Journal
JOURNAL OF THE CHEMICAL SOCIETY-DALTON TRANSACTIONS
Volume -, Issue 10, Pages 2112-2118Publisher
ROYAL SOC CHEMISTRY
DOI: 10.1039/b201611g
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CD3ND3GeCl3 has been studied by high-resolution neutron powder diffraction and H-2 NMR investigation over a wide temperature range to understand the static and dynamic structures and successive phase transitions. A monoclinic crystal of CD3ND3GeCl3 (Phase IV, space group P2(1)/n) undergoes a phase transition to an orthorhombic system (Phase III, Pnma) at 203 K where the symmetry of the anionic sublattice and the geometry of the N-D...Cl hydrogen bonds change. Furthermore, Phase III undergoes a phase transition to a trigonal system (Phase II, R3m) at 349 K where an orientational disorder of the cation is excited. Our Cl-35 NQR measurement also suggested an onset of the reorientation of the pyramidal GeCl3- anion just below the phase transition to Phase II with an activation energy E-a = 60.5 kJ mol(-1). However, a transition from Phase II to a cubic phase (Phase I, Pm3m), which was reported to be 396 K on the CH3NH3GeCl3, was not complete by 475 K. The Rietveld analysis at 475 K suggested that only 7% of the sample transformed to a cubic perovskite structure in which not only orientational disorder of the cation but also positional disorder of the chloride ion were confirmed, similar to CH3NH3GeCl3.
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