The modified electrocatalysts ( 3 and 4) show efficient hydrogen evolution reaction activities almost comparable to those of high-grade Pt/C at 0.1 M KOH. Compounds 1 and 2 represent an important class of structurally isolated organometallic POM-based clusters that were successfully nanostructured onto Ni foam and electrochemically reduced after 48 h of electrolysis to M/MoO 2, where M = Rh ( 3) and Ir ( 4), nanocomposite hybrid materials on a Ni foam surface in a 0.1 M KOH solution. Compounds 1 and 2 were well characterized in the solid state by single-crystal X-ray diffraction, IR, and thermogravimetric analysis and in solution by UV–vis, electrospray ionization mass spectrometry, and electrochemistry. Herein, two new clusters, H 3♱4H 2O ( 1) and H 5♱3H 2O ( 2) (Cp* = pentamethylcyclopentadienyl), based on a heterooctamolybdate anionic core were successfully obtained via a one-pot reaction using 2 and Na 2MoO 4 in acidic conditions. Thus, it is imperative to design and structurally explore new catalysts including noble metals. Among them, noble-metal-decorated POMs have a profound impact as catalytic materials. Polyoxometalates (POMs), emerging as a new class of porous molecular materials, play a promising role in homo- and heterogeneous catalysis.
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