一种具有超结构的[Zn(C_2H_8N_2)_3]Cl_2·2H_2O晶体

试图在Eu2O3、Zn粉、HCl、H_2S、Me4NCl、H_2O、CH_3COOH等起始物参加的反应系统中,合成某种二价铕配合物时得到一棱柱状透明[Zn(C2H8N2)3]Cl2 · 2H_2O晶体, 其主要晶体学参数如下：Mr = 350.60,单斜, C2/c, a = 26.3749(7), b =13.9613(5), c =12.9565(4) ?, β = 93.285(1) o, V = 4763.1 ?3, Z = 12, Dx = 1.467g·cm－3, μ(MoKα) = 1.885 mm－1, F(000) = 2208, R = 0.0552。单晶结构分析结果表明本文标题配合物具有一种超结构形式。     

[Cu(TOL)_4]Cl_2·2C_2H_5OH·2H_2O的合成和晶体结构

三唑醇(Triadimenol,简写TOL)是一内吸性的广谱低毒杀菌剂,主要用于禾谷类作物,腥黑穗病、丝黑穗病、散黑穗病、白粉病、锈病等病害的防治犤1～3犦。其化学名称为1-(4-氯苯氧基)-3,3-二甲基-1-(1H-1,2,4三唑-1基)丁基-2-醇,结构式如下:以农药为配体的金属配合物近年来逐渐被人重视犤4,5犦,它不仅保持了某些金属离子的杀菌特性,扩大了杀菌谱,而且作为一种缓释技术,使农药具有提高持效、延长半衰期、降低对哺乳动物的毒性以及使农药从非内吸性转化为内吸性等优越性。铜化合物作为杀菌剂使用已有60多年的历史,至今仍无抗性,由于其广谱、低毒,…     

配合物[Zn(tren)(H-SSA)]的合成、晶体结构及表征

A new mixed complex [Zn(tren) (H-SSA)] was synthesized based on the reaction of ZnO,5-sulfosalicylic acid and tren in water-methanol mixed solvents where tren was tris(2-aminoethyl)amine for the first time. The structure of the mixed complex was characterized by elemental analysis, IR, ¹H NMR and thermal analysis. The crystal structure of the complex was also determined by X-ray single crystal diffraction. Its crystal belongs to trigonal system with space group P3₁, a=1.109 67(18) nm, b=1.109 67(18) nm, c=1.236 8(4) nm, V=1.318 9(5) nm³; D_c=1.616 g·cm^-3; Z=3; F(000)=666; μ=1.553 mm^-1. CCDC: 253908.     

配合物[Zn(BCBI)2(H2O)4]·2H2O的合成及其晶体结构

以 ZnCl2,1,3-二羧甲基苯并咪唑为原料,采用常温溶剂挥发法,在甲醇水溶液中合成了Zn(Ⅱ)配合物{[Zn(BCBI)2(H2O)4]·2H2O(1) },其结构经IR,元素分析和X-射线单晶衍射表征.1属三斜晶系,P -1空间群,晶胞参数a=7.400 9(15)(A),b=9.406 6(19)(A),c=9.655 9(19)(A),α=81.58(3)°,β=75.97(3)°,γ=78.08(3)°,V=634.8(2)(A)3,Z=1,Dc=1.674 mg·cm-3,μ=1.050 mm-1,S=1.023.1中Zn(Ⅱ)与六个氧原子配位(两个氧原子来自两个配体H2BCBI分子中的羧基氧,四个氧原子为四个H2O的氧原子)形成变形的八面体构型.1的分子间氢键及H2BCBI间的π-π堆积将其拓展为三维结构,并对稳定晶体结构起着重要作用.     

