Abstract
Cyclic voltammetry (CV), rotating disk electrode voltammetry (RDE) and bulk electrolysis were used to investigate the electrochemical oxidation of the title cluster in acetonitrile (CH3CN). Two irreversible 2-electron oxidation processes occur at +0.95 V and +1.15 V vs. SCE. Bulk electrolysis demonstrates that the d9–d9 Pd2(dppm)2(NCCH3)22+4 complex is generated among the first intermediates, and the d8 Pd(dppm)(NCCH3)22+3 is formed as the final product. The intermediacy of “Pd3(dppm)3(CO)4+” and “Pd3(dppm)34+” is suspected but not confirmed. This oxidation process exhibits a close resemblance to the photo oxidative reactivity of the title cluster in the presence of chlorocarbons (R–Cl) for which the sole observed product is Pd(dppm)Cl2.
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