Nanocrystalline lanthanide nitride materials synthesised by thermal treatment of amido and ammine metallocenes: X-ray studies and DFT calculations

Chemistry : a European Journal
Ulrich BaischWolfgang Schnick

Abstract

The decomposition process of ammine lanthanide metallocenes was studied by X-ray diffractometry, spectroscopy and theoretical investigations. A series of ammine-tris(eta(5)-cyclopentadienyl)lanthanide(III) complexes 1-Ln (Lanthanide (Ln)=Sm, Gd, Dy, Ho, Er, Yb) was synthesised by the reaction of [Cp(3)Ln] complexes (Cp=cyclopentadienyl) with liquid ammonia at -78 degrees C and structurally characterised by X-ray diffraction methods, mass spectrometry and vibrational (IR, Raman) spectroscopy. Furthermore, amido-bis(eta(5)-cyclopentadienyl)lanthanide(III) complexes 2-Ln (Ln=Dy, Ho, Er, Yb) were synthesised by heating the respective ammine adduct 1-Ln in an inert gas atmosphere at temperatures of between 240 and 290 degrees C. X-ray diffraction studies, mass spectrometry and vibrational (IR, Raman) spectroscopy were carried out for several 2-Ln species and proved the formation of dimeric mu(2)-bridged compounds. Species 1-Ln are highly reactive coordination compounds and showed different behaviour regarding the decomposition to 2-Ln. The reaction of 1-Ln and 2-Ln with inorganic bases yielded lanthanide nitride LnN powders with an estimated crystallite size of between 40 and 90 nm at unprecedented low temperatures of 240 to 300 deg...Continue Reading

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Citations

Jan 1, 2008·Acta Crystallographica. Section E, Structure Reports Online·Sandro Pagano, Wolfgang Schnick
Mar 10, 2016·Chemical Society Reviews·Christos E KefalidisLaurent Maron
Jun 4, 2010·Dalton Transactions : an International Journal of Inorganic Chemistry·Takanori Shima, Zhaomin Hou
May 2, 2007·Dalton Transactions : an International Journal of Inorganic Chemistry·Patricia A Hunt
Mar 22, 2018·Dalton Transactions : an International Journal of Inorganic Chemistry·Monica D BoshartWilliam J Evans
Jun 25, 2008·The Journal of Physical Chemistry. a·John L Lewin, Christopher J Cramer
Nov 8, 2011·Journal of the American Chemical Society·Robert G DenningMark Irwin
Nov 23, 2017·Inorganic Chemistry·Selvan DemirWilliam J Evans
Nov 5, 2020·Inorganic Chemistry·Thuy-Ai D NguyenDamon A Parrish

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