The application of in situ and operando spectroscopic techniques has significantly advanced the understanding of reticular materials, particularly metal-organic frameworks (MOFs) and covalent organic frameworks (COFs). These techniques offer real-time insights into the dynamic structural, electronic, and chemical changes that occur within these materials during various processes, such as catalysis, sorption, and material synthesis. This review offers a comprehensive overview of key in situ and operando techniques used to investigate the formation, functionalization, and catalytic behavior of reticular materials. How these techniques have elucidated the roles of active sites, reaction intermediates, and structural transformations under reaction conditions, especially in single-site catalysis, electrocatalysis, and photocatalysis, is highlighted. The review also discusses the challenges and opportunities that lie ahead in integrating advanced spectroscopic methods with reticular materials, aiming to foster further innovation in the design and application of these versatile materials.