CRYSTAL STRUCTURES OF [Bu4N]2[M2Ag3（ μ3—S）2（μ—S）4S2Et2dtc]（M=W,Mo）

<正> The title compounds were prepared from the reation of (NH4)2MS4 (M=W,Mo),AgNO3,NadtcEt2 and Et4NBr in CH3CN-H2O solution. The isomorphous compounds [Bu4N]2[W2Ag3S8Et2du] ( I ) and [Bu4N]2[Mo2Ag3S8Et2dtc] (Ⅱ) crystallize in triclinic space qroup Pi with the following crystal parameters:α=13. 043(4),b = 21. 640(6),c=10. 757(6)A ,α=95. 09(5),β = 91. 90(4),γ = 98. 57(3)°,Z = 2,V = 2987A3,Dc=1. 76g/cm3 for I 5;a= 12. 989(2) ,b=21. 574 (9) ,c= 10. 7/1(1) A .α= 95. 06(7), β=91. 61(4), γ=98. 52(2)°, Z = 2,V = 2961 A3.Dc= 1. 58g/cm3 for Ⅱ . The final R and Rw values are 0. 061 and 0. 072 for Ⅰ ,and 0. 062 and 0. 076 for Ⅱ The M2Ag3 (M = W, Mo) unit in anion M2Ag3S8Et2dtc forms a five-membered ring.     

STRUCTURE OF {Mo4S4（μ—OAc）2[S2P（OC2H5）2]4H}

<正> {Mo4S4(μ-OAc)2(dtp)4H}3,(dtp=S2P(OEt)2),Mr=1371.60,Or-thorhombic, space group Pcab, a = 18. 90 (2) ,b = 21. 678 (4 ) , c = 24. 491 (4 ) A , V = 10031(7)A3,Z=8,Dc=1.818g/cm-3,F(000)=5464,λ(MoKa)=0.71073A,finalR= 0. 069 for 3738 independent reflections. This is a successful example of the formation of [Mo4S4]5+ from[3+1] reaction mode. The results of the structure determination indicate that the configuration of the title compound exhibits a tetranuclear cubane-type core [Mo4S4]5+ with six Mo - Mo distances in the range 2. 685~2. 969A and is very similar to that of the previously characterized compound {Mo4S4(μ-OAc)2(dtp)4}2, [Mo4S4]6+, which was obtained directly by the reaction of MoCl3·3H2O with dtp. Some notable differences, however, can be found when six Mo - Mo bond distances and bonding parameters of the four terminal bidentate ligands (dtp) are compared between these two compounds , That can be attributed to the difference in the oxidation state of these two clusters .     

[Cl3Sb（u0S）sBCl3]^2—阴离子的红外光谱和简正坐标分析

在500－100cm^-1波段范围内测定了[Cl3Sb(u-S)SbCl3]2-阴离子的Fourier变换红外光谱，采用简化的普遍价力场（SGVFF）进行了简正坐标分析，振动基频的计算值与观测值符合良好，两者平均差小于1．0％，证实了振动谱带的归属，确定了相应的力常数，最后讨论了谱带归属问题和所得结果的合理性和可靠性。     

Mo—Cu—S原子簇化合物[Mo2Cu6S6（SCMe3）2（O）2（PPh3）4]（Ⅰ）和[MoCu3S3（S2COEt）

基于标题簇合物的快原子质谱研究，提出该二簇合物在质谱过程中的可能断裂途径及其簇骼转换的相关性。     

新型六核钼原子簇化合物{[Mo3（μ3—S）（μ—S2）2（dtp）3]—（μ3—S）（η…

［Ｍｏ３（μ３－Ｏ）（μ－Ｓ）３（μ－ＯＡｃ（ｄｔｐ）３（ｐｙ）］和［Ｍｏ３（μ－Ｓ）３（μ－ＯＡｃ（ｄｔｐ）３－（ｐｙ）］（ｄｔｐ＝Ｓ２Ｐ（ＯＣ２Ｈ５）２＾－）族合物分别与金属化合物ＢｉＩ３和ＳｂＢｒ３进行原子簇反应均能获得意外产物｛［Ｍｏ３（μ３－Ｓ）（μ－Ｓ２）２（ｄｔｐ）３］（μ３－Ｓ）（η＾３－Ｓ２）［Ｍｏ２（μ３－Ｓ）（μ－Ｓ）３（μ－ＯＡｃ）（ｄｔｐ）２］｝六核钼簇。其结构实际上是由     

盖帽三核钴羰基簇合物（u3—CH3C）Co3（CO）7（u0—PPh2CH2PPh2）和（u3—CH3C）Co3（

本文从结构化学角度，阐述了标题化合物的EI质谱断裂行为，这些化合物的分子离子基本上按分步断裂分别失去羰基，直至获得[CH3CCo3[PPh2CH2PPh2)]^ 和[CH3CCO3]^ ，然后，这些残基和含膦配体继续断裂，失去Ph,PhP,Ph3P,C7H7,C6H6,C2H2,H2和Co等，生成各种相应的三核，二核和单核钴的碎片离子。     

CRYSTAL STRUCTURE OF A SILVER COMPLEX Ag（PPh3）2（S2P—（OCH3）2）

<正> The crystal structure of the title silver complex has been determined by the single crystal X-ray diffraction method.The white plate crystal is tri-clinic.space group P1 with a=12.289(1),b=13.330(2),c=14.846(1)A.α=59.78(1),β=70.33(1),γ=64.01(1)°,V=1867.9A3,Z=2,Dc=1.404 g/ cm3,Mr=789.6,F(000)=808,MoKa radiation,μ(MoKa)=7.891 cm-1,final R=0.049 and Rw=0.051 for 5753 observed reflections.The silver(I)is surrounded by two P and two S atoms in a distorted tetrahedral coordination.