# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_YY_3_a
_database_code_depnum_ccdc_archive 'CCDC 2104203'
loop_
_audit_author_name
_audit_author_address
'Yuangang Xu'
;Nanjing University of Science and Technology
China
;
_audit_update_record             
;
2021-09-28 deposited with the CCDC.	2022-03-08 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         'H4 N20 O4 Pb4'
_chemical_formula_sum            'H4 N20 O4 Pb4'
_chemical_formula_weight         1176.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   7.6556(10)
_cell_length_b                   13.6507(17)
_cell_length_c                   8.5962(11)
_cell_angle_alpha                90
_cell_angle_beta                 106.440(4)
_cell_angle_gamma                90
_cell_volume                     861.61(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6056
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      30.23

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.537
_exptl_crystal_F_000             1008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    39.026
_shelx_estimated_absorpt_T_min   0.387
_shelx_estimated_absorpt_T_max   0.387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4065
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source.type              microfocus
_diffrn_radiation_type           MoK\a
_diffrn_source.source            'Ius 2.0'
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            9072
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.470
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_full        24.993
_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 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3013
_reflns_number_gt                2850
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.897
_reflns_Friedel_fraction_max     0.985
_reflns_Friedel_fraction_full    0.985

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0354P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3013
_refine_ls_number_parameters     254
_refine_ls_number_restraints     41
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0302
_refine_ls_wR_factor_ref         0.0672
_refine_ls_wR_factor_gt          0.0659
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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
Pb1 Pb 0.78330(12) 0.62502(6) 0.50629(9) 0.0244(2) Uani 1 1 d . . . . .
Pb2 Pb 0.94024(12) 0.40915(5) 0.80611(9) 0.0251(2) Uani 1 1 d . . . . .
Pb3 Pb 0.56478(11) 0.57787(6) 0.84131(10) 0.0261(2) Uani 1 1 d . . . . .
Pb4 Pb 1.04856(12) 0.66947(6) 0.95281(9) 0.0262(2) Uani 1 1 d . . . . .
O1 O 0.684(2) 0.4953(10) 0.6447(16) 0.024(3) Uani 1 1 d . . . . .
H1 H 0.600254 0.455301 0.597380 0.036 Uiso 1 1 d R U . . .
O2 O 0.756(2) 0.6877(10) 0.7621(16) 0.023(3) Uani 1 1 d . . . . .
H2 H 0.740310 0.742912 0.714063 0.035 Uiso 1 1 d R U . . .
O3 O 0.8636(18) 0.5376(10) 0.9777(15) 0.020(3) Uani 1 1 d . . . . .
H3 H 0.831273 0.499596 1.042238 0.030 Uiso 1 1 d R U . . .
O4 O 1.0392(18) 0.5639(10) 0.7341(16) 0.021(3) Uani 1 1 d . . . . .
H4 H 1.097944 0.550980 0.667212 0.031 Uiso 1 1 d R U . . .
N1 N 0.958(3) 0.3791(13) 0.499(2) 0.028(4) Uani 1 1 d . . . . .
N2 N 0.898(3) 0.4515(13) 0.404(2) 0.027(4) Uani 1 1 d . . . . .
N3 N 0.891(3) 0.4232(14) 0.258(2) 0.032(5) Uani 1 1 d . . . . .
N4 N 0.941(3) 0.3295(15) 0.264(2) 0.036(5) Uani 1 1 d . . . . .
N5 N 0.991(3) 0.3050(14) 0.416(2) 0.032(5) Uani 1 1 d . . . . .
N6 N 0.461(3) 0.4410(17) 0.320(3) 0.046(6) Uani 1 1 d . . . . .
N7 N 0.335(3) 0.3884(13) 0.220(2) 0.032(5) Uani 1 1 d . . . . .
N8 N 0.253(3) 0.4425(16) 0.097(2) 0.039(5) Uani 1 1 d . . . . .
N9 N 0.335(3) 0.5260(15) 0.121(3) 0.045(6) Uani 1 1 d . . . . .
N10 N 0.459(3) 0.5257(15) 0.253(2) 0.037(5) Uani 1 1 d . . . . .
N11 N 0.403(5) 0.366(2) 0.802(3) 0.069(8) Uani 1 1 d . . . . .
N12 N 0.560(5) 0.352(2) 0.898(4) 0.073(9) Uani 1 1 d . . . . .
N13 N 0.565(3) 0.2685(19) 0.975(3) 0.054(7) Uani 1 1 d . . . . .
N14 N 0.397(4) 0.2361(17) 0.927(3) 0.056(7) Uani 1 1 d . . . . .
N15 N 0.295(3) 0.294(3) 0.823(3) 0.076(10) Uani 1 1 d . . . . .
N16 N 0.389(4) 0.724(2) 0.444(4) 0.069(5) Uani 1 1 d . U . . .
N17 N 0.374(4) 0.656(2) 0.546(3) 0.066(5) Uani 1 1 d . U . . .
N18 N 0.216(4) 0.614(2) 0.488(3) 0.067(5) Uani 1 1 d . U . . .
N19 N 0.131(4) 0.660(2) 0.349(3) 0.076(6) Uani 1 1 d . U . . .
N20 N 0.245(5) 0.725(2) 0.328(3) 0.071(5) Uani 1 1 d . 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 O1 2.377(15) . ?
Pb1 O2 2.422(13) . ?
Pb1 O4 2.489(13) . ?
Pb1 N2 2.759(17) . ?
Pb2 O1 2.372(14) . ?
Pb2 O4 2.384(14) . ?
Pb2 O3 2.466(13) . ?
Pb2 N1 2.715(19) . ?
Pb3 O3 2.322(13) . ?
Pb3 O2 2.331(14) . ?
Pb3 O1 2.414(14) . ?
Pb3 N17 2.76(3) . ?
Pb4 O3 2.338(14) . ?
Pb4 O4 2.354(14) . ?
Pb4 O2 2.382(14) . ?
O1 H1 0.8506 . ?
O2 H2 0.8509 . ?
O3 H3 0.8456 . ?
O4 H4 0.8425 . ?
N1 N2 1.28(2) . ?
N1 N5 1.30(2) . ?
N2 N3 1.30(2) . ?
N3 N4 1.33(3) . ?
N4 N5 1.30(3) . ?
N6 N10 1.29(3) . ?
N6 N7 1.31(3) . ?
N7 N8 1.30(3) . ?
N8 N9 1.29(3) . ?
N9 N10 1.26(3) . ?
N11 N12 1.26(4) . ?
N11 N15 1.33(4) . ?
N12 N13 1.31(4) . ?
N13 N14 1.31(4) . ?
N14 N15 1.28(4) . ?
N16 N20 1.25(4) . ?
N16 N17 1.31(4) . ?
N17 N18 1.30(4) . ?
N18 N19 1.34(4) . ?
N19 N20 1.29(4) . ?

