化学学报 ›› 2005, Vol. 63 ›› Issue (12): 1087-1094. 上一篇    下一篇

研究论文

巢式十一顶铂硼烷簇合物的合成与晶体结构

窦建民*1 2,武立斌1,郭庆良1,李大成1,王大奇1,胡春华2,郑培菊2   

  1. (1聊城大学化学化工学院 聊城 252059)
    (2复旦大学分析测试中心 上海 200433)
  • 投稿日期:2004-11-16 修回日期:2005-02-16 发布日期:2010-12-10
  • 通讯作者: 窦建民

Synthesis and Crystal Structure of the nido 11-Vertex Platinaborane Clusters

DOU Jian-Min*1,2, WU Li-Bin1, GUO Qing-Liang1, LI Da-Cheng1, WANG Da-Qi1, HU Chun-Hua2, ZHENG Pei-Ju2   

  1. (1 Department of Chemistry, Liaocheng University, Liaocheng 252059)
    (2 Research Center of Analysis and Measurement, Fudan University, Shanghai 200433)
  • Received:2004-11-16 Revised:2005-02-16 Published:2010-12-10
  • Contact: DOU Jian-Min

[PtCl2(PPh3)2]与B10H102-在异丙醇中回流反应, 得到3个巢式十一顶铂十硼烷簇合物: [(PPh3)2PtB10H11-9-O-i-Pr] (1), [(PPh3)2PtB10H10-8,10-(O-i-Pr)2] (2)和[(PPh3)2PtB10H11-8-O-i-Pr] (3). 簇合物13都具有PtB10多面体骨架结构, 其中Pt原子位于敞开的PtB4面上, 且与4个B原子成键, 每个Pt原子还与2个PPh3基团中的P原子成键. 将溶剂热合成的方法引入到硼簇合物的合成中并进行同一反应, 得到2个B10H102-降解的巢式十一顶双铂九硼烷簇合物: [(PPh3)2(μ-PPh2)Pt2B9H6-3,9,11-(O-i-Pr)3] (4)和[(PPh3)2(μ-PPh2)Pt2B9H6-3,9-(O-i-Pr)2-11-Cl] (5). 簇合物45都具有Pt2B9多面体骨架结构, 2个Pt原子位于敞开的Pt2B3面上的相邻位置, 且由一个PPh2基团桥连, 每个Pt原子还与3个B原子和一个PPh3基团中的P原子成键. 通过红外光谱、元素分析、X射线单晶衍射对5个簇合物进行了结构表征.

关键词: 巢式构型, 铂硼烷, 簇合物, 溶剂热合成, 晶体结构

Three nido 11-vertex platinaundecaborane clusters: [(PPh3)2PtB10H11-9-O-i-Pr] (1), [(PPh3)2PtB10H10-8,10-(O-i-Pr)2] (2) and [(PPh3)2PtB10H11-8-O-i-Pr] (3) were obtained from the reaction of [PtCl2(PPh3)2] with (Et4N)2B10H10 in i-PrOH under reflux conditions. They all have a nido 11-vertex PtB10 polyhedral skeleton, in which Pt atom lies on the open PtB4 face. Each Pt atom was connected with four B atoms and two P atoms of PPh3 ligand. Two novel B10H102- deboronated nido 11-vertex diplatinaundecaboranes: [(PPh3)2(μ-PPh2)Pt2B9H6-3,9,11-(O-i-Pr)3] (4) and [(PPh3)2(μ-PPh2)Pt2B9H6-3,9-(O-i-Pr)2-11-Cl] (5) were obtained when the same reaction was carried out under solvothermal conditions. Cluster compounds 4 and 5 have a nido 11-vertex Pt2B9 polyhedral skeleton, in which two Pt atoms stay at neighbouring positions of the open Pt2B3 face and bridged by a PPh2 ligand. Each Pt atom was connected with three B atoms and a P atom of PPh3 ligand. They were characterized by IR spectroscopy, elemental analysis and single-crystal X-ray diffraction.

Key words: nido configuration, platinaborane, cluster, solvothermal synthesis, crystal structure