We have prepared new chiral bimetallic assemblies of discrete binuclear [CuL2][Ni(CN)4]·2H2O or onedimensional cyanide-bridged [CuL2][Pd(CN)4] (and [CuL2][Pt(CN)4]) (L = (1S,2S)-(+)-N,N'-dimethyl-cyclohexane-1,2- diamine). The numbers of co-crystallized water molecules contained are different from each other and their compositions are easy to vary due to co-crystallized water molecules. As far as we studied on the related [Cu(diamine)2]a [M(CN)b]c·dH2O compounds, actually such a feature has been found for the first time. According to crystal structures, the elongated axial bond distances of [CuL2]2+ moieties are Cu-N = 2.195(7) Å for [CuL2][Ni(CN)4]·2H2O, Cu-N = 2.443(4)and 2.519(2) Å for [CuL2][Pd(CN)4]. Single crystal structure analyses, variable low temperature XRD, measurements of electronic, CD, emission, and XPS spectra and magnetic properties have been carried out. We compared their structural preference between NiII and PdII (or PtII) metal ions. Novel emission band of [CuL2][Pt(CN)4] appeared at 410 nm (λex = 360 nm) in the solid state regardless of quenching by cyanide-bridged CuL2]2+ moieties.