Abstract We report on two regioisomeric, diazocine ligands 1 and 2 that can both be photoswitched between the E‐ and Z‐configurations with violet and green light. The self‐assembly of the four species (1‐Z, 1‐E, 2‐Z, 2‐E) with CoII ions was investigated upon changing the coordination vectors as a function of the ligand configuration (E vs Z) and regioisomer (1 vs 2). With 1‐Z, Co2(1‐Z)3 was self‐assembled, while a mixture of ill‐defined species (oligomers) was observed with 2‐Z. Upon photoswitching with 385 nm to the E configurations, the opposite was observed with 1‐E forming oligomers and 2‐E forming Co2(2‐E)3. Light‐controlled dis/assembly was demonstrated in a ligand competition experiment with sub‐stoichiometric amounts of CoII ions; alternating irradiation with violet and green light resulted in the reversible transformation between Co2(1‐Z)3 and Co2(2‐E)3 over multiple cycles without significant fatigue by photoswitching.
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