0000000000009908

AUTHOR

Barbara M. Schmidt

Dimeres und Trimers 1-Methyl-1-aza-5-stannabicyclo[3.3.01,5]-octan sulfid [MeN(CH2CH2CH2)2SnS]n, Röntgenstrukturanalyse des Dimeren und Gleichgewicht Dimer-Trimer gemäß 119Sn-NMR und FD-Massenspektrometrie

Abstract The crystal structure of the dimeric title compound has been determined and refined to R = 0.0266. The core of the nearly centrosymmetric dimer is formed by an almost perfect [SnS]2 rectangle (Sn-S 2.39 and 2.51 A). The two sulfur atoms of this rectangle establish the connecting edge of two distorted trigonal bipyramids around the two tin atoms (Sn … N 2.55 A). Solutions of the title compound contain in addition to the dimer (σ(119Sn) = −4.6 ppm) about 20% of the trimer (+ 10.3 ppm). By quick crystallization a mixture of both oligomers can be transferred into the solid state.

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Über blei-haltige Heterocyclen

Abstract Crystal structures of alternating six-membered rings [Ph2PbS]3-P21/c and [Ph2SnS]3-P21/n have been determined by X-ray methods. Both heterocycles exhibit a C2-symmetric twisted boat conformation with tetrahedral coordination of the metal atoms [dPbS 2.491 A (dSnS 2.401 A, dPbC 2.19 A (dSnC 2.129 A)]. No additional intermolecular contacts have been found. A ring-segment exchange reaction in solution has been observed by NMR. In the resulting equilibrium new cyclic compounds containing both tin and lead atoms with coupling constants 2J(207PbS119Sn) 226 Hz have been detected. FD-mass spectra indicate formation of dimeric molecular units.

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Über bismut-haltige heterocyclen

Abstract Methyl and phenyl oxadithia and trithiabismocanes have been synthesized from methyl or phenyl diethoxybismutane and the respective dithiol. The light-sensitive compounds have been investigated by mass, vibrational and 13C NMR spectra: ν(BiMe) 470–460, ν(BiS2) 300–240 cm−1; δ(13Me) −12 ppm. The crystal structure of 5-phenyl-1,4,6,5-oxadithiabismocane has been determined (R = 0.056). The eight-membered ring has the chair-chair conformation. Besides three direct bonds (BiPh 225(2), BiS 256.0(2) and 260.2(3) pm) there are one transannular (Bi⋯O 297(1) and two intermolecular contacts (Bi ⋯S 344.0(3) and 350.9(3) pm) to bismuth in resulting a ψ-monocapped octahedral sphere of coordina…

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