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 |
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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2.39Å。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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