Mg 2 (dobpdc) was synthesised according to a previously reported procedure. Mg(NO 3 ) 2 •6H 2 O (11.5 g, 45.0 mmol, 1.24 equiv), H 4 dobpdc (9.90 g, 36.0 mmol, 1.00 equiv), N,N-dimethylformamide (DMF) (90 mL), and methanol (110 mL) were mixed together in a 350 mL glass heavy wall pressure vessel (Chemglass, CG-1880-42). The reaction mixture was sonicated for 15 min until all of the solids had dissolved, and was then sparged with N 2 for 1 h. The reaction vessel was sealed and heated at 120 °C with stirring for 21 h. This resulted in the precipitation of a white solid from solution. The solid was collected via vacuum filtration and quickly returned to the reaction vessel along with fresh DMF (250 mL). The reaction vessel was then heated to 60 °C for 3 h with stirring. Following this, the solid was again collected via vacuum filtration and returned to the reaction vessel with fresh DMF (250 mL) and again heated to 60 °C for 3 h with stirring. This washing process with DMF was repeated a total of three times, after which the solid was washed three more times in methanol (250 mL) at 60 °C to yield the desired product, Mg 2 (dobpdc). A small portion of the product (ca 0.1 g) was collected via filtration and activated for characterisation by powder diffraction (Figure ) by heating to 60 °C in N 2 for 15 h. The remaining Mg 2 (dobpdc) was stored in methanol.