The reaction of [{Cpx(CO)2Fe}SbCl2] [1a: Cpx = η5‐C5H3tBu2‐1,3 (Cp"); 1b: Cpx = η5‐C5Me5 (Cp*)] with Na2[Fe(CO)4] or K[Co(CO)4] affords the novel antimony‐transition metal cluster compounds [{μ3‐SbFe(CO)2Cp"}3{Fe(CO)3}4] (2), [{Fe3(CO)9}{μ3‐SbFe(CO)2Cp"}2] (3) and [{μ4‐SbFe(CO)2Cp*}2{Co4(CO)10(μ‐CO)}] (4). All products were characterised by X‐ray structure analyses and other methods. Cluster 2 reveals a novel Sb3Fe4 core, which does not follow the Wade−Mingos rules. Cluster 3 forms a square‐pyramidal nido‐cluster. The Sb2Co4 cluster core of 4 derives from a pentagonal bipyramid and consists of apical Sb and equatorial Co atoms with one missing pentagonal core atom.
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