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手性镍（II）配合物与三脚架配体三[2-(((2-苯基咪唑-4-基)亚甲基)氨基)乙基]胺的合成、表征及自发拆分

Synthesis, characterization, and spontaneous resolution of chiral nickel(II) complexes with the tripod ligand tris[2-(((2-phenylimidazol-4-yl)methylidene)amino)ethyl]amine.

作者信息

Katsuki I, Matsumoto N, Kojima M

机构信息

Department of Chemistry, Faculties of Science, Kumamoto University, Kurokami 2-39-1, Kumamoto 860-8555, Japan.

出版信息

Inorg Chem. 2000 Jul 24;39(15):3350-4. doi: 10.1021/ic9909025.

DOI:10.1021/ic9909025
PMID:11196874
Abstract

The chiral nickel(II) complexes of a tripod-type ligand with the chemical formulas Ni(H3L)2.MeOH (1), Ni(H3L)2.MeOH (2), and Ni(H3L)2.6H2O (3) were synthesized and characterized (H3L = tris[2-(((2-phenylimidazol-4-yl)methylidene)amino)ethyl]amine). The crystal structures of 1-3 were determined by their single-crystal X-ray analyses. 1, C37H40N12O7Ni: orthorhombic, P2(1)2(1)2(1); a = 14.198(2) A, b = 22.422(2) A, c = 12.019(2) A, Z = 4. 2, C37H40N10O9Cl2Ni: orthorhombic, P2(1)2(1)2(1); a = 14.206(2) A, b = 22.735(3) A, c = 12.696(3) A, Z = 4. 3, C50H58N10O10Ni: triclinic, P1; a = 14.191(5) A, b = 16.048(4) A, c = 13.692(4) A, alpha = 115.25(2) degrees, beta = 111.07(3) degrees, gamma = 64.75(2) degrees, Z = 2. Each complex has an octahedral coordination environment for the nickel(II) ion, formed by the six nitrogen donor atoms, and is either a delta (clockwise) or a lambda (anticlockwise) enantiomorph, depending on the screw arrangement of the tripod-type ligand around the nickel(II) ion. The circular dichroism (CD) spectrum of a powdered sample of a crystal of 1 showed a positive and a negative peak at 915 and 630 nm, respectively, and that of another crystal showed an enantiomeric pattern. The observation of the Cotton effect and the crystal structure provided evidence for spontaneous resolution of the chiral complex molecule.

摘要

合成并表征了化学式为Ni(H3L)2·MeOH (1)、Ni(H3L)2·MeOH (2) 和 Ni(H3L)2·6H2O (3) 的三脚架型配体的手性镍(II)配合物（H3L = 三[2-(((2-苯基咪唑-4-基)亚甲基)氨基)乙基]胺）。通过单晶X射线分析确定了1 - 3的晶体结构。1，C37H40N12O7Ni：正交晶系，P2(1)2(1)2(1)；a = 14.198(2) Å，b = 22.422(2) Å，c = 12.019(2) Å，Z = 4。2，C37H40N10O9Cl2Ni：正交晶系，P2(1)2(1)2(1)；a = 14.206(2) Å，b = 22.735(3) Å，c = 12.696(3) Å，Z = 4。3，C50H58N10O10Ni：三斜晶系，P1；a = 14.191(5) Å，b = 16.048(4) Å，c = 13.692(4) Å，α = 115.25(2)°，β = 111.07(3)°，γ = 64.75(2)°，Z = 2。每个配合物中镍(II)离子具有八面体配位环境，由六个氮供体原子形成，并且根据三脚架型配体围绕镍(II)离子的螺旋排列，它要么是δ（顺时针）对映体，要么是λ（逆时针）对映体。1的晶体粉末样品的圆二色性(CD)光谱在915和630 nm处分别显示一个正峰和一个负峰，另一个晶体的光谱显示出对映体模式。科顿效应的观察和晶体结构为手性配合物分子的自发拆分提供了证据。

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