高等学校化学学报

高等学校化学学报 ›› 2004, Vol. 25 ›› Issue (7): 1199.

• 研究论文 • 上一篇    下一篇

稀土氧化膦取代杯芳烃配合物的合成与结构

赵明新1, 朱文祥1, 马淑兰1, 袁大强1, 王哲明2, 王如骥3   

  1. 1. 北京师范大学化学系, 北京 100875;
    2. 北京大学化学与分子工程学院, 稀土材料化学与应用国家重点实验室, 北京 100871;
    3. 清华大学分析测试中心, 北京 100084
  • 收稿日期:2003-08-18 出版日期:2004-07-24 发布日期:2004-07-24
  • 通讯作者: 朱文祥(1941年出生),男,教授,博士生导师,从事大环配位化学研究.E-mail:wx-zhu@263.net E-mail:wx-zhu@263.net
  • 基金资助:

    北京市自然科学基金(批准号:2022011)资助

Syntheses and Crystal Structures of Rare Earth Nitrate Complexes with Phosphinoxide [-CH2P(O)Ph2]-substituted Calix[4]arene

ZHAO Ming-Xin1, ZHU Wen-Xiang1, MA Shu-Lan1, YUAN Da-Qiang1, WANG Zhe-Ming2, WANG Ru-Ji3   

  1. 1. Departement of Chemistry, Beijing Normal University, Beijing 100875, China;
    2. State Key Laboratory of Rare Earth Materials Chemistry and Application, College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China;
    3. Center of Analysis and Measurement, Tsinghua University, Beijing 100084, China
  • Received:2003-08-18 Online:2004-07-24 Published:2004-07-24

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被引次数

6

摘要： 合成了一种新的氧化膦取代杯芳烃衍生物的稀土离子(La3+,Eu3+)硝酸盐配合物.通过元素分析和红外光谱对配合物进行了表征.在无水甲醇中培养出了配合物的单晶,用X射线单晶衍射法测定了其晶体结构.硝酸镧配合物晶体[L·La(OH2)(NO3)2]NO3{L为四(亚甲基二苯基氧化膦)杯[4]芳烃}属四方晶系,空间群P43212,晶胞参数a=b=1.8977(4)nm,c=3.1087(11)nm;Z=4;V=11.196(5)nm3;Dc=1.097g/cm3,F(000)=3712,μ=0.491mm-1,R1=0.1181,wR2=0.1930.硝酸铕配合物晶体[L·Eu(OH2)(NO3)2]NO3·CH3OH属单斜晶系,空间群C2/c,晶胞参数a=2.88172(11)nm,b=5.4015(2)nm,c=2.01189(7)nm;β=133.4067(9)°,Z=8;V=22.7511(14)nm3,Dc=1.106g/cm3,F(000)=7464,R1=0.0671,wR2=0.1794.2个配合物的晶体结构相类似,配合物中配体的4个磷氧键上的氧原子、2个双齿配位的硝酸根中的4个氧原子还有1个水分子中的氧原子分别参与了配位.中心离子配位数为9,配位多面体为单帽四方反棱柱体.另外在铕配合物的杯芳烃中还包合了1个甲醇分子.

关键词: 镧铕稀土离子配合物, 氧化膦取代杯芳烃, 晶体结构

Abstract: Two rare earth nitrate complexes with phosphinoxide (-CH2P(O)Ph2)-substituted calix arene were prepared and characterized by elemental analysis and IR spectroscopy. Their crystal structures were determined by X-ray diffraction method. Lanthanum nitrate complex [L·La(OH2)(NO3)2]NO3( L=tetrakis(methylenediphenylphosphinoxide)calixarene) belongs to tetragonal crystal system, space group P43212 with a=1.897 7(4) nm, b=1.897 7(4) nm, c=3.108 7(11) nm; Z=4; V=11.196(5) nm3; Dc=1.097 g/cm3, F(000)=3 712, μ=0.491 mm-1, R1=0.118 1, wR2=0.193 0. Europium nitrate complex [L·Eu(OH2)(NO3)2]NO3·CH3OH belongs to monoclinic crystal system, space group C2/c with a=2.881 72(11) nm, b=5.401 5(2) nm, c=2.011 89(7) nm; β=133.406 7(9)°, Z=8; V=22.751 1(14) nm3, F(000)=7 464, R1=0.067 1, wR2=0.179 4. The structures of the two complexes are very similar, the rare earth atoms are both nine-coordinated with four oxygen atoms from phosphorus-oxygen bonds and four oxygen atoms from two bidentate nitrate anions and one oxygen atom from a water molecule. The coordination polyhedron is a single-capped square antiprism. In the europium complex, a methanol molecule was included in the calixarene.

Key words: Lanthanum and europium ionic complexes, Phosphinoxide[-CH2P(O)Ph2]-substituted calix[4]arene, Crystal structures

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