Metal organometallic carboxylates with unusual polyhedral and rectangular shapes have been prepared by the reaction of 1,1'-ferrocenedicarboxylic acid (H(2)FDCA) with Zn-II and Cu-II to give [Zn6O2(FDCA)(5)(H2O)(DMF)]center dot(DMF)(4) (1), [Zn8O4(FDCA)(6)(H2O)(3)]center dot(DMA)(4)center dot(H2O)(2) (2), and [CU4(FDCA)(2)] (3), respectively (DMF = N,N'-dimethylformamide; DMA = N,N'-dimethylacetoamide). SQUID data of zinc compounds show that iron ions of the ferrocene moieties in the compounds exhibit antiferromagnetic coupling.