Synthesis and Crystal Structure of 2-(4-Nitrophenyl)-1,2-benzisoselenazol-3(2H)-one DMF (1:1) Solvate

The title compound (C13H8N2O3Se-C3H7NO) has been synthesized by a simple synthetic route and by recrystallization from DMF. The molecular structure of this compound was obtained by single-crystal X-ray diffraction. The compound crystallized in the triclinic space group P with a = 7.450(6), b = 8.150(7), c = 13.859(12) , α = 75.014(14), β = 83.072(18), γ = 84.409(14)°, V = 805.0(12)3, Z = 2 and R = 0.0271 for 2575 observed reflections with I > 2σ(I). X-ray analysis reveals that not only intermolecular Se…O and C-H…O interactions, but also π…π stacking interactions exist in the adjacent molecules. The above three kinds of intermolecular interactions extend the complex into an infinite three-dimensional layered network.     

Synthesis and Crystal Structure of Pd(AETYF)Cl_2CH_2Cl_2 [AETYF = 4''''5''''Diaza-9'''' (4,5-bis(ethylthio)-1,3-dithiole-2-ylidene)-fluorene]

1 INTRODUCTION Over the past decades, extensive work has been carried out to study palladium complexes in organic synthesis, structural analysis, chemical reactivity, catalytic process, spectroscopy and functional mate- rials[1]. Especially the anti…     

二硝酸根二4′,5′-二氮-9′-(4,5-二(硫乙基)-1,3-二硫杂环戊烯-2-叶立德)-芴合镉的合成、结构及光谱性质(英文)

Cd(NO3)·24H2O与配体4′,5′-二氮-9′-(4,5-二(硫乙基)-1,3-二硫杂环戊烯-2-叶立德)-芴(L)在甲醇和二氯甲烷的混合溶剂中生成配合物Cd(NO3)2(L)2。晶体的空间群是Pbcn(#60),晶体学参数分别是a=1.5787(2)nm,b=0.98796(11)nm,c=2.7195(3)nm。V=4.2416(8)nm3,Z=4。2个硝酸根离子各提供1个氧原子,2个配体L各提供2个氮原子,形成了镉的6配位结构。晶体结构显示分子通过平面之间的π-π相互作用沿b轴形成柱状结构,这些柱通过中心原子镉!的配位连接形成二维层状结构,再通过2个硫乙基上的短距离S…S接触进一步形成了三维结构。对其1HNMR、UV-Vis和荧光光谱进行了研究。     

二硝酸根二4′，5′-二氮-9′-(4，5-二(硫乙基)-1，3-二硫杂环戊烯-2-叶立德)-芴合镉的合成、结构及光谱性质

Cd(NO₃)₂·4H₂O与配体4′,5′-二氮-9′-(4，5-二(硫乙基)-1，3-二硫杂环戊烯-2-叶立德)-芴(L)在甲醇和二氯甲烷的混合溶剂中生成配合物Cd(NO₃)₂(L)₂。晶体的空间群是Pbcn(#60)，晶体学参数分别是a=1.578 7(2) nm，b=0.987 96(11) nm，c=2.719 5(3) nm。V=4.241 6(8) nm³，Z=4。2个硝酸根离子各提供1个氧原子，2个配体L各提供2个氮原子，形成了镉的6配位结构。晶体结构显示分子通过平面之间的π-π相互作用沿b轴形成柱状结构，这些柱通过中心原子镉(Ⅱ)的配位连接形成二维层状结构，再通过2个硫乙基上的短距离S…S接触进一步形成了三维结构。对其 ¹H NMR、UV-Vis和荧光光谱进行了研究。     

Synthesis and Crystal Structure of a New Complex （H3IDC）（Prz）0.5（H2O）

The compound （H3IDC）（Prz）0.5（H2O） （H3IDC = imidazole-4,5-dicarboxylate, Prz = piperazine） has been prepared from a hydrothermal approach and was characterized by IR analysis and X-ray diffraction. Its crystal structure consists of discrete 4,5-imidazole-dicarboxylate, H2O and piperazine molecules. The whole structural motif was assembled by three different non-covalent interactions of O-H…O, N-H…O and π-π stacking, which play an important role in packing the molecules. Interestingly, the connections between imidazole-4,5-dicarboxylate molecule and water molecule result in a helical polymeric chain. Crystal data for compound 1： monoclinic system, space group P21/c, a = 6.4600（13）, b = 19.910（4）, c = 6.9123（14） A^°, β = 94.26（3）°, V= 886.6（3） A^°^3, Z= 4, C7H10O5N3, Mr = 216.18.     

