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Two novel quino-aza-crown ethers, 1,22-diaza-3,6,17,20-diquino-7,10,13,16,25-pentaoxacyclotetracosane,1,22,25-triaza-3,6,17,20-diquino-7,10,13,16-tetraoxa-cycloheptacosane and theirs solid complexes with aluminium nitrate have been prepared.The two ligands investigated by 1H NMR, IR, and ESI-HRMS spectroscopy and the complexes were characterized by elemental analyses, molar conductivity and IR spectra.The fluorescence properties of Al(Ⅲ) complexes in solid were studied.