# Electronic Supplementary Material (ESI) 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_shelx
_audit_block_doi                 10.5517/ccdc.csd.cc2fr3z9
_database_code_depnum_ccdc_archive 'CCDC 2256551'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1016/j.molstruc.2023.136768 2024
loop_
_audit_author_name
_audit_author_address
'Hema M K'
;university of mysore
India
;
_audit_update_record             
;
2023-04-15 deposited with the CCDC.	2024-01-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H11 Cl2 N5 O Pb, C H4 O'
_chemical_formula_sum            'C13 H15 Cl2 N5 O2 Pb'
_chemical_formula_weight         551.39

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'
Cl Cl 0.1484 0.1585 '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                   8.8359(15)
_cell_length_b                   9.5857(18)
_cell_length_c                   10.325(2)
_cell_angle_alpha                90.933(7)
_cell_angle_beta                 92.085(7)
_cell_angle_gamma                107.286(6)
_cell_volume                     834.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9488
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      28.31

_exptl_crystal_description       needle
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.195
_exptl_crystal_F_000             520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    10.449
_shelx_estimated_absorpt_T_min   0.344
_shelx_estimated_absorpt_T_max   0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7618
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41701
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.974
_diffrn_reflns_theta_max         28.275
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4147
_reflns_number_gt                3929
_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       'APEX3 Software (Bruker, 2019)'
_computing_cell_refinement       'APEX3 Software (Bruker, 2019)'
_computing_data_reduction        'APEX3 Software (Bruker, 2019)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'Diamond (Brandenburg, 1999, Crystal impact GbR)'
_computing_publication_material  'Wingx Version 2018.3 (Farrugia, 2012)'

_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)+(0.0066P)²+0.8906P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4147
_refine_ls_number_parameters     219
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0155
_refine_ls_R_factor_gt           0.0134
_refine_ls_wR_factor_ref         0.0275
_refine_ls_wR_factor_gt          0.0270
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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
Pb Pb 0.07309(2) 0.14903(2) 0.18903(2) 0.01403(3) Uani 1 1 d . . . . .
Cl1 Cl 0.17152(6) 0.17439(5) -0.06376(5) 0.01664(10) Uani 1 1 d . . . . .
Cl2 Cl -0.13023(6) 0.16665(6) 0.42429(5) 0.02310(12) Uani 1 1 d . . . . .
N1 N -0.1488(2) 0.24129(19) 0.08890(17) 0.0143(4) Uani 1 1 d . . . . .
N2 N 0.1189(2) 0.40739(19) 0.20329(17) 0.0145(4) Uani 1 1 d . . . . .
N3 N 0.2642(2) 0.49955(19) 0.25180(17) 0.0147(4) Uani 1 1 d . . . . .
N4 N 0.8130(2) 0.6740(2) 0.43581(18) 0.0205(4) Uani 1 1 d . . . . .
H4A H 0.906(3) 0.724(3) 0.472(3) 0.025 Uiso 1 1 d . U . . .
N5 N 0.0389(2) 0.6183(2) 0.19331(18) 0.0159(4) Uani 1 1 d . . . . .
H5A H -0.019(3) 0.659(3) 0.160(2) 0.019 Uiso 1 1 d . U . . .
H5B H 0.133(3) 0.668(3) 0.222(2) 0.019 Uiso 1 1 d . U . . .
O1 O 0.33464(18) 0.28490(16) 0.27526(16) 0.0208(3) Uani 1 1 d . . . . .
C1 C -0.2792(2) 0.1542(2) 0.0277(2) 0.0166(4) Uani 1 1 d . . . . .
H1 H -0.284268 0.055518 0.009034 0.020 Uiso 1 1 calc R U . . .
C2 C -0.4076(3) 0.2016(2) -0.0098(2) 0.0182(4) Uani 1 1 d . . . . .
H2 H -0.498708 0.136694 -0.053190 0.022 Uiso 1 1 calc R U . . .
C3 C -0.4002(3) 0.3451(2) 0.0174(2) 0.0177(4) Uani 1 1 d . . . . .
H3 H -0.487424 0.379916 -0.005361 0.021 Uiso 1 1 calc R U . . .