基于二-吡嗪-(2, 3-f: 2′3′-h)-喹喔啉和吡啶-2，5-二羧酸混合配体的两个新奇金属有机超分子骨架的水热合成、晶体结构与光致发光

以二-吡嗪-(2, 3-f: 2′3′-h)-喹喔啉(Dpq)和吡啶-2,5-二羧酸(2,5-H2pda)两种混合配体与不同金属硝酸盐为原料,通过水热反应得到了两个新奇的金属有机骨架[Zn2(Dpq)2(2,5-pda)2(H2O)2]·2H2O(1)和[Cd2(Dpq)2(2,5-pda)2]·2H2O(2),并经元素分析、TG、IR、X-射线单晶衍射分析进行了表征。结构分析表明,2,5-pda采取不同的配位方式桥连金属离子分别形成了二聚物1和2D菱形网络2。在化合物1中,相邻的二聚物通过氢键和π-π堆积作用形成扭曲的a-Po超分子结构。在化合物2中,相邻的配位聚合物层通过氢键拓展成扭曲的a-Po超分子骨架,而π-π堆积起到巩固骨架的作用。化合物1和2的结构差异表明了金属离子和配体在配位聚合物自组装过程中对结构的影响。此外固态标题化合物在室温下表现出蓝色的发光性质。     

Fast and efficient synthesis of flavanones from cinnamic acids

A fast and efficient synthesis of flavanones from cinnamic acids in three steps has been developed. First, the cinnamic acid was converted to cinnamyol chlorides using SOCl₂. The acid chlorides were then treated with substituted phenols in BF₃?·?OEt₂ to furnish corresponding chalcones in 42(75% yields. Base-catalyzed cyclization of the chalcones at room temperature afforded corresponding flavones in 85–95% yields. The conversion of the cinnamic acid derivatives to corresponding chalcones was found to be sensitive to the position and nature of the substituents on the aromatic rings.     

Crystal structures,Hirshfeld analysis,and energy framework analysis of two differently 3′-substituted 4-methylchalcones: 3′-(N=CHC6H4-p-CH3)-4-methylchalcone and 3′-(NHCOCH3)-4-methylchalcone

Two crystal structures of chalcones, or 1,3-diarylprop-2-en-1-ones, are presented; both contain a p-methyl substitution on the 3-Ring, but differ with respect to the m-substitution on the 1-Ring. Their systematic names are (2E)-3-(4-methylphenyl)-1-(3-{[(4-methylphenyl)methylidene]amino}phenyl)prop-2-en-1-one (C₂₄H₂₁NO) and N-{3-[(2E)-3-(4-methylphenyl)prop-2-enoyl]phenyl}acetamide (C₁₈H₁₇NO₂), which are abbreviated as 3′-(N=CHC₆H₄-p-CH₃)-4-methylchalcone and 3′-(NHCOCH₃)-4-methylchalcone, respectively. Both chalcones represent the first reported acetamide-substituted and imino-substituted chalcone crystal structures, adding to the robust library of chalcone structures within the Cambridge Structural Database. The crystal structure of 3′-(N=CHC₆H₄-p-CH₃)-4-methylchalcone exhibits close contacts between the enone O atom and the substituent arene ring, in addition to C…C interactions between the substituent arene rings. The structure of 3′-(NHCOCH₃)-4-methylchalcone exhibits a unique interaction between the enone O atom and the 1-Ring substituent, contributing to its antiparallel crystal packing. In addition, both structures exhibit π-stacking, which occurs between the 1-Ring and R-Ring for 3′-(N=CHC₆H₄-p-CH₃)-4-methylchalcone, and between the 1-Ring and 3-Ring for 3′-(NHCOCH₃)-4-methylchalcone.     

晶体工程及其在化学中的应用

晶体工程是实现分子到材料的一条重要途径 ,化学家致力于晶体工程是为了更好了解分子间的相互作用以便设计新颖的固体材料及固体反应     

由2',4'-二氢-6'-甲氧基-3',5'-二甲基查耳酮合成新黄酮

在DMSO/ I2的氧化作用下,由2',4'-二氢-6'-甲氧基-3',5'-二甲基查耳酮可合成一种全新结构的黄酮:7-羟基-5-甲氧基-6,8-二甲基黄酮(产率91%),而在HCl/MeOH作用下则得到了两种黄烷酮:7-羟基-5-甲氧基-6,8-二甲基黄烷酮 (产率70%) 和 5,7-二羟基-6,8-二甲基黄烷酮 (产率20%).     

