# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_co560_0m
_audit_block_doi                 10.5517/ccdc.csd.cc27z48n
_database_code_depnum_ccdc_archive 'CCDC 2084541'
loop_
_audit_author_name
_audit_author_address
'Brian Patrick'
;UBC Chemistry
Canada
;
_audit_update_record             
;
2021-05-19 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_audit_creation_date             2019-08-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H28 N8 O5 Pb, 2(N O3), 4(H2 O)'
_chemical_formula_sum            'C14 H36 N10 O15 Pb'
_chemical_formula_weight         791.72
_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           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                   8.9884(7)
_cell_length_b                   20.3731(16)
_cell_length_c                   14.8713(11)
_cell_angle_alpha                90
_cell_angle_beta                 93.436(2)
_cell_angle_gamma                90
_cell_volume                     2718.4(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.549
_cell_measurement_theta_min      2.27
_shelx_estimated_absorpt_T_max   0.653
_shelx_estimated_absorpt_T_min   0.241
_exptl_absorpt_coefficient_mu    6.293
_exptl_absorpt_correction_T_max  0.6302
_exptl_absorpt_correction_T_min  0.3910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1067 before and 0.0480 after correction. The Ratio of minimum to maximum transmission is 0.6204. 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    1.935
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.074
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50045
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.548
_diffrn_reflns_theta_min         1.697
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7492
_reflns_number_total             8315
_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 V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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         0.759
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.00020(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         8315
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0235
_refine_ls_restrained_S_all      1.052
_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)+(0.0130P)²+8.1729P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0517
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O12(H12a,H12b), O13(H13c,H13d), O14(H14a,H14b), O15(H15a,H15b)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C3(H3c,H3d), C5(H5c,H5d), C6(H6a,H6b), C7(H7c,H7d), C9(H9a,H9b),
 C10(H10a,H10b), C11(H11a,H11b), C13(H13a,H13b)
2.c X=CH2 refined with riding coordinates:
 N1(H1a,H1b), N3(H3a,H3b), N5(H5a,H5b), N7(H7a,H7b), N8(H8a,H8b)
;
_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
Pb01 Pb 0.42510(2) 0.09689(2) 0.52181(2) 0.00664(3) Uani 1 1 d . . . . .
O1 O 0.5632(2) 0.02630(9) 0.39519(12) 0.0126(4) Uani 1 1 d . . . . .
O2 O 0.1719(2) 0.03890(9) 0.47762(12) 0.0119(4) Uani 1 1 d . . . . .
O3 O 0.2617(2) 0.10391(9) 0.65812(12) 0.0104(3) Uani 1 1 d . . . . .
O4 O 0.5690(2) 0.18751(9) 0.44417(12) 0.0123(4) Uani 1 1 d . . . . .
O5 O 0.6721(2) 0.10159(10) 0.65859(13) 0.0153(4) Uani 1 1 d . . . . .
N1 N 0.5869(3) 0.00665(11) 0.24714(15) 0.0119(4) Uani 1 1 d . . . . .
H1A H 0.638523 -0.028309 0.257953 0.014 Uiso 1 1 calc R . . . .
H1B H 0.566813 0.019032 0.192468 0.014 Uiso 1 1 calc R . . . .
N2 N 0.3227(2) 0.10853(10) 0.34840(14) 0.0083(4) Uani 1 1 d . . . . .
N3 N -0.0144(3) 0.01272(12) 0.37429(15) 0.0140(4) Uani 1 1 d . . . . .
H3A H -0.071370 -0.001176 0.414671 0.017 Uiso 1 1 calc R . . . .
H3B H -0.044713 0.011664 0.318350 0.017 Uiso 1 1 calc R . . . .
N4 N 0.2118(2) 0.18761(10) 0.50546(14) 0.0078(4) Uani 1 1 d . . . . .
N5 N 0.0877(3) 0.15856(12) 0.73096(15) 0.0143(4) Uani 1 1 d . . . . .
H5A H 0.116733 0.140977 0.781583 0.017 Uiso 1 1 calc R . . . .
H5B H 0.014787 0.185945 0.728347 0.017 Uiso 1 1 calc R . . . .
N6 N 0.5015(2) 0.21149(11) 0.62255(14) 0.0087(4) Uani 1 1 d . . . . .
N7 N 0.7582(3) 0.25987(11) 0.44899(15) 0.0123(4) Uani 1 1 d . . . . .
H7A H 0.774438 0.253090 0.393345 0.015 Uiso 1 1 calc R . . . .
H7B H 0.812280 0.287455 0.480127 0.015 Uiso 1 1 calc R . . . .
N8 N 0.6769(3) 0.11579(12) 0.81016(15) 0.0152(4) Uani 1 1 d . . . . .
H8A H 0.732978 0.082122 0.820664 0.018 Uiso 1 1 calc R . . . .
H8B H 0.647778 0.138893 0.854207 0.018 Uiso 1 1 calc R . . . .
C1 C 0.5384(3) 0.04134(12) 0.31453(17) 0.0095(4) Uani 1 1 d . . . . .
C2 C 0.4488(3) 0.10275(12) 0.29003(16) 0.0086(4) Uani 1 1 d . . . . .
H2A H 0.512287 0.141118 0.297394 0.010 Uiso 1 1 calc R . . . .
H2B H 0.411817 0.100488 0.227482 0.010 Uiso 1 1 calc R . . . .
C3 C 0.2132(3) 0.05723(13) 0.32206(16) 0.0098(4) Uani 1 1 d . . . . .
H3C H 0.265622 0.019384 0.300118 0.012 Uiso 1 1 calc R . . . .
H3D H 0.147616 0.073541 0.272917 0.012 Uiso 1 1 calc R . . . .
C4 C 0.1199(3) 0.03573(12) 0.39826(16) 0.0095(4) Uani 1 1 d . . . . .
C5 C 0.2568(3) 0.17498(12) 0.34089(16) 0.0092(4) Uani 1 1 d . . . . .
H5C H 0.207753 0.180090 0.281421 0.011 Uiso 1 1 calc R . . . .
H5D H 0.336076 0.207273 0.347106 0.011 Uiso 1 1 calc R . . . .
C6 C 0.1446(3) 0.18842(12) 0.41147(16) 0.0098(4) Uani 1 1 d . . . . .
H6A H 0.099173 0.230967 0.399562 0.012 Uiso 1 1 calc R . . . .
H6B H 0.066362 0.155631 0.405879 0.012 Uiso 1 1 calc R . . . .
C7 C 0.0950(3) 0.17442(13) 0.56913(16) 0.0103(4) Uani 1 1 d . . . . .
H7C H 0.020972 0.145370 0.540483 0.012 Uiso 1 1 calc R . . . .
H7D H 0.045811 0.215352 0.582439 0.012 Uiso 1 1 calc R . . . .
C8 C 0.1553(3) 0.14347(12) 0.65705(17) 0.0098(4) Uani 1 1 d . . . . .
C9 C 0.2831(3) 0.25262(12) 0.52430(17) 0.0102(4) Uani 1 1 d . . . . .
H9A H 0.206097 0.286047 0.522757 0.012 Uiso 1 1 calc R . . . .
H9B H 0.348966 0.262487 0.476780 0.012 Uiso 1 1 calc R . . . .
C10 C 0.3720(3) 0.25637(12) 0.61472(17) 0.0107(4) Uani 1 1 d . . . . .
H10A H 0.407061 0.301028 0.624025 0.013 Uiso 1 1 calc R . . . .
H10B H 0.306284 0.246205 0.662216 0.013 Uiso 1 1 calc R . . . .
C11 C 0.5336(3) 0.19215(13) 0.71751(16) 0.0106(4) Uani 1 1 d . . . . .
H11A H 0.440783 0.182464 0.744816 0.013 Uiso 1 1 calc R . . . .
H11B H 0.581000 0.228485 0.750208 0.013 Uiso 1 1 calc R . . . .
C12 C 0.6350(3) 0.13223(12) 0.72537(17) 0.0104(4) Uani 1 1 d . . . . .
C13 C 0.6351(3) 0.24077(13) 0.58675(16) 0.0101(4) Uani 1 1 d . . . . .
