(2S,4R)-2-(溴甲基)-2-(2,4-二氯苯基)-1,3-二氧环戊环-4-甲基苯甲酸酯的合成及晶体结构

合成了标题化合物并测定了其晶体结构。该化合物的化学式为C18H15O4BrCl2, Mr = 446.12。晶体为正交晶系, P212121空间群, 晶胞参数为: a = 7.1540(7), b = 23.367(1), c = 11.161(2) , V = 1865.7(3) 3, Z = 4, Dc = 1.588 g/cm3, F(000) = 896, (MoK? = 2.515 cm-1, R = 0.037, wR = 0.074, Flack系数为0.14(1)。晶体结构显示, 化合物中有2个手性碳原子, 为(2S,4R)构型, 整个分子呈沿b轴排列的波浪形的链状结构。     

对甲苯基硫脲和对溴苯基硫脲的晶体结构和电子结构

本文测定了对甲苯基硫脲(1)和对溴苯基硫脲(2)的晶体结构,并用 CNDO/2程序对生物活性较大的对甲苯基硫脲分子进行了量子化学计算。1属单斜晶系,空间群 P2_1/n,a=0.5618(1),b=0.8487(4),c=1.7865(3)nm,Bβ=93.53(1)°,Z=4,D。=1.298 g·cm~(-3),最终偏离因子 R=0.0396;2属单斜晶系,空间群 P 2_1/n,a=0.9096(6),b=0.8991(4),c=1.0659(8)nm,β=105.59(6)°,Z=4,D。=1.836g·Cm~(-3),最终偏离因子R=0.073。晶体结构测定结果表明,硫脲部分的四个原子组成平面三角形,苯环平面与硫脲平面的夹角分别为63.5°和68.6°。量化计算结果和晶体结构测定相吻合。     

K_3[Cr_3O(OOCH)_6(H_2O)_3][α-GeW_(12)O_(40)]·17H_2O的合成、结构及特性研究

研究了多金属氧酸盐分子基化合物K3[Cr3O(OOCH)6(H2O)3][α GeW12O40]·17H2O的合成、晶体结构及其结晶水可逆脱附和吸附性能.该化合物属于单斜晶系,C2/m空间群,a=2 7383(6)nm,b=1 5830(3)nm,c=1 7304(4)nm,β=102 43(3)°,V=7 325(3)nm3,Z=4,R1(wR2)=0 0678(0 1719).该晶体具有孔道结构,孔道内的结晶水能够可逆的脱附和吸附,而晶体结构随之恢复,因此具有分子筛的特性.     

Schiff碱水杨醛缩异烟肼和水杨醛缩4-氨基安替吡啉的合成和晶体结构

通过水杨醛和异烟肼,4-氨基安替吡啉的缩合反应分别合成了Schiff 碱水杨醛缩异烟肼1,水杨醛缩4-氨基安替吡啉2,并获得其单晶结构。用元素分析,UV-Vis和IR谱进行表征。晶体结构通过X-射线衍射法测定,晶体结构均用直接法解出, 经全矩阵最小二乘法对原子参数进行修正。化合物1:化学计量式为:C13H11N3O2,Mr = 241.25,晶体属于单斜晶系,空间群P21/n, 晶胞参数:a = 8.153(1),b = 15.574(4) , c = 9.554(2) ? b =105.48(1)? V =1169.1(4) ? , Z = 4, Dc =1.371 g/cm3 , m =0.096 mm-1, F(000) = 504,结构偏离因子R = 0.0832, wR = 0.1158,共收集到2384个独立衍射点,其中其I >2(I)的可观测点为2059个。化合物2:化学计量分子式为:C18H17N3O2,Mr = 307.35,晶体属于单斜晶系,空间群P21/n, 晶胞参数: a = 7.597(1),b = 7.500(1) , c = 27.266(5) , b = 95.31(1), V = 1546.7(4) ? , Z = 4, Dc = 1.320 g/cm3 , m = 0.088 mm-1, F(000) = 648,结构偏离因子R = 0.0413, wR = 0.0952,共收集到3282个独立衍射点,其中其I >2(I)的可观测点为2711个。X-射线分析显示化合物1和2的晶体结构均由分子间氢键和-弱相互作用堆积而成的二维层状结构。     

