Light‐driven biocatalytic processes are notoriously hampered by poor penetration of light into the turbid reaction media. In this study, wirelessly powered light‐emitting diodes are found to represent an efficient and scalable approach for process intensification of the photobiosynthetic production of diesel alkanes from renewable fatty acids.

Carbon−carbon bond formation by dual Iridium‐Nickel photoredox catalysis has gained a lot of attention for late‐stage cross‐couplings of alkyls with aryls. However, the scalability of such reactions is greatly impeded by the poor light penetration depth into the strongly absorbing reaction media. Wireless internal illumination is a novel technique which circumvents the light penetration issue efficiently and therefore allows to scale photon‐driven reactions by conventional methods. Here we demonstrate that industrially relevant photoredox C−C couplings can be scaled seamlessly to different volumes, achieving qualitatively and quantitatively the same results at all scales. The use of conventional reactor types allows stirred, bubble column or fixed‐bed operation mode and is fully compatible with heterogeneous reaction mixtures. By minimizing reflection losses, we could also show a significant advantage in the reaction rate over an externally illuminated setup at the same light intensity.

This experimental study reveals the presence of mainly two-fold positively charged aluminium complexes in NMA : Al(TfO)3 : urea mixtures caused by bidentate hydrogen bonding between Al triflate and urea at a specific 1 : 4 ratio.

The Front Cover shows free‐moving wirelessly‐powered light emitters, which can be used to internally illuminate photochemical reactions. This enables easier scalability of reactions like the illustrated photoredox C–C coupling via Ir/Ni dual catalysis. More information can be found in the Communication by B. O. Burek, K. Lovis, J. Z. Bloh et al.