H13A H 0.722552 0.223529 0.620164 0.012 Uiso 1 1 calc R . . . .
H13B H 0.632967 0.287820 0.596605 0.012 Uiso 1 1 calc R . . . .
C14 C 0.6499(3) 0.22784(12) 0.48672(16) 0.0085(4) Uani 1 1 d . . . . .
O6 O -0.0261(2) 0.18438(10) 0.17032(14) 0.0178(4) Uani 1 1 d . . . . .
O7 O -0.1344(2) 0.24441(9) 0.26740(13) 0.0134(4) Uani 1 1 d . . . . .
O8 O -0.2012(3) 0.14299(11) 0.24741(17) 0.0246(5) Uani 1 1 d . . . . .
N9 N -0.1210(2) 0.18970(11) 0.22860(15) 0.0115(4) Uani 1 1 d . . . . .
O9 O 0.4346(2) 0.44756(11) 0.57066(14) 0.0212(4) Uani 1 1 d . . . . .
O10 O 0.4773(2) 0.37810(11) 0.46410(14) 0.0182(4) Uani 1 1 d . . . . .
O11 O 0.6577(2) 0.41102(12) 0.55646(16) 0.0232(5) Uani 1 1 d . . . . .
N10 N 0.5241(3) 0.41275(11) 0.53043(15) 0.0133(4) Uani 1 1 d . . . . .
O12 O 0.1937(2) 0.40753(10) 0.39520(13) 0.0161(4) Uani 1 1 d . . . . .
H12A H 0.130892 0.395927 0.432684 0.024 Uiso 1 1 d G . . . .
H12B H 0.277979 0.398788 0.421454 0.024 Uiso 1 1 d G . . . .
O13 O -0.0378(2) 0.37382(10) 0.49914(13) 0.0159(4) Uani 1 1 d . . . . .
H13C H -0.038679 0.370010 0.556015 0.024 Uiso 1 1 d G . . . .
H13D H -0.089382 0.408086 0.486940 0.024 Uiso 1 1 d G . . . .
O14 O 0.1623(2) -0.01477(10) 0.08716(15) 0.0173(4) Uani 1 1 d . . . . .
H14A H 0.224111 0.012863 0.068343 0.026 Uiso 1 1 d G . . . .
H14B H 0.090930 0.008380 0.104453 0.026 Uiso 1 1 d G . . . .
O15 O 0.0842(2) -0.02395(10) 0.82267(13) 0.0145(4) Uani 1 1 d . . . . .
H15A H 0.143257 -0.056312 0.819395 0.022 Uiso 1 1 d G . . . .
H15B H 0.137938 0.006611 0.846114 0.022 Uiso 1 1 d G . . . .


_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
Pb01 O1 2.7267(19) . ?
Pb01 O2 2.6128(18) . ?
Pb01 O3 2.5776(18) . ?
Pb01 O4 2.5680(19) . ?
Pb01 O5 2.921(2) . ?
Pb01 N2 2.696(2) . ?
Pb01 N4 2.664(2) . ?
Pb01 N6 2.836(2) . ?
O1 C1 1.245(3) . ?
O2 C4 1.245(3) . ?
O3 C8 1.249(3) . ?
O4 C14 1.245(3) . ?
O5 C12 1.236(3) . ?
N1 C1 1.322(3) . ?
N2 C2 1.473(3) . ?
N2 C3 1.472(3) . ?
N2 C5 1.479(3) . ?
N3 C4 1.324(3) . ?
N4 C6 1.489(3) . ?
N4 C7 1.480(3) . ?
N4 C9 1.491(3) . ?
N5 C8 1.324(3) . ?
N6 C10 1.479(3) . ?
N6 C11 1.478(3) . ?
N6 C13 1.470(3) . ?
N7 C14 1.324(3) . ?
N8 C12 1.337(3) . ?
C1 C2 1.520(3) . ?
C3 C4 1.514(3) . ?
C5 C6 1.523(3) . ?
C7 C8 1.522(3) . ?
C9 C10 1.525(3) . ?
C11 C12 1.524(4) . ?
C13 C14 1.524(3) . ?
O6 N9 1.257(3) . ?
O7 N9 1.264(3) . ?
O8 N9 1.236(3) . ?
O9 N10 1.251(3) . ?
O10 N10 1.264(3) . ?
O11 N10 1.240(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 Pb01 O5 98.03(6) . . ?
O1 Pb01 N6 133.88(6) . . ?
O2 Pb01 O1 90.78(6) . . ?
O2 Pb01 O5 143.52(6) . . ?
O2 Pb01 N2 63.70(6) . . ?
O2 Pb01 N4 71.30(6) . . ?
O2 Pb01 N6 133.21(6) . . ?
O3 Pb01 O1 151.26(6) . . ?
O3 Pb01 O2 72.19(6) . . ?
O3 Pb01 O5 84.02(6) . . ?
O3 Pb01 N2 124.70(6) . . ?
O3 Pb01 N4 65.94(6) . . ?
O3 Pb01 N6 70.75(6) . . ?
O4 Pb01 O1 78.83(6) . . ?
O4 Pb01 O2 131.81(6) . . ?
O4 Pb01 O3 129.78(6) . . ?
O4 Pb01 O5 84.67(6) . . ?
O4 Pb01 N2 70.06(6) . . ?
O4 Pb01 N4 80.75(6) . . ?
O4 Pb01 N6 62.16(6) . . ?
N2 Pb01 O1 61.92(6) . . ?
N2 Pb01 O5 149.85(6) . . ?
N2 Pb01 N6 119.39(6) . . ?
N4 Pb01 O1 131.14(6) . . ?
N4 Pb01 O5 123.62(6) . . ?
N4 Pb01 N2 69.45(6) . . ?
N4 Pb01 N6 68.11(6) . . ?
N6 Pb01 O5 57.01(6) . . ?
C1 O1 Pb01 118.21(16) . . ?
C4 O2 Pb01 122.27(16) . . ?
C8 O3 Pb01 119.83(16) . . ?
C14 O4 Pb01 122.74(16) . . ?
C12 O5 Pb01 110.23(16) . . ?
C2 N2 Pb01 109.02(14) . . ?
C2 N2 C5 110.33(19) . . ?
C3 N2 Pb01 112.11(14) . . ?
C3 N2 C2 108.18(19) . . ?
C3 N2 C5 111.8(2) . . ?
C5 N2 Pb01 105.36(14) . . ?
C6 N4 Pb01 110.03(14) . . ?
C6 N4 C9 108.19(19) . . ?
C7 N4 Pb01 110.48(14) . . ?
C7 N4 C6 109.85(19) . . ?
C7 N4 C9 110.8(2) . . ?
C9 N4 Pb01 107.49(14) . . ?
C10 N6 Pb01 107.64(14) . . ?
C11 N6 Pb01 108.21(15) . . ?
C11 N6 C10 110.36(19) . . ?
C13 N6 Pb01 108.67(14) . . ?
C13 N6 C10 112.1(2) . . ?
C13 N6 C11 109.70(19) . . ?
O1 C1 N1 123.4(2) . . ?
O1 C1 C2 119.7(2) . . ?
N1 C1 C2 116.9(2) . . ?
N2 C2 C1 109.85(19) . . ?
N2 C3 C4 113.4(2) . . ?
O2 C4 N3 123.9(2) . . ?
O2 C4 C3 120.1(2) . . ?
N3 C4 C3 116.0(2) . . ?
N2 C5 C6 113.0(2) . . ?
N4 C6 C5 113.4(2) . . ?
N4 C7 C8 113.3(2) . . ?
O3 C8 N5 121.9(2) . . ?
O3 C8 C7 120.7(2) . . ?
N5 C8 C7 117.4(2) . . ?
N4 C9 C10 114.0(2) . . ?
N6 C10 C9 114.0(2) . . ?
N6 C11 C12 111.6(2) . . ?
O5 C12 N8 123.9(2) . . ?
O5 C12 C11 122.1(2) . . ?
N8 C12 C11 114.0(2) . . ?
N6 C13 C14 113.8(2) . . ?
O4 C14 N7 122.1(2) . . ?
O4 C14 C13 121.9(2) . . ?
