Data for Combining X-ray and NMR crystallography to explore the crystallographic disorder in salbutamol oxalate

Here, we establish the crystal structure of its oxalate form, salbutamol oxalate, and explore the nature of its crystallographic disorder by combined X-ray crystallography and 13C cross-polarization magic-angle spinning solid-state NMR. The *C−OH chiral center of salbutamol (note that the crystal structures are a racemic mixture of the two enantiomers of salbutamol) is disordered over two positions, and the tert-butyl group is rotating rapidly, as revealed by 13C solid-state NMR.

The impact of crystallization conditions on the disorder was investigated, finding variations in the occupancy ratio of the *C−OH chiral center between single crystals and a consistency across samples in the bulk powder. Overall, this work highlights the contrast among investigating crystallographic disorder by X-ray diffraction, solid-state NMR crystallography, and gauge-including projector-augmented-wave density functional theory calculations, with their combined use, yielding an improved understanding of the nature of the crystallographic disorder between the local (i.e., as viewed by NMR) and longer-range periodic (i.e., as viewed by diffraction) scale.<br><br>Raw data file from the solid-state NMR experiments