super(1)H, super(89)Y HMQC and Further NMR Spectroscopic and X-ray Diffraction Investigations on Yttrium-Containing Complexes Exhibiting Various Nuclearities

2D super(1)H, super(89)Y 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 super(89)YNMR 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 [Y sub(5)(OH) sub(5)(L-Val) sub(4)(Ph sub(2)acac) sub(6)] (1) (Ph sub(2)acac=dibenzoylmethanide, L-Val=L-valine), [Y(2)(OTf) sub(3)] (3), and [Y sub(2)(4)(OTf) sub(5)] (5) (2: [(S)P{N(Me)N[double horizonal line]C(H)Py} sub(3)], 4: [B{N(Me)N[double horizonal line]C(H)Py} sub(4)] super(-)) 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. super(1)H, super(19)FHOESY and super(19)F, super(19)FEXSY 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. The Ys and wherefores: 2D super(1)H, super(89)Y heteronuclear shift correlation through scalar coupling was applied to the chemical-shift determination of a set of yttrium complexes with various nuclearities. Multinuclear NMR spectroscopy as a function of temperature, PGSE NMR diffusion experiments, heteronuclear NOE measurements, and X-ray crystallography were applied to determine the structures in solution and in the solid state.