N7 C14 C13 115.9(2) . . ?
O6 N9 O7 118.5(2) . . ?
O8 N9 O6 121.2(2) . . ?
O8 N9 O7 120.2(2) . . ?
O9 N10 O10 119.7(2) . . ?
O11 N10 O9 120.3(2) . . ?
O11 N10 O10 119.9(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
Pb01 O1 C1 N1 -172.97(19) . . . . ?
Pb01 O1 C1 C2 7.5(3) . . . . ?
Pb01 O2 C4 N3 -172.9(2) . . . . ?
Pb01 O2 C4 C3 8.8(3) . . . . ?
Pb01 O3 C8 N5 -166.03(19) . . . . ?
Pb01 O3 C8 C7 16.2(3) . . . . ?
Pb01 O4 C14 N7 157.92(18) . . . . ?
Pb01 O4 C14 C13 -19.0(3) . . . . ?
Pb01 O5 C12 N8 142.2(2) . . . . ?
Pb01 O5 C12 C11 -36.7(3) . . . . ?
Pb01 N2 C2 C1 51.1(2) . . . . ?
Pb01 N2 C3 C4 32.4(2) . . . . ?
Pb01 N2 C5 C6 -52.1(2) . . . . ?
Pb01 N4 C6 C5 -35.7(2) . . . . ?
Pb01 N4 C7 C8 33.0(2) . . . . ?
Pb01 N4 C9 C10 -54.6(2) . . . . ?
Pb01 N6 C10 C9 -33.3(2) . . . . ?
Pb01 N6 C11 C12 46.3(2) . . . . ?
Pb01 N6 C13 C14 29.4(2) . . . . ?
O1 C1 C2 N2 -41.1(3) . . . . ?
N1 C1 C2 N2 139.4(2) . . . . ?
N2 C3 C4 O2 -28.9(3) . . . . ?
N2 C3 C4 N3 152.7(2) . . . . ?
N2 C5 C6 N4 63.7(3) . . . . ?
N4 C7 C8 O3 -34.8(3) . . . . ?
N4 C7 C8 N5 147.3(2) . . . . ?
N4 C9 C10 N6 63.4(3) . . . . ?
N6 C11 C12 O5 -6.0(3) . . . . ?
N6 C11 C12 N8 175.1(2) . . . . ?
N6 C13 C14 O4 -11.0(3) . . . . ?
N6 C13 C14 N7 172.0(2) . . . . ?
C2 N2 C3 C4 152.6(2) . . . . ?
C2 N2 C5 C6 -169.7(2) . . . . ?
C3 N2 C2 C1 -71.0(2) . . . . ?
C3 N2 C5 C6 69.9(3) . . . . ?
C5 N2 C2 C1 166.40(19) . . . . ?
C5 N2 C3 C4 -85.7(2) . . . . ?
C6 N4 C7 C8 154.6(2) . . . . ?
C6 N4 C9 C10 -173.4(2) . . . . ?
C7 N4 C6 C5 -157.5(2) . . . . ?
C7 N4 C9 C10 66.2(3) . . . . ?
C9 N4 C6 C5 81.5(2) . . . . ?
C9 N4 C7 C8 -86.0(2) . . . . ?
C10 N6 C11 C12 163.9(2) . . . . ?
C10 N6 C13 C14 -89.4(2) . . . . ?
C11 N6 C10 C9 -151.1(2) . . . . ?
C11 N6 C13 C14 147.5(2) . . . . ?
C13 N6 C10 C9 86.2(3) . . . . ?
C13 N6 C11 C12 -72.1(3) . . . . ?


_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_co583
_audit_block_doi                 10.5517/ccdc.csd.cc27z4bq
_database_code_depnum_ccdc_archive 'CCDC 2084543'
loop_
_audit_author_name
_audit_author_address
'Brian Patrick'
;UBC Chemistry
Canada
;
_audit_update_record             
;
2021-05-19 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_audit_creation_date             2021-02-23
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C24 H34 N8 O6 Pb, 2(N O3), 2.085(H2 O), 0.582(O)'
_chemical_formula_sum            'C24 H38.58 N10 O14.67 Pb'
_chemical_formula_weight         909.10
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   14.0872(7)
_cell_length_b                   22.5964(10)
_cell_length_c                   12.3531(9)
_cell_angle_alpha                90
_cell_angle_beta                 123.133(2)
_cell_angle_gamma                90
_cell_volume                     3292.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      2.67
_shelx_estimated_absorpt_T_max   0.712
_shelx_estimated_absorpt_T_min   0.443
_exptl_absorpt_coefficient_mu    5.208
_exptl_absorpt_correction_T_max  0.695
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker, 2016/2) was used for absorption correction.
wR2(int) was 0.1339 before and 0.0768 after correction.
The ratio of minimum to maximum transmission is 0.5157.
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    1.834
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1808
_exptl_crystal_recrystallization_method 
'The material was recrystallised from water by slow evaporation'
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19580
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.705
_diffrn_reflns_theta_min         1.802
_diffrn_ambient_temperature      115(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker-Nonius Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.99
_diffrn_source_power             0.0495
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4486
_reflns_number_total             5069
_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 V8.40B (Bruker, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.568
_refine_diff_density_min         -2.072
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5069
_refine_ls_number_restraints     139
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0319
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0334P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0742
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H) groups, All O(H,H) groups
2. Restrained distances
 N5-O4 = N5-O6
 1.25 with sigma of 0.02
 N5-O5
 1.24 with sigma of 0.02
 N5A-O6A = N5A-O4A
 1.25 with sigma of 0.02
 N5A-O5A
 1.24 with sigma of 0.02
 N5B-O4B = N5B-O5B
 1.25 with sigma of 0.02
 N5B-O6B
 1.24 with sigma of 0.02
 N5-O4 \\sim N5-O5 \\sim N5-O6
 with sigma of 0.02
 O6A-O5A \\sim O5A-O4A \\sim O4A-O6A
 with sigma of 0.04
 O4-O5 \\sim O5-O6 \\sim O6-O4
 with sigma of 0.04
 N5A-O6A \\sim N5A-O5A \\sim N5A-O4A
 with sigma of 0.02
 O4B-O6B \\sim O6B-O5B \\sim O5B-O4B
 with sigma of 0.04
 N5B-O4B \\sim N5B-O6B \\sim N5B-O5B
 with sigma of 0.02
3. Restrained planarity
 O4, O6, O5, N5
 with sigma of 0.1
 O6A, O4A, O5A, N5A
 with sigma of 0.1
 N5B, O4B, O6B, O5B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O4 \\sim O6 \\sim O5 \\sim N5: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
O6A \\sim O4A \\sim O5A \\sim N5A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
N5B \\sim O4B \\sim O6B \\sim O5B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(O6) = Uanis(O6B)
5. Rigid body (RIGU) restrains
 O4, O6, O5, N5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6A, O4A, O5A, N5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5B, O4B, O6B, O5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(O4)+Sof(O6)+Sof(O5)+Sof(N5)]+1*[Sof(N5B)+Sof(O4B)+Sof(O6B)+Sof(O5B)]+1*
 [Sof(O6A)+Sof(O4A)+Sof(O5A)+Sof(N5A)]=1 with esd of 0.005
 Sof(O4)=Sof(O6)=Sof(O5)=Sof(N5)=FVAR(1)
 Sof(N5B)=Sof(O4B)=Sof(O6B)=Sof(O5B)=FVAR(2)
 Sof(O6A)=Sof(O4A)=Sof(O5A)=Sof(N5A)=FVAR(3)
 Sof(O7)=Sof(H7A)=Sof(H7B)=FVAR(4)
 Sof(O9)=Sof(H9A)=Sof(H9B)=FVAR(5)
7.a Free rotating group:
 O7(H7A,H7B), O9(H9A,H9B)
7.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
7.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7)
;
_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 0.500000 0.36753(2) 0.750000 0.02072(6) Uani 1 2 d S T P . .
O1 O 0.43947(18) 0.45719(9) 0.8492(2) 0.0266(5) Uani 1 1 d . . . . .
O2 O 0.5089(2) 0.32584(10) 0.5509(2) 0.0298(5) Uani 1 1 d . . . . .
