“…The 61 Ni NMR data of 7 , 8 , and 11 are in accord with those of the corresponding butyl- and ethyldiphenylphosphine nickel complexes . The IR data agree with those of similar di- and tricarbonylnickel complexes very well. ,, …”
Section: Resultssupporting
confidence: 66%
“…These ligands are successfully applied for the synthesis and immobilization of di- and tricarbonylnickel phosphine complexes. Nickel catalysts are of interest for academic as well as commercial reasons. , In particular, carbonylnickel phosphine complexes catalyze a variety of reactions, − and therefore early attempts at their immobilization on different supports were undertaken. − However, IR spectroscopy was the only analytical tool at that time and all research efforts were obviously halted in their beginnings. …”
Section: Introductionmentioning
confidence: 99%
“…23,24 In particular, carbonylnickel phosphine complexes catalyze a variety of reactions, [23][24][25] and therefore early attempts at their immobilization on different supports were undertaken. [26][27][28] However, IR spectroscopy was the only analytical tool at that time and all research efforts were obviously halted in their beginnings.…”
Silica is commonly modified with bifunctional phosphines like
PPh2CH2CH2Si(OEt)3
prior to immobilization of
catalysts. Here, besides
PPh2(CH2)3Si(OEt)3,
ligands that are more stable toward oxidation, namely
PPh2(C6H4)Si(OEt)3,
PPh2(C6H4)SiMe2(OEt),
and PPh2(CH2)4OH, are applied.
The di- and tricarbonylnickel complexes of
these ligands are synthesized, characterized by 61Ni,
31P, 13C, and 1H NMR and IR
spectroscopy, and immobilized
on silica. Alternatively, the corresponding phosphine-modified
silicas are treated with Ni(CO)4. The
obtained
materials are investigated by 31P and 13C
solid-state NMR spectroscopy. Di- and tricarbonylnickel species
can
be distinguished by their different chemical shift anisotropies and
also by their IR data. While the first route
allows immobilization of both di- and tricarbonylnickel complexes,
reaction of surface-bound phosphines with
Ni(CO)4 gives the tricarbonyl species exclusively.
Among the different ligands,
PPh2(CH2)4OH has
optimal
qualities: It gives high surface coverages without oxidation or
cross-linking, and therefore narrow NMR lines,
and it allows 13C CP/MAS NMR spectroscopy.
“…The 61 Ni NMR data of 7 , 8 , and 11 are in accord with those of the corresponding butyl- and ethyldiphenylphosphine nickel complexes . The IR data agree with those of similar di- and tricarbonylnickel complexes very well. ,, …”
Section: Resultssupporting
confidence: 66%
“…These ligands are successfully applied for the synthesis and immobilization of di- and tricarbonylnickel phosphine complexes. Nickel catalysts are of interest for academic as well as commercial reasons. , In particular, carbonylnickel phosphine complexes catalyze a variety of reactions, − and therefore early attempts at their immobilization on different supports were undertaken. − However, IR spectroscopy was the only analytical tool at that time and all research efforts were obviously halted in their beginnings. …”
Section: Introductionmentioning
confidence: 99%
“…23,24 In particular, carbonylnickel phosphine complexes catalyze a variety of reactions, [23][24][25] and therefore early attempts at their immobilization on different supports were undertaken. [26][27][28] However, IR spectroscopy was the only analytical tool at that time and all research efforts were obviously halted in their beginnings.…”
Silica is commonly modified with bifunctional phosphines like
PPh2CH2CH2Si(OEt)3
prior to immobilization of
catalysts. Here, besides
PPh2(CH2)3Si(OEt)3,
ligands that are more stable toward oxidation, namely
PPh2(C6H4)Si(OEt)3,
PPh2(C6H4)SiMe2(OEt),
and PPh2(CH2)4OH, are applied.
The di- and tricarbonylnickel complexes of
these ligands are synthesized, characterized by 61Ni,
31P, 13C, and 1H NMR and IR
spectroscopy, and immobilized
on silica. Alternatively, the corresponding phosphine-modified
silicas are treated with Ni(CO)4. The
obtained
materials are investigated by 31P and 13C
solid-state NMR spectroscopy. Di- and tricarbonylnickel species
can
be distinguished by their different chemical shift anisotropies and
also by their IR data. While the first route
allows immobilization of both di- and tricarbonylnickel complexes,
reaction of surface-bound phosphines with
Ni(CO)4 gives the tricarbonyl species exclusively.
Among the different ligands,
PPh2(CH2)4OH has
optimal
qualities: It gives high surface coverages without oxidation or
cross-linking, and therefore narrow NMR lines,
and it allows 13C CP/MAS NMR spectroscopy.
“…[(Ph 3 P) 2 Pd(N 3 ) 2 ], react in solution with CO under very mild conditions to give isocyanato complexes [3–5, 34–38] [Scheme , Equation (11)]. This reaction even occurs with the solid, polystyrene‐fixed [(PPh 2 ) 2 Pd(N 3 ) 2 ] 39. Azido bridges react more slowly than terminal N 3 ligands.…”
Section: Reactions Of Azido Metal Complexes With Carbon Monoxidementioning
, Contents, 1. Introduction, 2. Reactions of Carbonyl Metal Complexes with the Azide Ion, 3. Reactions of Azido Metal Complexes with Carbon Monoxide, 4. Reactions of the Azide Ion with the NO+ Cation, 5. Reaction of Nitrosyl Complexes with the Azide Ion, 6. Nitrosation of the Coordinated Azide Ligand
“…Zur Fixierung von Metallcarbonylverbindungen wurden bisher vor allem N-und PLiganden verwendet [2]. In Fortführung unserer Untersuchungen über polymere Metallkomplexe [3,4] berichten wir über die Synthese von Polystyrolderivaten mit Isocyanidfunktionen und die Fixierung von Metallcarbonylen auf diesen Trägern.…”
Abstract Polyisocyanides with the groups -CH2N ≡ C and -C(O)O(CH2)2N≡C attached to polystyrene have been prepared and reacted with various metal carbonyl compounds resulting in the fixation on the polymeric supports of-M(CO)5, -M(CO)4 (M = Cr, Mo, W), -MO(Cl)(η-C5H5)(CO)2, -Mn2(CO)η -Mn(CO)ηX (N = 3, 4; X = Cl, Br), -Fe(CO)4, -Fe3(CO)11, -FeI2(CO)2, -FeX(η-C5H5)(CO) (X = Cl, Br, I), -Ru(CO)4, -Ru3(CO)9, ,,-Os3H2(CO)10", and -RhCl(CO)2. The cyano complexes [Fe(CN)2(η-C5H5)CO]- and [Mo(CN)2(η-C5H5)(CO)2]- have been immobilized by alkylation with chloromethylated polystyrene
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