Reactions of Co 2(CO) 8 and of Co 2(CO) 6L (L = 3-pentyn-1-ol, 1,4-butyn-diol or 2-methyl-3-butyn-2-ol) with 2(diphenylphosphino)ethyl-trietoxysilane and tris(hydroxymethyl)phosphine for applications to new sol–gel materials

Abstract

The complex Co 2(CO) 6[μ-η 2-(H 3CC CCH 2CH 2OH)] ( 1) with the ligand 3-pentyn-1-ol ( pol) has been synthesized following established procedures. Its structure has been determined by X-ray analysis. The complex Co 2(CO) 6( mbo) ( mbo = 2-methyl-3-butyn-2-ol, HC CC(CH 3) 2OH), ( 3), along with the already known Co 2(CO) 6( bud) ( bud = 1,4-butyn-diol, HOCH 2C CCH 2OH) ( 2), and Co 2(CO) 8 were reacted with 2(diphenylphosphino)ethyl-triethoxysilane [Ph 2PCH 2CH 2Si(OCH 2CH 3) 3] ( dpts) and tris(hydroxymethyl)phosphine [P(CH 2OH) 3] ( thp). With dpts, mono- and di-substituted complexes were obtained: these were characterized by analytical and spectroscopic techniques. The structures of Co 2(CO) 6( dpts) 2 ( 5) and of Co 2(CO) 4( pol)( dpts) 2 ( 8) have been determined by X-ray analysis. Complex ( 1) was reacted with 3-(triethoxysilyl)propyl isocyanate [(H 3CCH 2O) 3Si(CH 2) 3NCO] ( tsi): the new complex Co 2(CO) 6[H 3CC CCH 2CH 2OC( O)NH(CH 2) 3Si(OCH 2CH 3) 3] ( 9) was obtained and spectroscopically characterized. The complex has also been reacted with tetraethyl orthosilicate ( teos); a new inorganic–organometallic material was obtained. Complex ( 5) has been grafted on the mesoporous material SBA-15. The hybrid inorganic–organometallic materials obtained have been characterized by inductively coupled plasma-mass spectrometry (ICP-MS), infrared spectroscopy (FT-IR) under vacuum conditions, X-ray diffraction (XRD) and scanning electron microscopy coupled to EDS probe (SEM–EDS).