87Sr, 119Sn, 127I Single and {1H/19F}-Double Resonance Solid-State NMR Experiments: Application to Inorganic Materials and Nanobuilding Blocks

Laurencin, D. and Ribot, F. and Gervais, C. and Wright, A.J. and Baker, A.R. and Campayo, L. and Hanna, J.V. and Iuga, D. and Smith, M.E. and Nedelec, J.-M. and Renaudin, G. and Bonhomme, C. (2016) 87Sr, 119Sn, 127I Single and {1H/19F}-Double Resonance Solid-State NMR Experiments: Application to Inorganic Materials and Nanobuilding Blocks. ChemistrySelect, 1 (15). pp. 4509-4519. ISSN 2365-6549

Abstract

87Sr, 127I and 119Sn wideline NMR spectroscopy was successfully applied to inorganic and hybrid materials: (i) Sr derivatives of medicinal interest (Sr-malonate, Sr-pyrophosphates, mixed Ca,Sr-fluoroapatites); (ii) apatitic structures acting as host matrices for iodine; and (iii) Sn-derived oxo-clusters which can be used as inorganic nanobuilding blocks. The BRAIN (BRoadband Adiabatic INversion) CP (Cross Polarization) approach (by Schurko et al.) was applied to a non integer quadrupolar nucleus (87Sr, I=9/2). The sequence was used in combination with WURST (Wideband Uniform-Rate Smooth-Truncation) QCPMG (Quadrupolar Carr-Purcell Meiboom-Gill) for optimal sensitivity. We showed that 127I WURST QCPMG experiments were sufficiently sensitive to allow rapid characterization of the incorporation of iodide (I−) anions in lead vanadate/phosphate apatites, and that 127I acted as a sensitive probe for the description of local disorder. 1H/19F → 119Sn BRAIN CP was successfully applied to the detailed characterization of tin oxo-clusters, using 1H and 19F as spin baths. We demonstrated that BRAIN CP can be effectively used as a tool of spectral editing leading to the estimation of spatial proximities between 119Sn and 1H/19F nuclei. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim