# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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_32089101_0m
_database_code_depnum_ccdc_archive 'CCDC 2305213'
loop_
_audit_author_name
_audit_author_address
'Laura Valencia Matarranz'
;Universidade de Vigo
Spain
;
_audit_update_record             
;
2023-11-01 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;
_audit_creation_date             2023-09-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C26 H38 N10 O4 Pb, 2(F6 P)'
_chemical_formula_sum            'C26 H38 F12 N10 O4 P2 Pb'
_chemical_formula_weight         1051.79
_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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   13.5776(7)
_cell_length_b                   16.3882(9)
_cell_length_c                   32.7592(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7289.3(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.70
_shelx_estimated_absorpt_T_max   0.812
_shelx_estimated_absorpt_T_min   0.470
_exptl_absorpt_coefficient_mu    4.828
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1440 before and 0.0619 after correction. The Ratio of minimum to maximum transmission is 0.7400. 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    1.917
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.045
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            40984
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.298
_diffrn_reflns_theta_min         2.045
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Incoatec HeliosTM multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2125
_reflns_number_total             2280
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.256
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2280
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0338
_refine_ls_restrained_S_all      1.208
_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)+(0.0325P)²+153.5051P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0858
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All F(H) groups
2. Restrained distances
 N3-H3b
 0.873 with sigma of 0.02
3. Restrained planarity
 H3b, H3a, N3, C7
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.0025
5. Others
 Fixed Sof: P1(0.5) F4(0.5)
 Fixed X: H3a(0.4671)
 Fixed Y: H3a(0.51807)
 Fixed Z: H3a(0.59582)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C5(H5a,H5b), C4(H4a,H4b)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.125000 0.625000 0.625000 0.01977(10) Uani 1 4 d S T P . .
P1 P 0.6214(7) 0.6509(5) 0.71070(12) 0.104(4) Uani 0.5 1 d . . . . .
O1 O 0.2990(3) 0.5503(2) 0.65068(12) 0.0382(8) Uani 1 1 d . . . . .
N2 N 0.1903(4) 0.4861(3) 0.58768(14) 0.0393(10) Uani 1 1 d . . . . .
N1 N 0.125000 0.625000 0.54423(17) 0.0406(15) Uani 1 2 d S T P . .
N3 N 0.4451(4) 0.5246(4) 0.6205(2) 0.0665(18) Uani 1 1 d D . . . .
H3A H 0.467100 0.518070 0.595820 0.080 Uiso 1 1 d R . . . .
C3 C 0.1359(4) 0.5539(4) 0.52378(17) 0.0472(14) Uani 1 1 d . U . . .
C7 C 0.3460(4) 0.5276(3) 0.6207(2) 0.0429(13) Uani 1 1 d . . . . .
F2 F 0.5095(5) 0.6277(7) 0.70927(16) 0.172(4) Uani 1 1 d . . . . .
C6 C 0.2967(5) 0.4998(4) 0.5815(2) 0.0508(16) Uani 1 1 d . . . . .
H6A H 0.306370 0.541730 0.560092 0.061 Uiso 1 1 calc R . . . .
H6B H 0.327899 0.448600 0.571980 0.061 Uiso 1 1 calc R . . . .
F3 F 0.625000 0.625000 0.7528(2) 0.151(5) Uani 1 2 d S T P . .
C5 C 0.1742(5) 0.4145(3) 0.6140(2) 0.0549(18) Uani 1 1 d . . . . .
H5A H 0.227537 0.412220 0.634588 0.066 Uiso 1 1 calc R . . . .
H5B H 0.178825 0.364608 0.597106 0.066 Uiso 1 1 calc R . . . .
C4 C 0.1391(5) 0.4775(4) 0.5483(2) 0.0548(18) Uani 1 1 d . . . . .
H4A H 0.070780 0.459083 0.553429 0.066 Uiso 1 1 calc R . . . .
H4B H 0.172422 0.434640 0.532069 0.066 Uiso 1 1 calc R . . . .
F1 F 0.6158(5) 0.5598(7) 0.6756(3) 0.182(4) Uani 1 1 d . . . . .
C2 C 0.1350(6) 0.5526(6) 0.4812(2) 0.069(2) Uani 1 1 d . U . . .
H2 H 0.141190 0.502711 0.466654 0.083 Uiso 1 1 calc R . . . .
C1 C 0.125000 0.625000 0.4610(4) 0.081(3) Uani 1 2 d S TU P . .
H1 H 0.124998 0.625002 0.431966 0.097 Uiso 1 2 calc RS T P . .
F4 F 0.6348(10) 0.7338(11) 0.7319(4) 0.120(5) Uani 0.5 1 d . . . . .
H3B H 0.485(8) 0.535(5) 0.641(3) 0.144 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N2 2.732(4) 8 ?
Pb1 N2 2.732(4) 11_455 ?
Pb1 N2 2.732(4) . ?
Pb1 N2 2.732(4) 14_455 ?
Pb1 N1 2.646(6) . ?
Pb1 N1 2.646(6) 11_455 ?
P1 P1 0.855(18) 14 ?
P1 F2 1.567(10) . ?
P1 F2 1.684(13) 14 ?
P1 F3 1.443(8) . ?
P1 F1 1.886(13) . ?
P1 F1 1.329(11) 14 ?
P1 F4 1.536(18) . ?
O1 C7 1.229(7) . ?
N2 C6 1.477(7) . ?
N2 C5 1.472(8) . ?
N2 C4 1.473(8) . ?
N1 C3 1.352(7) 14_455 ?
N1 C3 1.352(7) . ?
N3 H3A 0.868(8) . ?
N3 C7 1.347(8) . ?
N3 H3B 0.87(2) . ?
C3 C4 1.487(10) . ?
C3 C2 1.396(9) . ?
C7 C6 1.518(9) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C5 C5 1.518(13) 11_455 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C2 H2 0.9500 . ?
C2 C1 1.366(11) . ?
C1 H1 0.9500 . ?

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 Pb1 N2 126.8(2) 8 11_455 ?
N2 Pb1 N2 67.1(2) 8 14_455 ?
