We investigated the growth and surface properties of GaSb thin films on a Si(0 0 1) substrate prepared using a tailor-made fully alkyl-substituted heterocyclic single-source precursor. The precursor properties were monitored during the evaporation process by residual gas analysis (RGA). The initial film growth was monitored by Auger electron spectroscopy (AES). Using a high-vacuum cold wall reactor, dense GaSb films could be produced and were characterized by AES, AFM and synchrotron X-ray photoelectron spectroscopy (S-XPS). The results are discussed in terms of a correlation of the electronic and geometrical properties with the composition and structure of the films.