摘要
研究了 18 冠 6与NiCl2 ·6H2 O,K2 dmit(dmit=4,5 dimercapto 1,3 dithiole 2 thione,C3S2 -5)在不同溶剂中反应生成的两个标题配合物{[K(18 C 6)]2 (C2 H4 Cl2 )}[Ni(dmit)2 ]2 (1)和[K(18 C 6)][Ni(dmit)2 ](2).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均属三斜晶系,空间群P 1.1的晶体学数据:a =1 0 2 72 (2)nm,b =1 2 2 82 (3 )nm,c=1 42 0 5(3 )nm,α =113 473(3 )°,β =90 60 9(3)°,γ =91 43 9(3)°,V =1 64 3 0 (6)nm3,Z =2,F(0 0 0 )=876,R1=0 0 5 0 3 2的晶体学数据:a =0 85 0 2 (2)nm,b=1 2 178(4)nm,c =1 5 118(4)nm,α =86 45 4(5 )°,β =77 73 4(5 )°,γ =85 3 64 (5)°,V =1 5 2 2 8(8)nm3,Z =2,F(0 0 0) =774,R1=0 0 5 65.配合物 1,2分别通过K S,K Cl,S S和K S,S S弱相互作用形成二维。
The novel two- and three-dimensional 18-crown-6 ( 18-C-6) complexes: {[ K (18-C-6)](2)-(C2H4Cl2)}[Ni(dmit)(2)](2) (1) and [K(18-C-6)][Ni(dmit)2] (2) (dmit=4,5-dimereapto-1,3-dithiole-2-thione, C3S(5)(2-)) were synthesized and characterized by elemental analysis, IR spectrum and X-ray diffraction analysis. 1 and 2 belong to triclinic, space group P 1 with cell dimensions of 1: a = 1.0272(2) nm, b = 1.2282(3) nm, c = 1.4205(3) mn, alpha = 113.473(3)degrees, beta = 90.609(3)degrees, gamma = 91.439(3)degrees, V = 1.6430(6) nm(3), Z = 2, F(000) = 876, R-1 = 0.0503 and 2: a = 0.8502(2) nm, b = 1.2178(4) nm, c = 1.5118(4) nm, alpha = 86.454(5)degrees, beta = 77.734(5)degrees, gamma = 85.364(5)degrees, V = 1.5228(8) nm(3), Z = 2, F(000) = 774, R, = 0.0565. The complexes show two- or three-dimensional structure consisting of [K(18-C-6)](+) complex cations and [Ni(dmit)(2)](-) complex anions bridged by (KS)-S-..., (KCl)-Cl-..., (SS)-S-... or (KS)-S-..., (SS)-S-... weak interactions.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
2002年第12期2145-2152,共8页
Acta Chimica Sinica