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

Acta chimica Slovenica (2015-06-19)
Saša Petriček, Alojz Demšar
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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Chlorotrimethylsilane solution, 1.0 M in THF
Sigma-Aldrich
Vanadium(III) chloride, 97%
Sigma-Aldrich
Hydrochloric acid solution, 32 wt. % in H2O, FCC
Supelco
Hydrochloric acid solution, volumetric, 0.1 M HCl (0.1N), endotoxin free
Sigma-Aldrich
Hydrochloric acid solution, 1.0 N, BioReagent, suitable for cell culture
Sigma-Aldrich
Chlorotrimethylsilane, purified by redistillation, ≥99%
Sigma-Aldrich
Diethylene glycol dimethyl ether, anhydrous, 99.5%
Sigma-Aldrich
Chlorotrimethylsilane, ≥98.0% (GC)
Sigma-Aldrich
Hydrochloric acid solution, ~6 M in H2O, for amino acid analysis
Sigma-Aldrich
Chlorotrimethylsilane, produced by Wacker Chemie AG, Burghausen, Germany, ≥99.0% (GC)
Sigma-Aldrich
Hydrochloric acid, 36.5-38.0%, BioReagent, for molecular biology
Sigma-Aldrich
Hydrogen chloride solution, 3 M in cyclopentyl methyl ether (CPME)