Abstract: | The crystal structure of the title compound, [RhI(C18H15Sb)3(CO)], represents a rare example of a crystallographically characterized five‐coordinate RhI–SbPh3 complex. The compound crystallizes with the I—Rh—CO core on a threefold rotation axis, with three crystallographically equivalent triphenylstibine ligands. Selected geometric parameters are: Rh—I = 2.7159 (8), Rh—Sb = 2.5962 (4), Rh—CCO = 1.825 (6) and CCO—O 1.153 (6) Å, and Sb—Rh—I = 89.374 (10) and Sb—Rh—CCO = 90.626 (10)°. The cone angle of the SbPh3 ligand was determined as 137°, according to the Tolman model. |