期刊
CHEMISTRY-A EUROPEAN JOURNAL
卷 18, 期 17, 页码 5325-5334出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/chem.201102636
关键词
cluster compounds; ligand effects; NMR spectroscopy; X-ray diffraction; yttrium
资金
- Federal Ministry of Education and Research (BMBF) [02NUK012B]
- Center for Functional Nanostructures (CFN)
- Ramon y Cajal program
- Junta de Andalucia
- Alexander von Humboldt foundation
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)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. 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.
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