N2 Pb1 N2 142.1(2) 8 . ?
N2 Pb1 N2 67.1(2) 11_455 . ?
N2 Pb1 N2 126.8(2) 14_455 . ?
N2 Pb1 N2 142.1(2) 11_455 14_455 ?
N1 Pb1 N2 116.59(11) 11_455 . ?
N1 Pb1 N2 116.59(11) . 11_455 ?
N1 Pb1 N2 63.41(11) . 14_455 ?
N1 Pb1 N2 63.41(11) 11_455 11_455 ?
N1 Pb1 N2 63.41(11) 11_455 8 ?
N1 Pb1 N2 63.41(11) . . ?
N1 Pb1 N2 116.59(11) 11_455 14_455 ?
N1 Pb1 N2 116.59(11) . 8 ?
N1 Pb1 N1 180.0 . 11_455 ?
P1 P1 F2 67.3(13) 14 14 ?
P1 P1 F2 82.5(10) 14 . ?
P1 P1 F3 72.8(4) 14 . ?
P1 P1 F1 38.6(4) 14 . ?
P1 P1 F1 117.8(8) 14 14 ?
P1 P1 F4 149.8(9) 14 . ?
F2 P1 F2 149.6(6) . 14 ?
F2 P1 F1 78.5(6) 14 . ?
F2 P1 F1 75.5(5) . . ?
F3 P1 F2 85.0(5) . 14 ?
F3 P1 F2 89.4(4) . . ?
F3 P1 F1 110.5(6) . . ?
F3 P1 F4 79.9(6) . . ?
F1 P1 F2 89.2(7) 14 14 ?
F1 P1 F2 102.6(6) 14 . ?
F1 P1 F3 164.7(6) 14 . ?
F1 P1 F1 82.0(9) 14 . ?
F1 P1 F4 87.0(8) 14 . ?
F4 P1 F2 110.1(9) . . ?
F4 P1 F2 98.3(7) . 14 ?
F4 P1 F1 168.6(6) . . ?
C6 N2 Pb1 104.6(3) . . ?
C5 N2 Pb1 110.7(3) . . ?
C5 N2 C6 110.3(5) . . ?
C5 N2 C4 111.6(5) . . ?
C4 N2 Pb1 108.6(4) . . ?
C4 N2 C6 110.9(5) . . ?
C3 N1 Pb1 119.7(3) 14_455 . ?
C3 N1 Pb1 119.7(3) . . ?
C3 N1 C3 120.6(7) 14_455 . ?
H3A N3 H3B 121(9) . . ?
C7 N3 H3A 110.7(7) . . ?
C7 N3 H3B 127(9) . . ?
N1 C3 C4 117.5(5) . . ?
N1 C3 C2 120.5(7) . . ?
C2 C3 C4 121.8(6) . . ?
O1 C7 N3 122.3(6) . . ?
O1 C7 C6 122.6(5) . . ?
N3 C7 C6 115.2(6) . . ?
P1 F2 P1 30.2(6) . 14 ?
N2 C6 C7 111.1(5) . . ?
N2 C6 H6A 109.4 . . ?
N2 C6 H6B 109.4 . . ?
C7 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
P1 F3 P1 34.5(7) 14 . ?
N2 C5 C5 114.1(5) . 11_455 ?
N2 C5 H5A 108.7 . . ?
N2 C5 H5B 108.7 . . ?
C5 C5 H5A 108.7 11_455 . ?
C5 C5 H5B 108.7 11_455 . ?
H5A C5 H5B 107.6 . . ?
N2 C4 C3 114.0(5) . . ?
N2 C4 H4A 108.8 . . ?
N2 C4 H4B 108.8 . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
P1 F1 P1 23.6(6) 14 . ?
C3 C2 H2 120.9 . . ?
C1 C2 C3 118.2(9) . . ?
C1 C2 H2 120.9 . . ?
C2 C1 C2 121.9(11) . 14_455 ?
C2 C1 H1 119.0 14_455 . ?
C2 C1 H1 119.0 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_32078702_0r
_database_code_depnum_ccdc_archive 'CCDC 2305214'
loop_
_audit_author_name
_audit_author_address
'Laura Valencia Matarranz'
;Universidade de Vigo
Spain
;
_audit_update_record             
;
2023-11-01 deposited with the CCDC.	2023-12-22 downloaded from the CCDC.
;
_audit_creation_date             2023-11-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C34 H46 N10 O12 Pb, 1.906(N O3), 0.094(Br), 5(H2 O)'
_chemical_formula_sum            'C34 H56 Br0.10 N11.90 O22.72 Pb'
_chemical_formula_weight         1209.84
_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'
Br Br -0.2901 2.4595 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.1973(11)
_cell_length_b                   10.1543(5)
_cell_length_c                   20.7147(10)
_cell_angle_alpha                90
_cell_angle_beta                 99.397(2)
_cell_angle_gamma                90
_cell_volume                     4606.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9142
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   0.887
_shelx_estimated_absorpt_T_min   0.495
_exptl_absorpt_coefficient_mu    3.842
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2442
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.032
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            107981
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.303
_diffrn_reflns_theta_min         1.860
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Incoatec HeliosTM multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10652
_reflns_number_total             11459
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.440
_refine_diff_density_min         -0.890
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         11459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0231
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0187P)²+9.3757P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0530
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Shared sites
{N2N, Br1}
3. Uiso/Uaniso restraints and constraints
Uanis(N2N) = Uanis(Br1)
4. Others
 Sof(Br1)=1-FVAR(1)
 Sof(N2N)=Sof(O4N)=Sof(O5N)=Sof(O6N)=FVAR(1)
5.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA), O5W(H5WA,H5WB)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C23(H23A,H23B),
 C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B),
  C21(H21A,H21B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), N7(H7), N8(H8), N9(H9),
 N10(H10)
5.d Idealised tetrahedral OH refined as rotating group:
 O6(H6), O9(H9C), O12(H12A), O2(H2A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.25409(2) 0.63667(2) 0.59936(2) 0.01266(3) Uani 1 1 d . . . . .
