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This article presents the synthesis and characterisation (Fourier transform infrared spectroscopy, 1H NMR and 13C NMR spectroscopy, CHNS (carbon, hydrogen, nitrogen, sulfur) analysis, atomic absorption spectrometry, and single-crystal X-ray diffraction) of a single source molecular precursor 1-(2-fluorolbenzoyl)-3-(3-ferrocenylphenyl)selenourea (M2F). This precursor has been used for the fabrication of FeSe thin films by aerosol-assisted chemical vapour deposition (AACVD) in the presence of different concentrations of two different surfactants (triton and span) keeping all other conditions the same. Fabricated thin films have been characterised with powder X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The interaction of the surfactants with the precursor (M2F) has been evaluated with cyclic voltammetry and UV–vis spectroscopy.