Synthesis of 1,2-bis(di-tert-butylphosphino)ethane (dtbpe) complexes of nickel: radical coupling and reduction reactions promoted by the nickel(I) dimer [(dtbpe)NiCl]2

Add time:08/16/2019    Source:sciencedirect.com

Tetrahydrofuran solutions of (dtbpe)NiCl2 (dtbpe=1,2-Bis(di-tert-butylphosphino)ethane (cas 107783-62-0)) are reduced by KC8 to afford the dimeric Ni(I) complex [(dtbpe)NiCl]2 (1) in 73% yield. Reaction of 1 with [FeCp2][PF6] effects a one-electron oxidation to give the mixed-valent Ni(I,II) binuclear species [{(dtbpe)NiCl}2][PF6], [1][PF6]. Complex 1 reacts with the radicals NO and TEMPO (2,2,6,6-tetramethyl-1-piperidine-N-oxyl) to give the diamagnetic Ni(0) nitrosyl (dtbpe)Ni(Cl)(NO) (2) and the Ni(II) complex (dtbpe)Ni(Cl)(O,N:η2-TEMPO) (3). Reduction of the SS bond of diphenyldisulfide by 1 results in formation of the Ni(II) arylthiolate complex (dtbpe)NiCl(SPh) (4). The radical anions NaOCPh2 and KN2Ph2 react cleanly with 1 to afford (dtbpe)Ni(η2-OCPh2) (5) and (dtbpe)Ni(η2-N2Ph2) (6). Phenylacetylide CC bond coupling is effected by reaction of 1 with LiCCPh to form [(dtbpe)Ni(C,C′:η2-CCPh)]2 (7). In addition to standard spectroscopic (IR, NMR, EPR) and magnetic measurements, complexes 1, [1][PF6], 3, and 5 were also characterized by single-crystal X-ray diffraction methods.

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