Abstract
The binary lead fluoride Pb3F8 was synthesized by the reaction of anhydrous HF with Pb3O4 or by the reaction of BrF3 with PbF2. The compound was characterized by single‐crystal and powder X‐ray diffraction, IR, Raman, and solid‐state MAS 19F NMR spectroscopy, as well as thermogravimetric analysis, XP and near‐edge X‐ray absorption fine structure (NEXAFS) spectroscopy. Solid‐state quantum‐chemical calculations are provided for the vibrational analyses and band assignments. The electronic band structure offers an inside view of the mixed valence compound.
Highlights
The binary lead fluorides PbF2 and PbF4 are well established compounds.[1,2] Their first lab synthesis dates back to the first half of the 19th century and the determination of their crystal structures to 1944 and 1962, respectively.[1,2,3,4] In addition, PbF3, which is better described as Pb2F6 containing PbII and PbIV atoms, was reported.[5]
Pb3O4 is reacted with an excess of anhydrous HF at room temperature, so that the equilibrium of the reaction is shifted to the product side
If the reaction mixture is allowed to stand for three days at room temperature, or, if an excess of anhydrous HF (aHF) is used that is too small, a
Summary
Nothing besides this average composition has been reported. Pb3F8 was first mentioned in 1972 by Banner and co-workers as a result of the reaction of Pb3O4 with gaseous HF on a thermogravimetric scale.[14] In their search for Pb2F6, Charpin and co-workers described reactions leading to Pb3F8 as a product or side product. No details on Pb3F8 were given, even not how the compound was identified as Pb3F8.[15] we present the synthesis and characterization of the binary lead(II/IV) fluoride Pb3F8
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