In this project, linker exchange in the metal–organic frameworks Zn2(C2O4)(1,2,4-triazolate)2 will be investigated using solution-phase (solvothermal) and mechanochemical methods. The possibility of replacing the triazolate ligands in these compounds with triazole ligands substituted at the 3- and/or 5-positions will then be explored, with substituents including alkyl groups (e.g., methyl, ethyl, phenyl), halogens (chlorine, bromine, trifluoromethyl), or nitrogen-containing groups (cyano, carboxamide). The resulting products will subsequently be thoroughly characterized using diffraction, spectroscopic, and thermal analysis techniques, followed ultimately by physisorption measurements (CO2, N2, H2O).