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Amide Coupling Reaction for the Synthesis of Bispyridine-based Ligands and Their Complexation to Platinum as Dinuclear Anticancer Agents
Published on: May 28, 2014
Synthesis and Crystal Structure Determination of Bifunctional Phosphine-Linked Triplatinum Double-Cluster Complexes
Daniel Imhof1, Urs Burckhardt, Klaus-Hermann Dahmen
1Laboratorium für Anorganische Chemie, ETH, Zürich, Switzerland, and Department of Chemistry and MARTECH, The Florida State University, Tallahassee, Florida 32306-3006.
Abstract:
Reactions of [Pt(3)(&mgr;-CO)(3)(PCy(3))(3)] (1) and [Pt(3)(&mgr;-CNXyl)(2)(&mgr;-CO)(CNXyl)(PCy(3))(2)] (2) (Cy = C(6)H(11), Xyl = C(8)H(9)) with (1)/(2) equiv of a bifunctional metal phosphine cation [(MPR'(2))(2)(R)](2+) (M = Cu, Ag, Au; R = C(6)H(4), (CH(2))(2)C(6)H(4), Fe(C(5)H(5)); R' = C(6)H(5), C(6)H(11)) yielded quantitatively [{Pt(3)(&mgr;-CO)(3)(PCy(3))(3)}(2){(MPR'(2))(2) (R)}](2+) and [{Pt(3)(&mgr;-CNXyl)(2)(&mgr;-CO)(CNXyl)(PCy(3))(2)}(2){(MPR'(2))(2)(R)}](2+), respectively. The compounds were characterized by IR-, MS-, and (31)P-NMR spectroscopy. The X-ray structure is given for [{Pt(3)(&mgr;-CO)(3)(PCy(3))(3)}(2){(AuPPh(2))(2)(CH(2))(2)C(6)H(4))}][PF(6)](2) (14), which crystallizes in the triclinic space group P&onemacr; with Z = 1, a = 15.350 Å, b = 17.150 Å, c = 20.446 Å, alpha = 84.54 degrees, beta = 84.84 degrees, and gamma = 64.56 degrees. The structure was refined to R = 0.0435 for the 8430 observed reflections (I > 3sigma(I)).
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