With spatially separated, site-isolated bimetallic pairs in mind, we targeted the synthesis of carbamate-crosslinked Mg2dotpdc at relatively low crosslinker loadings (<20 mol%). Heating a mixture of crosslinked ligand dimer (0.100 equiv), H4dotpdc (0.900 equiv), and Mg(NO3)2•6H2O (2.75 equiv) in a solution of DMF and MeOH produced microcrystalline powders with the desired Mg2dotpdc structure. Keeping in mind that each equivalent of L1 or L2 contains two ligand monomers, this reaction mixture should theoretically lead to ~18% functional group loading. The exact composition of the framework was quantified by digestion 1 H NMR (Table ). Consistent with previous work, the experimentally observed incorporation of L1 or L2 varied slightly, but was typically slightly higher than the value expected based on the initial ratio of starting materials. Using the ligand dimer L1, we obtained a framework containing 18% crosslinked (i.e., functionalized) ligand, which we have abbreviated as 1-XL-18% (Fig. ). Similarly, using the ligand dimer L2 under these conditions produced a material containing 23% crosslinked ligand, which we have abbreviated 2-XL-23% (Fig. ). Both chemically crosslinked frameworks are permanently porous, displaying high Brunauer-Emmett-Teller (BET) surface areas of 2370 m 2 /g and 2400 m 2 /g for 1-XL-18% and 2-XL-23%, respectively (Fig. ).