Versatile New Bis(thiosemicarbazone) Bifunctional Chelators: Synthesis, Conjugation to Bombesin(7-14)-NH2, and Copper-64 Radiolabeling
Brett M. Paterson; John A. Karas; Denis B. Scanlon; Jonathan M. White; Paul S. Donnelly; Inorganic Chemistry 49 (2010) 1884–1893; doi:10.1021/ic902204e

data_4314871
_publ_section_title
;
 Versatile New Bis(thiosemicarbazone) Bifunctional Chelators: Synthesis,
 Conjugation to Bombesin(7-14)-NH2, and Copper-64 Radiolabeling
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1884
_journal_page_last               1893
_journal_paper_doi               10.1021/ic902204e
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C9 H18 N6 S2'
_chemical_formula_weight         274.41
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.1160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4720(2)
_cell_length_b                   6.81020(10)
_cell_length_c                   13.66470(10)
_cell_measurement_reflns_used    3396
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.1169
_cell_measurement_theta_min      3.0215
_cell_volume                     1360.42(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6556
_diffrn_reflns_theta_full        73.27
_diffrn_reflns_theta_max         73.27
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    3.469
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.2403
_exptl_crystal_size_mid          0.1416
_exptl_crystal_size_min          0.1200
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                2216
_reflns_number_total             2679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902204e_si_001.cif
_cod_data_source_block           jmwpd57
_cod_database_code               4314871