Use of the monocationic fragment [Ru(η5-C5H5)(MeCN)3]+ as a capping reagent in the synthesis of mixed-metal clusters: Synthesis and structural characterisation of [Os3RuH(CO)11(η5-C5H 5)] and [Os3Ru2(CO)9(μ3-CO) 2...

Radchada Buntem; Jack Lewis; Catherine A. Morewood; Paul R. Raithby; M. Carmen Ramirez De Arellano; Gregory P. Shields

doi:10.1039/a708714d

Use of the monocationic fragment [Ru(η⁵-C₅H₅)(MeCN)₃]⁺ as a capping reagent in the synthesis of mixed-metal clusters: Synthesis and structural characterisation of [Os₃RuH(CO)₁₁(η⁵-C₅H ₅)] and [Os₃Ru₂(CO)₉(μ₃-CO) ₂...

Radchada Buntem
, Jack Lewis
, Catherine A. Morewood
, Paul R. Raithby
, M. Carmen Ramirez De Arellano
, Gregory P. Shields

University of Cambridge

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

20 Citations (SciVal)

Abstract

Title full: Use of the monocationic fragment [Ru(η⁵-C₅H₅)(MeCN)₃]⁺ as a capping reagent in the synthesis of mixed-metal clusters: Synthesis and structural characterisation of [Os₃RuH(CO)₁₁(η⁵-C₅H ₅)] and [Os₃Ru₂(CO)₉(μ₃-CO) ₂(η⁵-C₅H₅)₂]. The reaction of the monoanion [Os₃H(CO)₁₁]^- 1 with 1 equivalent of the cation [Ru(C₅H₅)(MeCN)₃]⁺ 2, in CH₂Cl₂, formed the mixed-metal, tetranuclear cluster [Os₃RuH(CO)₁₁(η⁵-C₅H ₅)] 3 in high yield. Subsequent deprotonation of 3 with 1,8-diazabicyclo[5.4.0]undec-7-ene, in CH₂Cl₂, afforded the anion [Os₃Ru(CO)₁₁-(η⁵-C₅H ₅)]^- 4, and reaction of 4 with a second equivalent of [Ru(C₅H₅)(MeCN)₃]⁺ provided the new bis-(cyclopentadienyl) cluster [Os₃Ru₂(CO)₉(μ₃-CO) ₂(η⁵-C₅H₅)₂] 5 in ca. 80% yield. Alternatively, reduction of [Os₃(CO)₁₂] with K/Ph₂CO afforded the known cluster dianion [Os₃(CO)₁₁]^2- 6 which can be treated with 2 equivalents of [Ru(C₅H₅)(MeCN)₃]⁺ to produce 5 in 75% yield. The clusters 3 and 5 have been fully characterised by both spectroscopic and crystallographic methods. The structure of 3 contains an Os₃Ru tetrahedron in which the cyclopentadienyl ligand is co-ordinated to the Ru atom in an η⁵ terminal mode. The metal framework in 5 is a trigonal bipyramid, but may be viewed as an Os₃Ru tetrahedral unit, as in 3, to which a second Ru atom capping an Os₂Ru triangular face has been added. Both the cyclopentadienyl ligands remain in η⁵ terminal bonding sites co-ordinated to the two Ru atoms.

Original language	English
Pages (from-to)	1091-1095
Number of pages	5
Journal	Journal of the Chemical Society - Dalton Transactions
Issue number	7
DOIs	https://doi.org/10.1039/a708714d
Publication status	Published - 7 Apr 1998

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General Chemistry

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Buntem, R., Lewis, J., Morewood, C. A., Raithby, P. R., Ramirez De Arellano, M. C., & Shields, G. P. (1998). Use of the monocationic fragment [Ru(η⁵-C₅H₅)(MeCN)₃]⁺ as a capping reagent in the synthesis of mixed-metal clusters: Synthesis and structural characterisation of [Os₃RuH(CO)₁₁(η⁵-C₅H ₅)] and [Os₃Ru₂(CO)₉(μ₃-CO) ₂... Journal of the Chemical Society - Dalton Transactions, (7), 1091-1095. https://doi.org/10.1039/a708714d

Use of the monocationic fragment [Ru(η⁵-C₅H₅)(MeCN)₃]⁺ as a capping reagent in the synthesis of mixed-metal clusters: Synthesis and structural characterisation of [Os₃RuH(CO)₁₁(η⁵-C₅H ₅)] and [Os₃Ru₂(CO)₉(μ₃-CO) ₂... / Buntem, Radchada; Lewis, Jack; Morewood, Catherine A. et al.
In: Journal of the Chemical Society - Dalton Transactions, No. 7, 07.04.1998, p. 1091-1095.

