Schiff碱6-甲基-N-氧化吡啶-2-甲醛缩硫代氨基脲的合成及晶体结构

合成了标题Schiff碱并测定了其晶体结构。化合物化学式为C8H10N4OS·H_2O, Mr = 228.27,晶体属单斜晶系,Cc空间群,晶胞参数： a = 13.251(3), b = 24.919(6),c = 13.670(3) ?,β= 101.334(5)°,V = 4425.8(19) ?3,Z = 16,Dc = 1.370 g/cm3,μ=0.280 mm-1, F(000)=1920, R = 0.0468,wR = 0.1417。化合物Schiff碱通过氢键作用,形成一种罕见的链状结构。同时与N-氧化吡啶-2-甲醛硫代氨基脲进行比较,讨论了结构变化。     

Synthesis and Structure of the Manganese Complex with 2-Aminopyridine N-oxide

1 INTRODUCTIONMany complexes of 2-aminopyridine N-oxide (apo) have been characterized by infrared spectra, X-ray powder diffraction spectra, and by magnetic measurements and electronic spectra to liquid nitrogen temperature, but very few are on their crystal X-ray studies[1~3]. We have been studying complexes of pyridine N-oxide ligands containing a donor substitutes at the 2-position, in an attempt to broaden the range of N-oxide ligands complexes[4,5]. As continuing work of research on…     

Schiff碱N-氧化吡啶-2-甲醛缩氨基硫脲的晶体结构

合成了标题Ｓｃｈｉｆｆ碱并获得了其单晶,化学式为Ｃ７Ｈ８Ｎ４ＯＳ,Ｍｒ＝ １９６．２３,经Ｘ射线单晶衍射分析,该晶体属于单斜晶系,空间群为Ｃ２／ｃ,晶胞参数： ａ＝ １３．１９８（２）,ｂ＝ ８．０７０（１）,ｃ＝ １６．９９９（２）,β＝ １０２．７６０（１０）°,Ｖ＝ １７６５．８（４）３,Ｚ＝ ８,Ｄｃ＝１．４７６ｇ／ｃｍ ３,μ＝ ０．３３０ｍ ｍ － １,Ｆ（０００）＝ ８１６,在２．４６°＜ θ＜ ２９．００°范围内以ω扫描方式收得独立衍射点２３４７ 个,其中Ｉ＞ ２σ（Ｉ）的可观测点为１６８７ 个。最终偏离因子Ｒ＝０．０３４４,ｗ Ｒ＝ ０．０８４３,（Δ／σ）ｍ ａｘ＝ ０．００１,Ｓ＝ １．０８２。分子为平面构型。与相应配合物的晶体结构进行了比较并讨论了配位前后标题化合物主要的键性质的变化。     

Synthesis and Crystal Structure of a Zinc(II) Complex Salt with the Schiff Base of Picolinaldehyde N-oxide and Semicarbazone

1 INTRODUCTION The donor properties of pyridine N-oxide and its substituted derivatives to form metal complexes have been widely investigated[1～3]. The resulting comple- xes were used as drugs[4] and catalysts[5]. So far, there have been a few reports on the synthesis of Schiff base derived from picolinaldehyde N-oxide with se- micarbazone (PNOS Scheme 1) and its metal com- plexes. And crystal structures of the complexes of PNOS with Au(III)[6], Pd(II)[7] and Cu(II)[8] were re- …     

Synthesis and Crystal Structure of a Zinc(Ⅱ) Complex Salt with the Schiff Base of Picolinaldehyde N-oxide and Semicarbazone

The title zinc(Ⅱ) complex salt [Zn(H2O)6](ClO4)2·(PNOS)4, where PNOS is derived from picolinaldehyde N-oxide with semicarbazone, has been prepared and structurally characterized by X-ray single-crystal analysis. It crystallizes in triclinic, space group P1 with a = 7.529(3),b = 10.206(4), c = 14.678(6) A, α = 86.293(6), β = 87.686(7), γ= 81.382(6)°, C28H44Cl2N16O22Zn,Mr = 1093.06, V= 1112.3(8) A3, Z = 1, Dc = 1.632 g/cm3, S = 1.089,μ(MoKα) = 0.773 mm-1 ,F(000) = 564, the final R = 0.0438 and wR = 0.1076 for 3888 independent reflections with Rint =0.0224. The crystal structure possesses a [Zn(H2O)6]2+ cation, two ClO4- anions and four PNOSs.In the crystal structure, Zn2+ cation is located at the symcenter and coordinated by six water molecules. In [Zn(H2O)6]2+, an elongate octahedral complex cation, the average Zn-O bond length is 2.087(2) A. There exist a lot of H bonds in the structure, linking the cation [Zn(H2O)6]2+, anion ClO4-and PNOS to form a 3D network.     

