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首页> 外文期刊>Inorganica Chimica Acta >catena-[mu-Tris(1,2-bis(tetrazol-1-yl)ethane-N4,N4 ')iron(II)] bis(tetrafluoroborate): synthesis, structure, spectroscopic and magnetic characterization of a chain-type coordination polymer spin-crossover compound
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catena-[mu-Tris(1,2-bis(tetrazol-1-yl)ethane-N4,N4 ')iron(II)] bis(tetrafluoroborate): synthesis, structure, spectroscopic and magnetic characterization of a chain-type coordination polymer spin-crossover compound

机译:链-[μ-Tris(1,2-双(四唑-1-基)乙烷-N4,N4']铁(II)]双(四氟硼酸酯):链型配位化合物的合成,结构,光谱和磁性表征聚合物自旋交联化合物

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摘要

In analogy to a common synthesis of I-substituted 5-H tetrazoles (Tetrahedron Lett. 36 (1995)1759; Beloruss. Gos. Univ., Minsk, USSR. Khim. Geterotsikl. Soedin. 11 (1985) 1521; Beloruss. Gos. Univ., Minsk, USSR. Khim. Geterotsikl. Soedin. 1 (1991) 66; BGU, Belarus. Vestsi Akad. Navuk Belarusi, Ser. Khim. Navuk 1 (1992) 73), the new bidentate ligand 1,2-bis(tetrazol-1-yl)ethane [endi] was synthesized and characterized by X-ray diffraction, NMR, IR and UV-Vis spectroscopy. By using iron(II) tetrafluoroborate hexahydrate the complexation with this ligand yields a 1-dimensional linear coordination polymer similar to the recently published chain compound (Inorg. Chem. 39 (2000) 1891) exhibiting a thermally induced spin-crossover phenomenon. Similar to the 1,2-bis(tetrazol-1-yl)propane-bridged compound, our 1,2-bis(tetrazol-1-yl)ethane-bridged compound shows a gradual spin transition, but the spin-crossover temperature T-1/2 approximate to 140 K is found to be 10 K above the other T-1/2,. The T11, was determined by temperature-dependent Fe-57-Mossbauer, far FT-IR and UV-Vis spectroscopy as well as by temperature-dependent magnetic susceptibility measurements. Single crystals of the complex were grown in situ from a solution of the ligand and iron(II) tetrafluoroborate. The X-ray structure determinations of both the high spin as well as the low spin state of the compound revealed a solid state structure, which is comparable to that of catena-[Fe(1,2-bis(tetrazole-1-yl)propane)(3)](ClO4)(2) (Inorg. Chem. 39 (2000) 1891; 2nd TMR-TOSS Meeting, 4th Spin Crossover Family Meeting, Lufthansa Training Center, Sceheim/Germany, April 30-May 2, 1999). Both the 1,2-bis(tetrazol-1-yl)propane-bridged and our compound do not show a thermal hysteresis effect (J. Am. Chem. Soc. 115 (1993) 98 10; Inorg. Chim. Acta 37 (1979) 169; Chem. Phys. Lett. 93 (1982) 567). The synthesis of the complex described in the experimental section yielded a fine powdered product being poorly soluble in most common solvents. The single crystal measurements were done with crystals obtained by various diffusion methods. Most of them yielded either thin needles or small hexagonal prism crystals depending on the specific conditions. (C) 2002 Elsevier Science B.V. All rights reserved. [References: 22]
机译:类似于I-取代的5-H四唑的一般合成法(Tetrahedron Lett.36(1995)1759; Beloruss。Gos。Univ。,明斯克,苏联。Khim。Geterotsikl。Soedin。11(1985)1521; Beloruss。Gos ,明斯克,苏联大学。Khim。Geterotsikl。Soedin。(1991)66;白俄罗斯BGU。Vestsi Akad。Navuk白俄罗斯,Shim。Khim。Navuk 1(1992)73),新的双齿配体1,2-合成了双(四唑-1-基)乙烷[endi],并通过X射线衍射,NMR,IR和UV-Vis光谱进行了表征。通过使用六水合四氟硼酸铁(II),与该配体的络合产生一维线性配位聚合物,其类似于最近公开的链化合物(Inorg。Chem。39(2000)1891),表现出热诱导的自旋交叉现象。与1,2-双(四唑-1-基)丙烷桥联的化合物相似,我们的1,2-双(四唑-1-基)乙烷桥联的化合物显示出逐渐的自旋转变,但自旋交叉温度为T发现大约140 K的-1/2比另一个T-1 / 2高10K。 T11是由温度依赖性的Fe-57-Mossbauer,远红外光谱和紫外可见光谱以及温度依赖性的磁化率测量确定的。从配体和四氟硼酸铁(II)的溶液中原位生长复合物的单晶。化合物的高自旋态和低自旋态的X射线结构测定均显示出固态结构,该结构与catena- [Fe(1,2-双(四唑-1-基)]丙烷)(3)](ClO4)(2)(Inorg。Chem。39(2000)1891年;第二届TMR-TOSS会议,第四届自旋交叉家庭会议,德国汉莎航空培训中心,1999年4月30日至5月2日)。 1,2-双(四唑-1-基)丙烷桥接的和我们的化合物都没有显示出热滞后作用(J.Am.Chem.Soc.115(1993)98 10; Inorg.Chim.Acta 37( 1979)169;化学物理学通讯93(1982)567)。在实验部分中描述的复合物的合成产生了细粉状产物,其在大多数普通溶剂中难溶。用通过各种扩散方法获得的晶体进行单晶测量。根据具体条件,它们大多数产生细针状或小的六边形棱柱晶体。 (C)2002 Elsevier Science B.V.保留所有权利。 [参考:22]

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