C1 C 0.17859(10) 0.9293(2) 0.54601(12) 0.0161(4) Uani 1 1 d . . . . .
C2 C 0.14102(11) 1.0389(3) 0.54870(13) 0.0211(5) Uani 1 1 d . . . . .
H2 H 0.117086 1.073003 0.510106 0.025 Uiso 1 1 calc R U . . .
C3 C 0.13952(13) 1.0967(3) 0.60900(14) 0.0249(5) Uani 1 1 d . . . . .
H3 H 0.113484 1.169774 0.612447 0.030 Uiso 1 1 calc R U . . .
C4 C 0.17630(12) 1.0473(3) 0.66435(13) 0.0229(5) Uani 1 1 d . . . . .
H4 H 0.176041 1.086285 0.705995 0.027 Uiso 1 1 calc R U . . .
C5 C 0.21335(11) 0.9402(2) 0.65775(12) 0.0173(5) Uani 1 1 d . . . . .
C6 C 0.25530(11) 0.8811(2) 0.71610(12) 0.0185(5) Uani 1 1 d . . . . .
H6A H 0.298341 0.899105 0.711960 0.022 Uiso 1 1 calc R U . . .
H6B H 0.247062 0.923267 0.756857 0.022 Uiso 1 1 calc R U . . .
C7 C 0.29188(11) 0.6783(2) 0.77234(11) 0.0182(5) Uani 1 1 d . . . . .
H7A H 0.275948 0.593729 0.786293 0.022 Uiso 1 1 calc R U . . .
H7B H 0.297743 0.738098 0.810609 0.022 Uiso 1 1 calc R U . . .
C8 C 0.35338(11) 0.6540(2) 0.75112(11) 0.0170(5) Uani 1 1 d . . . . .
H8A H 0.371258 0.739638 0.741349 0.020 Uiso 1 1 calc R U . . .
H8B H 0.381277 0.612954 0.787761 0.020 Uiso 1 1 calc R U . . .
C9 C 0.34141(12) 0.4285(2) 0.70992(12) 0.0189(5) Uani 1 1 d . . . . .
H9A H 0.309751 0.422657 0.738377 0.023 Uiso 1 1 calc R U . . .
H9B H 0.380220 0.396131 0.735391 0.023 Uiso 1 1 calc R U . . .
C10 C 0.32334(11) 0.3391(2) 0.65105(12) 0.0158(4) Uani 1 1 d . . . . .
C11 C 0.33917(11) 0.2060(2) 0.65426(13) 0.0191(5) Uani 1 1 d . . . . .
H11 H 0.363113 0.170726 0.692549 0.023 Uiso 1 1 calc R U . . .
C12 C 0.31946(11) 0.1262(2) 0.60080(13) 0.0196(5) Uani 1 1 d . . . . .
H12 H 0.329955 0.035407 0.601887 0.024 Uiso 1 1 calc R U . . .
C13 C 0.28408(10) 0.1803(2) 0.54541(12) 0.0172(5) Uani 1 1 d . . . . .
H13 H 0.269920 0.127044 0.508311 0.021 Uiso 1 1 calc R U . . .
C14 C 0.26994(10) 0.3133(2) 0.54546(12) 0.0158(4) Uani 1 1 d . . . . .
C15 C 0.23305(11) 0.3773(2) 0.48531(12) 0.0180(5) Uani 1 1 d . . . . .
H15A H 0.261435 0.416962 0.458566 0.022 Uiso 1 1 calc R U . . .
H15B H 0.209120 0.308600 0.458549 0.022 Uiso 1 1 calc R U . . .
C16 C 0.16472(11) 0.5569(2) 0.44326(12) 0.0194(5) Uani 1 1 d . . . . .
H16A H 0.126148 0.598097 0.451108 0.023 Uiso 1 1 calc R U . . .
H16B H 0.154798 0.496282 0.405586 0.023 Uiso 1 1 calc R U . . .
C17 C 0.20735(12) 0.6638(2) 0.42598(12) 0.0191(5) Uani 1 1 d . . . . .
H17A H 0.244615 0.622035 0.414806 0.023 Uiso 1 1 calc R U . . .
H17B H 0.186988 0.711644 0.386780 0.023 Uiso 1 1 calc R U . . .
C18 C 0.17560(11) 0.8554(2) 0.48197(12) 0.0184(5) Uani 1 1 d . . . . .
H18A H 0.136088 0.808281 0.472882 0.022 Uiso 1 1 calc R U . . .
H18B H 0.176233 0.920404 0.446456 0.022 Uiso 1 1 calc R U . . .
C19 C 0.18426(11) 0.7057(2) 0.73133(12) 0.0195(5) Uani 1 1 d . . . . .
H19A H 0.154203 0.752767 0.698825 0.023 Uiso 1 1 calc R U . . .
H19B H 0.179050 0.736203 0.775485 0.023 Uiso 1 1 calc R U . . .
C20 C 0.17239(12) 0.5578(3) 0.72567(12) 0.0210(5) Uani 1 1 d . . . . .
C23 C 0.40333(11) 0.5850(2) 0.66185(12) 0.0166(4) Uani 1 1 d . . . . .
H23A H 0.403051 0.518603 0.626812 0.020 Uiso 1 1 calc R U . . .
H23B H 0.440473 0.570881 0.694705 0.020 Uiso 1 1 calc R U . . .
C24 C 0.40489(11) 0.7227(2) 0.63287(11) 0.0147(4) Uani 1 1 d . . . . .
C25 C 0.46908(11) 0.8931(2) 0.59746(12) 0.0188(5) Uani 1 1 d . . . . .
H25A H 0.434980 0.914955 0.562003 0.023 Uiso 1 1 calc R U . . .
H25B H 0.507331 0.894603 0.578701 0.023 Uiso 1 1 calc R U . . .
C26 C 0.47273(11) 0.9968(2) 0.65058(12) 0.0187(5) Uani 1 1 d . . . . .
C27 C 0.14239(11) 0.4226(2) 0.53275(13) 0.0198(5) Uani 1 1 d . . . . .