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 Pb1 O2 71.8(5) . . ?
O1 Pb1 O4 69.5(5) . . ?
O2 Pb1 O4 69.8(5) . . ?
O1 Pb1 N2 72.4(5) . . ?
O2 Pb1 N2 135.3(5) . . ?
O4 Pb1 N2 73.3(5) . . ?
O1 Pb2 O4 71.4(5) . . ?
O1 Pb2 O3 72.5(5) . . ?
O4 Pb2 O3 70.9(5) . . ?
O1 Pb2 N1 76.5(5) . . ?
O4 Pb2 N1 77.0(5) . . ?
O3 Pb2 N1 140.8(5) . . ?
O3 Pb3 O2 71.8(5) . . ?
O3 Pb3 O1 74.4(5) . . ?
O2 Pb3 O1 72.7(5) . . ?
O3 Pb3 N17 138.2(7) . . ?
O2 Pb3 N17 72.3(7) . . ?
O1 Pb3 N17 75.0(6) . . ?
O3 Pb4 O4 73.7(5) . . ?
O3 Pb4 O2 70.7(5) . . ?
O4 Pb4 O2 72.8(5) . . ?
Pb2 O1 Pb1 109.4(6) . . ?
Pb2 O1 Pb3 103.6(5) . . ?
Pb1 O1 Pb3 103.9(5) . . ?
Pb2 O1 H1 110.3 . . ?
Pb1 O1 H1 122.9 . . ?
Pb3 O1 H1 104.7 . . ?
Pb3 O2 Pb4 106.1(5) . . ?
Pb3 O2 Pb1 105.1(5) . . ?
Pb4 O2 Pb1 106.5(6) . . ?
Pb3 O2 H2 133.9 . . ?
Pb4 O2 H2 114.0 . . ?
Pb1 O2 H2 84.9 . . ?
Pb3 O3 Pb4 107.9(5) . . ?
Pb3 O3 Pb2 103.5(5) . . ?
Pb4 O3 Pb2 103.9(5) . . ?
Pb3 O3 H3 92.7 . . ?
Pb4 O3 H3 146.0 . . ?
Pb2 O3 H3 96.9 . . ?
Pb4 O4 Pb2 106.0(5) . . ?
Pb4 O4 Pb1 105.2(5) . . ?
Pb2 O4 Pb1 105.3(5) . . ?
Pb4 O4 H4 140.5 . . ?
Pb2 O4 H4 105.2 . . ?
Pb1 O4 H4 89.2 . . ?
N2 N1 N5 110.0(17) . . ?
N2 N1 Pb2 113.5(13) . . ?
N5 N1 Pb2 135.9(14) . . ?
N1 N2 N3 107.4(17) . . ?
N1 N2 Pb1 123.1(13) . . ?
N3 N2 Pb1 129.3(13) . . ?
N2 N3 N4 108.2(17) . . ?
N5 N4 N3 106.7(18) . . ?
N4 N5 N1 107.4(18) . . ?
N10 N6 N7 106.5(19) . . ?
N8 N7 N6 108.6(19) . . ?
N9 N8 N7 105.7(18) . . ?
N10 N9 N8 111(2) . . ?
N9 N10 N6 108.5(19) . . ?
N12 N11 N15 108(3) . . ?
N11 N12 N13 110(3) . . ?
N14 N13 N12 105(2) . . ?
N15 N14 N13 111(3) . . ?
N14 N15 N11 105(2) . . ?
N20 N16 N17 108(3) . . ?
N18 N17 N16 108(3) . . ?
N18 N17 Pb3 112(2) . . ?
N16 N17 Pb3 140(2) . . ?
N17 N18 N19 108(3) . . ?
N20 N19 N18 105(3) . . ?
N16 N20 N19 111(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
_geom_hbond_publ_flag
O1 H1 N6 0.85 2.33 2.92(2) 127.4 . yes
O2 H2 N4 0.85 2.67 3.08(2) 110.6 2_756 yes
O2 H2 N7 0.85 2.18 2.84(2) 133.8 2_656 yes
O3 H3 N3 0.85 2.06 2.83(2) 150.3 1_556 yes
O4 H4 N18 0.84 2.17 2.90(3) 144.1 1_655 yes

