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Mixed halide/phosphine complexes of the dirhenium core. Part 7. Reactions of [Re2I8]2- with monodentate phosphines
Angaridis, Panagiotis,Cotton,Dikarev, Evgeny V.,Petrukhina, Marina. A
, p. 755 - 765 (2001)
Reactions of the octaiododirhenate anion [Re2I8]2- with monodentate phosphines (PR3 = PMe3 (1), PMe2Ph (2), PEt3 (3), and PEt2Ph (4)) have been studied in two different solvents, ethanol and benzene, at room temperature. The reactions in ethanol resulted in two-electron reduction products having the Re4+2 core, Re2I4(PR3)4 (R3 = Me3 (1a) and Me2Ph (2a)), for which X-ray diffraction study revealed a 1,3,6,8 isomer type. The reaction of [Re2I8]2- with PMe3 in benzene led to an intermediate edge-sharing bioctahedral dirhenium(III) complex, Re2(μ-I)2I4(PMe3)4 (1b), with no metal-metal bond. The interaction of PEt3 with [Re2I8]2- in benzene again yielded a kinetic product with a different stoichiometry and a Re5+2 core, [Bun4N][Re2I6 (PEt3)2] (3c). The analogous reactions of [Re2I8]2- with PMe2Ph and PEt2Ph in benzene involved two-electron reductions and gave complex 2a and Re2I4(PEt2Ph)4 (4a), as products. Reduction of 1b with KC8 gave 1a as the main product along with a few crystals of 1,3,6-Re2I5(PMe3)3 (1d). Mixed iodide/phosphine complexes of the dirhenium core Ren+2, where n = 4 (1a, 2a, 4a), 5 (1d, 3c), and 6 (1b) have for the first time been characterized by X-ray crystallography. In addition, these products have been further identified by a combination of mass spectrometry and cyclic voltammetric measurements.
