Solution-state nuclear magnetic resonance spectroscopy of crystalline cellulosic materials using a direct dissolution ionic liquid electrolyte

Extended Data Fig. 1 Multiplicity-edited HSQC of acetylated MCC.

Multiplicity-edited HSQC of acetylated MCC showing significant peak superposition ([P 4444 ][OAc]:DMSO- d 6 1:4 wt%, 65 °C, 5 wt%; 600 MHz 1 H frequency. For multiplicity edited HSQC green = CH, blue = CH 2 ).

Extended Data Fig. 2 Effect of diffusing-editing on the 1 H 1D data for surface acetylated MCC.

Comparison of the quantitative 1 H spectrum ( a ) with the diffusion edited 1 H spectrum ( b ) allows to quickly assess the introduction of functionalities of species exhibiting resonances in the heavily crowded IL spectral region ([P 4444 ][OAc]:DMSO- d 6 1:4 wt%, 65 °C, 5 wt%; 600 MHz 1 H frequency).

Extended Data Fig. 3 Utility of the 2D HSQC-TOCSY experiment for further peak assignment of cellulose derivatives.

( a ) HSQC-TOCSY in the full view allows to further assign the AGA moiety over interactions of the C1 signal with peaks in the crowded areas., ( b ) HSQC-TOCSY with zoom into the C2–C5 region shows that full characterisation of the spin system can be possible. However, owing to strong superpositions with the AGU, NRE and RE moieties the peak assignments can become tedious. Spectra shown with diffusion-edited 1 H trace (top trace) and 13 C trace (left trace). AGU = anhydroglucose unit; AGA = anhydroglucopyranosiduronic acid unit; NRE = non-reducing end; RE = reducing end. In the spectra HSQC correlations are shown in green (CH) and blue (CH 2 ) and TOCSY correlations are shown in gray.

Extended Data Fig. 4 Diffusion-edited 1 H spectra of food insects.

Diffusion-edited 1 H spectra ([P 4444 ][OAc]:DMSO- d 6 1:4 wt%, 65 °C, 5 wt%, 600 MHz) for fruit flies, damselfly tail and whole food crickets, after Wiley milling and dissolution.

Supplementary Information

Supplementary Figs. 1–12 and Note.