Abstract
New heterometallic alkoxides [LiNb(OCH 2CMe 3) 6] 2 ( 4), LiNb(OCH 2CMe 3) 6(Me 3CCH 2OH) 2 ( 5), and [LiNb(OCH 2SiMe 3) 6] 2 ( 6) have been prepared from the corresponding homometallic alkoxides. All are moderately soluble in hydrocarbons and sublime in moderate to good recoveries. The structure of 6 determined crystallographically contains an Nb 2Li 2( μ-O) 4( μ 3-O) 2 central-core geometry. Compound 4 appears to be isostructural on the basis of 1H NMR data. Bulk pyrolysis of 4 gives crystalline LiNbO 3 under N 2 at 600°C. However, LiNbO 3 films are not obtained from 4 by spray MOCVD under conditions that give LiNbO 3 films from [LiNb(OEt) 6] ∞. Crystallographic structure determination for the precursor compound [Nb(μ-OCH 2SiMe 3)(OCH 2SiMe 3) 4] 2 ( 3) reveals an edge-shared biotahedral geometry in which the μ-O atoms are distinctly pyramidal. This structure is maintained in solution; the pyramidal bridge configurations allow coexistence of syn and anti dimeric isomers. Precursor 3 also exhibits a dimer-monomer equilibrium for which ΔH = 63(3) kJ/mol and ΔS = 180(10) J/(K mol).
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