<正> Reaction of 2-pyridone, copper acetate and terbium(or yttrium) perchlorate in acetone with the moleratio 6: 2: 1 results in the formation of heteronuclear complex Ln2Cu4L8 (HL)4 (OH)2 (ClO4)4 (H20)102CH3COCH3(Ln = Tb (1), Y (2)). By recrystallizing (1) in CHCl3 single crystals were obtained and thestructure was determined by four-circle diffractometer. Data showed that the crystal is in space groupC2/m with a=27. 454(9)A, b=13, 608A, c=30. 556(11)A, β=99. 89(3)°, v=11245. 7(7. 5)A3. Thestructure was solved by a combination of Patterson method and Fourier technique. The final R value is0. 103. In the structure, four copper and two terbium ions are bridged by 2-pyridone anions to form anessentially octahedral Cu4Tb2 core. The terbium atoms are each eight-coordinate and the copper atomsare five-coordinate.