title: Structure determination of two metal-organic complexes from high-resolution synchrotron powder diffraction data.
abstract: The crystal structures of [1,2-bis(2,6-diisopropylphenylimino)acenaphthene-N,N']carbonylchlororhodium(I) (1) and [N,N'-ethylene-bis(3-methylsalicylideneiminato)-O,N,N',O'](tetrahydrofurfuryl)-cobalt(II) (2) have been determined from high-resolution synchrotron X-ray powder diffraction data. Compound 1 is the first neutral Rh complex, in contrast with findings in the literature, containing a bidentate nitrogen ligand, and compound 2 is the first three-dimensional structure of a (five-coordinated) tetrahydrofurfurylcobalt(III) complex. Grid-search and Rietveld refinement have been used to determine and refine the structures, respectively. Crystals of 1 are orthorhombic, space group Pbca, Z = 8, with cell parameters a = 21.729 (2), b = 27.376 (3), c = 11.580 (1) A. Crystals of 2 are monoclinic, space group P2(1)/n, Z = 4, a = 16.6701 (6), b = 9.4170 (4), c = 13.7088 (7) A and beta = 96.520 (3) degrees. Chemical diagrams for the two compounds are given. Soft restraints were applied during Rietveld refinement; for 1 converging 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.
authors.affiliation: Laboratory for Crystallography, Institute of Molecular Chemistry, Universiteit van Amsterdam, Nieuwe Achtergracht 166, 1018WV Amsterdam, The Netherlands.
authors.forename: E
authors.initials: E
authors.lastname: Dova
authors.forename: K
authors.initials: K
authors.lastname: Goubitz
authors.forename: A
authors.initials: A
authors.lastname: van Langevelde
authors.forename: R
authors.initials: R
authors.lastname: Driessen
authors.forename: T
authors.initials: T
authors.lastname: Mahabiersing
authors.forename: R
authors.initials: R
authors.lastname: Blaauw
authors.forename: R
authors.initials: R
authors.lastname: Peschar
authors.forename: H
authors.initials: H
authors.lastname: Schenk