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. 2007 Jun 6;129(22):7127-35.
doi: 10.1021/ja071137t. Epub 2007 May 12.

Synthesis and characterization of the Keggin-type ruthenium-nitrido derivative [PW11O39{RuN}]4- and evidence of its electrophilic reactivity

Vanina Lahootun  1 , Claire Besson, Richard Villanneau, Françoise Villain, Lise-Marie Chamoreau, Kamal Boubekeur, Sébastien Blanchard, René Thouvenot, Anna Proust
Affiliations

Synthesis and characterization of the Keggin-type ruthenium-nitrido derivative [PW11O39{RuN}]4- and evidence of its electrophilic reactivity

Vanina Lahootun et al. J Am Chem Soc. .

Abstract

The ruthenium-nitrido POM derivative [PW11O39{RuVIN}]4- has been synthesized by reaction between [PW11O39]7- and [RuVINCl5]2- or [RuVINCl4]-. Its molecular structure has been confirmed from multinuclear 31P and 183W NMR spectroscopy together with an EXAFS study, while the oxidation state of the ruthenium bearing the nitrido ligand has been inferred both from 183W NMR and XANES analysis at the Ru-K edge. The potential of [PW11O39{RuVIN}]4- in N-atom transfer reactions has been demonstrated through reaction with triphenylphosphine, which ultimately leads to the release of the bis(triphenylphosphane)iminium cation [PPh3=N=PPh3]+ through several intermediates, among which the phosphoraniminato derivative [PW11O39{RuVNPh3}]3- has been structurally characterized. Its unusual oxidation state is in accordance with its EPR spectrum.

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