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A discrete heterotrinuclear complex [{Ni 2 LDy(OAc) 3 (CH 3 OH)} 2 ] · 2CH 3 OH · 3CH 2 Cl 2 , with a naphthalenediol-based acyclic bis(salamo) ligand H 4 L, has been synthesized and structurally characterized using elemental analyses, IR, UV/Vis and fluorescence spectra and single crystal X-ray diffraction. The crystal structure shows two crystallographically independent but chemically identical molecules (molecules  I  and  II ). All the Ni(II) atoms are hexa-coordinated with slightly distorted octahedral geometries. The central Dy atoms are nona-coordinated with slightly distorted tricapped trigonal prism geometries. An infinite 3D supramolecular structure is formed via intermolecular hydrogen bonding and C–H…π interactions.

A heterotrimetallic Ni(II)–Dy(III) bis(salamo)-based complex: synthesis, structure and fluorescent property