_refine_diff_density_max         2.522
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.255

####################################################################### 
# 
# 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_b_a
_database_code_depnum_ccdc_archive 'CCDC 2104205'
loop_
_audit_author_name
_audit_author_address
'Yuangang Xu'
;Nanjing University of Science and Technology
China
;
_audit_update_record             
;
2021-09-28 deposited with the CCDC.	2022-03-08 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         'H10 N16 O10 Pb4'
_chemical_formula_sum            'H10 N16 O10 Pb4'
_chemical_formula_weight         1223.00

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3'
_space_group_name_Hall           'R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   8.9224(2)
_cell_length_b                   8.9224(2)
_cell_length_c                   22.5833(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1556.97(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3470
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      28.25

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.913
_exptl_crystal_F_000             1590
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    32.418
_shelx_estimated_absorpt_T_min   0.181
_shelx_estimated_absorpt_T_max   0.210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0288
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source.type              microfocus
_diffrn_radiation_type           MoK\a
_diffrn_source.source            'Ius 2.0'
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            3927
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.706
_diffrn_reflns_theta_max         24.930
_diffrn_reflns_theta_full        24.930
_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 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             1206
_reflns_number_gt                1156
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.971
_reflns_Friedel_fraction_max     0.971
_reflns_Friedel_fraction_full    0.971

_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       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0675P)²] 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_abs_structure_details 
;
 Flack x determined using 536 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.09(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1206
_refine_ls_number_parameters     91
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.1137
_refine_ls_wR_factor_gt          0.1125
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.333333 0.666667 0.66633(6) 0.0303(5) Uani 1 3 d S T P . .
Pb2 Pb 0.08311(14) 0.66408(14) 0.52963(7) 0.0334(4) Uani 1 1 d . . . . .
O1 O 0.333333 0.666667 0.4873(14) 0.027(7) Uani 1 3 d S T P . .
H1 H 0.333332 0.666667 0.443868 0.040 Uiso 1 3 calc R U P . .
O2 O 0.330(2) 0.846(2) 0.5892(8) 0.028(4) Uani 1 1 d . . . . .
H2 H 0.328920 0.948889 0.603981 0.041 Uiso 1 1 calc R U . . .
O3 O 0.146(3) 0.011(3) 0.5223(12) 0.064(8) Uani 1 1 d . . . . .
O4 O 0.889(4) 0.361(4) 0.4598(16) 0.080(9) Uani 1 1 d . . . . .
H4A H 0.959068 0.358592 0.434927 0.119 Uiso 1 1 d R U . . .
H4B H 0.886496 0.298192 0.488177 0.119 Uiso 1 1 d R U . . .
N1 N -0.204(5) 0.683(5) 0.7089(15) 0.072(11) Uani 1 1 d . . . . .
N2 N -0.067(5) 0.681(5) 0.7321(13) 0.060(8) Uani 1 1 d . . . . .
N3 N -0.205(4) 0.669(5) 0.6517(13) 0.058(9) Uani 1 1 d . . . . .
N4 N -0.069(4) 0.657(5) 0.6381(12) 0.053(7) Uani 1 1 d . . . . .
N5 N 0.017(3) 0.669(4) 0.6865(12) 0.036(6) Uani 1 1 d . . . . .
N6 N 0.000000 0.000000 0.525(2) 0.044(12) Uani 1 3 d S T 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 O2 2.377(18) . ?
Pb1 O2 2.377(18) 2_665 ?
Pb1 O2 2.377(18) 3_565 ?
Pb2 O2 2.393(19) . ?
Pb2 O2 2.409(19) 2_665 ?
Pb2 O1 2.418(12) . ?
Pb2 N4 2.79(3) . ?
O1 H1 0.9800 . ?
O2 H2 0.9800 . ?
O3 N6 1.26(3) . ?
O4 H4A 0.8509 . ?
O4 H4B 0.8455 . ?
N1 N3 1.30(4) . ?
N1 N2 1.33(5) . ?
N2 N5 1.31(4) . ?
N3 N4 1.31(4) . ?
N4 N5 1.31(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Pb1 O2 72.2(7) . 2_665 ?
O2 Pb1 O2 72.2(7) . 3_565 ?
O2 Pb1 O2 72.2(7) 2_665 3_565 ?
O2 Pb2 O2 71.3(9) . 2_665 ?
O2 Pb2 O1 71.5(7) . . ?
O2 Pb2 O1 71.3(7) 2_665 . ?
O2 Pb2 N4 78.1(8) . . ?
O2 Pb2 N4 77.3(7) 2_665 . ?
O1 Pb2 N4 141.7(9) . . ?
Pb2 O1 Pb2 105.4(8) 3_565 2_665 ?
Pb2 O1 Pb2 105.4(8) 3_565 . ?
Pb2 O1 Pb2 105.4(8) 2_665 . ?
Pb2 O1 H1 113.3 3_565 . ?
Pb2 O1 H1 113.3 2_665 . ?
Pb2 O1 H1 113.3 . . ?
Pb1 O2 Pb2 105.7(7) . . ?
Pb1 O2 Pb2 105.2(7) . 3_565 ?
Pb2 O2 Pb2 106.5(7) . 3_565 ?
Pb1 O2 H2 112.9 . . ?
Pb2 O2 H2 112.9 . . ?
Pb2 O2 H2 112.9 3_565 . ?
H4A O4 H4B 104.8 . . ?
N3 N1 N2 111(3) . . ?
N5 N2 N1 105(3) . . ?
N1 N3 N4 106(3) . . ?
N5 N4 N3 109(3) . . ?
N5 N4 Pb2 118(2) . . ?
N3 N4 Pb2 132(2) . . ?
N4 N5 N2 109(3) . . ?
O3 N6 O3 119.8(5) 3 . ?
O3 N6 O3 119.8(5) 3 2 ?
O3 N6 O3 119.8(5) . 2 ?

