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.