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Mono-, di- and tetra-nuclear <i>p</i>-cymeneruthenium complexes containing oxalato ligands
Auteur(s)
Yan, Hong
Neels, Antonia
Date de parution
1997
In
Journal of the Chemical Society, Dalton Transactions, 1997//4345-4350
Résumé
The oxalato complexes [Ru<sub>2</sub>(µ-η<sup>4</sup>-C<sub>2</sub>O<sub>4</sub>)Cl<sub>2</sub>(η<sup>6</sup>-<i>p</i>-Pr<sup>i</sup>C<sub>6</sub>H<sub>4</sub>Me)<sub>2</sub>] <b>1</b> and [Ru(η<sup>2</sup>-C<sub>2</sub>O<sub>4</sub>)(NH<sub>3</sub>)(η<sup>6</sup>-<i>p</i>-Pr<sup>i</sup>C<sub>6</sub>H<sub>4</sub>Me)] <b>2</b> have been prepared from the reaction of ammonium oxalate with [{RuCl<sub>2</sub>(η<sup>6</sup>-<i>p</i>-Pr<sup>i</sup>C<sub>6</sub>H<sub>4</sub>Me)}<sub>2</sub>] and [Ru(H<sub>2</sub>O)<sub>3</sub>(η<sup>6</sup>-<i>p</i>-Pr<sup>i</sup>C<sub>6</sub>H<sub>4</sub>Me)]<sup>2+</sup>, respectively. With triphenylphosphine, <b>1</b> reacted to give [Ru<sub>2</sub> (µ-η<sup>4</sup>-C<sub>2</sub>O<sub>4</sub>)(PPh<sub>3</sub>)<sub>2</sub> (η<sup>6</sup>-<i>p</i>-Pr<sup>i</sup>C<sub>6</sub>H<sub>4</sub>Me)<sub>2</sub>]<sup>2+</sup><b>3</b>, while <b>2</b> gave [Ru(η<sup>2</sup>-C<sub>2</sub>O<sub>4</sub>)(PPh<sub>3</sub>)(η<sup>6</sup>-<i>p</i>-Pr<sup>i</sup>C<sub>6</sub>H<sub>4Me)] <b>4</b>. The dichloro complex <b>1</b> can also be converted into the cationic dimethanol complex [Ru<sub>2</sub> (µ-η<sup>4</sup>-C<sub>2</sub>O<sub>4</sub>)(MeOH)<sub>2</sub>(η<sup>6</sup>-<i>p</i>-Pr<sup>i</sup>C<sub>6</sub>H<sub>4</sub>Me)<sub>2</sub>]<sup>2+</sup><b>5</b> by precipitation of the chloride with a silver salt in methanol. Complex <b>5</b> reacted with 4,4-bipyridine to afford a novel tetranuclear metallomacrocycle [Ru<sub>4</sub>(µ-η<sup>4</sup>-C<sub>2</sub>O<sub>4</sub>)<sub>2</sub>(µ-η<sup>1</sup>:η<sup>1</sup>-bipy)<sub>2</sub> (η<sup>6</sup>-<i>p</i>-Pr<sup>i</sup>C<sub>6</sub>H<sub>4</sub>Me)<sub>4</sub>]<sup>4+</sup><b>6</b> with alternating oxalato and 4,4-bipyridine bridges. The reaction between <b>1</b> and azide yielded the known azido-bridged complex [{Ru(µ-η<sup>1</sup>-N<sub>3</sub>)Cl(η<sup>6</sup>-<i>p</i>-Pr<sup>i</sup>C<sub>6</sub>H<sub>4</sub>Me)}<sub>2</sub>] <b>7</b>. The molecular structures of <b>1</b> (two conformational isomers), <b>4</b>, <b>5</b> and <b>6</b> have been solved by X-ray crystallography.
Identifiants
Type de publication
journal article
