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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >Pentanuclear complexes with unusual structural topologies from the initial use of two aliphatic amino-alcohol ligands in Fe chemistry
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Pentanuclear complexes with unusual structural topologies from the initial use of two aliphatic amino-alcohol ligands in Fe chemistry

机译：最初在铁化学中使用两个脂族氨基醇配体产生具有异常结构拓扑的五核配合物

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摘要

Five novel pentanuclear Fe ~(3+) clusters with the aliphatic amino-alcohol ligands 3-amino-1-propanol (Hap) and 2-(hydroxymethyl)piperidine (Hhmpip) [Fe _5(μ _3-Ο) _2(L) _4(O _2CR) _7] [L = ap ~-, R = Ph (1); L = ap ~-, R = C(CH _3) _3 (2); L = hmpip ~-, R = Ph (3); L = hmpip ~-, R = C(CH _3) _3 (4)] and [Fe _5(μ _4-Ο)(μ _3-Ο)(O _2CC(CH _3) _3) _8(ap) _2Cl(HO _2CC(CH _3) _3)] (5) are reported. Compounds 1-4 were prepared from reactions of preformed trinuclear Fe ~(3+) clusters with the ligands in a molar ratio 1:5 in MeCN (1, 3, 4) or DMF (2), whereas compound 5 was prepared from the reaction of FeCl _3 with Hap in the presence of HO _2CC(CH _3) _3 in a molar ratio 1:3:2 in MeCN. To the best of our knowledge, 1-5 are the first examples of Fe ~(3+) complexes with the ligands Hap and Hhmpip. The structures of 1-4 are composed of a quasi-planar [Fe _5(μ _3-O) _2] ~(11+) core which consists of two vertex-sharing [Fe _3(μ _3-O)] ~(7+) triangles. The structure of 5 is based on the [Fe _5(μ _4- O)(μ _3-O)] ~(11+) core, in which the five Fe ~(3+) ions adopt a monocapped trigonal pyramidal topology. Variable-temperature magnetic susceptibility measurements on powdered microcrystalline samples of 1 and 5 revealed the existence of antiferromagnetic interactions which led to an S = 5/2 ground state. M?ssbauer spectroscopy studies on powdered microcrystalline samples of 1 and 5 confirmed that all iron ions of both complexes are in the Fe ~(3+) (S = 5/2) state. The variation of the ligand environment in the various iron sites was reflected in their different quadruple splitting parameters. At T < 50 K the M?ssbauer spectra indicated the onset of spin relaxation effects in the time scale of the technique (10 ~(-7)-10 ~(-8) s).
机译：五个新颖的五核Fe〜（3+）簇与脂肪族氨基醇配体3-氨基-1-丙醇（Hap）和2-（羟甲基）哌啶（Hhmpip）[Fe _5（μ_3-Ο）_2（L） _4（O _2CR）_7] [L = ap〜-，R = Ph（1）; L = ap〜-，R = C（CH _3）_3（2）; L = hmpip〜-，R = Ph（3）; L = hmpip〜-，R = C（CH _3）_3（4）]和[Fe _5（μ_4-Ο）（μ_3-Ο）（O _2CC（CH _3）_3）_8（ap）_2Cl（HO _2CC（CH _3）_3）]（5）被报告。化合物1-4是从预先形成的三核Fe〜（3+）簇与配体在MeCN（1、3、4）或DMF（2）中以1：5的摩尔比反应制备的，而化合物5是从在MeCN中，摩尔比为1：3：2的HO _2CC（CH _3）_3存在下，FeCl _3与Hap的反应。据我们所知，1-5是Fe〜（3+）与配体Hap和Hhmpip配合物的第一个例子。 1-4的结构由准平面[Fe _5（μ_3-O）_2]〜（11+）核组成，该核由两个顶点共享的[Fe _3（μ_3-O）]〜（7 +）三角形。 5的结构基于[Fe _5（μ_4- O）（μ_3-O）]〜（11+）核，其中五个Fe〜（3+）离子采用单封顶三角锥拓扑。在粉末微晶样品1和5上进行的温度可变磁化率测量表明，存在反铁磁相互作用，导致S = 5/2基态。 Mssbauer光谱学对1和5的粉末状微晶样品的研究证实，两种络合物的所有铁离子均处于Fe〜（3+）（S = 5/2）状态。各个铁位点上配体环境的变化反映在它们不同的四重分裂参数上。在T <50 K时，Msssbauer光谱表明在该技术的时间范围内（10〜（-7）-10〜（-8）s）出现了自旋弛豫效应。

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