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Syntheses And Characterizations Of Polynuclear Lead(Ⅱ)-Sulfur Cluster Compounds

Posted on:2014-05-27Degree:MasterType:Thesis
Country:ChinaCandidate:F HuFull Text:PDF
GTID:2181330434952276Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Polynuclear Lead(II)-Sulfur compounds have been synthesized and structurallycharacterized in this thesis. Reaction of Pb(SR)2(R=iPr,tBu,PhMe-p) with AgX(Cl,Br,I) in polar solvents gave five coordination polymers {[Pb2(S-iPr)3]Cl}n(1),{[Pb2(S-iPr)3]Br}n(2),[Pb2I(S-iPr)3]n(3),[Pb2I2(S-iPr)2]n(4) and [Pb2Cl(SPhMe-p)3]n(5). Interaction of Pb(S-iPr)2with AgX in ratio of1:0.5resulted in the formation oftwo dimensional polymers1-3. Chlorine and Bromine in the covalent skeletonstructure of1and2as ions. Pb-I was involved in the formation of covalent skeletonstructure of3as covalent bond. Treatment3with0.5equivalents of the AgI affordedone-dimensional chain polymer4. Especially, Reaction of Pb(SPhMe-p)2with0.5equivalents of AgCl afforded not two dimensional polymer, one-dimensional polymerchain5isolated instead.On the basis of the study of the reaction of Pb(SR)2with AgX, supernumeraryfour multi-lead sulfide clusters have been synthesized. During the reaction, Pb(S-iPr)2have been lost-S-iPr and the original covalent polymeric structure has been destroyed,while the solution in the presence of O2-afforded Clusters [Pb13(S-iPr)6O8][NO3]46and [Pb14(S-iPr)16O6]n7. Treatment of Pb(S-tBu)2with Cu(PPh3)2NO3in equalequivalent, giving ternary heterobimetallic complex Pb(S-tBu)3Cu(PPh3)8which ledto a dimer through weak interactions of Intermolecular. Reaction of [Pb(SPhMe-p)2]with [Ag(PPh3)2NO3] in a ratio of1:2, affording a two-dimensional bimetallicpolymer [PbAg2(SPhMe-p)4]n9. All complexes have been comfirmed bysingle-crystal X-ray diffraction.
Keywords/Search Tags:Lead(II) thiolate compound, Coordination polymer, cluster compound, Heterometallic complexe, Molecularstructure
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