Cyclopentadienylmolybdenum(VI) and molybdenum(V) oxo chemistry: New synthetic and structural features
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Convenient syntheses for Cp, Cp*, and related cyclopentadienyl derivatives (Cp-4 = C(5)HiPr(4); CP' = C(5)H(2)tBu(3)-1,2,4) of formula [(Ring)(2)MO2O5] 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 [(CP2Mo2O5)-C-4], [CP'2Mo2O5], and [(CpMoO2Cl)-Cp-4] in good yields, in addition to the by-product [CP' MoO2](2). X-ray structures are reported for compounds [(CP2Mo2O5)-C-4], [CP'2Mo2O5], [Cp*MoO2](2), [Cp'MoO2](2), and [(CpMoO2Cl)-Cp-4]. (C) Wiley-VCH Verlag GmbH, 69451 Weinheim, Germany, 2002.