Addition of NHC→SiCl4 to the highly Lewis acidic bis(pentafluoroethyl)silane ((C2F5)2SiH2) afforded the salt [(NHC)2SiCl2H][(C2F5)2SiCl3] with pentacoordinate silicon in the cation and the anion. The anion represents the first example of a chlorosilicate structurally characterized in the solid state. In this reaction, the long sought pentacoordinate NHC-adduct of silicochloroform was identified as an intermediate and its crystal structure is presented.
Durch Reduktion einer Lösung von Heptafluor‐n‐propyl‐eisen‐tetracarbonyljodid, C3F7Fe(CO)4J, in Methanol mittels Natriumboranats entsteht eine Lösung, aus der Quecksilbercyanid und Tri‐o‐phenanthrolin‐eisen(II)‐sulfat Derivate des Heptafluor‐n‐propyl‐eisentetracarbonylwasserstoffs, [C3F7Fe(CO)4]2Hg und [C3F7Fe(CO)(4)]2[Fe(N2C12H8)3] ausfällen. Aus dem Phenanthrolinderivat kann mittels Phosphorsäure das äußerst zersetzliche Carbonylhydrid C3F7Fe(CO)4H in Freiheit gesetzt werden. Die beiden beständigen Verbindungen sind durch IR‐, NMR‐ und Massenspektren charakterisiert worden.
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