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Crystal Structure, and the Infrared and Raman Spectra, of Tripotassium Methanetrisulphonate Hydrate, K3.H2O

DOI: 10.1039/DT9800000149

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 149 - 155 (1980)

Update date:2022-08-04

Topics:

Authors:

Hall, John R.Hall, John R.

Johnson, Robert A.Johnson, Robert A.

Kennard, Colin H. L.Kennard, Colin H. L.

Smith, GrahamSmith, Graham

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Article abstract of DOI:10.1039/DT9800000149

The crystal structure of the title compound has been determined using three-dimensional X-ray diffraction data, from 839 reflections; crystals are orthorhombic, space group P212121, with unit-cell dimensions a=9.405(1), b=9.405(1), c=12.321(1) Angstroem, Z=4.The structure has been solved using direct methods and refined by full-matrix least squares to R 0.045.The S-C-S angles (ca. 113 deg) indicate an expansion from tetrahedral stereochemistry and the S-C bond lengths (ca. 1.81 Angstroem) are appreciably longer than those for K2 (1.77 Angstroem) and Ca2 (1.75 Angstroem).The i.r. (4 000-50 cm-1) and Raman spectra of K3.H2O and K3.D2O at 77 K are reported and interpreted according to the crystal structure.To assist with the assignment, spectra of the anhydrous salt, K3, and of aqueous solutions of the soluble lithium salts, have also been recorded.The SO3 groups show their characteristic group frequencies: νsym(C-S) and νasym(C-S) are assigned to 762 and 820 cm-1, respectively; δsym(CS3) and δasym(CS3) to 170 and ca. 210 cm-1, respectively.I.r. spectra of samples containing the isotopically dilute HDO species confirm the presence of two types of hydrogen bond per water molecule.

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