由2′,4′-二氢-6′-甲氧基-3′,5′-二甲基查耳酮合成新黄酮

在DMSO/I2的氧化作用下,由2′,4′-二氢-6′-甲氧基-3′,5′-二甲基查耳酮可合成一种全新结构的黄酮:7-羟基-5-甲氧基-6,8-二甲基黄酮(产率91%),而在HCl/MeOH作用下则得到了两种黄烷酮:7-羟基-5-甲氧基-6,8-二甲基黄烷酮(产率70%)和5,7-二羟基-6,8-二甲基黄烷酮(产率20%)。     

Synthesis,characterization, crystal structure,and antimicrobial studies of novel thiourea derivative ligands and their platinum complexes

N,N-Di-R-N′-(4-chlorobenzoyl)thiourea (Di-R: diethyl, di-n-propyl, di-n-butyl and diphenyl) ligands (HL^1–4) and their Pt(II) complexes (cis-[Pt(L^1–4-S,O)₂]) have been synthesized and structurally characterized by elemental analyses, FT-IR and NMR spectroscopy. HL² ligand and cis-[Pt(L⁴-S,O)₂] metal complex have been also characterized by a single-crystal X-ray diffraction study. HL², C₁₄H₁₉ClN₂OS, crystallizes in the monoclinic space group P2₁/n (no. 14), with Z = 4, and unit cell parameters, a = 11.1405(16) Å, b = 9.7015(12) Å, c = 14.790(2) Å, β = 106.547(7)°. The cis-[Pt(L⁴-S,O)₂], C₄₀H₂₈Cl₂N₄O₂PtS₂: triclinic, space group P-1 (no. 2), a = 8.9919(3) Å, b = 14.7159(6) Å, c = 15.7954(6) Å, α = 113.9317(18)°, β = 97.4490(18)°, and γ = 105.0492(16)°. Single crystal analysis of complex, cis-[Pt(L^1–4-S,O)₂], revealed that a square planar coordination geometry is formed around the platinum atom by two sulfur and two oxygen atoms of the related ligands, which are in a cis configuration. In addition, the thiourea derivative ligands and their complexes were evaluated for both their in-vitro antibacterial and antifungal activity. The results have been reported, explained, and compared with fluconazole and ampicillin, used as reference drugs.     

Synthesis and Crystal Structure of a New Zn(II) Nitronyl Nitroxide Complex [Zn(NIT4Py)(PDA)(H2O)3]

1 INTRODUCTION Nitronyl nitroxides, independently or in combina- tion with metal ions, have been one of the most wi- dely studied systems in molecular magnetism for understanding radical-radical or metal-radical inte- ractions as well as for synthesizing organic ferroma- gnets and metal-radical magnetic materials[1～4]. Up to now, lots of metal-radical complexes have been reported[5～8]. On the other hand, cooperative inter- molecular interactions, such as coordination bonds, hydrogen bon…     

Relationship between Structure and SHG Effect of Substituted Thienyl Chalcone

1INTRODUCTIONRecentlyorganicnonlinearoptical(NLO)materialsarebeingdevelopedforfre-quencyconversionoflaserinopto-electrics-Especiallybluelightisrequiredforopti-calmemoryofhighdensityrecording.Becauseadiodelaserisusedasalightsource,thenonlinearmaterialswhichhaveextremelyhighvalueofNLOcoefficientsandthetransmissionofblueregionarenecessary.Sincethesecond-orderNLOpropertyoforganiccompoundisderivedfromconjugateddelocalizedrrelectrons,thecompoundswhichhavebeenreportedhavefocusedonthenitroanil…     

硝酰胺二聚体静电能和交换能的理论计算

根据对称性匹配微扰理论, 并运用多个微扰和非微扰方法, 计算了硝酰胺二聚体在不同分子间距(R)时静电能和交换能. 这些具有轨道弛豫的静电能不仅含有第4级单、双、四和三重激发态项, 而且含有CCSD的第5级和更高级的能量项. 同时发现: 第4级的三重激发态能量项比第5级和更高级的能量项之和还重要. 求得的含有分子内电子相关效应的交换能达到了CCSD水平. 用于计算交换能关联校正项的单对交换近似在硝酰胺二聚体的范德华最小距离0.42 nm附近区域才较合理. 在R为0.32～1.42 nm范围, 静电能与R的关系有两种: 一是在小于等于0.47 nm时, (R^－7.64; 二是大于0.47 nm时, (R^－3.97. 交换能具有明显的短程作用特点, 其与R间的关系为指数衰减: 21.061exp(－R/0.318). 最后发现: 在硝酰胺二聚体中, 分子内的电子相关效应对和的影响很显著.     

3-乙酰基-8-叔丁基香豆素晶体结构及密度泛函理论研究

本文合成了3-乙酰基-8-叔丁基香豆素,并通过X-射线单晶衍射法测定分子结构,随后进行红外、核磁共振、紫外可见吸收光谱表征,并通过密度泛函理论(DFT)研究晶体中的分子间作用,模拟光谱并预测表面活性位点。结果表明,分子为大共轭平面结构,在晶体中主要以π-π堆积作用和氢键作用结合,结合能分别为17. 2和3. 9 kcal/mol。分子在近紫外可见光范围内的最大吸收波长在310nm,摩尔消光系数为16000L·mol-1·cm-1,主要对应苯环上π电子向内酯环以及羰基氧上的跃迁。该分子6号位碳最易发生芳环上亲电取代反应,内酯可发生水解、氨解等反应,苯环上氢、羰基氧均可形成氢键等弱相互作用。