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Updated: May 23, 2025

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
Published on: September 17, 2017
CP/MAS NMR studies on binding environment of CH3CN in Cu(i) complexes with disilane-bridged bis(methylpyridine)
Kei-Ichi Sato1, Mineyuki Hattori1, Yoshinori Yamanoi2
1National Institute of Advanced Industrial Science and Technology AIST Central 5, 1-1-1 Higashi Tsukuba Ibaraki 305-8565 Japan mineyuki.hattori@aist.go.jp.
Abstract:
CP/MAS NMR spectroscopies have developed as an important tool for studying the structure in the crystalline state. In this work, the structures of representative Cu(i) complexes 1-3 with disilane-bridged bis(methylpyridine) ligands in the crystalline state were investigated by CP/MAS NMR. 13C CP/MAS NMR confirmed the presence of CH3CN in the crystals of 2 and 3, but the environment around CH3CN could not be determined. Natural abundance (ca. 0.36%) 15N CP/MAS NMR measurements could confirm the difference of CH3CN environment between coordinating solvent in 2 and crystal solvent in 3. The 15N CP/MAS of CH3CN in 3 shows a singlet because it is not coordinated to Cu(i) and the crystal structure is stabilized by multiple intermolecular interactions. These data have provided valuable information on Cu(i) coordination environment, which was in good accordance with single-crystal X-ray analysis.
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