Synthesis and structural characterization of (perfluoroalkyl) fluoroiridium(III) and (perfluoroalkyl)methyliridium(III) compounds

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A new family of metal perfluoroalkyl fluoro compounds has been obtained by treatment of the iodo precursors Cp*Ir(PMe 3)(R F)I with AgF in CH 2Cl 2 solution in the dark to give Cp*Ir(PMe 3)(R F)F (R F = CF 3, CF 2CF 3, CF 2CF 2CF 3, CF(CF 3) 2, CF(CF 3)(CF 2CF 3)). The molecular structures of the compounds with RF = CF 2CF 3, CF 2CF 2CF 3, CF(CF 3) 2 have been determined crystallographically. These fluoro compounds provide a ready and reproducible route to the analogous methyl complexes Cp*Ir(PMe 3)-(R F)CH 3, by treatment with exactly 0.5 equiv of Zn(CH 3) 2 at low temperatures in toluene. Alkylation with other reagents such as CH 3Li and Cp 2Zr(CH 3) 2 leads to inseparable mixtures. This metathesis of Ir-F and Zn-CH 3 represents the only way to date for the clean reproducible synthesis of Cp*Ir(PMe 3)-(R F)CH 3 compounds containing primary perfluoroalkyl groups. The molecular structures of Cp*Ir(PMe 3)-(R F)CH 3 (R F = CF 2CF 3, CF 2CF 2CF 3) have been determined crystallographically. © 2006 American Chemical Society.

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