新型咔唑衍生物的合成及其晶体结构

通过9-乙基咔唑-3-甲醛与4-氨基-3,5-二甲基-1,2,4-三氮唑反应,合成了一种新型咔唑衍生物-- 9-乙基咔唑-3-甲醛缩4-氨基-3,5-二乙基-1,2,4-三氮唑(1),其结构经1H NMR, IR和X-射线单晶衍射表征.1属单斜晶系,P2(1)/n空间群,晶胞参数为:a=8.829(8)(A), b=9.863(10)(A), c=19.530(15)(A), β=101.65(5)°, V=1 666(3)(A)3, Dc=1.266 g·cm-3, Z=4, F(000)=672, μ=0.079 mm-1.最终偏离因子R1=0.075 6.     

新型镍配合物的溶剂热合成及其晶体结构

以2-乙氧基-6-亚氨甲基苯酚(HL)为配体,与氨水和Ni(ClO4)2.6H2O经溶剂热法合成了新型镍配合物[Ni(L)2](1),其结构经IR,元素分析和XRD表征。1属三斜晶系,Pī空间群,晶胞参数a=0.843 3(3)nm,b=1.009 4(2)nm,c=1.188 4(2)nm,α=111.16(3)°,β=97.43(3)°,γ=102.43(3)°,V=0.897 2(11)nm3,Mr=387.05,Z=2,Dc=1 433 g.cm-3,F(000)=404,μ=1.105 mm-1,S=1.015。1中Ni2-分别与两个L-上的两个N原子和两个O原子配位,形成了平面四边形几何构型。分子通过一对N-H┈O氢键形成二聚体;二聚体进一步通过N-H┈O氢键和C-H┈Ni氢键的相互作用形成二维网状结构。     

新型大环Schiff 碱化合物的合成及其晶体结构

以间苯二酚和二乙烯三胺为原料, 经缩合成环作用得到一新型Schiff 碱大环化合物1. 单晶X射线衍射结果表明, 该化合物属于单斜晶系, P21/c空间群, 晶胞参数为a＝0.81977(9) nm, b＝1.27817(14) nm, c＝1.60193(17) nm, α＝90°, β＝93.34(3)°, γ＝90°, V＝1.6757(3) nm3, Z＝4, R1＝0.0553, wR2＝0.1603. 在分子的大环结构中形成了四个N＋—H…O－离子型氢键, 化合物分子呈现为一四边形结构框架, 两个相互平行的苯环间存在较强p-p相互作用.     

Synthesis and Crystal Structure of a Novel Lactone Derived from Dehydroabietic Acid

A novel lactone derived from dehydroabietic acid,C20H21BrO4,has been charac-terized by IR,1H NMR,13C NMR and single-crystal X-ray diffraction method.It crystallizes in orthorhombic,space group P212121 with a = 6.4195(15),b = 11.535(3),c = 24.654(6) ,V = 1825.5(7) 3,Z = 4,Mr = 405.28,Dc = 1.475 g/cm3,λ = 0.71075 ,μ(MoKα) = 2.27 mm-1,F(000) = 832,the final R = 0.024 and wR = 0.045 for 2152 observed reflections with I 2σ(I).The molecules of lactone are mainly linked through intermolecular hydrogen bonds.     

Synthesis and Crystal Structure of Novel Fe_3 Cluster Compound

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Hydrothermal Synthesis and Crystal Structure of a Novel 3-D Porous Lanthanum Sulfate

A new lanthanum compound with three-dimensional channels, La₂(H₂O)(SO₄)₃ has been synthesized hydrothermally by using 1,2-dizminiopnopane as a structure-directing agent (SDA). The colorless block crystals were characterized by IR, TGA, ICP and XRD. The structure was determined by single-crystal diffraction. The title compound crystallizes in the orthorhombic, P2₁2₁2₁(No. 19) with cell parameters, a = 17.095(3) ?, b = 17.331(3) ?, c = 6.8633(12) ?, V = 1659.0(8) ?³, Z = 4, R = 0.0545, wR = 0.1246. The open framework of title compound is built up by LaO₁₀, LaO₉ polyhedra and SO₄ tetrahedra, connected to form interesting eight-membered ring channels along crystallographic a axis.     

