The Bragg peak corresponding to the interlayer planes of the final cathode structure (i.e., (003) peak of the layered transition metal oxide structure with R-3m space group symmetry) becomes visible after 330 °C when lithiation starts to take place (Figure . This indicates that the first lithiated phase that forms is layered, rather than a disordered rocksalt (as is occasionally observed in Ni-rich materials ). We note that the asymmetric broadening of the (104) peak could be interpreted as a spinel-like distortion (see SI Figure ), consistent with intermediates observed in other studies. However, we could not perform quantitative refinement due to the lack of any isolated peaks attributable to a second phase. Under the conditions of this study, the lithiation reaction proceeds in a straightforward way from the rocksalt product of thermal treatment of the TM precursor to the layered oxide, without the formation of isolated intermediate phases.