In situ solid-state NMR of a magnetically oriented microcrystal suspension

In situ solid-state NMR measurements of a magnetically oriented microcrystal suspension (MOMS) were demonstrated. Under modulated rotation of the static field, or equivalently, of the sample tube, randomly oriented microcrystals in a viscous liquid medium feel a torque arising from the anisotropic bulk susceptibility and eventually aligned in the same direction. In this way, a three-dimensional MOMS (3D-MOMS) was obtained. To apply an elliptically rotating magnetic field to microcrystals in suspension, a probe to rotate the sample tube around an axis perpendicular to the static magnetic field was developed. Single-crystal (SC) rotation patterns were obtained from the 3D-MOMS by solid-state CP measurements triggered in synchronous with the sample-tube rotation. Unlike the traditional SC method, the 3D-MOMS approach presented here does not require the elaborate adjustment of the direction of the reference frame. The process of three-dimensional magnetic alignment was also studied by monitoring the spectral changes during continuous application of the modulated sample rotation. (C) 2019 Elsevier Inc. All rights reserved.