Two novel guanidinium iodoantimonate(III) and iodobismuthate(III) crystals, [C(NH2)3]3[Sb2I9] and [C(NH2)3]3[Bi2I9], have been synthesized and their structures have been determined by means of single-crystal x-ray diffraction studies at three temperatures (293, 348 and 362 K). Both compounds appeared to be isomorphous in corresponding phases. The crystal structure of the title compounds is composed of discrete M2I93− (M = Sb, Bi) anions and C(NH2)3+ guanidinium cations. A non-equivalence of two guanidinium cations has been found. Both guanidinium analogs exhibit a rich sequence of phase transitions. In Gu3Sb2I9, three solid–solid structural phase transformations of the first order type are detected at 119/121, 341/344 and 355/362 K (on cooling/heating) by the DSC and dilatometric techniques. Gu3Bi2I9 displays four first order phase transitions: 179/185, 202/215, 287/291 and 358/368 K. The low temperature phases appear to have ferroic (ferroelastic) properties. The prototypic paraelastic phase for both compounds belongs to hexagonal symmetry (space group P63/mmc). The dielectric response has been measured in a wide frequency region (100 Hz–1 MHz), but no dielectric dispersion has been detected. Possible mechanisms of the phase transitions in Gu3M2I9 (M = Sb, Bi) are discussed on the basis of the presented results.

Diisobutylammonium bromide is found to be a unique improper ferroelastic in which the elastic degrees of freedom seem to play the essential role, giving rise to a domain pattern resembling that of martensitic phase transitions. A weak canted ferroelectricity turns out switchable by an electric field.

The results of dielectric relaxation spectroscopy and polarizing microscope observation of the 4'-butyl-4-(2-methylbutoxy)azoxybenzene (abbreviated as 4ABO5*) are presented. Numerical analysis of the dielectric spectra results points to complex dynamics of 4ABO5* molecules in isotropic, cholesteric, and crystalline phases. Two well-separated maxima on the imaginary part of dielectric permittivity and the third low frequency relaxation process, hidden in the conductivity region, were detected and described in cholesteric and crystalline phases. Temperature dependence of mean relaxation times characterizing flip-flop motions and rotation around long axes, observed in all phases, is of the Arrhenius type.

Two hybrid crystals imidazolium iodoantimonate(iii) and iodobismuthate(iii) have been synthesized and characterized in a wide temperature range (100–350 K) by means of X-ray diffraction, dielectric spectroscopy, proton magnetic resonance, FT-IR spectroscopy and optical observations.

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