Synthesis, characterization and crystal structure of [(Hdmpz){HB(dmpz)3}VO(μ-η5-C 5H4CO2)Fe(η5-C5 H5)] (Hdmpz = 3,5-dimethylpyrazole)
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS(1997)
摘要
The complex [(Hdmpz){HB(dmpz)(3)}VO(mu-eta(5)-C5H4CO2)Fe(eta(5)-C5H5)] 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) over bar, with a = 10.563(2), b = 12.460(4), c = 13.028(5) Angstrom, alpha = 95.16(3), beta = 38.93(2), gamma = 99.59(2)degrees 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 degrees 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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关键词
crystal structure
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