Bis(1,5-cyclooctadiene)nickel(0)

Wender, Paul A.; Smith, Thomas E.

doi:10.1002/047084289x.rb118

Cited by 1 publication

(2 citation statements)

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“…Last, the identity of the yellow compound could be verified using solution NMR. The 1 H NMR chemical shifts [ 1 H NMR: δ 4.28 (br, CH), 2.05 (br, CH 2 )] are consistent with the literature, 34 as is the 61 Ni chemical shift (δ iso = 936.5 ppm compared to the literature value of 937 ppm 10 ). Solution 13 C NMR also indicates the presence of the compound, with the cyclooctadiene ligands observed [ 13 C NMR: δ 89.30 (CH), 30.49 (CH 2 )].…”

Section: ■ Introductionsupporting

confidence: 84%

“…Ni(PPh 3 ) 4 and Ni[P(OPh) 3 ] 4 were received as fine powders (red-brown and white, respectively). Two lots of Ni(cod) 2 received had different physical characteristics: the first consisted of olive-gray crystals and was not ground before use or studied in solution because of the mechanochemical sensitivity of the compound; the second consisted of fine yellow crystals consistent with the literature 34 and was ground before use and also characterized by solution NMR spectroscopy. Spectra were collected for stationary powder samples packed under an inert atmosphere in 7-mm-o.d.…”

Section: ■ Introductionmentioning

confidence: 99%

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Structural and Crystallographic Information from ⁶¹Ni Solid-State NMR Spectroscopy: Diamagnetic Nickel Compounds

Werhun

Bryce

2017

Inorg. Chem.

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Despite the significance of nickel compounds, NMR spectroscopy of the active nickel isotope Ni remains a largely unexplored field. While nickel(0) compounds have been studied byNi NMR in solution, solid-state experiments have been limited to Knight shift studies of nickel metal and nickel intermetallics. In conjunction with an NMR study of their ligands and Ni relativistic computations, the firstNi solid-state NMR (SSNMR) spectra of diamagnetic compounds are reported here. Specifically, bis(1,5-cyclooctadiene)nickel(0) [Ni(cod)], tetrakis(triphenylphosphite)nickel(0) [Ni[P(OPh)]], and tetrakis(triphenylphosphine)nickel(0) [Ni(PPh)] were studied. Ni SSNMR spectra of Ni(cod) were used to determine its isotropic chemical shift (δ = 965 ± 10 ppm), span (Ω = 1700 ± 50 ppm), skew (κ = -0.15 ± 0.05), quadrupolar coupling constant (C = 2.0 ± 0.3 MHz), quadrupolar asymmetry parameter (η = 0.5 ± 0.2), and the relative orientation of the chemical shift and electric field gradient tensors. A solution study of Ni(cod) in CD yielded a narrow Ni signal, and the temperature dependence of δ(Ni) was assessed (δ being 936.5 ppm at 295 K). The solution is proposed as a secondary chemical shift reference for Ni NMR in lieu of the extremely toxic Ni(CO) primary reference. For Ni[P(OPh)], Ni SSNMR was used to infer the presence of two distinct crystallographic sites and establish ranges for δ in the solid state, as well as an upper bound for C (3.5 MHz for both sites). For Ni(PPh), line shape fitting provided a δ value of 515 ± 10 ppm, Ω of 50 ± 50 ppm, κ of 0.5 ± 0.5, C of 0.05 ± 0.01 MHz, and η of 0.0 ± 0.2. The study of Ni(PPh), in particular, demonstrates the utility of Ni SSNMR given the lack of a previously reported crystal structure and transient nature of Ni(PPh) in solution.

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Section: ■ Introductionsupporting

confidence: 84%

Section: ■ Introductionmentioning

confidence: 99%

Structural and Crystallographic Information from ⁶¹Ni Solid-State NMR Spectroscopy: Diamagnetic Nickel Compounds

Werhun

Bryce

2017

Inorg. Chem.

View full text Add to dashboard Cite

show abstract

Bis(1,5-cyclooctadiene)nickel(0)

Cited by 1 publication

References 120 publications

Structural and Crystallographic Information from ⁶¹Ni Solid-State NMR Spectroscopy: Diamagnetic Nickel Compounds

Structural and Crystallographic Information from ⁶¹Ni Solid-State NMR Spectroscopy: Diamagnetic Nickel Compounds

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Bis(1,5-cyclooctadiene)nickel(0)

Cited by 1 publication

References 120 publications

Structural and Crystallographic Information from 61Ni Solid-State NMR Spectroscopy: Diamagnetic Nickel Compounds

Structural and Crystallographic Information from 61Ni Solid-State NMR Spectroscopy: Diamagnetic Nickel Compounds

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Structural and Crystallographic Information from ⁶¹Ni Solid-State NMR Spectroscopy: Diamagnetic Nickel Compounds

Structural and Crystallographic Information from ⁶¹Ni Solid-State NMR Spectroscopy: Diamagnetic Nickel Compounds