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
N3 N1 N2 N5 1(5) . . . . ?
N2 N1 N3 N4 0(5) . . . . ?
N1 N3 N4 N5 -1(5) . . . . ?
N1 N3 N4 Pb2 -171(3) . . . . ?
N3 N4 N5 N2 2(4) . . . . ?
Pb2 N4 N5 N2 173(3) . . . . ?
N1 N2 N5 N4 -2(4) . . . . ?

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
_geom_hbond_publ_flag
O2 H2 N3 0.98 1.91 2.86(3) 165.5 2_675 yes
O4 H4A N1 0.85 2.06 2.91(5) 179.1 7_644 yes
O4 H4B O3 0.85 2.21 2.94(4) 145.3 2_655 yes

_refine_diff_density_max         1.115
_refine_diff_density_min         -1.570
_refine_diff_density_rms         0.288

# start Validation Reply Form
_vrf_PLAT420_b_a                 
;
PROBLEM: D-H Bond Without Acceptor O1 --H1 . Please Check
RESPONSE: The O1 is hydroxyl oxygen atom.
;
# 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_YY210323_a
_database_code_depnum_ccdc_archive 'CCDC 2104204'
loop_
_audit_author_name
_audit_author_address
'Yuangang Xu'
;Nanjing University of Science and Technology
China
;
_audit_update_record             
;
2021-09-28 deposited with the CCDC.	2022-03-08 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         
'2(H18 N16 O12 Pb3), 4(N5), H3 O1.50, 2(O0.50), 2(H)'
_chemical_formula_sum            'H41 N52 O26.50 Pb6'
_chemical_formula_weight         2436.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 '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'

_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'

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

_cell_length_a                   14.9624(5)
_cell_length_b                   14.9624(5)
_cell_length_c                   7.3194(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1419.09(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7396
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      27.47

