Compound 3a
(κ1-N,κ1-N',η6,η6-trans-calix[2]benzene[2]pyrrolyl)(dimethoxyethylether)neptunium(II)
Synthetic procedure: See article for the definitive version of this procedure and for full experimental details.
A 25-mL Schlenk tube was charged with [(LAr)NpCl], 1, (43.2 mg, 0.060 mmol) and 8 mL of dme. An excess of NaK3 alloy (0.24 mL, eutectic) was added and the suspension was orbital shaken (2800 rpm) for 20 s. During this time the reddish solid was consumed and the colour of the solution changed to brown and later to intense purple black. The excess of the NaK alloy and any particulate matter were removed by syringe filtration (silylated glass fibre membrane in PE housing, 1.0 μm porosity) and the solution of [(LAr)Np(dme)] (3a) analysed for direct Vis-nIR measurements (340 μL load into 1.00 mm cell) and crystallization studies (7.4 mL).
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313063383
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