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Microcrystalline Samples (microcrystalline + sample)
Selected AbstractsSynthesis and Photophysical Properties of LnIII,DOTA,Bipy Complexes and LnIII,DOTA,Bipy,RuII Coordination ConjugatesEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 28 2010Miguel Vázquez López Abstract The synthesis and the systematic and comparative photophysical study of a series of visible (EuIII, TbIII) and NIR-emitting (NdIII, YbIII) lanthanide complexes (Ln2L) and ruthenium,lanthanide coordination conjugates (Ln2LRu) are reported. The GdIII complex, the GdIII,RuII coordination conjugate, as well as the RuII complex of the ligand H6L have also been synthesized and photophysically studied as control systems. The ligand H6L, composed of a central bipyridine binding unit and functionalized on each 5,-position with a DOTA macrocycle, has been successfully synthesized from cyclen, 5,5,-dimethyl-2,2,-bipyridine and 1,2-ethylendiamine in a nine-step process. Detailed luminescence studies of all complexes, including the determination of the quantum yield and lifetime, were carried out on finely powdered microcrystalline samples as well as in water, deuterated water and [D6]DMSO at ambient (295 K) and low temperature (77 K). The photophysical data corroborate the existence of energy transfer in the Ln2L complexes and in the Nd2LRu coordination conjugate. However, no (or at most, very little) energy transfer is takes place from the Ru(bipy)3 chromophore to the LnIII ion in the other Ln2LRu heteropolymetallic complexes. Moreover, the photophysical studies reveal that all the complexes and coordination conjugates adopt different conformations and hydration states in solution and in the solid state, which influences the efficiency of the energy transfer between the bipy and/or Ru(bipy)3 antennae and the LnIII ions. [source] Electrical Conductivity and Lattice Defects in Nanocrystalline Cerium Oxide Thin FilmsJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 9 2001Toshio Suzuki The results of the electrical conductivity and Raman scattering measurements of CeO2 thin films obtained by a polymeric precursor spin-coating technique are presented. The electrical conductivity has been studied as a function of temperature and oxygen activity and correlated with the grain size. When compared with microcrystalline samples, nanocrystalline materials show enhanced electronic conductivity. The transition from extrinsic to intrinsic type of conductivity has been observed as the grain size decreases to <100 nm, which appears to be related to a decrease in the enthalpy of oxygen vacancy formation in CeO2. Raman spectroscopy has been used to analyze the crystalline quality as a function of grain size. A direct comparison has been made between the defect concentration calculated from coherence length and nonstoichiometry determined from electrical measurements. [source] Investigation of structure and dynamics in the sodium metallocenes CpNa and CpNa·THF via solid-state NMR, X-ray diffraction and computational modellingMAGNETIC RESONANCE IN CHEMISTRY, Issue S1 2007Cory M. Widdifield Abstract Solid-state 23Na NMR spectra of two organometallic complexes, cyclopentadienylsodium (CpNa) and the tetrahydrofuran (THF) solvate of CpNa (CpNa·THF), are presented. Analytical simulations of experimental spectra and calculated 23Na electric-field gradient (EFG) tensors confirm that both complexes are present in microcrystalline samples of CpNa recrystallized from THF. For the solvate, 23Na NMR experiments at 9.4 T and 11.7 T elucidate sodium chemical shielding (CS) tensor parameters, and establish that the EFG and CS tensor frames are non-coincident. Single-crystal X-ray diffraction (XRD) experiments are used to determine the crystal structure of CpNa·THF: Cmca (a = 9.3242(15) Å, b = 20.611(3) Å, c = 9.8236(14) Å, , = , = , = 90° , V = 1887.9(5)Å3, Z = 8). For CpNa, 23Na NMR data acquired at multiple field strengths establish sodium CS tensor parameters more precisely than in previous reports. Variable-temperature (VT) powder XRD (pXRD) experiments determine the temperature dependence of the CpNa unit cell parameters. The combination of 23Na quadrupolar NMR parameters, pXRD data and calculations of 23Na EFG tensors is used to examine various models of dynamic motion in the solid state. It is proposed that the sodium atom in CpNa undergoes an anisotropic, temperature-dependent, low frequency motion within the ab crystallographic plane, in contrast with previous models. Copyright © 2007 John Wiley & Sons, Ltd. [source] Polymorphism of CaTeO3 and solid solutions CaxSr1,,,xTeO3ACTA CRYSTALLOGRAPHICA SECTION B, Issue 2 2009Berthold Stöger Single crystals and microcrystalline samples of the calcium tellurate(IV) phases ,-, ,-, ,,- and ,-CaTeO3 as well as of two solid solutions CaxSr1,,,xTeO3 (x = 0.55 and 0.77) have been synthesized and characterized by X-ray diffraction and thermal analysis. A comparative description of the structures and the relations between the polymorphs is given. The main building units of the hitherto unknown structures are isolated [TeIVO3]2, units and [(Ca,Sr)Ox] (x = 6,8) polyhedra. All structures exhibit channels in which the TeIV electron lone pairs protrude. The low-temperature phase ,-CaTeO3 is stable up to 1168,K. It exhibits nearly cylindrical channels (diameter ,,4,Å) and differs structurally from the other phases, whereas the metastable high-temperature phases are closely related to each other. They feature oval channels (shortest and longest diameter ,,2 and 8,Å). ,-CaTeO3 can be described as an order,disorder (OD) structure of two non-polar layers with layer groups p121/m1 and p1211. The ,-CaTeO3 crystal under investigation consists of two polytypes with a maximum degree of order. The two phases CaxSr1,,,xTeO3 (x = 0.55 and 0.77) are isostructural to the MDO1 polytype of ,-CaTeO3. ,-CaTeO3 shows a distinct reversible phase transition at ,,293,K. The low-temperature modification ,,-CaTeO3 as well as its high-temperature modification ,-CaTeO3 can be considered as threefold superstructures along [100] based on the MDO1 polytype of ,-CaTeO3. [source] | ||||||||||