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1996 (1)
1994 (1)
1Author    K. Yamada, K. Isobe, T. Okuda, Y. FurukawaRequires cookie*
 Title    Successive Phase Transitions and High Ionic Conductivity of Trichlorogermanate (II) Salts as Studied by 35C1 NQR and Powder X-Ray Diffraction  
 Abstract    A series o f trichlorogermanate(II) salts (AG eCl3, A = Rb, Cs, C H 3N H 3, and (C H 3)4N) have been synthesized and characterized by 35C1 N Q R , 35C1 N M R , AC conductivity, DTA, and X-ray diffrac­ tion techniques. In the temperature range studied two, two, five, and four phases were confirmed for the Rb, Cs, C H 3N H 3, and (C H 3)4N salts, respectively. From the 35C1 N Q R and structural data, isolated pyramidal G eC l3 anions were recognized in the low temperature phases. With increasing temperature the relaxation times of the 35C1 N Q R decreased exponentially and the signals disap­ peared far below the melting point. This suggests that the reorientation of the anion about the pseudo three-fold axis is excited. With further increase in temperature, the ionic conductivity of C H 3N H 3G eC l3 and (C H 3)4N G eC l3 increased drastically at the phase transitions to their cubic perovskite phases (C H 3N H 3G eC l3: a = 10-1 S m -1 at 400 K, (C H 3)4N G eC l3: a = 5 x 10-2 S m _1 at 420 K). The mobile ion was confirmed to be the chloride ion by means of 35C1 N M R and X-ray diffraction. 
  Reference    Z. Naturforsch. 49a, 258 (1994); received July 23 1993 
  Published    1994 
  Keywords    35C1 N Q R, 35C1 N M R, Ionic conductivity, Rietveld analysis, Phase transition 
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 TEI-XML for    default:Reihe_A/49/ZNA-1994-49a-0258.pdf 
 Identifier    ZNA-1994-49a-0258 
 Volume    49 
2Author    K. Yamada, T. Ohtani, S. Shirakawa, H. Ohki, T. Okuda, T. Kamiyama, K. OikawaRequires cookie*
 Title    Phase Transition of C 5 H 5 NHSbBr 4 Having a Hypervalent Bond: A 2 H NMR and X-Ray Diffraction Study* [Phase Transition of C 5 H 5 NHSbBr 4 l  
 Abstract    The second order phase transition at 253 K of pyridinium tetrabromoantimonate(III), C 5 H 5 NHSbBr 4 , has been characterized by means of X-ray diffraction and 2 H NMR. As was suggested from the 81 Br NQR spectra, the Rietveld refinements of the X-ray diffraction patterns at 297 K and 116 K confirm the structural change of the anion from SbBr 4 to SbBr 3 • Br -. The line shape analysis of the 2 H NMR using the deuterated analog revealed that the librational amplitude of the pyridinium ring about the axis normal to the plane increased with temperature and its rms amplitude reaching ca. 25° at T c . The librational motion may induce the phase transition breaking the hydrogen bonds of the type N-H -Br. However, nearest-neighbor 2n/6 jump or reorientation such as seen in benzene were not observed even at 350 K. 
  Reference    Z. Naturforsch. 51a, 739—744 (1996); received October 11 1995 
  Published    1996 
  Keywords    2 H NMR, 81 Br NQR, Rietveld analysis, Phase transition, Hypervalent bond 
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 TEI-XML for    default:Reihe_A/51/ZNA-1996-51a-0739.pdf 
 Identifier    ZNA-1996-51a-0739 
 Volume    51