Synthesis and Structural Characterization of (Perfluoroalkyl)fluoroiridium(III) and (Perfluoroalkyl)methyliridium(III) Compounds
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- 作者：Cheryl J. Bourgeois ; Shaun A. Garratt ; Russell P. Hughes ; Roman B. Larichev ; Jeremy M. Smith ; Antony J. Ward ; Stefan Willemsen ; Donghui Zhang ; Antonio G. DiPasquale ; Lev N. Zakharov ; and Arnold L. Rhe
- 刊名：Organometallics
- 出版年：2006
- 出版时间：July 3, 2006
- 年：2006
- 卷：25
- 期：14
- 页码：3474 - 3480
- 全文大小：140K
- 年卷期：v.25,no.14(July 3, 2006)
- ISSN：1520-6041
文摘
A new family of metal perfluoroalkyl fluoro compounds has been obtained by treatment of the iodoprecursors Cp*Ir(PMe3)(RF)I with AgF in CH2Cl2 solution in the dark to give Cp*Ir(PMe3)(RF)F (RF =CF3, CF2CF3, CF2CF2CF3, CF(CF3)2, CF(CF3)(CF2CF3)). The molecular structures of the compoundswith RF = CF2CF3, CF2CF2CF3, CF(CF3)2 have been determined crystallographically. These fluorocompounds provide a ready and reproducible route to the analogous methyl complexes Cp*Ir(PMe3)(RF)CH3, by treatment with exactly 0.5 equiv of Zn(CH3)2 at low temperatures in toluene. Alkylationwith other reagents such as CH3Li and Cp2Zr(CH3)2 leads to inseparable mixtures. This metathesis ofIr-F and Zn-CH3 represents the only way to date for the clean reproducible synthesis of Cp*Ir(PMe3)(RF)CH3 compounds containing primary perfluoroalkyl groups. The molecular structures of Cp*Ir(PMe3)(RF)CH3 (RF = CF2CF3, CF2CF2CF3) have been determined crystallographically.