Cluster build-up reactions via the ionic coupling of tetraosmium anions and the [RhCp*(NCMe)3]2+ cation; The crystal and molecular structures of [Os4Rh(μ-H)3(MeC=NH)(CO)11(η 5-Cp*)], [Os4Rh(μ-H)2(CO)13(η5-Cp *)]

William Clegg; Neil Feeder; Ana M. Martin Castro; Saifun Nahar; Paul R. Raithby; Gregory P. Shields; Simon J. Teat

doi:10.1016/S0022-328X(98)00834-1

Cluster build-up reactions via the ionic coupling of tetraosmium anions and the [RhCp(NCMe)₃]²⁺ cation; The crystal and molecular structures of [Os₄Rh(μ-H)₃(MeC=NH)(CO)₁₁(η ⁵-Cp)], [Os₄Rh(μ-H)₂(CO)₁₃(η⁵-Cp ^*)]

William Clegg, Neil Feeder, Ana M. Martin Castro, Saifun Nahar, Paul R. Raithby, Gregory P. Shields, Simon J. Teat

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

13 Citations (SciVal)

Abstract

The reaction of [Os₄H₄(CO)₁₁]^2- 2, formed by the reduction of [Os₄H₄(CO)₁₂] 1 with K/Ph₂CO, with the cation [Rh(η⁵-Cp*)(MeCN)₃]²⁺ (Cp*=C₅Me₅) 3, affords a number of penta- and hexanuclear mixed-metal clusters depending on the reaction conditions. If only sufficient K/Ph₂CO is added to dissolve all of 1, and the dication 3 added, a low yield of a blue cluster [Os₄Rh(μ-H)₃(MeC=NH)(CO)₁₁(η ⁵-Cp*)] (Cp*=C₅Me₅) 4 is obtained in addition to large quantities of 1. If an excess of K/Ph₂CO is added so that reduction of 1 is complete, and then the dication 3 added, two new products [Os₄Rh(μ-H)₂(CO)₁₃(η ⁵-Cp*)] 5 and [Os₄Rh₂(μ-H)₂(CO)₁₁(η ⁵-Cp*)₂] 6 are obtained in low yield. The three new complexes have been characterised spectroscopically and crystallographically. Cluster 4 contains the uncommon MeC=NH group coordinated to an edge-bridged tetrahedral metal framework. The metal framework in 5 is also a Rh edge-bridged Os₄ tetrahedron while that of 6 is a bicapped tetrahedron, with two Rh atoms face capping two faces of an Os₄ tetrahedron.

Original language	English
Pages (from-to)	237-246
Number of pages	10
Journal	Journal of Organometallic Chemistry
Volume	573
Issue number	1-2
DOIs	https://doi.org/10.1016/S0022-328X(98)00834-1
Publication status	Published - 31 Jan 1999

Keywords

Cluster
Crystal structures
Cyclopentadienyl
Osmium
Rhodium

ASJC Scopus subject areas

Biochemistry
Physical and Theoretical Chemistry
Organic Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/S0022-328X(98)00834-1

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Clegg, W., Feeder, N., Martin Castro, A. M., Nahar, S., Raithby, P. R., Shields, G. P., & Teat, S. J. (1999). Cluster build-up reactions via the ionic coupling of tetraosmium anions and the [RhCp*(NCMe)₃]²⁺ cation; The crystal and molecular structures of [Os₄Rh(μ-H)₃(MeC=NH)(CO)₁₁(η ⁵-Cp*)], [Os₄Rh(μ-H)₂(CO)₁₃(η⁵-Cp ^*)]. Journal of Organometallic Chemistry, 573(1-2), 237-246. https://doi.org/10.1016/S0022-328X(98)00834-1

Cluster build-up reactions via the ionic coupling of tetraosmium anions and the [RhCp*(NCMe)₃]²⁺ cation; The crystal and molecular structures of [Os₄Rh(μ-H)₃(MeC=NH)(CO)₁₁(η ⁵-Cp*)], [Os₄Rh(μ-H)₂(CO)₁₃(η⁵-Cp ^*)]. / Clegg, William; Feeder, Neil; Martin Castro, Ana M. et al.

In: Journal of Organometallic Chemistry, Vol. 573, No. 1-2, 31.01.1999, p. 237-246.

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

Clegg, W, Feeder, N, Martin Castro, AM, Nahar, S, Raithby, PR, Shields, GP & Teat, SJ 1999, 'Cluster build-up reactions via the ionic coupling of tetraosmium anions and the [RhCp*(NCMe)₃]²⁺ cation; The crystal and molecular structures of [Os₄Rh(μ-H)₃(MeC=NH)(CO)₁₁(η ⁵-Cp*)], [Os₄Rh(μ-H)₂(CO)₁₃(η⁵-Cp ^*)]', Journal of Organometallic Chemistry, vol. 573, no. 1-2, pp. 237-246. https://doi.org/10.1016/S0022-328X(98)00834-1

Clegg W, Feeder N, Martin Castro AM, Nahar S, Raithby PR, Shields GP et al. Cluster build-up reactions via the ionic coupling of tetraosmium anions and the [RhCp*(NCMe)₃]²⁺ cation; The crystal and molecular structures of [Os₄Rh(μ-H)₃(MeC=NH)(CO)₁₁(η ⁵-Cp*)], [Os₄Rh(μ-H)₂(CO)₁₃(η⁵-Cp ^*)]. Journal of Organometallic Chemistry. 1999 Jan 31;573(1-2):237-246. doi: 10.1016/S0022-328X(98)00834-1