基于萘基块新型开链冠醚的合成及晶体结构研究

以3,6-二溴-2,7-二羟基萘为起始原料,经与2-溴-N-苯基乙酰胺醚化,再用硼氢化钠和三氟化硼乙醚还原得基于萘基块新型的开链冠醚,两步总收率为96%.利用单晶X衍射研究其结构,晶体为三斜晶系,P-1空间群,a=9.588(3),b=10.898(3),c=13.060(4),α=103.190(4)°,β=93.953(4)°,γ=115.622(5)°,V=1176.0(6)3,Z=2,Dc=1.571 g/cm3,λ=0.71075 nm,μ(Mo Kα)=3.472 mm-1,Mr=353.22,F(000)=560.在晶体结构中,分子中的一个N—H基团与另外一分子形成双分叉氢键N—H…Br和N—H…O,进而组装成二聚体.这些中心对称的二聚体进一步通过C—H…π相互作用叠加成二维层状结构平行于(110)面.     

A Facile Synthesis and Crystal Structure of 1-Amino-3-(2''-methylphenyl)isoquinolin Hydrochloride

The title compound(C16H15ClN2)has been synthesized by a facile self-condensation of ο-tolunitrile promoted by potassium tert-butanolate in DMPU,and its structure was characterized by 1H NMR,13C NMR,IR,UV,HRMS and X-ray single-crystal diffraction.The crystal belongs to orthorhombic.space group Pna21 with a=19.560(3),b=7.8500(14),c=18.428(3)(A),Dc=1.271g/cm3,Z=8,λ=0.71073(A),μ(MoKα)=0.257 mm-1,Mr=270.75,V=2829.5(8)(A)3,Hack parameter=0.12(12),F(000)=1136,the final R=0.0571 and wR=0.1445 for 2701 observed reflections with I＞2σ(I).The intermolecular N-H…Cl hydrogen bonds link the molecules into a one-dimensional chain running along axis a.     

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 Novel Two-dimensional Layered Polymer

The title complex [Zn(μ-O2CCH=CHCO2)(C3H4N2)(H2O)]n was prepared by the reaction of zinc carbonate with maleic acid and imidazole in an aqueous-alcohol solution at 333 K, and its crystal structure has been solved by single-crystal X-ray diffraction. The complex crystallizes in the monoclinic system, space group Pc with a = 5.3858(7), b = 22.685(3), c =7.6782(1) A, β = 92.261(2)°, V = 937.4(2) A3, Z = 1, C14H16N4O10Zn2, Mr= 531.05, Dc= 1.882g/cm3,μ = 2.623 mm-1, F(000) = 532, the final R = 0.0372 and wR = 0.0930 for 1926 observed reflections with I＞2σ(I). The central zinc atom is five-coordinated in a distorted square pyramidal environment to three oxygen atoms of two different maleate ligands, a nitrogen atom of the imidazole ligand and an oxygen atom of water. In the complex two carboxylate groups of the maleate ligands have two coordination modes. One acts as a bidentate chelate ligand and the other a monoatomic monodentate ligand to bridge two zinc centers. As a result, 1-D infinite polymeric coordination water OH groups and carboxylate oxygen atoms to construct a 2-D layered polymer,and the layer structure is stabilized by π-π stacking of the imidozel ligands.     

