Reaction of [Cp*2W2O5] with mercaptocarboxylic acids: Addition rather than reduction. Isolation and characterization of Cp*WO2(SCH2CH2COOH)
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2011
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Abstract
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.
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Hydraulic structures , Molybdenum , Nuclear magnetic resonance spectroscopy , Oxidation , Single crystals , Sodium , Tungsten , Water absorption , X ray diffraction , X ray diffraction analysis , Alkylsulfido ligands , Asymmetric structures , Elemental analysis , H NMR spectra , Isolation and characterization , Metal reduction , Oxidation state , Oxido ligands , Pentamethylcyclopentadienyl , Room temperature , Single crystal x-ray diffraction , Ligands