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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(OtBu)4Cl(THF)2] (1) and [LiCr(OtBu)2(PyCH=COCF3)2(THF)2] (2) was unambiguously established in the solid state by single-crystal X-ray diffraction, revealing the formation of a coordination polymeric chain in compound 1, 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.

Molecularly Engineered Lithium–Chromium Alkoxide for Selective Synthesis of LiCrO2 and Li2CrO4 Nanomaterials