三核镍配合物Ni_3(C_(14)H_8N_3O_5)_2(C_5H_5N)_4的合成、晶体结构和抗癌活性(英文)

The title complex Ni3(C14H8N3O5)2(C5H5N)4 has been synthesized by the reaction of 2-hydroxy-N′-(4- nitrobenzoyl)benzohydraizide with nickel acetate in pyridine solution. Its molecular structure was characterized by elemental analysis, IR spectra and X-ray crystal structure determination. Crystal data for this compound: Mono- clinic, space group P21/c, Mr=1 089.00, a=0.249 27(5) nm, b=0.161 40(3) nm, c=0.121 81(2) nm, β=94.59(3)°, V= 4.885 2(17) nm3, Z=4, Dc=1.481 Mg·m-3, F(000)=2 232, R1=0.049 7, wR2=0.106 8 (observed reflections with I2σ(I)) and R1=0.105 1, wR2=0.119 4 (all reflections), GOF=1.021. The complex was evaluated for their antitumor activi- ties against two kinds of cell lines (K562 and BGC) by MTT method. A preliminary bioactivity study indicates that the complex shows distinct antitumor activity.     

超分子化合物[Ni(C_6H_4O_2N)_2·(H_2O)_4]_n的水热合成及晶体结构

用皮考林酸和六水合氯化镍反应制备了一种三维氢键超分子配合物,经X射线衍射分析确定了单晶结构.该晶体属单斜晶系,P21/m空间群,晶胞参数为:a=0.976 0(2)nm,b=0.522 54(10)nm,c=1.450 1(3)nm,Mr=374.98,α=90.08(3)°,β=90.08(3)°,γ=90°,V=0.739 63(3)nm3,Z=2,ρ=1.684 g/cm3,F(000)=388,μ=1.357 mm-1,R=0.039 0,wR=0.090 8.共收集2 656个衍射数据,其中1 569个为独立衍射点(Rint=0.033 2),可观测点数1 382个(I>2σ(I)).结果表明,在组成该超分子体系的基本结构单元[N i(C6H4O2N)2.(H2O)4]中,N i(Ⅱ)离子形成六配位的稍拉长的八面体构型,配合物单元之间通过氢键相互连接,形成了无限延伸的具有网状结构的三维超分子体系.     

新型配位聚合物[Zn6(bta)4(2,2''''-bipy)3 ]的合成、晶体结构和荧光性质

采用水热法合成了一种新的三维配位聚合物[Zn6(bta)4(2,2'-bipy)3](H3bta=1,3,5-苯三乙酸; 2,2'-bipy=2,2'-二联吡啶), 并通过X 射线单晶结构分析、红外光谱、元素分析和热重分析对该配合物进行了表征. 结构分析数据表明, 该配合物属单斜晶系, Cc空间群, 晶胞参数a=1.7714(4) nm, b=2.4391(5) nm, c=1.7120(3) nm, β=104.39(3)°, Z=4, V=7.165(2) nm3, Dc=1.722 g/cm3, μ=2.065 mm-1, F(000)=3768, R1=0.0645, wR2=0.1424. 荧光光谱结果表明, 配合物具有良好的荧光性质.     

配合物[M(C_(14)H_(10)N_4)_2·HPO_4]·0.25H_2O(M=Cd,Mn)的水热合成、晶体结构及荧光性质

通过水热反应,合成了2种新的2,2′-联苯并咪唑超分子配合物[M(C14H10N4)2·HPO4]·0.25H2O(配合物1:M=Cd,配合物2:M=Mn)。经元素分析、红外光谱、热重对其结构进行了表征,用X-射线单晶衍射测定了该化合物的晶体结构。两晶体均为三斜晶系,P1空间群,均由1个M髤离子、2个2,2′-联苯并咪唑分子、1个磷酸氢根阴离子及0.25个结晶水组成。其中2,2′-联苯并咪唑分子中的碱性氮原子和磷酸氢根阴离子中的氧原子与M髤离子配位,形成6配位的畸变八面体构型。分子之间通过氢键N-H…O和π-π堆积作用相互构成二维层状超分子结构。室温固态荧光测试显示,配合物1在491.0nm(λmax)具有强的荧光发射。     

