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A new ternary complex of nickel(Ⅱ) with L-aspartate (L-Asp) and 1, 10-phenanthroline(Phen), [Ni3(L-Asp)(Phen)5(H2O)3](ClO4)4.4.75H2O, has been synthesized in a mixed solvent of H2OC2H5OH at the pH value of 3. It crystallizes in triclinic, space group P-1