O3 O 0.3813(2) 0.26705(9) 0.6900(2) 0.0282(5) Uani 1 1 d . . . . .
N1 N 0.3825(3) 0.45708(14) 0.9869(3) 0.0314(7) Uani 1 1 d . . . . .
H1A H 0.433(4) 0.480(2) 1.038(4) 0.047 Uiso 1 1 d . U . . .
H1B H 0.340(4) 0.448(2) 0.999(5) 0.047 Uiso 1 1 d . U . . .
N2 N 0.2753(2) 0.38004(12) 0.6802(3) 0.0247(5) Uani 1 1 d . . . . .
N3 N 0.3257(2) 0.38729(12) 0.4964(3) 0.0248(5) Uani 1 1 d . . . . .
N4 N 0.4488(3) 0.31818(19) 0.3421(4) 0.0499(9) Uani 1 1 d . . . . .
H4A H 0.508(5) 0.292(2) 0.367(5) 0.075 Uiso 1 1 d . U . . .
H4B H 0.391(5) 0.326(2) 0.261(6) 0.075 Uiso 1 1 d . U . . .
C1 C 0.3736(2) 0.44028(13) 0.8796(3) 0.0247(6) Uani 1 1 d . . . . .
C2 C 0.2782(2) 0.39708(15) 0.7966(3) 0.0274(6) Uani 1 1 d . . . . .
H2A H 0.288218 0.361221 0.847948 0.033 Uiso 1 1 calc R U . . .
H2B H 0.204886 0.415454 0.770914 0.033 Uiso 1 1 calc R U . . .
C3 C 0.2207(3) 0.42704(15) 0.5828(3) 0.0296(7) Uani 1 1 d . . . . .
H3A H 0.252720 0.465767 0.624421 0.036 Uiso 1 1 calc R U . . .
H3B H 0.138618 0.427563 0.548171 0.036 Uiso 1 1 calc R U . . .
C4 C 0.2366(3) 0.41889(14) 0.4730(3) 0.0268(7) Uani 1 1 d . . . . .
C5 C 0.1629(3) 0.44557(16) 0.3529(4) 0.0337(8) Uani 1 1 d . . . . .
H5 H 0.099293 0.467704 0.337421 0.040 Uiso 1 1 calc R U . . .
C6 C 0.1846(3) 0.43899(16) 0.2578(4) 0.0366(8) Uani 1 1 d . . . . .
H6 H 0.136832 0.457583 0.176328 0.044 Uiso 1 1 calc R U . . .
C7 C 0.2754(3) 0.40553(17) 0.2804(3) 0.0352(8) Uani 1 1 d . . . . .
H7 H 0.291073 0.400445 0.215273 0.042 Uiso 1 1 calc R U . . .
C8 C 0.3433(3) 0.37950(14) 0.4010(3) 0.0273(7) Uani 1 1 d . . . . .
C9 C 0.4407(3) 0.33921(16) 0.4365(3) 0.0307(7) Uani 1 1 d . . . . .
C10 C 0.2146(3) 0.32307(15) 0.6275(3) 0.0305(7) Uani 1 1 d . . . . .
H10A H 0.191086 0.319489 0.536154 0.037 Uiso 1 1 calc R U . . .
H10B H 0.145188 0.323298 0.629182 0.037 Uiso 1 1 calc R U . . .
C11 C 0.2850(3) 0.27040(15) 0.7010(4) 0.0335(7) Uani 1 1 d . . . . .
H11A H 0.310853 0.273945 0.793125 0.040 Uiso 1 1 calc R U . . .
H11B H 0.239030 0.233904 0.665885 0.040 Uiso 1 1 calc R U . . .
C12 C 0.4504(3) 0.21739(14) 0.7580(4) 0.0338(8) Uani 1 1 d . . . . .
H12A H 0.406325 0.180366 0.722690 0.041 Uiso 1 1 calc R U . . .
H12B H 0.478049 0.220072 0.850734 0.041 Uiso 1 1 calc R U . . .
O6A O -0.2773(17) 0.3159(13) 0.452(3) 0.080(9) Uani 0.266(7) 1 d D U P A 2
O4A O -0.0893(12) 0.3177(7) 0.578(2) 0.087(7) Uani 0.266(7) 1 d D U P A 2
O5A O -0.1870(17) 0.3971(6) 0.5035(18) 0.053(4) Uani 0.266(7) 1 d D U P A 2
N5A N -0.1838(10) 0.3421(5) 0.5095(12) 0.047(3) Uani 0.266(7) 1 d D U P A 2
O4 O -0.0279(12) 0.3725(5) 0.5685(18) 0.112(6) Uani 0.451(16) 1 d D U P B 1
O6 O -0.1781(11) 0.4171(9) 0.5288(18) 0.049(3) Uani 0.451(16) 1 d D U P B 1
O5 O -0.0265(12) 0.4659(5) 0.5781(16) 0.079(4) Uani 0.451(16) 1 d D U P B 1
N5 N -0.0773(9) 0.4188(4) 0.5613(14) 0.054(3) Uani 0.451(16) 1 d D U P B 1
O7 O -0.2827(8) 0.3024(4) 0.4369(12) 0.067(3) Uani 0.661(13) 1 d G . P C 3
H7A H -0.244490 0.283446 0.507707 0.101 Uiso 0.661(13) 1 d G U P C 3
H7B H -0.262817 0.338215 0.457645 0.101 Uiso 0.661(13) 1 d G U P C 3
O9 O -0.0638(12) 0.2811(6) 0.6725(18) 0.111(7) Uani 0.381(12) 1 d G . P D -1
H9A H -0.126728 0.263635 0.623634 0.167 Uiso 0.381(12) 1 d G U P D -1
H9B H -0.071369 0.314100 0.635492 0.167 Uiso 0.381(12) 1 d G U P D -1
O8 O -0.1711(18) 0.2601(8) 0.5684(19) 0.044(8) Uani 0.162(12) 1 d . . . E 4
O10 O 0.000000 0.4381(12) 0.750000 0.085(11) Uiso 0.26(2) 2 d S . . F 7
N5B N -0.0823(13) 0.4058(8) 0.573(2) 0.064(7) Uani 0.283(17) 1 d D U P G 3
O4B O -0.0755(14) 0.3507(9) 0.5710(19) 0.075(7) Uani 0.283(17) 1 d D U P G 3
O6B O -0.1780(16) 0.4293(13) 0.504(3) 0.049(3) Uani 0.283(17) 1 d D U P G 3
O5B O 0.0029(10) 0.4377(9) 0.643(2) 0.080(7) Uani 0.283(17) 1 d D U P G 3


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.734(2) . ?
Pb1 O1 2.734(2) 2_656 ?
Pb1 O2 2.700(2) . ?
Pb1 O2 2.700(2) 2_656 ?
Pb1 O3 2.673(2) . ?
Pb1 O3 2.673(2) 2_656 ?
Pb1 N3 2.763(3) . ?
Pb1 N3 2.763(3) 2_656 ?
O1 C1 1.237(4) . ?
O2 C9 1.236(4) . ?
O3 C11 1.438(4) . ?
O3 C12 1.421(4) . ?
N1 H1A 0.82(5) . ?
N1 H1B 0.73(5) . ?
N1 C1 1.317(4) . ?
N2 C2 1.468(4) . ?
N2 C3 1.469(4) . ?
N2 C10 1.485(4) . ?
N3 C4 1.331(4) . ?
N3 C8 1.342(5) . ?
N4 H4A 0.93(6) . ?
N4 H4B 0.90(6) . ?
N4 C9 1.322(5) . ?
C1 C2 1.518(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.502(5) . ?
C4 C5 1.400(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.373(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.377(6) . ?
C7 H7 0.9500 . ?
C7 C8 1.387(5) . ?
C8 C9 1.498(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.497(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C12 1.513(8) 2_656 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
O6A N5A 1.252(13) . ?
O4A N5A 1.250(12) . ?
O5A N5A 1.244(12) . ?
O4 N5 1.232(9) . ?
O6 N5 1.247(11) . ?
O5 N5 1.237(10) . ?
O7 H7A 0.8498 . ?
O7 H7B 0.8498 . ?
