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. Hay; Brian F. G. Johnson; Jack Lewis; Paul R. Raithby; Alan J. Whitton

doi:10.1039/DT9880002091

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. Hay, Brian F. G. Johnson, Jack Lewis, Paul R. Raithby, Alan J. Whitton

University of Cambridge

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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.

Original language	English
Pages (from-to)	2091-2097
Number of pages	7
Journal	Journal of the Chemical Society, Dalton Transactions
Issue number	8
DOIs	https://doi.org/10.1039/DT9880002091
Publication status	Published - 31 Dec 1988

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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]. / Hay, Caroline M.; Johnson, Brian F. G.; Lewis, Jack et al.
In: Journal of the Chemical Society, Dalton Transactions, No. 8, 31.12.1988, p. 2091-2097.

Research output: Contribution to journal › Article › peer-review

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title = "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]",

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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AU - Hay, Caroline M.

AU - Johnson, Brian F. G.

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AU - Raithby, Paul R.

AU - Whitton, Alan J.

PY - 1988/12/31

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N2 - 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.

AB - 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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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]

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