C4 C -0.2632(2) 0.4384(2) 0.0785(2) 0.0153(4) Uani 1 1 d . . . . .
H4 H -0.254714 0.538001 0.096756 0.018 Uiso 1 1 calc R U . . .
C5 C -0.1398(2) 0.3825(2) 0.1120(2) 0.0135(4) Uani 1 1 d . . . . .
C6 C 0.0140(2) 0.4744(2) 0.17281(19) 0.0131(4) Uani 1 1 d . . . . .
C7 C 0.3622(2) 0.4238(2) 0.2825(2) 0.0147(4) Uani 1 1 d . . . . .
C8 C 0.5224(2) 0.5145(2) 0.3341(2) 0.0156(4) Uani 1 1 d . . . . .
C9 C 0.5653(3) 0.6667(2) 0.3391(2) 0.0189(5) Uani 1 1 d . . . . .
H9 H 0.493455 0.715851 0.306985 0.023 Uiso 1 1 calc R U . . .
C10 C 0.7125(3) 0.7455(3) 0.3908(2) 0.0218(5) Uani 1 1 d . . . . .
H10 H 0.742735 0.849324 0.394730 0.026 Uiso 1 1 calc R U . . .
C11 C 0.7757(3) 0.5281(3) 0.4310(2) 0.0228(5) Uani 1 1 d . . . . .
H11 H 0.849894 0.481733 0.463706 0.027 Uiso 1 1 calc R U . . .
C12 C 0.6312(3) 0.4448(2) 0.3792(2) 0.0181(4) Uani 1 1 d . . . . .
H12 H 0.605677 0.341284 0.374067 0.022 Uiso 1 1 calc R U . . .
O2 O 0.7214(3) 0.1048(3) 0.6994(2) 0.0601(7) Uani 1 1 d . . . . .
H2A H 0.764757 0.124065 0.628157 0.090 Uiso 1 1 calc R U . . .
C13 C 0.5711(3) 0.0026(3) 0.6789(3) 0.0337(6) Uani 1 1 d . . . . .
H13A H 0.531767 -0.038231 0.761882 0.051 Uiso 1 1 calc R U . . .
H13B H 0.578832 -0.076181 0.620234 0.051 Uiso 1 1 calc R U . . .
H13C H 0.497688 0.050875 0.640119 0.051 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
Pb N2 2.3889(18) . ?
Pb O1 2.4194(15) . ?
Pb N1 2.5702(17) . ?
Pb Cl1 2.7727(7) . ?
Pb Cl2 3.1050(7) . ?
Pb Pb 4.7058(8) 2 ?
N1 C1 1.335(3) . ?
N1 C5 1.349(3) . ?
N2 C6 1.308(3) . ?
N2 N3 1.395(2) . ?
N3 C7 1.318(3) . ?
N4 C11 1.338(3) . ?
N4 C10 1.348(3) . ?
N4 H4A 0.89(3) . ?
N5 C6 1.343(3) . ?
N5 H5A 0.80(3) . ?
N5 H5B 0.87(3) . ?
O1 C7 1.281(3) . ?
C1 C2 1.387(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.382(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.395(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.492(3) . ?
C7 C8 1.498(3) . ?
C8 C9 1.393(3) . ?
C8 C12 1.395(3) . ?
C9 C10 1.378(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.373(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
O2 C13 1.403(3) . ?
O2 H2A 0.8400 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 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
N2 Pb O1 65.79(6) . . ?
N2 Pb N1 64.47(6) . . ?
O1 Pb N1 129.89(5) . . ?
N2 Pb Cl1 89.66(4) . . ?
O1 Pb Cl1 92.20(4) . . ?
N1 Pb Cl1 81.85(4) . . ?
N2 Pb Cl2 80.49(4) . . ?
O1 Pb Cl2 100.66(4) . . ?
N1 Pb Cl2 76.94(4) . . ?
Cl1 Pb Cl2 158.773(16) . . ?
N2 Pb Pb 126.27(4) . 2 ?
O1 Pb Pb 129.39(4) . 2 ?
N1 Pb Pb 78.57(4) . 2 ?
Cl1 Pb Pb 45.799(14) . 2 ?
Cl2 Pb Pb 128.629(15) . 2 ?
C1 N1 C5 118.50(18) . . ?