三苄基锡吗啉二硫代氨基甲酸盐的合成、表征及晶体结构

利用三苄基氯化锡和吗啉二硫代氨基甲酸钠反应,合成了三苄基锡吗啉二硫代氨基甲酸盐。通过元素分析、红外光谱、核磁共振氢谱和质谱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。化合物为三斜晶系,空间群P1,a=0.98417(16)nm,b=1.08163(19)nm,c=1.3788(2)nm,α=72.850(3)°,β=88.895(3)°,γ=64.231(3)°,Z=2,V=1.2528(4)nm³,D_x=1.469g·cm^-3,μ(MoKα)=1.204mm^-1,F(000)=564,R₁=0.0215,wR₂=0.0531。化合物中,锡原子呈五配位畸变三角双锥构型。     

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 Supramolecular Structure of a Novel :r-Extended TTF Derivative

A novel x-extended TTF derivative (C24H20N6S8, Mr=649.02) has been synthesized and characterized by IR,1H NMR and MS. The crystal structure was prepared by crystallization from CH2Cl2-MeOH. The crystal belongs to the monoclinic system, space group P21/c with a=5.465(5), b=26.835(5), c=10.180(5) A, β=101.929(5)°, V=1460.7(15) A3, Z=2, Dc=1.476 g/cm3,F(000)=668,μ=0.638 mm-1, the final R=0.0390 and wR=0.0586 for 1694 observed reflections with I > 2σ(I). The structure reveals planarity of the two dithiole tings, different from the boat-shaped structure usually found in neutral derivatives of TTF. The central ring of the benzene also adopts a planar conformation, while it is twisted from planarity of the two dithiole rings and forms a dihedral angle of 61.8°. The molecule exhibits a three-dimensional supramolecular architecture constructed through hydrogen bonds. In the molecular structure a noticeable feature can be found that there exist S…S interactions which further reinforce the 3D supramolecular framework.     

双缩二氨基硫脲类化合物的合成与结构

合成了1，5-二（4-甲氧基苯甲醛）双缩二氨基硫脲（1），1，5-二（对二甲 基氨基苯甲醛）双缩二氨基硫脲（2），1，5-二（2-呋喃甲醛）双缩二氨基硫脲（ 3）三个化合物，并通过元素分析、红外光谱、核磁共振、质谱进行了结构表征。 首次报道了双缩二氨基硫脲类化合物的^13C NMR数据，并发现在溶液中由于构象异 构体或二聚体的存在，该类化合物的部分^13C NMR谱峰出现矮而宽、不易检测的特 征。配体1形成的晶体为单斜晶系，具有P21/c空间群，a=1.4363(3)nm，b=1.2622 (2)nm，c=1.0970(2)nm，β=101.730（10）°，V=1.9472（6）nm^3，Z=4，Dc=1. 318g/cm^3，μ=0.193mm^-1，F(000)=816，R1=0.0560，ωR2=0.1496。由于分子间 弱氢键力的作用，在晶体中以二聚体的形式存在。     

一种新颖酰基硫脲金属簇合物的合成与晶体结构

报道了一种新型酰基硫脲金属簇合物[Cu₆(HL)₆] (HL＝N-乙氧羰基-N'-4-氟苯基硫脲)的合成和晶体结构. 对化合物用元素分析、红外光谱、核磁共振谱、差热-热重分析确定了配合物的组成, 并经X射线单晶衍射法确定了其单晶结构. 晶体结构表明, 该化合物属于三斜晶系, 空间群, a＝1.2508(11) nm, b＝1.3011(11) nm, c＝1.4686(12) nm, a＝102.401(14)°, β＝97.859(2)°, γ＝114.700(13)°, V＝2.051(3) nm³, Z＝1, D_c＝1.687 Mg/m³. 标题化合物是由六个铜离子和六个硫脲配体组成的笼状金属簇合物, 每一个硫脲配体上与乙氧酰基相连的氮原子与铜进行配位, 并且配体上硫羰基上的硫原子与铜也发生配位作用, 使它们互相连接形成畸变的多面体结构.     