O9 H9A 0.8493 . ?
O9 H9B 0.8503 . ?
N5B O4B 1.251(12) . ?
N5B O6B 1.252(13) . ?
N5B O5B 1.253(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O1 84.37(10) . 2_656 ?
O1 Pb1 N3 70.95(7) . 2_656 ?
O1 Pb1 N3 94.98(8) 2_656 2_656 ?
O1 Pb1 N3 70.95(7) 2_656 . ?
O1 Pb1 N3 94.98(8) . . ?
O2 Pb1 O1 147.99(7) . . ?
O2 Pb1 O1 70.68(7) . 2_656 ?
O2 Pb1 O1 70.68(7) 2_656 . ?
O2 Pb1 O1 147.99(7) 2_656 2_656 ?
O2 Pb1 O2 139.16(10) . 2_656 ?
O2 Pb1 N3 129.36(8) . 2_656 ?
O2 Pb1 N3 129.36(8) 2_656 . ?
O2 Pb1 N3 58.57(8) 2_656 2_656 ?
O2 Pb1 N3 58.57(8) . . ?
O3 Pb1 O1 116.90(7) 2_656 2_656 ?
O3 Pb1 O1 143.73(7) 2_656 . ?
O3 Pb1 O1 116.90(7) . . ?
O3 Pb1 O1 143.73(7) . 2_656 ?
O3 Pb1 O2 77.57(7) 2_656 2_656 ?
O3 Pb1 O2 67.83(7) 2_656 . ?
O3 Pb1 O2 77.57(7) . . ?
O3 Pb1 O2 67.83(7) . 2_656 ?
O3 Pb1 O3 63.73(10) 2_656 . ?
O3 Pb1 N3 119.02(8) . 2_656 ?
O3 Pb1 N3 119.02(8) 2_656 . ?
O3 Pb1 N3 77.84(8) 2_656 2_656 ?
O3 Pb1 N3 77.84(8) . . ?
N3 Pb1 N3 161.40(12) . 2_656 ?
C1 O1 Pb1 112.13(18) . . ?
C9 O2 Pb1 124.2(2) . . ?
C11 O3 Pb1 114.14(18) . . ?
C12 O3 Pb1 112.57(19) . . ?
C12 O3 C11 111.3(3) . . ?
H1A N1 H1B 118(5) . . ?
C1 N1 H1A 122(3) . . ?
C1 N1 H1B 120(4) . . ?
C2 N2 C3 109.6(3) . . ?
C2 N2 C10 111.0(3) . . ?
C3 N2 C10 110.4(3) . . ?
C4 N3 Pb1 118.8(2) . . ?
C4 N3 C8 119.0(3) . . ?
C8 N3 Pb1 119.9(2) . . ?
H4A N4 H4B 127(5) . . ?
C9 N4 H4A 116(3) . . ?
C9 N4 H4B 117(4) . . ?
O1 C1 N1 122.8(3) . . ?
O1 C1 C2 121.9(3) . . ?
N1 C1 C2 115.3(3) . . ?
N2 C2 C1 111.7(3) . . ?
N2 C2 H2A 109.3 . . ?
N2 C2 H2B 109.3 . . ?
C1 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
H2A C2 H2B 107.9 . . ?
N2 C3 H3A 109.1 . . ?
N2 C3 H3B 109.1 . . ?
N2 C3 C4 112.4(3) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
N3 C4 C3 117.3(3) . . ?
N3 C4 C5 121.8(3) . . ?
C5 C4 C3 120.9(3) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 C4 118.5(3) . . ?
C6 C5 H5 120.8 . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.2(3) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 121.0 . . ?
C6 C7 C8 118.0(4) . . ?
C8 C7 H7 121.0 . . ?
N3 C8 C7 122.6(3) . . ?
N3 C8 C9 113.6(3) . . ?
C7 C8 C9 123.8(3) . . ?
O2 C9 N4 122.2(4) . . ?
O2 C9 C8 120.0(3) . . ?
N4 C9 C8 117.8(3) . . ?
N2 C10 H10A 109.0 . . ?
N2 C10 H10B 109.0 . . ?
N2 C10 C11 113.1(3) . . ?
H10A C10 H10B 107.8 . . ?
C11 C10 H10A 109.0 . . ?
C11 C10 H10B 109.0 . . ?
O3 C11 C10 109.3(3) . . ?
O3 C11 H11A 109.8 . . ?
O3 C11 H11B 109.8 . . ?
C10 C11 H11A 109.8 . . ?
C10 C11 H11B 109.8 . . ?
H11A C11 H11B 108.3 . . ?
O3 C12 C12 107.8(2) . 2_656 ?
O3 C12 H12A 110.1 . . ?
O3 C12 H12B 110.1 . . ?
C12 C12 H12A 110.1 2_656 . ?
C12 C12 H12B 110.1 2_656 . ?
H12A C12 H12B 108.5 . . ?
O4A N5A O6A 125.2(17) . . ?
O5A N5A O6A 116.5(17) . . ?
O5A N5A O4A 118.2(14) . . ?
O4 N5 O6 119.8(12) . . ?
O4 N5 O5 117.8(10) . . ?
O5 N5 O6 122.2(12) . . ?
H7A O7 H7B 104.5 . . ?
H9A O9 H9B 104.5 . . ?
O4B N5B O6B 118.2(17) . . ?
O4B N5B O5B 122.1(15) . . ?
O6B N5B O5B 119.6(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A O1 0.82(5) 2.11(5) 2.931(4) 173(4) 5_667 yes
N1 H1B O6 0.73(5) 2.22(5) 2.922(15) 162(5) 2_556 yes
N4 H4A O9 0.93(6) 2.00(6) 2.830(14) 148(5) 7_556 yes
N4 H4B O7 0.90(6) 2.13(6) 2.944(12) 151(5) 2 yes
O7 H7A O7 0.85 2.02 2.70(2) 136.6 7_456 yes

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 O1 C1 N1 138.0(3) . . . . ?
Pb1 O1 C1 C2 -40.2(3) . . . . ?
Pb1 O2 C9 N4 179.3(3) . . . . ?
Pb1 O2 C9 C8 -2.0(4) . . . . ?
Pb1 O3 C11 C10 51.5(3) . . . . ?
Pb1 O3 C12 C12 -50.1(4) . . . 2_656 ?
Pb1 N3 C4 C3 -16.9(4) . . . . ?
Pb1 N3 C4 C5 160.6(2) . . . . ?
Pb1 N3 C8 C7 -159.0(2) . . . . ?
Pb1 N3 C8 C9 22.4(3) . . . . ?
O1 C1 C2 N2 -0.8(4) . . . . ?
N1 C1 C2 N2 -179.2(3) . . . . ?
N2 C3 C4 N3 -24.1(4) . . . . ?
N2 C3 C4 C5 158.4(3) . . . . ?
N2 C10 C11 O3 -63.4(4) . . . . ?
N3 C4 C5 C6 -0.6(5) . . . . ?
N3 C8 C9 O2 -13.8(4) . . . . ?
N3 C8 C9 N4 164.9(3) . . . . ?
C2 N2 C3 C4 167.8(2) . . . . ?
C2 N2 C10 C11 -77.8(3) . . . . ?
C3 N2 C2 C1 -79.4(3) . . . . ?
C3 N2 C10 C11 160.4(3) . . . . ?
C3 C4 C5 C6 176.9(3) . . . . ?
C4 N3 C8 C7 3.3(5) . . . . ?
C4 N3 C8 C9 -175.4(3) . . . . ?
C4 C5 C6 C7 1.7(5) . . . . ?
C5 C6 C7 C8 -0.4(5) . . . . ?
C6 C7 C8 N3 -2.1(5) . . . . ?
C6 C7 C8 C9 176.4(3) . . . . ?
C7 C8 C9 O2 167.6(3) . . . . ?
C7 C8 C9 N4 -13.7(5) . . . . ?
C8 N3 C4 C3 -179.4(3) . . . . ?
C8 N3 C4 C5 -1.9(5) . . . . ?
C10 N2 C2 C1 158.4(3) . . . . ?
C10 N2 C3 C4 -69.6(3) . . . . ?
