General macrocyclization conditions. Macrocycles with alkyl linkers were prepared using standard iodoalkyne azide click reaction conditions at varying concentrations. Cu(MeCN)4PF6 (9 mg, 50 mol%) and TBTA (13 mg, 50 mol%) were dissolved in dry DCM (100 or 10 mL) and stirred for 30 minutes. Di-iodoethynyl arene (0.05 mmol, 1 eq.) and bis-azide (0.05 mmol, 1 eq.) were added, and the reaction was left to stir in the dark for 48 hours or until complete conversion. The reaction mixture was washed with EDTA/NH4OH solution, dried over MgSO4, adsorbed onto silica and purified with flash column chromatography in 2% MeOH in DCM to give a mixture of [1+1] and [2+2] macrocycles. This mixture was adsorbed onto silica and subjected to reverse-phase flash column chromatography in 60:40 to 100:0 MeCN:Water mixtures to give the desired [1+1] macrocycle as the first elution band, which was then further purified by recrystalisation from a hot 1:4 mixture of EtOAc:heptane to afford the pure [1+1] macrocycle.