Three highly fluorinated dirhodium (II) tetrakis (benzoates),[Rh2 (O2CRF) 4, RF= C6H4-4- C6F13 (3) and C6H3-3, 5-di (CnF2n+ 1)(n= 6: 4; n= 8: 5)], have been prepared and characterized. Only 4 and 5 are suited for applications in fluorous synthesis due to their excellent solubility in fluorous solvents. They were found to catalyze the following carbenoid reactions of diazo compounds in the fluorous solvents 1, 1, 2-trichloro-1, 2, 2- ...