Synthesis,Structure and Norbornene Polymerization Activity of a Novel Palladium(Ⅱ) Complex with N,N-bis(2-benzoyl-3-oxobutane)-trans-1,2-diaminocyclohexane Ligand

The title complex N,N-bis(2-benzoyl-3-oxobutane)-trans-1,2-diaminocyclohexane-palladium(C28H28N2PdO4) has been synthesized by the reaction of N,N-bis(2-benzoyl-3-oxobutane)-trans-1,2-diamino-cyclohexane with PdCl2,and characterized by elemental analysis,IR spectrum,WAXD and TG.The spatial structures of the complex have been confirmed by single-crystal X-ray diffraction analysis.The compound crystallizes in the monoclinic system,space group C2/c with a = 29.763(6),b = 10.320(2),c = 18.921(4) ,β = 102.75(3)°,V = 5668(2) 3,C28H28N2PdO4·CH3OH,Mr = 594.97,Z = 8,Dc = 1.394 g/cm3,μ(MoKα) = 0.694 mm-1,F(000) = 2448,T = 293(2) K,R = 0.0572 and wR = 0.1347(I 2(I)).The compound was investigated for the catalytic behavior towards norbornene(NB) vinyl addition polymerization.And the palladium complex showed excellent catalytic activity up to 9.97×106 g of PNB(mol of Pd)-1 h-1 with high monomer conversion using methylaluminoxane(MAO) as a cocatalyst.     

3个联苯甲酰类配体的合成与晶体结构

合成得到3个新型联苯甲酰类配体C6H5N=CPh(C=O)Ph(L1)、2,6-(CH3)2C6H5N=CPh(C=O)Ph(L2)及2,6-(CH(CH3)2)2C6H5N=CPh(C=O)Ph(L3).利用红外光谱分析对其结构进行表征;并通过单晶XRD测定了配体L1、L2的晶体结构(CCDC No:860489&860490);元素分析进一步确定了配体L3的结构.     

磷钼杂多化合物[H3PMo12O40]·2（4,4’-bipy）·1.75H2O的合成、结构及电化学性能研究

采用水热法合成了一个有机-无机杂化的Keggin型磷钼杂多化合物[H3PMo12O40]·2(4,4’-bipy)·1.75H2O(简称化合物1 bipy=联吡啶);通过元素分析、单晶X-射线衍射对其结构进行表征.结果表明,该化合物属于单斜晶系,P2(1)/c空间群,晶胞参数a=1.146 6(3)nm,b=2.122 7(6)nm,c=2.146 1(7)nm,β=98.082(12)°,V=5.171 0(3)nm3,C20H19Mo12N4O41.75P,Mr=2 165.64,Z=4,Dc=2.782 Mg·m-3,μ(MoKα)=2.946 mm-1,F(000)=4 080,R=0.062 2和wR=0.182 2.该化合物由一个Keggin型结构的多阴离子[PMo12O40]3-、两个2,2’-联吡啶和1.75个晶格水分子组成.杂多阴离子中的端氧原子、联吡啶分子中的氮原子以及水分子中的氧原子之间通过氢键作用形成超分子结构而使晶体稳定存在.通过循环伏安法详细研究了该化合物的微粒修饰电极的电化学行为和电催化性能.