500 mg of as-synthesized TBAP was covered by DMF (40 mL) in a large vial. The mixture was sonicated for 10 min. and left overnight so all remaining undissolved material settled at the bottom of the vial. 20 mL of the supernatant solution was the filtered into two 40 mL vial using a 0.45 µm PTFE syringe filter to remove any particulates. For batches 1 and 3, the 40 mL vials were capped with a septum that had been pierced using a needle and these vials were placed in a sealed chamber containing chloroform. For batch 2, the 40 mL sample vials were left uncapped and placed in a sealed chamber containing chloroform. Vapor diffusion of chloroform into the TBAP solution was carried out for until the vials containing the TBAP material were nearly full of solvent. Most of the solvent was then removed via syringe, until the level of solvent was just above the TBAP crystals. Acetone (10 mL) was then injected into the solution and subsequently removed via syringe. This process was repeated twice more, and enough acetone was then added to fill the vial completely. This solvent was removed and then replenished every 12 hours for 5 days, which yielded the solvent exchanged the TBAP•x (acetone) solvate (Figures and), the yellow crystalline material was filtered off and allowed to dry under ambient conditions. The solid was then evacuated at 120 ºC for 14 hours to give the activated material (Figures and). Complete removal of the solvent was confirmed by the absence of any DMF, CHCl3, or acetone peaks in the 1 H NMR spectra of the activated sample (Figure ).