¹⁹F/²⁹Si distance determination and heteronuclear spin counting under fast magic-angle spinning in fluoride-containing octadecasil

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• 作者：Bertani ; Philippe ; Raya ; J&eacute ; sus ; Hirschinger ; J&eacute ; rô ; me
• 关键词：Solid-state NMR ; Magic-angle spinning ; Dipolar recoupling ; Cross-polarization ; Rotational-echo double-resonance ; Spin-counting ; RMN du solide ; Rotation à ; l'angle magique ; Recouplage dipolaire ; Polarisation crois&eacute ; e ; REDOR ; Comptage de spin
• 刊名：Comptes Rendus Chimie
• 出版年：2004
• 期刊代码：119_16310748
• 类别：ch
• 出版时间：March - April, 2004
• 卷：7
• 期：3-4
• 页码：363-369
• 文件大小：334 K

摘要

¹⁹F/²⁹Si rotational-echo double-resonance (REDOR), θ-REDOR and Hartmann–Hahn cross-polarization (CP) NMR techniques have been applied under fast magic-angle spinning (MAS) to a powder sample of fluoride-containing octadecasil. The internuclear distance of the ¹⁹F–²⁹Si spin pairs formed by the silicons in the D4R units (T-1 site) and the fluoride anions deduced directly from the CP and REDOR measurements is in very good agreement with the X-ray crystal structure. Moreover, heteronuclear spin-counting θ-REDOR experiments unambiguously show that the ¹⁹F and the T-1 ²⁹Si nuclei form fairly isolated spin pairs, whereas multiple-spin behaviour is clearly evidenced at the T-2 site. To cite this article: P. Bertani et al., C. R. Chimie 7 (2004).