Preparation of U[N(EPPh2)2]3 (E = S or Se) by treating U[N(SiMe3)2]3 with three equivalents of NH(EPPh2)2 is described together with presentation of a hitherto unreported molecular crystal structure containing An(III)-Se bonds (An = actinide).
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Homoleptic Acetylacetonate (acac) and β-Ketoiminate (acnac) Complexes of Uranium.
Inorg Chem
February 2023
Department of Chemistry and Pharmacy, Inorganic Chemistry, Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU), Egerlandstraße 1, Erlangen 91058, Germany.
Transmetalation of potassium salts of differently substituted acetylacetonate (acac) and β-ketoiminate (acnac) with [U(I)(dioxane)] and [U(I)(dioxane)] resulted in the formation of homoleptic, octahedral complexes [U(acnac)] (with acnac = 2,2,6,6-tetramethyl-5-(phenylimino)heptan-3-onate) in the oxidation states +III and +IV and the homoleptic, square prismatic complexes [U(acnac)] (with acnac = 4-(phenylimino)pentan-2-onate) and the homoleptic, square antiprismatic complexes [U(acac)] [with acac = 2,2,6,6-tetramethyl-3,5-heptanedionate (acac), 2,2,6,6-tetramethyl,4-methyl-3,5-heptanedionate (acac), and 2,2,6,6-tetramethyl-4-phenyl-3,5-heptanedionate (acac)] in oxidation states +III, +IV, and +V. Oxidation of [U(acnac)] () with AgOTf yielded [U(acnac)][OTf] (), which was fully characterized by single-crystal X-ray diffraction analysis, a combination of ultraviolet/visible/near-infrared, nuclear magnetic resonance, and infrared spectroscopies, and solid-state superconducting quantum interference device magnetization studies. Complexation of the sterically less encumbering ligand derivative acnac provided access to the tetravalent, square antiprismatic complex [U(acnac)] ().
View Article and Find Full Text PDFWerner-Type Complexes of Uranium(III) and (IV).
Inorg Chem
February 2020
Inorganic Chemistry, Department of Chemistry and Pharmacy , Friedrich-Alexander-University Erlangen-Nürnberg (FAU), Erlangen 91058 , Germany.
Transmetalation of the β-diketiminate salt [M][nacnac] (M = Na or K; nacnac = {PhNC(CH)}CH) with UI(THF) resulted in the formation of the homoleptic, octahedral complex [U(nacnac)] (). Green colored was fully characterized by a solid-state X-ray diffraction analysis and a combination of UV/vis/NIR, NMR, and EPR spectroscopic studies as well as solid-state SQUID magnetization studies and density functional theory calculations. Electrochemical studies of revealed this species to possess two anodic waves for the U(III/IV) and U(IV/V) redox couples, with the former being chemically accessible.
View Article and Find Full Text PDFUranium(iii) complexes supported by hydrobis(mercaptoimidazolyl)borates: synthesis and oxidation chemistry.
Dalton Trans
August 2018
Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, Estrada Nacional 10, 2695-066 Bobadela LRS, Portugal.
The reaction of [UI3(thf)4] with the sodium or lithium salts of hydrobis(2-mercapto-1-methylimidazolyl)borate ligands ([H(R)B(timMe)2]-) in a 1 : 2 ratio, in tetrahydrofuran, gave the U(iii) complexes [UI{κ3-H,S,S'-H(R)B(timMe)2}2(thf)2] (R = H (1), Ph (2)) in good yields. Crystals of [UI{κ3-H,S,S'-H(Ph)B(timMe)2}2(thf)2] (2) were obtained by recrystallization from a tetrahydrofuran/acetonitrile solution, and the ion-separated uranium complex [U{κ3-H,S,S'-H(Ph)B(timMe)2}2(CH3CN)3][I] (3-I) was obtained by dissolution of 2 in acetonitrile followed by recrystallization. One-electron oxidation of 2 with AgBPh4 or I2 resulted in the formation of the cationic U(iv) complexes [U{κ3-H,S,S'-H(Ph)B(timMe)2}3][X] (X = BPh4 (6-BPh4), I (6-I)), due to a ligand redistribution process.
View Article and Find Full Text PDFA Homoleptic Uranium(III) Tris(aryl) Complex.
J Am Chem Soc
December 2016
Department of Chemistry, University of California, Berkeley , and Chemical Sciences Division, Lawrence Berkeley Laboratory, Berkeley, California 94720, United States.
The reaction of 3 equiv of Li-CH-2,6-(CH-4-Bu) (Terph-Li) with UI(1,4-dioxane) led to the formation of the homoleptic uranium(III) tris(aryl) complex (Terph)U (1). The U-C bonds are reactive: treatment with excess PrN═C═NPr yielded the double-insertion product [TerphC(NPr)]U(Terph) (2). Complexes 1 and 2 were characterized by X-ray crystallography, which showed that the U-C bond length in 2 (2.
View Article and Find Full Text PDFSingle-molecule-magnet behavior in mononuclear homoleptic tetrahedral uranium(III) complexes.
Inorg Chem
November 2014
C2TN, Instituto Superior Técnico, Universidade de Lisboa/CFMCUL , Estrada Nacional 10, 2695-066 Bobadela LRS, Portugal.
The magnetic properties of the two uranium coordination compounds, [K(18c6)][U(OSi(O(t)Bu)3)4] and [K(18c6)][U(N(SiMe3)2)4], both presenting the U(III) ion in similar pseudotetrahedral coordination environments but with different O- or N-donor ligands, have been measured. The static magnetic susceptibility measurements and density functional theory studies suggest the presence of different ligand fields in the two compounds. Alternating-current susceptibility studies conducted at frequencies ranging from 95 to 9995 Hz and at temperatures in the 1.
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