Reactions of singly-bonded dimolybdenum complexes [(eta(5)-RC5H4)(2)Mo-2(CO)(6)] (1, R = CH3CO; II R = C6H5CO; III, R = CH3O2C; IV. R = C2H5O2C) with diphenyiditelluride in the presence of (Bu4NI)-Bu-n were investigated. Although complex I reacted with diphenylditelluride in refluxing xylene to give both mononuclear complex 1 [(eta(5)-C5H5)Mo(CO)(3)Te] and dinuclear complex 2 cis/ae-[(eta(5)-CH3COC5H4)(2)Mo-2(mu-Te)(2)(mu-TePh)(2)], reactions of complexes II, III and IV with diphenylditelluride under the same conditions only afforded dinuclear complexes cis/ae-[(eta(5)-RCC5H4)(2)Mo-2(mu-Te)(2)(mu-TePh)(2)] (3, R = C6H5CO; 4, R - CH3O2C; 5, R = C2H5O2C). All the new complexes have been characterized by elemental analyses, H-1 NMR, C-13 NMR and IR spectroscopies. Crystal structures of complexes I and 5 have been determined by X-ray diffraction analyses. (C) 2004 Elsevier Ltd. All rights reserved.