Synthesis and Structure of bis(μ-2-aminopyridine N-oxide)-bis[dichlorocopper(II)]

1 INTRODUCTIONMany complexes of 2-aminopyridine N-oxide (apo) have been characterized by infrared spectra, X-ray powder diffraction spectra, and by magnetic measurements and electronic spectra at liquid nitrogen temperature, but very few of them are their crystal X-ray studies[1~3]. Recently, a number of bridged binuclear copper (II) complexes have been reported, some of which have important potential applications in bioinorganic chemistry and materials[4~6]. Particularly, the complexes …     

秋水仙胺半合成新方法

秋水仙胺半合成新方法;秋水仙胺;秋水仙碱;半合成     

氧化-4-吡啶甲酸桥联的一维链状三丁基锡配合物的合成与晶体结构

利用双三丁基氧化锡与氧化-4-吡啶甲酸(HOCOC5H4NO)以物质的量比1∶2反应,合成了有机锡配合物[Bu3Sn(OCOC5H4NO)]n。通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征,用X射线单晶衍射测定了它的晶体结构。结果表明,该配合物晶体属单斜晶系,空间群为C2/c,晶胞参数a=2.002 8(9)nm,b=1.224 7(6)nm,c=1.913 6(12)nm,β=119.145(6)°,Z=8,V=4.166(4)nm3,Dc=1.365 g.cm-3,μ=1.239 mm-1,F(000)=1 760,R=0.052 9,wR=0.192 1,GOF=1.013。在配合物中锡原子由氧化-4-吡啶甲酸桥联为五配位的畸变的三角双锥构型。氧化-4-吡啶甲酸配体中N-O基团中的氧原子和另一配体中的羧基氧原子与中心锡原子配位,形成无限一维链状有机锡配合物。该配合物具有良好的热稳定性和较高的抗肿瘤活性。     

Synthesis and Crystal Structure of Tri—（2—mercaptopyridine N—oxide）bis（dimethyl sulfoxide） Dysprosium（Ⅲ）

A range of rare earth metal complexes of 2-mercaptopyridine N-oxide (Hmpo) have been synthesized, and studied by elemental analysis and IR spectroscopic technique. Crystal structure of Dy(mpo)3(DMSO)2 (DMSO = dimethyl sulfoxide) has been determined. The complex crystallizes in the triclinic system, space group Pī with lattice parameters: a = 9.602(3), b = 9.803(3), c = 15.498(5)A, α= 89.51(1), β= 85.73(1), γ= 62.99(1)°, Dc = 1.787 g/cm3, C19H24N3O5S5Dy, Mr = 697.21, Z = 2, F(000) = 690, μ = 3.321mm-1, the final R = 0.0237 and wR = 0.0587 for 4116 reflections with I>σ2(I). The coordination number of dysprosium Ⅲ is eight, and its coordination geometry is a somewhat distorted square antiprism with O(3), O(4), O(5), S(3) and O(1), O(2), S(1), S(2) at the tetragonal bases (dihedral angle between their mean planes is 2.9(1)0). Around the Dy atom, three five-membered ring planes (Dy, O, N, C, S) make the dihedral angles of 74.42, 11.31 and 83.72, respectively.     

Synthesis and Crystal Structure of Tri-(2-mercaptopyridine N-oxide)bis(dimethyl sulfoxide) Dysprosium(III)

1 INTRODUCTION Transition-metal thiolato complexes have been of interest for the simulation of many metallo- enzymes where the thiolato group mimics the ligation of cysteinyl residues in proteins. Numerous complexes of transition elements with 1,2-bidentate oxothiolate ligands have been prepared[1~4]. Re- cently, we have studied a few transition metal complexes of 2-mercaptopyridine N-oxide (Hmpo) as bactericidal and antifungal reagents[5～7]. Although Hmpo exhibits unusual versatility…     

配合物[Sb(mpo)2Cl]的合成及晶体结构(Hmpo = 2-巯基氧化吡啶)

标题化合物 C10H8ClN2O2S2Sb 由[C5H5NH][SbCl4]与 2-巯基氧化吡啶钠盐(Nampo)反应制得。其结构通过元素分析、IR 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,晶体属于三斜晶系, 空间群为 P1, Mr = 409.50, 晶体参数:a = 9.4022(6), b =10.2910(7), c = 14.4631(9) ?, α= 104.321(1), β = 96.978(1), γ = 90.179(1)?, V = 1345.09(15)?3, Z = 4, Dc = 2.022 g/cm3, μ = 2.553 mm–1, F(000) = 792。晶体结构用直接法解出, 经全矩阵最小二乘法修正,最终结构偏离因子 R = 0.0368, wR = 0.0854。化合物分子中, 锑与一个氯原子和两个配体 mpo 配位,形成五配位变形的四角锥构型配合物。在晶胞堆积图中,锑原子又与另一分子中的氯原子以次级键形式作用,形成缺位配位多面体构型。     

Synthesis and Crystal Structure of a One-dimensional Infinite Chain Organotin Complex [(n-Bu)_3Sn(OCOC_5H_4NO)]_n

