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有机化学
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有机化学 ›› 2004, Vol. 24 ›› Issue (7): 788-791. 上一篇    下一篇

研究论文

含环偶磷氮烷配体的羰基铁衍生物的合成和晶体结构

宫培军, 吴秉芳*, 刘树堂, 王丁泽   

  1. 内蒙古大学化学化工学院 呼和浩特 010021
  • 收稿日期:2003-07-15 修回日期:2003-10-09 接受日期:2004-02-09 发布日期:2022-09-20
  • 通讯作者: *E-mail: ndwbf@imu.edu.cn
  • 基金资助:
    国家自然科学基金(No. 29861001)和内蒙古自治区高等学校科学基金(No. ZD01071)资助项目

Synthesis and Crystal Structures of Carbonyl Iron Derivatives Containing Cyclodiphosphazane Ligand

GONG, Pei-Jun, WU, Bing-Fang*, LIU, Shu-Tang, WANG, Ding-Ze   

  1. College of Chemistry and Chemical Engineering , Inner Mongolia University, Huhhot 010021
  • Received:2003-07-15 Revised:2003-10-09 Accepted:2004-02-09 Published:2022-09-20

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用Fe3(CO)12与顺-2,4-二(叔丁基胺基)-1,3-二(叔丁基)-1,3,2,4-环偶磷氮烷cis-[P(NHBu-t)NBu-t]2 (L) 反应,得到两个新的含偶磷氮环的单核羰基铁衍生物:Fe(CO)4[｛P(NHBu-t)NBu-t｝2] (1)和Fe(CO)4[P(NHBu-t)(NBu-t)2P(O)H] (2).对它们进行了元素分析,IR和1H NMR谱表征,并用X-ray单晶衍射法测定了晶体结构.1:正交晶系,Pna2(1)空间群,a=1.7038(9) nm, b=0.8856(5) nm, c=3.5659(18) nm, V=5.381(5) nm3, Dc=1.275 g/cm3, Z=8. 2:单斜晶系,P2(1)/n空间群,a=0.9999(2) nm, b=1.4476(3) nm, c=1.5559(3) nm, β=92.40(3)°, V=2.2504(8) nm3, Dc=1.361g/cm3, Z=4.在两个羰基铁化合物中,配位基偶磷氮烷环以单齿P原子与Fe原子配位.2中,未配位P(III)被氧化成具有膦酰基结构[P(O)H]的P(V).

关键词: 羰基铁衍生物, 环偶磷氮烷配体, 合成, 晶体结构

The reaction of Fe3(CO)12 with cis-2,4-di(tert-butylamino)-1,3-di(tert-butyl)-1,3,2,4-cyclodiphosph-azane (L), yielded two novel mononuclear carbonyl iron derivativescontaining cyclodiphosphazane ligand, Fe(CO)4[｛P(NHBu-t)NBu-t｝2] (1) and Fe(CO)4[P(NHBu-t) (NBu-t)2P(O)H] (2). These compounds were characterized by elemental analysis, IR and 1H NMR spectra, and the structures of 1 and 2were determined by single-crystal X-ray diffraction. 1: orthorhombic, Pna2(1), a=1.7038(9) nm, b=0.8856(5) nm, c=3.5659(18)nm, V=5.381(5) nm3, Dc=1.275 g/cm3, Z=8. 2:monoclinic, P2(1)/n, a=0.9999(2) nm, b=1.4476(3) nm, c=1.5559(3) nm, β=92.40(3)°, V=2.2504(8) nm3, Dc=1.361 g/cm3, Z=4. In the two carbonyl iron derivatives, the phosphorus-nitrogen heterocycles were not cleaved during the reaction, and one P atom of them was coordinated to Featom. In the compound 2, another P(III) atom was oxidized to the P(V), phosphonic amide P(O)H, in which the bond between P and NHBu-t group was cleaved and one P—H bond was formed.

Key words: carbonyl iron derivative, cyclophosphazaneligand, synthesis, crystal structure