H27A H 0.160305 0.360688 0.567565 0.024 Uiso 1 1 calc R U . . .
H27B H 0.113972 0.372620 0.499840 0.024 Uiso 1 1 calc R U . . .
C28 C 0.10766(11) 0.5297(2) 0.56199(12) 0.0190(5) Uani 1 1 d . . . . .
C29 C 0.01867(12) 0.5949(3) 0.60562(14) 0.0242(5) Uani 1 1 d . . . . .
H29A H 0.042360 0.608657 0.649903 0.029 Uiso 1 1 calc R U . . .
H29B H -0.021486 0.557569 0.610728 0.029 Uiso 1 1 calc R U . . .
C30 C 0.00895(11) 0.7265(3) 0.57097(14) 0.0236(5) Uani 1 1 d . . . . .
C31 C 0.28138(11) 0.8276(2) 0.47144(12) 0.0171(5) Uani 1 1 d . . . . .
H31A H 0.290373 0.896602 0.505422 0.021 Uiso 1 1 calc R U . . .
H31B H 0.275273 0.871521 0.428194 0.021 Uiso 1 1 calc R U . . .
C32 C 0.33583(11) 0.7344(2) 0.47618(11) 0.0159(4) Uani 1 1 d . . . . .
C33 C 0.44088(11) 0.7127(2) 0.45705(12) 0.0187(5) Uani 1 1 d . . . . .
H33A H 0.448648 0.663528 0.498839 0.022 Uiso 1 1 calc R U . . .
H33B H 0.474432 0.777072 0.457301 0.022 Uiso 1 1 calc R U . . .
C34 C 0.44159(12) 0.6171(2) 0.40095(12) 0.0202(5) Uani 1 1 d . . . . .
N1 N 0.21427(9) 0.88274(19) 0.59931(10) 0.0161(4) Uani 1 1 d . . . . .
N1N N 0.36550(11) 1.3742(2) 0.91762(11) 0.0232(5) Uani 1 1 d . . . . .
N2 N 0.24599(9) 0.7367(2) 0.72013(10) 0.0166(4) Uani 1 1 d . . . . .
N3 N 0.34911(9) 0.56802(19) 0.69281(9) 0.0151(4) Uani 1 1 d . . . . .
N4 N 0.28973(9) 0.39066(19) 0.59722(10) 0.0157(4) Uani 1 1 d . . . . .
N5 N 0.19104(9) 0.47999(19) 0.50177(10) 0.0155(4) Uani 1 1 d . . . . .
N6 N 0.22519(9) 0.75943(19) 0.47984(9) 0.0150(4) Uani 1 1 d . . . . .
N7 N 0.13060(11) 0.5144(2) 0.76042(11) 0.0253(5) Uani 1 1 d . . . . .
H7 H 0.112766 0.571981 0.782839 0.030 Uiso 1 1 calc R U . . .
N8 N 0.45987(9) 0.7619(2) 0.62138(10) 0.0173(4) Uani 1 1 d . . . . .
H8 H 0.490873 0.706855 0.628499 0.021 Uiso 1 1 calc R U . . .
N9 N 0.05080(10) 0.5012(2) 0.57045(11) 0.0222(4) Uani 1 1 d . . . . .
H9 H 0.033171 0.427398 0.555125 0.027 Uiso 1 1 calc R U . . .
N10 N 0.38373(10) 0.7834(2) 0.45314(10) 0.0182(4) Uani 1 1 d . . . . .
H10 H 0.380543 0.861793 0.434810 0.022 Uiso 1 1 calc R U . . .
O1 O 0.19855(9) 0.48667(18) 0.69099(10) 0.0259(4) Uani 1 1 d . . . . .
O1N O 0.34442(15) 1.2627(2) 0.90346(14) 0.0576(8) Uani 1 1 d . . . . .
O2N O 0.35531(12) 1.4688(2) 0.88267(10) 0.0405(6) Uani 1 1 d . . . . .
O3N O 0.40115(11) 1.3864(3) 0.97238(12) 0.0502(7) Uani 1 1 d . . . . .
O4 O 0.35880(7) 0.79190(16) 0.61949(8) 0.0165(3) Uani 1 1 d . . . . .
O5 O 0.46291(9) 0.97626(18) 0.70561(9) 0.0242(4) Uani 1 1 d . . . . .
O6 O 0.48622(10) 1.11287(18) 0.62929(9) 0.0270(4) Uani 1 1 d . . . . .
H6 H 0.486468 1.168745 0.659230 0.041 Uiso 1 1 calc R U . . .
O7 O 0.13111(8) 0.63724(18) 0.57947(9) 0.0224(4) Uani 1 1 d . . . . .
O8 O -0.00371(9) 0.73636(19) 0.51149(10) 0.0264(4) Uani 1 1 d . . . . .
O9 O 0.01403(11) 0.8255(2) 0.61179(10) 0.0345(5) Uani 1 1 d . . . . .
H9C H 0.000921 0.894264 0.591740 0.052 Uiso 1 1 calc R U . . .
O10 O 0.33565(8) 0.62380(16) 0.50219(8) 0.0174(3) Uani 1 1 d . . . . .
O11 O 0.39836(9) 0.5979(2) 0.35827(9) 0.0266(4) Uani 1 1 d . . . . .
O12 O 0.49370(8) 0.55463(19) 0.40106(9) 0.0256(4) Uani 1 1 d . . . . .
H12A H 0.518982 0.578523 0.433642 0.038 Uiso 1 1 calc R U . . .
N2N N 0.04937(7) -0.22762(15) 0.82385(7) 0.0308(6) Uani 0.9062(19) 1 d . . P A
1
O4N O 0.06173(18) -0.1852(4) 0.76800(19) 0.0761(11) Uani 0.9062(19) 1 d . . P A
1
O5N O 0.07663(17) -0.3266(3) 0.84540(15) 0.0634(10) Uani 0.9062(19) 1 d . . P A
1
O6N O 0.01460(18) -0.1678(3) 0.85008(17) 0.0693(10) Uani 0.9062(19) 1 d . . P A
1
Br1 Br 0.04937(7) -0.22762(15) 0.82385(7) 0.0308(6) Uani 0.0938(19) 1 d . . P A
2
O2 O 0.10648(16) 0.1986(3) 0.83705(15) 0.0589(8) Uani 1 1 d . . . . .
