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A 3D mixed-valence Co(III)–Co(II) compound [Co9(bta)10(Hbta)2(H2O)10]n·[22(H2O)]n(1)(H2bta=N,N-bis(1H-tetrazole-5-yl)-amine) was hydrothermally synthesized by reaction of Co(NO3)2·6H2O with H2bta·H2O. Compound 1 consists of three kinds of d