Data for Exploring the potential of multinuclear solid‐state 1H, 13C, and 35Cl magnetic resonance to characterize static and dynamic disorder in pharmaceutical hydrochlorides

Disorder can result in a loss of manufacturing control leading to batch to batch variability and can lengthen the process of structural characterization. The range of NMR active nuclei makes solid-state NMR a unique technique for gaining nucleus-specific information about crystallographic disorder.

Here, we explore the use of high-field 35Cl solid-state NMR at 23.5 T to characterize both static and dynamic crystallographic disorder: Specifically, dynamic disorder occurring in duloxetine hydrochloride (1), static disorder in promethazine hydrochloride (2), and trifluoperazine dihydrochloride (3). In all structures, the presence of crystallographic disorder was confirmed by 13C cross-polarization magic-angle spinning (CPMAS) NMR and supported by GIPAW-DFT calculations, and in the case of 3, 1H MAS NMR provided additional confirmation.