Two polytopic azoles, 1,4-bis(pyrazol-4-yl)benzene and 1,4-bis(tetrazol-5-yl)benzene, were prepared in sizable amounts by high yield syntheses employing, in mild conditions, cheap reactants and, whenever possible, aqueous Solutions. The two species were characterized by H-1 and (CNMR)-C-13 spectroscopy and by thermal analyses, the latter evidencing their high chemical and thermal stability. X-ray powder diffraction methods disclosed their non isomorphous crystal structures. in which individual molecules interact via hydrogen bonds to form two-dimensional sheets.