C1 N1 Pb 123.57(13) . . ?
C5 N1 Pb 117.53(13) . . ?
C6 N2 N3 114.34(17) . . ?
C6 N2 Pb 125.06(14) . . ?
N3 N2 Pb 120.55(12) . . ?
C7 N3 N2 110.68(17) . . ?
C11 N4 C10 122.3(2) . . ?
C11 N4 H4A 117.9(17) . . ?
C10 N4 H4A 119.8(17) . . ?
C6 N5 H5A 121.1(19) . . ?
C6 N5 H5B 116.4(17) . . ?
H5A N5 H5B 120(2) . . ?
C7 O1 Pb 115.20(13) . . ?
N1 C1 C2 122.86(19) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 118.6(2) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 119.3(2) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 118.47(19) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
N1 C5 C4 122.28(19) . . ?
N1 C5 C6 115.01(18) . . ?
C4 C5 C6 122.69(19) . . ?
N2 C6 N5 123.45(19) . . ?
N2 C6 C5 116.63(18) . . ?
N5 C6 C5 119.92(18) . . ?
O1 C7 N3 127.75(19) . . ?
O1 C7 C8 117.93(18) . . ?
N3 C7 C8 114.30(18) . . ?
C9 C8 C12 119.1(2) . . ?
C9 C8 C7 121.75(19) . . ?
C12 C8 C7 119.10(19) . . ?
C10 C9 C8 119.7(2) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
N4 C10 C9 119.4(2) . . ?
N4 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
N4 C11 C12 120.5(2) . . ?
N4 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C8 119.0(2) . . ?
C11 C12 H12 120.5 . . ?
C8 C12 H12 120.5 . . ?
C13 O2 H2A 109.5 . . ?
O2 C13 H13A 109.5 . . ?
O2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 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
C6 N2 N3 C7 178.77(18) . . . . ?
Pb N2 N3 C7 1.2(2) . . . . ?
C5 N1 C1 C2 -1.9(3) . . . . ?
Pb N1 C1 C2 170.71(16) . . . . ?
N1 C1 C2 C3 0.0(3) . . . . ?
C1 C2 C3 C4 1.5(3) . . . . ?
C2 C3 C4 C5 -1.1(3) . . . . ?
C1 N1 C5 C4 2.3(3) . . . . ?
Pb N1 C5 C4 -170.74(15) . . . . ?
C1 N1 C5 C6 -176.13(18) . . . . ?
Pb N1 C5 C6 10.8(2) . . . . ?
C3 C4 C5 N1 -0.8(3) . . . . ?
C3 C4 C5 C6 177.51(19) . . . . ?
N3 N2 C6 N5 -3.9(3) . . . . ?
Pb N2 C6 N5 173.57(15) . . . . ?
N3 N2 C6 C5 175.93(17) . . . . ?
Pb N2 C6 C5 -6.6(3) . . . . ?
N1 C5 C6 N2 -3.6(3) . . . . ?
C4 C5 C6 N2 177.98(19) . . . . ?
N1 C5 C6 N5 176.28(19) . . . . ?
C4 C5 C6 N5 -2.2(3) . . . . ?
Pb O1 C7 N3 1.8(3) . . . . ?
Pb O1 C7 C8 -179.50(14) . . . . ?
N2 N3 C7 O1 -2.0(3) . . . . ?
N2 N3 C7 C8 179.27(17) . . . . ?
O1 C7 C8 C9 176.7(2) . . . . ?
N3 C7 C8 C9 -4.5(3) . . . . ?
O1 C7 C8 C12 -3.8(3) . . . . ?
N3 C7 C8 C12 175.01(19) . . . . ?
C12 C8 C9 C10 -1.4(3) . . . . ?
C7 C8 C9 C10 178.1(2) . . . . ?
C11 N4 C10 C9 0.7(3) . . . . ?
C8 C9 C10 N4 0.1(3) . . . . ?
C10 N4 C11 C12 0.0(3) . . . . ?
N4 C11 C12 C8 -1.3(3) . . . . ?
C9 C8 C12 C11 2.0(3) . . . . ?
C7 C8 C12 C11 -177.5(2) . . . . ?

_refine_diff_density_max         0.578
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.086

