Self-assembly of arene ruthenium acylpyrazolone fragments to tetranuclear metallacycles. Molecular structures and solid-state 15N CPMAS NMR correlations. Issue 9 (3rd February 2016)

• Record Type: Journal Article
• Authors: Pettinari, Riccardo; Marchetti, Fabio; Pettinari, Claudio; Condello, Francesca; Skelton, Brian W.; White, Allan H.; Chierotti, Michele R.; Gobetto, Roberto
• Is Part Of: Dalton transactions. Volume 45:Issue 9(2016)
• Page Start: 3974
• Page End: 3982
• Publication Date: 2016-02-03
• Subjects: Chemistry, Inorganic -- Periodicals; Chemistry, Physical and theoretical -- Periodicals; Chemistry, Inorganic -- Periodicals; 546.05
• DOI: 10.1039/c6dt00168h
• Languages: English
• ISSNs: 1477-9226

Abstract

Abstract : Mono- and tetranuclear Ru(ii ) half-sandwich complexes containing acylpyrazolone ligands. 13 C and 15 N solid state NMR spectroscopy. Abstract : Reactions of [(η 6 -cymene)Ru(μ-Cl)Cl]2 with acylpyrazolone ligands HQ′ (HQ′ in general; in detail, HQ CH2 Cl = 2-chloro-1-(5-hydroxy-3-methyl-1-phenyl-1 H -pyrazol-4-yl)ethanone), HQ hex = 1-(5-hydroxy-3-methyl-1-phenyl-1 H -pyrazol-4-yl)heptan-1-one), HQ nPe = 1-(5-hydroxy-3-methyl-1-phenyl-1 H -pyrazol-4-yl)-3, 3-dimethylbutan-1-one)), in the presence of base, gave the corresponding [(η 6 -cymene)Ru(Q′)Cl] mononuclear complexes. They react with AgX (where X = O3 SCF3 or BF4 ) in dry acetone affording cationic metalla-cycles [(η 6 -cymene)Ru(Q′)]4 (X)4 . The complexes were fully characterized by analytical and spectroscopic methods and the solid-state structures of mononuclear and tetranuclear complexes have been determined by single-crystal X-ray diffraction. The hapticity of the acylpyrazolone ligands to the Ru metal centre has also been established by 13 C and 15 N CPMAS NMR spectroscopy for the complexes where the lack of crystallinity prevented the elucidation of the crystal structure by SCXRD data.