Abstract The crystal structure determination of the title compound was undertaken to determine the coordination geometry of nickel atom. Bis(glyoxal‐bis‐tert.butylimine)nickel(0) (C20H40NiN4) crystallizes in the space group Pna21 with Z = 4, a = 18.546(6), b = 9.331(8), and c = 13.505(8) Å. The structure was solved by the heavy atom method and refined to R = 0.065. The molecule has four‐coordinate nickel atom. The coordination geometry about the nickel atom is tetragonal.