含二芳胺基的吡啶甲酰胺的合成、晶体结构与除草活性

新化合物N-[2-(苯胺基)苯基]-2甲氧基吡啶-3-甲酰胺(C19H17N3O2)通过三步反应合成, 其结构通过1H-NMR, 13C-NMR, ESI-MS表征,其晶体结构通过 X-ray单晶射线衍射仪解析。该晶体属单斜晶系,空间群为P 1 21/n 1,晶胞参数为：a = 10.6329(18)?,b = 13.026(2) ?,c = 12.267(2) ?;Z =4, V =1669.7(5) ?3, Mr = 319.35, Dc = 1.270 mg/m3, S = 1.027, F(000) = 672, μ (MoKα) = 0.085 mm-1 ,可观测点精修最终偏离因子R = 0.0535 以及wR = 0.1353 和3854 个可观测点 I > 2σ(I). 晶体结构表明分子间存在氢键N(3)–H(3)???O(2)对晶体结构起到稳定的作用。初步除草活性表明,化合物N-[2-(苯胺基)苯基]-2甲氧基吡啶-3-甲酰胺在3000 g a.i/hm2对稗草的茎叶处理抑制率为91.81%。     

高氯酸化三邻菲啰啉合镍晶体结构研究

用Ni(ClO4)2合成了高氯酸阴离子和三邻菲啰啉合镍阳离子组成的盐晶体, 晶体结构由X射线衍射确定. 晶体属P21/n空间群, a=0.9388(2) nm, b=3.0139(5) nm, c=1.2974(2) nm, β=111.054(3)º, V=3.426(1) nm3. 采用hyperchem程序包的半经验方法ZINDO/1计算了该配合物的最优化结构, 原子电荷分布很好地佐证了晶体结构的配位环境.     

新型含硫化合物的合成及其晶体结构研究

通过简单的一步亲核取代反应合成了一新型含硫化合物(4-羧基甲硫醇基-2,3,5,6-四氯-苯硫醇基)乙酸(1),产物经乙酸乙酯重结晶分离纯化,并在适当的条件下培养得到单晶,测定了该化合物的晶体结构,以及其DMSO加合物的晶体结构.其中该化合物晶体属于单斜晶系,空间群为P21/c,a=0.508 93(4)nm,b=0.969 81(7)nm,c=1.439 1(1)nm,β=91.036(4)°,V=0.710 20(9)nm3,Z=2,Dc=1.843 g/cm3,F(000)=392,μ=1.133,R1[I2σ(I)]=0.097 3,wR2[I2σ(I)]=0.193 1.其DMSO加合物的晶体结构属于正交晶系,空间群为Pnma,a=1.372 48(2)nm,b=2.883 6(4)nm,c=0.461 48(6)nm,V=1.826 4(4)nm3,Z=4,Dc=1.703 g/cm3,F(000)=936,μ=1.010,R1[I2σ(I)]=0.088 8,wR2[I2σ(I)]=0.203 9.晶体结构分析表明,分子间氢键是这一化合物的一大特点.     

K3[Cr3O(OOCH)6(H2O)3][α-GeW12O40]·17H2O 的合成、结构及特性研究

研究了多金属氧酸盐分子基化合物K3[Cr3O(OOCH)6(H2O)3][α-GeW12O40]·17H2O的合成、晶体结构及其结晶水可逆脱附和吸附性能.该化合物属于单斜晶系,C2/m空间群,α=2.738 3(6)nm,b=1.58 3 0(3)nm,c=1.730 4(4)nm,β=102.43(3)°,V=7.325(3)nm3,Z=4,R1(wR2)=0.067 8(0.171 9).该晶体具有孔道结构,孔道内的结晶水能够可逆的脱附和吸附,而晶体结构随之恢复,因此具有分子筛的特性.     