C11 O3 C12 C12 -179.7(3) . . . 2_656 ?
C12 O3 C11 C10 -179.7(3) . . . . ?

# end Validation Reply Form
_olex2_diffrn_ambient_temperature_device Kryoflex
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop in oil'
_olex2_submission_original_sample_id AI-[Pb(ampam)]2+
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT973_co583               
;
PROBLEM: Check Calcd Positive Resid. Density on       Pb1       1.51 eA-3  
RESPONSE: This residual electron density is adjacent the central Pb atom.
While it is a bit large, it is not an unrealistic amount of residual density,
given the metal in question.
;
####################################################################### 
# 
# 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_co582
_audit_block_doi                 10.5517/ccdc.csd.cc27z49p
_database_code_depnum_ccdc_archive 'CCDC 2084542'
loop_
_audit_author_name
_audit_author_address
'Brian Patrick'
;UBC Chemistry
Canada
;
_audit_update_record             
;
2021-05-19 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_audit_creation_date             2021-01-27
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
''
''
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H28 N7 O9 Pb, H2 O, N O3'
_chemical_formula_sum            'C14 H30 N8 O13 Pb'
_chemical_formula_weight         725.65
_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           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                   11.2179(2)
_cell_length_b                   27.5158(5)
_cell_length_c                   7.7860(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.6860(10)
_cell_angle_gamma                90
_cell_volume                     2400.66(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.72
_shelx_estimated_absorpt_T_max   0.614
_shelx_estimated_absorpt_T_min   0.232
_exptl_absorpt_coefficient_mu    7.108
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker, 2016/2) was used for absorption correction.
wR2(int) was 0.0702 before and 0.0534 after correction.
The ratio of minimum to maximum transmission is 0.8345.
The λ/2 correction factor is not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1424
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 0.00 0.0300
0.00 -1.00 0.00 0.0380
1.00 -1.00 1.00 0.0560
-1.00 1.00 -1.00 0.0630
1.00 0.00 -1.00 0.1140
-1.00 0.00 1.00 0.0450

_exptl_crystal_recrystallization_method 
'The material was recrystallised from a mixture of water and acetone  by slow evaporation'
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.076
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            34585
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.553
_diffrn_reflns_theta_min         1.962
_diffrn_ambient_temperature      110(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5751
_reflns_number_total             7328
_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 V8.40B (Bruker, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.514
_refine_diff_density_min         -2.005
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7328
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0400
_refine_ls_restrained_S_all      1.075
_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)+(0.0296P)²+3.5713P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0785
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O10(H10C,H10D)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3C,H3D), C5(H5A,H5B), C6(H6C,H6D), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B)
2.c X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B)
;
_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 0.71160(2) 0.62746(2) 0.51920(2) 0.01167(5) Uani 1 1 d . . . . .
O1 O 0.7787(3) 0.71005(12) 0.6401(4) 0.0177(7) Uani 1 1 d . . . . .
O2 O 0.9231(3) 0.61917(12) 0.3512(4) 0.0183(7) Uani 1 1 d . . . . .
O3 O 0.7134(3) 0.58635(12) 0.8379(4) 0.0155(7) Uani 1 1 d . . . . .
O4 O 0.5292(3) 0.56158(12) 0.5877(4) 0.0166(7) Uani 1 1 d . . . . .
O5 O 0.6961(3) 0.69031(12) 0.2680(4) 0.0201(8) Uani 1 1 d . . . . .
O6 O 0.5235(3) 0.66927(12) 0.6643(4) 0.0173(7) Uani 1 1 d . . . . .
O7 O 0.7010(3) 0.55222(12) 0.2751(4) 0.0192(7) Uani 1 1 d . . . . .
O8 O 0.7960(3) 0.53102(12) 0.5136(4) 0.0171(7) Uani 1 1 d . . . . .
O9 O 0.8001(4) 0.48461(13) 0.2888(5) 0.0254(8) Uani 1 1 d . . . . .
N1 N 0.9224(4) 0.76313(16) 0.7303(6) 0.0216(9) Uani 1 1 d . . . . .
H1A H 0.874(6) 0.788(2) 0.739(8) 0.034(18) Uiso 1 1 d . . . . .
H1B H 0.995(7) 0.770(3) 0.755(9) 0.05(2) Uiso 1 1 d . . . . .
N2 N 0.9291(3) 0.63161(14) 0.6979(5) 0.0140(7) Uani 1 1 d . . . . .
N3 N 1.0729(4) 0.56381(16) 0.3622(5) 0.0229(9) Uani 1 1 d . . . . .
H3A H 1.070891 0.560175 0.249832 0.027 Uiso 1 1 calc R U . . .
H3B H 1.124408 0.547161 0.427443 0.027 Uiso 1 1 calc R U . . .
N4 N 0.6352(4) 0.70794(14) -0.0065(5) 0.0173(8) Uani 1 1 d . . . . .
H4A H 0.688991 0.731004 -0.014822 0.021 Uiso 1 1 calc R U . . .
H4B H 0.585659 0.701417 -0.094424 0.021 Uiso 1 1 calc R U . . .
N5 N 0.4995(3) 0.63515(13) 0.3187(5) 0.0126(8) Uani 1 1 d . . . . .
N6 N 0.3356(5) 0.6993(2) 0.6393(7) 0.0299(11) Uani 1 1 d . . . . .
H6A H 0.329(7) 0.701(3) 0.751(10) 0.05(2) Uiso 1 1 d . . . . .
H6B H 0.280(7) 0.707(3) 0.570(9) 0.04(2) Uiso 1 1 d . . . . .
N7 N 0.7660(4) 0.52261(14) 0.3584(5) 0.0150(8) Uani 1 1 d . . . . .
C1 C 0.8849(4) 0.71923(17) 0.6813(6) 0.0161(9) Uani 1 1 d . . . . .
C2 C 0.9803(4) 0.68029(17) 0.6730(6) 0.0172(10) Uani 1 1 d . . . . .
H2A H 1.016879 0.681698 0.559833 0.021 Uiso 1 1 calc R U . . .
H2B H 1.043645 0.686439 0.763110 0.021 Uiso 1 1 calc R U . . .
C3 C 1.0083(4) 0.59517(17) 0.6292(6) 0.0152(9) Uani 1 1 d . . . . .
H3C H 0.987464 0.562747 0.674144 0.018 Uiso 1 1 calc R U . . .
H3D H 1.091671 0.602438 0.668079 0.018 Uiso 1 1 calc R U . . .
C4 C 0.9983(4) 0.59434(17) 0.4332(6) 0.0156(9) Uani 1 1 d . . . . .
C5 C 0.9069(4) 0.62320(18) 0.8830(5) 0.0162(9) Uani 1 1 d . . . . .
H5A H 0.866873 0.652152 0.928993 0.019 Uiso 1 1 calc R U . . .
H5B H 0.984557 0.619422 0.947451 0.019 Uiso 1 1 calc R U . . .
C6 C 0.8314(4) 0.57906(18) 0.9135(6) 0.0181(10) Uani 1 1 d . . . . .
H6C H 0.867981 0.550117 0.861831 0.022 Uiso 1 1 calc R U . . .
H6D H 0.826995 0.573344 1.038561 0.022 Uiso 1 1 calc R U . . .
C7 C 0.6436(5) 0.54257(17) 0.8468(6) 0.0172(10) Uani 1 1 d . . . . .
H7A H 0.637541 0.532516 0.968165 0.021 Uiso 1 1 calc R U . . .
H7B H 0.682376 0.516018 0.784264 0.021 Uiso 1 1 calc R U . . .
C8 C 0.5207(5) 0.55221(17) 0.7668(5) 0.0165(9) Uani 1 1 d . . . . .
H8A H 0.468767 0.523669 0.783483 0.020 Uiso 1 1 calc R U . . .
H8B H 0.484807 0.580562 0.823208 0.020 Uiso 1 1 calc R U . . .
C9 C 0.4147(4) 0.57071(19) 0.5044(6) 0.0184(10) Uani 1 1 d . . . . .
H9A H 0.371002 0.595120 0.570548 0.022 Uiso 1 1 calc R U . . .
