A new di-Schiff base ligand, 1,2-bis(3′-pyridylmethyleneamino)ethane(L), was designed and its Ag(Ⅰ) complex[Ag 2(L) 2](CF 3SO 3) 2 was synthesized. The crystal structure analysis indicates that the complex crystallizes in monoclinic system, space group of C2/c with a=3.770 4(2) nm, b=0.797 90(10) nm, c=2.471 3(2) nm, β=101.840(10)°, V=7.276 5(12) nm 3, Z=8, D c=1.808 g/cm 3, \{F(000)=\}3 936, R=0.058 3, wR=0.076 6, (Δρ) max=0.657×10 3 e/nm 3,(Δρ) min=-0.562×10 3 \{e/nm 3\}. It is interesting that one L ligand coordinates to three Ag(Ⅰ) atoms using four N atoms, while another L ligand connects two Ag(Ⅰ) atoms with three of four N atoms and one N atom keeps free of coordination.
