Unexpectedly, a sharp isotropic feature at g = 2.002 was observed in all thermolyzed samples. We assign this feature to a ligand-based organic radical generated during the thermal deprotection step, as it is observed even in the unfunctionalized Mg2dotpdc after thermal treatment (Fig. ). We note that careful air-free thermolysis under microwave conditions minimizes, but does not fully eliminate, the presence of this radical species, suggesting it arises due to oxidation of the framework backbone at high temperatures.