Series of new TTF and bis-TTF containing a thiophene ring as a substituent or as a spacer group were prepared by using a pall adium-catalyzed cross-coupling reaction from tributylstannyl-trimethyltetrathiafulvalene (tMeTTF-SnBu3) and different halogeno and dihalogenothiophene derivatives. The reducing power of each new precursor was determined by cyclic voltammetry. Radical cations salts and charge transfer complexes of the donors with TCNQ were prepared and characterized. The electrical conductivity of these materials was measured and discussed in terms of (electronic) structure. (C) 2007 Elsevier B.V. All rights reserved.