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DOI: 10.1039/A606707G (Paper) Reference Section for: J. Chem. Soc., Dalton Trans., 1997, 1201-1204

Synthesis, characterization and crystal structure of [(Hdmpz){HB(dmpz)3}VO(µ-η5-C 5H4CO2)Fe(η5-C5 H5)] (Hdmpz = 3,5-dimethylpyrazole)

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David Collison, Frank E. Mabbs, Scott S. Turner, Anne K. Powell, Eric J. L. McInnes and Lesley J. Yellowlees

Abstract

The complex [(Hdmpz){HB(dmpz)3}VO(µ-η5-C 5H4CO2)Fe(η5-C5 H5)] 1 (Hdmpz = 3,5-dimethylpyrazole) has been synthesized and its spectroscopic properties and crystal structure determined. It crystallizes in the triclinic space group P[1 with combining macron], with a = 10.563(2), b = 12.460(4), c = 13.028(5) Å, α = 95.16(3), β = 98.93(2), γ = 99.59(2)° and Z = 2. The vanadium(IV) ion is in a distorted-octahedral environment with nitrogen atoms of the borate ligand occupying three facial sites and the other sites by an oxo group, an oxygen atom from the ferrocenecarboxylate, and a nitrogen atom from a neutral Hdmpz. The cyclic voltammogram in CH2Cl2 showed two oxidations at +0.70 and +1.41 V vs. Ag–AgCl, which are completely reversible at -30 °C. The first corresponds to oxidation of the ferrocenecarboxylate moeity, giving 1+. The reversibility of 1 → 1+ has also been demonstrated by electronic absorption and EPR resonance spectroscopies. Complex 1 is EPR active giving spectra as expected from an isolated vanadium(IV) centre, whilst 1+ is EPR silent.

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