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Charge transfer molecular solids [diaqua tetrabenzo (b,f,j,n,) {1,5,9,13) tetraazacyclohexadecine] Ni(II) and Cu(II) bisanthraflavates were synthesized and characterized by IR, Mass Spectrometry, TGA, and X-ray diffraction on single crystals. Unit cell dimensions (A) a = 12.291(1), c = 14.574(1) A and a = 12.434(1), c = 14.066(1) A for Cu(II) and Ni(II) derivatives, respectively, space group P42/n in both cases. The obtained compounds show expected chemical and structural similarities. Tetraazamacrocycles are surrounded individually by a zig-zag, ribbon-like motif extending in the crystal by head-to-tail hydrogen bonding of monosubstituted anthraflavates. Electric conductivities were measured by the four points method as pellets from the variation of electric current through the sample as a function of temperature, for fixed voltages in the ohmic regime. Preliminary results indicate low conductivity values at room temperature but semiconductivity behaviour in the temperature range −150 to 170°C.