1H,89Y HMQC and further NMR spectroscopic and X-ray diffraction investigations on yttrium-containing complexes exhibiting various nuclearities.

2D 1H,89Y heteronuclear shift correlation through scalar coupling has been applied to the chemical-shift determination of a set of yttrium complexes with various nuclearities. This method allowed the determination of 89Y NMR data in a short period of time. Multinuclear NMR spectroscopy as function of temperature, PGSE NMR-diffusion experiments, heteronuclear NOE measurements, and X-ray crystallography were applied to determine the structures of [Y5(OH)5(L-Val)4(Ph2acac)6] (1) (Ph2acac=dibenzoylmethanide, L-Val=L-valine), [Y(2)(OTf)3] (3), and [Y2(4)(OTf)5] (5) (2: [(S)P{N(Me)NC(H)Py}3], 4: [B{N(Me)NC(H)Py}4]−) in solution and in the solid state. The structures found in the solid state are retained in solution, where averaged structures were observed. NMR diffusion measurements helped us to understand the nuclearity of compounds 3 and 5 in solution. 1H,19F HOESY and 19F,19F EXSY data revealed that the anions are specifically located in particular regions of space, which nicely correlated with the geometries found in the X-ray structures.