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.852
_exptl_crystal_F_000             1109
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    17.850
_shelx_estimated_absorpt_T_min   0.125
_shelx_estimated_absorpt_T_max   0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3675
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source.type              microfocus
_diffrn_radiation_type           MoK\a
_diffrn_source.source            'Ius 2.0'
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            14760
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.144
_diffrn_reflns_theta_max         27.503
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             1172
_reflns_number_gt                1039
_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       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0160P)²+3.8176P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1172
_refine_ls_number_parameters     86
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0206
_refine_ls_wR_factor_ref         0.0409
_refine_ls_wR_factor_gt          0.0392
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
Pb1 Pb 0.49955(2) 0.58062(2) 0.250000 0.02420(8) Uani 1 2 d S T P . .
N1 N 0.5042(2) 0.3426(2) 0.3957(4) 0.0227(6) Uani 1 1 d . . . . .
N2 N 0.4943(3) 0.2542(2) 0.3403(4) 0.0272(7) Uani 1 1 d . . . . .
N3 N 0.5106(3) 0.3963(3) 0.250000 0.0196(9) Uani 1 2 d S T P . .
N4 N 0.333333 0.666667 0.250000 0.0219(16) Uani 1 6 d S T P . .
O3 O 0.3066(3) 0.5729(3) 0.250000 0.0326(9) Uani 1 2 d S T P . .
O1 O 0.6646(4) 0.7653(4) 0.250000 0.0607(14) Uani 1 2 d S T P . .
H1A H 0.646631 0.810998 0.250000 0.091 Uiso 1 2 d R U P . .
H1B H 0.696981 0.774728 0.149970 0.091 Uiso 0.5 1 d R U P . .
O2 O 0.37214(19) 0.4332(2) 0.0053(4) 0.0276(6) Uani 1 1 d . . . . .
H2A H 0.324731 0.376466 0.071517 0.041 Uiso 1 1 d R U . . .
H2B H 0.328741 0.449936 -0.044883 0.041 Uiso 1 1 d R U . . .
N5 N 0.1397(9) 0.2239(10) 0.750000 0.073(3) Uani 0.6667 2 d S T P A 1
N6 N 0.0239(5) 0.2581(6) 0.6640(11) 0.0547(18) Uani 0.6667 1 d . . P A 1
N7 N 0.0988(7) 0.2400(7) 0.6077(12) 0.082(3) Uani 0.6667 1 d . . P A 1
O4 O -0.0212(18) 0.2581(16) 0.750000 0.048(5) Uani 0.25 2 d S T P B 2
H4 H -0.034378 0.224183 0.849080 0.072 Uiso 0.25 1 d R U P B 2
O5 O 1.000000 1.000000 0.500000 0.126(12) Uani 0.5 6 d S T P . .
H5A H 1.036790 0.973530 0.528920 0.188 Uiso 0.0833 1 d R U P . .
H5B H 0.938230 0.950990 0.512490 0.188 Uiso 0.0833 1 d R 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 O1 2.629(5) . ?
Pb1 O2 2.739(3) 12_556 ?
Pb1 O2 2.739(3) . ?
N1 N3 1.310(4) . ?
N1 N2 1.319(4) . ?
N2 N2 1.322(6) 12_556 ?
N4 O3 1.252(4) 8_566 ?
N4 O3 1.252(4) 9_666 ?
N4 O3 1.252(4) . ?
O1 H1A 0.8500 . ?
O1 H1B 0.8500 . ?
O1 H1B 0.8501 12_556 ?
O2 H2A 0.9254 . ?
O2 H2B 0.8843 . ?
N5 N7 1.290(10) . ?
N5 N7 1.290(10) 12_557 ?
N6 N6 1.258(15) 12_557 ?
N6 N7 1.344(10) . ?
N6 H4 0.76(2) 12_557 ?
O4 H4 0.8500 . ?
O4 H4 0.8501 12_557 ?
O5 H5A 0.8501 . ?
O5 H5B 0.8500 . ?
O5 H5A 0.8502 7_776 ?
O5 H5A 0.8502 4_765 ?
O5 H5A 0.8502 10_566 ?
O5 H5A 0.8502 5_675 ?
O5 H5A 0.8502 11_656 ?
O5 H5B 0.8500 7_776 ?
O5 H5B 0.8500 4_765 ?
O5 H5B 0.8500 10_566 ?
O5 H5B 0.8500 5_675 ?
O5 H5B 0.8500 11_656 ?

