60147-18-4Relevant academic research and scientific papers
THIOPHENOPHANE-METAL COMPLEXES. I. PREPARATION, X-RAY STRUCTURE, AND CYCLIC VOLTAMMETRY OF 2,5,8-TRITHIA(2,5)THIOPHENOPHANE, L, AND OF ITS METALCOMPLEXCATION BIS(2,5,8-TRITHIA(2,5)THIOPHENOPHANE-S2,S3)COPPER(I), +1
Lucas, C. Robert,Shuang, Liu,Newlands, Michael J.,Charland, Jean-Pierre,Gabe, Eric J.
, p. 1506 - 1512 (2007/10/02)
Preparation of the thiophenophane C10H14S4. (L), and syntheses of its copper(I) complex ClO4 or BF4 are described.The 13C and 1H nmr spectra of L and the ir spectra (4000-200 cm-1) of ClO4 and BF4 are reported.The molecular structures of L and ClO4 have been determined.For L: space group P21/a, a=7.9347(2) Angstroem, b=18.7479(3) Angstroem, c = 8.8596(2) Angstroem, β = 108.446(2) deg, Z = 4, Rf = 0.048, and Rw = 0.034.For ClO4; space group P21/c, a=9.4363(1) Angstroem, b = 18.2768(3) Angstroem, c = 16.2157(3) Angstroem, β = 96.520(2) deg, Z = 4, Rf = 0.056, and Rw = 0.037.The Cu(I)complex has distorted tetrahedral coordination geometry; its perchlorate anion is non-coordinating and disordered.The Cu-S bond lengths lie in the range 2.301-2.392 Angstroem and the S-Cu-S angles in the range 92.43-150.26 deg.Cyclic voltammetry of ClO4 (1E-3 mol/L in dimethylsulfoxide, 0.1 mol/L Et4NClO4, glassy carbon working electrode, platinum counter electrode, aqueous saturated calomel reference electrode against which the ferrocenium/ferrocene potential under similar conditions was 400 mV) shows a quasi-reversible oxidation (E1/2 = 0.150 V, ΔEp = 170 mV at 50 mV/s).Thiophene's effect as a sub-unit in a small macrocycle upon properties of the latter is discussed.
