301-04-2Relevant articles and documents
Studies on the synthesis of Pb-Ti-oxo-alkoxo-carboxylato complexes
Spiccia,West,Zhang
, p. 1851 - 1861 (1998)
Reactions between lead carboxylates Pb(O2CR)2 and Ti(OPr-i)4 produce complexes of empirical formulae Pb2Ti2(O)(O2CR)2(OPr i)8 (R = C3F7 1 ; C(CH3)3 2) in toluene and Pb2Ti4(O)2(O2CR) 2(OPri)14 (R = CH(CH3)2 3) in PriOH solution. 201Pb NMR evidence indicates that both types of complex form in alcoholic solution. The compound 4 having a Pb3Ti3 core is produced when Pb(O2CCH(CH3)2)2 reacts with Ti (OPri) 4 in toluene. Attempts to prepare acetylacetonate derivatives of compounds having 1:1 or 1:2 Pb : Ti stoichiometries by direct substitution of the compounds gave poorly soluble Pb containing products but direct reaction of Pb(O2CCH3)2 or PbO with Ti-acetylacetonate-alkoxide species gave compounds of empirical formulae Pb3Ti3(O)4(O2CCH3) 2(OPri)7(acac) 5 and Pb2Ti2(O)(OEt)8(acac)2 6. Reaction of Ti(OR)4 (R = OPri, Et) with acetic acid yields products which further react with PbO to form the previously characterised Pb - Ti compounds Pb2Ti2(O)(O2CCH3) 2(OPri)8 7 and Pb2Ti4(O)2(O2CCH3) 2(OEt),14 8. Molecular weight measurements, 207Pb, 19F, 1H and 13C NMR and IR spectral data have been used to derive empirical formulae for the various complexes isolated.
Synthesis and characterization of the heterometallic aggregate Pb2Al5(μ3-O)(μ4-O)(μ-OiPr)9(OiPr)3(μ-OAc)3
Pandey, Ashutosh,Gupta, Vishnu D.,N?th, Heinrich
, p. 1291 - 1293 (1999)
A novel heterometallic aggregate Pb2Al5(μ3-O)(μ4-O)(μ- OiPr)9(OiPr)3(μ-OAc)3 obtained from the interaction of Pb(OAc)2 and Al(O-iPr)3 is the first structurally characterized example based on lead and aluminum. This compound has been isolated in high yield and examined by 1H-, 13C-, and 27Al NMR, and in the solid state by X-ray crystallography.
Syntheses of needle-shaped layered perovskite (C6H5CH2NH3)2PbI4bundles via a two-step processing technique
Ma, Dewei,He, Yidan
, p. 1213 - 1219 (2017)
Similar to the three-dimensional perovskites, two-dimensional (2D) layered lead halide perovskites constitute a particular class of semiconductor materials in the family of perovskites. This article reports syntheses of needle-like bundles of 2D perovskite (C6H5CH2NH3)2PbI4by a two-step processing technique. The concentration of C6H5CH2NH3I precursor has a great influence on the product, structural and compositional analyses prove the phase and stoichiometry of 2D perovskite (C6H5CH2NH3)2PbI4with high crystallinity for the needle bundles synthesized with concentration of C6H5CH2NH3I higher than 25 mg/mL. Intensive studies on the growth mechanism of the products were carried out; we believe the involvement of C6H5CH2NH3+group determines the layered structure and the final morphology of the products. Photoluminescence measurement show that the needles possess a band-edge emission peak centering around 540 nm and a narrow full width at half maximum of about 30 nm.
Structural investigations of a lead(IV) tetraacetate-pyridine complex
Buston, Jonathan E. H.,Claridge, Tim D. W.,Heyes, Stephen J.,Leech, Michael A.,Moloney, Mark G.,Prout, Keith,Stevenson, Maya
, p. 3195 - 3203 (2005)
A 1 : 1 crystalline complex of lead(IV) tetraacetate and pyridine (LTA-py) has been prepared. The single-crystal X-ray structure, at 296 and 150 K, establishes the presence of a relatively short Pb-N bond (2.307 A) within an intriguing seven-coordinate lead inner sphere consisting of the pyridine ligand and two bidentate and two monodentate acetate ligands. The pyridine occupies a surprising amount of the available coordination space and has induced a dramatic change in coordination compared to the four chelating acetate ligands found in lead tetraacetate (LTA). Thermal measurements (TGA/DSC) indicate the de-coordination of pyridine and its loss from the solid between 360 and 380 K. 207Pb CP/MAS NMR spectroscopy also demonstrates the existence of the Pb-N bond through observation of 1( 207Pb,14N) = 63 Hz and a 207Pb-14N dipolar coupling constant, of 149 Hz. The solid-state 207Pb NMR parameters are used to give insight into the coordination environment of Pb(IV) in LTA-py. In solution, ligand exchange is rapid on chemical shift and J-coupling time scales. A 207Pb NMR study of the titration of an LTA solution by pyridine yields a stability constant for LTA-py of K = 1.5 M -1 and predicts it to have a 207Pb NMR chemical shift essentially identical to that observed by CP/MAS NMR in the solid state. This correlation between the solid state and solution indicates that the seven-coordinate LTA-py structure found in the crystalline state does persist in solution, and this could further explain why the addition of pyridine has such profound effects on lead(IV) carboxylate-mediated organic reactions. Simulations of exchange-broadened line shapes of 13C CP/MAS NMR spectra in the temperature regime above 280 K indicate local motion of the pyridine rings in the form of 180° jumps (activation energy 72.5 kJ mol-1); these are first such ring flips reported for a coordinated pyridine ligand. The Royal Society of Chemistry 2005.
