NDLI: Homoleptic borates and aluminates containing the difluorophosphato ligand – $[M(O_{2}PF_{2})_{x}]^{y−}$

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	Eiden, Philipp Schulz, Christoph Ermantraut, Andreas Schmidt, Michael Krossing, Ingo Garsuch, Arnd Klose, Petra
Description	Author Affiliation: Schulz C ( Institut für Anorganische und Analytische Chemie and Freiburger Materialforschungszentrum (FMF), Universität Freiburg, Albertstr. 21, 79104 Freiburg, Germany. krossing@uni-freiburg.de.)
Abstract	Weakly coordinating anions (WCAs) with the difluorophosphato ligand $(O_{2}PF_{2})$ were the target of this study. Initial experiments were conducted towards the preparation of homoleptic aluminates of the well-studied $[Al(OR)_{4}]^{−}-type.$ The preparation of the initial target structure $Li[Al(O_{2}PF_{2})_{4}]$ failed due to the remaining Lewis acidic character of the central aluminum atom. Instead, the formation of $Li_{3}[Al(O_{2}PF_{2})_{6}]$ and $Al(O_{2}PF_{2})_{3}$ was observed with hexacoordinate aluminum atoms and verified by NMR, IR and X-ray crystallography. A possible mechanism towards these compounds was postulated in the solvent induced dismutation of the tetracoordinate $Li[Al(O_{2}PF_{2})_{4}].$ A singly charged WCA was realized by the exchange of the central aluminum atom for boron. The $[B(O_{2}PF_{2})_{4}]^{−}$ anion was prepared starting from $BH_{3}·S(CH_{3})_{2}$ and boron tribromide leading to the protic room temperature Ionic Liquid (IL) $[H(S(CH_{3})_{2})][B(O_{2}PF_{2})_{4}]$ and the neat liquid Brønsted acid $H[B(O_{2}PF_{2})_{4}],$ respectively, representing a significantly improved synthesis with regard to the first experiments of Dove et al. The basicity of the $[B(O_{2}PF_{2})_{4}]^{−}$ anion and its WCA quality were investigated on the basis of the IR-spectroscopic NH-scale and the salt $[H(N(Oct)_{3})][B(O_{2}PF_{2})_{4}]$ that places it better than all oxyanions and close to the carboranate based WCAs. A pathway to the solvent free pure $Li[B(O_{2}PF_{2})_{4}]$ salt was established on a multi-gram scale with excellent purities enabling electrochemical applications (verified by NMR, IR, X-ray crystallography and cyclovoltammetry).
ISSN	14779226
Issue Number	15
Journal	Dalton Trans.
Volume Number	44
e-ISSN	13645447
Language	English
Publisher	Royal Society of Chemistry
Publisher Date	2015-04-21
Publisher Place	Great Britain (UK)
Access Restriction	Subscribed
Subject Keyword	Chemistry
Content Type	Text
Resource Type	Article
Subject	Inorganic Chemistry

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