# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_tt
_database_code_depnum_ccdc_archive 'CCDC 1537811'
_audit_update_record             
;
2017-06-05 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_audit_creation_date             2017-06-05
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.05.22 svn.r3414 for OlexSys, GUI svn.r5347)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C24 H8 N56 Pb4), O'
_chemical_formula_sum            'C6 H2 N14 O Pb'
_chemical_formula_weight         493.41
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'x+1/2, -y, -z+1/2'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'-x-1/2, y, z-1/2'
'x, -y, z-1/2'

_cell_length_a                   13.743(4)
_cell_length_b                   6.963(2)
_cell_length_c                   13.777(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1318.4(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2546
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.57
_cell_measurement_theta_min      3.26
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.827
_exptl_absorpt_correction_T_max  0.245
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker;SADABS;2012
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.486
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7862
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.297
_diffrn_reflns_theta_min         1.478
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1424
_reflns_number_total             1522
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.453
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.357
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1522
_refine_ls_number_restraints     194
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0574
_refine_ls_restrained_S_all      1.129
_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)+28.0998P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1394
_refine_special_details          
;
 Refined as a 4-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 3(10)
 0.12(6) -2(10) 0.30(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Shared sites
{C4, N7}
{C9, N8}
4. Restrained distances
 C1_$1-C1_$2 = C1-C1_$3
 1.455 with sigma of 0.001
5. Uiso/Uaniso restraints and constraints
N3 \\sim C9 \\sim C2 \\sim N1 \\sim N2: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(N7) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(N4) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N8) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C4) = Uanis(N7)
Uanis(C9) = Uanis(N8)
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Fixed Sof: C4(0.5) H4(0.5) N7(0.5) C9(0.5) H9(0.5) N8(0.5)
8.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C9(H9)
;
_atom_sites_solution_hydrogens   geom
_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 0.2500 1.0000 0.46875(6) 0.0447(3) Uani 1 2 d S TU P . .
C1 C 0.2740(9) 0.9069(9) 0.7205(13) 0.040(4) Uani 1 1 d D U . . .
N3 N 0.5858(10) 0.8077(18) 0.4574(12) 0.041(2) Uani 1 1 d . U . . .
C4 C 0.3428(12) 0.646(2) 0.7716(13) 0.047(3) Uani 0.5 1 d . U . . .
H4 H 0.3660 0.5442 0.8111 0.057 Uiso 0.5 1 calc R . . . .
N7 N 0.3428(12) 0.646(2) 0.7716(13) 0.047(3) Uani 0.5 1 d . U . . .
N6 N 0.2987(11) 0.817(2) 0.8058(11) 0.047(3) Uani 1 1 d . U . . .
N4 N 0.3014(11) 0.8158(19) 0.6424(10) 0.043(3) Uani 1 1 d . U . . .
C9 C 0.4615(10) 0.670(2) 0.3971(12) 0.038(2) Uani 0.5 1 d . U . . .
H9 H 0.4253 0.5737 0.3643 0.046 Uiso 0.5 1 calc R . . . .
N8 N 0.4615(10) 0.670(2) 0.3971(12) 0.038(2) Uani 0.5 1 d . U . . .
N5 N 0.3465(11) 0.653(2) 0.6760(11) 0.045(3) Uani 1 1 d . U . . .
C2 C 0.5013(17) 0.913(2) 0.4784(14) 0.043(3) Uani 1 1 d . U . . .
N1 N 0.4221(9) 0.8199(18) 0.4327(11) 0.040(2) Uani 1 1 d . U . . .
N2 N 0.5531(10) 0.6597(18) 0.4090(11) 0.041(2) Uani 1 1 d . U . . .
O1 O 0.2500 1.5000 0.476(3) 0.18(2) Uani 1 2 d S TU 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 N6 2.668(15) 7_655 ?
Pb1 N6 2.668(15) 8_575 ?
Pb1 N4 2.805(14) . ?
Pb1 N1 2.723(13) 2_575 ?
Pb1 N1 2.723(13) . ?
C1 C1 1.4550(8) 2_575 ?
C1 N6 1.37(2) . ?
C1 N4 1.30(2) . ?
N3 C2 1.40(2) . ?
N3 N2 1.307(18) . ?
C4 N6 1.41(2) . ?
C4 N5 1.32(2) . ?
N6 Pb1 2.668(15) 7_656 ?
N4 N5 1.375(18) . ?
