ICP－AES法同时测定人体牙、骨中多种生命元素

由于牙、骨中存在大量Ｃａ，Ｐ等基体元素（以羟基磷酸钙为主的无机盐类占骨总重的２／３），使得ＩＣＰ－ＡＥＳ同时测定牙、骨中多元素时，光谱干扰严重。因而，同时测定牙、骨中多种生命元素时，必须进行化学预处理或应用光谱学技术校正干扰。本文研究了基体干扰情况，使用基体匹配标准溶液，并配合对样品进行不同倍率的稀释，分步测定了十二种常量、微量生命元素。方法简便，结果可靠。     

含手性膦配体和邻巯基氧化吡啶配体的金,钯配合物的2D NMR研究

对含手性膦配体甲基-3-脱氧-3－（二苯膦基）－4，6-氧-苄叉基-a-D-吡喃阿卓糖苷（3－MBPA）和甲基-2-脱氧-2－（二苯膦基）－4，6-氧-苄叉基-a－D-吡喃阿卓糖苷（2－MN-PA）及邻巯基氧化吡啶配体mpo的金配合物An[（3－MBPA）（mpo）]（1）、An[（2－MBPA）（mpo）]（2）和钯配合物Pd[（3－MBPA）（mpo）C1]（3）、Pd[（2－MBPA）（mpo）-C1]（4）进行1H和13CNMR谱测定，利用一维和二维NMR技术归属了所有的1H和13CNMR谱线，结果表明：配体MBPA与金属配伍的是P原子，糖苷上H－5的化学位移变化最大，而且与配位金属的种类有关；配体mpo以单齿形式与金属配位时，是S原子参与配位。     

三种1,10-邻菲咯啉-铜(Ⅱ)-L-氨基酸配合物与DNA的相互作用

The Interaction of three complexes [Cu(phen)(Gly)(H₂O)]·ClO₄·2.5H₂O (1), [Cu(phen)(L-Val)(H₂O)]·ClO₄ (2) and [Cu(phen)(L-Ile)(H₂O)]·ClO₄ (3) (phen=1,10-phenanthroline, Gly=glycinate, L-Val=L-valinate, L-Ile=L-isoleucinate) with DNA have been investigated by electronic absorption spectroscopy, ethidium bromide(EB) fluorescence spectroscopy, viscosity and gel electrophoresis measurements. The intensity of maximal absorption peaks from absorption spectra are weakened with dropping DNA into the complexes. The emission intensity of EB-DNA systems in fluorescence spectroscopy have descended 50%, when the data of C_Cu / C_DNA is 30～40. Moreover, the viscosity of DNA increase and then decrease with the increasing of complexes. All of the results indicate that the interaction of complexes with DNA are partial intercalation, and the result of agarose gel electrophoresis show that the complexes can cleave pBR322 DNA in the present of H₂O₂ / vitamin C.     

配合物[Cu(L-Ile)(TATP)(H2O)]ClO4的结构、表征及与DNA之间的相互作用

Ternary complex [Cu(L-Ile)(TATP)(H₂O)](ClO₄)] was synthesized and characterized by molar conductivity, rotational analysis, spectroscopic (IR and UV-Vis) and X-ray diffraction methods, where L-Ile=L-Isoleucine, and TATP=1,4,8,9-tetraazatriphenylene. The complex crystallizes in triclinic space group P1 with two molecules in a unit cell of dimensions a=8.240 3(9) nm, b=11.914 9(13) nm, c=13.436 0(15) nm, α=109.136(2)°, β=101.101(2)°, γ=106.302(2)°. V=1.209 2(5) nm³, Z=2, D_c=1.589 Mg·m^-3, μ=1.132 mm^-1，R₁=0.036 9, wR₂=0.098 0. The crystal contains two independent [Cu(L-Ile)(TATP)(H₂O)]⁺ complexes for Cu₁ and Cu₂, respectively, having essentially the same distorted square-pyramidal structure, where each Cu(Ⅱ) ion is coordinated with two nitrogen atoms of TATP and the amino nitrogen atom and one carboxylate oxygen atom of L-Ile in the equatorial positions and one water oxygen atom at an axial position. Furthermore, the primary studies on the interaction between the complex and calf thymus DNA were also performed by electronic absorption spectroscopy and viscosity methods. CCDC: 244231.     

