Linear dichroism and second‐harmonic generation (SHG) have been measured in Langmuir‐Blodgett (LB) multilayers of Z‐type structure of amphiphilic indandione‐1,3 pyridinium betaine (IPB) with an aliphatic tail containing 17 carbon atoms (C17IPB). The dichroic ratio As/Ap of electronic absorption of s‐ and p‐polarised light and the SHG intensity show that the ‘heads’ of C17IPB molecules are predominantly oriented along the deposition direction of monolayers on a quartz substrate. Orientation parameters and mean statistical azimuthal and tilt angles are evaluated as a function of the number of monolayers. The SHG efficiency has been measured in C17IPB monolayers on a water surface as a function of surface pressure. The effective hyperpolarisability β of the IPB molecule has been determined experimentally in a chloroform solution by the hyper‐Rayleigh‐scattering method. The obtained value of β = (138 ± 16) × 10−30 esu is in good agreement with theoretical estimates.
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