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One-step cyclization of a tetraazamacrocycle 5 with 70% yield in a 25-g scale was performed. Its chiral DOTA derivatives, L4 , has ∼93% of TSAP coordination isomer in its Eu(III) and Yb(III) complexes in aqueous solution. [GdL4]   5-  exhibits a high relaxivity, making it a promising and efficient MRI contrast agent. High luminescence dissymmetry factor ( g  lum ) values of 0.285 (Δ J = 1) for [TbL3]   -  and 0.241 (Δ J = 1) for [TbL4]   5-  in buffer solutions were recorded.

Synthesis of Water-Soluble Chiral DOTA Lanthanide Complexes with Predominantly Twisted Square Antiprism Isomers and Circularly Polarized Luminescence