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198 2年 Fujimura等 [1~ 3]曾报道具有液晶特性的配合物用作气相色谱固定相 ,但未引起人们的重视 ,所以至今对此几乎没有研究 .我们首次制备了对 -十二烷氧基二硫代苯甲酸镍 ( DDBN)气相色谱固定相 ,这是一种液晶型配合物固定相 ,既表现出金属离子在高温下良好的热稳定性 ,又表现出液晶配体对位置异构体的特殊选择性 ,能使最难分离的多环芳烃异构体得到满意的分离[4~ 6 ] .1 实验部分1 .1 仪器与试剂 二硫化碳和四氢呋喃在使用前重新蒸馏并干燥 ,对 -十二烷氧基溴苯在真空干燥器中于室温下干燥 4 8h.岛津 GC- 1 6A气相色谱仪 ,FID… 相似文献
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Three binuclear Nickel(Ⅱ) complexes were synthesized, bridged with dithiooxalate, Ni2(Bpy)3(Dto)2(H2O)3(1), Ni2(Phen)3(Dto)2(H2O)3(2) and Ni2(Me2Bpy)3(Dto)2(H2O)2 (3) (Bpy=2,2′-Bipyridine, Phen=1,10-phenanthroline, Me2Bpy=4,4′-dimethyl-2,2′-bipyridine, Dto2-=Dithiooxalate), and characterized by elemental analyses, IR, UV-Visible spectra, conductance. The variable temperature magnetic susceptibilities for the complexes were measured in the range of temperature between 1.5 K and 298 K. Experimental data of magnetic susceptibility were successfully fit to theoretical value based on the spin Hamiltonian operator:(?), S1=S2=1, giving the magnetic exchange parameters of 2J=-52.8 cm-1. This result indicates the presence of a strong antiferromagnetic spin exchange interaction between the Ni(Ⅱ) ions. The magnetic exchange parameters of the binuclear Nickel(Ⅱ) complexes bridged with dithiooxalate is larger than that of the binuclear Nickel(Ⅱ) complexes bridged with oxalate. Dithiooxalate is more effective to transfer antiferromagnetic spin exchange interaction between the Ni(Ⅱ) ions than oxalate. 相似文献
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Sn(Ⅱ),Pb(Ⅱ) complexes of 1,5-bis(benzophnone) thiocarbohydrazon were synthesized by the electrochemical oxidation of anodic metal in non-aqueous solvents.The complexes were characterized by elemental analysis,IR,UV and molar conductivity etc. 相似文献
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Homochiral bis[(O,O′-di-2-isopropyl-5-methylcyclohexyl) dithiophosphato] nickel(Ⅱ) (1), prepared by the reaction of O,O′-di-2-isopropyl-5-methylcyclohexyl) dithiophosphato potassium with Ni(OAc)2 displays a almost planar tetragonal geometry around Ni center composed of four S atoms from two different ligands. CCDC: 252341. 相似文献
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合成了一种新的含取代苄基三苯基鏻的马来二氰基二硫烯镍配合物[ClBzTPP]2[Ni(mnt)2].H2O([ClBzTPP]+代表对氯苄基三苯基鏻阳离子,mnt2-代表马来二氰基二硫烯阴离子).配合物为三斜晶系,空间群P墿,晶胞参数为a=1.058 5(2)nm,b=1.108 9(2)nm,c=1.157 0 nm,α=81.98(1)°,β=84.95(1)°,γ=84.45(1)°,V=1.369 1(4)nm3,Z=1,最终一致性因子R=0.058 4.该配合物由2个[ClBzT-PP]+阳离子,1个[Ni(mnt)2]2-阴离子和1个H2O组成.其结构特点是配合物中的[ClBzTPP]+阳离子和Ni(mnt)22-阴离子沿c轴方向堆积成柱,并通过C—H…S,C—H…π,C—H…Ni氢键和π-π堆积作用形成了二维网状结构. 相似文献
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meso-四(对烷氧基苯基)卟啉配合物的合成、表征和液晶性研究 总被引:7,自引:0,他引:7
The method of Adler was improved to prepare a series of 5,10,15,20-tetrakis(4-alkoxyphenyl)porphyrins and their complexes containing Fe3+, Mn3+, Pb2+, Co2+, Cu2+, Zn2+. Among them there were seven new compounds. All these compounds were identified through 1H NMR, MS, IR, UV and Element analysis. The correlation between the structure of compounds and their 1H NMR, MS, IR, UV spectra was discussed and their specific spectra were explained. We found nine metalloporphyrins exhibited liquid crystal behaviour through DSC and polarized-light microscope. They had one to three mesophases and certain phase transition temperature, ΔH and temperature range of L.C(ΔT). 相似文献
