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A new thiolate-bridged diiron complex with two mono-coordinated azido ligands, [Cp*Fe(μ-SMe)N3]2 (Cp* =η5-C5Me5 ), was synthesized from [Cp*Fe(μ-SMe)MeCN]2[PF6] 2 and NaN 3 in a bi-solvent system of acetone and methanol. X-ray crystal structural analysis