反式-1,2-双[5-(2,5-二甲基苯基)(口恶)唑-2-基]-环丙烷的晶体结构与构象

合成了标题化合物并测定其晶体结构.晶体属P2₁/c空间群,a=1.3465(2)nm,b=0.8021(1)nm,c=1.9277(37)nm;β=105.99(1)°,Z=4.分子力学法计算与测定结果一致,环丙烷环与噁唑环间呈g式构象,与噁唑环π体系间有共轭效应,讨论了构象对紫外光谱的影响.     

细胞毒活性二萜Wangzaozin A的晶体结构

采用单晶X射线衍射技术对对映-贝壳杉烷化合物WangzaozinA的晶体结构进行了研究.研究结果表明,在最小不对称单元中存在两个构象稍有差异(键长和键角不同)的分子,其中两者的3个六元环均为椅式构象,而五元环为扭曲信封式构象.WangzaozinA晶体结构属正交晶系,P2₁2₁2₁空间群,晶胞参数a=0.66485(8)nm,b=2.5796(4)nm,c=1.0473(2)nm,Z=4.分子通过分子内氢键O₃-H₃0…O₂和O₃'-H₃0'…O₂'以及分子间氢键O1-H10…O₃,O1'-H10'…O₃',O₂-H₂0…O₄'和O₂'-H₂0'…O₄形成网络结构,并在晶体中沿c轴排列.体外抗肿瘤实验证实,标题化合物具有显著的细胞毒活性,由SRB法测试其抗Bel-7402及HO^-8910细胞株的IC₅₀值分别为(5.32±0.79)和(4.10±1.00)μmol/L.     

应用分子图形学、分子力学、量子化学及静电势研究农药分子结构与性能关系(XI)──抗植物病毒病药物──胡椒醛肟醚基-4-喹唑啉的结构特征

测定了标题化合物的晶体结构,它是由2个相似结构的化合物分子组成.晶体属单斜晶系,空间群为P2₁,晶胞参数:a=0.8431(3)nm,b=0.7297(1)nm,c=2.1880(7)nm,β=100.90(3)°,V=1.322(1)nm₃,Z=2.应用分子力学程序MMX及逐步旋转单键法探讨了它的构型和其它可能的优势构象.还应用MNDO方法计算了电荷分布及CNDO/2方法计算了静电势.结果表明,在该化合物中存在3个明显的负电区域,此结构与活性密切相关.     

二(四氢糠基茚)稀土氯化物的合成及晶体结构

将四氢糠基茚锂分别与无水三氯化钇和无水三氯化钆以摩尔比2;1反应,除去不溶物和溶剂后,将产物在甲苯/THF中冷冻得到晶体(C₄H₇OCH₂C₉H₆)₂LnCl[Ln=Y(1);Ln=Gd(2)].这两种配合物都是单分子无溶剂化合物,在空气中稳定.配合物1和2的晶体结构都属于正交晶系,P2₁2₁2₁空间群,晶胞参数分别为a=1.04252(9)nm,b=1.47455(12)nm,c=1.49799(13)nm,Z=4,Dc=1.508g/cm³;a=1.03701(10)nm,b=1.47233(12)nm,c=1.51354(14)nm,Z=4,Dc=1.699g/cm³.它们的结构相似,但空间构象不同.稀土中心离子分别与两个茚中的五元环和两个氧原子及氯原子成键,形成九配位结构.     

(+)-O-萘基环状磷酰二胺酯的合成、晶体结构及绝对构型

合成了目标化合物(+)-O-萘基环状磷酰二胺酯,其结构由¹HNMR,³¹PNMR及元素分析确定,并在273K下进行了X射线衍射晶体结构分析.该化合物晶体属正交晶系,P2₁2₁2₁空间群,晶胞参数a=1.0028(4)nm,b=1.1406(4)nm,c=2.4455(8)nm,V=2.7971(18)nm₃,Z=4,Dc=1.212g/cm³,F(000)=1088,μ=0.129mm^-1.晶体的结构收敛最终偏离因子R和wR分别为0.0585和0.0827.Flackx参数为0.03(12).目标化合物中磷原子的绝对构型为S.     

