We next wanted to confirm that none of these observed phosphorous peaks correspond to the intermediate phosphoryl chloride that is formed before hydrolysis to the desired phosphoric acid. To do so, the phosphoryl chloride was selectively synthesized and a 31 P-NMR was recorded (See Supporting Information). The measured shift significantly differs from the acid (by around 2 ppm in CDCl3), but also showed multiple peaks. Therefore, it can be concluded that the chloride is not the source for the three signals. Since HRMS and 1 H-NMR indicate that the desired phosphoric acid photo catalyst PCII was synthesized, we believe that PCII was obtained, and that splitting was caused by conformational effects. PCII was therefore used in the following proof of principle reactions.