Study of the reactivity of tris(pyrazolyl)amine and bis(pyrazolyl)amine ligands toward Rh(I). Crystal structure of [Rh<inf>3</inf>Cl<inf>3</inf>(cod)<inf>3</inf> tdma]·CH<inf>3</inf>CN (tdma=tris[(3,5-dimethyl-1-pyrazolyl) methyl]amine), a C<inf>3</inf>-symmetric compound

Gemma Zamora, Josefina Pons, Xavier Solans, Mercè Font-Bardia, Josep Ros

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13 Citations (Scopus)

Abstract

Rh(I) compounds [Rh2Cl2(cod)2L] (L=tris[(1-pyrazolyl)methyl]amine (tpma) (1), tris[2-(1-pyrazolyl)ethyl]amine (tpea) (2), tris[2-(3,5-dimethyl-1-pyrazolyl)ethyl]amine (tdea) (3), bis[2-(1-pyrazolyl)ethyl]amine (bpea) (4) and bis[2-(3,5-dimethyl-1-pyrazolyl)ethyl]amine (bdea) (5)), and [Rh3Cl3(cod)3tdma] (tdma=tris[3,5-dimethyl-1-pyrazolyl)methyl]amine (6), have been prepared, and characterised by elemental analyses, conductivity, IR, 1H and 13C NMR spectroscopy and liquid mass spectrometry (with electrospray and APCI interfaces). The 1H NMR spectra and molar conductance of [Rh2Cl2(cod)2L] complexes suggested the presence of 1:1 electrolyte species [Rh(cod)L]+ [RhCl2(cod)]- in solution. A combined electrospray and APCI liquid mass spectrometry study confirmed the presence of both [Rh(cod)L]+ and [RhCl2(cod)] - ions in solution, but the neutral molecular form of complexes in solution was not found. The crystal structure of complex [Rh3Cl3(cod)3tdma] was resolved by X-ray diffraction. The molecular structure is unusual and consists of a ligand tdma coordinated to three "RhCl(cod)" units with a C3-symmetry. © 2004 Elsevier B.V. All rights reserved.
Original languageEnglish
Pages (from-to)980-986
JournalJournal of Organometallic Chemistry
Volume689
Issue number5
DOIs
Publication statusPublished - 1 Mar 2004

Keywords

  • C -symmetry 3
  • Crystal structure
  • Pyrazole complexes
  • Rhodium complexes
  • Trinuclear complex

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