AbstractWhereas reaction of PhCH2NMe32Te6Fe8(CO)24 (1) in refluxing CH2CI2forms Fe2(CO)6(μ0‐) TeCH2Te), treatment of 1 with Ph2SnCl2or Mel gave the oxidation product Te2Fe3(CO)9. Oxidation of 1 with Cu(CH3CN)4BF4afforded Te2Fe3(CO)9in good yield. Cluster 1 was converted to PhCH2NMe3Te4Fe5(CO)14 (2) in MeOH/CH2Cl2solution. Cluster 2 was structurally characterized by single‐crystal X‐ray diffraction and spectral methods. Complex 2 is composed of two Te2Fe2(CO)6fragments linked by one Fe(CO)2group. 2 crystallizes in the orthorhombic space group Pbcn with a = 13.351 (4) Å, b = 13.417 (4) Å, c = 26.077 (3) Å, V = 4671 (2)
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