H-NMR (600 MHz, DMSO-d6): δ 10.52 (s, 4H), 9.09 (s, 2H), 8.94 (s, 4H), 7.94 (app. s, 4H), 7.39 (dd, J = 6.1, 3.6 Hz, 4H). The reaction flask containing the 5-nitroisophthaloyl dichloride (0.58046 g) was evacuated and charged with dry N2(g). The predried TBACl (3.25227 g, 5 equivs.) was pre-dissolved in CH2Cl2 (20 mL). The CH2Cl2:TBACl solution (10 mL) was added directly to the reaction flask and allowed to stir for 10 min. The 2,3-diaminonapthalene (0.4907 g, 1.1 equivs.) was pre-dissolved in the CH2Cl2:TBACl solution (10 mL) and then added to the reaction mixture over 2 min. After 10 min, the crude product was precipitated by adding CH3OH (40 mL). The precipitate was separated and washed with H2O (excess) and n-hexane (4×10 mL) to remove residual diamine. The crude was then triturated in boiling DMSO (10 mL), after which the solution was allowed to stand at r.t. while the Cl -complex slowly precipitated. Once at r.t., the solid was separated from the trituration mixture; it was washed again with water (excess) and n-hexane (4×10 mL). The solid was collected, and anion exchange was then performed by suspending the solid in CH3CN (150 mL), KPF6 (10 equivs.) was added, and the mixture was stirred for 12 h. The bright yellow solid was filtered and washed with H2O (excess) before being dried in vacuo, with a final yield of 0.07751 g (6%). The reaction flask containing the 5-nitroisophthaloyl dichloride (0.58889 g) was evacuated and charged with dry N2(g). The predried TBACl (3.29947 g, 5 equivs.) was pre-dissolved in CH2Cl2 (20 mL). The CH2Cl2:TBACl solution (10 mL) was added directly to the reaction flask and allowed to stir for 10 min. The 1,2-diamino-4,5-difluorobenzene (0.37641 g, 1.1 equivs.) was also predissolved in the CH2Cl2:TBACl solution (10 mL) and then added to the reaction mixture over 2 min. After 10 min, the crude product was precipitated by adding CH3OH (40 mL). The precipitate was separated and washed with H2O (excess) and nhexane (4×10 mL) to remove residual diamine. The crude was then triturated in boiling DMSO (10 mL), after which the solution was allowed to stand at r.t. while the Cl -complex slowly precipitated. Once at r.t., the solid was separated from the trituration mixture; it was washed again with water (excess) and n-hexane (4×10 mL). The solid was collected, and anion exchange was then performed by suspending the solid in CH3CN (150 mL), KPF6 (10 equivs.) was added, and the mixture was stirred for 12 h. The off-white solid was filtered and washed with H2O (excess) before being dried in vacuo, with a final yield of 0.25827 g (17%). The reaction flask containing the 5-fluoroisophthaloyl dichloride (0.30044 g) was evacuated and charged with dry N2(g). The pre-dried TBACl (1.88904 g, 5 equivs.) was pre-dissolved in CH2Cl2 (20 mL). The CH2Cl2:TBACl solution (10 mL) was added directly to the reaction flask and allowed to stir for 10 min. The ortho-phenylenediamine (0.16162 g, 1.1 equivs.) was predissolved in the CH2Cl2:TBACl solution (10 mL) and then added to the reaction mixture over 2 min. After 10 min, the crude product was precipitated by adding CH3OH (40 mL). The precipitate was separated and washed with H2O (excess) and nhexane (4×10 mL) to remove residual diamine. The crude was allowed to dry in the glass frit before being dissolved in a minimum volume of CHCl3:acetone (8:2, v/v) with excess TBACl added as a solubilising agent and loaded onto a prep-TLC plate, which was run in an eluent system of CHCl3:acetone (8:2, v/v). The silica containing the separated UV-active spot of the Cl -complex was collected and stirred in a system of CH2Cl2:acetone (7:3, v/v) for a minimum of 12 h before being filtered and evaporated under reduced pressure. The solid was collected, and anion exchange was then performed by suspending the solid in CH3CN (150 mL), KPF6 (10 equivs.) was added, and the mixture was stirred for 12 h. The bright white powdery solid was filtered and washed with H2O (excess) before being dried in vacuo, with a final yield of 0.02826 g (4%).