Syntheses and crystal structures of vanadium and iron chloride complexes with diglyme

Abstract

A mononuclear molecular complex fac-[VCl₃(diglyme)] (1) resulted from the reaction of VCl₃ and diglyme (diglyme = di(2-methoxyethyl)ether) in dichloromethane. The violet complex 1 is a sensitive substance which slowly oxidized to a new, blue mononuclear molecular complex, fac-[VOCl₂(diglyme)] (2) in the presence of air.

The synthesis of iron(II), iron(III) complex [FeCl(diglyme)(THF)]₂[FeCl₄)]₂ (3) was achieved by the reaction of yellow-green, partly oxidized FeCl₂^.4H₂O, diglyme and chlorotrimethyl-silane in tetrahydofuran. The compound consists of the dinuclear cations with octahedral environment of iron(II) and the tetrahedral anions of iron(III). A pure iron(II) chloride-diglyme complex [FeCl₂(diglyme)]₂ (4) was gained by the reaction of freshly prepared iron(II) chloride hydrate, diglyme and chlorotrimethylsilane in dichloromethane. Diglyme is coordinated in the meridional mode to octahedral iron(II) in dinuclear cations of 3 and in dinuclear molecules 4.