Synthesis of the dioxidomolybdenum(VI) complexes [MoO 2 (HL R )(MeOH)]Cl (1-3) was carried out by usingMoO 2 Cl 2 and the corresponding ONO aroylhydrazone ligand H 2 L R (ligand H 2 L R is salicylaldehyde iso-were obtained upon exposure of the corresponding mononuclear complexes 1-3 to moisture. Deprotonation of the mononuclear complexes 1-3 was performed by using Et 3 N as a base (by the conventional solution based-method and by the mechanochemical approach) as well as by UV-light assisted reactions yielding [MoO 2 (L SIH )(MeOH)] (4), [MoO 2 (L NIH )(MeOH)] (5) and [MoO 2 (L Et2NSIH )] n (6), respectively.Crystal and molecular structures of all complexes were determined by the single crystal X-ray diffraction method. The complexes were further characterized by elemental analysis, IR spectroscopy, TG analysis, one-and two-dimensional NMR spectroscopy and powder X-ray diffraction.
Abstract. The structure of the human manganese derivative of insulin was determined using the single crystal X-ray diffraction method. Single crystals were grown by the hanging drop vapour diffusion crystallization method using zinc-free insulin and manganese(II) sulphate monohydrate in citrate buffer at pH = 6.4. It crystallizes in the trigonal system in the space group R 3 with the unit cell parameters: a = b = 81.70 Å and c = 33.73 Å. There are two manganese ions per insulin hexamer in the human manganeseinsulin derivative. The manganese ions lie on the three-fold crystallographic axis on opposite sides of the hexamer. Both manganese ions are octahedrally coordinated by three N ε2 atoms from the imidazolyl side chains of three symmetry-related HisB10/HisD10 and three oxygen atoms of three symmetry-related water molecules. The investigated human manganese-insulin derivative adopts the T 6 conformation.
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