1 INTRODUCTION Organotin esters of carboxylic acid are widely used as biocides and fungicides and as homogeneous cata- lysts in industry[1~3]. In recent years, the pharmaceu- tical properties of carboxylic acid have been investi- gated for the antitumour activity[4~6]. In general, bio- cidcal activities of organotin complexes are greatly influenced by the molecular structures and coordina- tion numbers of the tin atom[7, 8]. It is revealed that organotin complexes containing carboxylate l…     

新型对称联苯双酯类液晶材料的合成和晶体结构

设计并合成了4个对称联苯双酯类液晶化合物,化合物结构通过红外和核磁表征,它们的介晶性通过差示扫描量热仪(DSC),X射线衍射仪(XRD)和热台偏光显微镜(POM)进行了研究.并测定了4,4'-3,3',5,5'-四甲基联苯-二(4-甲基苯甲酸酯)(Ⅲa)的单晶结构,结果显示:晶体属于单斜晶系,P21/c空间群,晶胞参数为a=18.525(3)(A),b=12.196(2)(A),c=12.195(2)(A),β=97.142(2)°,V=2733.7(9)(A)3,Z=4,Dc=1.163 Mg/m3,R=0.0521,Rw=0.1161.化合物均为热致型互变液晶,并讨论了氧原子、不饱和端基和端基链长对介晶性的影响.     

Synthesis and Crystal Structure of Fe（aapo）2Cl3 （aapo=2—Acetylamino Pyridine N—Oxide

1INTRODUCTIONComplexesofpyridineN-oxideligandshavereceivedmoreandmoreattention,andwehavereportedsomeofthemcontainingadonorsubstituteatthe2-positioninanattempttobroadentherangeofpyridineN-oxidecomplexes[1,2].MostcrystalstructuresofpyridineN-oxidesreportedareaboutdivalenttransitionmetalionsM(Ⅱ)[1～4],withonlyaveryfewontrivalenttransitionmetalionsM(Ⅲ)[5].Asthecontinuingworkofsystematicresearch,herewewillpresentthesynthesisandstructureofthetitlecompound.Toourknowledge,itisthefirstexamplet…     

雷酚萜醇的结构研究

雷酚萜醇属雷公藤二萜类化合物。雷公藤(Tripterygium wilfordii Hook f)系卫矛科(Celastraceae)雷公藤属植物。民间用于治疗风湿病、抗炎、抗肿瘤及抑制免疫系统等。     

Synthesis and Crystal Structure of p-Ferrocenylethylbenzoate

1 INTRODUCTION In the last decade the chemistry of ferrocene and the design of new compounds containing fer- rocene have received much attention, associated with the utility of these compounds in many fields such as organic synthesis, homogeneous cata…     

Synthesis and Crystal Structure of Carvedilol

1INTRODUCTI0NCarvedilol,1-(4-carbazolyloxy)-3-[2-methoxyphenoxy)ethylaminoj-2-propanol,isanewgblockingandvasodilatingagent"'.IthadsynthesizedbyF.Wiedemannetalt23.Howeverthereportaboutcrystalstructureofcarvedilolhasnotbeenseen.Inthispaper,wediscussthecrystalstructureofthecarvedilolsynthe-sized[2ibythereacti0nof4-(2,3-ex0xypropoxy)-carbazoleand2-(2-methoxyphe-noxy)ethylamine.Sinceknowledgeofthemolecularandcrystalstructureofcarvedil0lwasconsideredusefulforunderstandingthemechanismoftheactio…     

Synthesis and Crystal Structure of a New Chain Coordination Polymer [Cu（inio）2（H2O）]∞ （Inio = Isonicotinic Acid N-Oxide）

1 INTRODUCTION With deep studies on the complex biology system and syntheses of new functional complexes, people have paid more and more attention to the polynuclear complexes. In the construction of one to three dimensional frameworks, multi-dentate ligands are usually used to bridge the metal centers to form polymeric structures[1, 2]. The isonicotinic acid N-oxide can function as a good mono-dentate ligand[3～8] through one oxygen atom from the group of -NO or carboxyl, and the dep…     

Crystal and Molecular Structure of Cyanuric Acid

ＣｒｙｓｔａｌａｎｄＭｏｌｅｃｕｌａｒＳｔｒｕｃｔｕｒｅｏｆＣｙａｎｕｒｉｃＡｃｉｄＣｈｅｎＣｈａｎｇ－Ｚｈａｎｇ；ＳｈｉＪｉａｎ－ＱｉｕＬｉｎＺｈｏｕ－Ｂｉｎ；ＧａｏＤｏｎｇ－Ｓｈｏｕ；ＨｕａｎｇＸｉａｏ－Ｙｉｎｇ；ＬｉＤｉｎｇ（ＦｕｊｉａｎＩｎｓ...     

Synthesis and Crystal Structure of a New Binaphthylamide

Novel binaphthylamide has been synthesized and characterized by IR and ¹H NMR spectra. The crystal structure of the compound was determined by X-ray diffraction (MoK radiation, 8629 reflections,R_F = 0.0436, R_W= 0.0856). Monoclinic crystals with unit cell parameters a=10.796(3), b=11.441(3), and c=34.565(9) , Z=4. The results reveal that the title compound forms a supramolecular structure.