Bis(pyrene)metal complexes of vanadium, niobium and titanium: Isolable homoleptic pyrene complexes of transition metals

Benjamin E. Kucera, Robert E. Jilek, William W. Brennessel, John E. Ellis

Research output: Contribution to journalArticlepeer-review

15 Scopus citations

Abstract

Reduction of VCl3(THF)3 (THF is tetra-hydro-furan) and NbCl4(THF)2 by alkali metal pyrene radical anion salts in THF affords the paramagnetic sandwich complexes bis-[(1,2,3,3a,10a,10b-η)-pyrene]vanadium(0), [V(C16H10)2], and bis-[(1,2,3,3a,10a,10b-η)-pyrene]niobium(0), [Nb(C16H10)2]. Treat-ment of tris-(naphthalene)-titanate(2-) with pyrene provides the isoelectronic titanium species, isolated as an (18-crown-6)potassium salt, namely catena-poly[[(18- crown-6)potassium]-μ-[(1,2-η:1,2,3,3a,10a,10b-η)-pyrene]-titanate(-I) -μ-[(1,2,3,3a,10a,10b-η:6,7-η)-pyrene]], {[K(C12H24O6)][Ti(C16H10)2]} n. The first two compounds have very similar packing, with neighboring mol-ecules arranged orthogonally to one another, such that aromatic donor-acceptor inter-actions are likely responsible for the specific arrangement. The asymmetric unit contains a half-occupancy metal center η6-coordinated to one pyrene ligand, with the full M(pyrene)2 mol-ecule generated by a crystallographic inversion center. In the titanium compound, the cations and anions are in alternating contact throughout the crystal structure, in one-dimensional chains along the [101] direction. As in the other two compounds, the asymmetric unit contains a half-occupancy Ti atom η6-coordinated to one pyrene ligand. Additionally, the asymmetric unit contains one half of an (18-crown-6)potassium cation, located on a crystallographic inversion center coincident with the K atom. The full formula units are generated by those inversion centers. In all three structures, the pyrene ligands are eclipsed and sandwich the metals in one of two inversion-related sites. These species are of inter-est as the first isolable homoleptic pyrene transition metal complexes to be described in the scientific literature.

Original languageEnglish (US)
Pages (from-to)749-753
Number of pages5
JournalActa Crystallographica Section C: Structural Chemistry
Volume70
Issue number8
DOIs
StatePublished - Aug 2014

Keywords

  • crystal structure
  • homoleptic complexes
  • niobium
  • paramagnetic compounds
  • polycyclic aromatic hydro-carbons
  • pyrene
  • sandwich compounds
  • titanium
  • vanadium

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