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The (ether-phosphine) ligands R 2 PCH 2 C 5 H 9 O (1a-c) [R = Ph (a), Cy (= cyclo-C 6 H 11 ) (b), n-C 3 H 7  (c); C 5 H 9 O = tetrahydropyranyl] are obtained from the corresponding alkali metal phosphides MPR 2  (M = Li, Na) and 2-chloromethyltetrahydropyran in ether. Reaction of 1 a-c with either Cl 2 M(COD) (COD = 1,5-cyclooctadiene) or [Ni(OH 2 ) 6 ]Cl 2  in a2:1 ratio leads to the bis(ether-phosphine)metal complexes Cl 2 M(R 2 P∾O) 2  trans-2b,c, trans-3b, cis-2a,b, cis-3a, and 4a [M = Pd (2), Pt (3), Ni (4)], in which the ligands 1a-c are η 1 -P-coordinated. In 2—4 Cl -  is abstracted by AgClO 4  to give the cationic trans-bis(ether-phosphine) complexes [ClM(R 2 P ∾ O)(R 2 P~O)][ClO 4 ] (5a, 6a-c, 7a) [M = Ni (5), Pd (6), Pt (7); P∾O = η 1 -P-coordinated; P~O = η 2 -O,P-coordinated]. In contrast to 7a, the nickel and palladium complexes 5a and 6a-c show fluxional behavior as demonstrated by temperature dependent  31 P{ 1 H} NMR spectra. The coalescence temperatures and estimated free energie enthalpies ΔG ≉  of 5a and 6a-c are compared with the corresponding data of the complexes [ClPd(Ph 2 P ∾ O)(Ph 2 ~O)][ClO 4 ] (8a-10a) [O,P ligand = Ph 2 PCH 2 C 4 H 7 O (8a), Ph 2 PCH 2 C 4 H 7 O 2  (9a), Ph 2 PCH 2 CH 2 OCH 3  (10a)] and give an insight into the relative basicity of the ether oxygen atoms.

zeitschrift für naturforschung b

Neuartige basische Liganden für die homogenkatalytische Methanolcarbonylierung, XXXI Kationische Bis(Ether-Phosphan)metall-Komplexe der Nickeltriade mit fluktuierendem Verhalten / Novel Basic Ligands for the Homogeneous Catalytic Methanol Carbonylation, XXXI Cationic Bis(Ether-Phosphine)Metal Complexes of the Nickel Triad with Fluxional Behavior