Xray experimental

Data collections were performed at the X-ray diffraction beamline (XRD1) of the Elettra Synchrotron of Trieste (Italy), equipped with a Pilatus 2M image plate detector.

Collection temperature was 100 K (nitrogen stream supplied through an Oxford Cryostream 700); the wavelength of the monochromatic X-ray beam was 0.700 Å and the diffractograms were obtained with the rotating crystal method.

The crystals were dipped in N-paratone and mounted on the goniometer head with a nylon loop. The diffraction data were indexed, integrated and scaled using XDS [kabsch:2010].

The structures were solved by the dual space algorithm implemented in the SHELXT code [shelxt]. Fourier analysis and refinement were performed by the full-matrix least-squares methods based on F² implemented in SHELXL [shelxl]. The Coot and SHELXLE programs were used for modeling [coot,shelxle].

For the refinement of the crystal structure of complex [ka76], anisotropic thermal motion was allowed for all non-hydrogen atoms. Hydrogen atoms were placed at calculated positions with isotropic factors U=1.2×U_eq, U_eq being the equivalent isotropic thermal factor of the bonded non hydrogen atom.

The refinement of the X-ray data for the complexes [ka89_f2] and [ka104] and for the ligand of complex [ka89_f2] are still under work: in the ORTEP representations showed in this thesis thermal motion is thus represented isotropically.

References