| 双（N－氰基亚氨基二硫代甲酸）合镍（Ⅱ）酸－（5，7，7，12，14，14－六甲基－1，4，8，11－四氮杂环十四－4，11－二烯）合镍（Ⅱ）的合成与晶体结构 |
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| 引用本文： | 谢斌,李金山. 双（N－氰基亚氨基二硫代甲酸）合镍（Ⅱ）酸－（5，7，7，12，14，14－六甲基－1，4，8，11－四氮杂环十四－4，11－二烯）合镍（Ⅱ）的合成与晶体结构[J]. 四川理工学院学报(自然科学版), 1995, 0(4) |
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| 作者姓名： | 谢斌 李金山 |
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| 作者单位： | 四川轻化工学院基础部，南开大学元素有机化学研究所 |
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| 摘 要： | 通过盐消除反应合成了双核镍的加合物［Ｎｉ（ｈｍｔａｄｅ）］［Ｎｉ（ｃｄｃ）２］，其中ｈｍｔａｄｅ＝５，７，７，１２，１４，１４－六甲基－１，４，８，１１－四氮杂环十四－４，１１－二烯，ｃｄｃ＝Ｎ－氰基亚氨基二硫代甲酸根。用元素分析、红外光谱、电子光谱和磁化率对它进行了表征。用Ｘ－射线测定了单晶的晶体结构，晶体属单斜晶系，空间群为Ｃ２／Ｃ，晶胞参数ａ＝１１．８８３（２）Ａ，ｂ＝１１．７５３（２）Ａ，Ｃ＝２０．４８２（４）Ａ，ａ＝９０°，β＝１００．１９（１）°，ｒ＝９０°，Ｖ＝２８１５．４Ａ３，Ｍ＝６２８．１９，Ｄｘ＝１．４８２ｇ／ｃｍ２，Ｚ＝４，Ｒ＝０．０４７，Ｒｗ＝０．０５４。正离子的［ＮｉＮ４］为近似平面构型，整个正离子的外形是马鞍型；负离子的［ＮｉＳ４］为绝对平面。在Ｎ（１）和Ｎ（１１）之间形成了氢键，使得加合物呈一维线性链结构。
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| 关 键 词： | 加合物；光谱；晶体结构 |
SYNTHESIS&CRYSTAL STRUCTURE OF (5,7,7,12, 14, 14-HEXAMETHYL-1, 4,8, 11-TETRAAZACYCLOTETRADECA-4,11-DIENO)NICKELOUS BIS(N-CY ANODITHIOCARBAMITO)NICKELATE(Ⅱ) |
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| Xie Bin. SYNTHESIS&CRYSTAL STRUCTURE OF (5,7,7,12, 14, 14-HEXAMETHYL-1, 4,8, 11-TETRAAZACYCLOTETRADECA-4,11-DIENO)NICKELOUS BIS(N-CY ANODITHIOCARBAMITO)NICKELATE(Ⅱ)[J]. Journal of Sichuan University of Science & Engineering(Natural Science Editton), 1995, 0(4) |
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| Authors: | Xie Bin |
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| Affiliation: | Xie Bin(Dept.of Basic Courses Sichuan Institute of Light Ind. & Chem.Tech. Zigong 643033 )Li Jinshan(Institute of Elementorganic Chemistry Nankai University Tinjing 300071 ) |
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| Abstract: | A binuclear nickel adduct [Ni(hmtade )][Ni (cdc )2] is prapared by the salt elliment reactions,where hmtade=5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene and cdc=N-cyanodithiocarbamic acid radical,and characterized with elemental analyses, infrared and electronic spctra, as well as magnetic susceptibility.The crystal and molecular structrue are determined hi single-crystal X-ray diffracton.The unin-cell is triclinic,space group C2/C with a= 11.883(2)A, b= 11.753 (2)A,c= 20.482(4) A, a=90°,β= 1001.19(1 )°,r= 90°,y =2815.4A,M = 628.19, Dx = 1.482g/cm3, Z = 4, R = 0.047, Rw=0.054.The group[NiN4] of cation approximates a planar configuration,but the form and structure of canon is the shape of saddle;The group[NiS4] of anion is a absolute plane.The hydrogen bond is formed between N(1)and N(11),which result in the formation of one-dimentional linear chain for the adduct. |
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| Keywords: | adduct spectrum crystal structure |
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