Triphenylstibine substituted manganese and rhenium carbonyls: synthesis and multinuclear NMR spectroscopic studies. X-ray crystal structures of ax-[Mn-2(CO)(9)(SbPh3)], [Mn(CO)(5)(SbPh3)][CF3SO3] and fac-[Re(CO)(3)Cl(SbPh3)(2)]

摘要

The syntheses of [Mn-2(Co)(10-x)(SbPh3)(x)] (x = 1 or 2), [Re-2(CO)(9)(SbPh3)], [Mn(CO)(5)(SbPh3)][CF3SO3], [M(CO)(4)Cl(SbPh3)], fac-[M(CO)(3)Cl(SbPh3)(2) (M = Mn or Re) and mer,trans-[Mn(CO)(3)Cl(SbPh3)(2)] are reported. The complexes have been characterised by chemical analysis, IR and multinuclear NMR (H-1, C-13{H-1} and Mn-55) spectroscopies, and FAB mass spectrometry. The crystal structure of [Mn-2(CO)(9)(SbPh3)] established the axial position of the SbPh3 ligand (Mn-Sb 2.525(1), Mn-Mn 2.909(1) Angstrom) and that of [Mn(CO)(5)(SbPh3)][CF3SO3] confirmed the cation structure (Mn-Sb 2.596(3) Angstrom). The crystal structure of fac-[Re(CO)(3)Cl(SbPh3)(2)] establishes the stereochemistry (Re-Sb 2.726(1), 2.729(2) Angstrom). Differences in the products/isomers produced in reactions of [M-2(CO)(10)] and [M(CO)(5)Cl] with SbPh3 and with the corresponding PR3 and AsR3 ligands are identified and discussed. (C) 1998 Elsevier Science S.A. All rights reserved. [References: 32]