[ACCESS RESTRICTED TO THE UNIVERSITY OF MISSOURI AT AUTHOR'S REQUEST.] Supramolecular chemistry is the study of how to form complexes through molecular self-assembly and intermolecular bonding. Our research group has been doing a lot supramolecular research based on macrocycles such as calixarenes, pyrogallolarenes and resorcinarens. This research is interested in formation of novel C-alkyresorcin[n]arene( n=4,6) based cocrystals. The basic plan is to design and synthesize cocrystals, then analyze the crystal structure via single crystal X-ray diffraction technique, and determine if the novel cocrystal has the ability to absorb gases such as carbon dioxide and nitrogen. Chapter two is about the cocrystallization of six different C-alkylresorcin[4]arene according the chain length and guest molecule 1-(2-pyridylazo)-2-naphthol( PAN) in four solvent systems. Five successfully synthesized cocrystals' structure and synthesis are discussed. Chapter three talks how to use cocrystallization as a separation method to separate C-ethylresocin[6]arene from C-ethylresorcin[4]arene. Three noval C-ethylresorcin[6]arene based cocrystals from three different solvents are discussed. Chapter four investigates the cocrystallization between C-ethylresorcin[n]arene (n=4, 6) with 4, 4'-bipyridine. It discusses how solvent and component concentration affect such cocrystallization. Chapter five uses cocrystal formed from C-ethylresorcin[6]arene and 1,2-bis(4-pyridyl)ethane in acetone as the gas sorption candidate to test its ability to absorb gases after solvent removal. The conditions of removing solvents and gas sorption results are discussed.