摘要 : Heteroleptic nickel pentacoordinate complexes with the macrocyclic ligands 2,4,4-trimethyl-1,5,9-triazacyclododec-1-ene (Me-3-mcN(3)) or its 9-methyl derivative (Me-4-mcN(3)), as ancillary ligands, and O,O'-(diphenylphosphineoxide... 展开 Heteroleptic nickel pentacoordinate complexes with the macrocyclic ligands 2,4,4-trimethyl-1,5,9-triazacyclododec-1-ene (Me-3-mcN(3)) or its 9-methyl derivative (Me-4-mcN(3)), as ancillary ligands, and O,O'-(diphenylphosphineoxide) amidate ligands, [RC(O)NP(O)Ph-2] (R = C6H6 (1), C5H4N (2), C4H3S (3)), have been prepared as well as related acetylacetonate derivatives. The complexes have been studied by spectroscopic methods (IR, UV-Vis and H-1 NMR). In acetone solution, the complexes exhibit isotropically shifted H-1 NMR resonances. The full assignment of these resonances has been achieved using one- and two-dimensional H-1 NMR techniques. The single-crystal structures of {(Me-4-mcN(3)) Ni[OP(Ph-2)NC(Tf)O]}[PF6] (9) and {(Me-3-mcN(3))Ni(acac)}[PF6] (10) have been established by X-ray diffraction. (C) 2008 Elsevier B. V. All rights reserved. 收起