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Metallaphotoredox catalyzed cross‐coupling of an arylbromide (Ar−Br) with an alkyl bis(catecholato)silicate (R−Si⊖) has been analyzed in depth using a continuum of analytical techniques (EPR, fluorine NMR, electrochemistry, photophysics) and modeling (micro‐kinetics and DFT calculations). These studies converged on the impact of four control parameters consisting in the initial concentrations of the...
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