Metal-organic frameworks (MOFs) are a class of hybrid materials with high surface areas and porosity, offering potential applications in gas storage, separations, and catalysis. This review discusses the rational design, synthesis, purification, and activation of MOFs. The key challenges in MOF synthesis include achieving pure, well-structured materials and preventing unwanted interpenetration of networks. Researchers have developed strategies to control catenation (interpenetration) by designing organic components to limit framework connectivity, thereby creating larger pores. Additionally, density-based separation methods have been employed to isolate desired MOFs from impurities. Activation of MOFs, particularly using supercritical carbon dioxide, has been shown to effectively remove solvent molecules without damaging the structure, resulting in high internal surface areas and usable channels. These advancements in synthesis, purification, and activation are expected to lead to new MOF structures and improved performance in various applications. The review highlights the importance of careful design in controlling MOF properties and the potential of supercritical processing to enhance their functionality.Metal-organic frameworks (MOFs) are a class of hybrid materials with high surface areas and porosity, offering potential applications in gas storage, separations, and catalysis. This review discusses the rational design, synthesis, purification, and activation of MOFs. The key challenges in MOF synthesis include achieving pure, well-structured materials and preventing unwanted interpenetration of networks. Researchers have developed strategies to control catenation (interpenetration) by designing organic components to limit framework connectivity, thereby creating larger pores. Additionally, density-based separation methods have been employed to isolate desired MOFs from impurities. Activation of MOFs, particularly using supercritical carbon dioxide, has been shown to effectively remove solvent molecules without damaging the structure, resulting in high internal surface areas and usable channels. These advancements in synthesis, purification, and activation are expected to lead to new MOF structures and improved performance in various applications. The review highlights the importance of careful design in controlling MOF properties and the potential of supercritical processing to enhance their functionality.