A novel heteropoly tungstomolybdophosphate, [CH3NH3] [NH3 (CH2) 6NH3]H-3[P2Mo2W16O62].H2O has been synthesized and characterized by elemental analysis, IR, TGA-DSC and single-crystal Xray structure analysis. Crystal data: monoclinic, space group P2(1)/m, a = 1.259 6(3) nm, b = 1.871 5 (4) nm, c = 1.981 6(4) nm, alpha = gamma = 90degrees, beta = 90.16 (3)degrees, V = 4.671 (2) nm(3), Z = 2, M-r = 4 358.66, D-c = 3.100 g.cm(-3), mu = 19.978 mm(-1), F(000) = 3 792, R = 0.083 5, R-w = 0.2026. The structure analysis shows that a kind of micropore with size of 0.736 4 nm X 0.835 4 nm was formed in the crystal structure.

Sodium diacetate(SDA) is both an effective preservative mould-inhibitor can be used extensively in food feed industry.On the basis of developing a new technology to synthesize SDA successfully without any pollution, the single crystal of SDA in perfect shape suitable for X-ray diffraction was obtained. The crystal structure determined with four-circle diffractometer indicates that all the hydrogen-oxygen linkages in O-H...O of SDA crystal are the same equal to 0.1232 nm,in other words, the H atom in O-H...O linkage is located in the right center between two O atoms.This phenomenon appears very rarely in structural chemistry,and according to the suggestion of Professor XU Guang-xian ,the linkage O-H...O is not an ordinary hydrogen bond,but belongs in essence to a special covalent bond among three atoms provided with polyelectrons can be named as symmetrical hydrogen bond . In this article, the structure-activity relation and the symmetrical hydrogen bond are also dealt with to some extent.

在乙腈中,以12-钼钨磷杂多酸和8-羟基喹啉为原料,合成了标题配合物[Mo(Ⅱ)(C9H6NO)2(H2O)2]淡黄色四方柱状晶体,并测定了其单晶结构.晶体属单斜C格子,空间群为Cc,每一晶胞中有4个配合单元,形成链状结构.晶胞参数为α=1.3358(3) nm, b=0.9412(2) nm, c=1.3550(3) nm, β=109.71(3)°, V=1.6038(6) nm3, Z=4, Dc=1.741 g/cm3, F(000)=848,结构的偏离因子R=0.0237, ωR=0.0648.KMnO4滴定法、ESR和磁化率测定表明,该配合物显顺磁性,μeff=4.81 B.M, n=4.钼(Ⅱ)离子周围有反式氧配位,O(1)-Mo-O(2)键角为150.89(12)°,其配位数是6,形成畸变八面体.

合成表征了32个标题化合物BOCOCHR1CH2SnCl3·(2-HOC6H4CH＝NC6H4-X)(R=Me,Et,n-Bu;R1=H,Me;X=H,4'-Cl,3'-Br,3'-OH,3',4'-Cl2,4'-OMe),通过元素分析,UV-vis,IR和1H NMR进行了表征.n-BuOCOCh2CH2SnCl3·(2-HOC6H4CH＝NC6H4OMe-4')的晶体结构分析表明,该晶体属单斜晶系,a=1.4661(3)nm,b=0.9307(2)nm,c=1.7888(4)nm,β=94.04(3)°;V=2.43489m3,Z=4;空间群P21/c.该化合物为含有分子内羰基氧配位,Schiff碱以酚羟基上的氧原子配位,中心锡原子为六配位,空间构型为畸变八面体构型的单分子有机锡化合物.

A manganese molybdenum phosphate, (NH3CH2CH2NH3)10(H3O)3(H5O2)Na2[MnMo12O24(OH)6 (PO4)4(PO3OH)4][MnMo12O24 (OH)6(PO4)6(PO3OH)2]·9H2O, has been hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. The structure of this compound may be considered to be two [Mo6O12(OH)3(PO4)2(HPO4)2]7- units bonded together by a manganese atom, although several P–O groups are not protonated on account of coordination to a Na+ cation. One-dimensional tunnels were formed in the solid. A probe reaction of the oxidation of acetaldehyde with H2O2 using this compound as catalyst was carried out in a liquid–solid system, showing that the manganese molybdenum phosphate has high catalytic activity in the reaction.

各种各样的氨基多羧酸类配合物多年来一直是化学家们较为感兴趣的研究课题之一[1～4].特别是近年来,氨基多羧酸类配体作为一些有毒重金属的排泄剂[5]和与一些放射性金属离子形成配合物后作为核医学的显影剂[6]等方面得到了广泛的应用.金属Hg是有毒的,一般情况下,人们不希望它留在体内,但有时人们又不得不接触和使用它.因此,研究金属离子Hg2+与氨基多羧酸类配体形成配合物的性质及结构对于更好地了解Hg的生物活性会有一定的帮助.过去人们曾普遍认为金属离子Hg2+配合物的配位数是比较低而且比较单一的.最近的实验结果表明,如果配体合适,金属离子Hg2+也能形成相当高配位数的配合物.继八配位的[Hg(Ⅱ)(nta)2]4-配合物[7]之后,本文又报道了金属离子Hg2+与edta(乙二胺-N,N,N′,N′-四乙酸)形成的配合物,通过X-射线衍射仪的测定,得到了它不太常见的配位结构.

A novel heteropoly tungstophosphates, H-8[P4W14O58Na4(H2O)(20)] . 16H(2)O, was synthesized by hydrothermal method and characterized by elemental analysis, IR spectrum and single-crystal X-ray structure analysis. The thermal stability of the compound was investigated by using TG-DTA. The crystal is triclinic system with space group P (1) over bar, a = 1. 137 9(2) nm, b=1. 363 2(3) nm, c=1. 627 1(3) nm; alpha=78. 20(3)degrees, beta=71, 20(3)degrees, gamma= 71. 62(3)degrees; V = 2. 252 5(8) nm(3), Z=1, M-r= 4 374. 38, D-c = 3. 225 mg/cm(3), mu = 18. 007 mm(-1), F(000)=1 972, R=0. 074 2, R-w=0. 200 4. The result of structure analysis shows that the anion of the compound consists of two PW7O29Na2(H2O)(10) subunits and two linked phosphorous atoms. A kind of microporous with size of 0. 661 4 nm X 0. 318 9 nm was formed in the crystal structure.

金属离子ZnⅠ和HgⅠ分别是生物体必需的微量元素和对人体有害的毒性金属.如何有效地摄取ZnⅠ和排除HgⅠ一直是化学家感兴趣的研究课题.而ZnⅠ和HgⅠ能与各种氨基酸形成配合物,由于它们处于同一族,电子结构都是dl0,故其配位结构只取决于金属离子半径的大小和配体的形状[1～3].