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Solid state 13C and 2H NMR investigations of paramagnetic [Ni(II)(acac)2L2complexes

Artikel i vetenskaplig tidskrift
Författare Anders Lennartson
Lene Ulrikke Christensen
Christine J. McKenzie
Ulla Gro Nielsen
Publicerad i Inorganic Chemistry
Volym 53
Sidor 399-408
ISSN 00201669
Publiceringsår 2014
Publicerad vid
Sidor 399-408
Språk en
Ämneskategorier Kemi

Sammanfattning

Nine structurally related paramagnetic acetylacetonato nickel(II) complexes: [Ni(acac) 2 ] and trans-[Ni(acac) 2 (X) 2 ]nH/D 2 O, X = H 2 O, D 2 O, NH 3 , MeOH, PMePh 2 , PMe 2 Ph, or [dppe] 1/2 , n = 0 or 1, dppe = 1,2-bis(diphenylphosphino)ethane, as well as cis-[Ni(F 6 -acac) 2 (D 2 O) 2 ], F 6 -acac = hexafluoroacetylonato, have been characterized by solid state 13 C MAS NMR spectroscopy. 2 H MAS NMR was used to probe the local hydrogen bonding network in [Ni(acac) 2 (D 2 O) 2 ]D 2 O and cis-[Ni(F 6 -acac) 2 (D 2 O) 2 ]. The complexes serve to benchmark the paramagnetic shift, which can be associated with the resonances of atoms of the coordinated ligands. The methine (CH) and methyl (CH 3 ) have characteristic combinations of the isotropic shift (δ) and anisotropy parameters (d, η). The size of the anisotropy (d), which is the sum of the chemical shift anisotropy (CSA) and the paramagnetic electron-nuclei dipolar coupling, is much more descriptive than the isotropic shift. Moreover, the CSA is found to constitute up to one-third of the total anisotropy and should be taken into consideration when 13 C anisotropies are used for structure determination of paramagnetic materials. The 13 C MAS NMR spectra of trans-[Ni(acac) 2 (PMe 2 Ph) 2 ], trans-[Ni(acac) 2 (PMePh 2 ) 2 ], and the noncrystallographically characterized trans-[Ni(acac) 2 (dppe)] n were assigned using these correlations. The complexes with L = H 2 O, D 2 O, NH 3 , and MeOH can be prepared by a series of solid state desorption and sorption reactions. Crystal structures for trans-[Ni(acac) 2 (NH 3 ) 2 ] and trans-[Ni(acac) 2 (PMePh 2 ) 2 ] are reported. © 2013 American Chemical Society.

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