C9 N1 1.273(18) . ?
C9 N2 1.272(18) . ?
C2 C2 1.35(3) 5_676 ?
C2 N1 1.41(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Pb1 N6 65.4(6) 7_655 8_575 ?
N6 Pb1 N4 150.8(5) 8_575 . ?
N6 Pb1 N4 124.2(4) 7_655 . ?
N6 Pb1 N1 81.3(4) 7_655 2_575 ?
N6 Pb1 N1 81.3(4) 8_575 . ?
N6 Pb1 N1 81.1(5) 8_575 2_575 ?
N6 Pb1 N1 81.1(5) 7_655 . ?
N1 Pb1 N4 125.8(4) 2_575 . ?
N1 Pb1 N4 74.1(4) . . ?
N1 Pb1 N1 159.0(6) . 2_575 ?
N6 C1 C1 121.2(7) . 2_575 ?
N4 C1 C1 124.4(8) . 2_575 ?
N4 C1 N6 114.3(9) . . ?
N2 N3 C2 103.4(13) . . ?
N5 C4 N6 108.7(14) . . ?
C1 N6 Pb1 116.1(9) . 7_656 ?
C1 N6 C4 101.8(13) . . ?
C4 N6 Pb1 142.1(11) . 7_656 ?
C1 N4 Pb1 114.1(9) . . ?
C1 N4 N5 104.8(12) . . ?
N5 N4 Pb1 141.1(10) . . ?
N2 C9 N1 114.6(13) . . ?
C4 N5 N4 110.2(13) . . ?
N3 C2 N1 107.8(13) . . ?
C2 C2 N3 125(3) 5_676 . ?
C2 C2 N1 126(3) 5_676 . ?
C9 N1 Pb1 144.7(10) . . ?
C9 N1 C2 102.7(13) . . ?
C2 N1 Pb1 112.1(10) . . ?
C9 N2 N3 111.2(13) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 3(10)
2 0.12(6)
3 -2(10)
4 0.30(6)

####################################################################### 
# 
# 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_zz
_database_code_depnum_ccdc_archive 'CCDC 1534609'
_audit_update_record             
;
2017-02-24 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_audit_creation_date             2016-12-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H3 Ag N4'
_chemical_formula_sum            'C2 H3 Ag N4'
_chemical_formula_weight         190.95
_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'
Ag Ag -0.8971 1.1015 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   9.9881(3)
_cell_length_b                   11.4508(3)
_cell_length_c                   7.5151(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.850(2)
_cell_angle_gamma                90
_cell_volume                     846.84(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6679
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.73
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.594
_exptl_absorpt_correction_T_max  0.5321
_exptl_absorpt_correction_T_min  0.4521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0710 before and 0.0345 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0827 before and 0.0342 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 14067 reflections, Rint = 0.0319
 (10476 with I > 3sig(I), Rint = 0.0310)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.995
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1881
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.516
_diffrn_reflns_theta_min         2.729
_diffrn_ambient_temperature      170
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                912
_reflns_number_total             969
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         969
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0152
_refine_ls_restrained_S_all      1.157
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0157P)²+1.5187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0379
_refine_ls_wR_factor_ref         0.0385
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_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
Ag1 Ag 0.12821(2) 0.88032(2) 0.12541(2) 0.02329(8) Uani 1 1 d . . . . .
N1 N 0.27494(19) 0.74563(16) 0.2455(3) 0.0175(4) Uani 1 1 d . . . . .
N3 N 0.3550(2) 0.57551(17) 0.3302(3) 0.0192(4) Uani 1 1 d . . . . .
N2 N 0.2618(2) 0.62954(16) 0.2152(3) 0.0210(4) Uani 1 1 d . . . . .
N4 N 0.43083(19) 0.65488(17) 0.4366(3) 0.0180(4) Uani 1 1 d . . . . .
C1 C 0.3799(2) 0.75835(19) 0.3810(3) 0.0163(4) Uani 1 1 d . . . . .
C2 C 0.4328(3) 0.8719(2) 0.4577(3) 0.0231(5) Uani 1 1 d . . . . .
H2A H 0.5282 0.8802 0.4440 0.035 Uiso 1 1 calc GR . . . .
H2B H 0.4258 0.8749 0.5861 0.035 Uiso 1 1 calc GR . . . .
H2C H 0.3794 0.9355 0.3935 0.035 Uiso 1 1 calc GR . . . .