H9B H 0.367186 0.540374 0.499703 0.022 Uiso 1 1 calc R U . . .
C10 C 0.4307(5) 0.58912(18) 0.3253(6) 0.0190(10) Uani 1 1 d . . . . .
H10A H 0.472057 0.563915 0.259720 0.023 Uiso 1 1 calc R U . . .
H10B H 0.350997 0.594283 0.268057 0.023 Uiso 1 1 calc R U . . .
C11 C 0.5355(4) 0.64306(17) 0.1428(6) 0.0147(9) Uani 1 1 d . . . . .
H11A H 0.464940 0.652197 0.068793 0.018 Uiso 1 1 calc R U . . .
H11B H 0.568710 0.612570 0.097283 0.018 Uiso 1 1 calc R U . . .
C12 C 0.6289(4) 0.68311(16) 0.1381(6) 0.0141(9) Uani 1 1 d . . . . .
C13 C 0.4314(4) 0.67685(18) 0.3789(6) 0.0160(9) Uani 1 1 d . . . . .
H13A H 0.347390 0.673638 0.335586 0.019 Uiso 1 1 calc R U . . .
H13B H 0.463896 0.706947 0.329512 0.019 Uiso 1 1 calc R U . . .
C14 C 0.4343(4) 0.68173(17) 0.5746(6) 0.0179(10) Uani 1 1 d . . . . .
O10 O 0.8191(4) 0.43848(18) -0.0332(5) 0.0396(11) Uani 1 1 d G . . . .
H10C H 0.831916 0.459023 0.047069 0.059 Uiso 1 1 d G U . . .
H10D H 0.797993 0.412780 0.017972 0.059 Uiso 1 1 d G U . . .
O11 O 0.7474(4) 0.33803(18) 0.0247(5) 0.0390(11) Uani 1 1 d . . . . .
O12 O 0.8499(4) 0.31805(18) -0.1930(6) 0.0438(12) Uani 1 1 d . . . . .
O13 O 0.8340(5) 0.26677(18) 0.0214(7) 0.0556(15) Uani 1 1 d . . . . .
N8 N 0.8088(5) 0.3078(2) -0.0508(7) 0.0393(14) Uani 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 O1 2.559(3) . ?
Pb1 O2 2.772(3) . ?
Pb1 O3 2.726(3) . ?
Pb1 O4 2.803(3) . ?
Pb1 O5 2.611(3) . ?
Pb1 O6 2.697(3) . ?
Pb1 O7 2.809(3) . ?
Pb1 O8 2.818(3) . ?
Pb1 N2 2.754(4) . ?
Pb1 N5 2.792(4) . ?
O1 C1 1.245(6) . ?
O2 C4 1.240(5) . ?
O3 C6 1.438(5) . ?
O3 C7 1.440(6) . ?
O4 C8 1.426(5) . ?
O4 C9 1.434(5) . ?
O5 C12 1.249(5) . ?
O6 C14 1.241(6) . ?
O7 N7 1.253(5) . ?
O8 N7 1.261(5) . ?
O9 N7 1.246(5) . ?
N1 H1A 0.87(7) . ?
N1 H1B 0.85(7) . ?
N1 C1 1.329(6) . ?
N2 C2 1.474(6) . ?
N2 C3 1.458(6) . ?
N2 C5 1.492(6) . ?
N3 H3A 0.8800 . ?
N3 H3B 0.8800 . ?
N3 C4 1.324(6) . ?
N4 H4A 0.8800 . ?
N4 H4B 0.8800 . ?
N4 C12 1.321(6) . ?
N5 C10 1.486(6) . ?
N5 C11 1.462(6) . ?
N5 C13 1.468(6) . ?
N6 H6A 0.88(8) . ?
N6 H6B 0.84(7) . ?
N6 C14 1.329(7) . ?
C1 C2 1.518(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
C3 C4 1.525(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.506(7) . ?
C6 H6C 0.9900 . ?
C6 H6D 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.509(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.502(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.522(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.528(6) . ?
O10 H10C 0.8498 . ?
O10 H10D 0.8505 . ?
O11 N8 1.245(7) . ?
O12 N8 1.252(7) . ?
O13 N8 1.286(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O2 90.19(11) . . ?
O1 Pb1 O3 92.53(10) . . ?
O1 Pb1 O4 135.14(10) . . ?
O1 Pb1 O5 72.28(10) . . ?
O1 Pb1 O6 71.91(11) . . ?
O1 Pb1 O7 154.91(11) . . ?
O1 Pb1 O8 138.45(10) . . ?
O1 Pb1 N2 62.55(11) . . ?
O1 Pb1 N5 111.51(10) . . ?
O2 Pb1 O4 133.24(10) . . ?
O2 Pb1 O7 68.29(10) . . ?
O2 Pb1 O8 67.65(10) . . ?
O2 Pb1 N5 117.91(10) . . ?
O3 Pb1 O2 115.19(9) . . ?
O3 Pb1 O4 62.15(9) . . ?
O3 Pb1 O7 107.95(9) . . ?
O3 Pb1 O8 68.61(9) . . ?
O3 Pb1 N2 65.72(11) . . ?
O3 Pb1 N5 120.67(10) . . ?
O4 Pb1 O7 69.14(10) . . ?
O4 Pb1 O8 69.07(10) . . ?
O5 Pb1 O2 74.30(11) . . ?
O5 Pb1 O3 162.59(11) . . ?
O5 Pb1 O4 123.17(10) . . ?
O5 Pb1 O6 90.30(11) . . ?
O5 Pb1 O7 88.98(10) . . ?
O5 Pb1 O8 128.52(10) . . ?
O5 Pb1 N2 112.19(11) . . ?
O5 Pb1 N5 60.37(10) . . ?
O6 Pb1 O2 159.46(10) . . ?
O6 Pb1 O3 76.60(10) . . ?
O6 Pb1 O4 66.66(10) . . ?
O6 Pb1 O7 126.05(10) . . ?
O6 Pb1 O8 132.68(10) . . ?
O6 Pb1 N2 117.56(10) . . ?
O6 Pb1 N5 62.55(10) . . ?
O7 Pb1 O8 45.51(9) . . ?
N2 Pb1 O2 58.96(10) . . ?
N2 Pb1 O4 124.61(10) . . ?
N2 Pb1 O7 112.38(11) . . ?
N2 Pb1 O8 75.91(10) . . ?
N2 Pb1 N5 172.31(11) . . ?
N5 Pb1 O4 62.93(10) . . ?
N5 Pb1 O7 70.71(10) . . ?
N5 Pb1 O8 109.92(10) . . ?
C1 O1 Pb1 122.4(3) . . ?
C4 O2 Pb1 112.3(3) . . ?
C6 O3 Pb1 113.4(3) . . ?
C6 O3 C7 110.8(3) . . ?
C7 O3 Pb1 114.2(2) . . ?
C8 O4 Pb1 112.7(3) . . ?
C8 O4 C9 112.0(4) . . ?
C9 O4 Pb1 116.6(3) . . ?
C12 O5 Pb1 121.2(3) . . ?
C14 O6 Pb1 120.5(3) . . ?
N7 O7 Pb1 97.1(2) . . ?
N7 O8 Pb1 96.5(2) . . ?
H1A N1 H1B 115(6) . . ?
C1 N1 H1A 122(4) . . ?
C1 N1 H1B 123(5) . . ?
C2 N2 Pb1 108.2(3) . . ?
C2 N2 C5 110.6(4) . . ?
C3 N2 Pb1 109.1(3) . . ?
C3 N2 C2 109.2(4) . . ?
C3 N2 C5 112.3(4) . . ?
C5 N2 Pb1 107.3(3) . . ?
H3A N3 H3B 120.0 . . ?
C4 N3 H3A 120.0 . . ?
C4 N3 H3B 120.0 . . ?
H4A N4 H4B 120.0 . . ?
C12 N4 H4A 120.0 . . ?
C12 N4 H4B 120.0 . . ?
C10 N5 Pb1 110.3(3) . . ?
C11 N5 Pb1 105.6(3) . . ?
C11 N5 C10 109.0(3) . . ?
C11 N5 C13 110.7(3) . . ?
C13 N5 Pb1 108.9(3) . . ?
