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A novel hexanuclear Co(II) coordination compound with a nonsymmetrical Salamo-type bisoxime ligandH4L, namely [{Co3(HL)(MeO)(MeOH)2(OAc)2}2]·2MeOH, was prepared and characterized by elemental analyses, UV–vis, IR and fluorescence spectra, and X-ray single-crystal diffraction analysis. Each Co(II) is hexacoordinated, and possesses a distorted CoO6 or CoO4N2 octahedrons. The Co(II) coordination compound possesses a self-assembled infinite 2D supramolecular structure with the help of the intermolecular C–H···O interactions. Meanwhile, the photophysical properties of the Co(II) coordination compound were studied.