Layered double hydroxides (LDHs) with the Cu 2+ /Ni 2+ /Cr 3+ molar ratio of 1/2/1 on the brucite-like layers and interlayer anions (viz sulfate, nitrate and carbonate, respectively) were synthesized by a coprecipitation method. The effects of interlayer anions on the structural properties of as-synthesized LDHs and resulting calcined products at 773 K. Calcination of well-crystallized LDHs leads to the formation of mixed metal oxides including CuO, NiO and Cu 2+ -, Ni 2+ - and Cr 3+ -containing spinel phases, the composition distributions of which obtained from LDHs precursors depend on the nature of interlayer anions, thus resulting in the difference of the reducibility of reducible metal species in the calcined LDHs. Moreover, the surface basicity of the calcined material, which is related to the different behaviour of LDHs precursors during the thermal decomposition depending on the interlayer anions, increases progressively following the order of calcined LDHs from sulfate to nitrate and carbonate.