Smith Sarah J, Noble Christopher J, Palmer Randahl C, Hanson Graeme R, Schenk Gerhard, Gahan Lawrence R, Riley Mark J
School of Molecular and Microbial Sciences, The University of Queensland, St Lucia, QLD 4072, Australia.
J Biol Inorg Chem. 2008 May;13(4):499-510. doi: 10.1007/s00775-007-0334-7.
A binuclear copper complex, [Cu2(BPMP) (OAc)2][ClO4] x H2O, has been prepared using the binucleating ligand 2,6-bis[bis(pyridin-2-ylmethylamino)methyl]-4-methylphenol (H-BPMP). The X-ray crystal structure reveals the copper centers to have a five-coordinate square pyramidal geometry, with the acetate ligands bound terminally. The bridging phenolate occupies the apical position of the square-based pyramids and magnetic susceptibility, electron paramagnetic resonance (EPR) and variable-temperature variable-field magnetic circular dichroism (MCD) measurements indicate that the two centers are very weakly antiferromagnetically coupled (J = -0.6 cm(-1)). Simulation of the dipole-dipole-coupled EPR spectrum showed that in solution the Cu-O-Cu angle was increased from 126 degrees to 160 degrees and that the internuclear distance was larger than that observed crystallographically. The high-resolution spectroscopic information obtained has been correlated with a detailed ligand-field analysis to gain insight into the electronic structure of the complex. Symmetry arguments have been used to demonstrate that the sign of the MCD is characteristic of the tetragonally elongated environment. The complex also displays catecholase activity (k(cat) = 15 +/- 1.5 min(-1), K(M) = 6.4 +/- 1.8 mM), which is compared with other dicopper catechol oxidase models.
已使用双核配体2,6-双[双(吡啶-2-基甲基氨基)甲基]-4-甲基苯酚(H-BPMP)制备了双核铜配合物[Cu2(BPMP)(OAc)2][ClO4]·xH2O。X射线晶体结构表明铜中心具有五配位的四方锥几何构型,乙酸根配体以端基形式配位。桥连酚氧占据四方锥的顶端位置,磁化率、电子顺磁共振(EPR)和变温变场磁圆二色性(MCD)测量表明两个中心存在非常弱的反铁磁耦合(J = -0.6 cm-1)。对偶极-偶极耦合EPR谱的模拟表明,在溶液中Cu-O-Cu角从126°增加到160°,且核间距大于晶体学观测值。所获得的高分辨率光谱信息已与详细的配体场分析相关联,以深入了解该配合物的电子结构。已使用对称性论据证明MCD的符号是四方拉长环境的特征。该配合物还表现出儿茶酚酶活性(k(cat)=15±1.5 min-1,K(M)=6.4±1.8 mM),并与其他二铜儿茶酚氧化酶模型进行了比较。