3124-29-6Relevant academic research and scientific papers
Synthesis and characterization of lead (IV) precursors and their conversion to PZT materials through a CVD process
Kim, Euk Hyun,Moon, Cheong Won,Lee, Jung Gyu,Lah, Myoung Soo,Koo, Sang Man
, (2020)
New Pb(IV) precursors for lead zirconate titanate (PZT) thin films were synthesized, and their solid-state structures were elucidated by single-crystal X-ray crystallography. First, tetraphenyl lead (Ph4Pb) was synthesized from the reaction of PbCl2 with the Grignard reagent, PhMgBr, by a published method. Two of the phenyl ligands in Ph4Pb were replaced by bromines, and then were substituted with bis(trimethylsilyl)amides (btsa) to yield Ph2Pb(btsa)2 (1), or with 2,2,6,6-tetramethyl-3,5-heptadiketonate (thd) ligands to yield Ph2Pb(thd)2 (2). Single crystals of these two new Pb(IV) precursors were obtained by recrystallization in hexane, and their chemical compositions were characterized by FT-IR and 1H NMR. In TG analyses, both compounds exhibited sharp decomposition curves, with major mass losses in the region of 200–250 °C. PZT films were fabricated from one of the newly prepared Pb(IV) precursors by an MOCVD process involving Ti(OiPr)4 and Zr(OPr)4, and the development of the perovskite phase with temperature was monitored by an XRD method.
Tuning the sulfur-heterometal interaction in organolead(IV) complexes of [Pt2(μ-S)2(PPh3)4]
Pham, Kristina,Henderson, William,Nicholson, Brian K.,Hor, T.S. Andy
, p. 4933 - 4942 (2008/03/13)
Reactions of [Pt2(μ-S)2(PPh3)4] with Ph3PbCl, Ph2PbI2, Ph2PbBr2 and Me3PbOAc result in the formation of bright yellow to orange solutions containing the cations [Pt2(μ-S)2(PPh3)4PbR3]+ (R3 = Ph3, Ph2I, Ph2Br, Me3) isolated as PF6- or BPh4- salts. In the case of the Me3Pb and Et3Pb systems, a prolonged reaction time results in formation of the alkylated species [Pt2(μ-S)(μ-SR)(PPh3)4]+ (R = Me, Et). X-ray structure determinations on [Pt2(μ-S)2(PPh3)4PbMe3]PF6 and [Pt2(μ-S)2(PPh3)4PbPh2I]PF6 have been carried out, revealing different coordination modes. In the Me3Pb complex, the (four-coordinate) lead atom binds to a single sulfur atom, while in the Ph2PbI adduct coordination of both sulfurs results in a five-coordinate lead centre. These differences are related to the electron density on the lead centre, and indicate that the interaction of the heterometal centre with the {Pt2S2} metalloligand core can be tuned by variation of the heteroatom substituents. The species [Pt2(μ-S)2(PPh3)4PbR3]+ display differing fragmentation pathways in their ESI mass spectra, following initial loss of PPh3 in all cases; for R = Ph, loss of PbPh2 occurs, yielding [Pt2(μ-S)2(PPh3)3Ph]+, while for R = Me, reductive elimination of ethane gives [Pt2(μ-S)2(PPh3)3PbMe]+, which is followed by loss of CH4.
