Search results for "Crystallization"
showing 10 items of 774 documents
Pyrolysis study of sol-gel derived TiO2powders
2004
An amorphous TiO2 gel was obtained by hydrolysing titanium(IV) isopropoxide with a stoichiometric amount of water using SnCl2 as catalyst. In these operative conditions, a TiO2 gel matrix containing a lower fraction of organic residual was obtained with respect to samples prepared by previously modifying the titanium alkoxide precursor with chelating ligands. Dried gel powders were characterized by N2 adsorption analyses, FT-IR and XRD measurements. Thermogravimetric (TG) and differential thermal analysis (DTA) coupled with mass spectrometric (MS) and gas chromatographic (GC) measurements were performed in order to identify the organic products released from TiO2 gel pyrolysis. The Tg-MS se…
Microwave assisted synthesis and solid-state characterization of lithocholyl amides of isomeric aminopyridines
2011
Microwave (MW) assisted synthesis and solid state structural characterizations of novel lithocholyl amides of 2-, 3-, and 4-aminopyridine are reported. It is shown that the MW technique is a proper method in the preparation of N-lithocholyl amides of isomeric aminopyridines. It offers many advantages compared to conventional heating. The molecular and crystal structures as well as the polymorphic and hydrated forms of prepared conjugates with their thermodynamic stabilities have been characterized by means of high resolution liquid- and solid-state NMR spectroscopy, single crystal and powder X-ray diffraction, and thermogravimetric analysis. Owing to the many biological functions of bile ac…
Solvent Modulated Assembly of Two Ni(II) Complexes: Syntheses, Structures and Magnetic Properties
2016
A dinuclear [Ni2(L)2(DMSO)2(MeOH)2] (1) and a tetra-nuclear [Ni4(L)4(DMF)2(H2O)2].DMF (2) Ni(II) complexes have been prepared by treating nickel nitrate hexahydrate with the Schiff base ligand H2L (H2L=(E)-2-(2-hydroxybenzyliden)amino-4-nitrophenol) in a one-pot reaction. Complex 1 was obtained after recrystallization of the precipitate from the reaction with a 1:1:1 mixture of DMSO/CH2Cl2/MeOH. In contrast, the tetrameric complex 2 was obtained after slow evaporation of the filtrate. Both complexes were characterized by analytical, thermogravimetric, optical and magnetic techniques. The solid state molecular structures of 1 and 2 were determined by single crystal X-ray crystallography. Com…
Ca[Ag2(SCN)4]·2H2O
2004
Calcium tetrathiocyanatodiargentate(I) dihydrate, Ca[Ag(2)(SCN)(4)].2H(2)O, contains eight-membered Ag(4)S(4) rings bonded together through shared atoms to form layers parallel to (100). The thiocyanate groups link the layers to Ca-O chains running parallel to the c axis. The Ca atom is located on a twofold rotation axis parallel to b and is surrounded by four water molecules of crystallization and four thiocyanate N atoms in a distorted square antiprism.
The effect of ions at the surface of calcium oxalate monohydrate crystals on cell-crystal interactions
2003
Magnesium is an abundant ion in biologic systems, including renal tubular fluid; however, the precise role of magnesium during the interaction of calcium oxalate crystals with cells has not been previously defined. In addition, the respective roles of calcium and hydrogen ions during the cell-crystal bonding interaction remain poorly defined. Here we report an atomic level three-dimensional study of a single crystal of calcium oxalate monohydrate (COM; whewellite) which was bathed in a solution of magnesium hexahydrate for 1 year. Magnesium was not incorporated into the structure of whewellite to any significant degree. Instead, COM accepted magnesium primarily as an adsorbate in a binding …
Time-Gated Raman Spectroscopy for Quantitative Determination of Solid-State Forms of Fluorescent Pharmaceuticals
2018
Raman spectroscopy is widely used for quantitative pharmaceutical analysis, but a common obstacle to its use is sample fluorescence masking the Raman signal. Time-gating provides an instrument-based method for rejecting fluorescence through temporal resolution of the spectral signal and allows Raman spectra of fluorescent materials to be obtained. An additional practical advantage is that analysis is possible in ambient lighting. This study assesses the efficacy of time-gated Raman spectroscopy for the quantitative measurement of fluorescent pharmaceuticals. Time-gated Raman spectroscopy with a 128 X (2) X 4 CMOS SPAD detector was applied for quantitative analysis of ternary mixtures of sol…
Key Role of the Cation in the Crystallization of Chiral Tris(Anilato)Metalate Magnetic Anions
2015
A complete study of the role played by the usually considered “innocent” cation in the synthesis of chiral tris(anilato)metalate magnetic complexes is presented. This study is based on the rational synthesis of the family of compounds formulated as A3[MIII(C6O4X2)3] with A+ = [PPh3Et]+, [PPh3Pr]+, [PBu4]+, [NHep4]+, and [PPh4]+; MIII = CrIII, FeIII, and GaIII; and [C6O4X2]2– (X = Cl, Br, and NO2; [C6O4X2]2– = dianion of the 3,6-disubstituted derivatives of 2,5-dihydroxy-1,4-benzoquinone, H4C6O4). We show and explain the unexpected key role played by the cations in isolating chiral or achiral crystals of these [MIII(C6O4X2)3]3– anions with D3 point group symmetry. Thus, among the 18 new comp…
UV-induced solvent free synthesis of truxillic acid–bile acid conjugates
2009
The solvent free UV-induced [2 + 2] intermolecular cycloaddition of two molecules of 3α-cinnamic acid ester of methyl lithocholate produced in 99% yield of α- and e-truxillic acid-bis(methyl lithocholate) isomers, which possess two structurally different potential binding sites. A prerequisite for this effective solid state reaction is a proper self-assembled crystal structure of the starting conjugate crystallized from acetonitrile. The crystallization of cinnamic acid ester of methyl lithocholate from acetonitrile produces two different crystalline forms (polymorphs), which is the reason for the solid state formation of two isomers of truxillic acid-bis(methyl lithocholate).
Crystallization and preliminary X-ray analysis of strictosidine synthase and its complex with the substrate tryptamine
2005
Strictosidine synthase (STR1) is a central enzyme that participates in the biosynthesis of almost all plant monoterpenoid indole alkaloids. After heterologous expression in Escherichia coli, crystals of STR1 and its substrate complex with tryptamine were obtained by the hanging-drop technique at 302–304 K with potassium sodium tartrate tetrahydrate as precipitant. All crystals belong to space group R3. The native STR1 crystals diffract to 2.95 Å and have unit-cell parameters a = b = 150.3, c = 122.4 Å. The tryptamine complex crystals diffract to 2.38 Å, with unit-cell parameters a = b = 147.3, c = 122.3 Å.
Amorphous calcium carbonate in the shells of adult Unionoida
2011
Shells of adult individuals from two different bivalve families, Hyriopsis cumingii and Diplodon chilensis patagonicus, were studied by Micro-Raman spectroscopy and Focussed Ion Beam-assisted TEM. The shells contain amorphous calcium carbonate in a zone at the interface between the periostracum and the prismatic layer. In this area, the initial prism structures protrude from the inner periostracum layer and it is demonstrated that these structures systematically consist of highly disordered and amorphous calcium carbonate. Within this zone, ordered and disordered areas are intermingled discounting the existence of a crystallization front and favouring models of domainal crystallization proc…