Synthesis and characterization of a series of mononuclear tantalum (V) hydride compounds containing aryloxide ligation
- Purdue Univ., West lafayette, IN (United States)
In this paper we report on the synthesis, structure and spectroscopic properties of an extensive series of mononuclear hydride compounds of tantalum(V). We find that two synthetic procedures are superior for the formation of hydrido aryloxides in high yield. The first involves addition of Bu{sup n}{sub 3}SnH to the corresponding chloride in the presence of phosphine ligands. The second involves initial formation of the corresponding alkyl intermediate followed by hydrogenolysis, again in the presence of a suitable phosphine ligand. Two sets of six-coordinate dihydride complexes were obtained either by the hydrogenolysis of the bisalkyl [Ta(OC{sub 6}H{sub 3}Pr{sup i}{sub 2}-2,6){sub 3}(CH{sub 2}C{sub 6}H{sub 4 }-4Me){sub 2}] or by treating the trichloride [Ta(OC{sub 6}H{sub 3}Bu{sup t}{sub 2}-2,6){sub 2}Cl{sub 3}] with Bu{sup n}{sub 3}SnH/L in benzene solution. Some alternative methods have been evaluated for the synthesis of the tantalum-hydride compounds 1-5. The addition of hydride reagents such as LiBH{sub 4} and LiAlH{sub 4} to hydrocarbon solutions of phosphine ligands and halides such as [Ta(OC{sub 6}H{sub 3}Pr{sup i}{sub 2}-2,6){sub 2}Cl{sub 3}] will generate detectable amounts of hydrido complexes, but isolation of the compounds from the reaction mixtures was not convenient. We find that hydride compounds are generated by this procedure, although again yields of isolated material are lower than these obtained via hydrogenolysis of the alkyl precursor. 15 refs., 10 figs., 8 tabs.
- Sponsoring Organization:
- USDOE
- OSTI ID:
- 70375
- Journal Information:
- Organometallics, Journal Name: Organometallics Journal Issue: 6 Vol. 14; ISSN ORGND7; ISSN 0276-7333
- Country of Publication:
- United States
- Language:
- English
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