A rectangular Ni-Fe cluster with unusual cyanide bridgesElectronic supplementary information (ESI) available: Crystal structure and magnetic data of 2. CCDC 883725-883727. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c2dt31152f

An asymmetric polycyanide iron complex, K 2 [Fe III (L1)(CN) 4 ](MeOH) (HL1 = 2,2-(1 H -pyrazole-3,5-diyl)bis-pyridine), was synthesized and its complexation compatibility with nickel ions was examined. Two kinds of enantiomeric nickel-iron squares were obtained in the presence of a chiral bidentate capping ligand. The compounds display unusual cyanide bridge geometry and have ferromagnetic interactions between nickel and iron ions. An asymmetric polycyanide iron complex, K 2 [Fe III (L1)(CN) 4 ](MeOH) (HL1 = 2,2-(1 H -pyrazole-3,5-diyl)bis-pyridine), was synthesized and its complexation compatibility with nickel ions was examined.