Organometallic flow chemistry: solvento complexes

Abstract

Photolysis under optimised flow conditions of metal carbonyls [{Ln}M(CO)x] [{Ln}M(CO)x = Cr(CO)6, Mo(CO)6, W(CO)6, Mn(CO)3(-C5H4Me), Re(CO)3(-C5H5)] in tetrahydrofuran (THF) conveniently affords the synthetically versatile and labile solvento complexes [{Ln}M(CO)x-1(THF)], thereby...

Free and coordinated biarsolyls

“…The addition of excess [Mn(THF)(CO) 2 (η 5 -C 5 H 4 Me)] 9 to a THF solution of 4d provided a bright orange mixture from which a single, moderately air-stable orange product was isolated following column chromatography; IR and 1 H NMR spectra are in perfect agreement with those of the side-product mentioned above and the proposed dimeric composition was confirmed by high-resolution mass spectrometry. Despite its novelty, the 13 C{ 1 H} NMR spectrum (C 6 D 6 ) is rather unremarkable: the four equivalent ( C 2h ) carbonyl nuclei are found at 232.4 ppm and the biarsolyl ring-carbons at 143.5 (2,5-positions) and 139.7 (3,4) ppm.…”

Bridging arsolido complexes

“…The σ-arsolido complex [Mo(AsC 4 Me 4 )(CO) 3 (η-C 5 H 5 )] ( 1 ) is readily obtained from the reaction of [Mo(SnBu 3 )(CO) 3 (η-C 5 H 5 )] with ClAsC 4 Me 4 . 8 The addition of in situ photochemically generated 9 metal- solvento reagents [Cr(THF)(CO) 5 ] and [Mn(THF)(CO) 2 (η 5 -C 5 H 4 Me)] to the metallo-ligand 1 provides the binuclear arsolido-bridged complexes [CrMo(μ-AsC 4 Me 4 )(CO) 8 (η-C 5 H 5 )] ( 2 , Fig. 2) and [MoMn(μ-AsC 4 Me 4 )(CO) 5 (η-C 5 H 5 )(η-C 5 H 4 Me)] ( 3 , Fig.…”