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The secondary phosphines R(Ar*)PH(R = Me, iPr, Ph, Mes, Ar*) (2a-2h) with bulky aromatic substituents Ar* (Ar* = 2,3,6-R′  3 C 6 H 2 , R′ = iPr, tBu) are obtained in good yields by reaction of RPCl 2 , PCl 3 , PBr 3  or Ar*P(Cl, Br) 2  with 2,4,6-tBu 3 C 6 H 2 Li or 2,4,6- iPr 3 C 6 H 2 MgBr and subsequent reduction of the intermediate halophosphines R(Ar*)PX(X = Cl, Br) with LiAlH 4 . The X-ray structural analysis of Ph(2,4,6-iPr 3 C 6 H 2 )PH (2g), space group P 1 , shows P-C-distances of 1.824(1) and 1.838(1)Å. The lithium derivatives of 2a-2c are monomeric in solution as indicated by the 1 :1 :1 : 1-quartet  7 L i -  31 P fine structure of the  31 P {1H} NMR signals at low temperatures. 2a-2c and 2f-2h form Ni(0) and Fe(0) complexes (CO) 3 NiL (6a-6f) and Fe(CO) 4 L (7a-7d), respectively. The Tolman electronic parameters of the bulky ligands are almost identical. Within the series 2a-2h the spatial shielding of the P atoms has been estimated using advanced molecular modeling techniques. The bulky ligand 2c forms coinage metal complexes [C u(CH 3 CN) 2 (2c) 2 ] [PF 6 ] (8), Cu 2 Cl 2 (2c) 2  (9) and Cl-Au(2c) (10). While 10 is monomeric in solution, in the solid state it forms pairs of head to tail oriented monomers with almost linear Cl - Au - P skeletons (Cl - Au - P 175.47(9)°) as shown by an X-ray structural analysis.

zeitschrift für naturforschung b

Synthese, Koordinationschemie und Ligandeneigenschaften sekundärer Phosphane R(Ar*)PH mit sperrigen aromatischen Resten - Molekülstruktur von Ph(2,4,6-iPr 3 C 6 H 2 )PH, (2,4,6-iPr 3 C 6 H 2 ) 2 PH und ClAu[PhP(2,4,6-Bu 3 C 6 H 2 )H] / Synthesis, Coordination Chemistry and Ligand Properties of Secondary Phosphines R(Ar*)PH with Bulky Aromatic Substituents - Molecular Structure of Ph(2,4,6-iPr 3 C 6 H 2 )PH, (2,4,6-iPr 3 C 6 H 2 ) 2 PH and ClAu[PhP(2,4,6-tBu 3 C 6 H 2 )H]