Synthesis and Stereochemistry of Thiacrown Ethers with Unsaturated Bonds

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• Compound 2 crystallized in the triclinic space group P-1, with a = 5.235(9), b = 10.422(19), c = 12.33(2) Å, α = 104.39(2), β = 93.69(2), γ = 100.46(2)o, V = 636.2(19) Å3, Z = 2, and Dc = 1.380 g cm−3. 2788 data collected with Mo-Kα radiation (λ = 0.71070 Å) and Fo > 2.0σ (I) were used in the least-squares refinement to yield R = 0.0522, R w = 0.1246
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• Compound 1,2-alternate- 4 crystallized in the monoclinic space group P21/n, with a = 7.234(2), b = 9.968(3), c = 19.387(5) Å, β = 98.563(5)o, V = 1382.4(7) Å3, Z = 2, and Dc = 1.425 g cm−3. 7519 data collected with Mo-Kα radiation (λ = 0.71073 Å) and Fo > 2.0σ (I) were used in the least-squares refinement to yield R = 0.105, R w = 0.284
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• Cyclic voltammograms were measured in acetonitrile. A 0.1 M solution of tetra-n-butylammonium perchlorate was used as supporting electrolyte solution. The samples were added and dissolved in this solution to yield 0.5 mM concentrations of the respective materials. Cyclic voltammograms were recorded at scan rate of 100 mVs−1. Formal oxidation potentials are given versus the reference system ferrocene/ferrocenium (Fc/Fc+) in volts
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