Tantalum(V) alkoxides : Electrochemical synthesis, mass-spectral investigation and oxoalkoxocomplexes

Add time:07/22/2019    Source:sciencedirect.com

Ta(OR)5 (R = Me(1), Et(2), Bun(3)) and Ta2O(OPri)8·PriOH (4) were obtained by the anodic oxidation of metallic tantalum in absolute alcohols in the presence of LiCl (electroconductive additive). Ta(OPri)5 (5) was isolated by distillation in the course of thermolysis of 4 under reduced pressure. Ta(OC2H4OMe)5 (6) was obtained by reaction of 5 with 2-methoxyethanol. Compounds 1 and 5 are isostructural with the corresponding [Nb(OR)5]2 (R = Me,Pr'); their molecules involve two [M061 octrahedra sharing a common edge. Recrystallization of 1 from McOH at < 20°C resulted in the isolation of a monosolvate Ta(OMe)5·MeOH. The solubility of Ta(OMe)5 in . was studied in the temperature range of −80°C to 50°C. The dinuclear molecule 4 has one, μ-O(oxo) and one μ-OR group, ROH is in an axial position. Compound 4 is the first example of a stable oxoalkoxide (in solution and gas phase) with as few as two metal nuclei, in contrast to most MxOx(OR)z, which are usually of higher nuclearity. Crystalline Ta709(OPri)17 (7) was obtained by the uncontrolled hydrolysis of 4 and 5. Its molecule is a heptanuclear metal oxoalkoxide of a new type containing a metal core consisting of tetrahedra [Ta4] with a common vertex. In the mass spectra of 1–3 and 5, along with the ions obtained on fragmentation of Ta(OR)5, fragments of Ta20(OR)8 (R = Me, Et, Bu, Pr') molecules were recorded, the latter are formed as a result of elimination of R2O from Ta(OR)5.

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