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Dedicated to Professor N. S. Zefirov on the occasion of his 70 th birthday (Abstract The synthesis and characterization of a series of cross-conjugated oligo(phenylene enynylene)s via the Sonogashira protocol is reported. The structural properties of these oligomers have been established by 1 H and 13 C NMR and IR spectroscopies, as well as mass spectrometry. Their electronic absorption and emission behavior has been investigated via UV/Vis and fluorescence spectroscopy. The results of thisdoi:10.3998/ark.5550190.0006.411 fatcat:vmarla254vgmjkwhaa4uypfb7m