H2A H 0.095654 0.165392 0.799822 0.088 Uiso 1 1 calc R U . . .
C21 C 0.11340(15) 0.3779(3) 0.76287(15) 0.0334(7) Uani 1 1 d . . . . .
H21A H 0.136420 0.326027 0.734566 0.040 Uiso 1 1 calc R U . . .
H21B H 0.069389 0.369027 0.745143 0.040 Uiso 1 1 calc R U . . .
C22 C 0.12528(18) 0.3222(3) 0.83065(17) 0.0433(8) Uani 1 1 d . . . . .
O3 O 0.14959(19) 0.3833(3) 0.87774(14) 0.0739(10) Uani 1 1 d . . . . .
O1W O 0.58147(9) 0.66206(19) 0.68480(10) 0.0254(4) Uani 1 1 d G . . . .
H1WA H 0.586539 0.577190 0.683406 0.038 Uiso 1 1 d G U . . .
H1WB H 0.607267 0.693835 0.661329 0.038 Uiso 1 1 d G U . . .
O2W O 0.48132(10) 1.2717(2) 0.72240(9) 0.0287(4) Uani 1 1 d G . . . .
H2WA H 0.462231 1.233559 0.750746 0.043 Uiso 1 1 d G U . . .
H2WB H 0.504038 1.334931 0.741374 0.043 Uiso 1 1 d G U . . .
O3W O 0.58541(9) 0.5951(2) 0.49166(11) 0.0299(4) Uani 1 1 d G . . . .
H3WA H 0.600260 0.666121 0.511757 0.045 Uiso 1 1 d G U . . .
H3WB H 0.613348 0.534279 0.495719 0.045 Uiso 1 1 d G U . . .
O4W O -0.01896(12) 1.0528(2) 0.56701(15) 0.0468(6) Uani 1 1 d G . . . .
H4WA H -0.035350 1.096340 0.595908 0.070 Uiso 1 1 d G U . . .
O5W O 0.05041(15) 0.0728(4) 0.7357(2) 0.0726(9) Uani 1 1 d G . . . .
H5WA H 0.054963 -0.002100 0.756276 0.109 Uiso 1 1 d G U . . .
H5WB H 0.011765 0.092261 0.726744 0.109 Uiso 1 1 d G U . . .
H4WB H -0.0072(17) 1.104(4) 0.5396(19) 0.041(11) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 N1 2.650(2) . ?
Pb1 N2 2.733(2) . ?
Pb1 N3 2.7109(19) . ?
Pb1 N4 2.623(2) . ?
Pb1 N5 2.7663(19) . ?
Pb1 N6 2.753(2) . ?
Pb1 O1 2.8648(19) . ?
Pb1 O4 2.7828(17) . ?
Pb1 O7 2.6935(18) . ?
Pb1 O10 2.9217(17) . ?
C1 C2 1.397(3) . ?
C1 C18 1.516(3) . ?
C1 N1 1.336(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.385(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.389(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(3) . ?
C5 C6 1.523(3) . ?
C5 N1 1.347(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 N2 1.485(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.521(3) . ?
C7 N2 1.483(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 N3 1.481(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.521(3) . ?
C9 N3 1.477(3) . ?
C10 C11 1.395(3) . ?
C10 N4 1.342(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.385(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.393(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.387(3) . ?
C14 C15 1.520(3) . ?
C14 N4 1.344(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 N5 1.476(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.520(4) . ?
C16 N5 1.479(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 N6 1.483(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 N6 1.476(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.526(4) . ?
C19 N2 1.461(3) . ?
C20 N7 1.338(3) . ?
C20 O1 1.229(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.524(3) . ?
C23 N3 1.463(3) . ?
C24 N8 1.341(3) . ?
C24 O4 1.235(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.516(3) . ?
C25 N8 1.448(3) . ?
C26 O5 1.213(3) . ?
C26 O6 1.310(3) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.516(3) . ?
C27 N5 1.464(3) . ?
C28 N9 1.334(3) . ?
C28 O7 1.238(3) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.516(4) . ?
C29 N9 1.454(3) . ?
C30 O8 1.222(3) . ?
C30 O9 1.306(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.526(3) . ?
C31 N6 1.461(3) . ?
C32 N10 1.331(3) . ?
C32 O10 1.245(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.517(3) . ?
C33 N10 1.448(3) . ?
C34 O11 1.210(3) . ?
C34 O12 1.319(3) . ?
N1N O1N 1.241(3) . ?
N1N O2N 1.202(3) . ?
N1N O3N 1.279(3) . ?
N7 H7 0.8800 . ?
N7 C21 1.441(4) . ?
N8 H8 0.8800 . ?
N9 H9 0.8800 . ?
N10 H10 0.8800 . ?
O6 H6 0.8400 . ?
O9 H9C 0.8400 . ?
O12 H12A 0.8400 . ?
N2N O4N 1.305(4) . ?
N2N O5N 1.220(3) . ?
N2N O6N 1.182(3) . ?
O2 H2A 0.8400 . ?
O2 C22 1.336(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.497(4) . ?
C22 O3 1.207(5) . ?
O1W H1WA 0.8702 . ?
O1W H1WB 0.8713 . ?
O2W H2WA 0.8694 . ?
O2W H2WB 0.8695 . ?
O3W H3WA 0.8698 . ?
O3W H3WB 0.8699 . ?
O4W H4WA 0.8700 . ?
O4W H4WB 0.85(4) . ?
O5W H5WA 0.8699 . ?
O5W H5WB 0.8703 . ?

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 N2 65.06(6) . . ?
N1 Pb1 N3 117.60(6) . . ?
N1 Pb1 N5 114.40(6) . . ?
N1 Pb1 N6 62.87(6) . . ?
N1 Pb1 O1 108.78(6) . . ?
