Atomic/molecular layer deposition (ALD/MLD) is currently strongly emerging as an intriguing route for novel metal–organic thin-film materials. This approach already covers a variety of metal and organic components, and potential applications related to e.g. sustainable energy technologies. Among the 3d metal components, nickel has remained unexplored so far. Here we report a robust and efficient ALD/MLD process for the growth of high-quality nickel terephthalate thin films. The films are deposited from Ni(thd)2 (thd: 2,2,6,6-tetramethyl-3,5-heptanedionate) and terephthalic acid (1,4-benzenedicarboxylic acid) precursors in the temperature range of 180–280 °C, with appreciably high growth rates up to 2.3 Å per cycle at 200 °C. The films are amorphous but the local structure and chemical state of the films are addressed based on XRR, FTIR and RIXS techniques.