Synthesis and structural characterization of Mo-2(mu-SC6H4-Cl-p)(2)(mu-dppm)(CO)(6) and [(dppm)(CO)(2)Mo(mu-SC6H4-Cl-p)(2)Mo(O)](2)(mu-SC6H4-Cl-p)(2)(mu-O) and electrochemical property of Mo-2(mu-SC6H4-Cl-p)(2)(mu-dppm)(CO)(6)

Dimolybdenum(I) compound Mo-2(mu-SC6H4-Cl-p)(2)(mu-dppm)(CO)(6) (1), (dppm = (C6H5)(2)PCH2P(C6H5)(2)), and a trace unexpected mixed-valence tetranucle ar molybdenum compound [(dppm)(CO)(2)Mo(mu-SC6H4-Cl-p)(2)Mo(O)](2)(mu-SC6H4 -Cl-p)(2)(mu-O) (2) were obtained from the reaction of Mo-2(mu-SC6H4-Cl-p)( 2)(CO)(8) with dppm in CH2Cl2. The crystal structures of the two compounds have been determined by X-ray diffraction studies, 1: monoclinic, P2(1)/n, a = 13.1082(3), b = 23.9584(4), c = 14.8510(2) Angstrom, beta = 105.865(1)d egrees, V = 4486.32(14) Angstrom(3), Z = 4, 9859 unique data, R-1 = 0.0805, wR(2) = 0.1076. 2 . CH2Cl2: monoclinic, C2/c, a = 22.0955(13), b = 19.1563 (11), c = 25.1981(14) Angstrom, beta = 112.243(1)degrees, V = 9871.9(1) Ang strom(3), Z = 4, 7053 unique data, R-1 = 0.0450, wR(2) = 0.1222. The cyclic voltammetry (CV) measurement for 1 showed a reversible two-electron transf er in a single step. (C) 1999 Elsevier Science S.A. All rights reserved.