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本文引用的文献

1
Synthesis and characterization of an iron(IV) ketimide complex.合成与铁(IV)酰亚胺配合物的表征。
J Am Chem Soc. 2010 Sep 22;132(37):12814-6. doi: 10.1021/ja104934n.
2
Formation, structure, and EPR detection of a high spin Fe(IV)-oxo species derived from either an Fe(III)-oxo or Fe(III)-OH complex.高自旋 Fe(IV)-氧物种的形成、结构和 EPR 检测，该物种来源于 Fe(III)-氧或 Fe(III)-OH 配合物。
J Am Chem Soc. 2010 Sep 8;132(35):12188-90. doi: 10.1021/ja1047818.
3
The crystal structure of a high-spin oxoiron(IV) complex and characterization of its self-decay pathway.高自旋氧桥双核铁(IV)配合物的晶体结构及其自衰变途径的表征。
J Am Chem Soc. 2010 Jun 30;132(25):8635-44. doi: 10.1021/ja100366c.
4
Catalytic N-N coupling of aryl azides to yield azoarenes via trigonal bipyramid iron-nitrene intermediates.通过三角双锥铁-氮宾中间体催化芳基叠氮与芳基偶氮化合物的 N-N 偶联反应。
J Am Chem Soc. 2010 Mar 31;132(12):4083-5. doi: 10.1021/ja910224c.
5
A diiron(IV) complex that cleaves strong C-H and O-H bonds.一种能够裂解强 C-H 和 O-H 键的二铁(IV)配合物。
Nat Chem. 2009 May;1(2):145-50. doi: 10.1038/nchem.162.
6
A synthetic high-spin oxoiron(IV) complex: generation, spectroscopic characterization, and reactivity.一种合成的高自旋氧代铁（IV）配合物：生成、光谱表征及反应活性
Angew Chem Int Ed Engl. 2009;48(20):3622-6. doi: 10.1002/anie.200900863.
7
Substrate-triggered formation and remarkable stability of the C-H bond-cleaving chloroferryl intermediate in the aliphatic halogenase, SyrB2.脂肪族卤化酶SyrB2中碳氢键裂解氯高铁中间体的底物触发形成及显著稳定性
Biochemistry. 2009 May 26;48(20):4331-43. doi: 10.1021/bi900109z.
8
Axial ligand effects on the geometric and electronic structures of nonheme oxoiron(IV) complexes.轴向配体对非血红素氧代铁（IV）配合物的几何结构和电子结构的影响。
J Am Chem Soc. 2008 Sep 17;130(37):12394-407. doi: 10.1021/ja8022576. Epub 2008 Aug 20.
9
Synthesis, structure, and physical properties for a series of monomeric iron(III) hydroxo complexes with varying hydrogen-bond networks.一系列具有不同氢键网络的单体铁（III）羟基配合物的合成、结构及物理性质
Inorg Chem. 2008 Jul 7;47(13):5780-6. doi: 10.1021/ic800048e. Epub 2008 May 23.
10
Electronic design criteria for O-O bond formation via metal-oxo complexes.通过金属-氧络合物形成O-O键的电子设计标准。
Inorg Chem. 2008 Mar 17;47(6):1849-61. doi: 10.1021/ic701972n.

三价三角双锥铁(IV)氰化物配合物的特性，具有非常高的还原电位，以及其铁(II)和铁(III)同系物。

Characterization of a tricationic trigonal bipyramidal iron(IV) cyanide complex, with a very high reduction potential, and its iron(II) and iron(III) congeners.

机构信息

Department of Chemistry, University of Minnesota, Minneapolis, Minnesota 55455, USA.

出版信息

Inorg Chem. 2011 Apr 4;50(7):2885-96. doi: 10.1021/ic102094d. Epub 2011 Mar 7.

