K. Nomiya, C. Nozaki, Atsuyuki Kano
Apr 15, 1997
Citations
0
Influential Citations
14
Citations
Journal
Journal of Organometallic Chemistry
Abstract
Abstract The preparations of A-β-Na7SiW9Nb3O40 and Na5[(η5-C5Me5)Rh · SiW9Nb3O40] are described. The water-soluble form of the Keggin-type trisubstituted heteropolyanion, A-β-SiW9Nb3O407−, of interest as a polyoxoanion support for organometallic complexes, was isolated in pure form in 61% yield as its heptasodium salt with 16 waters of hydration. The polyoxoanion-supported organometallic complex as its all-sodium salt, [(η5-C5Me5)Rh·SiW9Nb3O40]5− was obtained in 21% yield as an analytically pure, homogeneous yellow-brown solid by the reaction of [(η5-C5Me5)Rh(CH3CN)3]2+ with the trisubstituted heteropolyanion SiW9Nb3O407− in CH3CN-DMSO. These all-sodium salts have required their own novel preparations and purifications, and have never been derived directly from the known all-Bu4N+ salts of the corresponding Keggin heteropolyanions. Compositional characterization was accomplished by complete elemental analyses, TG/DTA, and FT-IR. Structural characterization in solution was achieved by combination of 1H, 13C and 183W NMR spectroscopies.