Among the Ln[15MC CuRha -5] metallacrowns (MC; Rha = R-substituted hydroximate ligands), the simple glycinehydroximate (Glyha) complex is presented as the primary model for studying various aspects of the guest interaction with the Ln III ion. We report a one-pot synthesis of several glycinehydroximate LnL[15MC CuGlyha -5] derivatives in the presence of calcium compounds. The complexes with biden-II Glyha -5](NO 3 ) 2 (3), and biden-[a] G.A. Razuvaev 5202 tate lactate Gd(CH 3 CHOCOO)[15MC Cu II Glyha -5]Cl 2 [4(Gd)]have been prepared and characterized by X-ray analysis. The lactate was chosen as an example of the essential oxyanions that exist as metabolites in all living organisms. We examined the lanthanide-induced NMR spectroscopy shifting ability of a series of lactate 4(Ln) metallacrown complexes (Ln = La, Y, Ce, Pr, Nd, Sm, Eu, Gd, Tb, or Dy). The corresponding Gd III complex was characterized by 1 H NMR spectroscopy relaxometric techniques in aqueous media. II Glyha -5](NO 3 ) 2 can be easily prepared by a onepot method in the presence of calcium compounds. [15] Herein, we have developed this synthetic strategy when pre-Scheme 2. Synthetic pathway to nitrate 1.

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