Structure determination of two metal-organic complexes from high-resolution synchrotron powder diffraction data

The crystal structures of [1,2-bis(2,6-diisopropylphenylimino)acenaphthene- N, N']carbonylchlororhodium(I) (1) and [N,N'-ethylene-bis(3-methylsalicylid eneiminato)-O,N,N',O'](tetrahydrofurfuryl)cobalt(II) (2) have been determin ed from high-resolution synchrotron X-ray powder diffraction data. Compound 1 is the first neutral Rh complex, in contrast with findings in the litera ture, containing a bidentate nitrogen ligand, and compound 2 is the first t hree-dimensional structure of a (five-coordinated) tetrahydrofurfuryl-cobal t(III) complex. Grid-search and Rietveld refinement have been used to deter mine and refine the structures, respectively. Crystals of 1 are orthorhombi c, space group Pbca, Z = 8, with cell parameters a = 21.729 (2), b = 27.376 (3), c = 11.580 (1) Angstrom. Crystals of 2 are monoclinic, space group P2 (1)/n, Z = 4, a = 16.6701 (6), b = 9.4170 (4), c = 13.7088 (7) Angstrom and beta = 96.520 (3)degrees. Chemical diagrams for the two compounds are give n. Soft restraints were applied during Rietveld refinement; for 1 convergin g to R-p = 8.4%, R-w = 11.0%, GoF = 2.3, and for 2 converging to R-p = 8.5% , R-w = 11.4%, GoF = 7.6.