The interactions of MoCl5 (1) with a variety of organic compounds were studied in dichloromethane and the metal products were isolated in the solid state. The 3:1 molar reactions of 1 with OCRR′ (R = R′ = Ph, R = H, R′ = 2-C6H4Me) afforded the complexes Mo(O)Cl3(OCRR′)2 (R = R′ = Ph, 2a; R = H, R′ = 2-C6H4Me, 2b) in high yields. Compound Mo(O)Cl3[ ], 3, was isolated in 35% yield from 1 and 2-acetylfuran. The 1:1 reactions of 1 with, respectively, MeO2CCCCO2Me and phenazine (C12H8N2) resulted in the formation of the polynuclear complexes [MoCl4:2-L]n (L = MeO2CCCCO2Me, 4; L = C12H8N2, 6). The mononuclear Mo(O)Cl3[1(N)-C12H8N2], 7, was prepared straightforwardly by addition of phenazine to Mo(O)Cl3, formed in situ upon treatment of 1 with tetrahydrofuran. The 1:2 reaction of 1 with Me2NCH2CH2CO2Me gave MoCl4[1(N)-Me2NCH2CH2CO2Me]2, 5, in 72% yield. The molecular structures of 2a, 3 and 7 were elucidated by X-ray diffraction studies; the X-ray structure of 7 represents a rare example of crystallographically-characterized pentacoordinated Mo(V) complex.
Reactions of Molybdenum Pentachloride with Oxygen and Nitrogen Donor Ligands
MARCHETTI, FABIO;PAMPALONI, GUIDO;
2013-01-01
Abstract
The interactions of MoCl5 (1) with a variety of organic compounds were studied in dichloromethane and the metal products were isolated in the solid state. The 3:1 molar reactions of 1 with OCRR′ (R = R′ = Ph, R = H, R′ = 2-C6H4Me) afforded the complexes Mo(O)Cl3(OCRR′)2 (R = R′ = Ph, 2a; R = H, R′ = 2-C6H4Me, 2b) in high yields. Compound Mo(O)Cl3[ ], 3, was isolated in 35% yield from 1 and 2-acetylfuran. The 1:1 reactions of 1 with, respectively, MeO2CCCCO2Me and phenazine (C12H8N2) resulted in the formation of the polynuclear complexes [MoCl4:2-L]n (L = MeO2CCCCO2Me, 4; L = C12H8N2, 6). The mononuclear Mo(O)Cl3[1(N)-C12H8N2], 7, was prepared straightforwardly by addition of phenazine to Mo(O)Cl3, formed in situ upon treatment of 1 with tetrahydrofuran. The 1:2 reaction of 1 with Me2NCH2CH2CO2Me gave MoCl4[1(N)-Me2NCH2CH2CO2Me]2, 5, in 72% yield. The molecular structures of 2a, 3 and 7 were elucidated by X-ray diffraction studies; the X-ray structure of 7 represents a rare example of crystallographically-characterized pentacoordinated Mo(V) complex.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
