A laser vaporization flow reactor (LVFR) has been utilized for the gas phase synthesis of ligand-coated nanomaterials. Exploration into the gas phase synthesis of ultra-small nanoclusters and nanoparticles can help scientists understand the differences in material structure and properties in the nanoscale compared to the bulk material. The structural, electronic, and vibrational properties of nanomaterials are studied by mass spectrometry, spectroscopy, electron microscopy and computational calculations. Transition metal oxides are of particular interest due to their applications in catalysis, fuel cells, magnetic storage, photovoltaics, and other electronic devices. Chromium oxide and molybdenum oxide were studied in these synthesis experiments. Ultra-small chromium oxide nanoclusters were obtained in solution with stoichiometries not typically observed in the bulk material. We find that the complex CrxOy(MeCN)z solution contains a mixture of cluster sizes and isomers making spectroscopic interpretation difficult. Molybdenum oxide nanorods were produced with a morphology unlike other molybdenum oxide nanorods made by more traditional synthetic methods. These nanorods are much smaller and have increased catalytic activity over other molybdenum oxide nanomaterials but have optical and electronic properties similar to those of other molybdenum oxide nanorods.