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3, the presence of closely overlapping reflections in the powder data does not allow us to unequivocally distinguish between a monoclinic and orthorhombic space group for any composition except x = 3, where we have single crystal data. The overall changes in β (and hence symmetry) are insignificant, however (see Table 1). Upcoming synchrotron experiments will resolve this minor issue, which is nonetheless not important in the context of the relationship to the electrochemical transformation described here. Note: subsequent to the submission of this manuscript, two reports on the monoclinic phase appeared: a) M.Y. Saïdi, J. Barker, H. Huang, J.L. Swoyer, G. Adamson, Electrochem. Solid-State Lett. 2002, 5, A149.
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0011985166
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note
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The stoichiometries of chemically oxidized materials were confirmed by placing the materials into an electrochemical cell and determining the composition directly from examining the effect of lithium insertion on the curve shape. All compositions were also verified by ICP analysis.
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0024732929
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R.W. Pekala, J. Mater Sci. 1989, 24, 3221. After aging, the gel was immersed in acetone and washed three times prior to use, to extract water and any carbonate impurities.
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Pekala, R.W.1
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0011978187
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note
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Chemical analysis (Galbraith Labs, Tennessee USA): Li, 4.28 %; V, 20.52 %; P, 18.35 %; V, 38.43 %; C, 14.7 %.
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0011918585
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note
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More information can be obtained from the authors.
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