Compound 3a

[Mo(CO)2(2,6-bis(di-tert-butylphosphinomethyl)pyridine)]2(μ-N2)

From: A molybdenum complex bearing PNP-type pincer ligands leads to the catalytic reduction of dinitrogen into ammonia

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InChIKey PLOANHSTARATAH-UHFFFAOYSA-N

Compound data: CIF

Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.

A solution of 2a (55.7 mg. 0.050 mmol) in THF (5 mL) was stirred at room temperature for 12 h under CO atmosphere. The resultant dark blue solution was concentrated in vacuo. The residue was extracted with THF (5 mL) and concentrated in vacuo to about 3 mL. Slow addition of hexane (20 mL) to the obtained solution afforded 3a·C6H14 as purple crystals, which were collected by filtration and dried in vacuo to afford 3a (35.6 mg, 0.032 mmol, 64% yield). 1H NMR (THF-d8) δ 7.37 (br s, ArH, 2H), 6.64 (br s, ArH, 1H), 3.68 (br s, CH2PtBu2, 4H), 1.35 (br s, CH2PtBu2, 36H). 31P{1H} NMR (THF-d8) δ 103.1 (s). IR (KBr, cm−1) 1833 (s, νCO), 1801 (s, νCO), 1780 (br, νCO). Raman (THF, cm−1; νexcite = 514.5 nm) 1893 (νNN). Anal Calcd for C50H86Mo2N4O4P4: C, 53.48; H, 7.72; N, 4.99. Found: C, 53.50; H, 8.00; N, 4.71.

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