) . . . . ?
N6 N7 N8 Pb2 169.3(18) . . . . ?
N6 N7 N8 Pb3 147.6(19) . . . . ?
N6 N7 N8 C4 -5(3) . . . . ?
N8 C4 N5 Pb1 147.5(16) . . . 4_556 ?
N8 C4 N5 N6 1(3) . . . . ?
N9 C3 C4 N5 169(2) . . . . ?
N9 C3 C4 N8 -11(3) . . . . ?
N9 N10 N11 Pb1 -152.7(14) . . . . ?
N9 N10 N11 C2 3(2) . . . . ?
N11 C2 C3 C4 -176(2) . . . . ?
N11 C2 C3 N9 -5(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT420_Pb1                 
;
PROBLEM: D-H Bond Without Acceptor  O1W      --H1WA     .     Please Check 
RESPONSE: There is no suitable hydrogen bond for  H1WA and H1Wb.
;
_vrf_PLAT971_Pb1                 
;
PROBLEM: Check Calcd Resid. Dens.  0.50Ang From Pb2             3.21 eA-3  
RESPONSE: It is because of the heavy atom effect of lead ions. 
;
# end Validation Reply Form

####################################################################### 
# 
# 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_Pb2
_database_code_depnum_ccdc_archive 'CCDC 2360851'
loop_
_audit_author_name
_audit_author_address
'Yuan-Chun He'
;Qufu Normal University
China
;
_audit_update_record             
;
2024-07-26 deposited with the CCDC.	2024-08-02 downloaded from the CCDC.
;
_audit_creation_date             2024-07-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C8 H4 N22 Pb, 3(H2 O)'
_chemical_formula_sum            'C8 H10 N22 O3 Pb'
_chemical_formula_weight         669.57
_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      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                   11.0514(6)
_cell_length_b                   8.2260(6)
_cell_length_c                   19.8646(12)
_cell_angle_alpha                90
_cell_angle_beta                 90.055(2)
_cell_angle_gamma                90
_cell_volume                     1805.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9285
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      31.02
_cell_measurement_theta_min      3.09
_shelx_estimated_absorpt_T_max   0.602
_shelx_estimated_absorpt_T_min   0.332
_exptl_absorpt_coefficient_mu    9.420
_exptl_absorpt_correction_T_max  0.4334
_exptl_absorpt_correction_T_min  0.2769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0811 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.6389.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.463
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9891
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.015
_diffrn_reflns_theta_min         3.087
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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                   ?
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1559
_reflns_number_total             1591
_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       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         3.042
_refine_diff_density_min         -2.041
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       0.00064(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         1591
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0384
_refine_ls_restrained_S_all      1.219
_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)+(0.0364P)²+58.2765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.0985
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N5) = Uanis(C2)
3. Others
 Fixed Sof: H2A(0.5) H2B(0.5)
4.a Free rotating group:
 O1(H1A,H1B,O2,H2A,H2B)
4.b Aromatic/amide H refined with riding coordinates:
 N7(H7), N11(H11)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 0.53140(6) 0.250000 0.0206(2) Uani 1 2 d S T P . .
N1 N 0.3714(7) 0.2954(11) 0.2920(4) 0.0308(19) Uani 1 1 d . . . . .
C1 C 0.3686(8) 0.2280(11) 0.3539(4) 0.0245(19) Uani 1 1 d . . . . .
N2 N 0.2798(8) 0.2314(11) 0.2582(4) 0.036(2) Uani 1 1 d . . . . .
C2 C 0.4615(13) 0.2868(16) 0.4007(6) 0.051(2) Uani 1 1 d . . . . .
N3 N 0.2222(8) 0.1288(11) 0.2970(4) 0.035(2) Uani 1 1 d . . . . .
C3 C 0.4828(11) 0.2562(15) 0.4688(6) 0.046(3) Uani 1 1 d . . . . .
C4 C 0.4138(9) 0.1506(12) 0.5172(5) 0.029(2) Uani 1 1 d . . . . .
N4 N 0.2771(8) 0.1258(11) 0.3579(4) 0.036(2) Uani 1 1 d . . . . .
