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Synthetic Reactivity of Cupro-selenometallic Clusters

Author: YuZhan
Tutor: ZhangQianFeng
School: Anhui University of
Course: Applied Chemistry
Keywords: heteroselenometallic cluster cupro-selenometallic cluster synthetic reactivity
CLC: O611.3
Type: Master's thesis
Year: 2007
Downloads: 17
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Abstract


Seven cupro-selenometallic cluster compounds with four types of structural modes have been synthesized in this thesis. The solid-state structures of these compounds have been established by X-ray crystallography. The seven cluster compounds have also been characterized by the infrared, electronic, 1H and （31）P{1H} NMR and FAB mass spectroscopies. The nonlinear optical properties of several cluster compounds with new structural types have been tested by using the z-scan technique. Treatment of [Et4N]2[WSe4] with trinuclear trigonal-bipyramid copper （I） complexes [Cu3（μ3-X）2（μ-dppx）3]X [X = I, x = m, dppm = bis（diphenylphosphino）methane; X = Cl, x = a, dppa = bis（diphenyl- phosphino）amine] afforded the tetranuclear cluster compounds [（μ3-WSe4）Cu3（μ-X）（μ- dppx）2] （X = I, x = m, 1; X = Cl, x = a, 2） which exhibit an open butterfly configuration, the formation of 1 and 2 involved the metathetical reaction of [Et4N]2[WSe4] with [Cu3（μ3-X）2（μ-dppx）3]X. Interaction of [Et4N]2[WSe4] with [Cu（MeCN）4][PF6] in the presence of dppm or dppa gave the pentanuclear cluster compounds [（μ4-WSe4）Cu4（μ- dppx）4][PF6]2 （x = m, 3; a, 4） which contain an open co-planar WCu4 core. In this reaction, dppm or dppa acted as a bridging ligand for the construction of [Cu2（dppx）]2+ species obtained from the 1 : 1 mixture of [Cu（MeCN）4]+ and dppx, subsequently, [Cu2（dppx）]2+ reacted with [WSe4]2- to give cluster compounds 3 and 4, respectively. Two isostructural crown-like heteroselenometallic cluster compounds [Et4N]4[（μ5-WSe4）（CuX）5（μ-X）2] （X = Cl, 5; Br, 6） were prepared from the reactions of [Et4N]2[WSe4] with CuX and [Et4N]X·xH2O in the presence of 2-picoline which acted as a co-solvent instead of ligand and increased the solubility of the reactants and products. It is believed that this reaction is due to the relatively low solubility of CuCl and CuBr. Treatment of [Cu3（μ3-X）2（μ- dppa）3][CuCl2] with （Me3Si）2Se in the tetrahydrofuran （THF） afforded aμ8-selenide- centered octanuclear copper （I） complex [Cu8（μ8-Se）（μ4-Se）（μ4-SeH）3（μ-dppa）4]- [（Ph2PO）2N] （7）, （Me3Si）2Se is the selenium source and SiMe3Cl derived from （Me3Si）2Se is a driving force in the reaction.

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