A Redetermination of the Structure of Tetraethylammonium Meroxidotrichlorido (thenoyltrifluoroacetyl Acetonato-K2-O,O')niobate(V)

"SynopsisThe tetraethylammonium salt of the mono-anionic coordination compound mer-oxidotrichlorido(thenoyltrifluoroacetylacetonato- K2O,O’)niobate(V) (NEt4)[NbOCl3](ttfa)], has been prepared under aerobic conditions and characterized by single-crystal X-ray diffraction. (NEt4)[NbOCl3](ttfa)] crystallized in the monoclinic P21/c space group, with a = 11.483 (5), b = 12.563 (5), c = 17.110(5) Å, and ß = 100.838 (5)o. The complex structure exists in a 50.0% (NbA) : 50.0% (NbB) positional disorder ratio.IntroductionComplexes containing organometallic type ß- diketone ligands with O,O and O,N donor atoms are used widely in coordination chemistry and have applications in catalysis, radiopharmaceuticals, etc. (Schutte et al., 2011; Roodt, Visser and Brink, 2011; Brink et al., 2010; Otto et al., 1998). These ligand systems are very useful because of their highly coordinative nature, high solubility, and also due to their ability to be functionalized with various substituents on the carbonyl carbon atoms (Schutte et al., 2011).Only a small number of ß-diketonate ligands have successfully been coordinated to a Nb(V) metal centre, with only a select few being characterized by X-ray crystallography (Viljoen, 2009; Bullen, Mason and Pauling, 1965; Preuss, Lamding and Mueller-Becker, 1994; Funk, 1934; Davies, Leedlam and Jones, 1999; Allen, 2002. The synthesis and crystal structure determination at room temperature of mer-oxidotrichlorido (thenoyltrifluoroacetylacetonato- k2O,O’)niobate(V) {(NEt4)[NbOCl3(ttfa)]} was first reported by Daran et al. in 1979. Accordingly, for this current investigation, (NEt4)[NbOCl3(ttfa)] was re-evaluated at 100 K to determine if the structural features might change with temperature."