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The ligand azobis(2-pyridine) L was used in the synthesis of two new organic-inorganic coordination complexes: [Ni(L)2(NCS)2] 1 and [Co(L)2(NCS)2] 2. Crystal data for 1: monoclinic, space group C2/c, a = 13.361(18), b = 10.731(15), c = 18.14(2) (A), β = 109.86(2)°, V = 2446(6)(A)3, Z = 4, Mr = 543.25, Dc = 1.410 g/cm3, μ = 0.993 mm-1, F(000) = 1064, T = 298(2) K, R = 0.0454 and wR = 0.1010 for 1288 observed reflections with I > 2((I); and those for 2: monoclinic, space group C2/c, a = 13.35(2), b = 10.806(15), c = 18.06(2) (A), β = 110.34(2)°, Z = 4, Mr = 543.49, Dc = 1.413 g/cm3, μ = 0.902 mm-1, F(000) = 1060, T = 298(2) K, R = 0.0699 and wR = 0.1354 for 728 observed reflections with I > 2((I). Single-crystal X-ray diffraction studies revealed that 1 and 2 have similar structures, in which each Ni(II) or Co(II) cation is coordinated by two L ligands and two terminal thiocynates (NCS-).