N1 Pb1 O4 74.72(5) . . ?
N1 Pb1 O7 70.63(6) . . ?
N1 Pb1 O10 106.62(5) . . ?
N2 Pb1 N5 141.41(6) . . ?
N2 Pb1 N6 127.93(6) . . ?
N2 Pb1 O1 59.42(6) . . ?
N2 Pb1 O4 80.24(5) . . ?
N2 Pb1 O10 142.00(5) . . ?
N3 Pb1 N2 66.52(6) . . ?
N3 Pb1 N5 128.01(6) . . ?
N3 Pb1 N6 143.00(6) . . ?
N3 Pb1 O1 76.05(6) . . ?
N3 Pb1 O4 60.34(5) . . ?
N3 Pb1 O10 89.03(5) . . ?
N4 Pb1 N1 177.99(6) . . ?
N4 Pb1 N2 115.74(6) . . ?
N4 Pb1 N3 64.25(6) . . ?
N4 Pb1 N5 63.76(6) . . ?
N4 Pb1 N6 116.28(6) . . ?
N4 Pb1 O1 70.63(6) . . ?
N4 Pb1 O4 107.17(6) . . ?
N4 Pb1 O7 107.48(6) . . ?
N4 Pb1 O10 73.93(6) . . ?
N5 Pb1 O1 87.55(6) . . ?
N5 Pb1 O4 138.22(6) . . ?
N5 Pb1 O10 76.54(5) . . ?
N6 Pb1 N5 65.63(6) . . ?
N6 Pb1 O1 140.76(6) . . ?
N6 Pb1 O4 86.82(5) . . ?
N6 Pb1 O10 58.68(5) . . ?
O1 Pb1 O10 144.57(5) . . ?
O4 Pb1 O1 129.88(5) . . ?
O4 Pb1 O10 62.11(5) . . ?
O7 Pb1 N2 85.57(6) . . ?
O7 Pb1 N3 139.53(6) . . ?
O7 Pb1 N5 60.68(6) . . ?
O7 Pb1 N6 77.29(6) . . ?
O7 Pb1 O1 64.37(6) . . ?
O7 Pb1 O4 145.34(5) . . ?
O7 Pb1 O10 128.41(5) . . ?
C2 C1 C18 119.2(2) . . ?
N1 C1 C2 121.7(2) . . ?
N1 C1 C18 118.9(2) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.4(2) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.6(2) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.8(2) . . ?
C5 C4 H4 120.6 . . ?
C4 C5 C6 121.8(2) . . ?
N1 C5 C4 121.7(2) . . ?
N1 C5 C6 116.5(2) . . ?
C5 C6 H6A 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N2 C6 C5 111.15(19) . . ?
N2 C6 H6A 109.4 . . ?
N2 C6 H6B 109.4 . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
N2 C7 H7A 108.9 . . ?
N2 C7 H7B 108.9 . . ?
N2 C7 C8 113.34(19) . . ?
C7 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
N3 C8 C7 112.98(19) . . ?
N3 C8 H8A 109.0 . . ?
N3 C8 H8B 109.0 . . ?
H9A C9 H9B 107.7 . . ?
C10 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
N3 C9 H9A 108.8 . . ?
N3 C9 H9B 108.8 . . ?
N3 C9 C10 113.94(19) . . ?
C11 C10 C9 120.6(2) . . ?
N4 C10 C9 118.1(2) . . ?
N4 C10 C11 121.2(2) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 C10 119.0(2) . . ?
C12 C11 H11 120.5 . . ?
C11 C12 H12 120.3 . . ?
C11 C12 C13 119.3(2) . . ?
C13 C12 H12 120.3 . . ?
C12 C13 H13 120.6 . . ?
C14 C13 C12 118.7(2) . . ?
C14 C13 H13 120.6 . . ?
C13 C14 C15 120.5(2) . . ?
N4 C14 C13 121.7(2) . . ?
N4 C14 C15 117.8(2) . . ?
C14 C15 H15A 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
N5 C15 C14 112.9(2) . . ?
N5 C15 H15A 109.0 . . ?
N5 C15 H15B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C17 C16 H16A 109.0 . . ?
C17 C16 H16B 109.0 . . ?
N5 C16 H16A 109.0 . . ?
N5 C16 H16B 109.0 . . ?
N5 C16 C17 113.07(19) . . ?
C16 C17 H17A 109.0 . . ?
C16 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
N6 C17 C16 113.0(2) . . ?
N6 C17 H17A 109.0 . . ?
N6 C17 H17B 109.0 . . ?
C1 C18 H18A 108.5 . . ?
C1 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
N6 C18 C1 115.25(19) . . ?
N6 C18 H18A 108.5 . . ?
N6 C18 H18B 108.5 . . ?
H19A C19 H19B 108.1 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
N2 C19 C20 110.7(2) . . ?
N7 C20 C19 114.1(2) . . ?
O1 C20 C19 122.1(2) . . ?
O1 C20 N7 123.8(2) . . ?
H23A C23 H23B 108.1 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
N3 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
N3 C23 C24 110.73(19) . . ?
N8 C24 C23 114.9(2) . . ?
O4 C24 C23 122.6(2) . . ?
O4 C24 N8 122.4(2) . . ?
H25A C25 H25B 107.8 . . ?
C26 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
N8 C25 H25A 109.1 . . ?
N8 C25 H25B 109.1 . . ?
N8 C25 C26 112.6(2) . . ?
O5 C26 C25 124.5(2) . . ?
O5 C26 O6 123.8(2) . . ?
O6 C26 C25 111.6(2) . . ?
H27A C27 H27B 108.1 . . ?
C28 C27 H27A 109.6 . . ?
C28 C27 H27B 109.6 . . ?
N5 C27 H27A 109.6 . . ?
N5 C27 H27B 109.6 . . ?
N5 C27 C28 110.4(2) . . ?
N9 C28 C27 116.8(2) . . ?
O7 C28 C27 122.2(2) . . ?
O7 C28 N9 121.0(2) . . ?
H29A C29 H29B 107.8 . . ?
