trans-Bis[(thiocyanato-S)(1-methylimidazoline-2(3H)-thione)-μ2-(1-methylimidazoline-2(3H)-thione)copper(I)]: preparation, thermal analysis and crystal structure |
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Authors: | Eric S. Raper |
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Abstract: | 1-Methylimidazoline-2(3H)-thione (mimtH) and copper(I) thiocyanate in refluxing ethanolacetonitrile produce a colourless, diamagnetic complex, [Cu2(mimtH)4(SCN)2], which crystallises in an orthorhombic cell (a=8.0724(3), b=15.9545(6), c=21.3357(8) Å), space GROUP=Pbca, Z=4, final R=0.0319 from 2427 observed reflections F>4σc(F)). In the dimeric complex the copper(I) atoms are pseudo-tetrahedrally coordinated by pairs of, respectively, asymmetrically μ2-S bridging mimtH, terminal monodentate-S mimtH, (Cu---S=2.290(1) Å), and terminal monodentate-S thiocyanate, (Cu---S=2.332(1) Å). Each pair of ligands is trans-related to its partner across crystallographic centres of symmetry, consequently, each copper(I) atom has an identical S4 donor set with angles at the metal ranging from 95.9(1)° to 121.8(1)°. The centro-symmetric Cu2S2 core is rhomboid with Cu---S=2.377(1) and 2.457(1) Å, Cu---Sbr---Cu=72.6(1)° and Cu---Cu, Sbr---Sbr separation distances of 2.861(1) and 3.897(2) Å, respectively. Thermal decomposition of the complex in flowing air, (133–1000 °C), involves de-sulfurisation of mimtH and thiocyanate with concomitant production of copper(II) sulfide followed by oxidation to copper(II) oxide. |
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