新型夹心双核配和物[Zn_2(ABTC)(phen)_2(H_2O)_6·2H_2O]的合成及其荧光性能

以3,3',4,4'-偶氮苯四羧酸(ABTC)和1,10-菲罗啉(phen)为配体,金属Zn(Ⅱ)为配位中心,采用溶剂挥发法在乙醇水中合成了新型夹心双核配合物[Zn2(ABTC)(phen)2(H2O)6·2H2O(1)],其结构和荧光性能经元素分析,X-射线单晶衍射和FL表征。1属单斜晶系,空间群C12/c1(15),晶胞参数a=24.774(3),b=12.853 8(13),c=14.698 3(15),β=94.195(2)°,V=4 668.0(8)3,Dc=1.584 Mg·cm-3,Z=24,F(000)=2 232,μ=43.083 mm-1,Goo F=0.969,R1=0.164 2,ωR2=0.047 3。ABTC作为桥梁配体,夹在两个配位中心中间。通过两个游离的水分子及配位分子的氢键作用,堆积成三维超分子孔道结构。在280 nm激发波长激发下,1在415 nm处有强的荧光发射峰。     

混配配合物[Zn(CF3COO)2(C7H6NS)2]的合成、晶体结构及表征

A mixed complex [Zn(CF₃COO)₂(C₇H₆NS)₂] was synthesized based on the reaction of Zn(CF₃COO)₂ and 2-aminobenzothiazol (C₇H₆NS) in methanol. The structure of the complex was characterized by elemental analysis, IR, ¹H NMR and thermal analysis. The crystal structure of the complex was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group C2/c, a=3.174 3(9) nm, b=1.010 0(3) nm, c=1.723 1(5) nm, β=118.841(4)°, V=4.839(2) nm³; D_c=1.625 g·cm^-3; Z=8; F(000)=2 368; μ=1.266 mm^-1. CCDC: 600233.     

(C5H7S2)2[Cu3I5]的合成和晶体结构

我们曾经对二硫代乙酰丙酮和多种金属离子的配合反应进行了系统的研究.在成功合成(C_5H_7S_2)_2[CuBr_3]的基础上,最近我们试图用类似方法合成(C_5H_7S_2)[CuI_3].但对产物晶体的X 射线衍射分析结果却表明,所得到的化合物的分子式为(C_5H_7S_2)_2[Cu_3I_5].[Cu_3I_5]~(2-)是以[CuI_3]配位三角形和两个相邻[CuI_4]配位四面体连接的无限链状配合阴离子形式存在.     

SYNTHESIS AND CRYSTAL STRUCTURE OF POLYMERIC STRUCTURE CONFLEX [Ag_2(C6H5CS_2)_2]_n

<正> Structural units Ag2(C6H5CS2)2,in which the distance between the unbridged silver atoms is only 2.890A, are connected by Ag...S interactions of neighbouring units along a and b axes to form a nonmolecular poly-meric structure [Ag2(C6H5CS2)2]n.     

THE CRYSTAL STRUCTURE AND SECOND-HARMONIC EFFECT OF COMPOUND C_9H_9N_3O_6· C_5H_5N

<正> The title compound (PAP) with excellent nonlinear optical prpper-ties has been synthesized. CHCHSCOO , monoclinic with space group P21, a = 4. 521(1), b = 9.601(6), c=17. 892(2)(?) , β=96. 12(1)°, V =772.8(?)3, Z = 2, Dc=1.44g · cm-3, F(000)-348, μ= 1.24cm-1. The second-harmonic intensities of PAP, MAP and NaAP HAP were measured,with the values which are 100, 50, 5. 0 times as large as that of KDP, respectively, Indicating that PAP is a new NLO crystal.     

CRYSTAL AND MOLECULAR STRUCTURE OF [K(18-CROWN-6)][Bi(SCN)Cl_3]

<正> The crystal and Molecular structure of [K(18-crown-6)](Bi(SCN)Cl3] has been deterained by X-ray diffraction Method. Its crystal is triclinic, space group Pl,with a = 9.233(4), b = 11.661(5), c=11.738(5)A,a= 81.82(4)° ,β=71.47(4)°,γ=75.55(4)°, and Z = 2. The final structural refine-ment converged with unweighted and weighted R factors of 0.051 and 0.047 for 2924 observed reflections. Results of the structure analysis indicate that the K+ ion enters the cavity of the 18-crown-6 to form the complex cation and one Bi(Ⅲ) atom, one SCN ligand and three Cl atoms fora the anion. Each Bi(Ⅲ) atoa is coordinated by four Cl atoas, of which two are shared with other Bi(Ⅲ) atom, one N atom and one S atoa from two SCN ligands respectively shared with a third Bi(Ⅲ) atoa, forming octahedral geometry.     