C13 N5 C10 112.1(4) . . ?
H6A N6 H6B 122(7) . . ?
C14 N6 H6A 121(5) . . ?
C14 N6 H6B 117(5) . . ?
O7 N7 O8 119.9(4) . . ?
O9 N7 O7 120.2(4) . . ?
O9 N7 O8 119.8(4) . . ?
O1 C1 N1 123.0(4) . . ?
O1 C1 C2 120.9(4) . . ?
N1 C1 C2 116.1(4) . . ?
N2 C2 C1 110.9(4) . . ?
N2 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 H3C 109.4 . . ?
N2 C3 H3D 109.4 . . ?
N2 C3 C4 111.1(4) . . ?
H3C C3 H3D 108.0 . . ?
C4 C3 H3C 109.4 . . ?
C4 C3 H3D 109.4 . . ?
O2 C4 N3 124.2(4) . . ?
O2 C4 C3 121.6(4) . . ?
N3 C4 C3 114.1(4) . . ?
N2 C5 H5A 108.9 . . ?
N2 C5 H5B 108.9 . . ?
N2 C5 C6 113.4(4) . . ?
H5A C5 H5B 107.7 . . ?
C6 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
O3 C6 C5 109.7(4) . . ?
O3 C6 H6C 109.7 . . ?
O3 C6 H6D 109.7 . . ?
C5 C6 H6C 109.7 . . ?
C5 C6 H6D 109.7 . . ?
H6C C6 H6D 108.2 . . ?
O3 C7 H7A 109.9 . . ?
O3 C7 H7B 109.9 . . ?
O3 C7 C8 108.7(4) . . ?
H7A C7 H7B 108.3 . . ?
C8 C7 H7A 109.9 . . ?
C8 C7 H7B 109.9 . . ?
O4 C8 C7 109.5(4) . . ?
O4 C8 H8A 109.8 . . ?
O4 C8 H8B 109.8 . . ?
C7 C8 H8A 109.8 . . ?
C7 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
O4 C9 H9A 109.7 . . ?
O4 C9 H9B 109.7 . . ?
O4 C9 C10 109.6(4) . . ?
H9A C9 H9B 108.2 . . ?
C10 C9 H9A 109.7 . . ?
C10 C9 H9B 109.7 . . ?
N5 C10 C9 113.9(4) . . ?
N5 C10 H10A 108.8 . . ?
N5 C10 H10B 108.8 . . ?
C9 C10 H10A 108.8 . . ?
C9 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N5 C11 H11A 109.5 . . ?
N5 C11 H11B 109.5 . . ?
N5 C11 C12 110.6(4) . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
O5 C12 N4 123.6(4) . . ?
O5 C12 C11 119.0(4) . . ?
N4 C12 C11 117.4(4) . . ?
N5 C13 H13A 108.8 . . ?
N5 C13 H13B 108.8 . . ?
N5 C13 C14 113.6(4) . . ?
H13A C13 H13B 107.7 . . ?
C14 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
O6 C14 N6 123.5(5) . . ?
O6 C14 C13 121.0(4) . . ?
N6 C14 C13 115.5(4) . . ?
H10C O10 H10D 104.5 . . ?
O11 N8 O12 120.1(6) . . ?
O11 N8 O13 119.7(6) . . ?
O12 N8 O13 120.2(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A O5 0.87(7) 2.11(7) 2.871(6) 146(6) 4_576 yes
N1 H1B O12 0.85(7) 2.26(7) 2.994(7) 145(6) 2_755 yes
N3 H3A O10 0.88 2.14 2.886(6) 142.6 3_765 yes
N4 H4A O1 0.88 2.23 2.969(5) 141.0 4_575 yes
N4 H4B O6 0.88 2.16 2.995(5) 157.8 1_554 yes
N6 H6A O11 0.88(8) 2.25(8) 2.999(7) 143(6) 3_666 yes
N6 H6B O13 0.84(7) 2.17(7) 2.900(7) 145(6) 2_655 yes
O10 H10C O9 0.85 2.06 2.827(5) 150.5 . yes
O10 H10D O11 0.85 2.13 2.919(7) 153.2 . yes

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 O1 C1 N1 174.1(4) . . . . ?
Pb1 O1 C1 C2 -4.2(6) . . . . ?
Pb1 O2 C4 N3 142.5(4) . . . . ?
Pb1 O2 C4 C3 -34.7(5) . . . . ?
Pb1 O3 C6 C5 43.0(4) . . . . ?
Pb1 O3 C7 C8 -50.7(4) . . . . ?
Pb1 O4 C8 C7 -46.6(4) . . . . ?
Pb1 O4 C9 C10 37.9(5) . . . . ?
Pb1 O5 C12 N4 -165.5(3) . . . . ?
Pb1 O5 C12 C11 13.3(6) . . . . ?
Pb1 O6 C14 N6 175.1(4) . . . . ?
Pb1 O6 C14 C13 -4.0(6) . . . . ?
Pb1 O7 N7 O8 10.1(4) . . . . ?
Pb1 O7 N7 O9 -170.7(4) . . . . ?
Pb1 O8 N7 O7 -10.0(4) . . . . ?
Pb1 O8 N7 O9 170.8(4) . . . . ?
Pb1 N2 C2 C1 41.0(4) . . . . ?
Pb1 N2 C3 C4 42.9(4) . . . . ?
Pb1 N2 C5 C6 49.9(4) . . . . ?
Pb1 N5 C10 C9 50.2(5) . . . . ?
Pb1 N5 C11 C12 -48.7(4) . . . . ?
Pb1 N5 C13 C14 -40.6(4) . . . . ?
O1 C1 C2 N2 -28.1(6) . . . . ?
O3 C7 C8 O4 65.7(5) . . . . ?
O4 C9 C10 N5 -60.3(6) . . . . ?
N1 C1 C2 N2 153.6(4) . . . . ?
N2 C3 C4 O2 -6.0(6) . . . . ?
N2 C3 C4 N3 176.5(4) . . . . ?
N2 C5 C6 O3 -65.4(5) . . . . ?
N5 C11 C12 O5 28.0(6) . . . . ?
N5 C11 C12 N4 -153.1(4) . . . . ?
N5 C13 C14 O6 32.8(7) . . . . ?
N5 C13 C14 N6 -146.4(5) . . . . ?
C2 N2 C3 C4 -75.1(5) . . . . ?
C2 N2 C5 C6 167.7(4) . . . . ?
C3 N2 C2 C1 159.6(4) . . . . ?
C3 N2 C5 C6 -70.0(5) . . . . ?
C5 N2 C2 C1 -76.3(4) . . . . ?
C5 N2 C3 C4 161.8(4) . . . . ?
C6 O3 C7 C8 179.7(4) . . . . ?
C7 O3 C6 C5 173.0(4) . . . . ?
C8 O4 C9 C10 169.8(4) . . . . ?
C9 O4 C8 C7 179.6(4) . . . . ?
C10 N5 C11 C12 -167.2(4) . . . . ?
C10 N5 C13 C14 81.6(5) . . . . ?
C11 N5 C10 C9 165.7(4) . . . . ?
C11 N5 C13 C14 -156.4(4) . . . . ?
C13 N5 C10 C9 -71.3(5) . . . . ?
C13 N5 C11 C12 69.0(5) . . . . ?

# end Validation Reply Form
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a mylar loop in oil'
_olex2_submission_original_sample_id 'AI-[Pb(EGTAm)]2+ pH4'
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT971_co582               
;
PROBLEM: Check Calcd Resid. Dens.  0.85A   From Pb1             2.59 eA-3  
RESPONSE: The largest +ve and -ve residual electron density peaks in the e-map
all fall along the O2-Pb1-O6 axis.  This likely represents Fourier ripples from 
a less than perfect absorption correction.
;
# start Validation Reply Form
_vrf_PLAT976_co582               
;
PROBLEM: Check Calcd Resid. Dens.  1.05A   From O2             -2.31 eA-3  
RESPONSE: The largest +ve and -ve residual electron density peaks in the e-map
all fall along the O2-Pb1-O6 axis.  This likely represents Fourier ripples from 
a less than perfect absorption correction. 
;
