Based on prior knowledge regarding the interaction of N2O/O2 and CH4 with Fe in Fe-SSZ-13, this proposal aims to use an operando multi-spectroscopy approach including RIXS, KBeta-HERFD-XAS, and KBeta,alfa-XES to elucidate the temperature-dependent reaction mechanism of CH4 hydroxylation to CH3OH and to isolate the atomic-scale reactivity of active Fe centres. This includes monitoring the Fe oxidation state, the structure of intermediates (Fe-O), spin dynamics, and preferential ligation as a function of reaction conditions.