铜锌异双核配合物[CuZn(fsan)(H_2O)]·H_2O的合成、晶体结构和电化学性质

合成了标题化合物[CuZn(fsan)(H2O)]H2O [H4(fsan)为N, N?- 二(3-羧基水杨醛叉)缩乙撑二胺],用单晶X-ray衍射法测定了它的晶体结构,该晶体属单斜晶系,空间群P21/n,a = 11.695(2), b = 14.646(3), c = 12.265(3) ? ?= 118.46(3)°, V = 1847.0(6) ?,C18H12CuN2O8Zn, Mr = 513.21, Z = 4, Dc = 1.846 g/cm3, (MoK? = 2.502mm-1,F(000) = 1028,R = 0.0478,wR = 0.0902 (I>2(I)), 2951个可观测衍射点。该分子结构为双核单元,铜原子位于“内部”由2个氮原子和2个酚氧原子构成的平面正方场中。“外部”锌原子与2个酚氧原子、2个端基羧氧原子及轴向水分子中的氧原子配位,锌原子处于变形四方锥几何构型之中。金属原子通过2个酚氧原子桥联在一起。结合晶体结构对配合物做了电化学研究。     

(R)-N-乙酰基-四氢噻唑-2-硫酮-4-甲酰TT的合成及其晶体结构

由N-乙酰(R)-四氢噻唑-2-硫酮-4-羧酸在三聚氯氰及三乙胺存在下与四氢噻唑-2-硫酮反应得到标题化合物，[α]^2^0~D +11.18°。用X射线衍射法测得其晶体结构，属单斜晶系，空间群为P2~1/c。晶体学数据：a=0.9959(4)nm，b=1.1469(4)nm，c=1.1108(3)nm，β=92.72(3)°，V=1.2673(8)nm^3，Z=4。分子中两个C=O基，两个C=S基团处于C(1)-N(1)-C(4)及C(6)-N(2)-C(7)键两侧呈反式。用PM3分子轨道方法研究了该化合物的电子结构，电荷和键序分布，得到该化合物前线轨道性质。     

己二胺-12-钼磷酸电荷转移盐的光化学合成与晶体结构

采用光化学法合成一种有机-无机电荷转移盐，（HMDH2）[H2PMo12O40]·AA·3H2O·DMF（HMD = 1,6-己二胺，AA = 乙醛，DMF = N,N-二甲基甲酰胺）超分子化合物。用元素分析，IR，固体漫反射电子光谱，ESR进行了表征。X-射线四圆衍射测定其晶体结构属三斜晶系，空间群Pī，Mr=2081.68，晶胞参数a = 14.092(3)，b =14.347(3)，c =14.358(3)?，α=75.10(3)，β=80.70(3)，γ=80.73(3)°,V=2746.6(10)?3，Z=2，Dc=2.517g/cm3，F(000)=1970，μ(MoKα)=2.766mm-1，全矩阵最小二乘法修正至R=0.0832，wR=0.2638。标题化合物是由1个质子化的1,6-己二胺、12-钼磷混合价杂多阴离子[PMo12O40]4ˉ、3个水分子、2个乙醛分子和1个二甲基甲酰胺分子构成。     

Synthesis and Crystal Structure of (p-{2-[p-(5''''-Phenyl-1'''',3'''',4''''-oxadiazole-2''''-yl)-phenyl]- vinyl}-phenyl)-di-p-tolyl-amine

1 INTRODUCTION Triarylamines constitute a well known class of hole conducting material[1～4]. On the other hand , oxadiazole-based compounds as good electron- transporting materials[5,6] have played an important role in the fabrication of multiple-layer light- emitting diode devices. It is well known that, to achieve good performance in electroluminescence (EL) devices, the injection of electron and hole should be in balance[7]. The requirement might be met in a new compound containing …     

Synthesis and Crystal Structure of Dinuclear Copper Complex[Cu（CH2O（C6H4）N=C（C6H4）O）（Py]2

1 INTRODUCTION Synthesis of transition metal complexes with Schiff-base has been a subject of considerable importance [1,2]. They are not only good complexing agents for Schiff-base, but also good bactericide and antitumour agent [3,4]. At present, there is a spectacular growth in this field. Recently, some bridged binuclear complexes have received much attention on account of their biological relevance and condensed-phase magnetic properties[5,6]. Especially, the complexes containin…     

Photosynthesis and Molecular Structure of2—Amino—3H—phenoxazin—3—one

1 INTRODUCTION 2-Amino-3H-phenoxazin-3-one (APX) is related to the naturally occurring antineoplastic actinomycin D and has been used as a chemical model of actinomycin D[1]. Usually APX is synthesized from 2-aminophenol with the phenoxazinone synthase in human body[2]. A variety of artificial synthesis methods of APX via the oxidation of 2-aminophenol have also been reported, but each method needs some artificial condition such as chemical catalysis[3～7], natural enzyme[8], UV…     

