Issue 17, 2001
From the journal:

Journal of the Chemical Society, Dalton Transactions

Syntheses of new ruthenium clusters containing sulfur, ynyl and diynyl ligands. Crystal structures of [Ru3(CO)9(μ-η2-SC[triple bond, length as m-dash]CSiMe3)(μ3-η2-C[triple bond, length as m-dash]CSiMe3)], [Ru4(CO)12(μ4-S)(μ-η2-C[triple bond, length as m-dash]CSiMe3)2] and [Ru4(CO)9(μ-CO)2(μ4-S)(μ4-η2-C(SiMe3)C(C[triple bond, length as m-dash]CSiMe3)]

M. I. Alcalde,a   A. J. Carty,b   Y. Chi,c   E. Delgado,*a   B. Donnadieu,d   E. Hernández,a   K. Dallmanna  and  J. Sánchez-Nievesa  

* Corresponding authors

a Departamento de Quimica Inorgánica, Universidad Autónoma de Madrid, Cantoblanco, Spain

b Institute for Molecular Sciences, National Research Council of Canada, 100 Sussex Drive, Ottawa, Ontario, Canada

c Department of Chemistry, National Tsing Hua University, Hsinchu, Taiwan

d Laboratoire de Chimie de Coordination du CNRS. 205, route de Narbonne, France

Abstract

Reaction of Ru3(CO)12 and S(C[triple bond, length as m-dash]CSiMe3)2 in toluene gave [Ru3(CO)9(μ-η2-SC[triple bond, length as m-dash]CSiMe3)(μ3-η2-C[triple bond, length as m-dash]CSiMe3)] 1. The thermolysis of 1 provokes the rupture of the S–Csp bond of the SC[triple bond, length as m-dash]CSiMe3 ligand and C–C coupling reactions between two acetylide groups affording the clusters [Ru3(CO)9(μ3-S)(μ3-η2-C(SiMe3)C(C[triple bond, length as m-dash]CSiMe3)] 2, [Ru2(CO)6(μ-η3-SC[triple bond, length as m-dash]CSiMe3)(μ-η2-C[triple bond, length as m-dash]CSiMe3)] 3, [Ru4(CO)12(μ4-S)(μ-η2-C[triple bond, length as m-dash]CSiMe3)2] 4 and [Ru4(CO)9(μ-CO)2(μ4-S)(μ4-η2-C(SiMe3)C(C[triple bond, length as m-dash]CSiMe3)] 5. All compounds have been characterized by IR and NMR techniques as well as FAB+ mass spectrometry. Crystal structures of 1, 4, and 5 have been determined by X-ray diffraction methods. The pathways of the thermolysis of 1 to give 2–5 have been investigated.

Graphical abstract: Syntheses of new ruthenium clusters containing sulfur, ynyl and diynyl ligands. Crystal structures of [Ru3(CO)9(μ-η2-SC [[triple bond, length as m-dash]] CSiMe3)(μ3-η2-C [[triple bond, length as m-dash]] CSiMe3)], [Ru4(CO)12(μ4-S)(μ-η2-C [[triple bond, length as m-dash]] CSiMe3)2] and [Ru4(CO)9(μ-CO)2(μ4-S)(μ4-η2-C(SiMe3)C(C [[triple bond, length as m-dash]] CSiMe3)]

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Article information

DOI
https://doi.org/10.1039/B103202J
Article type
Paper
Submitted
10 Apr 2001
Accepted
18 Jun 2001
First published
06 Aug 2001

J. Chem. Soc., Dalton Trans., 2001, 2502-2507

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Syntheses of new ruthenium clusters containing sulfur, ynyl and diynyl ligands. Crystal structures of [Ru3(CO)9(μ-η2-SC[triple bond, length as m-dash]CSiMe3)(μ3-η2-C[triple bond, length as m-dash]CSiMe3)], [Ru4(CO)12(μ4-S)(μ-η2-C[triple bond, length as m-dash]CSiMe3)2] and [Ru4(CO)9(μ-CO)2(μ4-S)(μ4-η2-C(SiMe3)C(C[triple bond, length as m-dash]CSiMe3)]

M. I. Alcalde, A. J. Carty, Y. Chi, E. Delgado, B. Donnadieu, E. Hernández, K. Dallmann and J. Sánchez-Nieves, J. Chem. Soc., Dalton Trans., 2001, 2502 DOI: 10.1039/B103202J

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