Complex metal oxides used in lithium-based energy storage technologies undergo distinct crystallographic changes based on chemical composition, specific voltage and current states, degree of lithiation, and more. Crystallographic studies via X-ray diffraction (XRD) are a critical part of understanding structure-property relationships and engineering devices to meet specific performance requirements. For the raw electrode materials, XRD provides information about exact crystal structure (e.g. symmetry, unit cell parameters, atomic site mixing) as well as the presence of impurity phases that might arise from a poor sintering process or non-stoichiometric starting reagents. For formed devices such as button- or pouch-cells, XRD can be used in operando to measure changes in phase composition, phase quantification, and crystal lattice expansion/contraction as a function of charge state. This can provide useful information such as the level of reversibility of a device or the onset of impurity phases during aging and long cycling.In this presentation, we will review diffraction data for case studies based on NMC electrodes and highlight key insights into reversible structural changes during device cycling. The figure attached to this abstract shows diffraction data as a function of charge state during a single charge/discharge cycle. The observed peaks show modifications to the crystalline lattice (expansion in one direction, contraction in another orthogonal direction). Figure 1