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Achieving control over the phase-selective synthesis of mixed metal oxide materials remains a challenge to the synthetic chemist due to diffusion-driven growth, which necessitates the search for new compounds with pre-existent chemical bonds between the phase-forming elements. We report here a simple solvothermal process to fabricate LiCrO₂ and Li₂CrO₄ nanoparticles from bimetallic single-source precursors, demonstrating the distinctive influence of molecular design and calcination conditions on the resulting nanomaterials. The chemical identity of [Li₂Cr(O<i>^t</i>Bu)₄Cl(THF)₂] (<b>1</b>) and [LiCr(O<i>^t</i>Bu)₂(PyCH=COCF₃)₂(THF)₂] (<b>2</b>) was unambiguously established in the solid state by single-crystal X-ray diffraction, revealing the formation of a coordination polymeric chain in compound <b>1</b>, whereas electron paramagnetic resonance spectroscopy (EPR) studies revealed a monomeric structure in solution. TEM analysis of synthesized LiCrO₂ nanoparticles showed nearly uniform particles size of approximately 20 nm. The sensitivity of the LiCrO₂ phase towards oxidation was investigated by X-ray diffraction, revealing the formation of the stable Li₂CrO₄ after calcination in air.