Two new pi-conjugated 1,3-dithiol-2-ylidene-containing ligands, 4,5-[1',4']dithiino[2',3'-b]quinoxaline-2-bis(2-pyridyl)methylene-1,3-dithiole (L(1)) and 4,5-bis(methylthio)-2-bis(2-pyridyl)methylene-1,3-dithiole (L(2)), have been synthesized and characterized. Using L(1), L(2), or dimethyl 2-[di(pyridin-2-yl)methylene]-1,3-dithiole-4,5-dicarboxylate (L(3)) as the auxiliary ligand and [(Tp)Fe(CN)(3)](-) or [(i-BuTp)Fe(CN)(3)](-) [Tp = tris(pyrazolyl)borate; i-BuTp = 2-methylpropyltris(pyrazolyl)borate] as the building block, two rectangular-square Fe(2)Ni(2) clusters [(Tp)Fe(CN)(3)Ni(L(1))(2)](2).2ClO(4).
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