第一个含桥基大环配体的CuⅡ-CoⅡ-CuⅡ异三核配合物的合成和结构

报道了结构新颖的异三核配合物[Co{Cu(μ-L>(N₃)₂}₂(H₂0)₂]·2H₂O的合成和晶体结构(H₂L:2,3-二羰基-1, 4, 8, 11-四氮杂十四烷).三核配合物由含有草酰胺外延桥基的大环铜(Ⅱ)配合物作为"配合物配体"与金属钴离子(Ⅱ)反应得到.晶体属单斜晶系,P2(l)/c空间群.a=0.77172(4) nm, b=1.531 30(3) nm, c=1.47298(7) nm,β=98.540(2)°, V=1.72137(13) nm³,Z=2,R=0.0843.晶体中包含三核配合物单元和溶剂水分子,并通过分子间氢键连成一维链状结构.     

双(2,4-二甲基戊二烯基)氯化钆的合成及晶体结构

合成双(2,4-二甲基戊二烯基)氯化钆{[2,4-(CH₃)₂C₅H₅]₂GD_cl}₂,并测定了晶体结构.晶体为单斜晶系,P2₁/n空间群.晶胞参数a=0.89141(18)nm,b=1.4486(3)nm,c=1.15925(15)nm,β=92.996(18)°,V=1.4949(4)nm³,Z=3.     

两种具有氢键网络的Ni(Ⅱ)-咪唑配合物的晶体结构和磁性

合成了两种配合物晶体[Ni(im)₆](NO₃)(OH)(H₂O)₄(Ⅰ)和[Ni(im)₄(H₂O)₂][C₆H₄(COO)₂](Ⅱ)(im=C₃H₄N₂).晶体结构测定表明,晶体(Ⅰ)属于六方晶系,空间群P6₃/m,a=0.8985(10)nm,c=2.1002(4)nm,V=1.4685(4)nm₃,Z=2,R=0.043,R_w=0.045.晶体(Ⅱ)属单斜晶系,空间群C2/c,a=2.2207(4)nm,b=0.7665(2)nm,c=1.6043(3)nm,β=120.60(3)°,V=2.3503(9)nm₃,Z=4,R=0.056,R_w=0.079.两种配合物在结构上的突出特点是通过氢键形成了三维无限伸展的氢键电荷传递体系,对分子间电子传递有调节和促进作用,从而对晶体的磁性质产生了一定影响。     

大环多胺配体BDBPH的设计合成及其晶体结构

用Pb(SN)₂作模板,2,6-二甲酰基对甲苯酚与二亚乙基三胺通过[2+2]缩合反应,经NaBH₄还原、脱Pb²⁺、酸化等操作,得晶体BDBPH·6HBr·4H₂O.晶体属单斜晶系,P2_1/c空间群,晶体学参数:a=1.4441(5)nm,b=1.1482(4)nm,c=1.2090(6)nm,α=90°,β=96.92°,γ=90°,V=1.9900nm³大环分子采取椅式构型,6个Br-和4个H₂O分子对称分布于大环两侧.该大环配体结构新颖,可用于多种金属配合物的研究,对进一步了解金属酶活性中心的结构及其催化作用机理具有重要价值.     

雷公藤内酯甲的制备和晶体结构

从雷公藤(TripterygiumwilfordiiHook.F.)根心部分的乙醇提取液中,采用硅胶柱色谱法和TLC方法得到纯的雷公藤内酯甲(WilforlideA).用IR,¹HNMR和元素分析表征,并测定其单晶结构.化合物分子式为C₃₀H₄₆O₃,M_r=454.70,晶体属正交晶系,P2₁2₁2₁空间群,晶胞参数:a=0.732(4)nm,b=1.283(7)nm,c=2.693(6)nm,V=2.5327nm₃,Z=4,D_c=1.192g·cm^-3,μ(MoKα)=0.695cm^-1,F(000)=1107,R=0.039,R_W=0.044,分子为五环三萜γ-内酯.分子中C22-C23为烯键,C11连有羟基,C33_O3为羰基,整个分子呈起伏状,不在同一平面内.从AM1计算结果可以看出,仲羟基中的O1及γ-内酯中的O3原子净电荷大,致使分子极性较大,易在O1和O3部位发生亲核反应和氧化还原反应,显示分子的反应活性     

8-羟基喹啉镍配合物[Ni2(HQ)3Q3]ClO4的晶体结构

8-羟基喹啉(HQ)是在化学分析中常用的试剂, 它与铝离子形成的配合物(AlQ3)也是目前有机电致发光领域最引人注目的明星分子. 在化学工业中, 8-羟基喹啉是有效的稀土及过渡金属的萃取剂, 它同中心离子的配合强度随条件改变亦有很大变化. 我们在钇和镍离子共同存在的条件下得到了标题化合物, 并测得其单晶结构.     

