Phenyl-substituted 'push-pull'diacetylenes If and lg have been prepared by acetylation and henzoylation of the appropriate lithiodiynylamines 4 (Scheme 2). 13C-NMR spectra of diacetylenes la-g (Table I) are discussed with respect to the expected polarisation of the diacetylene unit by 'push 'and 'pull'substituents. X-Ray investigations of lc, le, and If have been performed in view of the planned solid-state polymerisation of 'push-pull' ...