To synthesize the non-templated framework, we heated a mixture of H4dotpdc-CO2tBu (0.100 equiv), H4dotpdc-CH2NHBoc (0.100 equiv), H4dotpdc (0.800 equiv), and Mg(NO3)2•6H2O (2.50 equiv) in DMF and MeOH for 3 h. Powder X-ray diffraction (PXRD) and 1 H NMR digestion studies confirmed that the resulting framework, which contains protected carboxylic acid and benzylamine groups, adopts the desired Mg2dotpdc structure (Fig. ) with the expected functional group loading (~10% of each group, Fig. ). The tert-butyl ester and carbamates in this framework were removed via microwave thermolysis to reveal 1-nontemplated (Fig. ). Like the templated framework, a large increase in BET surface area from 2440 m 2 /g to 2780 m 2 /g was observed upon thermolysis and removal of the protecting groups (Fig. ). The control frameworks 1-CH2NH2 and 1-COOH were synthesized in a similar fashion, but with functional group loadings of ~20 mol%. Given how differences in particle size and internal mass transport limitations can obscure intrinsic differences catalytic activity, scanning electron microscopy (SEM) studies were carried out to confirm that all frameworks have similar morphologies. An average length of 0.307 ± 0.148 µm and an average diameter of 0.060 ± 0.018 µm was observed for 1-templated, while an average length of 0.338 ± 0.139 µm and an average diameter of 0.077 ± 0.025 µm was obtained for 1nontemplated (Figs. and). These lengths and diameters are all within error of each other, confirming that the use of crosslinked ligand dimers at these concentrations has little impact on the resulting framework morphology. Together, these analyses confirm that all frameworks are identical in terms of their overall structure, surface area, and particle morphology, and differ only in their functional group content and spatial distribution.