N5 N 0.5547(10) 0.3963(13) 0.3784(5) 0.051(2) Uani 1 1 d . . . . .
N6 N 0.6103(12) 0.4093(15) 0.4322(5) 0.063(3) Uani 1 1 d . . . . .
N7 N 0.5914(10) 0.3500(13) 0.4866(5) 0.053(3) Uani 1 1 d . . . . .
H7 H 0.629579 0.359546 0.524106 0.064 Uiso 1 1 calc R U . . .
N8 N 0.4583(8) 0.1436(10) 0.5800(4) 0.0302(18) Uani 1 1 d . . . . .
N9 N 0.3864(7) 0.0473(10) 0.6161(4) 0.0277(18) Uani 1 1 d . . . . .
N10 N 0.3016(8) -0.0033(10) 0.5761(4) 0.0313(19) Uani 1 1 d . . . . .
N11 N 0.3194(9) 0.0608(11) 0.5136(4) 0.040(2) Uani 1 1 d . . . . .
H11 H 0.275576 0.044051 0.478496 0.048 Uiso 1 1 calc R U . . .
O1 O 0.6359(6) 0.3080(9) 0.6442(3) 0.0305(15) Uani 1 1 d G . . . .
H1A H 0.577232 0.273421 0.620509 0.046 Uiso 1 1 d G U . . .
H1B H 0.654750 0.398475 0.626412 0.046 Uiso 1 1 d G U . . .
O2 O 0.50(2) 0.1079(15) 0.750(8) 0.052(3) Uani 1 2 d G T P . .
H2A H 0.451966 0.056200 0.720974 0.078 Uiso 0.5 1 d G U P . .
H2B H 0.552553 0.043348 0.758729 0.078 Uiso 0.5 1 d G U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N1 2.547(8) 2_655 ?
Pb1 N1 2.547(8) . ?
Pb1 N3 2.746(8) 3 ?
Pb1 N3 2.746(8) 4 ?
N1 C1 1.349(12) . ?
N1 N2 1.323(11) . ?
C1 C2 1.466(16) . ?
C1 N4 1.317(13) . ?
N2 N3 1.308(12) . ?
C2 C3 1.397(17) . ?
C2 N5 1.438(18) . ?
N3 N4 1.353(12) . ?
C3 C4 1.503(16) . ?
C3 N7 1.470(17) . ?
C4 N8 1.341(13) . ?
C4 N11 1.280(14) . ?
N5 N6 1.236(14) . ?
N6 N7 1.203(14) . ?
N7 H7 0.8600 . ?
N8 N9 1.332(11) . ?
N9 N10 1.298(11) . ?
N10 N11 1.362(12) . ?
N11 H11 0.8600 . ?
O1 H1A 0.8503 . ?
O1 H1B 0.8500 . ?
O2 H2A 0.8922 . ?
O2 H2A 0.9(5) 2_656 ?
O2 H2B 0.8(4) 2_656 ?
O2 H2B 0.8047 . ?

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
N1 Pb1 N1 80.7(4) 2_655 . ?
N1 Pb1 N3 127.6(3) 2_655 4 ?
N1 Pb1 N3 80.5(3) 2_655 3 ?
N1 Pb1 N3 80.5(3) . 4 ?
N1 Pb1 N3 127.6(3) . 3 ?
N3 Pb1 N3 146.1(4) 3 4 ?
C1 N1 Pb1 128.7(6) . . ?
N2 N1 Pb1 124.4(6) . . ?
N2 N1 C1 106.3(8) . . ?
N1 C1 C2 115.2(9) . . ?
N4 C1 N1 109.6(8) . . ?
N4 C1 C2 135.2(9) . . ?
N3 N2 N1 109.3(7) . . ?
C3 C2 C1 132.2(12) . . ?
C3 C2 N5 106.9(11) . . ?
N5 C2 C1 120.9(10) . . ?
N2 N3 Pb1 115.0(6) . 3_445 ?
N2 N3 N4 108.7(8) . . ?
N4 N3 Pb1 134.3(6) . 3_445 ?
C2 C3 C4 129.7(11) . . ?
