A new method for the synthesis of organopolyoxometalate hybrid compounds

Itsik Bar-Nahum; Jessica Ettedgui; Leonid Konstantinovski; Vladimir Kogan; Ronny Neumann

doi:10.1021/ic700540g

A new method for the synthesis of organopolyoxometalate hybrid compounds

Itsik Bar-Nahum, Jessica Ettedgui, Leonid Konstantinovski, Vladimir Kogan, Ronny Neumann^*

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

28 Scopus citations

Abstract

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]₂W₁₁O ₃₉]^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.

Original language	English
Pages (from-to)	5798-5804
Number of pages	7
Journal	Inorganic Chemistry
Volume	46
Issue number	14
DOIs	https://doi.org/10.1021/ic700540g
State	Published - 9 Jul 2007
Externally published	Yes

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title = "A new method for the synthesis of organopolyoxometalate hybrid compounds",

abstract = "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]2W11O 39]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.",

author = "Itsik Bar-Nahum and Jessica Ettedgui and Leonid Konstantinovski and Vladimir Kogan and Ronny Neumann",

year = "2007",

month = jul,

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doi = "10.1021/ic700540g",

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AU - Bar-Nahum, Itsik

AU - Ettedgui, Jessica

AU - Konstantinovski, Leonid

AU - Kogan, Vladimir

AU - Neumann, Ronny

PY - 2007/7/9

Y1 - 2007/7/9

N2 - 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]2W11O 39]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.

AB - 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]2W11O 39]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.

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JO - Inorganic Chemistry

JF - Inorganic Chemistry

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A new method for the synthesis of organopolyoxometalate hybrid compounds

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