The compounds 5(2-thienyl)-and 5(3-thienyl)-dipyrromethane (1 and2, respectively) have been synthesized and isolated from the acid-catalyzed reaction between thiophenes-carboxaldehyde and pyrrole. Characterization by X-ray diffraction confirms molecular structures involving twoortho-substituted pyrrolyl and one thienyl groups. Both the compounds1 and2 were crystallized in the monoclinic space groupP2(1)/n with cell parametersa = 5.7149(16) angstrom, b = 17.338(6) angstrom, and c = 11.785(4) angstrom, beta = 98.466(9)degrees,V = 1155.0(6) angstrom(3) for compound1; and a = 5.828(4) angstrom, b = 17.424(10) angstrom, c = 11.822(8) angstrom, beta = 98.10(2)degrees, and V = 1188.4(13) angstrom(3) for compound 2.