New diorganolead(IV) sulfanylpropenoates: Synthesis, characterization and analysis of their evolution in DMSO solution

Casas, José S.; Castaño, Marı́a V.; Couce, Marı́a D.; Sánchez, Agustı́n; Sordo, José; Torres, Marta; López, Esperanza

doi:10.1016/j.jorganchem.2015.04.036

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“…1.3 intensity ratio, which is close to the statistical distribution (3:2) of the meridional and facial geometric isomers of an octahedral Ph 3 Pb(OOH)(DMSO) 2 complex (Figures e and S1b). Such coordination of DMSO solvent molecules with triphenyl and diphenyl lead(IV) was previously reported in the presence of chloride, sulfanylpropenoate, , and 9 H -3-thia-1,4a,9-triaza-fluorene-2,4-dithione ligands . The 1 H NMR spectrum of 1 in a DMSO solution exhibits a sharp signal at 8.76 ppm corresponding to the proton of the OOH ligand.…”

Section: Resultssupporting

confidence: 71%

Triphenyllead Hydroperoxide: A 1D Coordination Peroxo Polymer, Single-Crystal-to-Single-Crystal Disproportionation to a Superoxo/Hydroxo Complex, and Application in Catalysis

et al. 2022

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The synthesis, transformation, and application in catalysis of triphenyllead hydroperoxide, the first dioxygen lead complex, are described. Triphenyllead hydroperoxide is characterized by 207Pb nuclear magnetic resonance (NMR), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and single-crystal X-ray diffraction, revealing the first one-dimensional (1D) coordination peroxo polymer. Photolytic isomorphous transformation of Ph3PbOOH yields a mixed hydroxo/superoxo crystalline structure, the first nonalkali superoxo crystalline metal salt, which is stable up to 100 °C. Upon further photolysis, another isomorphous transformation of the superoxide to hydroxide is observed. These are the first single-crystal-to-single-crystal hydroperoxide-to-superoxide and then to hydroxide transformations reported to date. Photolysis of triphenyllead hydroperoxide yields two forms of superoxide-doped crystalline structures that are distinguished by widely different characteristic relaxation times. The use of Ph3PbOOH as an easy-to-handle solid two-electron oxidant for the highly enantioselective epoxidation of olefins is described.

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