_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
Ag1 N1 2.2111(18) . ?
Ag1 N3 2.262(2) 4 ?
Ag1 N4 2.2595(19) 8_465 ?
N1 N2 1.351(2) . ?
N1 C1 1.338(3) . ?
N3 Ag1 2.262(2) 4_545 ?
N3 N2 1.312(3) . ?
N3 N4 1.354(3) . ?
N4 Ag1 2.2595(19) 8_566 ?
N4 C1 1.328(3) . ?
C1 C2 1.482(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ag1 N3 127.00(7) . 4 ?
N1 Ag1 N4 125.32(7) . 8_465 ?
N4 Ag1 N3 107.68(7) 8_465 4 ?
N2 N1 Ag1 125.37(15) . . ?
C1 N1 Ag1 127.79(15) . . ?
C1 N1 N2 106.04(18) . . ?
N2 N3 Ag1 126.12(15) . 4_545 ?
N2 N3 N4 109.57(18) . . ?
N4 N3 Ag1 123.81(15) . 4_545 ?
N3 N2 N1 108.37(18) . . ?
N3 N4 Ag1 126.24(15) . 8_566 ?
C1 N4 Ag1 127.07(15) . 8_566 ?
C1 N4 N3 105.51(17) . . ?
N1 C1 C2 124.9(2) . . ?
N4 C1 N1 110.50(19) . . ?
N4 C1 C2 124.62(19) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 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
Ag1 N1 N2 N3 -169.76(14) . . . . ?
Ag1 N1 C1 N4 169.35(14) . . . . ?
Ag1 N1 C1 C2 -11.1(3) . . . . ?
Ag1 N3 N2 N1 171.79(15) 4_545 . . . ?
Ag1 N3 N4 Ag1 19.3(2) 4_545 . . 8_566 ?
Ag1 N3 N4 C1 -172.45(15) 4_545 . . . ?
Ag1 N4 C1 N1 168.66(15) 8_566 . . . ?
Ag1 N4 C1 C2 -10.9(3) 8_566 . . . ?
N3 N4 C1 N1 0.5(2) . . . . ?
N3 N4 C1 C2 -179.0(2) . . . . ?
N2 N1 C1 N4 -0.7(3) . . . . ?
N2 N1 C1 C2 178.8(2) . . . . ?
N2 N3 N4 Ag1 -168.39(15) . . . 8_566 ?
N2 N3 N4 C1 -0.1(2) . . . . ?
N4 N3 N2 N1 -0.3(3) . . . . ?
C1 N1 N2 N3 0.6(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_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_tt_sq_s
_database_code_depnum_ccdc_archive 'CCDC 1534610'
_audit_update_record             
;
2017-02-24 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_audit_creation_date             2016-12-27
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C36 H54 Cd10 N72)'
_chemical_formula_sum            'C18 H27 Cd5 N36'
_chemical_formula_weight         1309.75
_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'
Cd Cd -0.8075 1.2024 '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'

_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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   13.149(2)
_cell_length_b                   13.149(2)
_cell_length_c                   13.596(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2035.8(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    692
_cell_measurement_temperature    205
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.636
_exptl_absorpt_correction_T_max  0.2616
_exptl_absorpt_correction_T_min  0.2210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0633 before and 0.0534 after correction. The Ratio of minimum to maximum transmission is 0.8448. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7105
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.473
_diffrn_reflns_theta_min         1.788
_diffrn_ambient_temperature      205
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                715
_reflns_number_total             892
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.089
_refine_diff_density_min         -3.522
_refine_diff_density_rms         0.278
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         892
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0624
_refine_ls_restrained_S_all      1.047
_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)+(0.1270P)²+23.4220P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2023
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C3, N5}
3. Restrained distances
 C2-C1
 1.54 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C3) = Uanis(N5)
5. Others
 Fixed Sof: C3(0.5) N5(0.5) H2A(0.25) H2C(0.25) H2B(0.25) C4(0.5) H4A(0.5)
 H4B(0.5) H4C(0.5)
6.a Riding coordinates:
 C2(H2A,H2C,H2B)
6.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C)
;
_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
Cd01 Cd 0.5000 0.0000 0.5000 0.0155(4) Uani 1 4 d S T P A .
Cd02 Cd 0.6667 0.3333 0.60209(12) 0.0233(5) Uani 1 6 d S T P . .
