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The last decade has witnessed significant advances in the scale-up synthesis of metal–organic frameworks (MOFs) using commercially available and affordable organic linkers. However, the synthesis of MOFs using elongated and/or multitopic linkers to access MOFs with large pore volume and/or various topologies can often be challenging due to multi-step organic syntheses involved for linker preparation.In this report, a orthogonal MOF synthesis strategy is developed by utilizing the coordination and covalent bonds formation in one-pot where monoacid-based ligands reacted to form ditopic ligands which then assembled into a 3-D MOF with Zr6 clusters. Chemical stability of the resulting materials was significantly enhanced through converting the imine bond into robust linkage via cycloaddition with phenylacetylene. Oxygen storage capacities of the MOFs were measured, and enhanced volumetric O2 uptake was observed for the stabilized MOF, NU-401-Q.