PubMed · 10360349
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A C North. 1999. David C. Phillips.. https://doi.org/10.1038/9272
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The new iridium(III) complex, imidazolium[trans(DMSO,imidazole)tetrachloroiridate(III)], (I) (DMSO=dimethyl sulfoxide), and the orange form of [(DMSO)(2)H][trans(DMSO)(2)tetrachloroiridate(III)], (II) have been prepared and characterized, both in the solid state and in solution, by X-ray diffraction and by various physicochemical techniques. Single crystal X-ray diffraction studies point out that complex (II) is isomorphous to the ruthenium(III) analogue, [(DMSO)(2)H][trans-RuCl(4)(DMSO)(2)], (III). Crystallographic data are the following: a=16.028(2) A, b=24.699(3) A, c=8.262(1) A, in space group Pbca (Z=8) for (imidazolium)[trans(DMSO,imidazole)tetrachloroiridate(III)], (I); and a=9.189(2) A, b=16.511(4) A, c=14.028(3) A, beta=100.82(2) degrees in space group P2/n (Z=4) for [(DMSO)(2)H][trans(DMSO)(2)tetrachloroiridate(III)], (II). Visible absorption spectra show that both complexes are stable for several days, at pH 7.4, at room temperature. No significant chloride hydrolysis is observed, even at high temperature (70 degrees C), over 24 h. The extreme stability of these iridium(III) complexes within a physiological buffer was further assessed by (1)H NMR; in addition, cyclic voltammetry measurements evidenced a high stability of the oxidation state +3. Preliminary biological studies show that both complexes do not bind appreciably bovine serum albumin nor inhibit significantly the proliferation of representative human tumor cell lines, suggesting that hydrolysis of coordinated chlorides is a crucial feature for the biological properties and the antitumor activity of the parent ruthenium(III) complexes.
Molecular dynamics (MD) simulations of beta-cyclodextrin (beta-CD) have been carried out in aqueous solution at 300 K over a period of about 200 ps using Tripos force field. The atomic trajectories obtained by these simulations have been analysed by means of the occurrence of hydrogen bonds. The MD simulations lead to an association of seven water molecules into the beta-CD cavity which is in a good agreement with X-ray crystallography experiments. This demonstrates that the force field used in the simulations is able to reproduce the experimentally observed hydrophilic-hydrophobic characteristics of beta-CD molecule.
Radiation damage sets a fundamental limit for studies with ionizing radiation; cryo-methods are known to ease these limits. Here, measurements on mass loss and the decrease in the C=O bond density as measured by oxygen-edge XANES (NEXAFS) spectroscopy in thin films of poly(methylmethacrylate) (PMMA), studied in a vacuum, are reported. While cryo-methods allow more than 95% of the mass to remain at doses up to 10(7) Gy, there is little difference in C=O bond density versus dose between 298 K and 113 K sample temperatures. At both temperatures the critical dose for bond breaking is approximately 15 x 10(6) Gy.