具有新颖结构的亚磷酸锌化合物的水热合成与表征

在水热体系中以二乙烯三胺为模板剂合成了结构新颖的亚磷酸锌化合物Zn(DETA)Zn₂(HPO₃)₃.单晶X射线衍射分析结果表明,该化合物属正交晶系,Cmca空间群,晶胞参数a=1.889 25(1)nm,b=1.001 04(5)nm,c=1.630 32(8)nm,β=90°,V=3.083 3(3)nm3,Z=4,DC=1.162 Mg.m^-3,最终因子R1[I>2σ(I)]=0.068 5,wR₂[I>2σ(I)]=0.160 5.该化合物的结构中含有{ZnO₄},{ZnO₂N₃}和{HPO₃}基本结构单元,其中{ZnO₄}和{HPO₃}通过桥氧原子共顶点相互交替连接形成具有4-,8-和12-元环的无限延伸的二维层.有趣的是,{ZnO₂N₃}结构单元以二聚体形式{ZnODETA}₂悬挂在12-元环孔道中,这种结构在亚磷酸锌中鲜有报道.     

Studies on α-Methacrylate Copper(Ⅱ) Complexes with Imidazole

Two complexes of α-methacrylate copper(Ⅱ) with imidazole, Cu[CH₂=C(CH₃)COO]₂· (imH)₂(1) and Cu ₂[CH₂C(CH₃)COO]₄(imH)₂(2) were prepared and characterized. The single crystal X-ray diffraction study of complex 1 showed that the copper(Ⅱ) atom in the symmetric centre of the square planar environment was coordinated by two monodentate α methacrylate groups and two imidazole ligands that were in trans position with each other. Each molecular unit is linked with four neighbouring units by means of hydrogen bond interactions, forming a two-dimensional supermolecular compound( d_N…O =0.278 1 nm). Complex 1 crystallizes in monoclinic, space group P2₁/n with a =1.023 94(12) nm, b =0.842 94(8) nm, c =1.079 35(10) nm, β=117.231(7)°, Z =2. The forming mechanism of the complexes was discussed.     

The crystal and molecular structure of N′-monomethylthiobinupharidine iodide dihydrate - the methiodide of nuphar alkaloid

The crystal structure of N′-monomethylthiobinupharidine iodide dihydrate has bee determined by single-crystal X-ray analysis. The crystals are orthorhombic, space group P2₁2₁2₁, with = 9.499(3), b = 15.522(5), c = 23.694(7) A. Block-diagonal least-squares refinement, with 2060 reflections measured on diffractometer, yielded a final value for R of 0.073. The cation was found to have a skeleton composed of two trans-quinolizidine systems with equatorially bonded methyl and furan groups; the central part of the cation (the tetrahydrothiophene ring) adopts a conformation between envelope and half-chair. Quaternization at the N(5′) atom does not change conformation of the quinolizidine. The results of X-ray analysis confirm the interpretation of the ¹³C NMR spectra.     

三维无机-有机杂化微孔化合物[Zn3(BTC)2(H2O)3]n的合成与结构

传统的沸石和分子筛微孔晶体材料是指以硅酸盐、硅铝酸盐、磷铝酸盐和无机金属磷酸盐为骨架的晶体材料^[1,2].     

Synthesis,Electrocatalytic Properties and Crystal Structure of a New Organic—Inorganic Hybrid Constructed from Dodecamolybdophosphoric Acid and Benzotriazole

IntroductionIn the last few years there has been a rapidlygrowing number of reports in the literature ad-dressing the use of polyoxometalate- based hybridmaterials as catalysts,non- linear optical materialsand anti- virus drugs[1— 5] . In all the cases men-tioned above,the size,the shape and the chargesof the inorganic counter anions strongly affect theproperties of the materials. Polyoxometalates arelarge in size and high in electron accepting abili-ty[6] .They can form novel compounds with …     

Two New Piperazine Templated Lanthanide Sulfates with 2D Corrugated Layered Crystal Structures

