Five novel complexes of formula [Ln(hfac)3] · BNPhOM, where La = Gd, Ho, Dy, Y, Er; Mac = hexfluoracetylacetonate; BNPhOM=1,3-[bis-2,2′,-(4,4,5,5-tetramethyl-4,5-di-hydro-1H-imidazolyl-1-oxyl-3-oxide) phenoxy] propane, have been prepared and characterized by elemental analysis, molar conductances, IR and electronic spectra. The temperature dependence of the magnetic susceptibility for Gd(III) and radical was measured (2—-300 K). The observed data were successfully simulated giving the exchange integral J = 0.28 cm?1, J' = - 0.33 cm?1. These results indicate a weak ferromagnetic spin exchange interaction between Gd(III) ion and the radical and a weak antiferromagnetic spin exchange interaction between the radical and radical.
The new compound was prepared by the reaction of Cd(ClO4)2·6H2O,1,10 phenanthroline (phen)and picric acid (HPA)(ratio 1∶3∶2) in methanol aqueous solution refluxing for 4 hours. The crystals used for X ray analysis was obtained by slow evaporation of the solution at room temperature. The crystal compound is in triclinic with space group with a=1.1363(4)nm,b=1.2593(2)nm,c=1.3972(4)nm,α=93.97(2)?,β=100.84(3)?,γ=106.29(2)?,Z=2,V=1.8690(9)nm3,Dc=1.715g·cm-3, μ(MoKα)=0.677mm-1,F(000)=972,R=0.0907,wR=0.2240. In the complex, the Cd? cation is octahedrally coordinated to two 1,10 phenanthroline ligands and two water molecules incis disposition. As outer sphere, picrate anions are combined with inner by hydrogen bond and static electricity interaction.
Seven new μ-isophthalato dinuclear lanthanide(Ⅲ) complexes, namely [Ln2(IPHTA)(Me2-phen)4-(ClO4)2](ClO4)2 (Ln = La, Nd, Sm, Eu, Gd, Ho, Er), where Me2-phen denotes 2,9-dimethyl-1, 10-phenanthroline (Me2-phen) , IPHTA represents isophthalate dianion, have been synthesized and characterized by elemental analyses, molar conductance measurements, IR, ESR and electronic spectra. The variable-temperature magnetic susceptibilities of [Gd2( IPHTA) (Mez-phen)4 (ClO4)2] (ClO4)2 complex were measured in the temperature range of 4-300 K and the observed data were successfully simulated by the equation based on the spin Hamiltonian operator, H = - 2JS1 · S2, giving the exchange parameter J =- 0.19 cm-1 . This result is commensurate with a weak antiferromagnetic spin-exchange interaction between Gd(Ⅲ)-Gd(Ⅲ) ions within the complex.
The title compound was prepared by the solid state reaction of stoichiometric amounts of CdCl2·H2O and 4 nitroaniline . The crystal used for X ray analysis was obtained by slow evaporation of an ethanol aqueous solution of the solid state reaction at room temperature. The structure of compound was characterized by X ray diffraction analysis. The crystal belongs to orthorhombic, space group Pbca, a=0.77864(7)nm,b=0.72547(6)nm,c=3.3126(2)nm,Z=4,V=1.8712(3)nm3,Dc=1.890g·cm-3,μ=1.763mm-1,F(000)=1048,R=0.0300,wR=0.0697. The title compound is a typical two dimensional organic intercalated compound. The inorganic layers of the compound are formed by CdCl6 octahedra sharing corner Cl atoms (i.e. catena poly[dihlorocadmium di μ chloro]). The organic ammonium cations are intercalated between every two metal halogen layers and formed the organic layers of the compound through hydrogen bonding.
Nanocrystalline Zn(Oxin)2·2H2O (Zinc 8-quinolinolate) was synthesized at near ambient temperature by solid state chemical reaction. Phases, particle sizes and morphology of the prepared nanocrystallite were characterized by Powder X-ray diffraction (XRD) and transmission electron microscopy(TEM). The results showed that the crystallite product had an average size about 30 nm. The effects of a series of reaction conditions on the synthesis of Zn(Oxin)2·2H2O (Zinc 8-quinolinolate) by solid state reaction were studied.