The Mo 13 clusters we previously reported were derived from MoS 2 flakes prepared from bulk MoS 2 , although the nature of the precursor species was not fully understood. The existence of the clusters in the condensed phase was a question. Here we report the preparation of MoS 2 nanoflakes from elemental precursors using the sonochemical method and study the gas-phase clusters derived from them using mass spectrometry. Ultraviolet-visible (UV-vis) spectrum of the precursor is comparable to nano MoS 2 derived from bulk MoS 2 . High-resolution transmission electron microscopy (HRTEM) revealed the formation of nanoflakes of MoS 2 with 10-to 30-nm length and 3-to 5-nm thickness. Laser desorption ionization mass spectrometry (LDI-MS) confirmed the formation of Mo 13 clusters from this nanomaterial. Matrix-assisted laser desorption ionization mass spectrometry (MALDI-MS) points to the existence of Mo 13 clusters in the condensed phase. The clusters appear to be stable because they do not fragment in the mass spectrometer even at the highest laser intensity. Computational analysis based on generalized Wannier orbitals is used to understand bonding and stability of the clusters. These clusters are highly stable with a rich variety in terms of centricity and multiplicity of MoOMo There are several synthetic approaches such as gas-phase deposition [5,6], laser ablation [7,8], electron irradiation [9], and high-temperature chemical routes [10,11] for the synthesis of clusters. Nano forms of these materials have their own advantages over the corresponding bulk materials. Electrochemical deposition [12] and sonochemical routes [13,14] are some other methods adapted for the synthesis of nanostructured materials. Electrochemical methods result in the formation of nanomaterials as a film, whereas sonochemical methods produce free-standing nanoflakes of metal chalcogenides with controlled size.