Hydrothermal Synthesis and Crystal Structure of a Novel Polymolybdate with Two Kinds of Organonitrogen Ligands

A novel inorganic-organic compound (C4N2H12)(C2N2H10)2[Mo5P2O23] (1) has been synthesized by the reaction of (NH4)2MoO4, H3PO4, C2N2H8 (ethylenediaminium), C4N2H10·6H2O (piperazine hexahydrate) and water in aqueous solution under mild hydrothermal conditions. Single-crystal X-ray analysis reveals that the title compound is crystallized in the triclinic system, space group P1 with a = 9.258(19), b = 9.382(19), c = 17.681(4), α = 76.28(3), β = 84.48(3), γ = 70.82(3)o, V = 1408.9(6)3, Mr = 1122.04, Z = 2, Dc = 2.645 g/cm3, μ = 2.384 mm-1, F(000) = 1092.0, the final R = 0.0391, wR = 0.1185 and S = 1.006 for 6169 observed reflections with I > 2σ(I). The crystal packing is stabilized by intra- and intermolecular N-H···O hydrogen bonds to form an infinite 3D network.     

取代萘并吡喃的合成和晶体结构研究

以芳醛、丙二腈（或氰乙酸酯）、β－萘酚为原料在六氢吡啶存在下以乙醇为 溶剂一锅合成了取代萘并吡喃，产物的结构通过单晶X射线衍射分析确定。     

多叠氮基三唑类高氮化合物的合成与晶体结构

2,5,2'-三氯-1,1'-偶氮-1,3,4-三唑(1)与叠氮化钠反应首次合成含有多叠氮和四氮烯(N—N＝N—N)结构的高氮化合物2,5,2'-三叠氮-1,1'-偶氮-1,3,4-三唑(3). 在相同条件, 2,5,2',5'-四氯-1,1'-偶氮-1,3,4-三唑(2)与叠氮化钠反应没有得到2,5,2',5'-四叠氮-1,1'-偶氮-1,3,4-三唑(b), 而是得到其分解产物3,5-二叠氮基-1,2,4-三唑(4). 用X 射线单晶衍射测定了化合物3和4的晶体结构. 晶体2b通过分子间氢键的相互作用形成具有9元环的三聚体,并由于三唑环共轭体系使氮上的H原子具有酸性,从而导致互变现象发生.     

ZnTPP Axially Coordinated with a Novel Dipyridylamine Ligand: Hydrothermal Synthesis and Crystal Structure

A novel complex ZnTPPL1·3DMF 1(TPP = tetraphenylporphyrin,L1 = N-(4-(9-carbazolyl) phenyl)-N,N-di(4-pyridyl)amine) was prepared by a hydrothermal method and characterized by elemental analysis,IR,and single-crystal X-ray diffraction analysis.Compound 1 crystallizes in triclinic,space group P1 with a = 13.3082(2),b = 14.3276(2),c = 18.6120(3) ,α = 109.853(1),β = 95.054(1),γ = 98.832(1)°,V = 3260.57(9) 3,Z = 2,Dc = 1.334 g/cm3,C81H69N11O3Zn,Mr = 1309.84,μ(MoKα) = 0.438 mm-1,F(000) = 1372,GOF = 1.159,the final R = 0.0482 and wR = 0.1479 for 12091 observed reflections(Ⅰ 2σ(Ⅰ)).Crystal structure analyses revealed that L1 utilizes one pyridyl N atom to bind Zn via axial coordination,affording a 1:1 complex.The binding constant was estimated to be 1.74(7) × 104 M-1 from electronic spectra measurements.     

Synthesis and Crystal Structure of 6—Bromo—piperonal—dimethyl—acetal

1 INTRODUCTION 6-Bromo-piperonal-dimethyl-acetal is an intermediate used for the synthesis of natural products, such as podophyllotoxin[1] and the related compounds[2～6] due to the useful biological activities associated with some of its derivatives[7, 8]. In particular, glycoside derivatives of 4?dimethyl- 4-epipodophyllotoxin have been used in cancer chemotherapy[9, 10]. The title compound has been synthesized from raw material piperonal, after bromo substitution and acetal protection…