联苯四羧酸配体化合物的核磁共振分析

近些年来,设计由有机配体和金属离子自组装构筑的配位聚合物是一个十分具有吸引力和发展前景的研究领域。本文采用核磁共振(NMR)实验技术中的氢谱、碳谱、DEPT135谱、同核化学位移相关谱(~1H-1H COSY)、异核单量子相关谱(1H-~(13)C HSQC)以及多健异核多量子相关谱(~1H-~(13)C HMBC)等研究方法对一个新联苯四羧酸配体化合物的结构进行了分析,并对所有的~1H NMR、~(13)C NMR谱信号进行了归属。     

噻吩基与苯基修饰的铱(Ⅲ)配合物合成与光谱性质对比

本研究将传统的2-苯基吡啶配体进行改性,用富电子的噻吩基团代替苯基,得到有机配体2-噻吩基吡啶(L1),并以L1合成铱(Ⅲ)配合物C1,而基于2-苯基吡啶(L2)配体的铱(Ⅲ)配合物C2也被合成得到,以用做性质对比;随后通过质谱(MS)、核磁共振谱(NMR)以及傅里叶变换红外光谱(FT-IR)对产物C1和C2进行结构表征,并利用紫外可见光吸收光谱(UV-Vis)以及光致发光光谱(PL)等测试手段,对比C1与C2的光谱性质,利用噻吩基代替苯基后,UV-Vis的吸收范围扩大,PL的最大发射峰发生了红移。     

水杨醛亚胺钛络合物的负载及在催化乙烯聚合中的应用

以3,5-二枯基水杨醛与2,3,4,5,6-五氟苯胺为原料缩合反应合成了水杨醛亚胺配体(Ⅰ),利用四氯化钛和水杨醛亚胺配体(Ⅰ)反应制得了相应的水杨醛亚胺钛络合物(Ⅱ),用核磁共振氢谱(1H NMR)和核磁共振碳谱(13C NMR)表征了配体及络合物的结构.以甲基铝氧烷(MAO)为助催化剂,在60℃、1.0 MPa压力...     

联苯羧酸配体化合物的NMR研究

近年来,构筑具有新颖结构和优良性能的金属-有机骨架配位聚合物已经引起了学术界研究者的广泛关注。本文应用核磁共振氢谱、碳谱、DEPT135谱、同核化学位移相关谱(~1H-~1H COSY)、异核单量子相关谱(~1H-~(13)C HSQC)以及多健异核多量子相关谱(~1H-~(13)C HMBC)等核磁共振研究方法对一个新的联苯羧酸配体化合物的结构进行了研究,并对~1H NMR、~(13)C NMR谱的信号进行了全归属。     

含香豆素的环金属钌配合物的合成与表征

以4-N,N-二乙基氨基水杨醛为原料合成3-{4-[2-(2,4-二氟苯基)]吡啶基乙烯基}-7-N,N二乙基氨基香豆素,将其作为C,N-配体与[Ru(cycme)Cl_2]_2和2,2'-二联吡啶反应,制备得到一种含有香豆素结构的环金属钌配合物,该配合物未见文献报道。通过~1H NMR,~(13)C NMR及MS表征了其结构,其光谱实验结果表明:该配合物的最大吸收峰位于485 nm,其摩尔消光系数达到5. 1×10~4mol~(-1)·L·cm~(-1),在酸碱中均表现出良好的稳定性。     

2,3-丁二酮缩苯甲酰肼Schiff碱的合成与抗肿瘤活性研究

合成了一种2,3-丁二酮缩苯甲酰肼Schiff碱配体及其过渡金属Cu(II)、Co(II)、Zn(II)、Mn(II)、Ni(II)的配合物,并用元素分析、红外光谱、~1H NMR、电子光谱、摩尔电导加以表征,表征结果表明所研究的结构与所预测的基本一致。配体及各配合物的体外抗肿瘤活性用四氮唑盐比色法进行测定,抗肿瘤活性结果表明,配体及与金属离子配位后,均有一定的抗肿瘤效果,其中,二价铜离子配合物的抑制肿瘤效果最佳。     

水杨醛亚胺合镍金属催化剂的合成、表征及应用

采用多步偶联的方式合成了基于氧杂蒽骨架的配体及相应的镍金属配合物,通过核磁共振谱、碳谱及元素分析对配合物及其配体进行结构表征分析,利用单晶衍射阐述了配合物的立体结构.采用该配合物与含铝助剂配合使用能有效催化乙烯寡聚,活性最高可达到5×106g/(mol·h),产品组成以C4为主.     

