10.1021/ic700540g.s002
Itsik Bar-Nahum
Itsik
Bar-Nahum
Jessica Ettedgui
Jessica
Ettedgui
Leonid Konstantinovski
Leonid
Konstantinovski
Vladimir Kogan
Vladimir
Kogan
Ronny Neumann
Ronny
Neumann
A New Method for the Synthesis of Organopolyoxometalate Hybrid
Compounds
American Chemical Society
2007
polyoxometalate cluster
New Method
compound
acid
PSn
quaternary ammonium salt
119 Sn
amine moiety
Organopolyoxometalate Hybrid Compounds
amines
1 H
2 W 11 O 39
15 N
31 P
nucleophile
183 W NMR
2007-07-09 00:00:00
Dataset
https://acs.figshare.com/articles/dataset/A_New_Method_for_the_Synthesis_of_Organopolyoxometalate_Hybrid_Compounds/2997796
The reaction of a quaternary ammonium salt of the tin chloride-substituted polyoxometalate, [PSn(Cl)W<sub>11</sub>O<sub>39</sub>]<sup>4-</sup>,
with a variety of <i>n</i>-nucleophiles including primary, secondary, and tertiary amines and a tertiary phosphine, yielded
tin-centered Lewis acid−base adducts, [PSn(Cl)W<sub>11</sub>O<sub>39</sub>]<sup>4-</sup>−<i>n</i>-nucleophile; with more nucleophilic secondary amines
such as diisopropylamine, apparently some [PSnN[CH(CH<sub>3</sub>)<sub>2</sub>]<sub>2</sub>W<sub>11</sub>O<sub>39</sub>]<sup>4-</sup> was formed as a minor product. The
compounds were identified by <sup>1</sup>H, <sup>119</sup>Sn, <sup>15</sup>N, <sup>31</sup>P, and <sup>183</sup>W NMR, ESI-MS, and elemental analyses. The key
connectivity of the Sn−Cl center with the amine was clarified by the observation of <sup>3</sup><i>J</i> Sn−H couplings (Sn from the
polyoxometalate cluster and H from the amine moiety) in a 2D <sup>119</sup>Sn−<sup>1</sup>H heteronuclear multiple-bond correlation
NMR experiment. This new, rather simple synthetic method was also utilized for preparing amino acid−polyoxometalate
hybrid compounds.