A series of poly(p-ethynylbenzoate esters) synthesized using group 6 metal catalysts was investigated with respect to substituent variation and their effect on film behavior at the air–water interface. The increase in length and stiffness of the lateral substituent has the effect of decreasing the trans isomer content as well as the pure configurational sequences of the chain microstructure for this particular catalyst system. The polymers essentially retain their configuration and conformation upon formation. This has a consequence on their film behavior at the air–water interface in which only minor local conformational changes are observed using the Langmuir–Blodgett technique. The presence of a long alkyl chain length attached terminal to the substituent enhances this behavior.
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