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Investigation of solvation effects on the solid‐state 31P NMR spectra of tertiary phosphine derivatives and metal complexes

An investigation of bis(diphenylphosphino)methane dioxide (dppm dioxide), cis‐[PtCl2(PPh3)2] cis‐[PtCl2{P(p‐C6H4Cl)3}2] and cis‐[PtBr2(PPh3)2] by solid‐state CP/MAS 31P NMR spectroscopy, x‐ray powder diffraction and 1H, 13C{1H} and 31P{1H} solution NMR methods illustrates the sensitivity of the appearance of solid‐state NMR spectra to solvation effects in crystalline solids. The presence or absence of solvent of crystallization and the slow loss of solvent of crystallization from a sample over time are clearly manifested in the solid‐state NMR spectra as the local site symmetry in the solid is changed. These effects have led workers to report different data for a given compound when, in fact, different types of solvates were investigated.