Journal of the American Chemical Society, volume 119, issue 36, pages 8459-8473
Photochemistry of M(PP3)H2 (M = Ru, Os; PP3 = P(CH2CH2PPh2)3): Preparative, NMR, and Time-Resolved Studies
Robert Osman
1
,
David I. PATTISON
1
,
Robin N. Perutz
1
,
Claudio Bianchini
1
,
Juan A Casares
1
,
Maurizio Peruzzini
1
1
Contribution from the Department of Chemistry, University of York, Heslington, York, YO1 5DD, U.K., and the Istituto per lo Studio della Stereochimica ed Energetica dei Composti di Coordinazione, ISSECC-CNR, Via J. Nardi 39, 50132 Firenze, Italy
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Publication type: Journal Article
Publication date: 1997-09-01
scimago Q1
SJR: 5.489
CiteScore: 24.4
Impact factor: 14.4
ISSN: 00027863, 15205126
General Chemistry
Catalysis
Biochemistry
Colloid and Surface Chemistry
Abstract
Photochemical reaction of Ru(PP3)H2 (PP3 = P(CH2CH2PPh2)3) in THF under a rigorously inert atmosphere yields the cyclometalated complex Ru[(Ph2PCH2CH2)2P(CH2CH2PPhC6H4)]H. The latter is converted back to Ru(PP3)H2 under H2 and reacts even with traces of N2 to yield Ru(PP3)(N2). The dinitrogen complex may be synthesized directly by a number of methods. NMR spectroscopy shows that photolysis of Ru(PP3)H2 under C2H4 and CO yields Ru(PP3)(C2H4) and Ru(PP3)(CO), respectively. Photolysis of Ru(PP3)H2 with HSiEt3 in THF yields Ru(PP3)(SiEt3)H, while photolysis in mixtures of THF and benzene at low temperature yields Ru(PP3)(Ph)H. The latter is also generated by reduction of Ru(PP3)Cl2 in the presence of benzene. Os(PP3)(Ph)H is formed either by photolysis of Os(PP3)H2 or by reduction of Os(PP3)Cl2 in the presence of benzene. Irradiation of Os(PP3)H2 in THF or THF/hexane mixtures initially yields the THF C−H activation product, Os(PP3)(2-C4H7O)H. This complex is also generated by reduction of Os(PP3)Cl2 with sodi...
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