The reaction of Fe(CO)2(NO)2 and Ni(N2S2) (N2S2 = N,N′-Bis(2-mercaptoethyl)-1,4-diazacycloheptane) by a single CO replacement yields [Ni(N2S2)]Fe(NO)2(CO), while an excess of Fe(CO)2(NO)2 leads to triply bridging thiolate sulphurs in a cluster of core composition Ni2S4Fe3, lacking one Fe(NO)2 unit to complete the adamantane-like structure. This structural type was earlier identified in a CuICl aggregate of MII(N2S2) (MII = Ni, Cu), in which complete MII2S4CuI4 core structures were obtained as the major, and, in the case of CuII(N2S2), the incomplete CuII2S4CuI3 as a minor, product. The full Ni2S4Fe4 cluster has not yet been realized for Fe = Fe(NO)2. Computational analysis of the NiFe-heterobimetallic complex addresses structural issues including a ∠Ni–S–Fe of 90° in the bimetallic complex.
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