Nanocrystalline NiGa
2
O
4
films were deposited on silicon substrates by the CVD of a new heterometal alkoxide, [NiGa
2
(O
t
Bu)
8
]. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) showed a single-step decomposition behavior for the molecular precursor at low temperature (240°C), suitable for a CVD process. [NiGa
2
(O
t
Bu)
8
] is monomeric in solid state with a tetrahedral Ni
2+
center coordinated by two monoanionic {Ga(O
t
Bu)
4
}-moieties. Despite an adequate vapor pressure, the gas-phase transport of [NiGa
2
(O
t
Bu)
8
] is susceptible to the distance and geometry of the effective diffusion path. Investigations on CVD deposits obtained using different transport pathways (reservoir — substrate) show that gas-phase travel through a long (39 cm) and angular reactor tube induces fragmentation of the heterometal compound, which yields minor amounts of Ni, NiO, and Ga
2
O
3
(amorphous), besides the target (NiGa
2
O
4
) composition. Shortened reservoir — substrate path length (13 cm) produced stoichiometric NiGa
2
O
4
films, apparently due to reduced collision probabilities and a laminar flow. In both cases, the chemical composition was determined using energy-dispersive X-ray (EDX) and X-ray photoelectron spectroscopy (XPS), whilst the structure was evaluated using powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). From these, the advantages and limitations of the single molecular source in the growth of NiGa
2
O
4
films could be determined.