A β-ketoiminato palladium(II) complex for palladium deposition

The ¦-ketoiminato complex [Pd(OAc)L] (3) can be synthesized by the reaction of bis(benzoylacetone)diethylenetriamine (1, = LH) with [Pd(OAc)2] (2). The structure of 3 in the solid state has been determined by single X-ray diffraction analysis. Complex 3 crystallizes as a dimer (32), which is formed by hydrogen bonds between NH and OOAc functionalities of two adjacent ligands. Each of the Pd atoms is complexed by one ON2 donor unit of the polydentate ligand L− and an acetate group. Pd–Pd interactions and hydrogen bond formation between a NH and the C=O acetate moiety lead to a [4 + 2] coordination at Pd. The non-coordinated part of L exists in its ¦-keto-enamine form. The thermal decomposition behavior of 32 was studied by TG (thermogravimetry) and TG-MS showing that 32 decomposes between 200 and 500°C independent of the applied atmosphere. Under oxygen PdO is produced, while under argon Pd is formed as confirmed by PXRD measurements. Complex 32 was applied as a spin-coating precursor (conc. 0.1 mol L−1, volume 1.5 mL, 3000 rpm, deposition time 6 min, heating rate 50 K min−1, holding time 60 min (Ar) and 120 min (air) at T = 800°C). The as-obtained samples are characterized by granulated particles of Pd/PdO on the substrate surface. EDX (energy-dispersive X-ray spectroscopy) and XPS (X-ray photoelectron spectroscopy) measurements confirmed the formation of Pd (Ar) or PdO (O2) with up to 12 mol% C impurity.

THE METHOD FOR OBTAINING A DERIVATIVE CLOSO-DECABORATE ANION WITH PENDANTE DTPA-GROUP

This paper describes the method for obtaining a new derivative of the closo-decaborate anion with diethylenetriaminepentaacetic acid (DTPA) as a pendant group attached to the boron cluster through an alkoxyl spacer chain. This derivative is formed by the interaction of 1,4-dioxane derivative of the anion [B10H10]2- with DTPA potassium salt in an aqueous medium. As a result of the reaction, an exo-polyhedral cyclic substituent is opened, and then the addition of a polyfunctional group through an oxygen atom occurs. The synthesized compound is in fact an effective polydentate ligand capable of coordinating to the complexing agent both due to the donor atoms of the attached DTPA fragment and through the formation of three-center two-electron bonds. The obtained compound interacts with gadolinium(III) carbonate forming a complex of the composition [Gd2B10H9O2C4H8(dtpa)]·3H2O. The synthesized substances were studied by IR spectroscopy, polynuclear (11B, 13C and 1H) NMR spectroscopy, ESI mass spectrometry, elemental and thermographic analysis. closo-Decaborate with the pendant DTPA group is of interest in 10B neutron capture therapy of malignant tumors due to the high content of boron atoms and a convenient way of their transport to the affected cells. The obtained boron-containing derivatives of gadolinium(III) can act as drugs of combined action, because they can perform, in addition to the above described therapeutic function, the diagnostic function due to the presence of gadolinium atoms int hem.