Solvent-free aerobic oxidation of benzyl alcohol using molecular O2 was conducted in a batch-type reactor, as described in our previous work (42). The amount of catalyst used for the reaction test was normalized to have the same Pd content of 1.6 μmol. Typically, 5 ml of benzyl alcohol (48 mmol) and the normalized Pd catalyst were co-added into a 25-ml three-necked glass flask equipped with a reflux condenser. Before reaction, the system was first charged with O2 by bubbling ultrahigh purity O2 (99.999%; Nanjing Special Gases) at a flow rate of 15 ml/min for 20 min to remove air. Under the continuous flow of O2, the reactor was quickly immersed into a silicon oil bath at the desired temperature (90, 120, or 140°C) to initiate the reaction. During each reaction, the mixture was vigorously stirred at a rate of 1500 rpm to exclude any mass transfer limitation. The effect of oxygen flow rates on the possible selectivity change was also ruled out. Last, the reaction products were analyzed using a Shimadzu GC-2014 gas chromatograph, equipped with an Rtx-1 capillary column and an autoinjector. The TOFs were calculated using Eq. 3Embedded Image(3)

Here, the moles of active sites were normalized to the number of exposed surface Pd sites calculated by the cubooctahedral “magic cluster” model. On alumina-coated samples, the number of exposed surface Pd sites was determined by the Pd dispersion data (table S3). The TOFs were calculated from the rate of the intitial 60-min reaction, unless otherwise noted. The specific rates were also calculated on the basis of Eq. 4Embedded Image(4)

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