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The local structure of the fast solid ion conductor Cu 2 P 3 I 2  = (CuI) 8 P 12  is investigated using one- and two-dimensional  31 P and  65 Cu magic-angle spinning NMR techniques. Peak assignments are proposed on the basis of anisotropic and isotropic spin-spin interactions recovered via  radio frequency driven dipolar recoupling  (RFDR) and  total through bond correlation spectroscopy  (TOBSY) methods. Especially the previously proposed R30 6  14  pulse symmetry (R-TOBSY), which exploits scalar spin-spin interactions for coherence transfer, offers outstanding spectral selectivity with respect to  1  J  coupling. Using sufficiently short mixing times it is thus possible to correlate selectively those  31 P spins that are directly bonded, thereby providing detailed insights into phosphorus-phosphorus connectivities in the network. The final assignment of the nine resolved  31 P resonances to the twelve crystallographically distinct phosphorus sites suggests a significant relationship between  31 P chemical shifts and the detailed pyramidal P(P 1/3 ) 3  bonding geometry.

Solid State NMR Connectivity Studies in Dipolarly Coupled Inorganic Networks: Site Assignments in the Solid Electrolyte Material (CuI) 8 P 12