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• W2019919118 abstract "The derivatized 19- and 20-membered macrocyclic thio crowns 3,6,9,12,15,18-hexathianonadecanol C13H26OS6 (19-aneS6-OH) (1) and 3,6,9,13,16,19-hexathiacycloicosanol C14H28OS6 (20-aneS6-OH) (2) have been synthesized by [1 + 1] cyclization in about 30% yield. The ligands 1 and 2 react readily at room temperature with different silver(I) salts in water and in organic solvents to form in quantitative yields the complexes [Ag(19-aneS6-OH)]+ (3) and [Ag(20-aneS6-OH)]+ (4) for which crystals of X-ray quality were grown by slow diffusion of diethylether into methanol. [Ag(19-aneS6-OH)][CF3SO3] crystallizes in the triclinic space group P1̄ with Z = 2, a = 10.760(1), b = 10.853(2) and c = 11.326(2)Å, and α = 78.73(1), β = 73.47(1), and γ = 74.99(1)°. [Ag(20-aneS6-OH)][BF4] also crystallizes in the triclinic space group P1̄ with Z = 4. The unit cell constants were determined with a = 10.076(4), b = 10.525(3), and c = 22.135(8)Å, α = 93.32(2), β = 102.43(2), and γ = 100.32(2)°. The complex cations [Ag(19-aneS6-OH)]+ and [Ag(20-aneS6-OH)]+ are coordinated through only four sulfur atoms; thus, a distorted tetrahedral coordination geometry is exhibited. In addition we found a highly asymmetric Ag−S bond lengths distribution throughout all complex cations. The stability constants of [Ag]+ with 1 and 2 and, for comparison with [18-aneS6] (5), have been determined in methanol by potentiometric [Ag]+ measurements. Log K values for the formation of 3, 4, and [Ag(18-aneS6]+ (6) are 12.04 ± 0.19, 11.49 ± 0.15, and 12.67 ± 0.13 respectively. Owing to a comparable macrocyclic effect, the similar log K values are reasonable but, since 6 coordinates octahedrally, not expected. 1H and 13C NMR investigations at various temperatures give evidence for fluxional coordinative behavior between all six sulfur atoms in solution. Consequently [Ag(19-aneS6-OH)]+, [Ag(20-aneS6-OH)]+, and [Ag(18-aneS6]+ seem to exhibit principally the same solution structures although the solid structures are very different." @default.
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• W2019919118 date "1996-01-01" @default.
• W2019919118 modified "2023-09-23" @default.
• W2019919118 title "Silver(I) Complexes of the Derivatized Crown Thioether Ligands 3,6,9,12,15,18-Hexathianonadecanol and 3,6,9,13,16,19-Hexathiaicosanol. Determination of Stability Constants and the Crystal Structures of [Ag(19-aneS6-OH)][CF₃SO₃] and [Ag(20-aneS6-OH)][BF₄]" @default.
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• W2019919118 doi "https://doi.org/10.1021/ic951421y" @default.
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