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以往合成芳香醛、酮缩氨基硫脲及其金属配合物多用乙醇作溶剂;电化学氧化法直接合成金属配合物操作简单收率高,还可以得到其它经典方法难以得到的低价金属化合物。本文以金属钛、镍、铜为阳极,2-氯苯甲醛单缩二氨基硫脲为配体,用电化学方法合成了配合物,并探讨电化学反应机理及产物的组成。1 实验部分1.1 仪器与试剂岛津-440型红外分光光度计(KBr压片,4000-300cm 1);XT-4型显微熔点仪;PE-2400型元素分析仪;岛津UV-240紫外可见分光光度计;国产DDS-11A型电导率仪(DMF,25℃);CTP-F82型法拉第磁天平(上海华师科教仪… 相似文献
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共轭的含氮配体,特别是其过渡金属配合物作为模拟生命体系中的一些现象而被人们广泛研究和重视[1]。我们在用二(三甲基硅基)甲基锂与两摩尔的不含α-H的腈进行加成反应时,由于三甲基硅基的1,3-迁移反应得到了一类非常有趣的五元共轭二亚胺配合物[2]。在本工作中,我们合成了两种新型的五元共轭二亚胺镍(Ⅱ)配合物:Ni[HNC(Ph)CHC(Ph)NH]2(2)和Ni[HNC(tBu)CHC(Ph)NH]2(4),并对配合物(2)做了X-射线单晶结构分析,其性能的研究正在进行中。 相似文献
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混合二烃基二氯化锡与水杨醛缩苯胺类Schiff碱配合物的合成和表征 总被引:1,自引:0,他引:1
由混合二烃基二氯化锡与水杨醛缩苯胺类Schiff碱反应,合成了24种新的有机锡配合物。经元素分析、NMR、TG-DSC测定和X射线粉末衍射分析,确定有14种是有机锡与Schiff碱的1:1配合物,10种是1:2配合物。配体是以酚羟基氧原子与锡原子配位,摩尔电导率测定表明这些配合物均为非电解质。 相似文献
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氢键联结锯齿链形成的新型二维网状铜配合物的合成及晶体结构 总被引:8,自引:0,他引:8
氨基酸类化合物如氨基乙酸、亚氨基二乙酸和氨基三乙酸等胺多羧酸有多个配位点 ,可以多种方式和金属离子配位 ,从而得到多种形式的簇合物及一维、二维或三维晶体结构 .我们已经得到了氨基乙酸、亚氨基二乙酸或氨基三乙酸等与稀土和铜的异核配合物 ,并研究了它们的晶体结构[1~ 3] .为深入研究胺多羧酸类配合物的结构特点以及苯环的存在对晶体结构的影响 ,本文合成了一种新型的氨基多羧酸类配合物 N-苯胺叉二乙酸与铜的配合物 ,并测定了其晶体结构 .1 实验部分1 .1 配体 N -苯胺叉二乙酸 [C6H5N ( CH2 COOH) 2 ,H2 L ]的合成 将 5 .… 相似文献
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本文用电化学方法和X射线单晶结构分析, 研究了混合簇合物(C5H5FeC5H4C2Ph)Co2(CO)6的结构, 由循环伏安结果, 分别讨论了簇合物中(C5H5FeC5H4和C2O2中心的成键性质, X射线单晶结构分析表明: 晶体属单斜晶系, 空间群为P21, 晶胞参数a=11.845(6), b=8.155(6), c=24.031(6)A, β=90.88°,晶胞中分子数Z=4, 密度Do=1.637g.cm^-^2, 分析了(C5H5FeC5H4C2Ph)Co2(CO)6的结构特点, 并从成键角度讨论了(RC2R^1)Co(CO)6类簇合物的结构随RC2R^1不同而变化的规律。 相似文献
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[(C6H5CH2C5H4)2GdCl.THF]2 (1) and (C6H5CH2C5H4)2ErCl.THF (2) were prepared by the reaction of LnCl3 (Ln? Gd, Er) with benzylcyclopentadienyl sodium in THF and characterized by elemental analysis, IR, 1H NMR, 13C NMR, MS and thermal gravimetry. The crystal structures of both compounds were determined. Complex 1 is dimeric and its structure belongs to the monoclinic, P21/c space group with a=1.1432(2), b=1.2978(2), c=1.7604(3) nm, β=108.75(2), V=2.4732(9) nm3, Z=2(four monomers), Dc“1.54 g.cm?3. R=0.0342 and Rw“0.0362. Complex 2 is monomer and its structure belongs to the orthorhombic, P212121 space group with a=0.8645(2), b=1.1394(3), c=2.5289(4) nm, V=2.4919(9) nm3, Z=4, Dc“1.56 g.cm?3. R=0.0514, Rw“0.0529. The determination of the crystal structure shows that in complex 1 the benzyl groups on the cyclopentadienyls coordinated to Gd3+ are located in the opposite direction (139°); in complex 2 the benzyl groups on the cyclopentadienyls coordinated to Er3+ are located in the same direction (6.5°). 相似文献
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Contributions to the Chemistry of Phosphorus. 67. About the Cyclotriphosphanes (PC6H5)3, (PC6H5)2(PC2H5), and (PC6H5)2(PCH3) The reaction of (CH3)3Si(C6H5)P? P(C6H5)Si(CH3)3 with RPCl2 (R = C6H5, C2H5, CH3) yields the cyclotriphosphanes (PC6H5)3 1 , (PC6H5)2(PC2H5) 3 , and (PC6H5)2(PCH3) 4 , respectively. Besides, the corresponding homo- and mixed-substituted cyclotetraphosphanes, cyclopentaphosphanes, and cyclohexaphosphanes are formed. The relative concentrations of the cyclotriphosphanes in the reaction mixtures decrease continuously, whereas those of the cyclopentaphosphanes increase. The reasons for these ring-interconversion reactions of the cyclophosphanes (PR)n are discussed. The cyclotriphosphanes 1, 3 , and 4 are characterized by 31P chemical shifts between +130 and +160 ppm that are at considerable high field compared to open-chain triphosphanes and cyclophosphanes of different ring-size. The substituents R are situated on both sides of the P3-ring plane, thus giving rise to two diastereomers of 3 that are observed simultaneously in the statistically expected ratio. The 31P n.m.r. parameters of 1 and 3 are reported and discussed. 相似文献
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《Journal of fluorine chemistry》1988,38(3):335-340
Ph2P-PF2Ph2 has been identified by means 19F- and 31P- NMR spectroscopy as an intermediate product of the disproportionation of Ph2PF. The disproportionation is catalyzed by acids. The reaction mechanism is discussed. PhPF2 disproportionates faster in solution in acetonitrile than neat, forming (PhP)6, instead of (PhP)5. 相似文献