梯形(phen)Zn-O-MoO2晶体的水热合成与表征

利用水热方法合成梯形(phen)Zn—O—MoO2晶体,并用X射线衍射仪对其结构进行了表征.结果表明,(phen)Zn—O—MoO2属单斜晶系:空间群为P2/m;a=0.881 64(17)nm,b=0.643 96(14)nm,c=1.065 9(6)nm,α=γ=90°,β=100.79(3)°,V=0.594 4(4)nm3,Z=2.Zn原子为三角双锥构型,Mo原子为四面体构型,(phen)Zn—O—MoO2为折叠梯形链状结构.     

含柠檬酸配体的钼硫簇合物的合成与晶体结构的测定

合成了含有Mo—S簇阴离子 [Mo2 O2 ( μ S) 2 (C6H5O7) (C6H4 O7) ]5-柠檬酸簇合物 ,并通过元素分析、红外光谱、紫外 可见光谱和X射线光电子能谱对配合物进行了表征 ,用X射线衍射法测定了该化合物的晶体结构 .结果表明 ,该簇合物属于单斜晶系 ,空间群P2 1/c,a =2 3 766( 5)nm ,b =1 3 2 74 ( 3 )nm ,c =2 2 4 71 ( 5)nm ,α=γ =90°,β=1 1 8 2 1°,V =6 2 4 7( 2 )nm3 ,Z =8,一致性因子R =0 0 83 1 ,R2 ,w=0 1 536.该簇合物阴离子中每一个Mo原子都采取扭曲的八面体结构 ,柠檬酸通过羟基、α 羧基、一个 β 羧基与Mo配位 .晶体结构表明在一个结晶学上不对称的结构单元内有两个结晶学上独立的分子 .     

微波辐射合成顺丁烯二酸单淀粉酯

以木薯淀粉为原料,顺丁烯二酸酐为酯化剂,在微波条件下合成了顺丁烯二酸单淀粉酯.着重研究了淀粉与酸酐的摩尔比、碳酸钠的用量、水的用量、反应时间、微波功率对产物取代度的影响.结果表明:当淀粉用量为10g、淀粉与酸酐的摩尔比为1:0.5、碳酸钠加入量为0.6g、水的加入量为8g、反应时间为4min、微波功率为400W时,可以...     

双核钨氧柠檬酸配合物K_6[W_2O_5(cit)_2]·6H_2O的合成及晶体结构

标题化合物是通过四硫代钨酸铵和柠檬酸钾反应而得。用ＩＲ、ＸＰＳ、元素分析进行了结构表征，Ｘ－ｒａｙ结构测定进一步肯定了以上结论。该晶体为三斜晶系，Ｐ１空间群，晶胞参数为：ａ＝０．８５１１１（９）ｎｍ，ｂ＝０．９７８４（１０）ｎｍ，ｃ＝１．０８２（１１）ｎｍ，α＝１１４．８５（１２）°，β＝１０６．５８（１１）°，γ＝９８．８９（１０）°，Ｚ＝１，Ｖ＝０．７４３６（１３）ｎｍ３，Ｄｃ＝２．５９４ｇ／ｃｍ３，Ｆ（０００）＝５５４，μ＝８６．６１ｃｍ－１，一致性因子Ｒ＝０．０７５，ＷＲ２＝０．１８８９。     

Hydrothermal synthesis, structure and quantum chemistry of transition metal complex supported by metal-oxo cluster[{Ni(phen)_2}_2(ξ-Mo_8O_(26))]

A nickel-1,10-phenanthroline complex supported on an octamolybdate, [{Ni(phen)2}2(ξ-Mo8O26)], has been hydrothermally synthesized with MoO3, H2MoO4, Ni(OAc)2 · 6H2O and 1,10-phenathroline (1,10-phen) as raw materials. The crystals of the compound belong to mono-clinic P21/n space group, a= 1.2952(2), b = 1.6659(10), c= 1.3956(12) nm, β=106.273(8)°, V = 2.8906(5) nm3, Z = 2. 5604 observable reflections (/>2σ(/)) were used for structure resolution and refinements to converge to final R1 = 0.0414, wR2 = 0.0815. The result of structure determination shows that the compound contains octamolybdate possessing a novel structure type (named as ξ-isomer). The feature of ξ-[Mo8O26]4- is that it is composed of Mo6O6 ring and two MoO6 octa-hedra located at cap positions on opposite faces. The Mo6O6 ring contains two octahedral and four trigonal-bipyramidal MovI atoms. Each ξ-[Mo8O26]4- unit is bonded with two [Ni(phen)2]2+ through terminal oxygen atoms of octahedral and neighbouring trigonal-bipyramidal Mo at     

改进多元醇法合成超小超顺磁性Fe3O4纳米颗粒

利用改进多元醇法,以无水FeCl3为铁源,3-氨基丙醇为碱性水解剂,聚丙烯酸为稳定剂,成功制备了水分散稳定的超小超顺磁性Fe3O4纳米颗粒.高分辨率透射电镜、X-射线粉末衍射和拉曼光谱分析证实合成的纳米粒子为Fe3O4,Zeta电位、热重和红外光谱分析证实表面包覆的有机物为聚丙烯酸.通过改变多元醇的链长,初步实现了纳米颗粒粒径在1～3 nm之间调控.     

新奇的双帽 pseudo-Keggin 结构磷钼钒酸盐的水热合成、晶体结构、性质及其量子化学计算

报道了一种新奇的磷钒酸盐[NH₄]₄H[PMo₈V₄^ⅣV₂^ⅤO₄₂]·24H₂O的合成方法,用元素分析、EPR、IR、UV谱和TG等手段进行了表征,并用X射线衍射法测定了晶体结构.结果表明,该杂多酸盐属于四方晶系,空间群P4/mnc,a=b=1.2592(2)nm,c=1.7565(4)nm,V=2.7848(8)nm³,Z=2.杂多阴离子具有双帽pseudoKeggin结构,不仅其中的8个金属位置被V和Mo无序占有,而且整个磷钼钒酸盐杂多阴离子的取向也是无序的.还应用EHMO方法研究了簇阴离子的电子结构.     

Hydrothermal Synthesis, Crystal Structure and Photoluminescent Property of a New Isophthalate- bridged Zinc(II) Polymer with One-dimensional Chain Structure: [Zn(ipt)(im)_2]_(2n)·3nH_2O (ipt = Isophthalate, im = Imidazole)

1 INTRODUCTION The design and synthesis of metal-organic frame- work structure have been studied widely during the past decade not only because of their intriguing architectures but also their unexpected properties for potential practical applications in a wide number of fields, such as asymmetric catalysis, magnetism, pho- toluminescence and so on[1～3]. These novel struc- tures can be rapidly and efficiently synthesized from simple subunits, where the metal ions, bi- or multi- dentate o…     

[Bmim]PF6萃取环境样品中四环素类抗生素残留

对用疏水性离子液体（[Bmim]PF6）萃取分离四环素类抗生素和传统的有机溶剂进行比较,实验结果表明,离子液体不仅有比有机溶剂好的萃取效果,而且对人类及其生存环境没有污染,并用疏水性离子液体萃取分离环境样品中四环素类抗生素残留,用紫外分光光度法检测其残留量．该方法简便、快速,回收率高,精密度高．