Six new MOFs have been synthesized by using transition metal ions and 2,5-furandicarboxylic acid, [M(fdc)(bpe)]n (M = Co(1)/Ni(2)); [M(fdc)(bpee)]n (M = Co(3)/Ni(4)); [M(fdc)(H2O)3]n (M = Mn(5)/Zn(6)), [where fdc = furan-2,5-dicarboxylic acid, bpe = 1,2-bis(4-pyridyl)ethylene, bpee = 1,2-bis(4-pyridyl)ethane]. All the compounds were characterized by single crystal X-ray analysis and show interesting diversities in their structures. Compounds 1–4 are interesting two-fold interpenetrated 3D frameworks, whereas 5 and 6 have zig-zag chains. Topological analysis on compounds 1–4 revealed that these compounds are uninodal 7-c nets with the Schläfli symbol 33.413.54.6. Compounds 1–4 were subjected for N2 adsorption study to measure the porosity of the materials. BET measurement shows that compounds 1–4 are microporous having surface areas of 128 m2 g−1. The variable temperature magnetic susceptibility measurement reveals the presence of weak interaction in the compounds.