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_4314872
_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            'C17 H31 Cu N7 O3 S2'
_chemical_formula_weight         509.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.916(6)
_cell_angle_beta                 72.470(6)
_cell_angle_gamma                85.134(6)
_cell_formula_units_Z            2
_cell_length_a                   9.0904(6)
_cell_length_b                   11.5022(9)
_cell_length_c                   12.4161(9)
_cell_measurement_reflns_used    3194
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      73.0636
_cell_measurement_theta_min      4.9528
_cell_volume                     1214.34(16)
_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      130(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8043
_diffrn_reflns_theta_full        73.80
_diffrn_reflns_theta_max         73.80
_diffrn_reflns_theta_min         4.95
_exptl_absorpt_coefficient_mu    3.143
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.505
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.3143
_exptl_crystal_size_mid          0.1471
_exptl_crystal_size_min          0.0280
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1502
_reflns_number_gt                3656
_reflns_number_total             4699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902204e_si_003.cif
_cod_data_source_block           jmwpd68
_cod_original_cell_volume        1214.34(15)
_cod_database_code               4314872