一种新型杂双金属Mo/Au/S簇合物的合成和晶体结构
Synthesis and crystal structure of a new heterobimetallic Mo/Au/S cluster
以[Et4N]2[Mo2S2(μ-S)2(edt)2] (edt = ethanedithiolate) (1)为预制件，与[Au(PPh3)Cl]在甲醇/乙腈的混合溶剂中反应得到一个新型杂双金属Mo/Au/S簇合物[Et4N][Mo2S4(AuPPh3)(edt)2]·0.25Et2O·0.25MeOH (2·0.25Et2O·0.25MeOH)。对其进行了元素分析、红外光谱及X-射线单晶衍射分析表征。2·0.25Et2O·0.25MeOH属于单斜晶系C2/c空间群，a = 20.117(4), b = 9.2705(19), c = 44.418(9) Å, β = 93.19(3)º, V = 8271(3) Å3, Z = 8, Dc = 1.794 g/cm3, T = 193 K, C31.25H43AuMo2NO0.50PS8, Mr = 1116.96, F(000) = 4380, μ(MoKα) = 4.603 mm-1, S = 1.019, R = 0.0672和wR = 0.1708 （对I > 2.0s(I)的7243个可观察衍射数据）。2的阴离子具有一个蝴蝶形的Mo2S4Au簇核，该簇核是由一个[AuPPh3]+阳离子与[(edt)2Mo2(S)2(m-S)2]中的一个桥联S原子和两个端基S原子配位所形成。中心Au(I)原子采取准四面体配位几何构型，Au-S的长度介于2.425(2)–2.898(3) Å之间。
Et4N]2[Mo2S2(μ-S)2(edt)2] (edt = ethanedithiolate) (1) was used as precursor to react with [Au(PPh3)Cl] in MeOH/MeCN, which resulted in a new heterobimetallic Mo/Au/S cluster [Et4N][Mo2S4(AuPPh3)(edt)2]·0.25Et2O·0.25MeOH (2·0.25Et2O·0.25MeOH). It was characterized by elemental analysis, IR spectrum and X-ray diffraction. 2·0.25Et2O·0.25MeOH crystallizes in the monoclinic system, space group C2/c with a = 20.117(4), b = 9.2705(19), c = 44.418(9) Å, β = 93.19(3)º, V = 8271(3) Å3, Z = 8, Dc = 1.794 g/cm3, T = 193 K, C31.25H43AuMo2NO0.50PS8, Mr = 1116.96, F(000) = 4380, μ(MoKα) = 4.603 mm-1, S = 1.019, R = 0.0672 and wR = 0.1708 for 7243 observed reflections with I > 2σ(I). The anion of 2 consists of a butterfly-shaped Mo2S4Au core in which one [AuPPh3]+ cation is coordinated by one bridging S and two terminal S atoms of the [(edt)2Mo2(S)2(m-S)2] moiety. The Au(I) center adopts a pseudo-tetrahedral coordination geometry, while the Au-S bond lengths vary from 2.425(2)–2.898(3) Å.
郎建平、唐晓艳、虞虹、张勇、张文华
化学晶体学
无机化学钼簇合物金簇合物硫簇合物合成晶体结构
inorganic chemistrymolybdenum clustergold(I) clustersulfur clustersynthesiscrystal structure
郎建平,唐晓艳,虞虹,张勇,张文华.一种新型杂双金属Mo/Au/S簇合物的合成和晶体结构[EB/OL].(2009-01-05)[2025-08-16].http://www.paper.edu.cn/releasepaper/content/200901-107.点此复制
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