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insertion reaction of cs
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Colorless (Bu~tSAg)_n and PPh_3 was dissolved in CS_2, from which orange crystal formed. The structure of the crystal was shown to be (PPh_3)_2Ag(S_2CSBu~t) by single crystal X-ray diffraction method. Thus, the reaction constitutes a novel insertion reaction of CS_2 into Ag—S bond. The reaction was reversible, CS_2 lost at 120—130℃. The crystal belongs to triclinic space group P1,with unit cell parameters: a=10.571(1), b=13.638 (3) ,c=14.391(3)(?), α=88.75(2), β=72.84(1), γ= 80.58...

Colorless (Bu~tSAg)_n and PPh_3 was dissolved in CS_2, from which orange crystal formed. The structure of the crystal was shown to be (PPh_3)_2Ag(S_2CSBu~t) by single crystal X-ray diffraction method. Thus, the reaction constitutes a novel insertion reaction of CS_2 into Ag—S bond. The reaction was reversible, CS_2 lost at 120—130℃. The crystal belongs to triclinic space group P1,with unit cell parameters: a=10.571(1), b=13.638 (3) ,c=14.391(3)(?), α=88.75(2), β=72.84(1), γ= 80.58 (1)~o, V=1954.9(?)~3, Z=2.D_c= 1.36g/cm~3, D_m=1.36g/cm~3. The structure was refined to R=0.0454 and R_w=0.043 for 3572 reflections. The Ag atom is pseudotetrahedrally coordinated by two S atoms of thioxanthate ligand, Bu~tSCS_2, and two P atoms of PPh_3 ligands. The trithiocarbonate CS_3 group resulted from insertion of CS_2 into Ag—S bond is approximately planar. The C—S bond lengths of CS_3 are distinctly longer than that of uncoordinated CS_2 molecule and shorter than the single-bond length. Its IR spectrum was determined.

白色的[Bu~tSAg]_n与PPh_3溶于CS_2中,析出桔黄色晶体。经X射线单晶结构分析其结构为(PPh_3)_2Ag(S_2CSBu~t)。发现了一个CS_2在Ag—S键中的插入反应。此反应为可逆反应,晶体在120—230℃失去CS_2。晶体属三斜晶系,空间群PI,a=10.571(1),b=13.638(3),c=14.391(3)A,a=88.75(2),β=72.84(1),γ=80.58(1)°,V=1954.9A~3,D_o=1.36g/cm~3,D_m=1.36g/cm~3,Z=2.3572个衍射点参与修正,R=0.045,R_w=0.043。Ag原子以变形四面体与硫代黄原酸配体Bu~tS—CS_2的两个S原子及两个PPh_3的P原子配位。插入反应形成的CS_3基团基本上共面,其C—S键长比CS_2中的键长明显加长,而比单键的C—S键长要短,并在红外光谱上出现特征吸收峰。

 
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