Bismetallic triangles T4 (Ru2/Fe) and T5 (Ru2/Zn) were effectively prepared via a stepwise method from a 60°-bent bisterpyridne. Compared with obtaining T4 by mixing metallo-organic ligand L2 with Fe(2+) directly and refluxing at a higher temperature (85 °C), the site to site metallo-transformation from T5 to T4 was employed at RT by simply adding Fe(2+) to T5. The structures were fully confirmed by the NMR, ESI-mass, UV-vis absorption and emission spectroscopies.