Kervern, GwendalPintacuda, GuidoZhang, YongOldfield, EricRoukoss, CharbelKuntz, EmileHerdtweck, EberhardtBasset, Jean-MarieCadars, SylvianLesage, AnneCoperet, ChristopheEmsley, Lyndon2015-01-082015-01-082015-01-08200610.1021/ja063510nhttps://infoscience.epfl.ch/handle/20.500.14299/110074WOS:000241157600050A general protocol for the structural characterization of paramagnetic molecular solids using solid-state NMR is provided and illustrated by the characterization of a high-spin FeII catalyst precursor. We show how good NMR performance can be obtained on a molecular powder sample at natural abundance by using very fast (> 30 kHz) magic angle spinning (MAS), even though the individual NMR resonances have highly anisotropic shifts and very short relaxation times. The results include the optimization of broadband heteronuclear (proton-carbon) recoupling sequences for polarization transfer; the observation of single or multiple quantum correlation spectra between coupled spins as a tool for removing the inhomogeneous bulk magnetic susceptibility (BMS) broadening; and the combination of NMR experiments and density functional theory calculations, to yield assignments.text::journal::journal article::research article