The synthesis of new functionalized organotin-chalcogenide complexes was achieved by systematic optimization of the reaction conditions. The structures of compounds [(R1, 2Sn)3S4Cl] (1, 2), [((R 2Sn)2SnS4)2(μ-S)2] (3), [(R1, 2Sn)3Se4][SnCl3] (4, 5), and [Li(thf)n][(R3Sn)(HR3Sn)2Se 4Cl] (6), in which R1=CMe2CH2C(O)Me, R2=CMe2CH2C(NNH2)Me, and R 3=CH2CH2COO, are based on defect heterocubane scaffolds, as shown by X-ray diffraction, 119Sn NMR spectroscopy, and ESI mass spectrometry analyses. Compounds 4, 5, and 6 constitute the first examples of defect heterocubane-type metal-chalcogenide complexes that are comprised of selenide ligands. Comprehensive DFT calculations prompted us to search for the formal intermediates [(R1SnCl2) 2(μ-S)] (7) and [(R1SnCl)2(μ-S) 2] (8), which were isolated and helped to understand the stepwise formation of compounds 1-6. Twis-tin the night away: Six defect heterocubane-based organotin-chalcogenide complexes of the general formula [(RFSn)3E4Cl] (E=S, Se; RF= functionalized organic ligand) have been synthesized through a stepwise condensation route, for example, by addition of (Me3Si)2S to R1SnCl3 (A) to give 1 (1=[(R1Sn) 3S4Cl]; R1=CMe2CH 2C(O)Me)) and characterized by using X-ray diffraction, 119Sn NMR spectroscopy (see figure), and mass spectrometry (ESI). Two intermediates, [(R1SnCl2)2(μ-S)] and [(R1SnCl)2(μ-S)2] (see figure), were also isolated. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
CITATION STYLE
Eußner, J. P., Barth, B. E. K., Leusmann, E., You, Z., Rinn, N., & Dehnen, S. (2013). Functionalized organotin-chalcogenide complexes that exhibit defect heterocubane scaffolds: Formation, synthesis, and characterization. Chemistry - A European Journal, 19(41), 13792–13802. https://doi.org/10.1002/chem.201301521
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