title: Isolation and structural characterization of tetra-n-propyl zirconate in hydrocarbon solution and the solid state.
abstract: Tetra-n-propyl zirconate has been purified by vacuum distillation and isolated as an extremely moisture sensitive, crystalline solid. According to a single-crystal X-ray diffraction study, crystalline tetra-n-propyl zirconate is composed of tetrameric Zr(4)(OPr(n))(16) (1) molecules whose Zr(4)O(16) metal-oxygen core structure has virtual C(2)(h) symmetry, the same structure observed previously for n-alkyl orthotitanates. Carbon-13 NMR spectroscopic data indicate that this core structure is retained in hydrocarbon solution. Molecule 1 has the same M(4)O(16) metal-oxygen core structure as [CH(3)C(CH(2)O)(3)](2)M(4)(OPr(i))(10), M = Ti, where the metal centers have octahedral coordination geometry, but a metal-oxygen core structure different from that of the M = Zr case, where trigonal metaprismatic coordination geometry is observed.
authors.affiliation: Department of Chemistry, University of Nebraska, Lincoln, Nebraska 68588, USA.
authors.forename: V W
authors.initials: VW
authors.lastname: Day
authors.forename: W G
authors.initials: WG
authors.lastname: Klemperer
authors.forename: M M
authors.initials: MM
authors.lastname: Pafford
mesh_terms: D002244:Carbon / Q000737:chemistry; D055598:Chemical Phenomena; D002627:Chemistry, Physical; D006838:Hydrocarbons / Q000737:chemistry; D008956:Models, Chemical; D008968:Molecular Conformation; D019906:Nuclear Magnetic Resonance, Biomolecular; D009942:Organometallic Compounds / Q000138:chemical synthesis / Q000737:chemistry*; D015040:Zirconium / Q000737:chemistry*
chemical_list: D006838:Hydrocarbons; D009942:Organometallic Compounds; D002244:Carbon; C444160:tetra-n-propyl zirconate; D015040:Zirconium