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Kogut E Zeller A Warren TH Strassner T 《Journal of the American Chemical Society》2004,126(38):11984-11994
Addition of BF(3).OEt(2) to ethereal solutions of the Ni(II) beta-diketiminates [Me(2)NN]Ni(R)(2,4-lutidine) (R = Et (1), Pr (2)) allows the isolation of the neutral beta-H agostic monoalkyls [Me(2)NN]Ni(R) (R = Et (3), Pr (4)). X-ray studies of primary alkyls 3 and 4a reveal acute Ni-C(alpha)-C(beta) angles with short Ni-C(beta) distances, indicating structures along the beta-H elimination pathway. Positional disorder of the alkyl group in the X-ray structure of 4 corresponds to partial (22%) occupancy by the secondary alkyl [Me(2)NN]Ni(CHMe(2)) (4b). Variable-temperature NMR spectra of 3 and 4 reveal fluxional behavior that result from beta-H elimination, in-plane rotation of the beta-CH(3) group, and a tetrahedral triplet structure for 3 that were investigated by density functional theory calculations at the Becke3LYP/6-31G level of theory without simplifications on the beta-diketiminate ancillary ligand. Calculations support low temperature NMR studies that identify the linear beta-H agostic propyl isomer 4a as the ground state with the branched beta-H agostic isomer 4b slightly higher in energy. NMR studies and calculations show that the beta-agostic 3 reluctantly coordinates ethene and that 3 is the ground state for this ethylene oligomerization catalyst. The thermodynamic isotope effect K(H)/K(D) = 1.3(2) measured for the loss of 2,4-lutidine from 1 to form beta-agostic 3 was also examined by DFT calculations. 相似文献
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Kogut E Wiencko HL Zhang L Cordeau DE Warren TH 《Journal of the American Chemical Society》2005,127(32):11248-11249
The synthesis and structure of the beta-diketiminato Ni(I) lutidine adducts [MexNN]Ni(2,4-lutidine) (x = 2 (2); x = 3 (3)) are described which serve as synthons to the "naked" 13-electron [MexNN]Ni fragments in reactions with N3Ad to give Ni-imido complexes. The singly bridged imide {[Me2NN]Ni}2(mu-NAd) (4) possesses short Ni-Ni (2.506(1) A) and Ni-N(imido) distances (1.732(4)-1.752(4) A). Steric modification of the beta-diketiminate ligand to include an additional methyl group in the N-aryl 4-position affords the Ni(III) terminal imide [Me3NN]Ni=NAd (8) isolated in 52% yield. The X-ray structure of terminal imide 8 reveals a contracted Ni-N(imido) bond distance (1.662(2) A) and an only somewhat bent imido linkage (Ni-N-C = 164.5(2) degrees ) consistent with a significant degree of multiple bond character. Frozen glass EPR studies of 5 indicate a rhombic environment in which one of the signals exhibits strong hyperfine coupling (A = 22 G) to the imido 14N (I = 1) nucleus. The terminal imide 5 undergoes complete imido group transfer to CO and CNBut to give AdNCO and AdNCNBut, respectively, as well as with PMe3 to afford AdN=PMe3. Exemplifying the radical character at the imido N atom, 5 adds to cobaltocene and abstracts a H atom from 1,4-cyclohexadiene to give the Ni(II)-amides [Me3NN]Ni-NAd(eta4-C5H5)CoCp (7) and [Me3NN]Ni-NHAd (8). 相似文献