Sanchez-Perez Clara, Knapp Caroline E, Karjalainen Minna M, Oilunkaniemi Raija, Carmalt Claire J, Laitinen Risto S
Laboratory of Inorganic Chemistry, Environmental and Chemical Engineering, University of Oulu, P. O. Box 3000, FI-90014 Oulu, Finland and Department of Chemistry, University College London, 20 Gordon Street, London, WC1H 0AJ, UK.
Department of Chemistry, University College London, 20 Gordon Street, London, WC1H 0AJ, UK.
Dalton Trans. 2018 Apr 17;47(15):5415-5421. doi: 10.1039/c8dt00300a.
Macrocyclic [Fe(η5-C5H4Se)2M(η5-C5H4R)2]2 [M = Ti (1), Zr (2), Hf (3), R = H; and M = Zr (4), Hf (5), R = tBu] were prepared and characterized by 77Se NMR spectroscopy and the crystal structures of 1-3 and 5 were determined by single-crystal X-ray diffraction. The crystal structure of 4 is known and the complex is isomorphous with 5. 1-5 form mutually similar macrocyclic tetranuclear complexes in which the alternating Fe(C5H4Se)2 and M(C5H4R)2 centers are linked by selenium bridges. The thermogravimetric analysis (TGA) of 1-3 under a helium atmosphere indicated that the complexes undergo a two-step decomposition upon heating. The final products were identified using powder X-ray diffraction as FexMSe2, indicating their potential as single-source precursors for functional materials.