Cyclopentadienylmolybdenum(VI) and molybdenum(V) oxo chemistry: New synthetic and structural features
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Date
2002
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Abstract
Convenient syntheses for Cp, Cp*, and related cyclopentadienyl derivatives (4Cp = C5HiPr4i CP‴ = C5H2tBU3-1,2,4) of formula [(Ring)2Mo2O5] are described. Compound [Cp2Mo2O5] was produced in good yields by the rapid oxidation of red [CpMoO2]4 with PhIO in CH2Cl2. [Cp*2Mo2O5] was obtained by CH3COOH acidification of aqueous solutions of [Cp*MoO3]-Na+, the latter being generated in a single step from [Cp*MoCl4] and more than 5 equiv. of aqueous NaOH in air. Minor quantities of [Cp*MoO2]2 were also isolated from this reaction, although the formation of this by-product may be reduced by using a two-step basic hydrolysis procedure. Extension of the latter strategy also allowed the preparation of [4Cp2Mo2O5], [Cp‴2Mo2O5], and [4CpMoO2Cl] in good yields, in addition to the by-product [Cp‴MoO2]2. X-ray structures are reported for compounds [4Cp2Mo2O5], [Cp‴2Mo2O5], [Cp*MoO2]2, [Cp‴MoO2]2, and [4CpMoO2Cl]. © Wiley-VCH Verlag GmbH, 69451 Weinheim, Germany, 2002.
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Keywords
Chlorine compounds , Ligands , Molybdenum oxide , Sodium hydroxide , cyclopentadienylmolybdenum , molybdenum complex , unclassified drug , Basic hydrolysis , Cyclopentadienyl ligands , Cyclopentadienyls , Oxo ligands , Rapid oxidation , Single-step , Structural feature , X-ray structure , acidification , aqueous solution , article , chemical structure , hydrolysis , oxidation , reduction , structure analysis , synthesis , X ray , X ray crystallography