A new method for the synthesis of organopolyoxometalate hybrid compounds.
The reaction of a quaternary ammonium salt of the tin chloride-substituted polyoxometalate, [PSn(Cl)W11O39]4-, with a variety of n-nucleophiles including primary, secondary, and tertiary amines and a tertiary phosphine, yielded tin-centered Lewis acid-base adducts, [PSn(Cl)W11O39]4--n-nucleophile; with more nucleophilic secondary amines such as diisopropylamine, apparently some [PSnN[CH(CH3)2]2W11O39]4- was formed as a minor product. The compounds were identified by 1H, 119Sn, 15N, 31P, and 183W NMR, ESI-MS, and elemental analyses. The key connectivity of the Sn-Cl center with the amine was clarified by the observation of 3J Sn-H couplings (Sn from the polyoxometalate cluster and H from the amine moiety) in a 2D 119Sn-1H heteronuclear multiple-bond correlation NMR experiment. This new, rather simple synthetic method was also utilized for preparing amino acid-polyoxometalate hybrid compounds.
Bar-Nahum
Itsik
I
Department of Organic Chemistry and Chemical Research Support Unit, Weizmann Institute of Science, Rehovot 76100, Israel.
Ettedgui
Jessica
J
Konstantinovski
Leonid
L
Kogan
Vladimir
V
Neumann
Ronny
R
D009682:Magnetic Resonance Spectroscopy; D008958:Models, Molecular; D009930:Organic Chemicals / Q000138:chemical synthesis / Q000737:chemistry*; D021241:Spectrometry, Mass, Electrospray Ionization; D017973:Tungsten Compounds / Q000138:chemical synthesis / Q000737:chemistry*; D000099294:Polyoxometalates
D009930:Organic Chemicals; D017973:Tungsten Compounds; C102296:polyoxometalate I; D000099294:Polyoxometalates