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_7707875
_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         'C14 H28 N7 O9 Pb, H2 O, N O3'
_chemical_formula_sum            'C14 H30 N8 O13 Pb'
_chemical_formula_weight         725.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc27z49p
_audit_creation_date             2021-01-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-05-19 deposited with the CCDC.	2021-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.6860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2179(2)
_cell_length_b                   27.5158(5)
_cell_length_c                   7.7860(2)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.72
_cell_volume                     2400.66(9)
_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      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       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_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_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_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 \l/2 correction factor is not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.008
_exptl_crystal_description       needle
_exptl_crystal_F_000             1424
_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
_refine_diff_density_max         2.514
_refine_diff_density_min         -2.005
_refine_diff_density_rms         0.185
_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_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0400
_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/[\s^2^(Fo^2^)+(0.0296P)^2^+3.5713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5751
_reflns_number_total             7328
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01653a2.cif
_cod_data_source_block           co582
_cod_depositor_comments
'Adding full bibliography for 7707873--7707875.cif.'
_cod_database_code               7707875
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.614
_shelx_estimated_absorpt_t_min   0.232
_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)
;
_shelx_res_checksum              64538
_shelx_hkl_checksum              99013
_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'