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 Pb1 O2 139.14(6) . 12_556 ?
O1 Pb1 O2 139.14(6) . . ?
O2 Pb1 O2 81.66(11) 12_556 . ?
N3 N1 N2 107.6(3) . . ?
N1 N2 N2 107.91(19) . 12_556 ?
N1 N3 N1 109.0(4) 12_556 . ?
O3 N4 O3 119.996(1) 8_566 9_666 ?
O3 N4 O3 120.001(1) 8_566 . ?
O3 N4 O3 120.003(1) 9_666 . ?
Pb1 O1 H1A 109.7 . . ?
Pb1 O1 H1B 109.4 . . ?
H1A O1 H1B 104.5 . . ?
Pb1 O1 H1B 109.39(5) . 12_556 ?
H1A O1 H1B 104.5 . 12_556 ?
H1B O1 H1B 118.9 . 12_556 ?
Pb1 O2 H2A 107.6 . . ?
Pb1 O2 H2B 111.0 . . ?
H2A O2 H2B 98.2 . . ?
N7 N5 N7 107.7(10) . 12_557 ?
N6 N6 N7 107.9(5) 12_557 . ?
N6 N6 H4 97.2(5) 12_557 12_557 ?
N7 N6 H4 128.1(16) . 12_557 ?
N5 N7 N6 108.1(8) . . ?
H5A O5 H5B 104.4 . . ?
H5A O5 H5A 180.0 . 7_776 ?
H5B O5 H5A 75.6 . 7_776 ?
H5A O5 H5A 114.0 . 4_765 ?
H5B O5 H5A 129.4 . 4_765 ?
H5A O5 H5A 66.0 7_776 4_765 ?
H5A O5 H5A 66.0 . 10_566 ?
H5B O5 H5A 50.6 . 10_566 ?
H5A O5 H5A 114.0 7_776 10_566 ?
H5A O5 H5A 180.0 4_765 10_566 ?
H5A O5 H5A 114.0 . 5_675 ?
H5B O5 H5A 15.5 . 5_675 ?
H5A O5 H5A 66.0 7_776 5_675 ?
H5A O5 H5A 114.0 4_765 5_675 ?
H5A O5 H5A 66.0 10_566 5_675 ?
H5A O5 H5A 66.0 . 11_656 ?
H5B O5 H5A 164.5 . 11_656 ?
H5A O5 H5A 114.0 7_776 11_656 ?
H5A O5 H5A 66.0 4_765 11_656 ?
H5A O5 H5A 114.0 10_566 11_656 ?
H5A O5 H5A 180.0 5_675 11_656 ?
H5A O5 H5B 75.6 . 7_776 ?
H5B O5 H5B 180.0 . 7_776 ?
H5A O5 H5B 104.4 7_776 7_776 ?
H5A O5 H5B 50.6 4_765 7_776 ?
H5A O5 H5B 129.4 10_566 7_776 ?
H5A O5 H5B 164.5 5_675 7_776 ?
H5A O5 H5B 15.5 11_656 7_776 ?
H5A O5 H5B 15.5 . 4_765 ?
H5B O5 H5B 118.9 . 4_765 ?
H5A O5 H5B 164.5 7_776 4_765 ?
H5A O5 H5B 104.4 4_765 4_765 ?
H5A O5 H5B 75.6 10_566 4_765 ?
H5A O5 H5B 129.4 5_675 4_765 ?
H5A O5 H5B 50.6 11_656 4_765 ?
H5B O5 H5B 61.1 7_776 4_765 ?
H5A O5 H5B 164.5 . 10_566 ?
H5B O5 H5B 61.1 . 10_566 ?
H5A O5 H5B 15.5 7_776 10_566 ?
H5A O5 H5B 75.6 4_765 10_566 ?
H5A O5 H5B 104.4 10_566 10_566 ?
H5A O5 H5B 50.6 5_675 10_566 ?
H5A O5 H5B 129.4 11_656 10_566 ?
H5B O5 H5B 118.9 7_776 10_566 ?
H5B O5 H5B 180.0 4_765 10_566 ?
H5A O5 H5B 129.4 . 5_675 ?
H5B O5 H5B 118.9 . 5_675 ?
H5A O5 H5B 50.6 7_776 5_675 ?
H5A O5 H5B 15.5 4_765 5_675 ?
H5A O5 H5B 164.5 10_566 5_675 ?
H5A O5 H5B 104.4 5_675 5_675 ?
H5A O5 H5B 75.6 11_656 5_675 ?
H5B O5 H5B 61.1 7_776 5_675 ?
H5B O5 H5B 118.9 4_765 5_675 ?
H5B O5 H5B 61.1 10_566 5_675 ?
H5A O5 H5B 50.6 . 11_656 ?
H5B O5 H5B 61.1 . 11_656 ?
H5A O5 H5B 129.4 7_776 11_656 ?
H5A O5 H5B 164.5 4_765 11_656 ?
H5A O5 H5B 15.5 10_566 11_656 ?
H5A O5 H5B 75.6 5_675 11_656 ?
H5A O5 H5B 104.4 11_656 11_656 ?
H5B O5 H5B 118.9 7_776 11_656 ?
H5B O5 H5B 61.1 4_765 11_656 ?
H5B O5 H5B 118.9 10_566 11_656 ?
H5B O5 H5B 180.0 5_675 11_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
N3 N1 N2 N2 -0.3(3) . . . 12_556 ?
N2 N1 N3 N1 0.4(5) . . . 12_556 ?
N7 N5 N7 N6 -5.3(16) 12_557 . . . ?
N6 N6 N7 N5 3.3(10) 12_557 . . . ?

_refine_diff_density_max         1.766
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.126

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 2104206'
loop_
_audit_author_name
_audit_author_address
'Yuangang Xu'
;Nanjing University of Science and Technology
China
;
_audit_update_record             
;
2021-09-28 deposited with the CCDC.	2022-03-08 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         'Cl H6 N15 O9 Pb4'
_chemical_formula_sum            'Cl H6 N15 O9 Pb4'
_chemical_formula_weight         1224.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   10.1088(8)
_cell_length_b                   13.5520(11)
_cell_length_c                   13.4401(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1841.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9944
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      27.51

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    4.417
_exptl_crystal_F_000             2112
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    36.686
_shelx_estimated_absorpt_T_min   0.527
_shelx_estimated_absorpt_T_max   0.527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5646
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source.type              microfocus
_diffrn_radiation_type           MoK\a
_diffrn_source.source            'Ius 2.0'
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON 100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.42
_diffrn_reflns_number            17903
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.935
_diffrn_reflns_theta_max         27.594
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_point_group_measured_fraction_full 0.960
_reflns_number_total             3982
_reflns_number_gt                3669
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.790
_reflns_Friedel_fraction_max     0.860
_reflns_Friedel_fraction_full    0.917

