毛细管区带电泳技术快速分离检测爆炸残留物中的无机离子

利用间接紫外毛细管区带电泳方法完成了对爆炸残留物中7种无机离子(K+,NH+4,NO-2,NO-3,SO2-4,ClO-3,ClO-4)的分离检测。阳离子测定采用的缓冲体系为10 mmol/L吡啶（pH 4.5）-3 mmol/L冠醚,K+和NH+4在2.6 min内达到基线分离,检出限分别为0.25 mg/L和0.10 mg/L(S/N=3)。阴离子测定采用的缓冲体系为40 mmol/L硼酸-1.8 mmol/L重铬酸钾-2 mmol/L硼酸钠（pH 8.6）,氢氧化四甲铵为电渗流改性剂,5种阴离子在4.6 min内达到基线分离,检出限为0.10～1.85 mg/L。该方法已成功地应用于实际爆炸物样品种类的判定分析,取得了很好的结果。     

［NaXY」_2W_nMo_（6－n）O_（19）的~1HNMR和IR研究

本文对二种具有新奇结构的［ＮａＸＹ］２ＷｎＭｏ６－ｎＯ１９（Ⅰ．Ｘ＝ＤＢ１８Ｃ６，Ｙ＝ＣＨ３ＯＨ，ｎ＝４；Ⅱ．Ｘ＝ＤＢ２４Ｃ８，ｎ＝１）冠醚钼钨杂多酸超分子配合物进行了核磁共振和红外光谱测定，判定了谱图的归属并考察了结构与谱学参数之间的关系。     

2,3-二羟基萘钼多酸有机衍生物的合成及1H NMR和IR谱学研究

本文对二种新合成的2，3－二羟基萘二钼和四钼多酸有机衍生物[n-Bu)4N]2[Mo2O5(OC10H6O)2](Ⅰ）和[n-Bu)4N]2[Mo4O10(OC10H6O)2(OCH3)2](Ⅱ)进行了红外光谱与核磁共振波谱研究，发现[Mo2O5]^2 中钼氧多桥键的红外振动频率较[Mo4O10(OCH3)2]^2 中钼氧多桥键的红外振动频率红移，而在配合物Ⅱ中2，3－二羟基中芳环的^1H化学位移较配合物Ⅰ中向低场移动。同时还发现含二钼配位中心[Mo2O5]^2 的[Mo2O5(OC10H6O)2]^2-与含四钼配位中心[Mo4O10(OCH3)2]^2 的[Mo4O10(OC10H6O)2(OCH3)2]^2-生成条件的差异仅仅只在反应体系的pH值的微小变化，说明钼多酸有机衍生物阴离子是对体系酸碱度极为敏感的物质。     

具有生物活性钼钨仿生配合物与ATP作用的NMR研究

在常温下合成了以邻苯二酚为配体,分别以乙二胺、1,2-丙二胺、1,3-丙二胺为抗衡离子的7种手性钼钨八面体配合物(NH2CH2CH2NH3)3[Mo(V)O2(OC6H4O)2](1),(NH2CH2CH2NH3)2[W(VI)O2(OC6H4O)2](2),(NH2CH2CH2NH3)2.5[Mo(V)0.5W(VI)0.5O2(O2C6H4)]2](3),(NH3CH2CHNH2CH3)3[Mo(V)O2(OC6H4O)2](4),(NH3CH2CHNH2CH3)2[W(VI)O2(OC6H4O)2](5),(NH3CH2CHNH2CH3)2.5[Mo(V)0.5W(VI)0.5O2(OC6H4O)2](6),(NH3CH2CH2CH3NH2)2.5[Mo(V)0.5W(VI)0.5O2(OC6H4O)2](7),并在生理条件下对其与ATP的相互作用进行了液体NMR研究,发现标题配合物的中心金属离子在纯D2O溶剂中大多数以+5价形式存在,W(VI)被还原为W(V),但与ATP混合后又转化为+6价,配合物原有的顺磁性特征完全消失.研究还发现ATP可以促进中心离子与原配体发生解离.     

（n—C4H9）4N2（OC14H8O2）Mo4O10（OCH3）2的合成和晶体结构

为探讨钼多酸根阴离子在有机化学反应中的催化机理，用菲醌作底物合成了（ｎ－Ｃ４Ｈ９）４Ｎ）２（ＯＣ１４Ｈ８Ｏ）２Ｍｏ４Ｏ１０Ｏ１０（ＯＣＨ３）２）配合物，Ｘ射线单晶结构分析表明，该晶体属单斜晶系，空间群Ｐ２１／ｃ，ａ＝１．３１４９（５）ｎｍ，ｂ＝１．８６６６（８）ｎｍ，ｃ＝１．８９０３（３）ｎｍ，β＝１０４．０６（３）Ｚ＝２．收集到独立衍射点３５０５个，其中１３８２个为可观测点，最终一致性因子Ｒ＝０     

