Compound 2

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Compound data: CIF

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

The solution of 2 was prepared as described for [(L^Ar)NpCl], 1, (Method A), using an equimolar mixture of ²³⁷NpCl₄ (58.0 mg, 0.153 mmol) and [K₂(L^Ar)] (80.6 mg, 0.153 mmol) in 4 mL of THF. The red supernatant was isolated by syringe filtration (PTFE membrane, 0.45μm porosity) and subsequently concentrated to 2.1 mL under reduced pressure. Layering of aliquots of this solution in silylated NMR tubes with hexane afforded 2 in the form of very dark red crystals, suitable for single crystal X-ray diffraction analysis, and an off-white precipitate of organic by‑products (<0.1 mg ²³⁷Np radioassay). The clustered nature of crystal-growth of 2 enabled mechanical separation from the organic material. Washing with n-pentane (3 × 1 mL) and rapid drying under a stream of argon gave pure 2; isolated yield: 92.6 mg, 91.9 %. The low solubility of 2 in THF precludes solution-state studies. ATR-IR: ν = 3106 w, 3069 w, 2965 w/m, 2928 w, 2868 w, 1599 w, 1579 w, 1484 w, 1462 w, 1413 w/m, 1381 w, 1359 w/m, 1307 w/m, 1238 s, 1209 m, 1180 m, 1131m br, 1094 m, 1043 m, 981 m/s, 938 w/m, 915 w/m, 817 m, 795 m, 763 m/s, 747 m/s, 706 s, 666 m, 647 w/m, 615 m, 482 m/s, 463 m/s, 427 m/s, 406 m/s cm^-1. Radiological regulations prohibit combustion-based analysis of the C, H and N content of 2.