We have investigated the growth of thin films of Cu and Co by CVD using the β-diketonate complexes of the metals, viz., the respective acetylacetonates, dipivaloylmethanates, and ketocarboxylates. Film growth rate was measured as a function of CVD parameters such as substrate temperature and reactor pressure. Film microstructure was examined by optical microscopy, XRD, SEM, and STM. Electrical resistivity was measured as a function of temperature and film thickness. It was found that film microstructure is a function of the molecular structure of the precursor and of the other growth parameters. For example, Cu films from Cu(II) ethylacetoacetate comprise uniform, fine grains which result in bulk electrical conductivity at a thickness as small as 75nm. Though grown under nearly the same conditions, Cu films from Cu(II) dipivaloylmethanate are porous, with faceted, large crystallites. Cobalt films from Co(II) acetylacetonate are x-ray amorphous even at a deposition temperature of 450°C. It is possible, by choosing CVD parameters, to obtain metal films with microstructures appropriate to devices and to structures of very small dimensions.