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二硝酸根二4′,5′-二氮-9′-(4,5-二(硫乙基)-1,3-二硫杂环戊烯-2-叶立德)-芴合镉的合成、结构及光谱性质
引用本文:朱琴玉,张勇,戴洁,桓雪锋.二硝酸根二4′,5′-二氮-9′-(4,5-二(硫乙基)-1,3-二硫杂环戊烯-2-叶立德)-芴合镉的合成、结构及光谱性质[J].无机化学学报,2006,22(7):1170-1174.
作者姓名:朱琴玉  张勇  戴洁  桓雪锋
作者单位:1. 南京大学配位化学国家重点实验室,南京,210093
2. 苏州大学化学化工学院,江苏省有机合成重点实验室,苏州,215006
基金项目:中国科学院资助项目;江苏省重点实验室基金
摘    要:Cd(NO3)2·4H2O与配体4′,5′-二氮-9′-(4,5-二(硫乙基)-1,3-二硫杂环戊烯-2-叶立德)-芴(L)在甲醇和二氯甲烷的混合溶剂中生成配合物Cd(NO3)2(L)2。晶体的空间群是Pbcn(#60),晶体学参数分别是a=1.578 7(2) nm,b=0.987 96(11) nm,c=2.719 5(3) nm。V=4.241 6(8) nm3Z=4。2个硝酸根离子各提供1个氧原子,2个配体L各提供2个氮原子,形成了镉的6配位结构。晶体结构显示分子通过平面之间的π-π相互作用沿b轴形成柱状结构,这些柱通过中心原子镉(Ⅱ)的配位连接形成二维层状结构,再通过2个硫乙基上的短距离S…S接触进一步形成了三维结构。对其 1H NMR、UV-Vis和荧光光谱进行了研究。

关 键 词:氮-芴    镉配合物    晶体结构    分子间相互作用
文章编号:1001-4861(2006)07-1170-05
收稿时间:2005-06-06
修稿时间:2006-06-01

Synthesis and Crystal Structure of a Cadmium Complex with 4',5'-diaza-9'-(4,5-bis(ethylthio)-1,3-dithiole-2-ylidene)-fluorene
ZHU Qin-Yu,ZHANG Yong,DAI Jie and HUAN Xue-Feng.Synthesis and Crystal Structure of a Cadmium Complex with 4'''',5''''-diaza-9''''-(4,5-bis(ethylthio)-1,3-dithiole-2-ylidene)-fluorene[J].Chinese Journal of Inorganic Chemistry,2006,22(7):1170-1174.
Authors:ZHU Qin-Yu  ZHANG Yong  DAI Jie and HUAN Xue-Feng
Institution:College of Chemistry and Chemical Engineering, Suzhou University, Key Laboratory of Organic Synthesis of Jiangsu Province, Suzhou, Jiangsu 215006;State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093,College of Chemistry and Chemical Engineering, Suzhou University, Key Laboratory of Organic Synthesis of Jiangsu Province, Suzhou, Jiangsu 215006;State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093,College of Chemistry and Chemical Engineering, Suzhou University, Key Laboratory of Organic Synthesis of Jiangsu Province, Suzhou, Jiangsu 215006;State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093 and College of Chemistry and Chemical Engineering, Suzhou University, Key Laboratory of Organic Synthesis of Jiangsu Province, Suzhou, Jiangsu 215006;State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093
Abstract:Reaction of Cd(NO3)2·4H2O with 4',5-diaza-9'-(4,5-bis(ethylthio)-1,3-dithiole-2-ylidene)-fluorene (L) in a mixture of methanol and dichloromethane forms a coordination compound Cd (NO3)2(L)2. The crystal is in orthorhombic space group Pbcn(#60) with crystallographic parameters a=1.578 7(2) nm, b=0.987 96(11) nm, c=2.719 5(3) nm, V=4.241 6(8) nm3 and Z=4. The coordination sphere of Cd(Ⅱ) is satisfied by coordination of two oxygen atoms from two nitrate ions and four nitrogen atoms from two ligands L. Crystal structure shows that the molecules are stacked via plane to plane π-π interactions forming columns along the b axis. These columns are linked to form two-dimensional layer structure by the coordination connection of the center atom Cd(Ⅱ). There are very short S…S contact (0.329 7 nm) between two ethylthio sulfur atoms, so that a three-dimensional structure is further completed. 1H NMR, UV-Vis and fluorescent spectra of the title compound were studied. CCDC: 283826.
Keywords:diaza-fluorene  cadmium complex  crystal structure  intermolecular interaction
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