Bimetallic complexes 3a-e of 1,1'-bisacetylacetoferrocene (2) were prepared by reactions of transition metal acetates M(OAc)2 (M = Co2+, Mn2+, Cu2+, Ni2+, Zn2+) with the 2 in refluxing methanol. The X-ray structures of the cobalt and manganese complexes were determined showing very similar centrosymmetric macrocyclic dimeric frameworks constituted by linkage of two Co2+ or Mn2+ ions and two 1,1'-diacetoacetylferrocene units with two additional methanols as bridges dividing this macrocyclic framework into two small cyclic subunits. The UV-Vis spectra and electronic properties were also studied.