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Structural Analysis of Powder Complex of Mn(phen)3(CF3S03)2.6.5H20

机译:Mn(Phen)3粉末络合物的结构分析(CF3S03)2.6.5H20

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The objective of this work was to synthesise of complex containing manganese(II), 1, 10-phenanthroline(phen)as ligand and a counter anion of trifluoromethanesulfonate(triflate). The complex was prepared by interaction of the corresponding nitrate salt and slightly excess of phenanthroline in aqueous solution, whereupon the precipitate was produced on addition of an excess of saturated potassium triflate solution when reducing the solvent. It was then characterised in terms of electrical conductivity, metal content, magnetic moment, electronic and infrared spectral properties, and powder XRD. The atomic absorption spectral data and the equivalent conductance suggest that the resulted complex was found to be ionic hydrated complex with the content of three ions per molecule, with an equivalent conductance in the range values of the three ionic standard, but much higher than the two ionic standard and much lower than the four ionic standard. The formula of [Mn(phen)3](CF3SO_3)_2.6, 5H20 was then proposed. The corresponding IR spectrum indicated the presence of typical function group of phenantroline and the triflate ion in the complex. The complex was found to be yellowish, and paramagnetic(μ_(eff)=5.8-5.95 BM)corresponding to high spin Mn(II)-3d~5. The electronic spectrum of [Mn(phen)_3]~(2+) revealed typical bands concentrated at vi ~ 13966 cm~(-1), V2~ 16474 cm~(-1), V3~ 19493 cm~(-1), V4~ 26325 cm~(-1) as a shoulder, and vs ~ 30769 cm~(-1). These bands might be respectively associated with the spin-forbidden transitions of ~6A_(1g) → 4T_(1g)(G), 6A_(1g) → 4T_(2g)(G), 6A_(1 g)→ 4E_g, 4A_(1g)(G), 6A_(1g) → 4T_(2g)(D), and 6A_(1g) → 4E_g(D). The powder X-ray diffraction of the complex was then solved with Rietica-Le Bail method, and found to be structurally triclinic with space group of PI(lattice parameters, a= 12. 633 ?; b= 17.062 ?; c= 22.481 ?; a =106.876~0; β= 110.901~0; y= 99.562~0; V=4130.4169; R_p= 3.67; R_(wp)= 7.34; R_(exp)= 3.61)for the cationi
机译:本作作品的目的是合成含有锰(II),1,10菲咯啉(Phen)作为配体的复合物和三氟甲磺酸盐(三氟甲磺酸酯)的抗衡阴离子。通过相应的硝酸盐和略微过量的菲咯啉在水溶液中的相互作用来制备该复合物,因此在还原溶剂时加入过量的饱和钾的三氟乙酸酯溶液制备沉淀物。然后在电导率,金属含量,磁矩,电子和红外光谱性能和粉末XRD方面表征。原子吸收光谱数据和等效电导表明所得复合物被发现与每分子三离子的含量为离子水合复合物,在三个离子标准的范围值中具有等同的电导,但远高于两种离子标准,远低于四种离子标准。然后提出[Mn(phen)3](CF 3 SO_3)_2.6,5H20的式。相应的IR光谱表明,在复合物中存在典型的酚丙烯碱和Triflate离子的存在。发现该复合物是淡黄色的,并且对应于高旋转Mn(II)-3d〜5的顺磁(μ_(μ_(eff)= 5.8-5.95bm)。 [Mn(phen)_3]〜(2+)的电子谱显示在VI〜13966cm〜(-1),V2〜16474cm〜(-1),V3〜19493cm〜(-1)中浓缩典型的带,V4〜26325cm〜(-1)作为肩部,而Vs〜30769 cm〜(-1)。这些频带可以分别与旋转禁止的转换相关的〜6a_(1g)→4t_(1g)(g),6a_(1g)→4t_(2g)(g),6a_(1g)→4e_g,4a_( 1g)(g),6a_(1g)→4t_(2g)(d)和6a_(1g)→4 e_g(d)。然后用Rietica-Le Bail方法解决该络合物的粉末X射线衍射,并发现与Pi的空间组的结构三级(晶格参数,a = 12.633.; b = 22.481? ; a = 106.876〜0;β= 110.901〜0; y = 99.562〜0; v = 4130.4169; r_p = 3.67; r_(wp)= 7.34; r_(exp)= 3.61)申请

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