title: Self-assembly of arene ruthenium acylpyrazolone fragments to tetranuclear metallacycles. Molecular structures and solid-state (15)N CPMAS NMR correlations.
abstract: Reactions of [(η(6)-cymene)Ru(μ-Cl)Cl]2 with acylpyrazolone ligands HQ' (HQ' in general; in detail, HQ(CH2Cl) = 2-chloro-1-(5-hydroxy-3-methyl-1-phenyl-1H-pyrazol-4-yl)ethanone), HQ(hex) = 1-(5-hydroxy-3-methyl-1-phenyl-1H-pyrazol-4-yl)heptan-1-one), HQ(nPe) = 1-(5-hydroxy-3-methyl-1-phenyl-1H-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 = O3SCF3 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.
authors.affiliation: School of Pharmacy, University of Camerino, via S. Agostino 1, 62032 Camerino, MC, Italy. riccardo.pettinari@unicam.it.
authors.forename: Riccardo
authors.initials: R
authors.lastname: Pettinari
authors.affiliation: School of Science and Technology, University of Camerino, via S. Agostino 1, 62032 Camerino, MC, Italy.
authors.forename: Fabio
authors.initials: F
authors.lastname: Marchetti
authors.affiliation: School of Pharmacy, University of Camerino, via S. Agostino 1, 62032 Camerino, MC, Italy. riccardo.pettinari@unicam.it.
authors.forename: Claudio
authors.initials: C
authors.lastname: Pettinari
authors.affiliation: School of Pharmacy, University of Camerino, via S. Agostino 1, 62032 Camerino, MC, Italy. riccardo.pettinari@unicam.it.
authors.forename: Francesca
authors.initials: F
authors.lastname: Condello
authors.affiliation: School of Chemistry and Biochemistry M310, The University of Western Australia, Crawley, WA 6009, Australia.
authors.forename: Brian W
authors.initials: BW
authors.lastname: Skelton
authors.affiliation: Centre for Microscopy, Characterization and Analysis M010, The University of Western Australia, Crawley, WA 6009, Australia.
authors.forename: Allan H
authors.initials: AH
authors.lastname: White
authors.affiliation: Dipartimento di Chimica and NIS Centre, University of Torino, Via P. Giuria 7, 10125 Torino, Italy.
authors.forename: Michele R
authors.initials: MR
authors.lastname: Chierotti
authors.affiliation: Dipartimento di Chimica and NIS Centre, University of Torino, Via P. Giuria 7, 10125 Torino, Italy.
authors.forename: Roberto
authors.initials: R
authors.lastname: Gobetto