Synthesis and Crystal Structure of a New Mo/Au/S Cluster [Et_4N][Mo_2S_4(AuPPh_3)(edt)_2]· 0.25Et_2O·0.25MeOH(edt=Ethanedithiolate)  

Synthesis and Crystal Structure of a New Mo/Au/S Cluster [Et_4N][Mo_2S_4(AuPPh_3)(edt)_2]· 0.25Et_2O·0.25MeOH(edt=Ethanedithiolate)

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作  者:张文华 虞虹 唐晓艳 张勇 郎建平 

机构地区:[1]College of Chemistry Chemical Engineering and Materials Science, Suzhou University

出  处:《Chinese Journal of Structural Chemistry》2009年第6期669-672,共4页结构化学(英文)

基  金:supported by the National Natural Science Foundation of China (No. 20525101 and 20871088);the "SooChow Scholar" Program and Program for Innovative Research Team of Suzhou University

摘  要:Reactions of the preformed cluster precursor [Et4N]2[Mo2S2(μ-S)2(edt)2] (edt = ethanedithiolate) (1) with [Au(PPh3)Cl] in MeOH/MeCN gave rise to 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 analysis. 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) A^°, β= 93.19(3)°, V = 8271(3) A^°^3, Z = 8, Dc = 1.794 g/cm^3, T = 193 K, C31.25H43AuMo2NO0.50PS8, Mr = 1116.96, F(000) = 4380, μ(MoKa) = 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(μ-S)2] moiety. The Au(I) center adopts a pseudo-tetrahedral coordination geometry, and the Au-S bond lengths vary from 2.425(2) to 2.898(3)A^°.Reactions of the preformed cluster precursor [Et4N]2[Mo2S2(μ-S)2(edt)2] (edt = ethanedithiolate) (1) with [Au(PPh3)Cl] in MeOH/MeCN gave rise to 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 analysis. 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) A^°, β= 93.19(3)°, V = 8271(3) A^°^3, Z = 8, Dc = 1.794 g/cm^3, T = 193 K, C31.25H43AuMo2NO0.50PS8, Mr = 1116.96, F(000) = 4380, μ(MoKa) = 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(μ-S)2] moiety. The Au(I) center adopts a pseudo-tetrahedral coordination geometry, and the Au-S bond lengths vary from 2.425(2) to 2.898(3)A^°.

关 键 词:molybdenum duster gold(I) duster sulfur cluster synthesis crystal structure 

分 类 号:O621.2[理学—有机化学]

 

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