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A novel peptide complex was synthesized by a solid-solid reaction of glycyl-L-glutamine monohydrate and bismuth trichloride powders. The formula of the complex is (BiCl3)2[NH2CH2CONHCH(COOH)CH2CH2COOH·H2O]3. The crystal structure of the complex belongs to monoclinic system with the lattice parameters: a = 0.6914 nm, b = 0.7378 nm, c = 1.0005 nm, β = 194.1° . The characterization results of IR, Raman spectra and thermal analysis show that complex is dimer and unidentate coordination. Each bismuth atom and three chlorine atoms are coplanar in the complex.