Metal-Organic Frameworks (MOFs) are crystalline hybrid materials composed of metal nodes—either isolated ions or clusters—coordinated with organic ligands to form porous, extended structures. While most MOFs utilize transition metal centers, non-transition metals have also been incorporated. Their unique architectures and high surface areas make MOFs highly promising for various applications including gas adsorption, separation, catalysis, and drug delivery. This review presents an in-depth analysis of the synthesis routes, activation methodologies, characterization techniques, and design of organic linkers critical for MOF construction. It also highlights the research gap in the utilization of silicon- and boron-based building blocks, compared to their carbon-based counterparts. This work aims to serve as a useful reference for researchers, industrial practitioners, and academics engaged in MOF research and development.