N1 N 0.5824(4) 0.1649(8) 0.7026(7) 0.0168(19) Uani 1 2 d S T P . .
N2 N 0.5259(4) 0.0518(8) 0.6689(7) 0.0142(18) Uani 1 2 d S T P . .
N3 N 0.4413(6) 0.1382(6) 0.4672(5) 0.0177(14) Uani 1 1 d . . . . .
N4 N 0.4978(8) 0.2489(4) 0.5002(7) 0.018(2) Uani 1 2 d S T P A .
C3 C 0.3513(7) 0.1255(8) 0.4140(6) 0.0281(19) Uani 0.5 1 d . . . A 1
N5 N 0.3513(7) 0.1255(8) 0.4140(6) 0.0281(19) Uani 0.5 1 d . . . A 2
C1 C 0.4927(6) -0.0146(13) 0.7500 0.017(3) Uani 1 4 d DS TU P . .
C2 C 0.4264(7) -0.1473(14) 0.7500 0.029(4) Uani 1 4 d DS TU P . .
H2A H 0.3527 -0.1755 0.7167 0.044 Uiso 0.25 1 d R . . . .
H2C H 0.4719 -0.1755 0.7167 0.044 Uiso 0.25 1 d R . . . .
H2B H 0.4123 -0.1754 0.8166 0.044 Uiso 0.5 2 d RS T P . .
C4 C 0.260(2) 0.024(2) 0.365(2) 0.043(6) Uani 0.5 1 d . U . . .
H4A H 0.2731 -0.0413 0.3722 0.064 Uiso 0.5 1 calc R . . A 2
H4B H 0.1844 0.0044 0.3938 0.064 Uiso 0.5 1 calc R . . A 2
H4C H 0.2593 0.0419 0.2957 0.064 Uiso 0.5 1 calc R . . A 2


_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
Cd01 N2 2.371(9) 13_656 ?
Cd01 N2 2.371(9) . ?
Cd01 N3 2.345(7) 8_556 ?
Cd01 N3 2.345(7) 20_655 ?
Cd01 N3 2.345(6) 13_656 ?
Cd01 N3 2.345(6) . ?
Cd02 N1 2.356(9) . ?
Cd02 N1 2.356(9) 2_655 ?
Cd02 N1 2.356(9) 3_665 ?
Cd02 N4 2.370(10) 2_655 ?
Cd02 N4 2.370(10) 3_665 ?
Cd02 N4 2.370(10) . ?
N1 N1 1.29(2) 16_557 ?
N1 N2 1.366(13) . ?
N2 C1 1.338(13) . ?
N3 N4 1.338(9) . ?
N3 C3 1.324(11) . ?
N3 N5 1.324(11) . ?
N4 N3 1.338(9) 21 ?
C3 C3 1.32(2) 21 ?
C3 C4 1.44(3) . ?
N5 N5 1.32(2) 21 ?
N5 C4 1.44(3) . ?
C1 N2 1.338(13) 16_557 ?
C1 C2 1.510(16) . ?
C2 H2A 0.9598 . ?
C2 H2C 0.9609 . ?
C2 H2B 0.9600 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?

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 Cd01 N2 180.00(11) . 13_656 ?
N3 Cd01 N2 91.0(2) 13_656 13_656 ?
N3 Cd01 N2 89.0(2) 20_655 13_656 ?
N3 Cd01 N2 89.0(2) . 13_656 ?
N3 Cd01 N2 91.0(2) 20_655 . ?
N3 Cd01 N2 89.0(2) 13_656 . ?
N3 Cd01 N2 89.0(2) 8_556 . ?
N3 Cd01 N2 91.0(2) 8_556 13_656 ?
N3 Cd01 N2 91.0(2) . . ?
N3 Cd01 N3 88.4(4) 8_556 . ?
N3 Cd01 N3 88.4(4) 20_655 13_656 ?
N3 Cd01 N3 180.0 20_655 8_556 ?
N3 Cd01 N3 180.0 . 13_656 ?
N3 Cd01 N3 91.6(4) 8_556 13_656 ?
N3 Cd01 N3 91.6(4) 20_655 . ?
N1 Cd02 N1 89.7(4) . 2_655 ?
N1 Cd02 N1 89.7(4) . 3_665 ?
N1 Cd02 N1 89.7(4) 2_655 3_665 ?
N1 Cd02 N4 90.5(2) . 2_655 ?
N1 Cd02 N4 179.7(3) 3_665 2_655 ?
