The complexation of Cd(II) by the tripodal ligand tris[(2-pyridyl)methyl]amine and dipodal ligand bis[(2-pyridyl)methyl]amine was investigated by solution-state NMR and X-ray crystallography. Cadmium coordination compounds exhibiting rarely observed solution-state NMR (1)H-(111/113)Cd satellites were characterized. The eight-coordinate complex [Cd(TMPA)(2)](ClO(4))(2).toluene (1) crystallizes in the triclinic space group P1 with a = 9.629(2) Å, b = 11.020(2) Å, c = 11.641(2) Å, alpha = 114.069(13) degrees, beta = 97.492(13) degrees, gamma = 91.034(14) degrees, and Z = 1. The average Cd-N(amine) distance is 2.53(4) Å and the average Cd-N(pyridyl) distance is 2.54(6) Å. The complex [Cd(BMPA)(NCCH(3))(OH(2))(OClO(3))][Cd(BMPA)(2)](ClO(4))(3).(CH(3)CN) (2) crystallizes in the triclinic space group P&onemacr; with a = 10.446(2) Å, b = 16.653(3) Å, c = 17.736(3) Å, alpha = 62.479(9) degrees, beta = 80.606(14) degrees, gamma = 84.66(2) degrees, and Z = 2. In the pseudo-octahedral monocation, the nitrogen-containing ligands occupy equatorial positions with Cd-N distances of 2.321(8), 2.283(7), and 2.263(8) Å for the amine, pyridyl (average) and acetonitrile nitrogens, respectively. Significant axial interactions occur with Cd-O bond distances of 2.313(7) Å (water) and 2.478(7) Å (perchlorate). In the pseudo-trigonal prismatic dication, the average Cd-N(amine) distances is 2.395(5) Å and the average Cd-N(pyridyl) distance is 2.362(8) Å. The solid-state structures and solution-state NMR trends were very similar to recently reported isovalent complexes of Hg(II), providing an exceptional opportunity to compare coupling constants of coordination compounds. Implications for the use of (111/113)Cd and (199)Hg NMR as metallobioprobes are discussed.
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