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The local structures around Fe and As were probed using X‐ray absorption spectroscopy in metastable derivatives of NaFeAs obtained by deintercalation of the metals with iodine in THF at room temperature. The deintercalated product with a defective ThCr2Si2 structure is unattainable through conventional high temperature routes due to the size‐mismatch between the eight‐coordinate site and the Na+ radius...
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