Quantitative Analysis of the Proximities of OH Ligands and Vanadium Sites in a Polyoxovanadate Cluster Using Frequency-Selective 1H鈥?sup>51V Solid-State NMR Spectroscopy

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• 作者：Fr茅d茅rique Pourpoint ; Julien Tr茅bosc ; Christian Bonhomme ; Olivier Durupthy ; Nathalie Steunou ; Olivier Lafon ; Jean-Paul Amoureux
• 刊名：Journal of Physical Chemistry C
• 出版年：2014
• 出版时间：August 14, 2014
• 年：2014
• 卷：118
• 期：32
• 页码：18580-18588
• 全文大小：361K
• ISSN：1932-7455

文摘

We introduce a magic-angle spinning NMR experiment to estimate specific distances in a solid material between a given site occupied by a quadrupolar nucleus and the nearby spin-1/2 nuclei. The new sequence, called DANTE-S-REDOR, consists of a frequency-selective dephasing experiment where heteronuclear dipolar couplings are reintroduced by applying a symmetry-based sequence (S-REDOR). The selectivity is achieved by applying a pulse train, such as Delays Alternating with Nutations for Tailored Excitation (DANTE), to the quadrupolar nucleus. This new method allows quantitative analysis of proximities in the 3鈥? 脜 range of protons in OH ligands and one of the ⁵¹V sites in a complex decavanadate cluster, namely Cs₄[H₂V₁₀O₂₈]路4H₂O. The high selectivity of the DANTE-S-REDOR sequence offers the possibility to investigate a wide range of materials with different quadrupolar nuclei, including polyoxometalates, oxides, zeolites, and aluminophosphates.