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作 者:张子红[1] 窦建民[1] 刘颖[1] 王大奇[1] 雍伟[2] 郑培菊[2] 杜晨霞[3] 朱玉[3]
机构地区:[1]聊城大学化学化工学院,聊城252059 [2]复旦大学分析测试中心,上海200433 [3]郑州大学应用化学重点实验室,郑州450052
出 处:《化学学报》2002年第9期1649-1655,共7页Acta Chimica Sinica
摘 要:合成了苯并 15 冠 5与Na2 [M(SCN) 4](M =Pd ,Pt)生成的配合物 :[Na(B15 C 5 ) ]2 [Pd(SCN) 4](1) ,{ [Na(B15 C 5 ) ][Na(B15 C 5 ) (H2 O) ]} [Pt(SCN) 4](2 ) .1为单斜晶系 ,空间群P2 1/n ,a =1.0 16 4(6 )nm ,b =1.3743(3)nm ,c=1.4987(7)nm ,β =95 .2 48(6 )° ,V =2 .0 847nm3 ,Z =2 ,Dcalcd=1.47g/cm3 ,F(0 0 0 ) =944 ,R =0 .0 5 3,wR =0 .0 72 .2为三斜晶系 ,空间群P1,a=1.1484(2 )nm ,b=1.42 10 (3)nm ,c=1.5 0 2 6 (3)nm ,α =6 2 .5 0 0 (3)°,β =72 .393(3)°,γ =73.10 6 (4 )° ,V =2 .0 398(7)nm3 ,Z =2 ,Dcalcd=1.6 74g/cm3 ,F(0 0 0 ) =10 2 8,R1=0 .0 32 7,wR2 =0 .0 885 .1由两个[Na(B15 C 5 ) ]+ 配阳离子和一个 [Pd(SCN) 4]2 -配阴离子组成 ,两者通过Na—N键形成中性配合物 ,[Na(B15 C 5 ) ]+相对钯原子呈反式排列 .2由 [Na(B15 C 5 ) ]+ 和 [Na(B15 C 5 ) (H2 O) ]+ 配阳离子和一个 [Pt(SCN) 4]2 -配阴离子组成 ,它们也通过Na—N键形成中性配合物 ,配阳离子相对铂原子呈顺式排列 .2的两个分子通过氢键形成二聚结构 .Two benzo-15-crown-5 (B15-C-5) complexes: [Na(B15-C-5)](2)[Pd(SCN)(4)] (1) and {[Na(B15-C-5)] [Na(B15-C-5) (H2O)]} [Pt(SCN)(4)] (2) have been synthesized and characterized by IR, elemental analysis, X-ray diffraction analysis. 1 belongs to monoclinic, space group P2(1)/n with cell dimensions: a = 1.0164(6) nm, b = 1.3743(3) nm, c = 1.4987(7) nm, beta = 95.248(6)degrees, V = 2.0847 nm(3), Z = 2, D-calcd = 1.47 g/cm(3), F (000) = 944, R = 0.053, wR = 0.072. 2 is triclinic crystal system, space group P (1) over bar with cell dimensions: a = 1.1484(2) nm, b = 1.4210(3) nm, c = 1.5026 (3) nm, alpha = 62.500 (3)degrees, beta = 72.393 (3)degrees, gamma = 73.106(4)degrees, V = 2.0398(7) nm(3), Z = 2, D-calcd = 1.674 g/cm(3), F (000) = 1028, R-1 = 0.0327, wR(2) = 0.0885. 1 is composed of two [Na(B15-C-5)](+) complex cations and one [Pd(SCN)(4)](2-) Complex anion. Complex cations and complex anion form neutral complex through Na-N interactions. Two [Na(B15-C-5)](+) are trans-orientation with respect to Pd atom. 2 is made up of [Na(B15-C-5)](+) and [Na(B15-C-5)(H2O)](+) Complex cations and one [Pt(SCN)(4)](2-) complex anion. They also form neutral complex through Na-N interactions. [Na(B15-C-5)](+) and [Na(B15-C-5)(H2O)](+) are cis-orientation with respect to Pt atom. Two molecules of 2 form dimer structure though hydrogen bonds of H2O and N atom of SCN group.
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