Getting a lead on Pb<sup>2+</sup>-amide chelators for <sup>203/212</sup>Pb radiopharmaceuticals.
Ingham, Aidan; Kostelnik, Thomas I.; McNeil, Brooke L.; Patrick, Brian O.; Choudhary, Neha; Jaraquemada-Peláez, María de Guadalupe; Orvig, Chris; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11579–11595; doi:10.1039/d1dt01653a

data_7707874
_publ_section_title
;
 Getting a lead on Pb<sup>2+</sup>-amide chelators for
 <sup>203/212</sup>Pb radiopharmaceuticals.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11579
_journal_page_last               11595
_journal_paper_doi               10.1039/d1dt01653a
_journal_volume                  50
_journal_year                    2021
_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
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc27z4bq
_audit_creation_date             2021-02-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-19 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.133(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0872(7)
_cell_length_b                   22.5964(10)
_cell_length_c                   12.3531(9)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      30.59
_cell_measurement_theta_min      2.67
_cell_volume                     3292.9(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_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)'
_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       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_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_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
_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 \l/2 correction factor is not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.834
_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
_refine_diff_density_max         1.568
_refine_diff_density_min         -2.072
_refine_diff_density_rms         0.138
_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_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0319
_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/[\s^2^(Fo^2^)+(0.0334P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4486
_reflns_number_total             5069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01653a2.cif
_cod_data_source_block           co583
_cod_depositor_comments
'Adding full bibliography for 7707873--7707875.cif.'
_cod_database_code               7707874
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.443
_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)
;
_shelx_res_checksum              13115
_shelx_hkl_checksum              4530
_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'