Reported herein is the preparation of a new-bis-bidentate ligand 4, 4′-methylene-bis-(1-(2- pyridyl) pyrazole), L, which forms a dinuclear triple helicate complex [Fe2L3] 4+, 1, on reaction with Fe (BF4) 2· 6H2O in acetonitrile or nitromethane solution. The formation of 1 was studied by 1H NMR and UV–vis spectroscopic titration experiments, which identified the existence of dinuclear triple-stranded species in solution (most likely the rac-helicate), and ...