Isomeric [RuCl2(dmso)2(indazole)2] complexes: ruthenium(II)-mediated coupling reaction of acetonitrile with 1H-indazole

Dalton Trans. 2005 Jul 21:(14):2355-64. doi: 10.1039/b503650j. Epub 2005 Jun 15.

Abstract

Reaction of the antitumor complex trans-[Ru(III)Cl4(Hind)2]- (Hind = indazole) with an excess of dimethyl sulfoxide (dmso) in acetone afforded the complex trans,trans,trans-[Ru(II)Cl2(dmso)2(Hind)2] (1). Two other isomeric compounds trans,cis,cis-[Ru(II)Cl2(dmso)2(Hind)2] (2) and cis,cis,cis-[Ru(II)Cl2(dmso)2(Hind)2] (3) have been obtained on refluxing cis-[Ru(II)Cl(2)(dmso)(4)] with 2 equiv. of indazole in ethanol and methanol, respectively. Isomers 1 and 2 react with acetonitrile yielding the complexes trans-[Ru(II)Cl2(dmso)(Hind){HN=C(Me)ind}].CH3CN (4.CH3CN) and trans,cis-[Ru(II)Cl2(dmso)2{HN=C(Me)ind}].H2O (5.H2O), respectively, containing a cyclic amidine ligand resulting from insertion of the acetonitrile C triple bond N group in the N1-H bond of the N2-coordinated indazole ligand in the nomenclature used for 1H-indazole. These are the first examples of the metal-assisted iminoacylation of indazole. The products isolated have been characterized by elemental analysis, IR spectroscopy, UV-vis spectroscopy, electrospray mass-spectrometry, thermogravimetry, differential scanning calorimetry, 1H NMR spectroscopy, and solid-state 13C CP MAS NMR spectroscopy. The isomeric structures of 1-3 and the presence of a chelating amidine ligand in 4 and 5 have been confirmed by X-ray crystallography. The electrochemical behavior of 1-5 and the formation of 5 have been studied by cyclic voltammetry.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acetonitriles / chemistry*
  • Antineoplastic Agents / chemical synthesis*
  • Carbon / chemistry
  • Cations, Divalent
  • Crystallography, X-Ray
  • Electrochemistry
  • Indazoles / chemistry*
  • Isomerism
  • Ligands
  • Molecular Conformation
  • Nitrogen / chemistry
  • Organometallic Compounds / chemical synthesis*
  • Ruthenium / chemistry*
  • Spectrum Analysis

Substances

  • Acetonitriles
  • Antineoplastic Agents
  • Cations, Divalent
  • Indazoles
  • Ligands
  • Organometallic Compounds
  • dichlorotetrakis(dimethyl sulfoxide)ruthenium II
  • Carbon
  • Ruthenium
  • Nitrogen
  • acetonitrile