Structural assignment and molecular order of three-ring mesogen by 13C NMR spectroscopy in mesophase

Autor: Mandadhi Guruprasad Reddy, Nitin P. Lobo, T. Narasimhaswamy
Rok vydání: 2016
DOI: 10.6084/m9.figshare.3099673
Popis: A homologous series of rod-like molecules with three phenyl rings in the core and terminal alkoxy chains are synthesised from mesogenic two-ring aldehyde by coupling with non-mesogenic 4-alkoxy anilines. The mesophase properties are evaluated with hot-stage optical polarising microscopy and differential scanning calorimetry, and accordingly, all the molecules exhibited enantiotropic nematic and smectic C phases along with monotropic low-temperature smectic phases. For a representative homologue, the existence of smectic C phase is further confirmed by noticing a sharp reflection at small angle region in powder X-ray diffraction which varies with change in temperature. The main focus of the investigation, however, is the clear demonstration of chemical shift assignment of static 13C NMR of a representative three-phenyl ring mesogen in smectic C phase. In this novel approach, the static 13C NMR spectral data of synthetic mesogenic intermediate namely two-ring aldehyde are utilised for the chemical shift assignment of three-ring mesogens. Further, the orientational order parameter of two-ring aldehyde in smectic A and three-ring mesogen in smectic C phase is carried out by measuring the 13C-1H dipolar couplings by 2D separated local field spectroscopy.
Databáze: OpenAIRE