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化学学报
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化学学报 ›› 1989, Vol. 47 ›› Issue (8): 744-750. 上一篇    下一篇

研究论文

铁铂硫原子簇化合物的合成与结构研究 V: [MoFe3S4]类立方烷簇合物的转化反应和[Et4N]3[Mo2Fe6S8(SC6H4CH3-m)3Cl6]的晶体结构

康北笙;蔡进华;吴达旭;刘汉钦;刘秋田;翁林红;卢嘉锡   

  1. 中国科学院福建物质结构研究所
  • 发布日期:1989-08-15

Synthesis and structural studies of Mo-Fe-S compounds V: Transformation of cluster skeletons of compounds with [MoFe3S4] unit and crystal structure of [Et4N]3[Mo2Fe6S8Cl6(SC6H4CH3-m)3]

KANG BEISHENG;CAI JINHUA;WU DAXU;LIU HANQIN;LIU QIUTIAN;WONG LINHONG;LU JIAXI   

  • Published:1989-08-15

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具[MoFe2S4]类立方烷结构单元的双类立方烷化合物[Et4N]4[Mo2Fe7S8(SR)12](1a,R=Ph; 1b, R=tolyl-m)或单类立方烷化合物[MoFe3S4(dteR2)5](2a, R=Me; 2b, R=Et)与酰氯在乙腈中反应, 分别得到不含Fe桥的双类立方烷化合物(Et4N)3[Mo2Fe6S8(SR)3Cl6](3a, R=Ph; 3b, R=toly-m)与[MoFe3S4]骨架支解后的Fe(dteR2)2Cl(4a, R=Me; 4b, R=Et)。说明在相同反应条件下, [MoFe3S4]单元在1中比在2中稳定, 本文首次将1型与3型结构通过一步化学反应连系起来。3型化合物的产生得到X射线衍射测定及^1H NMR谱的证实。本文报道3b的单晶结构及3的^!H NMR数据, 3b属六方晶系, P63/m, a=1.6827(3), c=1.5951(16)nm; V=3.91158nm^3; Dc=1.491g/cm^3;Z=2; F(000)=1780; 偏离因子R=0.048, 化合物2与酰氯反应产生4, 由红外及紫外可见光谱证实。

关键词: 晶体结构测定, Ｘ射线衍射分析, 转化, 铁络合物, 四氢呋喃, 固氮酶, 钼络合物, 簇状化合物, 硫络合物, 立方烷

Dicubane clusters [Et4N]4[Mo2Fe7S8(SR)12] (I; R = Ph, m-tolyl) of monocubane clusters [MoFe3S4(dtcR2)5] (II; R = Me, Et) reacted with AcCl in MeCN to give the dicubanes [Et4N]3[Mo2Fe6S8Cl6(SR)3] (III; R = Ph, m-tolyl) without bridging Fe atom and Fe(dtcR2)2Cl (IV; R = Me, Et) without the [MoFe3S4] skeleton, resp. These reactions indicate that under similar reaction conditions, the [MoFe3S4] cubane-like unit is more stable in I than in II. For the first time correlated structure I was correlated with structure III by chem. reactions. Single crystal of III (R = m-tolyl) is hexagonal, space group P63/m, a 1.6827(3), c 1.5951(16) nm; Z = 2; dc = 1.491 g/cm3; F(000) = 1780, for 1296 unique data, R = 0.048. The spectral data of III and IV are reported.

Key words: CRYSTAL STRUCTURE DETERMINATION, X-RAY DIFFRACTION ANALYSIS, EVOLUTIONS, IRON COMPLEX, TETRAHYDROFURAN, NITROGENASE, MOLYBDENUM COMPLEX, CLUSTER COMPOUND, SULFIDE COMPLEX, CUBANE

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