中性磷(膦)类希土萃合物的结构研究——Ⅱ.四(三苯基氧膦)合硫氰酸钕的合成及结构测定
STRUCTURAL STUDIES ON EXTRACT OF RARE EARTH WITH NEUTRAL ORGANOPHOSPHORUS EXTRACTANTS—II.SYNTHESIS AND CRYSTAL STRUCTURE OF TRITHIOCYANATOTETRAKIS (TRIPHENYL PHOSPHINE OXIDE) NEODYMIUM
作者单位
黄春辉 北京大学化学系 
徐荣芳 北京大学化学系 
徐小杰 北京大学化学系 
徐光宪 北京大学化学系 
摘要: 合成了四(三苯基氧膦)合硫氰酸钕配合物,通过元素分析及分子量测定,确定了该配合物的化学式为Nd(NCS)3·4ph3P=O。经x射线单晶衍射测定了该配合物的结构,晶体属单斜晶系,P21/C空间群,晶体学参数如下: a=13.221(7)Å v=6943Å3 b=23.544(14)Å z=4 c=22.821(18)Å d实验值=1.375g/cm3 β=102.19(5)° d计算值=1.370g/cm3 F(0,0,0,0)=2924e 吸收系数μ=9.8cm-1(MoKa) 钕的配位数为七,三个NCS-根以氮与钕配位,平均键长2.50Å,四个三苯基氧膦以膦酰基上的氧与钕配位,平均Nd—O键长2.39Å。分子具有近似的C8对称性。
关键词: 希土萃合物  结构  合成  四(三苯基氧膦)合硫氰酸钕
基金项目: 
Abstract: As a part of a project in our laboratory to carry out the complexes of rare earth with neutral organophosphorus extractants,the synthesis and crystal structure of a neodymium complex,Nd(NCS)34ph3P=O,have been presented in this report.The crystal and molecular structure have been determined by single crystal X-ray diffraction techniques with a four circle diffractometer of Nico-let model R3. The crystal is monoclinic with space group P21/c. The unit cell parameters are a=13.221(7)Åβ=102.19(5)°z=4 b=23.544(14)ÅF(0,0,0,0)=2924e Dexp.=1.375g/cm3c=22.821(18)Åv=6943Å3Dcal.=1.370g/cm3The neodymium atom is coordinated to three nitrogen atoms from the thiocyanates and four oxygen atoms from the triphenylphosphine oxides. The average bond lengths of Nd-N and Nd-O are 2.50Å and 2.39Å respectively. The molecule has a approximate Cs symmetry.
Keywords: extract of rare earth  structure synthesis  trithiocynatotetrakis (triphenyi phosphine oxide)  neodymium
投稿时间:1985-04-23 
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黄春辉,徐荣芳,徐小杰,徐光宪.中性磷(膦)类希土萃合物的结构研究——Ⅱ.四(三苯基氧膦)合硫氰酸钕的合成及结构测定[J].无机化学学报,1985,1(1):103-112.
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