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title = "Cluster build-up reactions via the ionic coupling of tetraosmium anions and the [RhCp*(NCMe)3]2+ cation; The crystal and molecular structures of [Os4Rh(μ-H)3(MeC=NH)(CO)11(η 5-Cp*)], [Os4Rh(μ-H)2(CO)13(η5-Cp *)]",

abstract = "The reaction of [Os4H4(CO)11]2- 2, formed by the reduction of [Os4H4(CO)12] 1 with K/Ph2CO, with the cation [Rh(η5-Cp*)(MeCN)3]2+ (Cp*=C5Me5) 3, affords a number of penta- and hexanuclear mixed-metal clusters depending on the reaction conditions. If only sufficient K/Ph2CO is added to dissolve all of 1, and the dication 3 added, a low yield of a blue cluster [Os4Rh(μ-H)3(MeC=NH)(CO)11(η 5-Cp*)] (Cp*=C5Me5) 4 is obtained in addition to large quantities of 1. If an excess of K/Ph2CO is added so that reduction of 1 is complete, and then the dication 3 added, two new products [Os4Rh(μ-H)2(CO)13(η 5-Cp*)] 5 and [Os4Rh2(μ-H)2(CO)11(η 5-Cp*)2] 6 are obtained in low yield. The three new complexes have been characterised spectroscopically and crystallographically. Cluster 4 contains the uncommon MeC=NH group coordinated to an edge-bridged tetrahedral metal framework. The metal framework in 5 is also a Rh edge-bridged Os4 tetrahedron while that of 6 is a bicapped tetrahedron, with two Rh atoms face capping two faces of an Os4 tetrahedron.",

keywords = "Cluster, Crystal structures, Cyclopentadienyl, Osmium, Rhodium",

author = "William Clegg and Neil Feeder and {Martin Castro}, {Ana M.} and Saifun Nahar and Raithby, {Paul R.} and Shields, {Gregory P.} and Teat, {Simon J.}",

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doi = "10.1016/S0022-328X(98)00834-1",

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T1 - Cluster build-up reactions via the ionic coupling of tetraosmium anions and the [RhCp*(NCMe)3]2+ cation; The crystal and molecular structures of [Os4Rh(μ-H)3(MeC=NH)(CO)11(η 5-Cp*)], [Os4Rh(μ-H)2(CO)13(η5-Cp *)]

AU - Clegg, William

AU - Feeder, Neil

AU - Martin Castro, Ana M.

AU - Nahar, Saifun

AU - Raithby, Paul R.

AU - Shields, Gregory P.

AU - Teat, Simon J.

PY - 1999/1/31

Y1 - 1999/1/31

N2 - The reaction of [Os4H4(CO)11]2- 2, formed by the reduction of [Os4H4(CO)12] 1 with K/Ph2CO, with the cation [Rh(η5-Cp*)(MeCN)3]2+ (Cp*=C5Me5) 3, affords a number of penta- and hexanuclear mixed-metal clusters depending on the reaction conditions. If only sufficient K/Ph2CO is added to dissolve all of 1, and the dication 3 added, a low yield of a blue cluster [Os4Rh(μ-H)3(MeC=NH)(CO)11(η 5-Cp*)] (Cp*=C5Me5) 4 is obtained in addition to large quantities of 1. If an excess of K/Ph2CO is added so that reduction of 1 is complete, and then the dication 3 added, two new products [Os4Rh(μ-H)2(CO)13(η 5-Cp*)] 5 and [Os4Rh2(μ-H)2(CO)11(η 5-Cp*)2] 6 are obtained in low yield. The three new complexes have been characterised spectroscopically and crystallographically. Cluster 4 contains the uncommon MeC=NH group coordinated to an edge-bridged tetrahedral metal framework. The metal framework in 5 is also a Rh edge-bridged Os4 tetrahedron while that of 6 is a bicapped tetrahedron, with two Rh atoms face capping two faces of an Os4 tetrahedron.

AB - The reaction of [Os4H4(CO)11]2- 2, formed by the reduction of [Os4H4(CO)12] 1 with K/Ph2CO, with the cation [Rh(η5-Cp*)(MeCN)3]2+ (Cp*=C5Me5) 3, affords a number of penta- and hexanuclear mixed-metal clusters depending on the reaction conditions. If only sufficient K/Ph2CO is added to dissolve all of 1, and the dication 3 added, a low yield of a blue cluster [Os4Rh(μ-H)3(MeC=NH)(CO)11(η 5-Cp*)] (Cp*=C5Me5) 4 is obtained in addition to large quantities of 1. If an excess of K/Ph2CO is added so that reduction of 1 is complete, and then the dication 3 added, two new products [Os4Rh(μ-H)2(CO)13(η 5-Cp*)] 5 and [Os4Rh2(μ-H)2(CO)11(η 5-Cp*)2] 6 are obtained in low yield. The three new complexes have been characterised spectroscopically and crystallographically. Cluster 4 contains the uncommon MeC=NH group coordinated to an edge-bridged tetrahedral metal framework. The metal framework in 5 is also a Rh edge-bridged Os4 tetrahedron while that of 6 is a bicapped tetrahedron, with two Rh atoms face capping two faces of an Os4 tetrahedron.

KW - Cluster

KW - Crystal structures

KW - Cyclopentadienyl

KW - Osmium

KW - Rhodium

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