1 H, 13 C and 77 Se NMR study of tetraselenafulvalene derivatives supported by novel H(Se)C and H(C)Se triple‐resonance experiments at natural abundance

A series of substituted tetraselenafulvalenes (TSeFs) was studied in solution using 1 H, 13 C and 77 Se NMR spectroscopy. Chemical shifts and heteronuclear coupling constant values were determined and assigned. Novel two‐dimensional H(Se)C and H(C)Se triple‐resonance correlation experiments were applied at natural abundance in order to accomplish 13 C and 77 Se signal assignments. Using this approach, all the signals were unambiguously assigned and atom connectivity was established in the studied TSeF derivatives. These experiments, allowing signal assignments of quaternary carbons, may find wide application in the study of substituted TSeF and other organoselenium compounds. To the best of our knowledge, triple‐resonance experiments with proton detection have been applied to organoselenium compounds for the first time. Copyright © 2007 John Wiley & Sons, Ltd.