1,3,5-均苯三羧酸根金属-有机多重框架结构配合物

综述了近年来1,3,5-均苯三羧酸(H3BTC)与金属配位形成金属配合物的研究进展。对1,3,5-均苯三羧酸根(BTC)作为桥基时的配位特点及其桥联多核配合物的合成方法和结构特点进行了简要介绍,并对今后BTC类超分子网络配合物应用与结构研究的发展方向进行了展望。     

Synthesis, Crystal Structure, UV-vis and EPR Studies of（ NH3CH2CH2NH2 ） 2.5 [ Mo0.5^（V）W0.5^（VI）O2 （ OC6H4O ） 2]

Cis-dioxo-metal complex ( NH3CH2CH2NH2 ) 2.5 [ Mo0.5^(V)W0.5^(VI)O2 ( OC6H4O ) 2] 1 was obtained by the reaction of tetra-butyl ammonium hexamolybdotungstate with 1, 2-dihydroxybenzene in the mixed solvent of CH3OH, CH3CN and ethylenediamine,and characterized by X-ray diffraction, UV-vis and EPR analysis. Compared with its analogous complexes (NH3CH2CH2NH2)3[Mo^(V)O2(OC6H40)2] 2 and (NH3CH2CH2NH2)2[W^(VI)O2(OC6H4O)2] 3, the results show that tungsten(VI) is less active in redox than molybdenum (VI) and that the change of the valence induced by substitution of W(VI) for Mo(V) in EMO2(OC6H40)2]n- does not influence the coordination geometry of the complex anion in which the metal center exhibits distorted octahedral coordination with cis-dioxo catechol. The responses to EPR of complexes 1 and 2 are active but complex 3 is silent,and the UV-vis spectra exhibited by the three complexes are obvious different because of the different electronic configuration between the central Mo(V) and W(VI) ions in the complexes.It is noteworthy that complexes 1 and 2 have the similar EPR signal to flavoenzyme, suggesting that the three complexes have the same coordination geometry feature with the co-factor of flavoenzyme.     

Macro-, Micro-, Nano- and Crystal Structures of a Homodinuclear Complex [NH3（ CH2）3NH3]2{Na2[（C6H4O2）2]（C6H4O2H）2}

A homodinuclear complex （NH3CH2CH2CH2NH3）2 {Na2[（C6H4O2）2] （C6H4O2H）2} （1） has been synthesized by a solution-based self-assembly route. It crystallized in monoclinic system with space group P21/c. Every sodium ion coordinates in a tetragonal prism fashion with two O atoms of a terminal chelating catecholate ligand and three O atoms from two bridging catecholate ligands. Two neighboring NaO5 tetragonal prisms are edge-shared and centrosymmetric with regard to the inversion center to form a binuclear cluster {Na2[（C6H4O2）2]（C6H4OOH）2}^4- anion. The complex anions were aligned parallelly by n-n interaction and linked with the protonated 1,3-propylenediamine through hydrogen bonds which were assembled into a multi-lamellar structure with channels. The crystal exhibits rectangular geometry with an interior triangle hollow structure under optical microscopy. And the scanning electron microscopy （SEM） indicates that the wall of the tubes shows multi-lamella morphologies. Further, the transmission electron microscopy （TEM） reveals that the crystal is composed of multi-lamellar nano-tubes with diameters less than 100 nm. The molecular structure of the complex was compared with that of its isomer complex 2.     

有特色的选修课教材——《色彩与微观世界》

颜色是物质的基本属性之一,是物质微观结构的宏观表现。围绕颜色这一广泛而生动的话题,化学工业出版社于2004年9月出版的《色彩与微观世界》一书较系统地论述了颜色与物质微观结构理论之间的关系。本书是编著者金增瑗在首都师范大学开设色彩与物质结构选修课9年后精心完成的。全书共9章:第1章,颜色的基本理论。第2章,物质的结构状态与光学颜色。以露珠彩虹、蓝天白云以及多种宝石的彩晕为例,剖析了色散、散射、干涉、衍射等物理效应产生的颜色与物质的微观结构的特有关系。第3章,原子的结构状态与简单激发产生的颜色。介绍了黑体辐射与彩色…     

H2Mo8O26 ［(n-Bu)4N］2［(CH3)2COHCH2COCH3］2的合成与晶体结构

在正四丁基八钼酸(β型)铵和微量乙二胺的存在下,丙酮分子发生羟醛缩合形成了4甲基4羟基2戊酮,并与八钼酸根和正四丁基铵阳离子组成了标题化合物。X射线单晶结构分析表明该晶体属三斜晶系,空间群为P1,Mr=190277,a=11512(6)nm,b=1.2790(3)nm,c=1.3395(4)nm,α=6522(2)°,β=78.26(4)°,γ=71.12(3)°,Z=1,R=0.053,Rw=0.067。结果表明4甲基4羟基2戊酮的形成有可能揭示钼多酸的另一催化功能。