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

Frédérique Pourpoint (1) , Julien Trébosc (1) , Christian Bonhomme (2) , Olivier Durupthy (3) , Nathalie Steunou (4) , Olivier Lafon (1) , Jean-Paul Amoureux (1)

1 UCCS - Unité de Catalyse et Chimie du Solide - UMR 8181
2 LCMCP (site Paris VI) - Laboratoire de Chimie de la Matière Condensée de Paris (site Paris VI)
3 LCMCP - Laboratoire de Chimie de la Matière Condensée de Paris
4 ILV - Institut Lavoisier de Versailles

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 3-4 angstrom range of protons in OH ligands and one of the V-51 sites in a complex decavanadate cluster, namely Cs-4[H(2)V(10)O(28]center dot)4H(2)O. 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.

Domaines: Matériaux

Frédérique Pourpoint, Julien Trébosc, Christian Bonhomme, Olivier Durupthy, Nathalie Steunou, et al.. Quantitative Analysis of the Proximities of OH Ligands and Vanadium Sites in a Polyoxovanadate Cluster Using Frequency-Selective H-1-V-51 Solid-State NMR Spectroscopy. Journal of Physical Chemistry C, 2014, 118 (32), pp.18580-18588. ⟨10.1021/jp505194q⟩. ⟨hal-01275061⟩