Cu(Ⅱ)联咪唑硝基衍生物配合物的合成表征及其与CT-DNA相互作用研究

以联咪唑硝基衍生物(NO₂Me₂biim)为配体,通过直接法合成了其铜(Ⅱ)配合物。利用元素分析、红外光谱、紫外-可见光谱、摩尔电导率等方法对配合物的组成和结构进行了表征。以电子光谱、荧光光谱和黏度法研究了配体NO₂Me₂biim及配合物与小牛胸腺DNA(CT-DNA)的相互作用机制。研究表明,配体NO₂Me₂biim和配合物与CT-DNA分别以典型插入和部分插入模式进行相互作用。     

邻苯二甲醛双缩氨基硫脲Schiff碱及其银配合物的合成与表征

Schiff碱及其配合物具有特殊的结构和性质.文章以邻苯二甲醛(OPA)和氨基硫脲为原料,在不同反应条件下合成出一种对称的邻苯二甲醛双缩氨基硫脲Schiff碱配体,并制备出其银配合物.通过红外光谱、紫外光谱、元素分析等手段对配体及配合物的结构进行了初步表征.测定了银配合物的电导性能.抑菌试验结果表明,配体和银配合物对金黄色葡萄球菌、枯草芽孢杆菌、大肠杆菌均有不同程度的抑菌效果.     

2-氨基苯并咪唑水杨醛席夫碱(SABI)钆(Ⅲ)配合物的合成、表征及抑菌活性的研究

以2-氨基苯并咪唑水杨醛席夫碱(SABI)为配体合成了新型金属钆(Ⅲ)的配合物,并通过元素分析、红外光谱、热重及摩尔电导率对其进行表征,确定配合物的组成为[Gd(HL)2(NO3)].H2O。席夫碱的配位原子是酚羟基的氧原子、席夫碱及咪唑环C=N中的氮原子。同时研究了配体及配合物的抑菌活性。     

含醚链桥联的新型大环席夫碱化合物的合成与表征

以烷基二溴（即1,2-二溴乙烷,1,4-二溴丁烷,1,6-二溴己烷）、水杨醛、邻苯二胺为原料合成了系列醚链桥联大环席夫碱配体（H2L＊）及其Zn（Ⅱ）配合物,通过元素分析、1HNMR、红外光谱、紫外光谱、摩尔电导、质谱等手段对醚链桥联大环席夫碱配体及其配合物进行组成和结构表征。关键词大环化合物席夫碱合成表征     

Synthesis and characterization of luminescent zinc complexes containing redox-active 1-(2-pyridylazo)-2-acenaphthequinol ligands with nonlinear optical property

The redox-active ligand 1-(2-pyridylazo)-2-acenaphthequinol (PAAL) and its zinc complex Zn(PAAL)₂ were isolated and characterized by single crystal X-ray diffraction, ¹H NMR, UV–Vis spectra and TGA, as well as their fluorescence and third-order nonlinear optical properties were preliminary investigated. The electronic structure of the complex is examined by cyclic voltammogram, while density functional theory calculations also support the redox-active nature of the PAAL ligand.     

不对称酰胺基卟啉的合成及表征

通过5-（4-氨基）苯基-10,152,0-三苯基卟啉（MATPP）与3-氰基苯甲酸在CH2Cl2中直接反应得到一种新型不对称酰胺基卟啉配体5-（4-3-氰基苯甲酸酰亚胺基）苯基-101,5,20-三苯基卟啉配体（CBTPPH2）,利用紫外-可见光谱、红外光谱、核磁共振氢谱、质谱、元素分析等测试方法对化合物的结构加以确认。     

一种新型液晶化合物的合成及表征

以CH2C12为溶剂,通过5-（4-氨基）苯基-10,15,20-三苯基卟啉（MATPP）与十二酸直接反应得到一种新型不对称酰胺基卟啉配体5-（4-十二酸酰亚胺基）苯基．10,15,20．三苯基卟啉配体（PDTPPH2）,利用紫外-可见光谱、红外光谱、核磁共振氢谱、元素分析等测试方法对化合物的结构加以确认。     

Paramagnetic shifts induced by europium and praseodymium complexes in the NMR spectra of some substituted phenols

An investigation into the shifts induced in the NMR spectra of some derivatives of substituted phenols by tris(dipivalomethanato)europium and tris(dipivalomethanato)praseodymium is reported. The phenol derivatives were studied to ascertain the possible utility of the shift reagents as an aid in the analysis of phenolformaldehyde resins by NMR spectroscopy, and to gain information on induced shifts with molecules having more than one possible co-ordination site.     

