The rhodium(III) distibine complexes trans-[Rh(L-L)(2)X-2]Y (L-L = Ph2Sb(CH2)(3)SbPh2 or o-C6H4(SbMe2)(2); X = Cl, Br or I; Y = X or BF4) have been prepared and studied by W-Vis, H-1 and Rh-103 NMR spectroscopies and electrospray mass spectrometry. The Rh-103 NMR spectroscopic data are reported and compared with data on related phosphine and arsine complexes. The sin le crystal X-ray structure of trans-[Rh{Ph2Sb(CH2)(3)SbPh2}(2)Cl-2][ClO4] is reported (Rh-Sb = 2.594(2), 2611(2); Rh-Cl = 2.369(7) Angstrom). (C) 1998 Elsevier Science S.A.