The initial metallopolymer, derived from two different organic building blocks, is a kinetic intermediate to the final stable hexanuclear (bearing 4Ru(2+) and 2Fe(2+)) metallomacrocycle obtained through a thermodynamic dis-assembly/re-assembly route. The heteroleptic metallomacrocyclic architecture was characterized by NMR, UV, IR, CV, 2D-ROESY, DOSY, and ESI-MS.