A 31P Spin Diffusion and 31P-113Cd CP/MAS NMR Study of Polycrystalline Cd3(PO4)2.
Two-dimensional 31P spin diffusion MAS NMR expts. on polycryst. Cd3(PO4)2, using a broad-banded dipolar recoupling scheme, are reported. Quant. anal. of the 31P spin diffusion expts. as a function of mixing times yields unambiguous assignment of the six 31P resonances to the six independent crystallog. P sites in the asym. unit of solid Cd3(PO4)2. Internuclear P-P connectivities detd. from these 31P spin diffusion MAS NMR expts. quant. agree with the P-P distance connectivities as detd. by single-crystal x-ray diffraction. From the known assignment of all 31P resonances for Cd3(PO4)2, all 113Cd resonances can be unambiguously assigned to the resp. nine independent crystallog. Cd sites, using 1-dimensional selective 31P -> 113Cd CP/MAS NMR techniques where a 31P chem. shift filter was used as a prepn. step for selective 31P -> 113Cd cross-polarization.
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