Synthesis and Structural Characterization of Bis(aziridine) Cobalt(II), Zinc(II) and Palladium(II) Complexes

2007 ◽  
Vol 62 (8) ◽  
pp. 1095-1101 ◽  
Author(s):  
J. Nicolas Roedel ◽  
Roman Bobka ◽  
Max Pfister ◽  
Martin Rieger ◽  
Bernd Neumann ◽  
...  
Keyword(s):  
Solid State ◽  
Molar Ratio ◽  
Tetrahedral Coordination ◽  
X Ray Diffraction ◽  
Metal Chlorides ◽  
X Ray ◽  
Square Planar ◽  
Solid State Structures ◽  
Planar Geometries

The reactions of anhydrous metal chlorides MCl2 [M = Co(II), Zn(II), Pd(II)] with aziridines (az) in CH2Cl2 at r. t. in a 1 : 5 molar ratio afforded the bis(aziridine)dichloro complexes M(az)2Cl2. After purification, all complexes were fully characterized. The solid state structures were determined using single crystal X-ray diffraction, and showed tetrahedral coordination geometries for the Co(II) and Zn(II) centers and trans-configurated square planar geometries for Pd(II).

Unprecedented transformation of [I−·I3−] to [I42−] polyiodides in the solid state: structures, phase transitions and characterization of dipyrazolium iodide triiodide

2015 ◽  
Vol 44 (42) ◽  
pp. 18447-18458 ◽  
Author(s):  
M. Węcławik ◽  
P. Szklarz ◽  
W. Medycki ◽  
R. Janicki ◽  
A. Piecha-Bisiorek ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Phase Transitions ◽  
Solid State ◽  
Dielectric Measurements ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Solid State Structures

Dipyrazolium iodide triiodide, [C3N2H5+]2[I−·I3−], has been synthesized and studied by means of X-ray diffraction, differential scanning calorimetry, dielectric measurements, and UV-Vis spectroscopy.

Characterization of some mesogenic alkyl 1-thioglycosides

2002 ◽  
Vol 80 (8) ◽  
pp. 1162-1165 ◽  
Author(s):  
B Henrissat ◽  
G K Hamer ◽  
M G Taylor ◽  
R H Marchessault
Keyword(s):  
Phase Transition ◽  
Liquid Crystal ◽  
Solid State ◽  
Solid State Nmr ◽  
Liquid Crystalline ◽  
Liquid Crystal Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Liquid Crystalline Phases

A series of dodecyl 1-thio-β-D-glycosides has been synthesized and characterized (DSC, NMR, CP MAS, X-ray diffraction) as possible new marking materials with liquid-crystalline properties. These compounds undergo solid to liquid crystal phase transitions at various temperatures, which depend on the nature of the carbohydrate part of the structure. Their liquid-crystalline phases show extreme shear thinning behaviour.Key words: liquid crystal, powder X-ray diffraction, phase transition, thioglycoside, solid-state NMR, marking material

scholarly journals Characterization of a brazilian smectite by solid state NMR and X-ray diffraction techniques

1997 ◽  
Vol 8 (6) ◽  
pp. 581-586 ◽  
Author(s):  
Alcides Wagner Serpa Guarino ◽  
Rosane A. S. San Gil ◽  
Helena Polivanov ◽  
Sonia M.C. Menezes
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals Making and Characterization of Limnpo4 Using Solid State Reaction Method for Lithium Ion Battery Cathodes

2019 ◽  
pp. 583-588
Author(s):  
Adelyna Oktavia ◽  
Kurnia Sembiring ◽  
Slamet Priyono
Keyword(s):  
Solid State ◽  
Lithium Ion Battery ◽  
Lithium Ion ◽  
Solid State Reaction Method ◽  
Raw Material ◽  
X Ray Diffraction ◽  
Solid State Method ◽  
X Ray ◽  
General Investigation

Hospho-material of olivine, LiMnPO4 identified as promising for cathode material generation next Lithium-ion battery and has been successfully synthesized by solid-state method with Li2Co3, 2MnO2, 2NH4H2PO4 as raw material. The influence of initial concentration of precursors at kalsinasi temperatures (400-800 ° C) flows with nitrogen. The purity and composition phase verified by x-ray diffraction analysis (XRD), scanning electron microscopy (SEM), spectroscopy, energy Dispersive x-ray Analysis (EDS), Raman spectra. General investigation shows that there is a correlation between the concentration of precursors, the temperature and the temperature of sintering kalsinasi that can be exploited to design lithium-ion next generation.