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0178P)²] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.034(15)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3982
_refine_ls_number_parameters     263
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0544
_refine_ls_wR_factor_gt          0.0530
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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
Pb1 Pb 0.78990(5) 0.35207(3) 0.25098(4) 0.02531(13) Uani 1 1 d . . . . .
Pb2 Pb 1.14069(5) 0.29182(4) 0.34914(4) 0.02577(13) Uani 1 1 d . . . . .
Pb3 Pb 1.03794(5) 0.20994(4) 0.08328(4) 0.02620(13) Uani 1 1 d . . . . .
Pb4 Pb 0.88389(5) 0.08651(4) 0.31274(4) 0.02916(14) Uani 1 1 d . . . . .
N1 N 0.9138(12) 0.4833(9) 0.3774(9) 0.031(3) Uani 1 1 d . . . . .
N2 N 1.0437(12) 0.4845(8) 0.3793(8) 0.030(3) Uani 1 1 d . . . . .
N3 N 1.0820(13) 0.5640(9) 0.4256(10) 0.035(3) Uani 1 1 d . . . . .
N4 N 0.9761(13) 0.6118(9) 0.4533(10) 0.035(3) Uani 1 1 d . . . . .
N5 N 0.8705(12) 0.5628(9) 0.4234(10) 0.034(3) Uani 1 1 d . . . . .
N6 N 0.5469(12) 0.5923(10) 0.5891(11) 0.038(3) Uani 1 1 d . . . . .
N7 N 0.6086(16) 0.5530(12) 0.6657(12) 0.055(4) Uani 1 1 d . . . . .
N8 N 0.7196(14) 0.6040(11) 0.6772(11) 0.049(4) Uani 1 1 d . . . . .
N9 N 0.7265(12) 0.6730(10) 0.6086(9) 0.031(3) Uani 1 1 d . . . . .
N10 N 0.6185(13) 0.6642(10) 0.5550(10) 0.037(3) Uani 1 1 d . . . . .
N11 N 0.8475(15) 0.8835(10) -0.0192(10) 0.043(3) Uani 1 1 d . . . . .
N12 N 0.9438(16) 0.9482(10) -0.0238(10) 0.045(4) Uani 1 1 d . . . . .
N13 N 0.9310(16) 1.0099(10) 0.0516(10) 0.048(4) Uani 1 1 d . . . . .
N14 N 0.8270(16) 0.9802(11) 0.1021(12) 0.057(4) Uani 1 1 d . . . . .
N15 N 0.7765(14) 0.9036(9) 0.0591(12) 0.050(4) Uani 1 1 d . . . . .
O1 O 0.8287(9) 0.1915(6) 0.1798(7) 0.028(2) Uani 1 1 d . . . . .
H1A H 0.754509 0.167209 0.139679 0.034 Uiso 1 1 calc R U . . .
O2 O 0.9144(9) 0.2498(6) 0.3722(7) 0.025(2) Uani 1 1 d . . . . .
H2A H 0.884236 0.258711 0.440925 0.031 Uiso 1 1 calc R U . . .
O3 O 1.0061(9) 0.3422(6) 0.2020(7) 0.024(2) Uani 1 1 d . . . . .
H3A H 1.036881 0.405342 0.174963 0.028 Uiso 1 1 calc R U . . .
O4 O 1.0837(9) 0.1451(6) 0.2443(7) 0.0235(19) Uani 1 1 d . . . . .
H4A H 1.153605 0.095008 0.243719 0.028 Uiso 1 1 calc R U . . .
Cl1 Cl 0.4716(4) 0.8347(3) 0.8044(3) 0.0366(8) Uani 1 1 d . . . . .
O5 O 0.4762(14) 0.7583(11) 0.7321(13) 0.077(5) Uani 1 1 d . . . . .
O6 O 0.5978(10) 0.8460(9) 0.8512(11) 0.052(3) Uani 1 1 d . . . . .
O7 O 0.4331(12) 0.9264(9) 0.7599(11) 0.054(3) Uani 1 1 d . . . . .
O8 O 0.3730(11) 0.8098(9) 0.8789(10) 0.053(3) Uani 1 1 d . . . . .
O9 O 0.7222(11) 0.3540(9) 0.0524(9) 0.052(3) Uani 1 1 d . . . . .
H9A H 0.781053 0.378356 0.014507 0.077 Uiso 1 1 d R U . . .
H9B H 0.654513 0.389956 0.042907 0.077 Uiso 1 1 d 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
Pb1 O3 2.286(9) . ?
Pb1 O1 2.410(9) . ?
Pb1 O2 2.482(9) . ?
Pb1 O9 2.755(12) . ?
Pb1 N1 2.760(12) . ?
Pb2 O2 2.378(9) . ?
Pb2 O3 2.496(9) . ?
Pb2 O4 2.504(9) . ?
Pb3 O4 2.381(9) . ?
Pb3 O3 2.422(9) . ?
Pb3 O1 2.494(10) . ?
Pb4 O1 2.351(10) . ?
Pb4 O4 2.357(9) . ?
Pb4 O2 2.373(9) . ?
N1 N2 1.313(16) . ?
N1 N5 1.318(17) . ?
N2 N3 1.303(17) . ?
N3 N4 1.306(17) . ?
N4 N5 1.320(17) . ?
N6 N10 1.298(18) . ?
N6 N7 1.32(2) . ?
N7 N8 1.326(19) . ?
N8 N9 1.314(18) . ?
N9 N10 1.314(17) . ?
N11 N15 1.303(19) . ?
N11 N12 1.312(19) . ?
N12 N13 1.320(18) . ?
N13 N14 1.314(19) . ?
N14 N15 1.292(19) . ?
Cl1 O5 1.419(14) . ?
Cl1 O6 1.432(12) . ?
Cl1 O7 1.434(12) . ?
Cl1 O8 1.453(12) . ?

