物理化学学报 >> 1987, Vol. 3 >> Issue (05): 491-500.doi: 10.3866/PKU.WHXB19870510

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中性磷(膦)类稀土萃合物的结构研究(Ⅲ)——三(三苯基氧膦)合硝酸镧的合成及结构测定

黄春辉; 徐荣芳; 周永芬; 徐光宪; 郭芳; 竺迺珏   

  1. 北京大学化学系; 中国科学院化学所
  • 收稿日期:1986-05-08 修回日期:1986-11-27 发布日期:1987-10-15

STUDIES ON NEUTRAL PHOSPHINE EXTRACTED COMPLEXES OF RARE EARTHS Ⅲ. SYNTHESIS AND CRYSTAL STRUCTURE OF TRINITRATOTRI (TRIPHENYL-PHOSPHINE OXIDE) LANTHANUM

Huang Chunhui; Xu Rongfang; Zhou Yongfeng; Xu Guangxian; Guo Fang; Zhu Naijue   

  1. Chemistry Department; Peking University; Institute of Chemistry Academia Sinica; Beijing
  • Received:1986-05-08 Revised:1986-11-27 Published:1987-10-15

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摘要：

合成了三(三苯基氧膦)合硝酸镧络合物, 经鉴定确定络合物化学式为La(NO_3)_3·3ph_3PO·C_2H_5OH·CHCl_3。其中C_2H_5OH和CHCl_3为溶剂化分子。经X射线单晶衍射, 测定了该络合物属单斜晶系P2_1/n空间群, 晶体学参数如下
a=1.3111(5) nm Z=4
b=2.5075(10) nm F(000)=2687.65
c=1.8725(6) nm μ吸收系数=9.83(cm~(-1))
β=98.53(3)° d计算=1.45 gcm~(-3)
V=6.088 nm d实验=1.43 gcm~(-3)
La与9个氧直接配位, 其中六个氧来自三个双卤配位硝酸根, 另三个氧分别由三个苯基氧膦上的膦酰基所提供。La-O平均键长0.2549 nm。

Abstract:

The Synthesis, character and crystal structure of La(NO_3)_3·3Ph_3PO·C_2H_5OH· CHCl_3 has been presented in this paper. Crystal and molecular structure has been determined by single-crystal X-ray diffraction techniques with a four circle diffrac- tometer. The crystal is monoclinic with space group P2_1/n. The unit cell parameters are:
a=1.3111(5) nm Z=4
b=2.5075(10) nm F(000)=2687.65
c=1.8725(6) nm μ(MoKa)=9.83 cm~(-1)
β=98.53(3)° d_(cal.)=1.45 gcm~(-3)
V=6.088 nm d_(lab.)=1.43 gcm~(-3)
8022 independent diffaraction data has been collected, of which 3362 observable independent reflections were used for structure refinement to a final R value of 0.08. The lanthanum atom is coordinated by nine oxygen atoms, of which six from three bidentate nitrate groups and the others from from three Ph_3PO each. The average bond length of La—O is 0.2549 nm.