Despite the fact that lead poisoning is the most common disease of environmental origin in the United States, the spectroscopic properties of aqueous Pb(II) coordination compounds have not been extensively investigated. Spectroscopic techniques that can be used to probe the fundamental coordination chemistry of Pb(TI) will aid in both the development of water-soluble ligands that bind lead both tightly and selectively and the characterization of potential biological targets. Here, we report the preparation and characterization of a series of Pb(II) complexes of amido derivatives of EDTA. The Pb-207, chemical shift observed in these complexes (2441, 2189, and 1764 ppm for [Pb(EDTA)](2-) Pb(EDTA-N-2), and [Pb(EDTA-N-4)](2+), respectively) provides an extremely sensitive measure of the local environment and the charge on each complex. These shifts help to map out the lead chemical measure of the local environment shift range that can be expected for biologically relevant sites. In addition, we report the first two-dimensional Pb-207-H-1 heteronuclear multiple-quantum correlation (HMQC) nuclear magnetic resonance spectra and demonstrate that this experiment can provide useful information about the lead coordination environment in aqueous Pb(II) complexes. Because this technique allows Pb-207-H-1 couplings through three bonds to;be identified readily, Pb-207-H-1 NMR spectroscopy should prove useful for the investigation of Pb(II) in more complex systems (e.g., biological and environmental samples).