Sample Originator: C. Sammon, E. S. Raper, R. Mansor, D. E. Hibbs, C. P. Constable and N. A. Bell.
Data Collection: Simon J. Colesa and Michael B. Hursthousea
Structure Determination: Simon J. Colesa and Michael B. Hursthousea.
University of Southamptona
C14H8HgN2S4
InChI=1/C14H9N2S4.C7H5NS2/c1-3-7-11-9(5-1)15-13(17-11)19-21-20-14-16-10-6-2-4-8-12(10)18-14;9-7-8-5-3-1-2-4-6(5)10-7/h1-8H;1-4H,(H,8,9)
| Identification Number: | 10.5258/ecrystals/97 |
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| Date Created: | 16 June 1997 |
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| Deposited On: | 21 Jan 2008 15:29 |
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| Deposited By: | A.N. Admin |
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Depositor Comments
Reactions of mercury(II) halides with 1,3-thiazolidine-2-thione (tzdSH) and benzo-1,3-thiazoline-2-thione (bztzSH) in aqueous ethanol produced the 1:2 complexes with the former ligand but, due to steric effects, only the previously described 1:1 complexes of the latter were isolated. Vibrational and 13C NMR spectral studies indicate η1-thione donation by the heterocyclic ligand and this has been confirmed by the crystal structure determination of (tzdSH)2HgBr2. The structure consists of pseudotetrahedral mercury (II) with longer C–S and shorter C–N bonds than in the free ligand and with the Br–Hg–Br angle being 20° smaller than the largest angle, S–Hg–S, around mercury due to deformation by inter- and intra-molecular interactions. The heterocyclic ligands are unsymmetrical round mercury relative to the two bromines. Reaction of the two thiones with mercury(II) acetate in ethanol in the presence of triethylamine results in deprotonation with the formation of the corresponding thionates. The former produced insoluble (tzdS)2Hg while the latter formed plate-like (bztzS)2Hg whose crystal structure showed linearity around mercury with digonal coordination via the thionate sulphur. The small Hg–S–C angle and HgN separation are indicative of a weak interaction between mercury and the nitrogen of the thioamide double bond.
Data collection parameters
| Chemical formula | C14 H8 Hg N2 S4 |
| Crystal morphology | |
| Crystal system | Monoclinic |
| Space group symbol | P2(1)/n |
| Cell length a | 11.817(2) |
| Cell length b | 5.9830(8) |
| Cell length c | 31.689(10) |
| Cell angle alpha | 90.00 |
| Cell angle beta | 97.34(4) |
| Cell angle gamma | 90.00 |
| Data collection temperature | 293(2) |
Refinement results
| Solution figure of merit | |
| R Factor (Obs) | 0.0459 |
| R Factor (All) | 0.0638 |
| Weighted R Factor (Obs) | 0.0963 |
| Weighted R Factor (All) | 0.0996 |
Citation: Sammon, C. and Raper, E. S. and Mansor, R. and Hibbs, D. E. and Constable, C. P. and Bell, N. A. and Coles, Simon J. and Hursthouse, Michael B. (1997) University of Southampton, Crystal Structure Report Archive. (doi:10.5258/ecrystals/97)
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