Polyferrocene　macrocycles　hold　immense　potential　in　the　fields　of　molecular　electronics　and　electrochemistry,　primarily　due　to　their　multiple　metal　centers.　However,　developing　highly　efficient　synthetic　strategies　for　constructing　these　rings　remains　a　significant　challenge.　In　this　study,　we　successfully　synthesized　triferrocenyl　macrocycles　using　Pt-mediated　coupling　strategy　and　determined　their　configuration　using　single-crystal　X-ray　diffraction　analysis,　revealing　a　structure　reminiscent　of　the　Penrose　Stair.　We　comprehensively　investigated　the　macrocycle’s　structure,　photophysical　properties,　and　employed　density　functional　theory　(DFT)　calculations　to　gain　further　insights.　Notably,　this　macrocycle　exhibits　several　advantageous　features,　including　a　flexible　structure,　good　solubility,　and　a　highly　efficient　synthetic　pathway.　(Figure　presented.).　©　Jilin　University,　The　Editorial　Department　of　Chemical　Research　in　Chinese　Universities　and　Springer-Verlag　GmbH　2024.