scholarly journals Bis(dicarbollide) Complexes of Transition Metals as a Platform for Molecular Switches. Study of Complexation of 8,8′-Bis(methylsulfanyl) Derivatives of Cobalt and Iron Bis(dicarbollides)

Molecules ◽  
2020 ◽  
Vol 25 (23) ◽  
pp. 5745
Author(s):  
Sergey A. Anufriev ◽  
Sergey V. Timofeev ◽  
Alexei A. Anisimov ◽  
Kyrill Yu. Suponitsky ◽  
Igor B. Sivaev
Keyword(s):  
Solid State ◽  
Transition Metal ◽  
Molecular Switches ◽  
X Ray Diffraction ◽  
Chelate Complexes ◽  
X Ray ◽  
Complexes Of Transition Metals ◽  
Silver Palladium ◽  
Solid State Structures ◽  
Derivatives Of

Complexation of the 8,8′-bis(methylsulfanyl) derivatives of cobalt and iron bis(dicarbollides) [8,8′-(MeS)2-3,3′-M(1,2-C2B9H10)2]− (M = Co, Fe) with copper, silver, palladium and rhodium leads to the formation of the corresponding chelate complexes, which is accompanied by a transition from the transoid to the cisoid conformation of the bis(dicarbollide) complex. This transition is reversible and can be used in design of coordination-driven molecular switches based on transition metal bis(dicarbollide) complexes. The solid-state structures of {(Ph3P)ClPd[8,8′- (MeS)2-3,3′-Co(1,2-C2B9H10)2-κ2-S,S′]} and {(COD)Rh[8,8′-(MeS)2-3,3′-Co(1,2-C2B9H10)2-κ2-S,S′]} were determined by single crystal X-ray diffraction.

Stability of sodalite relative to nepheline in NaCl–H2O brines at 750 °C: Implications for hydrothermal formation of sodalite

2020 ◽  
Vol 58 (1) ◽  
pp. 3-18 ◽  
Author(s):  
Jonathan B. Schneider ◽  
David M. Jenkins
Keyword(s):  
Infrared Spectroscopy ◽  
Constant Temperature ◽  
Molar Ratio ◽  
Standard State ◽  
X Ray Diffraction ◽  
Cage Structure ◽  
X Ray ◽  
Brine Concentration

ABSTRACT Formation of the feldspathoid sodalite (Na6Al6Si6O24·2NaCl) by reaction of nepheline (NaAlSiO4) with NaCl-bearing brines was investigated at 3 and 6 kbar and at a constant temperature of 750 °C to determine the brine concentration at which sodalite forms with variation in pressure. The reaction boundary was located by reaction-reversal experiments in the system NaAlSiO4–NaCl–H2O at a brine concentration of 0.16 ± 0.08 XNaCl [= molar ratio NaCl/(NaCl + H2O)] at 3 kbar and at a brine concentration of 0.35 ± 0.03 XNaCl at 6 kbar. Characterization of the sodalite using both X-ray diffraction and infrared spectroscopy after treatment in these brines indicated no obvious evidence of water or hydroxyl incorporation into the cage structure of sodalite. The data from this study were combined with earlier results by Wellman (1970) and Sharp et al. (1989) at lower (1–1.5 kbar) and higher (7–8 kbar) pressures, respectively, on sodalite formation from nepheline and NaCl which models as a concave-down curve in XNaCl – P space. In general, sodalite buffers the concentration of neutral aqueous NaCl° in the brine to relatively low values at P < 4 kbar, but NaCl° increases rapidly at higher pressures. Thermochemical modeling of these data was done to determine the activity of the aqueous NaCl° relative to a 1 molal (m) standard state, demonstrating very low activities (<0.2 m, or 1.2 wt.%) of NaCl° at 3 kbar and lower, but rising to relatively high activities (>20 m, or 54 wt.%) of NaCl° at 6 kbar or higher. The results from this study place constraints on the concentration of NaCl° in brines coexisting with nepheline and sodalite and, because of the relative insensitivity of this reaction to temperature, can provide a convenient geobarometer for those localities where the fluid compositions that formed nepheline and sodalite can be determined independently.