Two new piperazine templated lanthanide sulfates (C₄N₂H₁₂)_1.5[Ln(SO₄)₃(H₂O)]·H₂O[Ln=Gd(1), Tb(2)] have been synthesized solvothermally and structurally characterized by single crystal X-ray diffraction(XRD), infrared(IR) spectroscopy, thermal analysis, fluorescent spectra and inductively coupled plasma(ICP). Single crystal X-ray diffraction reveals that both compounds 1 and 2 crystallized in the monoclinic crystal system, with space group P2₁/c and cell dimensions: a=0.64468(19) nm, b=2.9979(9) nm, c=0.9818(3) nm, β=101.271(4)°, V=1.8608(10) nm³, Z=4 for compound 1; a=0.64259(19) nm, b=3.0010(9) nm, c=0.9812(3) nm, β=101.229(4)°, V=1.8560(10) nm³, Z=4 for compound 2. Compounds 1 and 2 are isomorphous and have similar 2D corrugated inorganic frameworks fabricated via the connection of single chains and S2O₄ groups, while fully protonated piperazine cations and water molecules are located between the inorganic layers. The solid state luminescent properties of compound 2 were investigated and it displayed a typical luminescent property of Tb³⁺ with excitation wavelength at 371 nm.     

rac-11-t-Butoxy-1,4-dihydro-1,4-methanoanthracene:A two-dimensional framework structure built from C-H…O and C-H…πhydrogen bonds

The title compound rac-11-t-butoxy-l,4-dihydro-l,4-methanoanthracene(C₁₉H₂₀O,M_r = 264.35) has been synthesized and characterized by FT-IR,’H NMR,HRMS spectra and single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P2₁/n,with a = 13.5240（10）,b = 8.3453（6）,c = 13.9604（9） ,β= 100.0190（10）°.The structure of the title compound comprises a norbomene unit with a t-butoxy group,having a naphthalene ring fused on one side.The naphthalene is essentially planar with a maximum deviation of 0.032（2） for atom C（3）.In the crystal,inversion-related molecules are linked by pairs of C-H…O hydrogen bonds,forming a cyclic dimer with R₂²（16） graph-set motif.The C-H…πinteractions are also observed,linking the molecules into a continuous two-dimensional framework structure.     

Synthesis and Crystal Structure of 1D Cd-amine Coordination Polymer and Its Luminescent Properties

A novel one dimension（1D） cadmium coordination polymer {[Cd（mpda）3]·2（NO3）}n（1） was synthesized via refluxing a mixture of tetradentate Schiff base ligand N,N＇-bis（2-pyridinylethylidene）phenylene-1,3-diamine（L） and Cd（NO3）2 in acetonitrile, whose structure was characterized by means of single crystal X-ray diffraction, FTIR spectroscopy, elemental analysis and proton nuclear magnetic resonance（1H NMR）. Center metal Cd（II） ion is six-coordinated by six nitrogen atoms from six different m-phenylenediamine（mpda）, giving rise to a [CdN6] octahe- dral coordination environment. The two adjacent cadmium centers are linked by three mpda molecules leading to the construction of 1D chain structure. The crystal structure is stabilized by N-H…O hydrogen bonds to form three-dimension supramolecule. Compound 1 exhibits intense yellow luminescence in solid state at 298 K（λem=554 nm）, which shows a blue shift at 77 K（ca. 147 nm）. Additionally, fluorescence characteristics of compound 1 were investigated in different solvents（polarity： DMSO〉CH3CN〉CH3OH〉CHC13〉toluene） at 298 and 77 K. The results show that the emission peak of compound 1 in solvent exhibits a slight bathochromic shift. However, the emission peaks of compound 1 in CH3OH and CHC13 are red shift compared with that in CH3CN. It is revealed that the lumi- nescence behavior of compound 1 depends on not only the polarity of solvent but also the hydrogen bonding proper- ties between solvent and solute. In addition, the emission peak of compound 1 in solution shows a red shift obviously at 77 K than that at 298 K（ca. 144-159 nm）, with the fluorescence lifetime increased at 77 K. The lifetime in DMSO at 77 K（r=12.470μs） was the longest one. The quantum yield of compoud 1 increases with increasing the polarity of solvent within a range of 1.8%-8.3 %.