Synthesis and Crystal Structure of Ethyl2—（2—Amino—3—ethoxycarbonyl—4H—benzopyran—4—yl）cyanoacetate

1 INTRODUCTION Inorganic solid supports as catalysts resulting in higher selectivity, milder conditions and easier work-up have been reported as useful catalysts for many reactions [1~3]. Recently, we have reported the Knoevenagel condensation catalyzed by KF-Al2O3[4]. In this paper, we discussed the crystal structure of the title compound synthesized by the reaction of salicylaldehyde and ethyl cyanoacetate in DMF using the catalyst KF-Al2O3 at room temperature KF-Al2O3. In or…     

Synthesis and Crystal Structure of Bi（2-nitrilethyl）aminoacetonitrile

1INTRODUCTIONTheresearchonorganicpolyaminesiscur-rentlyofgreatinterestbecauseoftheirpotentialapplicationsasusefulorganicligands,inwhichtheaminenitrogenatomshavestrongcoordinationabilitytothetransitionmetalions.Theirtransitionmetalcomplexesplayanexcellentr…     

Crystal Structure of 1,3-Dibenzyl-2-benzylaminothiocarbonyl-1,3,4- diazaphospholidin-5-thione-4-sulfide

1 INTRODUCTION Lawesson抯 reagent, 2,4-bis(4-methoxyphenyl)- 1,3,2,4-dithiadiphosphetane-2,4-disulfide, can react with certain substrates to give phosphorus heterocycle compounds. These compounds have some potential biological activities as herbicides, fungicides and insecticides[1,2]. By refluxing the Lawesson抯 reagent with benzylisonitrile in benzene, the title compound, 1,3-dibenzyl-2- benzylaminothio- carbonyl-1,3,4-diazaphospholidin-5-thione-4-sulfide was obtained. In the previous …     

Syntheses and Crystal Structures of 3,3''''-(9,10-Anthrylene)bis-pentane-2,4-dione and 3-(2-Methoxy-1-naphthalenyl)-pentane-2,4-dione

1 INTRODUCTION 3-Substituted pentane-2,4-diones, as a series of chelating ligands to coordinate with many metal ions, have been extensively studied in coordination chemistry. These compounds can also act as valuable intermediates in the synthesis of calamitic derivatives both with or without metal ion[1]. However, compared to the 3-alkylation of 2,4-pentanediones, the direct synthesis of 3-aromatic pentane-2,4-diones from pentane-2,4- diones is much difficult. Previous methods to direc…     

{[(n-C_4H_9)_4N]_2Ag_(4.95)Cu(Ⅰ)_(1.05)I_8}_n聚合物的合成和晶体结构

标题化合物由AgI、CuI和(n-C4H9)4NI在DMF溶剂中直接反应而得。晶体结.构通过单晶X-射线衍射法确定,其晶体属于单斜晶系,空间群P21/c,a=9.4342(4),b=15.7638(7),c=18.877(1)??=100.65(1)?V=2758.9(2)3,化学式C32H72N2Ag4.95Cu1.05I8,Mr=2100.79,Dc=2.529g/cm3,Z=2,(MoK?=6.618cm-1,F(000)=1930。在1.70≤?≤27.46范围内收集到22473个衍射点,独立衍射点6175(Rint=0.0753),其中可观测衍射点4158个(I>2(I))。晶体结构用直接法和差傅立叶合成方法找出初步结构模型,再分别对Ag和Cu的坐标进行修正,最后用全矩阵最小二乘法对266个变量进行精修,最终偏离因子R=0.0476,wR=0.1315。标题化合物的结构由[(M6I8)-]阴离子链和链间的n-Bu4N+阳离子组成。     

Synthesis and Crystal Structure of 3,4—Bis（azidoacetamino）furazan

1INTRODUCTIONDuringthepastthreedecades,1,2,5-oxadiazole(furazan)hasbeenstudiedintheN.D.ZelinskyInstituteofOrganicChemistry[1,2],anditwasfoundthatthearomaticityoffurazanringusuallyincreasesthethermalstabilityofitsderivativesandtheplanarityoftheringprovidesthemwithhighdensity.TheweaknessoftheNObondsinfurazanwassuggestedbyananalysisofitsmass-spectrum[3].Itagreeswiththeresultsoftheresonanceformsoffurazan,whichiscalculatedbySaegebrath[4].Thereby,whenthechloroacetaminogroupwasintroducedintot…