Imidazole-containing Bispidine Ligands: Synthesis, Structure and Cu(II) Complexation

2011 ◽  
Vol 66 (7) ◽  
pp. 721-728 ◽  
Author(s):  
Martin Walther ◽  
Madlen Matterna ◽  
Stefanie Juran ◽  
Silke Fähnemann ◽  
Holger Stephan ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Enol Form ◽  
Trans Configuration ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Impact ◽  
Configurational Isomerism

The preparation and characterization of tris-pyridyl bispidine (3,7-diazabicyclo[3.3.1]nonane) derivatives with benzimidazole and imidazole donor groups at the N-3 position of the bispidine skeleton and their copper(II) complexes are reported. The impact of the hetaryl substituents on the configurational isomerism of piperidones and their corresponding bispidones has been studied by NMR spectroscopy, revealing the exclusive appearance in the enol form for the piperidones in solution and the trans-configuration regarding the two pyridyl substituents, as well as the sole formation of the unsymmetric exo-endo isomers for the corresponding bispidones. Thus, the bispidones are preorganized ligands for building pentacoordinated complexes, confirmed by the preparation and characterization of the corresponding Cu(II) complexes. Of the di-pyridyl piperidones with benzimidazole and imidazole substituents, and of the Cu(II) complex of the benzimidazole-containing bispidone, crystals have become available for the analysis by X-ray diffraction, showing that the piperidones form the enol tautomers also in the solid state.

Structural Characterization of a Plutonium Sequestering Agent Complex by Synchrotron X-Ray Diffraction

2006 ◽  
Vol 986 ◽  
Author(s):  
Anne E. V. Gorden ◽  
G. Szigethy ◽  
D. K. Shuh ◽  
B. E. F. Tiedemann ◽  
J. Xu ◽  
...  
Keyword(s):  
National Laboratory ◽  
Selective Extraction ◽  
Biological Transport ◽  
X Ray Diffraction ◽  
X Ray ◽  
Selective Ligand ◽  
Detailed Evaluation ◽  
Biomimetic Approach ◽  
Solid State Structures

AbstractNew ligands and materials are required that can coordinate, sense, and purify actinides for selective extraction and reduction of toxic, radioactive wastes from the mining and purification of actinides. The similarities in the chemical, biological transport, and distribution properties of Fe(III) and Pu(IV) inspired a biomimetic approach to the development of sequestering agents for actinides. A detailed evaluation of the structure and bonding of actinide coordinating ligands like these is important for the design of new selective ligand systems. Knowing the difficulty with working with the crystals resulting from these ligand systems and safe handling considerations for working with Pu, procedures were developed that utilize the Advanced Light Source of Lawrence Berkeley National Laboratory to determine the solid-state structures of Pu complexes by X-ray diffraction.

Synthesis and Characterization of 3Y-TZP by Gel Solid-State Method

2011 ◽  
Vol 412 ◽  
pp. 61-64
Author(s):  
Xiao Bo Wu ◽  
Da Zhi Sun ◽  
Dan Yu Jiang ◽  
Hai Fang Xu ◽  
De Xin Huang ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
Solid State ◽  
Sintering Behavior ◽  
X Ray Diffraction ◽  
Solid State Method ◽  
X Ray ◽  
Powder Particles ◽  
State Method ◽  
Average Size

3Y-TZP powder has been successfully synthesized by gel solid-state method. The structural phases of powder particles were analyzed by X-ray diffraction and the morphology was analyzed by scanning electron microscopy. The average size of grains was 230 nm. The sintering behavior, mechanical properties and microstructure of 3Y-TZP ceramics sintered by this powder were investigated. The experiment results showed that the mechanical properties of ceramics were excellent.

Copper(II) Complexes of a Tripyridyl Ligand: Anion-Dependent Metallosupramolecular Structures

2013 ◽  
Vol 66 (11) ◽  
pp. 1447 ◽  
Author(s):  
James E. M. Lewis ◽  
James D. Crowley
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Coordination Polymer ◽  
Elemental Analysis ◽  
Spectroscopic Properties ◽  
Nitrate Salt ◽  
X Ray Diffraction ◽  
X Ray ◽  
Salt Structure ◽  
Solid State Structures

A series of copper(ii) complexes of the ligand 2,6-bis(pyridin-3-ylethynyl)pyridine have been synthesised and characterised by 1H and DOSY NMR, IR and UV-Vis spectroscopies, mass spectrometry, elemental analysis and single crystal X-ray diffraction. In solution these systems display almost identical spectroscopic properties, however the solid state structures are shown to vary widely, depending upon the choice of anion. The tetrafluoroborate salt was revealed to be a discrete Cu2L4 cage-like helicate. The tosylate salt, whilst of the same Cu2L4 stoichiometry, was shown to be a coordination polymer. Finally the nitrate salt structure was observed to be a discrete Cu2L2 metallocycle.

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