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

Buntem, R, Lewis, J, Morewood, CA, Raithby, PR, Ramirez De Arellano, MC & Shields, GP 1998, 'Use of the monocationic fragment [Ru(η⁵-C₅H₅)(MeCN)₃]⁺ as a capping reagent in the synthesis of mixed-metal clusters: Synthesis and structural characterisation of [Os₃RuH(CO)₁₁(η⁵-C₅H ₅)] and [Os₃Ru₂(CO)₉(μ₃-CO) ₂...', Journal of the Chemical Society - Dalton Transactions, no. 7, pp. 1091-1095. https://doi.org/10.1039/a708714d

Buntem R, Lewis J, Morewood CA, Raithby PR, Ramirez De Arellano MC, Shields GP. Use of the monocationic fragment [Ru(η⁵-C₅H₅)(MeCN)₃]⁺ as a capping reagent in the synthesis of mixed-metal clusters: Synthesis and structural characterisation of [Os₃RuH(CO)₁₁(η⁵-C₅H ₅)] and [Os₃Ru₂(CO)₉(μ₃-CO) ₂... Journal of the Chemical Society - Dalton Transactions. 1998 Apr 7;(7):1091-1095. doi: 10.1039/a708714d

Buntem, Radchada ; Lewis, Jack ; Morewood, Catherine A. et al. / Use of the monocationic fragment [Ru(η⁵-C₅H₅)(MeCN)₃]⁺ as a capping reagent in the synthesis of mixed-metal clusters : Synthesis and structural characterisation of [Os₃RuH(CO)₁₁(η⁵-C₅H ₅)] and [Os₃Ru₂(CO)₉(μ₃-CO) ₂... In: Journal of the Chemical Society - Dalton Transactions. 1998 ; No. 7. pp. 1091-1095.

@article{b290e90056e64a37b2dd9680ea0aa52c,

title = "Use of the monocationic fragment [Ru(η5-C5H5)(MeCN)3]+ as a capping reagent in the synthesis of mixed-metal clusters: Synthesis and structural characterisation of [Os3RuH(CO)11(η5-C5H 5)] and [Os3Ru2(CO)9(μ3-CO) 2...",

abstract = "Title full: Use of the monocationic fragment [Ru(η5-C5H5)(MeCN)3]+ as a capping reagent in the synthesis of mixed-metal clusters: Synthesis and structural characterisation of [Os3RuH(CO)11(η5-C5H 5)] and [Os3Ru2(CO)9(μ3-CO) 2(η5-C5H5)2]. The reaction of the monoanion [Os3H(CO)11]- 1 with 1 equivalent of the cation [Ru(C5H5)(MeCN)3]+ 2, in CH2Cl2, formed the mixed-metal, tetranuclear cluster [Os3RuH(CO)11(η5-C5H 5)] 3 in high yield. Subsequent deprotonation of 3 with 1,8-diazabicyclo[5.4.0]undec-7-ene, in CH2Cl2, afforded the anion [Os3Ru(CO)11-(η5-C5H 5)]- 4, and reaction of 4 with a second equivalent of [Ru(C5H5)(MeCN)3]+ provided the new bis-(cyclopentadienyl) cluster [Os3Ru2(CO)9(μ3-CO) 2(η5-C5H5)2] 5 in ca. 80\% yield. Alternatively, reduction of [Os3(CO)12] with K/Ph2CO afforded the known cluster dianion [Os3(CO)11]2- 6 which can be treated with 2 equivalents of [Ru(C5H5)(MeCN)3]+ to produce 5 in 75\% yield. The clusters 3 and 5 have been fully characterised by both spectroscopic and crystallographic methods. The structure of 3 contains an Os3Ru tetrahedron in which the cyclopentadienyl ligand is co-ordinated to the Ru atom in an η5 terminal mode. The metal framework in 5 is a trigonal bipyramid, but may be viewed as an Os3Ru tetrahedral unit, as in 3, to which a second Ru atom capping an Os2Ru triangular face has been added. Both the cyclopentadienyl ligands remain in η5 terminal bonding sites co-ordinated to the two Ru atoms.",

author = "Radchada Buntem and Jack Lewis and Morewood, \{Catherine A.\} and Raithby, \{Paul R.\} and \{Ramirez De Arellano\}, \{M. Carmen\} and Shields, \{Gregory P.\}",

year = "1998",

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pages = "1091--1095",

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T1 - Use of the monocationic fragment [Ru(η5-C5H5)(MeCN)3]+ as a capping reagent in the synthesis of mixed-metal clusters

T2 - Synthesis and structural characterisation of [Os3RuH(CO)11(η5-C5H 5)] and [Os3Ru2(CO)9(μ3-CO) 2...