N,N’-双-(1-苯基-3-甲基-4-α-呋喃甲酰基吡唑啉-5基)-乙二亚胺分子结构和核磁共振氢谱研究

合成了N,N’-双-(1-苯基-3-甲基-4-α-呋喃甲酰吡唑啉-5基)-乙二亚胺(PMFP.2 en),对其分子结构和核磁共振氢谱、紫外吸收光谱等进行了研究,并借助CSChemoffice的MM2方法对PMFP.2 en的可能结构进行了订正,同时对4-(a-呋喃甲酰基)-PMP与乙二胺缩合前后的结构变化及生成PMFP.2 en的可能机制进行了初步研究。     

酰胺基卟啉化合物的制备、表征及热分析

5-(4-氨基)苯基-10,15,20-三苯基卟啉(MATPP)与棕榈酸在CH2Cl2中直接反应,得到一种新型不对称酰胺基卟啉5-(4-棕榈酸酰亚胺基)苯基-10,15,20-三苯基卟啉(PITPPH2),利用紫外-可见光谱、红外光谱、核磁共振氢谱、元素分析等测试方法对化合物的结构加以确认。热分析表明,卟啉PITPPH2从200℃开始分解,具有较高的热稳定性。     

New antimicrobial polyurea: Synthesis,characterization, and antibacterial activities of polyurea‐containing thiosemicarbazide–metal complexes

A novel class of polymer–metal complexes was prepared by the condensation of a polymeric ligand with transition‐metal ions. The polymeric ligand was prepared by the addition polymerization of thiosemicarbazides with toluene 2,4‐diisocyanate in a 1 : 1 molar ratio. The polymeric ligand and its polymer–metal complexes were characterized by elemental analysis, thermogravimetric analysis, Fourier transform infrared spectroscopy, and ¹³C‐NMR and ¹H‐NMR spectroscopy. The geometries of the central metal ions were determined by electronic spectra (UV–visible) and magnetic moment measurement. The antibacterial activities of all of the synthesized polymers were investigated against Bacillus subtilis and Staphylococcus aureus (Gram positive) and Escherichia coli and Salmonella typhi (Gram negative). These compounds showed excellent antibacterial activities against these bacteria with the spread plate method on agar plates, and the number of viable bacteria were counted after 24 h of incubation period at 37°C. The antibacterial activity results revealed that the Cu(II) chelated polyurea showed a higher antibacterial activity than the other metal‐chelated polyureas. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

AU(DIEN)Cl]Cl(2): Exchange Phenomena Observed by H and C NMR Spectroscopy

The solution behaviour of the square-planar gold(III) complex [Au(dien)Cl]Cl(2) (dien = 1,5- diamino-3-azapentane) was investigated by (13)H and (13)C NMR spectroscopy. We have found that (1)H NMR spectra of [Au(dien)Cl] Cl(2) are characterised by exchange behaviour over the whole pH range, and some exchange effects are also seen in (13)C NMR spectra of the deprotonated hydroxo derivative of the complex in alkaline solution. An exchange rate of > 378 s(-1) was determined from (1)H NMR spectra at pH *(2) (coalescence temperature (40)C degrees ). In slightly acidic solutions of the complex, (1)H chemical shifts are in accordance with the known deprotonation of the central amine group of the complexed diethylenetriamine ligand. In (13)C NMR spectra, two separate sets of resonances are observed for the chloro and the hydroxo complex of gold(III) diethylenetriamine. The hydroxo complex [Au(dien-H)OH(+) shows exchange effects in (13)C NMR spectra. Variable temperature studies show the carbon atoms next to the central secondary amine to be inequivalent and each present in two different environments that are in intermediate to fast exchange on the NMR time-scale.     

Copolymerization of Norbornene and Methyl Acrylate by β-ketoiminato Palladium Complexes/MAO

Summary Neutral palladium complexes bearing β-ketoiminato ligand Pd[CH₃C(O)CHC(NAr)CH₃](PPh₃)(Me)(I Ar=α-napthyl, II Ar= fluorenyl) were activated by MAO to give catalytic system able to polymerize methyl acrylate (MA), thus producing atactic high molecular weight poly(methyl acrylate). Both catalysts exhibited catalytic activities for the copolymerization of norbornene with MA. The polymers were characterized by ¹³C NMR, GPC and FT-IR spectra. The analyses of the product by ¹H NMR and ¹³C NMR spectra gave the verification of random vinyl addition copolymer. The composition of the copolymers was controlled by varying the monomer feed ratio.