C30 C29 H29A 109.1 . . ?
C30 C29 H29B 109.1 . . ?
N9 C29 H29A 109.1 . . ?
N9 C29 H29B 109.1 . . ?
N9 C29 C30 112.5(2) . . ?
O8 C30 C29 122.7(2) . . ?
O8 C30 O9 124.8(3) . . ?
O9 C30 C29 112.4(2) . . ?
H31A C31 H31B 107.9 . . ?
C32 C31 H31A 109.1 . . ?
C32 C31 H31B 109.1 . . ?
N6 C31 H31A 109.1 . . ?
N6 C31 H31B 109.1 . . ?
N6 C31 C32 112.37(19) . . ?
N10 C32 C31 114.6(2) . . ?
O10 C32 C31 121.9(2) . . ?
O10 C32 N10 123.5(2) . . ?
H33A C33 H33B 107.8 . . ?
C34 C33 H33A 109.0 . . ?
C34 C33 H33B 109.0 . . ?
N10 C33 H33A 109.0 . . ?
N10 C33 H33B 109.0 . . ?
N10 C33 C34 113.1(2) . . ?
O11 C34 C33 123.8(2) . . ?
O11 C34 O12 121.0(2) . . ?
O12 C34 C33 115.2(2) . . ?
C1 N1 Pb1 119.13(15) . . ?
C1 N1 C5 119.7(2) . . ?
C5 N1 Pb1 117.51(15) . . ?
O1N N1N O3N 116.9(3) . . ?
O2N N1N O1N 124.0(3) . . ?
O2N N1N O3N 119.0(3) . . ?
C6 N2 Pb1 106.55(14) . . ?
C7 N2 Pb1 112.29(14) . . ?
C7 N2 C6 110.50(19) . . ?
C19 N2 Pb1 105.61(14) . . ?
C19 N2 C6 111.3(2) . . ?
C19 N2 C7 110.41(19) . . ?
C8 N3 Pb1 111.68(14) . . ?
C9 N3 Pb1 108.12(14) . . ?
C9 N3 C8 111.37(18) . . ?
C23 N3 Pb1 104.86(13) . . ?
C23 N3 C8 109.89(18) . . ?
C23 N3 C9 110.73(19) . . ?
C10 N4 Pb1 119.04(15) . . ?
C10 N4 C14 120.0(2) . . ?
C14 N4 Pb1 120.66(15) . . ?
C15 N5 Pb1 108.17(13) . . ?
C15 N5 C16 111.33(19) . . ?
C16 N5 Pb1 112.34(14) . . ?
C27 N5 Pb1 103.29(14) . . ?
C27 N5 C15 111.06(19) . . ?
C27 N5 C16 110.38(19) . . ?
C17 N6 Pb1 111.98(14) . . ?
C18 N6 Pb1 109.72(14) . . ?
C18 N6 C17 110.25(18) . . ?
C31 N6 Pb1 104.09(13) . . ?
C31 N6 C17 110.43(19) . . ?
C31 N6 C18 110.22(19) . . ?
C20 N7 H7 118.4 . . ?
C20 N7 C21 123.1(3) . . ?
C21 N7 H7 118.4 . . ?
C24 N8 C25 121.1(2) . . ?
C24 N8 H8 119.4 . . ?
C25 N8 H8 119.4 . . ?
C28 N9 C29 118.4(2) . . ?
C28 N9 H9 120.8 . . ?
C29 N9 H9 120.8 . . ?
C32 N10 C33 122.6(2) . . ?
C32 N10 H10 118.7 . . ?
C33 N10 H10 118.7 . . ?
C20 O1 Pb1 111.73(16) . . ?
C24 O4 Pb1 110.64(14) . . ?
C26 O6 H6 109.5 . . ?
C28 O7 Pb1 114.21(15) . . ?
C30 O9 H9C 109.5 . . ?
C32 O10 Pb1 107.68(14) . . ?
C34 O12 H12A 109.5 . . ?
O5N N2N O4N 115.7(2) . . ?
O6N N2N O4N 119.0(3) . . ?
O6N N2N O5N 125.3(3) . . ?
C22 O2 H2A 109.5 . . ?
N7 C21 H21A 109.0 . . ?
N7 C21 H21B 109.0 . . ?
N7 C21 C22 112.9(3) . . ?
H21A C21 H21B 107.8 . . ?
C22 C21 H21A 109.0 . . ?
C22 C21 H21B 109.0 . . ?
O2 C22 C21 116.0(3) . . ?
O3 C22 O2 120.6(3) . . ?
O3 C22 C21 123.4(3) . . ?
H1WA O1W H1WB 104.4 . . ?
H2WA O2W H2WB 109.5 . . ?
H3WA O3W H3WB 109.5 . . ?
H4WA O4W H4WB 111.0 . . ?
H5WA O5W H5WB 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
C1 C2 C3 C4 1.9(4) . . . . ?
C1 C18 N6 Pb1 37.3(2) . . . . ?
C1 C18 N6 C17 161.1(2) . . . . ?
C1 C18 N6 C31 -76.8(3) . . . . ?
C2 C1 C18 N6 167.8(2) . . . . ?
C2 C1 N1 Pb1 159.55(18) . . . . ?
C2 C1 N1 C5 1.6(3) . . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C3 C4 C5 C6 179.5(2) . . . . ?
C3 C4 C5 N1 -0.4(4) . . . . ?
C4 C5 C6 N2 128.2(2) . . . . ?
C4 C5 N1 Pb1 -158.46(19) . . . . ?
C4 C5 N1 C1 -0.2(4) . . . . ?
C5 C6 N2 Pb1 51.2(2) . . . . ?
C5 C6 N2 C7 173.48(19) . . . . ?
C5 C6 N2 C19 -63.4(3) . . . . ?
C6 C5 N1 Pb1 21.7(3) . . . . ?
C6 C5 N1 C1 179.9(2) . . . . ?
C7 C8 N3 Pb1 44.5(2) . . . . ?
C7 C8 N3 C9 -76.5(2) . . . . ?
C7 C8 N3 C23 160.46(19) . . . . ?
