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An EPR study of the transformation of Ni(cyclam)@CB[8] and Ni(cyclen)@CB[8] inclusion compounds during annealing in a hydrogen atmosphere

  • Current NMR and EPR Spectroscopy Methods in Structural Chemistry of Complex Crystals, Glasses, Composites, and Biological Membranes
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Abstract

The transformation is studied of the compounds {[Ni(cyclam)]@CB[8]}Cl2·16H2O and {cis-[Ni(cyclen)(H2O)Cl]@CB[8]}Cl·12H2O during thermal annealing in a temperature range of 20°C to 340°C. Using EPR spectroscopy, {cis-[Ni(cyclen)(H2O)Cl]@CB[8]}Cl·12H2O, Ni is found to reduce to the 3d 9 state during annealing in a hydrogen atmosphere yet oxidize to the 3d 7 state in the air at 20°C. In the case of {[Ni(cyclam)]@CB[8]}Cl2·16H2O, nickel ions remain in the 3d 8 state after annealing in a hydrogen atmosphere and make a transition to the 3d 7 state after air pumping. In both cases, annealing in a hydrogen atmosphere leads to the decomposition of the nickel complexes; simultaneously, a single line with g = 2.003 appears in the EPR spectra, which is likely to be due to the resulting metal nickel clusters.

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Correspondence to V. A. Nadolinnyi.

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Original Russian Text Copyright © 2013 by V. A. Nadolinnyi, A. S. Berezin, V. V. Bakovets, E. A. Kovalenko

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Translated from Zhurnal Strukturnoi Khimii, Vol. 54, Supplement 1, pp. S94–S98, 2013.

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Nadolinnyi, V.A., Berezin, A.S., Bakovets, V.V. et al. An EPR study of the transformation of Ni(cyclam)@CB[8] and Ni(cyclen)@CB[8] inclusion compounds during annealing in a hydrogen atmosphere. J Struct Chem 54 (Suppl 1), 92–96 (2013). https://doi.org/10.1134/S002247661307007X

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  • DOI: https://doi.org/10.1134/S002247661307007X

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