STRUCTURE OF MACROSPEGATRINE, [C_(40)H_(46)N_4O_3]Cl_2·3(H_2O)

<正> Mr=322.9, orthorhombic, P212121,a=19.867(4), b=15.793(3),c= 12.997(2)A, Z=4, Dc=1.23gcm-3,λ(CuKα)=1.5418A,μ=17.06cm-1, F(000)=1552. Final R=0.096 for 2764 unique diffractions with I≥3σ(I). Macrospegatrine obtained from the root of raurolfia Verticillata(Lour) Baill.f.rubrocarpa H. T.Chang.mss is a complex which involves double skeletons. It is a new alkaloid.     

THE CRYSTAL AND MOLECULAR STRUCTURE OF A FURAN-2-CARBOXYLATE HETEROBIMETALLIC COMPLEX [Zn(H2O)6]2+[Zn8Na2(C5H3O3)18(OH)2]2-

Abstract

The crystals of a zinc-sodium complex with furan-2-carboxylate (FCA) as a ligand, n[Zn(H₂O)₆]²⁺[Zn₈Na₂(FCA)₁₈(OH]₂]^2- _n , contain hexahydrated zinc cations and polyanions in which four differently coordinated zinc(II) cations are bridged by bidentate and monodentate (FCA) ligands. In addition, a number of carboxylate and furan ring oxygen atoms are coordinated to sodium(I) atoms which constitute the backbone of the polyanion. [Zn(H₂O)₆]²⁺ cations are located in cavities formed by adjacent polyanions and interact with them via a system of hydrogen bonds. The resulting molecular layers are stacked in the crystal along the [100] direction.     

CRYSTAL STRUCTURE OF TRINUCLEAR MOLYBDENUM CLUSTER H(Mo_3O(OAc)_3Cl_6)·3H_2O

<正> INTRODUCTION. Reacting of MoCl_3·3H_2O with organic ligands to-synthesize di- and trinuclear molybdenum complexes is an interesting research area. We wish to report the crystal structure of the title compound. It is one of our research results on structural chemistry of di- and trinuclear molybdenum complexes. The title compound was synthesized by reacting of MoCl_3·3H_2O with CH_3COCl。     

[(CH_3)_4N]_2Na[Mo_2O(S_2)_3S_5]·H_2O的合成和晶体结构

标题晶体属斜方晶系,空间群Pbn2_1,a=9.086(2),b=13.439(3),c=22.858(11),V=2791,Z=4,Dc=1.927g/cm~3。在CAD—4衍射仪上收集强度数据,采用直接法和Fourier技术解出结构,并用全矩降最小二乘法修正。对于1180个独立衍射最终偏离因子0.067。结构中的阴离子与其同系物[(CH_3)_4-N]_2K(Mo_2O(S_2)_3(NO)_2]·H_2O中的阴离子配位情况相似。只是结构中的Mo—S与Mo—O键长有差异。这种差异在两者的红外光谱上有着相应的表现。     

SYNTHESIS AND CRYSTAL STRUCTURE OF WCu_4S_4Cl_2Py_6

<正> Introduction. In recent years, the di-, tetra-. hexa-nuclear mixed metal cluster compounds of tungsten have been studied. In these compounds, more stable (WO_4-nSn)~2- skeleton remains unchanged. So far the penta-, hepta- and other polynuclear cluster compounds of tungsten have not yet been found. We describe here the preparation and structure of a new pentanuclear tungstencopper mixed metal cluster compound WCu_4S_4Cl_2y_6