C8 C7 N2 Pb1 37.8(2) . . . . ?
C8 C7 N2 C6 -81.0(2) . . . . ?
C8 C7 N2 C19 155.4(2) . . . . ?
C9 C10 C11 C12 176.9(2) . . . . ?
C9 C10 N4 Pb1 -2.6(3) . . . . ?
C9 C10 N4 C14 -176.3(2) . . . . ?
C10 C9 N3 Pb1 44.7(2) . . . . ?
C10 C9 N3 C8 167.7(2) . . . . ?
C10 C9 N3 C23 -69.7(3) . . . . ?
C10 C11 C12 C13 -0.4(4) . . . . ?
C11 C10 N4 Pb1 174.66(18) . . . . ?
C11 C10 N4 C14 0.9(4) . . . . ?
C11 C12 C13 C14 0.3(4) . . . . ?
C12 C13 C14 C15 178.2(2) . . . . ?
C12 C13 C14 N4 0.4(4) . . . . ?
C13 C14 C15 N5 144.1(2) . . . . ?
C13 C14 N4 Pb1 -174.61(17) . . . . ?
C13 C14 N4 C10 -1.0(4) . . . . ?
C14 C15 N5 Pb1 45.4(2) . . . . ?
C14 C15 N5 C16 169.28(19) . . . . ?
C14 C15 N5 C27 -67.3(2) . . . . ?
C15 C14 N4 Pb1 7.5(3) . . . . ?
C15 C14 N4 C10 -178.9(2) . . . . ?
C16 C17 N6 Pb1 43.6(2) . . . . ?
C16 C17 N6 C18 -78.9(2) . . . . ?
C16 C17 N6 C31 159.07(19) . . . . ?
C17 C16 N5 Pb1 40.5(2) . . . . ?
C17 C16 N5 C15 -81.0(2) . . . . ?
C17 C16 N5 C27 155.1(2) . . . . ?
C18 C1 C2 C3 173.2(2) . . . . ?
C18 C1 N1 Pb1 -16.1(3) . . . . ?
C18 C1 N1 C5 -174.1(2) . . . . ?
C19 C20 N7 C21 -178.8(2) . . . . ?
C19 C20 O1 Pb1 -16.0(3) . . . . ?
C20 C19 N2 Pb1 56.7(2) . . . . ?
C20 C19 N2 C6 171.9(2) . . . . ?
C20 C19 N2 C7 -64.9(3) . . . . ?
C20 N7 C21 C22 119.9(3) . . . . ?
C23 C24 N8 C25 -176.4(2) . . . . ?
C23 C24 O4 Pb1 -23.5(3) . . . . ?
C24 C23 N3 Pb1 53.09(19) . . . . ?
C24 C23 N3 C8 -67.1(2) . . . . ?
C24 C23 N3 C9 169.48(18) . . . . ?
C26 C25 N8 C24 76.9(3) . . . . ?
C27 C28 N9 C29 172.6(2) . . . . ?
C27 C28 O7 Pb1 -19.4(3) . . . . ?
C28 C27 N5 Pb1 52.5(2) . . . . ?
C28 C27 N5 C15 168.21(19) . . . . ?
C28 C27 N5 C16 -67.8(2) . . . . ?
C30 C29 N9 C28 62.8(3) . . . . ?
C31 C32 N10 C33 176.2(2) . . . . ?
C31 C32 O10 Pb1 -27.5(2) . . . . ?
C32 C31 N6 Pb1 56.3(2) . . . . ?
C32 C31 N6 C17 -64.0(2) . . . . ?
C32 C31 N6 C18 173.91(19) . . . . ?
C34 C33 N10 C32 85.0(3) . . . . ?
N1 C1 C2 C3 -2.5(4) . . . . ?
N1 C1 C18 N6 -16.4(3) . . . . ?
N1 C5 C6 N2 -51.9(3) . . . . ?
N2 C7 C8 N3 -57.1(3) . . . . ?
N2 C19 C20 N7 153.2(2) . . . . ?
N2 C19 C20 O1 -28.1(3) . . . . ?
N3 C9 C10 C11 152.2(2) . . . . ?
N3 C9 C10 N4 -30.6(3) . . . . ?
N3 C23 C24 N8 160.76(19) . . . . ?
N3 C23 C24 O4 -20.9(3) . . . . ?
N4 C10 C11 C12 -0.2(4) . . . . ?
N4 C14 C15 N5 -38.0(3) . . . . ?
N5 C16 C17 N6 -58.3(3) . . . . ?
N5 C27 C28 N9 156.6(2) . . . . ?
N5 C27 C28 O7 -25.8(3) . . . . ?
N6 C31 C32 N10 164.1(2) . . . . ?
N6 C31 C32 O10 -18.8(3) . . . . ?
N7 C20 O1 Pb1 162.6(2) . . . . ?
N7 C21 C22 O2 175.5(3) . . . . ?
N7 C21 C22 O3 -3.6(6) . . . . ?
N8 C24 O4 Pb1 154.71(18) . . . . ?
N8 C25 C26 O5 -7.2(4) . . . . ?
N8 C25 C26 O6 174.6(2) . . . . ?
N9 C28 O7 Pb1 158.05(19) . . . . ?
N9 C29 C30 O8 38.5(3) . . . . ?
N9 C29 C30 O9 -143.2(2) . . . . ?
N10 C32 O10 Pb1 149.37(19) . . . . ?
N10 C33 C34 O11 -2.3(4) . . . . ?
N10 C33 C34 O12 177.3(2) . . . . ?
O1 C20 N7 C21 2.5(4) . . . . ?
O4 C24 N8 C25 5.2(3) . . . . ?
O7 C28 N9 C29 -5.0(4) . . . . ?
O10 C32 N10 C33 -0.9(4) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.253 0.163 0.804 38.0 7.1 ?
2 0.253 0.337 0.304 38.0 7.0 ?
3 0.747 0.663 0.696 38.0 8.0 ?
4 0.747 0.837 0.196 38.0 7.9 ?

_olex2_submission_special_instructions 'No special instructions were received'