Solid- and solution-state structural transformations in flexible lead(ii) supramolecular polymers
Akhbari, Kamran,Morsali, Ali
, p. 8915 - 8918 (2013/11/19)
Reversible solid-state structural transformations of [Pb 2(Q-2-c)2(OAc)2(MeOH)2]n (1) and [Pb2(Q-2-c)2(OAc)2(EtOH) 2]n (2) to [Pb2(Q-2
Synthesis, structure, and properties of solid solutions based on bismuth ferrite
Korchagina,Ivanov,Proidakova, V. Yu.,Rush,Rybakova,Sadovskaya
, p. 568 - 573 (2009/09/24)
Solid solutions of Bi1 - x Pb x Fe1 - x Zr x O3 (x = 0.1-0.2) are synthesized by the methods of liquid-phase and modified solid-phase synthesis. Also, solid solutions of [Bi0.9(Pb0.9/
Precursors for mixed metal oxide nanoparticles: Synthesis and characterization of μ-oxoalkoxides of some bivalent metals and their β-diketonates
Sharma, Malti,Bhagi, Ajay K.,Sharma, Harish K.,Priti, Ritu Kansal,Kumar, Ram,Kapoor, Pramesh N.
, p. 256 - 260 (2007/10/03)
New heterobimetallic derivatives of the type M{OAl(OPri) 2}2 (M = Sn, Pb, Cd) have been prepared by the reactions of M(OAc)2 with Al(OPri)3 in 1:2 molar ratio in hydrocarbon solvent (xylene/toluene) with the continuous liberation of isopropyl acetate. Furthermore, reactions of M{OAl(OPri) 2}2 (M = Ca, Pb, Cd) with β-diketones (acetylacetone, benzoyl acetone) have also been carried out to obtain modified derivatives. These new derivatives have been characterized by elemental analyses and spectroscopic [IR, NMR (1H, 13C, 27Al and 119Sn)] studies.
Carbonylation of o-phenylenediamine and o-aminophenol with dimethyl carbonate using lead compounds as catalysts
Fu, Yue,Baba, Toshihide,Ono, Yoshio
, p. 91 - 97 (2007/10/03)
Lead compounds are active catalysts for carbonylation and carbonylation/methylation of o-phenylenediamine and o-aminophenol with dimethyl carbonate (DMC). 2-Benzimidazolone was obtained in 84% yield by the reaction of o-phenylenediamine with DMC for 1 h at 443 K in the presence of Pb(NO3)2. In the presence of Pb(OAc)2, the reaction quantitatively gave 1,3-dimethyl-2-benzimidazolone, which was formed by methylation of the primary product, 2-benzimidazolone, at 473 K. The effects of reaction variables on the yields of 2-benzimidazolone and 1,3-dimethyl-2-benzimidazolone were examined. The reaction of o-aminophenol with DMC selectively gave a carbonylation product, 2-benzoxazolone, or a carbonylation/methylation product, 3-methyl-2-benzoxazolone, depending on the reaction conditions in the presence of Pb(OAc)2.
Preparation of Bi-based high-Tc superconducting films from methacrylate solutions
Men'shikh,Geras'kina,Prutchenko,Rybakova,Tomashpol'skii
, p. 517 - 520 (2008/10/08)
Bi2Sr2CaCu2Ox superconducting films containing minor amounts of Bi2Sr2Ca2Cu3Ox were prepared by spray pyrolysis of methacrylate solutions on LaAlO3 substrates. The best superconducting properties (Tc ? 80 K, ΔTc ? 10 K) were shown by the films annealed at 850°C, which consisted mainly of platelike crystallites with a high degree of [001] orientation. The composition, content, and morphology of the calcium strontium cuprates and oxides present as impurity phases were found to correlate with the annealing temperature and film thickness.
PZT ferroelectric films obtained from metal alkoxides by sol-gel processing
Solov'eva,Obvintseva,Yanovskaya,Vorotilov,Vasil'ev
, p. 767 - 774 (2008/10/08)
Reaction of Pb(CH3COO)2 · 3H2O with acetic anhydride was shown to be the most convenient method for mild dehydration of this compound, which makes it possible to avoid decomposition of lead acetate and to stabilize precursor solutions in sol-gel technology. Anodic dissolution of titanium and zirconium in methylcellosolve substantially simplifies preparation of precursor solutions. X-ray diffraction analysis, scanning elecrton microscopy, and electrical measurements show that the introduction of 10 mol % excess Pb into the precursor solution ensures compensation for PbO evaporation during high-temperature firing.
