The synthesis of the crosslinked Mg2dotpdc framework, abbreviated 1-crosslinked, was achieved by heating a mixture of the unfunctionalized ligand H4dotpdc (0.875 equiv), crosslinked ligand dimer H8XL-AB (0.125 equiv), and Mg(NO3)2•6H2O (2.50 equiv) in a mixture of DMF and MeOH. After 3 h, a microcrystalline powder consistent with the Mg2dotpdc structure was obtained (Fig. ). Digestion 1 H NMR analysis was used to quantify the framework composition and ensure no premature crosslinker degradation occurred during framework synthesis. We obtained a framework in which 24% of the ligands are crosslinked, which is slightly higher than the expected incorporation of ~22% based on the ratio of the starting ligands (Fig. ). The presence of the crosslinker peaks in the NMR (0.9 ppm-1.6 ppm) confirmed that no crosslinker degradation occurs under these conditions.