含四氮杂十四元大环配体过渡金属配正离子与双(N-氰基亚胺基二硫代甲酸)合镍负离子加合物的合成、表征和[Ni(hmtade)][Ni(cdc)_2]的晶体结构  

Synthesis and Characterization of Adducts of Transition-metal Complex Cations Containing Tetra-azatetradeca-membered Ring Ligands with Bis( N-cyanodithiocarbimato)nickelate Anion and Crystal Structure of [Ni(hmtade)][Ni(cdc)_2]

作　　者：李金山[1] 谢斌[2] 

机构地区：[1]南开大学元素有机化学研究所,天津300071 [2]四川轻化工学院基础部,自贡643033

出　　处：《化学学报》1997年第9期892-900,共9页Acta Chimica Sinica

基　　金：国家自然科学基金资助课题

摘　　要：合成了七个含四氮杂十四元大环配体过渡金属配正离子与双(N-氰基亚胺基二硫代甲酸)合镍负离子的加合物[ML][Ni(cdc)_2](cdc=N-氰基亚胺基二硫代甲酸根;L=hmtade,hmta,dmtade,tmtate;M=Cu,Ni,Zn),通过元素分析、红外光谱、电子光谱、磁化率和顺磁共振谱对加合物结构进行了表征.测定了[Ni(hmtade)][Ni(cdc)_2」的晶体结构,其晶体属单斜晶系,C2/c空间群,晶胞参数:a=1.1883(2),b=1.1753(2),c=2.0482(4)nm.α=90°,β=100.19(1)°,r=90°.V=2.8154nm^3,M_r=630.19.D_x=1.482g/cm^3,Z=4.对正负离子间的相互作用进行了讨论.Seven adducts of transition - metal complex cations containing tetra - azatetradeca -membered ring ligands with bis(N - cyanodithiocarbimato)nickelate anion, [ML] [Ni(cdc)2] (cdc = N - cyanodithiocarbimate; L = hmtade, hmta, dmtade, tmtate; M - Cu, Ni, Zn), have been synthesized. The structures of these adducts have been characterized by elemental analysis, infra -red spectra, electronic spectra, electron paramagnetic resonance spectra and magnetic susceptibility. The crystal structure of [Ni(hmtade)] [Ni(cdc)2] has been determined. The crystal belongs to monoclinic, space group C2/c. The cell parameters are a = 1. 1883 (2), b = 1. 1753(2),c = 2.0482(4)nm. α = 90°,β= 100.19(1)°. γ = 90°, V = 2.8154nm3,Mr = 630.19, Dx = 1.482g/cm3,Z=4.The interaction between cation and anion has been discussed.

关 键 词：镍负离子 加合物 晶体结构 四氮杂 大环配体 

分 类 号：O614.813[理学—无机化学]