C2 C3 N7 105.9(11) . . ?
N7 C3 C4 124.4(10) . . ?
N8 C4 C3 115.7(9) . . ?
N11 C4 C3 135.4(10) . . ?
N11 C4 N8 108.9(8) . . ?
C1 N4 N3 106.2(8) . . ?
N6 N5 C2 98.3(11) . . ?
N7 N6 N5 130.8(15) . . ?
C3 N7 H7 131.0 . . ?
N6 N7 C3 98.0(11) . . ?
N6 N7 H7 131.0 . . ?
N9 N8 C4 108.0(8) . . ?
N10 N9 N8 106.9(8) . . ?
N9 N10 N11 109.2(8) . . ?
C4 N11 N10 107.0(8) . . ?
C4 N11 H11 126.5 . . ?
N10 N11 H11 126.5 . . ?
H1A O1 H1B 104.4 . . ?
H2A O2 H2A 123.0 . 2_656 ?
H2A O2 H2B 28.0 . 2_656 ?
H2A O2 H2B 104.7 2_656 2_656 ?
H2A O2 H2B 104.7 . . ?
H2B O2 H2A 28.1 . 2_656 ?
H2B O2 H2B 97.6 . 2_656 ?

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
Pb1 N1 C1 C2 -7.6(13) . . . . ?
Pb1 N1 C1 N4 170.4(6) . . . . ?
Pb1 N1 N2 N3 -171.1(6) . . . . ?
Pb1 N3 N4 C1 -163.1(7) 3_445 . . . ?
N1 C1 C2 C3 174.9(13) . . . . ?
N1 C1 C2 N5 -5.8(15) . . . . ?
N1 C1 N4 N3 0.4(11) . . . . ?
N1 N2 N3 Pb1 166.7(6) . . . 3_445 ?
N1 N2 N3 N4 0.2(12) . . . . ?
C1 N1 N2 N3 0.0(11) . . . . ?
C1 C2 C3 C4 -1(2) . . . . ?
C1 C2 C3 N7 179.2(12) . . . . ?
C1 C2 N5 N6 -179.0(11) . . . . ?
N2 N1 C1 C2 -178.2(9) . . . . ?
N2 N1 C1 N4 -0.3(11) . . . . ?
N2 N3 N4 C1 -0.4(11) . . . . ?
C2 C1 N4 N3 177.8(12) . . . . ?
C2 C3 C4 N8 178.9(12) . . . . ?
C2 C3 C4 N11 -1(2) . . . . ?
C2 C3 N7 N6 -0.2(12) . . . . ?
C2 N5 N6 N7 -0.8(17) . . . . ?
C3 C2 N5 N6 0.4(13) . . . . ?
C3 C4 N8 N9 179.3(9) . . . . ?
C3 C4 N11 N10 -179.4(11) . . . . ?
C4 C3 N7 N6 179.6(11) . . . . ?
C4 N8 N9 N10 0.5(10) . . . . ?
N4 C1 C2 C3 -2(2) . . . . ?
N4 C1 C2 N5 176.9(11) . . . . ?
N5 C2 C3 C4 -179.9(11) . . . . ?
N5 C2 C3 N7 -0.2(13) . . . . ?
N5 N6 N7 C3 0.7(17) . . . . ?
N7 C3 C4 N8 -0.8(16) . . . . ?
N7 C3 C4 N11 179.7(11) . . . . ?
N8 C4 N11 N10 1.1(11) . . . . ?
N8 N9 N10 N11 0.2(10) . . . . ?
N9 N10 N11 C4 -0.8(11) . . . . ?
N11 C4 N8 N9 -1.0(11) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT780_Pb2                 
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do !  
RESPONSE: We tried to use "move"  O1 to coordinate with Pb1, but failed. It may be because of 
the difference between SHELXL and Platon. 
;
_vrf_PLAT971_Pb2                 
;
PROBLEM: Check Calcd Resid. Dens.  1.51Ang From N4              2.79 eA-3  
RESPONSE: It may be because of heavy atom effect and twin crystal. 
;
# end Validation Reply Form

