phen=1,10-phenanthroline) have been synthesized, and characterized by elemental analysis, IR, UV-Vis spectra, thermal analyses, and single-crystal X-ray diffraction. Two M(II) (M=Zn or Co) ions are bridged by two FCA anions with syn-anti bridging ligands, leading to dimeric cores, [M 2 (phen) 4 (FCA) 2 ] 2+ , and each M(II) ion is six-coordinated in a distorted octahedral geometry by two chelate phen ligands and two µ 2 -carboxylate oxygen atoms from two FCA groups. The M(II)…M(II) intradimer distances are 0.4391 and 0.4462 nm in 1 and 2, respectively. Electrochemical properties of the complexes have been discussed.