title: 1H,89Y HMQC and further NMR spectroscopic and X-ray diffraction investigations on yttrium-containing complexes exhibiting various nuclearities.
abstract: 2D (1)H,(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 (89)Y 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 [Y(5)(OH)(5)(L-Val)(4)(Ph(2)acac)(6)] (1) (Ph(2)acac=dibenzoylmethanide, L-Val=L-valine), [Y(2)(OTf)(3)] (3), and [Y(2)(4)(OTf)(5)] (5) (2: [(S)P{N(Me)N=C(H)Py}(3)], 4: [B{N(Me)N=C(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. (1)H,(19)F HOESY and (19)F,(19)F 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.
authors.affiliation: Institute of Inorganic Chemistry, Karlsruhe Institute of Technology, Engesserstrasse 15, 76131 Karlsruhe, Germany.
authors.forename: Matthias W
authors.initials: MW
authors.lastname: Löble
authors.forename: María
authors.initials: M
authors.lastname: Casimiro
authors.forename: Dominique T
authors.initials: DT
authors.lastname: Thielemann
authors.forename: Pascual
authors.initials: P
authors.lastname: Oña-Burgos
authors.forename: Ignacio
authors.initials: I
authors.lastname: Fernández
authors.forename: Peter W
authors.initials: PW
authors.lastname: Roesky
authors.forename: Frank
authors.initials: F
authors.lastname: Breher
mesh_terms: D000838:Anions / Q000737:chemistry*; D018360:Crystallography, X-Ray; D009682:Magnetic Resonance Spectroscopy; D008958:Models, Molecular; D009942:Organometallic Compounds / Q000737:chemistry*; D013696:Temperature; D014961:X-Ray Diffraction; D015019:Yttrium / Q000737:chemistry*
chemical_list: D000838:Anions; D009942:Organometallic Compounds; D015019:Yttrium