Präparative, röntgenographische und schwingungsspektroskopische Untersuchungen an Iodaten zweiwertiger Übergangsmetalle : DRIFT-Experimente

The aim of this doctoral thesis, which was made in the inorganic solid state chemistry, was the preparation and characterization by x-ray diffraction and vibrational spectroscopy of some hydrate iodates of cobalt, nickel and zinc with following compositions: Ni(IO 3 ) 2 ⋅10H 2 O; M (IO 3 ) 2 ⋅4H 2 O with M =Co, Ni; M (IO 3 ) 2 ⋅2H 2 O with M = Co, Ni, Zn; 3 Co(IO 3 ) 2 ⋅2H 2 O; Co(IO 3 ) 2 ⋅H 2 O and M (IO 3 ) 2 with M =Co, Ni, Zn. The structures of three novel hydrate iodates with the compositions Ni(IO 3 ) 2 ⋅10H 2 O, Co(IO 3 ) 2 ⋅H 2 O and 2Co(IO 3 ) 2 ⋅3H 2 O was examined. In addition the structure of Zn(IO 3 ) 2 ⋅2H 2 O was solved by using single crystal data and the refinement of the structure of Co(IO 3 ) 2 ⋅H 2 O and β- Ni(IO 3 ) 2 by using powder data was presented. The structural relationship of some transition metal iodates were intensively discussed. For most of them the distances of the intra- and intermolecular hydrogen bonds were calculated. The results showed the exceptionally strong hydrogen bonds in Co(IO 3 ) 2 ⋅H 2 O. The influence of the solid state is discussed on vibrational spectra of halogenates with undisturbed C 3v symmetry. Furthermore experiments with a diffusive infrared-reflection unity (DRIFT) were presented. The DRIFT spectroscopy is an interesting alternative for vibrational spectroscopic measurements. The advantages of these technique compared with common transmission infrared spectroscopy were explained. As a result of the experiments some new embedding materials were introduced.