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

Fingerprint

X-Ray Diffraction
stannates
Activation energy
Crystal structure
Nuclear magnetic resonance
X ray diffraction
nuclear magnetic resonance
crystal structure
retraining
diffraction
Differential thermal analysis
activation energy
Hydrogen bonds
x rays
Salts
Phase transitions
Phase Transition
Single crystals
Hydrogen Bonding
thermal analysis

Keywords

  • Crystal structure spectroscopy
  • Molecular dynamics
  • Nuclear magnetic resonance

ASJC Scopus subject areas

  • Structural Biology
  • Organic Chemistry
  • Physical and Theoretical Chemistry
  • Spectroscopy
  • Atomic and Molecular Physics, and Optics

Cite this

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

In: Journal of Molecular Structure, Vol. 441, No. 1, 12.01.1998, p. 39-46.

Research output: Contribution to journalArticle

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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) {\AA}, V = 1182.0(7) {\AA}3 for the stannate, and a = 9.072(4), b = 11.399(5), c = 11.63(2) {\AA}, V = 1203(3) {\AA}3 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.",
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T1 - 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

AU - Sato, Setsuko

AU - Ishida, Hiroyuki

AU - Nagae, Makoto

AU - Kashino, Setsuo

AU - Furukawa, Yoshihiro

AU - Weiss, Alarich

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N2 - 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.

AB - 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.

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