A new porous metal–organic framework, Mo3(BTC)2 (BTC = 1,3,5-benzene-tricarboxylate) was obtained by oxidation of Mo(CO)6 with trimesic acid. The compound is microporous and has a high specific micropore volume (0.67 cm3 g−1) and BET surface area (1280 m2 g−1). The compound is isotypic to Cu3(BTC)2 crystallising in the cubic space group Fm
m with an extended lattice parameter (a = 27.129 Å). TUDMOF-1 is diamagnetic and has a high hydrogen adsorption capacity of 195 cm3 g−1 (1.75 wt.%) at 77 K (1 atm). The Mo–Mo stretching frequency depends on the solvation state of the sample, νsym(Mo–Mo) = 401 cm−1 for the solvated and 417 cm−1 for the desolvated (activated) sample.