The reaction of the sodium salt of the monoanion, nido-[2,3-(Si(CH3)(3))(2)-2,3-C2B4H5](-), with (chloromethyl)dimethylchlorosilane in a 1:1 molar ratio produced the B-(cage)-substituted cluster, nido-5-ClCH2Si(CH3)(2)-2,3-(Si(CH3)(3))(2)-2,3-C2B4H5 (1), in 81% yield. This product (1) was reacted further with the lithium salt of [closo-1-R-1,2-C2B10H10](-) monoanion (R =Me, Ph) to give the novel linked and mixed C2B4/C2B10 carborane species, 1-Me-2-[5'-SiMe2CH2-2',3'-(SiMe3)(2)-2',3-C2B4H5]-1,2-C2B10H10 (2), 1-Ph-2-[5'-SiMe2CH2-2',3'-(SiMe3)(2)-2',3'-C2B4H5]-1,2-C2B10 (3), in yields of 76% and 81%, respectively. (C) 2003 Elsevier B.V. All rights reserved.