N1 Cd02 N4 90.5(2) 2_655 2_655 ?
N1 Cd02 N4 179.7(3) . 3_665 ?
N1 Cd02 N4 90.5(2) 2_655 3_665 ?
N1 Cd02 N4 90.5(2) . . ?
N1 Cd02 N4 90.5(2) 3_665 3_665 ?
N1 Cd02 N4 179.7(4) 2_655 . ?
N1 Cd02 N4 90.5(2) 3_665 . ?
N4 Cd02 N4 89.3(3) 2_655 3_665 ?
N4 Cd02 N4 89.3(3) . 3_665 ?
N4 Cd02 N4 89.3(3) 2_655 . ?
N1 N1 Cd02 125.5(2) 16_557 . ?
N1 N1 N2 109.6(6) 16_557 . ?
N2 N1 Cd02 124.9(7) . . ?
N1 N2 Cd01 124.1(7) . . ?
C1 N2 Cd01 131.1(8) . . ?
C1 N2 N1 104.8(9) . . ?
N4 N3 Cd01 124.1(6) . . ?
C3 N3 Cd01 128.7(6) . . ?
C3 N3 N4 107.2(7) . . ?
N5 N3 Cd01 128.7(6) . . ?
N5 N3 N4 107.2(7) . . ?
N3 N4 Cd02 125.9(5) . . ?
N3 N4 Cd02 125.9(5) 21 . ?
N3 N4 N3 108.3(9) 21 . ?
N3 C3 C4 130.9(13) . . ?
C3 C3 N3 108.7(5) 21 . ?
C3 C3 C4 120.3(11) 21 . ?
N3 N5 C4 130.9(13) . . ?
N5 N5 N3 108.7(5) 21 . ?
N5 N5 C4 120.3(11) 21 . ?
N2 C1 N2 111.1(13) 16_557 . ?
N2 C1 C2 124.5(6) . . ?
N2 C1 C2 124.5(6) 16_557 . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2C 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2C 109.4 . . ?
H2A C2 H2B 109.4 . . ?
H2C C2 H2B 109.4 . . ?
N5 C4 H4A 109.5 . . ?
N5 C4 H4B 109.5 . . ?
N5 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.036 99 46 ' '

_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_mo_2017020_0m
_database_code_depnum_ccdc_archive 'CCDC 1534611'
_audit_update_record             
;
2017-02-24 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_audit_creation_date             2017-01-10
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H2 N18 O2 Pb3, H2 O'
_chemical_formula_sum            'C4 H4 N18 O3 Pb3'
_chemical_formula_weight         973.82
_chemical_absolute_configuration syn
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   10.106(3)
_cell_length_b                   10.342(3)
_cell_length_c                   15.143(5)
_cell_angle_alpha                90
_cell_angle_beta                 99.523(5)
_cell_angle_gamma                90
_cell_volume                     1560.9(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1441
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.428
_cell_measurement_theta_min      2.73
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    32.340
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1430 before and 0.0681 after correction. The Ratio of minimum to maximum transmission is 0.3042. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.144
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9022
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         2.728
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    0.950
_reflns_Friedel_fraction_max     0.925
_reflns_number_gt                3306
_reflns_number_total             3458
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.548
_refine_diff_density_min         -3.050
_refine_diff_density_rms         0.493
_refine_ls_abs_structure_details 
;
 Flack x determined using 1434 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         3458
_refine_ls_number_restraints     246
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0483
_refine_ls_restrained_S_all      1.047
_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)+(0.0670P)²+13.7430P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1167
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H3A-H3B
 1.46 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Free rotating group:
 O3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 N14(H14), N1AA(H1AA)
;
_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 0.31301(8) 0.18574(9) 0.30394(6) 0.0217(2) Uani 1 1 d . U . . .
Pb3 Pb 0.50354(10) 0.51767(8) 0.43161(7) 0.0211(2) Uani 1 1 d . U . . .
Pb2 Pb 0.38907(7) 0.17461(9) 0.55276(5) 0.0226(2) Uani 1 1 d . U . . .
N12 N 1.072(2) 0.276(2) 0.3090(14) 0.019(4) Uani 1 1 d . U . . .
N8 N 1.031(2) 0.385(2) 0.2659(16) 0.025(4) Uani 1 1 d . U . . .
O1 O 0.344(2) 0.3106(16) 0.4327(15) 0.023(3) Uani 1 1 d . U . . .
