Synthesis and Crystal Structure of Novel Sn-O Clusters Generated from ~nBu_2SnO and Esters  

作　　者：雷斌 贾永光 柳凌艳 常卫星 李靖 

机构地区：[1]State Key Laboratory and Institute of Elemento-organic Chemistry,Nankai University

出　　处：《Chinese Journal of Structural Chemistry》2010年第9期1373-1379,共7页结构化学（英文）

基　　金：supported by the National Natural Science Foundation of China (20421202,20372033)

摘　　要：A facile and credible strategy was demonstrated to synthesize two new Sn-O clusters 1 and 2 by the reactions of nBu2SnO with esters directly under mild conditions.Cluster 1 crystallizes in the triclinic system,space group P1 with a = 13.054（3）,b = 13.137（3）,c = 15.077（3） ,α = 80.009（9）,β = 77.187（10）,γ = 76.075（11）°,Z = 2,V = 2427.3（9） 3,Dc = 1.565 g/cm3,μ（MoKα） = 2.076 mm-1,F（000） = 1152,the final R = 0.0335 and wR = 0.0664 for 9416 observed reflections（I 2σ（I））.Cluster 2 belongs to the monoclinic system,space group P21/c with a = 13.673（3）,b = 13.342（3）,c = 16.296（4） ,β = 104.385（5）o,Z = 4,V = 2879.7（10） 3,Dc = 1.347 g/cm3,μ（MoKα） = 1.751 mm-1,F（000） = 1176,the final R = 0.0306 and wR = 0.0706 for 6390 observed reflections（I 2σ（I））.The crystal structures of the clusters consist of cen-trosymmetric [RCOOSnnBu2OSnnBu2OH）]2 molecules with an almost planar Sn4O4 framework.Each pair of exo-and endo-cyclic tin atoms was linked by one bridge-OH only.In addition,a novel structure of nBu2SnO different from the previous reports was proposed on the basis of 1H-NMR,TG analysis and X-ray diffraction.A facile and credible strategy was demonstrated to synthesize two new Sn-O clusters 1 and 2 by the reactions of nBu2SnO with esters directly under mild conditions.Cluster 1 crystallizes in the triclinic system,space group P1 with a = 13.054（3）,b = 13.137（3）,c = 15.077（3） ,α = 80.009（9）,β = 77.187（10）,γ = 76.075（11）°,Z = 2,V = 2427.3（9） 3,Dc = 1.565 g/cm3,μ（MoKα） = 2.076 mm-1,F（000） = 1152,the final R = 0.0335 and wR = 0.0664 for 9416 observed reflections（I 2σ（I））.Cluster 2 belongs to the monoclinic system,space group P21/c with a = 13.673（3）,b = 13.342（3）,c = 16.296（4） ,β = 104.385（5）o,Z = 4,V = 2879.7（10） 3,Dc = 1.347 g/cm3,μ（MoKα） = 1.751 mm-1,F（000） = 1176,the final R = 0.0306 and wR = 0.0706 for 6390 observed reflections（I 2σ（I））.The crystal structures of the clusters consist of cen-trosymmetric [RCOOSnnBu2OSnnBu2OH）]2 molecules with an almost planar Sn4O4 framework.Each pair of exo-and endo-cyclic tin atoms was linked by one bridge-OH only.In addition,a novel structure of nBu2SnO different from the previous reports was proposed on the basis of 1H-NMR,TG analysis and X-ray diffraction.

关 键 词：dibutyltin oxide Sn-O cluster X-ray diffraction 

分 类 号：O614.432[理学—无机化学]