Angew. Chem. Int. Ed. Engl. up to Apr 7, 2009

Angewandte Chemie International Edition
Volume 48 Issue 17, Pages 3082 - 3086
Published Online: 19 Mar 2009

Gwendal Kervern, Anthony D'Aléo, Loïc Toupet, Olivier Maury, Lyndon Emsley, Guido Pintacuda

Keywords
lanthanides • NMR crystallography • NMR spectroscopy • paramagnetism • structure elucidation

Abstract
Shifts for crystals: Solid-state NMR spectroscopy can be used for structure determination of microcrystalline paramagnetic solids at natural isotopic abundance. The protocol makes use of paramagnetic effects, measured on suitably recorded 1H NMR spectra, to define the conformation of a molecule in the lattice and the intermolecular packing in the solid phase. The method is illustrated with a family of lanthanide compounds (see picture).
Received: 29 October 2008; Revised: 7 January 2009
Digital Object Identifier (DOI) 10.1002/anie.200805302


Angewandte Chemie International Edition
Volume 48 Issue 15, Pages 2732 - 2736
Single-Scan 2D Hadamard NMR Spectroscopy

Assaf Tal, Boaz Shapira, Lucio Frydman

Keywords
Hadamard transform • multidimensional NMR • NMR spectroscopy • spatial/spectral encoding

Abstract
Scan and deliver: By combining imaging-based spectral/spatial 2D radiofrequency manipulations (see scheme, left) with Hadamard-weighting principles, 2D NMR spectra can be retrieved within a single scan (right). This approach can give homo- or heteronuclear correlations with an enhanced sensitivity over conventional ultrafast 2D NMR spectroscopy.


Angewandte Chemie International Edition
Volume 48 Issue 9, Pages 1673 - 1676
Revisiting Prussian Blue Analogues with Solid-State MAS NMR Spectroscopy: Spin Density and Local Structure in [Cd3{Fe(CN)6}2][sdot]15 H2O

by Alexandrine Flambard, Frank H. Köhler, Rodrigue Lescouëzec

Keywords
NMR spectroscopy • Prussian blue analogues • solid-state structures • spin density

Abstract
No legendary Prussian order! The distribution of vacancies in Prussian blue analogues is not random, and the spin density on the Cd2+ ion varies depending on the number of paramagnetic ions in its surroundings. This conclusion follows from 113Cd solid-state magic-angle spinning NMR studies of [Cd3{Fe/Co(CN)6}2]15 H2O, where the presence of small but significant spin density on the observed 113Cd nucleus leads to improved spectral resolution.
Received: 5 November 2008

Digital Object Identifier (DOI) 10.1002/anie.200805415 About DOI