The crystal structures of the self-assembled metallapentacycles [{Fe5(bptz)5(CH3CN)10} ⊂ 2SbF6][SbF6]8 (1) and [{Fe5(bmtz)5(CH3CN)10} ⊂ SbF6][SbF6]9 (2) with the π-acidic ligands bptz (3,6-bis(2-pyridyl)-1,2,4,5-tetrazine) and bmtz (3,6-bis(2-pyrimidyl)-1,2,4,5-tetrazine), respectively, revealed cationic pentagons templated by [SbF6]− ions. The short anion–π contacts established between the anions and the tetrazine rings play an important role in the stability of the pentagons.
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