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Two guanidinate-based terbium complexes [iPrNC(NiPr 2 )-NiPr] m TbCl 3-m [m = 3 (1), 2 (2)] were synthesized, and the crystal structure of 1 was determined by single-crystal X-ray diffraction. Complexes 1 and 2 were further characterized by elemental analysis, IR, and 1 H NMR spectroscopy. In complex 1 the guanidinate ligand coordinates to the terbium atom through the nitrogen atoms in a bidentate chelating coordination mode. As a result of an efficient energy transfer

Addition of one equivalent of LiN(i‐Pr)2 or LiN(CH2)5 to carbodiimides, RNCNR [R=cyclohexyl (Cy), isopropyl (i‐Pr)], generated the corresponding lithium of tetrasubstituted guanidinates {Li[RNC(N R2′)NR](THF)}2 [R=i‐Pr, N R2′=N(i‐Pr)2 (1), N(CH2)5 (2); R=Cy, N R2′=N(i‐Pr) 2 (3), N(CH2)5 (4)]. Treatment of ZrCl4 with freshly prepared solutions of their lithium guanidinates provided a series of bis(guanidinate) complexes of Zr with the general formula Zr[RNC(N R2′)NR]2Cl2 [R=i‐Pr, NR2′=N(i‐Pr) 2 (5), N(CH2)5 (6); R=Cy, N R2′=N(i‐Pr)2 (7), N(CH2)5 (8)]. Complexes 1, 2, 5–8 were characterized by elemental analysis, IR and 1H NMR spectra. The molecular structures of complexes 1, 7 and 8 were further determined by X‐ray diffraction studies.

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