A new 3d-4f coordination polymer {[CuTb 2(INAIP) 3(HCOO)(H 2O) 3] · 3H 2O} n (1) was obtained by solvothermal assembly of CuCl 2·H 2O and Tb(NO 3) 3·6H 2O with the H 2INAIP (5-(isonicotinamido)isophthalic acid) ligand. Complex l crystallizes in triclinic, space group P1̄ with a=1.088 79(16) nm, b = 1.518 5(2) nm, c = 1.565 3(2) nm, D=2.338 1(6) nm 3, Z=2, C 43H 37CuTb 2N 6O 23,M r=1387.17, D c=1.970 g·cm -3,μ=3.538 mm -1, F(000)=1360,R int=0.021 2, R=0.058 9, wR =0.129 2. Single-crystal X-ray diffraction analysis revealed that each INAIP ...