N11 N 0.965(2) 0.218(2) 0.3381(14) 0.021(4) Uani 1 1 d . U . . .
N1 N 0.521(2) 0.548(2) 0.7289(15) 0.025(4) Uani 1 1 d . U . . .
N13 N 0.894(2) 0.401(2) 0.2643(15) 0.024(4) Uani 1 1 d . U . . .
N7 N -0.014(3) 0.366(3) 0.6151(18) 0.037(6) Uani 1 1 d . U . . .
N4 N -0.055(3) 0.262(3) 0.566(2) 0.038(6) Uani 1 1 d . U . . .
O2 O 0.2523(16) 0.0609(17) 0.4244(12) 0.020(3) Uani 1 1 d . U . . .
N3 N 0.393(2) 0.560(2) 0.7387(16) 0.025(4) Uani 1 1 d . U . . .
N0AA N 0.412(2) 0.402(2) 0.6417(15) 0.024(4) Uani 1 1 d . U . . .
N2 N 0.538(2) 0.452(2) 0.6724(16) 0.025(4) Uani 1 1 d . U . . .
C7 C 0.862(3) 0.299(3) 0.309(2) 0.030(6) Uani 1 1 d . U . . .
O3 O 0.653(3) 0.303(3) 0.557(2) 0.049(6) Uani 1 1 d . U . . .
H3A H 0.7060 0.2717 0.6007 0.073 Uiso 1 1 d DG . . . .
H3B H 0.6401 0.2484 0.5142 0.073 Uiso 1 1 d DG . . . .
C3 C 0.117(3) 0.360(2) 0.6259(17) 0.023(4) Uani 1 1 d . U . . .
N5 N 0.561(2) 0.062(2) 0.4345(16) 0.028(5) Uani 1 1 d . U . . .
N2AA N 0.159(2) 0.262(2) 0.5806(16) 0.027(4) Uani 1 1 d . U . . .
N3AA N 0.558(2) 0.166(2) 0.3772(15) 0.024(4) Uani 1 1 d . U . . .
C6 C 0.685(3) 0.183(2) 0.3681(17) 0.019(4) Uani 1 1 d . U . . .
N6 N 0.047(2) 0.201(2) 0.5452(15) 0.022(4) Uani 1 1 d . U . . .
N9 N 0.679(2) 0.024(2) 0.4610(16) 0.028(5) Uani 1 1 d . U . . .
N10 N 0.767(2) 0.095(2) 0.4179(14) 0.019(4) Uani 1 1 d . U . . .
N14 N 0.731(2) 0.280(2) 0.3193(16) 0.025(4) Uani 1 1 d . U . . .
H14 H 0.6723 0.3338 0.2929 0.030 Uiso 1 1 calc R . . . .
N1AA N 0.193(2) 0.454(2) 0.6732(17) 0.028(5) Uani 1 1 d . U . . .
H1AA H 0.1492 0.5098 0.6994 0.033 Uiso 1 1 calc R . . . .
C2 C 0.328(3) 0.471(2) 0.6843(19) 0.023(4) 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 N12 2.63(2) 1_455 ?
Pb1 O1 2.32(2) . ?
Pb1 O2 2.396(18) . ?
Pb1 N3AA 2.55(2) . ?
Pb3 O1 2.680(18) . ?
Pb3 N11 2.50(2) 3_455 ?
Pb3 O2 2.574(17) 3 ?
Pb3 N6 2.55(2) 3 ?
Pb3 N10 2.50(2) 3_455 ?
Pb2 O1 2.28(2) . ?
Pb2 O2 2.486(17) . ?
Pb2 N0AA 2.70(2) . ?
Pb2 N2AA 2.60(2) . ?
N12 Pb1 2.63(2) 1_655 ?
N12 N8 1.34(3) . ?
N12 N11 1.36(3) . ?
N8 N13 1.39(3) . ?
N11 Pb3 2.50(2) 3_545 ?
N11 C7 1.36(3) . ?
N1 N3 1.33(3) . ?
N1 N2 1.34(3) . ?
N13 C7 1.32(4) . ?
N7 N4 1.34(4) . ?
N7 C3 1.30(3) . ?
N4 N6 1.28(4) . ?
O2 Pb3 2.574(17) 3_445 ?
N3 C2 1.33(3) . ?
N0AA N2 1.38(3) . ?
N0AA C2 1.36(3) . ?
