Reaction of [Cp*2W2O5] with mercaptocarboxylic acids: Addition rather than reduction. Isolation and characterization of Cp*WO2(SCH2CH2COOH)

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AKTAŞ P., Daran J., Manoury E., DEMİRHAN F., Poli R.

Journal of Organometallic Chemistry, cilt.696, sa.11-12, ss.2275-2279, 2011 (SCI-Expanded) identifier identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 696 Sayı: 11-12
  • Basım Tarihi: 2011
  • Doi Numarası: 10.1016/j.jorganchem.2010.12.002
  • Dergi Adı: Journal of Organometallic Chemistry
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Sayfa Sayıları: ss.2275-2279
  • Anahtar Kelimeler: Tungsten, Oxido ligands, High-oxidation state organometallics, Alkylsulfido ligands, Pentamethylcyclopentadienyl ligands
  • Manisa Celal Bayar Üniversitesi Adresli: Evet

Özet

The reaction of Cp*2W2O5 with HS(CH2)nCOOH (n = 1, 2) in MeOH or in CH 2Cl2 solutions at room temperature proceeds in slightly different ways depending on the value of n. For n = 2, it selectively yields compound Cp*WO2(SCH2CH2CO 2H), which has been isolated and characterized by elemental analysis, NMR and single crystal X-ray diffraction. The reaction is equilibrated, being shifted to the product by absorption of water by anhydrous Na2SO 4 in CH2Cl2, and to the reactants by addition of water. Contrary to the Mo analogue, no products resulting from metal reduction are obtained. The corresponding reaction for n = 1 occurs similarly at low substrate/W ratios (<0.5), but proceeds further to several uncharacterized products for greater substrate amounts. The primary product could not be isolated, but its 1H NMR spectrum suggests a different, asymmetric structure. © 2010 Elsevier B.V. All rights reserved.