AU - Buntem, Radchada

AU - Lewis, Jack

AU - Morewood, Catherine A.

AU - Raithby, Paul R.

AU - Ramirez De Arellano, M. Carmen

AU - Shields, Gregory P.

PY - 1998/4/7

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N2 - Title full: Use of the monocationic fragment [Ru(η5-C5H5)(MeCN)3]+ as a capping reagent in the synthesis of mixed-metal clusters: Synthesis and structural characterisation of [Os3RuH(CO)11(η5-C5H 5)] and [Os3Ru2(CO)9(μ3-CO) 2(η5-C5H5)2]. The reaction of the monoanion [Os3H(CO)11]- 1 with 1 equivalent of the cation [Ru(C5H5)(MeCN)3]+ 2, in CH2Cl2, formed the mixed-metal, tetranuclear cluster [Os3RuH(CO)11(η5-C5H 5)] 3 in high yield. Subsequent deprotonation of 3 with 1,8-diazabicyclo[5.4.0]undec-7-ene, in CH2Cl2, afforded the anion [Os3Ru(CO)11-(η5-C5H 5)]- 4, and reaction of 4 with a second equivalent of [Ru(C5H5)(MeCN)3]+ provided the new bis-(cyclopentadienyl) cluster [Os3Ru2(CO)9(μ3-CO) 2(η5-C5H5)2] 5 in ca. 80% yield. Alternatively, reduction of [Os3(CO)12] with K/Ph2CO afforded the known cluster dianion [Os3(CO)11]2- 6 which can be treated with 2 equivalents of [Ru(C5H5)(MeCN)3]+ to produce 5 in 75% yield. The clusters 3 and 5 have been fully characterised by both spectroscopic and crystallographic methods. The structure of 3 contains an Os3Ru tetrahedron in which the cyclopentadienyl ligand is co-ordinated to the Ru atom in an η5 terminal mode. The metal framework in 5 is a trigonal bipyramid, but may be viewed as an Os3Ru tetrahedral unit, as in 3, to which a second Ru atom capping an Os2Ru triangular face has been added. Both the cyclopentadienyl ligands remain in η5 terminal bonding sites co-ordinated to the two Ru atoms.

AB - Title full: Use of the monocationic fragment [Ru(η5-C5H5)(MeCN)3]+ as a capping reagent in the synthesis of mixed-metal clusters: Synthesis and structural characterisation of [Os3RuH(CO)11(η5-C5H 5)] and [Os3Ru2(CO)9(μ3-CO) 2(η5-C5H5)2]. The reaction of the monoanion [Os3H(CO)11]- 1 with 1 equivalent of the cation [Ru(C5H5)(MeCN)3]+ 2, in CH2Cl2, formed the mixed-metal, tetranuclear cluster [Os3RuH(CO)11(η5-C5H 5)] 3 in high yield. Subsequent deprotonation of 3 with 1,8-diazabicyclo[5.4.0]undec-7-ene, in CH2Cl2, afforded the anion [Os3Ru(CO)11-(η5-C5H 5)]- 4, and reaction of 4 with a second equivalent of [Ru(C5H5)(MeCN)3]+ provided the new bis-(cyclopentadienyl) cluster [Os3Ru2(CO)9(μ3-CO) 2(η5-C5H5)2] 5 in ca. 80% yield. Alternatively, reduction of [Os3(CO)12] with K/Ph2CO afforded the known cluster dianion [Os3(CO)11]2- 6 which can be treated with 2 equivalents of [Ru(C5H5)(MeCN)3]+ to produce 5 in 75% yield. The clusters 3 and 5 have been fully characterised by both spectroscopic and crystallographic methods. The structure of 3 contains an Os3Ru tetrahedron in which the cyclopentadienyl ligand is co-ordinated to the Ru atom in an η5 terminal mode. The metal framework in 5 is a trigonal bipyramid, but may be viewed as an Os3Ru tetrahedral unit, as in 3, to which a second Ru atom capping an Os2Ru triangular face has been added. Both the cyclopentadienyl ligands remain in η5 terminal bonding sites co-ordinated to the two Ru atoms.

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