Compound 2
[(iPr3P)Ni]5(μ2-H)4(μ5-C)
From: Cooperative carbon-atom abstraction from alkenes in the core of a pentanuclear nickel cluster
| 1H NMR | 31P{1H} NMR | 13C{1H} NMR | ChemDraw
Compound data: CIF
Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.
A stirring solution of [(iPr3P)Ni]5H6 (550 mg, 0.50 mmol) in 100 mL of n-pentane, was exposed to 2 equivalents of ethylene (0.0246 L, 1 mmol) through a Schlenk line. The solution was stirred for 0.25 hours. The dark brown solution was then evacuated and filtered through a plug of Celite and was concentrated until the precipitation of product was observed. The solution was left at −40 ˚C for 40 hours, which afforded dark brown plates suitable for X-ray diffraction. A second crop also afforded crystals and a combined yield of 281 mg (46.5 %) was obtained. 1H NMR (298 K, C6D6, 500 MHz): δ −7.17 (sextet, 2JPH=2.45 Hz, 4 H, Ni-H), 1.40 (dd, 3JHH= 7.1 Hz, 3JPH= 12.4 Hz, 90 H, P(CH(CH3)2)3), 2.21 (septet of d/apparent octet, 3JHH=7.2 Hz, 2JPH= 7.6 Hz, 15 H, P(CH(CH3)2)3. 31P{1H} NMR (298 K, C6D6, 202.5 MHz): δ 52.4 (s, 5P, P(CH(CH3)2) 13C{1H} NMR (298 K, C6D6, 125.7 MHz): δ 20.7 (s, 30 C, P(CH(CH3)2)), 24.1 (d, 1JPC=12.1 Hz, 15 C, P(CH(CH3)2) Anal Calcd. for C46H109Ni5P5: %C 49.74; %H 9.89. Found %C 49.96; %H 10.21.
