Abstract Attempts to prepare alkylidyne-trirhodium cluster complexes [RCRh 3 (CO) n (PPh 3) 9− n] by reactin of Na [Rh (CO) 2 (PPh 3) 2] with CX 4, CHX 3 (X= Cl or Br) and CCl 3 CF 3 have resulted only in the formtion of [RhX (CO)(PPh 3) 2]. With CHCl 3 at− 20 C the major product is [Rh (CO) 2 (PPh 3) 2] 2, though to be formed by decomposition of [RhH (CO) 2 (PPh 3) 2]. Reaction between Na [Rh (CO) 2 (PPh 3) 2] and perfluoroacyl chlorides has ...