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
O3 Pb1 O1 71.2(3) . . ?
O3 Pb1 O2 70.8(3) . . ?
O1 Pb1 O2 71.0(3) . . ?
O3 Pb1 O9 87.7(3) . . ?
O1 Pb1 O9 70.4(3) . . ?
O2 Pb1 O9 140.1(3) . . ?
O3 Pb1 N1 77.3(4) . . ?
O1 Pb1 N1 138.8(3) . . ?
O2 Pb1 N1 74.1(3) . . ?
O9 Pb1 N1 134.7(3) . . ?
O2 Pb2 O3 69.2(3) . . ?
O2 Pb2 O4 70.2(3) . . ?
O3 Pb2 O4 69.3(3) . . ?
O4 Pb3 O3 72.6(3) . . ?
O4 Pb3 O1 69.8(3) . . ?
O3 Pb3 O1 67.6(3) . . ?
O1 Pb4 O4 72.7(3) . . ?
O1 Pb4 O2 73.9(3) . . ?
O4 Pb4 O2 72.9(3) . . ?
N2 N1 N5 108.2(11) . . ?
N2 N1 Pb1 118.3(8) . . ?
N5 N1 Pb1 131.7(9) . . ?
N3 N2 N1 108.5(11) . . ?
N2 N3 N4 107.6(12) . . ?
N3 N4 N5 109.1(12) . . ?
N1 N5 N4 106.6(11) . . ?
N10 N6 N7 108.4(13) . . ?
N6 N7 N8 106.3(13) . . ?
N9 N8 N7 109.5(13) . . ?
N10 N9 N8 106.1(12) . . ?
N6 N10 N9 109.7(12) . . ?
N15 N11 N12 107.9(12) . . ?
N11 N12 N13 108.3(13) . . ?
N14 N13 N12 106.3(13) . . ?
N15 N14 N13 109.4(14) . . ?
N14 N15 N11 108.2(13) . . ?
Pb4 O1 Pb1 106.4(4) . . ?
Pb4 O1 Pb3 104.8(3) . . ?
Pb1 O1 Pb3 104.7(3) . . ?
Pb4 O2 Pb2 107.7(3) . . ?
Pb4 O2 Pb1 103.5(3) . . ?
Pb2 O2 Pb1 105.6(3) . . ?
Pb1 O3 Pb3 111.1(4) . . ?
Pb1 O3 Pb2 108.0(4) . . ?
Pb3 O3 Pb2 104.3(3) . . ?
Pb4 O4 Pb3 108.2(3) . . ?
Pb4 O4 Pb2 104.2(3) . . ?
Pb3 O4 Pb2 105.2(3) . . ?
O5 Cl1 O6 110.5(9) . . ?
O5 Cl1 O7 110.8(10) . . ?
O6 Cl1 O7 109.4(7) . . ?
O5 Cl1 O8 109.0(8) . . ?
O6 Cl1 O8 109.5(8) . . ?
O7 Cl1 O8 107.6(8) . . ?

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
N5 N1 N2 N3 -0.3(15) . . . . ?
Pb1 N1 N2 N3 166.3(9) . . . . ?
N1 N2 N3 N4 0.6(15) . . . . ?
N2 N3 N4 N5 -0.7(16) . . . . ?
N2 N1 N5 N4 -0.1(15) . . . . ?
Pb1 N1 N5 N4 -164.2(9) . . . . ?
N3 N4 N5 N1 0.5(16) . . . . ?
N10 N6 N7 N8 0.3(19) . . . . ?
N6 N7 N8 N9 -0.3(19) . . . . ?
N7 N8 N9 N10 0.2(18) . . . . ?
N7 N6 N10 N9 -0.2(18) . . . . ?
N8 N9 N10 N6 0.0(17) . . . . ?
N15 N11 N12 N13 -1(2) . . . . ?
N11 N12 N13 N14 1(2) . . . . ?
N12 N13 N14 N15 -1(2) . . . . ?
N13 N14 N15 N11 0(2) . . . . ?
N12 N11 N15 N14 1(2) . . . . ?

_refine_diff_density_max         1.186
_refine_diff_density_min         -1.251
_refine_diff_density_rms         0.225

# start Validation Reply Form
_vrf_PLAT420_1_a                 
;
PROBLEM: D-H Bond Without Acceptor O1 --H1A . Please Check
RESPONSE: No suitable acceptor has been located for this hydroxo group.
;
# end Validation Reply Form

