Synthesis, Spectroscopic and X-Ray Structural Characterization of |Cd(linpen)l2+, a Model for Metal Complexes of the Chelating Polymer Polyethyleneimine (linpen = Linear Pentaethylenehexamine)
نویسنده
چکیده
The isolation of 3,6,9,12-tetraazatetradecane-l,14-diamine (linear isomer of pentaethylene hexamine, linpen) from a technical polyamine mixture is described. In methanol, linpen acts as a hexadentate ligand towards cadmium(II). The solid compounds [Cd(linpen)](BPh4)2 (1), [Cd(linpen)](BPh4)2-2DM SO (2) and [Cd(linpen)](BF4)2 (3) have been isolated and character ized by elemental analysis, spectroscopy and X-ray powder diffraction. The 113Cd N M R reso nance of 1 is at 351 ppm (0.30 M in DMSO-d6, standard: 0.10 M Cd(C104)2 in D20). 2 and 3 have been structurally characterized by single-crystal X-ray diffraction. 2: C2/c; a = 19.337(1) A, b = 17.937(1)Ä, c = 18.584(1)Ä, ß = 1 11.54(1)°; Z = 4, R = 0.034, Rw = 0.033. 3: P2,/h; a = 8.607(1)Ä, b = 14.851(2)Ä, c = 15.703(2)Ä, ß = 91.21(2)°; Z = 4, R = 0.083, R„ = 0.072. Both compounds contain discrete [Cd(linpen)]2+ complexes. The hexamine wraps ar ound the metal ion in a helical manner. This results in a strong distortion of the coordination polyhedron. The mean C d -N bond lengths are 2.38Ä and 2.37Ä for 2 and 3, respectively. Models for M N 6 centers in metal-polyethyleneimine (PEI) complexes are derived from the structure of [Cd(linpen)]2+. For example, loops at the MN6 site in molecules of linear PEI are proposed.
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