Recent progress on solid-state cross-polarization (CP)/magic angle spinning (MAS) NMR measurements: a tool for investigating structural changes in stimuli-responsive organic compounds

Abstract

Abstract Over the years, cross-polarization/magic angle sample spinning (CP/MAS) NMR has proven to be valuable for obtaining detailed structural information in solid-state materials. A notable advantage of this technique is that it does not require a well-organized arrangement in the sample such as single crystals. Consequently, even materials with low crystallinity such as amorphous substances can be analyzed to obtain structural information. In recent years, research on externally stimuli-responsive molecules utilizing crystal phase transitions has attracted attention. Certain aryl disilane and oligosilane compounds exhibit external stimulus responsiveness even in the crystalline state due to the hindered rotation of the Si–Si σ bond and sparse crystal packing. Understanding the structural alternations linked to changes in physical properties is crucial for investigation of the responsiveness. High-resolution CP/MAS NMR spectra are particularly suitable for analyzing crystalline polymorphs, crystal phase transitions, and solid-state conformations. In this report, we present the results of natural abundance 13C, 29Si, and 15N CP/MAS NMR experiments conducted on externally stimuli-responsive disilane-bridged molecules. These measurements provide information on the structure before and after crystal phase transitions, as well as the amorphous state. A comprehensive analysis of our findings is essential for elucidating alternations in the structure and arrangement of crystalline materials under external stimuli.