两个由1,1′-环己烷二乙酸构筑的镉的配合物的合成、晶体结构和荧光性质

通过邻羧苯乙酸、1,10-邻菲啰啉及硝酸镉的溶剂热反应合成了2个配合物：[Cd(phen)(chdc)]_n (1)和[Cd(phen)(chdc)(H₂O)]_n (2)。X-射线单晶衍射显示：1是梯状双链结构；2是单链结构，单链再通过氢键连接成双链。虽然1和2的组分相似，但它们在固态条件下的荧光发射却大不一样，可能在光化学方面有潜在的应用。     

两个含草酸根及硫氰酸根的新型三脚架钴(Ⅱ)配合物的合成、晶体结构及光谱性质(英)

本文合成了两个新型Co(Ⅱ)配合物，[LCo(μ-C₂O₄)CoL]·(ClO₄)₂·2CH₃CN (1)和[CoL(SCN)]·ClO₄ (2)，其中，L即三(3，5-二甲基吡唑甲基)胺。在配合物1中，Co与来自三脚架配体的4个氮和草酸根桥联配体的2个氧原子配位，处于扭曲八面体配位环境。由草酸根桥联两套LCo，构成了一个双核结构。在单核配合物2中，Co(Ⅱ)处于三角双锥配位构型，SCN-通过N配位与中心离子Co(Ⅱ)键联。在同一晶胞中有两个构型略微不同的分子，两个分子之间通过SCN的S原子有弱相互作用。对化合物1和2在溶液中的光谱性质做了进一步的研究和讨论。     

配合物[Cu(CAM)(H2O)2]的水热合成与结构表征

A copper(II) complex [Cu(CAM)(H₂O)₂], (CAM=4-hydroxypyridine-2,6-dicarboxylic acid), has been hydr-othermally synthesized and characterized by elemental analysis, IR, and X-ray diffraction single crystal structure analysis. It belongs to triclinic system, with space group P1, a=0.783 3(3) nm, b=0.796 5(3) nm, c=0.798 6(3) nm, α=100.340(6)°, β=93.768(6)°, γ=109.348(5)°, V=0.458 3(3) nm³, Z=2. The copper(II) ion is 5-coordinated and exhi bits a distorted square pyramidal coordination environment. The two coordinated aqueous molecules and the oxygen atoms from the ligand generate the intermolecular hydrogen bonds, which result in the 2D supramolecular network. CCDC: 227156.     

一种新颖1D链状聚合物[Ni(acac)2(dadpm)]∞的合成与晶体结构

The title compound [Ni(acac)₂(dadpm)]_∞ (acac=acetylacetonate, dadpm=4,4′-diaminodiphenylmethane) was synthesized from Ni(acac)₂·2H₂O with dadpm in DMF. The structure was characterized by elemental analysis, IR spectroscopy, thermal analysis and single-crystal X-ray diffraction. X-ray analysis revealed that the central Ni atom is at a center of symmetry, and is octahedrally coordinated by four O atoms from two acac anions and two N atoms from two dadpm ligands. Each dadpm ligand, which has a two-fold axis passing through its methylene C atom, bridges two Ni atoms to form a 1D polymeric chain. Neighboring chains connect via H bonding interactions to generate a 2D network. It crystallizes in the monoclinic system, space group P2/c with a=0.556 79(7), b=0.896 06(12), c=2.187 3(3) nm, β=94.942(3)°, V=1.087 2(3) nm³, Z=2, D_c=1.390 g·cm^-3, F(000)=480, M_r=455.17, μ(Mo Kα)=0.924 mm^-1, R(F)=0.036 0, wR(F²)=0.101 0, S=1.013. CCDC: 254565.     

牛磺酸缩3，5-二溴水杨醛席夫碱镁配合物[Mg(Br2TSSB)(Phen)(H2O)]·H2O的合成及晶体结构

Reactions of bitter salt with taurine-3,5-dibromo-salicylaldehyde schiff base gave one new Complex [Mg(Br₂TSSB)(Phen)(H₂O)]·H₂O (Br₂TSSB=Taurine 3,5-dibromo-Salicylaldehyde Schiff Base, phen=o-phenanthroline), which was characterized by elemental analysis, IR and X-ray diffraction. The chemical formula weight of the complex is 625.58. It′s crystal belongs to monoclinic system with space group P2₁/c. The cell parameters are: a=1.814 2(3) nm, b=0.814 75(14) nm, c=1.641 7(3) nm, β=90.571(4)°, and Z=4, V=2.426 4(7) nm³, Dc=1.712 g·cm^-3, F(000)=1 248, μ=3.496 mm^-1. The complexes form a 3D net structure in which they are connected with hydrogen bonds and π-π stacking. The Mg(II) formed a distorted coordination tetragonal pyramid. CCDC: 286194.     

N，N′-双(4-甲基-2-苯并噻唑基)-2，6-吡啶二酰胺钴(Ⅱ)配合物的合成和晶体结构(英)

Treatment of deprotonated N，N′-bis(4-methyl-2-benzothiazolyl)-2, 6-pyridicarboxamide (L^2-) with CoCl2·6H2O yields the mononuclear complex, (Et₄N)₂[CoL₂]·0.5H₂O. Single crystal X-ray structural determination has been carried out for the complex, crystal system: Monoclinic, space group: P2₁/c, a=1.444(1) nm, b=1.969(1) nm, c=2.448(1) nm, β=118.02(1)°, V=6.143 0(15) nm³, Z=4. In this complex, the central Co(Ⅱ) atom is in an octahedron environment, with four deprotonated amide-N atoms in the equatorial plane and two pyridine-N atoms in the axial positions. CCDC: 252558.