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Complex formation of two novel polytopic mono- and bis- crown-containing 4-styryl bipyrydines 1 and 2 with Zn2+ and Ca2+ in MeCN was studied by absorption and emission spectroscopy, 1-D and 2-D 1H-NMR spectroscopy, ESI-mass spectrometry. Two binding centers of different nature in ligands 1 and 2 exhibit specific affinity to different metal cations. The crown ether moieties prefer to bind with alkaline, alkaline-earth metal cations, the bipyrydine moiety binds with heavy and transition metal ions.