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作 者:李增新[1] 张子红[2] 王彤[1] 李大成[2] 王大奇[2] 窦建民[2] 郑培菊[3]
机构地区:[1]青岛大学师范学院化学系,青岛266071 [2]聊城师范学院化学系,聊城252000 [3]复旦大学分析测试中心,上海200433
出 处:《化学学报》2002年第8期1465-1472,共8页Acta Chimica Sinica
摘 要:合成了苯并 18 冠 6 (B18 C 6 )与K2 [Pd(SCN) 4],K2 [Pt(SCN) 4]生成的配合物 [K(B18 C 6 ) ]2 [Pd(SCN) 4](1) ,[K(B18 C 6 ) ]2 [Pt(SCN) 4](2 )和 [K(B18 C 6 ) ]2 [Pt(SCN) 4]·C2 H4 Cl2 (3) ,并通过元素分析、红外光谱、单晶X射线衍射进行了表征 .1和 2为单斜晶系 ,空间群P2 1 n ,晶体学数据 :1,a =1 0 0 970 (17)nm ,b =1 315 7(2 )nm ,c=1 730 3(3)nm ,β =94 95 4 (2 )° ,V =2 2 90 2 (7)nm3,Z =2 ,F(0 0 0 ) =10 72 ,R1 =0 0 2 6 7;2 ,a =1 0 0 90 8(18)nm ,b =1 312 4 (2 )nm ,c=1 7317(3)nm ,β =94 84 1(2 )° ,V =2 2 85 2 (7)nm3,Z =2 ,F(0 0 0 ) =1136 ,R1 =0 0 2 5 7.3为三斜晶系 ,空间群P1,晶体学数据 :a =0 95 914 (18)nm ,b =1 2 137(2 )nm ,c =1 2 313(2 )nm ,α =6 3 6 93(2 )° ,β =76 2 93(2 )° ,γ =78 35 3(2 )° ,V =1 2 4 0 6 (4)nm3,Z =1,F(0 0 0 ) =6 18,R1 =0 0 36 6 .在固态 ,三个配合物相邻的两个[K(B18 C 6 ) ]+ 基团通过冠醚氧原子与钾原子相连接而形成一维链状结构 .The reactions of benzo-18-crown-6 (B18-C-6) with K-2[M(SCN)(4)] (M = Pd, Pt) were studied and the complexes [K(B18-C-6)](2)[Pd(SCN)(4)] (1), [K(B18-C-6)](2)[Pt(SCN)(4)] (2) and [K(B18-C-6)](2)[Pt-(SCN)(4)].C2H4Cl2 (3) were characterized by elemental analysis, IR and X-ray diffraction analysis. 1 and 2 belong to monoclihic, space group P2(1)/n with crystal data: 1, a = 1.00970(17) nm, b = 1.3157(2) nm, c = 1.7303(3) nm, beta = 94.954.(2)degrees, V = 2.2902(7) nm(3), Z = 2, F(000) = 1072, R-1 = 0.0267; 2, a = 1.00908(18) nm, b = 1.3124(2) nm, c = 1.7317(3) nm, beta = 94.841(2)degrees, V = 2.2852(7) nm(3), Z = 2, F(000) = 1136, R-1 = 0.0257. 3 belongs to triclinic, space group P1 with crystal data: a = 0.95914(18) nm, b = 1.2137 (2) nm, c = 1.2313(2) nm, alpha = 63.693(2)degrees, beta = 76.293(2)degrees, gamma = 78.353(2)degrees, V = 1.2406(4) nm(3), Z = 1, F(000) = 618, R-1 = 0.0366. In the solid state, the complexes exhibit one-dimensional chain structure of two [K(B18-C-6)](+) complex cations bridged by K atom and O atom of crown ether between adjacent complex cations.
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