DOI:10.1021/ic102094d
PMID:21381646
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC3065519/
Abstract

Currently, there are only a handful of synthetic S = 2 oxoiron(IV) complexes. These serve as models for the high-spin (S = 2) oxoiron(IV) species that have been postulated, and confirmed in several cases, as key intermediates in the catalytic cycles of a variety of nonheme oxygen activating enzymes. The trigonal bipyramidal complex Fe(IV)(O)(TMG(3)tren) (1) was both the first S = 2 oxoiron(IV) model complex to be generated in high yield and the first to be crystallographically characterized. In this study, we demonstrate that the TMG(3)tren ligand is also capable of supporting a tricationic cyanoiron(IV) unit, Fe(IV)(CN)(TMG(3)tren) (4). This complex was generated by electrolytic oxidation of the high-spin (S = 2) iron(II) complex Fe(II)(CN)(TMG(3)tren) (2), via the S = 5/2 complex Fe(III)(CN)(TMG(3)tren) (3), the progress of which was conveniently monitored by using UV-vis spectroscopy to follow the growth of bathochromically shifting ligand-to-metal charge transfer (LMCT) bands. A combination of X-ray absorption spectroscopy (XAS), Mössbauer and NMR spectroscopies was used to establish that 4 has a S = 0 iron(IV) center. Consistent with its diamagnetic iron(IV) ground state, extended X-ray absorption fine structure (EXAFS) analysis of 4 indicated a significant contraction of the iron-donor atom bond lengths, relative to those of the crystallographically characterized complexes 2 and 3. Notably, 4 has an Fe(IV/III) reduction potential of ∼1.4 V vs Fc(+/o), the highest value yet observed for a monoiron complex. The relatively high stability of 4 (t(1/2) in CD(3)CN solution containing 0.1 M KPF(6) at 25 °C ≈ 15 min), as reflected by its high-yield accumulation via slow bulk electrolysis and amenability to (13)C NMR at -40 °C, highlights the ability of the sterically protecting, highly basic peralkylguanidyl donors of the TMG(3)tren ligand to support highly charged high-valent complexes.

摘要

目前，仅有少数几个合成的 S = 2 氧代铁（IV）配合物。这些配合物作为高自旋（S = 2）氧代铁（IV）物种的模型，这些物种已被假定为多种非血红素氧激活酶催化循环中的关键中间体，并在某些情况下得到证实。三斜双锥配合物 [Fe（IV）（O）（TMG（3）tren）]（2+）（1）是第一个高产率生成的 S = 2 氧代铁（IV）模型配合物，也是第一个结晶学表征的配合物。在这项研究中，我们证明 TMG（3）tren 配体也能够支持三价氰基铁（IV）单元 [Fe（IV）（CN）（TMG（3）tren）]（3+）（4）。该配合物是通过高自旋（S = 2）铁（II）配合物 [Fe（II）（CN）（TMG（3）tren）]（+）（2）的电解氧化生成的，通过 S = 5/2 配合物 [Fe（III）（CN）（TMG（3）tren）]（2+）（3），其进展通过使用紫外-可见光谱方便地监测，以跟踪吸光度向长波长移动的配体-金属电荷转移（LMCT）带的增长。X 射线吸收光谱（XAS）、穆斯堡尔和 NMR 光谱的组合用于确定 4 具有 S = 0 铁（IV）中心。与顺磁性铁（IV）基态一致，4 的扩展 X 射线吸收精细结构（EXAFS）分析表明，铁供体原子键长显著收缩，与结晶学表征的配合物 2 和 3 相比。值得注意的是，4 的 Fe（IV/III）还原电位约为 1.4 V 相对于 Fc（+/o），这是迄今为止观察到的单核配合物的最高值。4 的相对稳定性（在含有 0.1 M KPF（6）的 CD（3）CN 溶液中 25°C 时的 t（1/2）≈15 分钟），反映在其通过缓慢的 bulk 电解高产率积累和在-40°C 下进行（13）C NMR 的适用性，突出了 TMG（3）tren 配体的空间位阻保护、高碱性全烷基胍基供体支持高电荷高价配合物的能力。