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使用2,2′-二硫代二苯甲酸和2,2′-联吡啶(2,2′-bipy)、硝酸铜在水热条件下发生的原位反应合成了一个铜配合物,即[Cu2(C14H8O4S)2(C10H8N2)2](1)(C14H8O4S=2,2′-二羧苯基硫醚,C10H8N2=2,2′-联吡啶);然后又利用2,2′-二硫代二苯甲酸和菲咯啉(phen)、氯化钙在水溶液中合成了一个钙配合物,即{[Ca(C14H8O4S2)(C12H8N2)2]·(H2O)2}n(2)(C14H8O4S=2,2′-二硫代二苯甲酸根,C12H8N2=菲咯啉),并对它们分别进行了元素分析、红外光谱、热稳定性、X射线粉末衍射和X射线单晶衍射的表征。结果表明:配合物1由2,2′-二羧苯基硫醚配体连接形成了一个双核的化合物,通过氢键和氮杂环之间的π…π作用形成三维超分子网络结构。配合物2由二硫代二苯甲酸配体桥联形成了一个一维链状结构,通过氢键和氮杂环之间的π…π作用也形成三维超分子网络结构。并且,对这2个配合物的热稳定性分别进行了研究。 相似文献
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稀土与含硫有机配体配合物的研究(Ⅷ)——甘氨酸二硫代甲酸镍与稀土醋酸盐多核配合物的合成与性质 总被引:1,自引:0,他引:1
在乙醇—水溶液中,用稀土醋酸盐与氨基乙酸二硫代甲酸镍[H_2Ni(Gc)_2]反应,制备出14种稀土元素的多核配合物,通过元素分析确定了配合物的组成为RENi(Gc)_2·AC·H_2O(RE=La—Gd,除Ce、Pm外)和RE_2[Ni(Gc)_2]_3·xH_2O(RE=Tb—Lu,Y;x=4,8,10),研究了配合物的溶解性、红外光谱、X射线光电子能谱和核磁共振氢谱。 相似文献
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以2,2′-二硫代二苯甲酸、2,2′-联吡啶、咪唑、硝酸锌和硝酸锰为原料,使用水热方法合成了配合物[Zn(EBLA)(2,2′-bipy)(H2O)](EBLA=2,2′-二苯甲酸硫醚)(2,2′-bipy=2,2′-联吡啶)(1),自然挥发法制备了配合物[Mn(EBSA)(im)2(H2O)]n(EBSA=2,2′-二硫代二苯甲酸)(im=咪唑)(2)。利用元素分析、红外和热重分析对其进行了表征。利用X-射线单晶衍射对结构进行了测定,并研究了配合物1的荧光性质。配合物1中,2,2′-二苯甲酸硫醚是通过水热方法由2,2′-二硫代二苯甲酸发生原位反应制备,Zn2+离子是五配位的四角锥双核结构;配合物2中,Mn2+离子是六配位的变形八面体一维链状结构。配合物中存在氢键和π-π堆积等弱的分子间作用力。 相似文献
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四-(对-十二酰氧基)苯基卟啉过渡金属配合物的合成及其液晶行为研究 总被引:6,自引:0,他引:6
合成了5,10,15,20-四-(对-十二酰氧基)苯基卟啉(简称TLPPH2)及其Mn(Ⅲ),Fe(Ⅲ),Co(Ⅱ),Ni(Ⅱ),Cu(Ⅱ)和Zn(Ⅱ)配合物,通过元素分析、紫外可见光谱、红外光声光谱、核磁共振氢谱和摩尔电导等分析方法表征了它们的组成和结构.用DSC和偏光显微镜研究了配体及其锌配合物的液晶行为.结果表明,锌配合物的液晶相变温度始于-50.67℃,相区宽度达143℃. 相似文献
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合成了一种新的含取代苄基三苯基镌的马来二氰基二硫烯镍配合物[ClBzTPP]2[M(mnt)2]·H2O([ClBzTPP]’代表对氯苄基三苯基锑阳离子,mnt^2-代表马来二氰基二硫烯阴离子).配合物为三斜晶系,空间群Pi,晶胞参数为a=1.0585(2)nm,b=1.1089(2)nm,c=1.1570nm,α=81.98(1)°,β=84.95(1)°,γ=84.45(1)°,V=1.3691(4)nm^3,Z=1,最终一致性因子R=0.0584.该配合物由2个[ClBzT—PP]^+阳离子,1个[M(mnt)2]^2-阴离子和1个H2O组成.其结构特点是配合物中的[C1BzTPP]’阳离子和Ni(mnt)2^2-阴离子沿c轴方向堆积成柱,并通过C—H…S,C—H…π,C—H…Ni氢键和π-π堆积作用形成了二维网状结构. 相似文献
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二硫代草酰胺和二环己酮草酰二腙桥联的双核Cu(Ⅱ)-Cu(Ⅱ)配合物的合成和磁性Ⅰ. 总被引:2,自引:0,他引:2
Three new binuclearcopper(Ⅱ) complexesbridged by dithio-oxamidate(dto) group or biscyclohexanone oxalyldihydrazone (BCO)[Cu2(en)2(dto)](Cl O4)2·3H2O(1)、[Cu2(dien)2(dto)](ClO4)2·2H2O (2) and [Cu2 (bipy)2(BCO)(Cl O4)2](ClO4)2(3),where en, bipy and dien denote ethylenediamine,2,2′-bipyridyl and diethylentriamine respectively, were synthesized and characterized by elemental analysis,IR,electronicspectra and variable temperature magnetic susceptibility. Variable temperature (4.0-300K) magnetic susceptibility data for the complexes show that there exists the antiferromagnetic exchange interaction between the two copper(Ⅱ) ionswith J(cm-1) valuesof-0.462 (1)、-1.03 (2) and -6.86 (3). The preliminary study of the electrochemical characteristicsof complex (3) was also carried out. 相似文献