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Issue 6, 2010
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Combining oximes with azides to create a novel 1-D [NaCoIII2] system: synthesis, structure and solid-state NMR

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Abstract

The synthesis and structure of a novel complex with the formula [NaCoIII2(dmo)2(μ-N3)3(N3)2], 1, are reported. Complex 1 was synthesized from the reaction of 1-(dimethylamino)propan-2-one oxime (Hdmo), CoCl2·6H2O, and NaN3 in MeOH. It crystallizes in the monoclinic space group C2/c. The molecular structure consists of one NaI and two CoIII ions bridged by two oxime ligands, two end-to-end azide and three end-on azide anions. The units are linked, forming a 1-D chain. This complex was characterized by UV-Vis spectroscopy where the data confirm the presence of low-spin CoIII ions. Solid-state 23Na NMR experiments indicate the presence of one magnetically unique site in the repeating unit, that sample purity in the bulk powdered form is high, and that it possesses microcrystalline order. Solid-state 59Co NMR experiments at ultra-high field (B0 = 21.1 T) are in agreement with the structure obtained through X-ray crystallography where the CoIII ions are coordinated to five nitrogen atoms as well as an oxygen atom.

Graphical abstract: Combining oximes with azides to create a novel 1-D [NaCoIII2] system: synthesis, structure and solid-state NMR

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Publication details

The article was received on 02 Sep 2009, accepted on 26 Oct 2009 and first published on 04 Dec 2009


Article type: Paper
DOI: 10.1039/B918082F
Citation: Dalton Trans., 2010,39, 1504-1510
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    Combining oximes with azides to create a novel 1-D [NaCoIII2] system: synthesis, structure and solid-state NMR

    T. Pathmalingam, F. Habib, C. M. Widdifield, F. Loiseau, T. J. Burchell, S. I. Gorelsky, A. M. Beauchemin, D. L. Bryce and M. Murugesu, Dalton Trans., 2010, 39, 1504
    DOI: 10.1039/B918082F

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