Nickel nitrate diammine, Ni(NH 3 ) 2 (NO 3 ) 2 , can be synthesised from the thermal decomposition of nickel nitrate hexammine, Ni[(NH 3 ) 6 ](NO 3 ) 2 . The hexammine decomposes in two distinct major stages; the first releases 4 equivalents of ammonia while the second involves the release of NO x , N 2 , and H 2 O to yield NiO. The intermediate diammine compound can be isolated following the first deammoniation step or synthesised as a single phase from the hexammine under vacuum. Powder X-ray diffraction (PXD) experiments have allowed the structure of Ni(NH 3 ) 2 (NO 3 ) 2 to be solved for the first time. The compound crystallises in orthorhombic space group Pca2 1 (a = 11.0628 (5) Å, b = 6.0454 (3) Å, c = 9.3526 (4) Å; Z = 4) and contains 11 non-hydrogen atoms in the asymmetric unit. Fourier transform infrared (FTIR) spectroscopy demonstrates that the bonding in the ammine is consistent with the structure determined by PXD.