Abstract: The first homometal dicubane nickel(II) complex based on unsymmetrically substituted 1,3-diketone (1,1,1-trifluoro-4-(2-methoxyphenyl)butan-2,4-dione) was synthesized and studied by X-ray diffraction using synchrotron radiation (CCDC no. 861889). In the crystal of the complex, nickel atoms are joined into tetrahedra sharing a common vertex with Ni…Ni distances of 3.026–3.127 Å; the geometry is completed to a distorted dicubane by μ3-bridging oxygen atoms of the hydroxyl groups. The coordination environment of each metal center is a distorted octahedron, the ligand is deprotonated and performs a bidentate function, forming six-membered chelate rings. © Pleiades Publishing, Ltd. 2024. ISSN 1070-3284, Russian Journal of Coordination Chemistry, 2024, Vol. 50, No. 7, pp. 485–491. Pleiades Publishing, Ltd., 2024.