C7 N14 1.37(4) . ?
O3 H3A 0.8501 . ?
O3 H3B 0.8499 . ?
C3 N2AA 1.33(3) . ?
C3 N1AA 1.37(3) . ?
N5 N3AA 1.38(3) . ?
N5 N9 1.25(3) . ?
N2AA N6 1.33(3) . ?
N3AA C6 1.33(3) . ?
C6 N10 1.36(3) . ?
C6 N14 1.38(3) . ?
N6 Pb3 2.55(2) 3_445 ?
N9 N10 1.40(3) . ?
N10 Pb3 2.50(2) 3_545 ?
N14 H14 0.8600 . ?
N1AA H1AA 0.8600 . ?
N1AA C2 1.36(3) . ?

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 N12 77.1(7) . 1_455 ?
O1 Pb1 O2 71.1(6) . . ?
O1 Pb1 N3AA 71.9(7) . . ?
O2 Pb1 N12 79.2(6) . 1_455 ?
O2 Pb1 N3AA 88.7(6) . . ?
N3AA Pb1 N12 148.9(7) . 1_455 ?
N11 Pb3 O1 128.9(6) 3_455 . ?
N11 Pb3 O2 83.8(6) 3_455 3 ?
N11 Pb3 N6 76.0(7) 3_455 3 ?
O2 Pb3 O1 136.9(6) 3 . ?
N6 Pb3 O1 128.9(7) 3 . ?
N6 Pb3 O2 80.7(7) 3 3 ?
N10 Pb3 O1 72.0(7) 3_455 . ?
N10 Pb3 N11 68.3(7) 3_455 3_455 ?
N10 Pb3 O2 150.3(6) 3_455 3 ?
N10 Pb3 N6 82.6(7) 3_455 3 ?
O1 Pb2 O2 70.0(7) . . ?
O1 Pb2 N0AA 81.4(7) . . ?
O1 Pb2 N2AA 81.4(8) . . ?
O2 Pb2 N0AA 142.5(6) . . ?
O2 Pb2 N2AA 83.9(6) . . ?
N2AA Pb2 N0AA 67.7(7) . . ?
N8 N12 Pb1 119.8(16) . 1_655 ?
N8 N12 N11 109.6(19) . . ?
N11 N12 Pb1 129.8(14) . 1_655 ?
N12 N8 N13 109(2) . . ?
Pb1 O1 Pb3 116.1(9) . . ?
Pb2 O1 Pb1 108.0(7) . . ?
Pb2 O1 Pb3 117.2(9) . . ?
N12 N11 Pb3 119.2(14) . 3_545 ?
C7 N11 Pb3 137.3(18) . 3_545 ?
C7 N11 N12 103(2) . . ?
N3 N1 N2 112(2) . . ?
C7 N13 N8 103(2) . . ?
C3 N7 N4 104(2) . . ?
N6 N4 N7 110(2) . . ?
Pb1 O2 Pb3 120.1(7) . 3_445 ?
Pb1 O2 Pb2 99.3(6) . . ?
Pb2 O2 Pb3 118.0(7) . 3_445 ?
N1 N3 C2 105(2) . . ?
N2 N0AA Pb2 119.6(15) . . ?
C2 N0AA Pb2 133.6(16) . . ?
C2 N0AA N2 105(2) . . ?
N1 N2 N0AA 106(2) . . ?
N11 C7 N14 125(3) . . ?
N13 C7 N11 115(2) . . ?
N13 C7 N14 120(2) . . ?
H3A O3 H3B 109.5 . . ?
N7 C3 N2AA 112(2) . . ?
N7 C3 N1AA 120(2) . . ?
N2AA C3 N1AA 128(2) . . ?
N9 N5 N3AA 112(2) . . ?
C3 N2AA Pb2 136.1(17) . . ?
N6 N2AA Pb2 119.7(17) . . ?
N6 N2AA C3 104(2) . . ?
N5 N3AA Pb1 105.0(14) . . ?
C6 N3AA Pb1 146.4(18) . . ?
C6 N3AA N5 103.9(19) . . ?
N3AA C6 N10 112(2) . . ?
N3AA C6 N14 125(2) . . ?
N10 C6 N14 124(2) . . ?
N4 N6 Pb3 117.9(17) . 3_445 ?
N4 N6 N2AA 110(2) . . ?
N2AA N6 Pb3 131.7(18) . 3_445 ?
