| Abstract |
The water-soluble Rh-I compound [ Rh( Tpms)( CO)( PTA)] ( 1) (Tpms = O3SC( pz) 3, PTA=1,3,5-triaza-7-phosphaadamantane) has been easily prepared in high yield by a single-pot reaction of [\Rh( CO)(2)( mu-Cl)\(2)] with PTA and the tris(1-pyrazolyl) methanesulfonate lithium salt Li( Tpms), in a CH2Cl2/MeOH solution at room temperature. This synthetic strategy can be easily applied to the preparation of general [ Rh( Tpms)( CO)( L)] ( L = phosphine) complexes and constitutes a substantial improvement over the previously described procedures. Compound 1 is air stable in the solid state and water-soluble, affording stable solutions under an inert atmosphere. It has been characterized by IR, H-1, P-31\H-1\ and C-13\H-1\ NMR spectroscopies, elemental and single crystal X-ray diffraction structural analyses. The solid state structure of 1 has a square-planar geometry with the Tpms ligand coordinating the metal centre in a (kappa(2): N, N) bipodal mode. The title compound has also been investigated by cyclic voltammetry in CH3CN, and values of the E-L Lever and P-L Pickett electrochemical parameters ( which measure the ligand net electron-donor character) are proposed for the PTA ligand. Complex 1 represents the first example of a transition metal complex bearing both PTA and Tpms ( or any other tris( 1-pyrazolyl) methane or derivative) ligands. (C) 2008 Elsevier B. V. All rights reserved. |
