The first reaction, enzymatic hydrolysis of sucrose, was performed in a standard 5 mm NMR tube directly in a spectrometer magnet. It proceeded with an immediate follow-up reaction of α-glucose conversion to β-glucose, as shown in Fig. . The sucrose hydrolysis has been performed as described previously. Namely, we mixed stock solutions of 2.0 M sucrose in D 2 O and of the enzyme in a 1:1 volumetric ratio. We obtained the enzyme's stock solution by dissolving β-D-fructofuranosidase (Sigma-Aldrich) in an acetate buffer (Sigma-Aldrich) (95 mM, H 2 O, pH =5.2) to reach the concentration of 4.6 µg/ml. Hydrosilylation reactions (Fig. and Fig. ) proceeded inside a 5 mm NMR tube with a septum. In both cases, the 1:1 silane/olefin mixtures in undeuterated 1,2-difluorobenzene were measured first without the catalyst. Then, the catalyst solution in 1,2-difluorobenzene was added. The spectra were collected at 5 °C.