CP/MAS NMR studies on binding environment of CH3CN in Cu(I) complexes with disilane-bridged bis(methylpyridine) ligands

Kei-ichi Sato; Mineyuki Hattori; Yoshinori Yamanoi

doi:10.1039/D5RA02962G

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CP/MAS NMR studies on binding environment of CH₃CN in Cu(i) complexes with disilane-bridged bis(methylpyridine) ligands†

Kei-ichi Sato,^a Mineyuki Hattori

*^a and Yoshinori Yamanoi

*^b

Author affiliations

* Corresponding authors

^a National Institute of Advanced Industrial Science and Technology, AIST Central 5, 1-1-1 Higashi, Tsukuba, Ibaraki 305-8565, Japan
E-mail: mineyuki.hattori@aist.go.jp

^b Department of Chemistry, School of Science, The University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-0033, Japan
E-mail: yamanoi@chem.s.u-tokyo.ac.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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Article information

DOI: https://doi.org/10.1039/D5RA02962G
Article type: Paper
Submitted: 28 Apr 2025
Accepted: 10 May 2025
First published: 20 May 2025
This article is Open Access

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RSC Adv., 2025,15, 16968-16972

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CP/MAS NMR studies on binding environment of CH₃CN in Cu(I) complexes with disilane-bridged bis(methylpyridine) ligands

K. Sato, M. Hattori and Y. Yamanoi, RSC Adv., 2025, 15, 16968 DOI: 10.1039/D5RA02962G

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