张秀兰,谢斌,邹立科,张玲丽.化学通报,2014,77(8):804-808. |
铬(III)配合物[(PhCH2CH2O)2PS2]3Cr 的合成、表征与晶体结构 |
Synthesis and Crystal Structure of Complex [(PhCH2CH2O)2PS2]3Cr |
投稿时间:2014-01-12 修订日期:2014-01-25 |
DOI: |
中文关键词: O,O’-二烃基二硫代磷酸 合成 表征 晶体结构 |
英文关键词:O,O’-Dialkyldithiophosphate synthesis characterization crystal structure |
基金项目:(cx20121308) |
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中文摘要: |
合成了铬(III)配合物[(PhCH2CH2O)2PS2]3Cr,通过元素分析、红外光谱、紫外-可见光谱、热重分析和X-射线衍射等进行了结构表征。该晶体属于三斜晶系,P-1空间群;晶胞参数为:a=1.39418(3) nm, b=1.40150(3) nm, c=1.47012(3) nm, α=76.3126 (19)?, β=101.033 (3)?, γ=78.7534(17)?, V=2.61241(9) nm3, Dc=1.353 Mg.m-3, Z=2, F(000)=1110, m(Mo Ka)=0.596 mm-1, S=1.019, (D/s)max=0.001, R1=0.0512, wR2=0.1576(I>2s(I))。晶体结构研究表明: 配合物中的(PhCH2CH2O)2PS2-为双齿配体,Cr(III)原子与3个配体(PhCH2CH2O)2PS2-的6个S原子配位形成了畸变八面体构型,Cr─S键长在0.24193(9) ~ 0.24476(9) nm。 |
英文摘要: |
A new complex [(PhCH2CH2O)2PS2]3Crwas synthesized and characterized by elemental analysis, IR, UV-vis, TG-DSC, single crystal and X-ray diffraction analysis. The complex crystallized in triclinic, P-1 space group with the cell parameters: a=1.39418(3) nm,b=1.40150(3) nm,c=1.47012(3) nm,α=76.3126 (19)?,β=101.033 (3)?,γ=78.7534(17)?, V=2.61241(9) nm3, Dc=1.353 Mg.m-3,Z=2,F(000)=1110,m(Mo Ka)=0.596 mm-1,S=1.019,(D/s)max=0.001,R1 = 0.0512,wR2=0.1576(I>2s(I)). In the complex [(PhCH2CH2O)2PS2]3Cr, the chromium(III) ion coordinates with six sulfur atoms from three ligands of (PhCH2CH2O)2PS2-, chromium(III) ion locates at the center of the distorted octagonal. The bond lengthes for Cr─S is in the range of 0.24193(9) ~ 0.24476(9) nm. |
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