Cationic motions and crystal structures of 1,3,5-trimethylpyridinium hexachlorometallates [(CH3)2C5H3N(CH3)]2MCl6 (M is SN and Te) studied by 1H NMR and X-ray diffraction

Setsuko Sato, Hiroyuki Ishida, Makoto Nagae, Setsuo Kashino, Yoshihiro Furukawa, Alarich Weiss

Research output: Contribution to journalArticle

4 Citations (Scopus)

Abstract

The crystal structure of 1,3,5-trimethylpyridinium hexachlorometallates [(CH3)2C5H3N(CH3)]2MCl6 (M is Sn and Te) were determined at 298 K and found to be orthorhombic Pnnm (No. 58) and Z = 2, a = 8.996(2), b = 11.330(2), c = I 1.596(2) Å, V = 1182.0(7) Å3 for the stannate, and a = 9.072(4), b = 11.399(5), c = 11.63(2) Å, V = 1203(3) Å3 for the tellurate, by single-crystal X-ray diffraction. No phase transition was detected by DTA from 80 to 573 K. The cationic motions were studied by 1H NMR and the C3 reorientation of the CH3 groups was observed below 273 K, having an activation energy of 3.1 kJ mol-1 for the stannate and 3.7 kJ mol-1 for the tellurate. Another cationic motion, with an activation energy of about 20 kJ mol-1, was observed above 380 K for both salts. This is attributable to the pseudo-C3 reorientation around the axis perpendicular to the pyridinium ring. The cationic motions and the crystal structure are discussed from the point of view of the hydrogen bonding.

Original languageEnglish
Pages (from-to)39-46
Number of pages8
JournalJournal of Molecular Structure
Volume441
Issue number1
DOIs
Publication statusPublished - Jan 12 1998

Keywords

  • Crystal structure spectroscopy
  • Molecular dynamics
  • Nuclear magnetic resonance

ASJC Scopus subject areas

  • Analytical Chemistry
  • Spectroscopy
  • Organic Chemistry
  • Inorganic Chemistry

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