The reaction of magnesium and selenium in dry methanol has been reported to yield a reagent tentatively identified as bis(methoxymagnesium) diselenide. The dark red-brown solution obtained from this reaction yielded red crystals that crystallized in the monoclinic space group C2/c, a=17.391(4) Å, b=15.823(3) Å, c=21.626(4) Å, β=110.71(3)°, V=5566.5(19) Å3, Z=4, R=0.0350, wR2=0.0850 for 4930 reflections. X-ray crystallographic analysis of this reagent showed it to be dodecamethanol-tetramethoxy-di(μ4-hydroxy)tetra(μ3-methoxy)hexamagnesium hexaselenide, Mg6(μ4-OH)2(μ3-OCH3)4(OCH3)4(CH3OH)12]Se6·2CH3OH (1), not the bis(methoxymagnesium) diselenide as previously described. The structure of 1 is composed of six magnesium ions and six bridging oxygen-containing ligands in a face-sharing cubic arrangement.
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We thank the NSF for research grant CHE-0545138 and for grant CHE-9808165 (CRIF) to support the X-ray diffractometer.
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Additional data of the X-ray structure reported in this paper have been deposited with the Cambridge Crystallographic Data Centre as supplementary publications, CCDC number 615359. Copies of the data can be obtained free of charge on application to CCDC, 12 Union Road, Cambridge CB21EZ, United Kingdom (fax: +44–1223–336033, email: deposit@ccdc.cam.ac.uk).
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Sathyamurthy, R., Brumaghim, J.L. & VanDerveer, D.G. Structure of “bis(methoxymagnesium)diselenide”: A reagent for the introduction of selenium into organic molecules. J Chem Crystallogr 37, 109–117 (2007). https://doi.org/10.1007/s10870-006-9156-7
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DOI: https://doi.org/10.1007/s10870-006-9156-7