European Journal of Inorganic Chemistry p. 4663 - 4668 (2007)
Update date:2022-08-03
Topics:
Sugimoto, Hideki
Tarumizu, Makoto
Miyake, Hiroyuki
Tsukube, Hiroshi
New tungsten(VI), -(V), and -(IV) complexes containing 3,6-dichloro-1,2- benzenedithiolate (bdtCl2), (Et4N)2[W VIO2(bdtCl2)2] {(Et 4N)2[1]}, (Et4N)[WVO(bdtCl 2)2] {(Et4N)[2]}, and (Et4N) 2[WIVO(bdtCl2)2] {(Et 4N)2[3]} were synthesized and characterized as active site models of tungstoenzymes. (Et4N)2[1] was prepared in high yield by the reaction of WO2Cl2 with 2bdtCl2 at low temperature, and its crystal structure was determined. Isomerization between octahedral structures (Δ and Λ forms) of the tungsten center of (Bu4N)2[1] was characterized by variable-temperature 1H NMR (VT 1H NMR) spectral analysis, which offers the first example of six-coordinate bis(dithiolene) tungsten(VI) complexes. The isomerization of the molybdenum center of (Bu4N) 2[MoVIO2(bdtCl2)2] {(Bu4N)2[4]} was similarly characterized. A comparison of their activation energies indicated that the tungsten center underwent slower isomerization than that of the molybdenum one. (Et4N)2[1] underwent an irreversible reduction at -2.1 V vs. SCE in CH3CN by a coupled electron-proton transfer (CEPT) process to yield (Et4N) 2[3], while (Et4N)2[3] underwent an irreversible oxidation by a CEPT process at -0.27 V in the presence of 2 equiv. of Et4NOH in CH3CN to yield (Et4N) 2[1]. (Et4N)[2] disproportionated into 0.5 equiv. of (Et4N)2[1] and 0.5 equiv. of (Et4N) 2[3] when treated with 1 equiv. of Et4NOH in CH 3CN. Wiley-VCH Verlag GmbH & Co. KGaA, 2007.
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