Preparation and characterisation of mixed bismuth and ruthenium clusters; X-ray crystal structures of [Ru3(µ-H)3(CO)9(µ3-Bi)], [Ru3(CO)9(µ3-Bi)2], and [Ru4(CO)12(µ4-Bi)2]
Caroline M. HayBrian F. G. JohnsonJack LewisPaul R. RaithbyAlan J. Whitton
Abstract
The inclusion of naked bismuth atoms into carbonyl cluster compounds of ruthenium has been achieved with the use of bismuth(III) nitrate pentahydrate, Bi(NO3)3·5H2O, as the bismuth containing reagent. We report the high-yield synthesis of [Ru3(µ-H)3(CO)9(µ3-Bi)](1) from the reaction of Bi(NO3)3·5H2O with [NBu4][Ru4H3(CO)12], the preparation of (1) and [Ru3(CO)9(µ3-Bi)2](2) from Bi(NO3)3·5H2O and Na[Ru3H(CO)11], and the preparation of [Ru4(CO)12(µ4-Bi)2](3) from Bi(NO3)3·5H2O and [Ru3(CO)12] in KOH–MeOH solution. The determination of the X-ray crystal structures of (1), (2), and (3) show that (1) has a slightly distorted tetrahedral heavy-metal framework with three hydrides, each bridging a Ru–Ru edge, that (2) has a trigonal-bipyramidal structure with the Ru3 ring capped above and below by µ3-Bi atoms, and that (3) has a square-bipyramidal metal framework with the Ru atoms defining the equatorial square plane and the Bi atoms symmetrically µ4-capping at the axial positions.
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