Dedicated to Professor Ernst Fischer on the occasion of his 65th birthdayThe discotic liquid crystalline phase of a new class of disc-like molecules (hexa-O-alkanoylscyllo-inositoles) is studied by small angle X-ray scattering, DSC and optical observations. Comparison of these three methods allows the determination of the structural arrangement. X-ray film exposures of oriented samples clearly demonstrate the hexagonal columnar ordered type of mesophases. A simple model calculation shows that the alkyl chains of neighbouring columns interpenetrate each other to a small extent.
IntroduetionThe different ways in which disc-like molecules can be arranged in the discotic mesomorphic state have recently been the subject of many investiga- [2], The series of hexa-O-alkanoyl-scyllo inositoles (HASI) is of interest because disc-like molecules with alicyclic saturated cores were recently found to form discotic phases [3,10]. The aim of this paper was to study various parameters of the mesogenic phases of those compounds. Especially the intercore distance d of the columns, the temperature dependence of d and the influence of the alkyl chain lengths on the mesomorphic behaviour have been measured.
ExperimentalThe compounds of the homologous series of HASI (alkyl chain length from n = 5 to n = 11) were synthesized and puriFied as described elsewhere [3,9]. The samples were filled in Lindemann capillaries (diameter 1 mm) and then placed into a tight-fitting rectangular brass holder (20 x 5 x 2 mm). The orientation was performed using a magnetic Field strength up to 2.4 Tesla in a Drusch electromagnet. The temperature and cooling rate (0.2 K/min) was controlled by a modified Mettler FP 52 heating stage (all magnetic materials have been replaced by aluminium). The direction of the magnetic field was perpendicular to the long axis of the capillary. The X-ray measurements were performed using small angle cameras of the type Kratky-Compact (A. Paar, Graz, Austria) and Kiessig (Seifert, Ahrensburg, FRG). We used film registration and detection by a curved linear position sensitive proportional counter PSPC (M. Braun. Munich) with an active length of 50 mm and a low flux of a mixture of 75% argon and 25% methane under a pressure of 11 bar. In order to calibrate the detector, the scattering curve of a cadmium-distearate multilayer (35 double layers) has been recorded at room temperature before each measurement. This calibration sample was prepared on a glass rod of 2 mm diameter using the Blodgett technique [4], Its diffraction pattern consists of sharp reflections with a First order period of d= (5.03 ± 0.01) nm [5], Ni-Filtered Cu-radiation was used. The temperature in the Kratkycompact camera was controlled by an electronic heating stage (A. Paar, Graz, Austria) with a relative accuracy of ± 0.02 K. In the Kiessigcamera we used a thermostated water flow cell with 0932-0784 / 87 / 0600-0611 S 01.30/0. -Please order a reprint rather than making your own copy.