In situ neutron and synchrotron X-ray diffraction deliver unique and complementary insight into the microstructural evolution of metals at high temperature . Neutrons illuminate a larger bulk volume and reveal quantitative phase abundance, bulk texture, lattice parameter changes and other ensemble averaged quantities. In contrast, fine-bundled high-energy X-rays deliver reflections from a number of individual grains. For each constituting phase, their statistics and behavior in time reveal information about grain growth or refinement, subgrain formation, static and dynamic recovery and recrystallization, slip systems, twinning, etc. The complementarity between neutron and synchrotron radiation is demonstrated to study atomic order under ambient and extreme conditions. Examples are given on various metallic systems including magnesium, zirconium alloys and titanium aluminides.