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• W2475796252 startingPage "949" @default.
• W2475796252 abstract "Reaction of ThBr4(THF)4 with 2 equiv of KOAr (Ar = 2,6-t-Bu2C6H3) produces the bis(aryloxide) complex ThBr2(OAr)2(THF)2 (1) in 67% yield. Alkylation of 1 with 2 equiv of Me3SiCH2MgCl allows the isolation of Th(OAr)2(CH2SiMe3)2 (2) in 61% yield. Thermolysis of 2 (benzene, 60 °C, 36 h) in the presence of NEt3 results in the formation of the cyclometalated ligand redistribution product Th(OC6H3-t-BuCMe2CH2)(OAr)2 (3). Reaction of 2 with 1 equiv of 2,6-dimethylphenyl isocyanate leads to insertion into the Th−C bond to yield (ArO)2Th[OC(NR)CH2SiMe3](CH2SiMe3) (4; R = 2,6-Me2C6H3). Aminolysis of 2 with 2 equiv of 2,6-diisopropylaniline allows the isolation of the bis(amido) species Th(OAr)2(NH-2,6-i-Pr2C6H3)2 (5) in 92% yield. 2 reacts with dihydrogen (1.5 atm) over a period of 7 days to form the trimeric dihydride complex Th3(μ3-H)2(μ2-H)4(OAr)6 (6). In the presence of 1 equiv of [HNMe2Ph][B(C6F5)4], 2 catalyzes the hydrogenation of 1-hexene (Nt = 1 h-1), while 6 is found to be a single-component catalyst for the analogous process (Nt = 3 h-1). Complexes 1−6 have been characterized by 1H NMR and IR spectroscopy, microanalysis, and, in the case of 2 and 6, by single-crystal X-ray diffraction studies. 2 comprises a pseudotetrahedral thorium metal center bearing two aryloxide and two alkyl ligands. The O−Th−O angle between the aryloxide ligands (119.2(4)°) is significantly larger than the C−Th−C angle (101.4(6)°). Th−O and Th−C distances average 2.137(11) and 2.462(18) Å, respectively, while Th−C−Si angles are 125.9(8) and 122.8(8)°. The alkyl groups of 2 also display a reduced C−H coupling constant (JCH = 98 Hz), suggestive of α-agostic interaction between the methylene group and the Th metal center. 6 exhibits a triangular arrangement of three thorium metal centers, each bearing two terminal aryloxide ligands. Two sides of the trimetallic core (Th−Th distances 3.781(1) and 3.818(1) Å) are bridged by single μ2-hydride ligands, while the third side is bridged by two μ2-hydride ligands (Th−Th distance 3.588(1) Å). Each face of the trimer is capped by a μ3-hydride ligand to produce a structurally unique M3(μ3-X)2(μ2-X)4X6 geometry. Th−(μ2-H) and Th−(μ3-H) distances lie in the ranges 2.0(1)−2.3(1) and 2.3(1)−2.6(1) Å, respectively, while Th−O distances range from 2.126(7) to 2.164(7) Å." @default.
• W2475796252 created "2016-08-23" @default.
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• W2475796252 creator A5033721117 @default.
• W2475796252 creator A5041147389 @default.
• W2475796252 creator A5084718930 @default.
• W2475796252 date "1996-02-06" @default.
• W2475796252 modified "2023-09-25" @default.
• W2475796252 title "Sterically Demanding Aryloxides as Supporting Ligands in Organoactinide Chemistry. Synthesis, Structural Characterization, and Reactivity of Th(O-2,6-<i>t</i>-Bu₂C₆H₃)₂(CH₂SiMe₃)₂ and Formation of the Trimeric Thorium Hydride Th₃H₆(O-2,6-<i>t</i>-Bu₂C₆H₃)₆" @default.
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• W2475796252 doi "https://doi.org/10.1021/om950654u" @default.
• W2475796252 hasPublicationYear "1996" @default.
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