Surface-active metalorganic complexes can be used to construct organic thin films with excellent electronic and catalytic properties. We have recently introduced a new versatile surface-active ligand, which can efficiently coordinate a wide range of transition metals. In the present work we report an investigation of Langmuir monolayers of V V, Mo VI and Ti IV complexes of this ligand, using surface pressure-area isotherms, Brewster-angle microscopy, and Grazing incidence X-ray diffraction. The monolayers of these complexes are stable enough over broad temperature ranges to allow efficient transfer to solid substrates