Synthesis and Characterization of the New Cluster Complex {Mo3S4} with the Hemilabile Phosphine-Selenoether Ligand

The reaction of [Mo 3 S 4 (Tu) 8 (H 2 O)]Cl 4 ·4H 2 O (Tu is thiourea) with (PhCH 2 CH 2 ) 2 -PCH 2 CH 2 SeC 5 H 11 ) (PSe) followed by purification on a chromatographic column packed with silica gel using a saturated solution of KPF 6 in acetone as an eluent results in the formation of [Mo 3 S 4 Cl...

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Bibliographic Details
Published in:Russian journal of coordination chemistry 2021-03, Vol.47 (3), p.209-218
Main Authors: Shmelev, N. Yu, Gongola, M. I., Malysheva, S. F., Belogorlova, N. A., Artem’ev, A. V., Fomenko, Ya. S., Komarov, V. Yu, Sopov, K. V., Kompan’kov, N. B., Sheven’, D. G., Sokolov, M. N., Gushchin, A. L.
Format: Article
Language:English
Subjects:
Acetone
Aniline
Catalytic activity
Chemistry
Chemistry and Materials Science
Infrared spectroscopy
Inorganic Chemistry
Ions
Ligands
Mass spectrometry
Nitrobenzene
NMR spectroscopy
Phosphines
Phosphorus
Physical Chemistry
Room temperature
Selenium
Silica gel
Silicon dioxide
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Summary:The reaction of [Mo 3 S 4 (Tu) 8 (H 2 O)]Cl 4 ·4H 2 O (Tu is thiourea) with (PhCH 2 CH 2 ) 2 -PCH 2 CH 2 SeC 5 H 11 ) (PSe) followed by purification on a chromatographic column packed with silica gel using a saturated solution of KPF 6 in acetone as an eluent results in the formation of [Mo 3 S 4 Cl 3 (PSe) 3 ]PF 6 ( I ) in a yield of 44%. Compound I is characterized by X-ray diffraction analysis, 1 H, 31 P{ 1 H}, and 77 Se NMR spectroscopy, IR spectroscopy, UV-Vis spectroscopy, cyclic voltammetry, and electrospray ionization mass spectrometry. Several species differed in the coordination mode of three PSe ligands, which can bind to molybdenum via one (phosphorus) or two (phosphorus and selenium) donor atoms, are formed in a solution of compound I at room temperature. This behavior is not observed for the compounds similar in structure with PS ligands of an analogous type. Complex I demonstrates a higher catalytic activity than its analogue with the PS ligand in the reduction of nitrobenzene to aniline under the action of diphenylsilane.
ISSN:1070-3284
1608-3318
DOI:10.1134/S1070328421030040