triangulo-Trirhenium(III) alkyl compounds. The X-ray crystal structures of Re3(µ-Cl)1.5(µ-Me)1.5(CH2Ph)6 and Re3(µ-Me)3(CH2Ph)6

Abstract

A new large scale synthesis of Re₃(µ-Cl)₃(CH₂Ph)₆, and the previously unknown Re₃(µ-Cl)₃(CH₂C₆H₄Bu^t-4)₆ are described. Substitution of the bridging halide with excess LiMe leads to the complexes Re₃(µ-Me)₃R₆(R = CH₂Ph or CH₂C₆H₄Bu^t–4). Stoicheiometric reactions with LiMe give mixed halide–methyl products. The X-ray crystal structures of Re₃(µ-Cl)_1.5(µ-Me)_1.5(CH₂Ph)₆ and Re₃(µ-Me)₃(CH₂Ph)₆ have been determined. PMe₃ displaces tetrahydrofuran (thf) from Re₃Cl₉(thf)₃ to give Re₃(µ-Cl)Cl₆(PMe₃)₃, which in turn with AlMe₃ yields the green compound Re₃(µ-Cl)₃Me₆(PMe₃)₃.