Abstract: | Whereas reaction of PhCH2NMe3]2|Te6Fe8(CO)24] (1) in refluxing CH2CI2 forms Fe2(CO)6(μ0-) TeCH2Te), treatment of 1 with Ph2SnCl 2 or Mel gave the oxidation product Te2Fe3(CO)9. Oxidation of 1 with Cu(CH3CN)4]BF4 afforded Te2Fe3(CO)9 in good yield. Cluster 1 was converted to PhCH2NMe3]Te4Fe5(CO)14] (2) in MeOH/CH2Cl2 solution. Cluster 2 was structurally characterized by single-crystal X-ray diffraction and spectral methods. Complex 2 is composed of two Te2Fe2(CO)6 fragments linked by one Fe(CO)2 group. 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) Å 3, Z = 4. |