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A new synthesis route to Li2NiF4 based on a fluorolytic process using Ni(acac)2 or Ni(OAc)2·4H2O as precursor is presented. Variation of the synthesis conditions allows crystallite size control of the obtained powders. 6Li and 7Li MAS NMR experiments were carried out to study local environments of the lithium ions. Several attempts were made to synthesize Li2CoF4, which are, unfortunately, hitherto...
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