✍ Scribed by Heinz Rüegger
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High‐resolution solid‐state ^31^P cross‐polarization magic angle spinning (CP/MAS) spectra of a series of Pd(II) complexes were obtained. All of these spectra exhibit low‐intensity satellite peaks flanking the main resonances which are assigned to originate from a combination of direct (D) and indirect (J) spin–spin coupling between the ^31^P and the ^105^Pd spins. The parameter ^1^J(^105^Pd,^31^P) is found to be sensitive to the nature of the ligand in a trans position and thus of great value in assigning the configuration, i.e. cis or trans, in square‐planar complexes of Pd(II). A linear relationship between ^1^J(^105^Pd,^31^P) and ^1^J(^195^Pt,^31^P) in analogous Pd(II) and Pt(II) complexes is suggested, the latter parameter being a factor of ca 14 larger. Two‐dimensional exchange spectroscopy proved valuable in resolving overlapping resonances and relating pairs of inequivalent ^31^P spins within the same complex and spreading their satellite manifolds into two dimensions. These two spectral features are unrelated, being due to dipolar coupling among the phosphorus spins in the former and finite lifetimes of the spin states of the ^105^Pd isotope in the latter case. Copyright © 2004 John Wiley & Sons, Ltd.
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