N5 N9 N10 109(2) . . ?
C6 N10 Pb3 138.1(17) . 3_545 ?
C6 N10 N9 103.4(19) . . ?
N9 N10 Pb3 117.7(15) . 3_545 ?
C7 N14 C6 126(2) . . ?
C7 N14 H14 117.2 . . ?
C6 N14 H14 117.2 . . ?
C3 N1AA H1AA 115.8 . . ?
C2 N1AA C3 128(2) . . ?
C2 N1AA H1AA 115.8 . . ?
N3 C2 N0AA 112(2) . . ?
N3 C2 N1AA 123(2) . . ?
N0AA C2 N1AA 125(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
Pb1 N12 N8 N13 169.2(15) 1_655 . . . ?
Pb1 N12 N11 Pb3 15(3) 1_655 . . 3_545 ?
Pb1 N12 N11 C7 -169(2) 1_655 . . . ?
Pb1 N3AA C6 N10 -150(2) . . . . ?
Pb1 N3AA C6 N14 34(5) . . . . ?
Pb3 N11 C7 N13 175.6(19) 3_545 . . . ?
Pb3 N11 C7 N14 -8(5) 3_545 . . . ?
Pb2 N0AA N2 N1 -167.3(16) . . . . ?
Pb2 N0AA C2 N3 163.3(18) . . . . ?
Pb2 N0AA C2 N1AA -17(4) . . . . ?
Pb2 N2AA N6 Pb3 -9(3) . . . 3_445 ?
Pb2 N2AA N6 N4 -179(2) . . . . ?
N12 N8 N13 C7 1(3) . . . . ?
N12 N11 C7 N13 1(3) . . . . ?
N12 N11 C7 N14 177(3) . . . . ?
N8 N12 N11 Pb3 -175.8(16) . . . 3_545 ?
N8 N12 N11 C7 0(3) . . . . ?
N8 N13 C7 N11 -1(3) . . . . ?
N8 N13 C7 N14 -178(3) . . . . ?
N11 N12 N8 N13 -1(3) . . . . ?
N11 C7 N14 C6 7(5) . . . . ?
N1 N3 C2 N0AA 1(3) . . . . ?
N1 N3 C2 N1AA -178(3) . . . . ?
N13 C7 N14 C6 -176(3) . . . . ?
N7 N4 N6 Pb3 -171(2) . . . 3_445 ?
N7 N4 N6 N2AA 1(4) . . . . ?
N7 C3 N2AA Pb2 177(2) . . . . ?
N7 C3 N2AA N6 -4(3) . . . . ?
N7 C3 N1AA C2 -173(3) . . . . ?
N4 N7 C3 N2AA 4(4) . . . . ?
N4 N7 C3 N1AA 179(3) . . . . ?
N3 N1 N2 N0AA 2(3) . . . . ?
N2 N1 N3 C2 -2(3) . . . . ?
N2 N0AA C2 N3 0(3) . . . . ?
N2 N0AA C2 N1AA 180(3) . . . . ?
C3 N7 N4 N6 -3(4) . . . . ?
C3 N2AA N6 Pb3 171.8(18) . . . 3_445 ?
C3 N2AA N6 N4 2(3) . . . . ?
C3 N1AA C2 N3 -174(3) . . . . ?
C3 N1AA C2 N0AA 7(5) . . . . ?
N5 N3AA C6 N10 -1(3) . . . . ?
N5 N3AA C6 N14 -177(2) . . . . ?
N5 N9 N10 Pb3 -168.2(18) . . . 3_545 ?
N5 N9 N10 C6 3(3) . . . . ?
N2AA C3 N1AA C2 1(5) . . . . ?
N3AA N5 N9 N10 -4(3) . . . . ?
N3AA C6 N10 Pb3 167.5(18) . . . 3_545 ?
N3AA C6 N10 N9 -1(3) . . . . ?
N3AA C6 N14 C7 180(3) . . . . ?
N9 N5 N3AA Pb1 166(2) . . . . ?
N9 N5 N3AA C6 3(3) . . . . ?
N10 C6 N14 C7 4(4) . . . . ?
N14 C6 N10 Pb3 -16(4) . . . 3_545 ?
N14 C6 N10 N9 175(2) . . . . ?
N1AA C3 N2AA Pb2 3(5) . . . . ?
N1AA C3 N2AA N6 -178(3) . . . . ?
C2 N0AA N2 N1 -1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
