The magnetic properties and structure of LixCoO2 for 0.5 < x < 1.0 are reported. Co4+ is found to be high spin in LixCoO2 for 0.94 <= x <= 1.00 and low spin for 0.50 <= x <= 0.78. Weak antiferromagnetic coupling is observed, and at x approximate to 0.65 the temperature-independent contribution to the magnetic susceptibility and the electronic contribution to the specific heat are largest. Neutron diffraction analysis reveals that the lithium oxide layer expands perpendicular to the basal plane and the Li ions displace from their ideal octahedral sites with decreasing x. Comparison of the structures of NaxCoO2 and LixCoO2 reveals that the CoO2 layer changes substantially with alkali content in the former but is relatively rigid in the latter, and that the CoO6 octahedra in LixCoO2 are less distorted.
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