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Synthesis and Characterization of Ga III , In III and Lu III Complexes of a Set of dtpa Bis‐Amide Ligands
Author(s) -
Greiser Julia,
Hagemann Tino,
Niksch Tobias,
Traber Philipp,
Kupfer Stephan,
Gräfe Stefanie,
Görls Helmar,
Weigand Wolfgang,
Freesmeyer Martin
Publication year - 2015
Publication title -
european journal of inorganic chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.667
H-Index - 136
eISSN - 1099-0682
pISSN - 1434-1948
DOI - 10.1002/ejic.201500436
Subject(s) - chemistry , amide , nuclear magnetic resonance spectroscopy , hexa , aqueous solution , chloroform , chelation , dota , mass spectrometry , coordination complex , metal , proton nmr , stereochemistry , nuclear chemistry , crystallography , inorganic chemistry , organic chemistry , chromatography
The synthesis and characterization of five new diethylenetriaminepentaacetic acid (dtpa) ligands, (dtpa)‐ N , N″ ‐bis(alkoxyphenylamide), and their complexation with Ga III , In III and Lu III are reported. The procedures for the synthesis of all complexes in aqueous media are described as well as a synthetic pathway for the preparation of Ga III complexes in chloroform. All substances were characterized by NMR spectroscopy, mass spectrometry, elemental analysis and HPLC. Single‐crystal structure analysis was performed where applicable, which revealed the presence of hepta‐ and octa‐coordinated isomers for In III complexes and a nine‐fold coordination of Lu III ions in the solid state. Additional NMR experiments suggested a hepta‐coordinated In III species in solution, whereas the Ga III complexes appear to be hexa‐coordinated and the Lu III complexes to be octa‐coordinated. Both NMR and HPLC studies indicated the presence of a single isomer in every complex.