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Synthesis of new ruthenium(II) complexes derived from labile nitrile ligands: an alternative route to the preparation of trans-dichlorotetrakis(diphenylphosphine)ruthenium(II)
Authors:Samson O Owalude  Adedibu C Tella  Ezekiel O Odebunmi  Uche B Eke  James E Golen  Arnold L Rheingold
Institution:1. Department of Chemistry, University of Ilorin, Ilorin, Nigeriaowalude@unilorin.edu.ng owalude12@yahoo.com;3. Department of Chemistry, University of Ilorin, Ilorin, Nigeria;4. Department of Chemistry and Biochemistry, University of California, San Diego, CA, USA
Abstract:New ruthenium(II) complexes containing labile nitrile ligands have been prepared by treatment of either the polymer {RuCl2(COD)}x] (COD = cycloocta-1,5-diene) (1) or its derivative RuCl2(COD)(NCCH3)2]·NCCH3 (2) with the appropriate nitrile ligands in refluxing acetonitrile under argon. A new route to synthesis of trans-dichlorotetrakis(diphenylphosphine)ruthenium(II) (7) was also reported. A redetermination of the structure of 7 was undertaken and X-ray crystallographic data revealed that the complex crystallizes in the triclinic space group P-1 with unit cell dimensions a = 12.7016(9) Å, b = 13.0847(10) Å, c = 14.1498(10) Å, α = 101.46(3)°, V = 2080.6(3) Å3, Z = 2 and R = 0.0309. Its polymorph 7′ was also obtained. The crystal structure of 4 was also determined. This complex crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 27.0510(3) Å, b = 11.0984(13) Å, c = 13.0450(16) Å, α = 90°, V = 3886.5(8) Å3, Z = 8 and R = 0.0282.
Keywords:Nitrile ligands  ruthenium(II) complex  diphenylphosphine  spectroscopic analysis  X-ray crystallography
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