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At least 235 records · Page 13Linked to original sources
PubMed2000

Wide spectral range nonlinear optical crystals of one-dimensional coordination solids [Et4N][Cd(SCN)3] and [Et4N][Cd(SeCN)3] and the general design criteria for [R4N][Cd(XCN)3] (Where R = Alkyl and X = S, Se, Te) as NLO crystals.

We report herein two new nonlinear optical (NLO) crystals, [Et4N][Cd(XCN)3], where X = S (1) and Se (2), that are transparent from 220 to 3300 nm, covering the entire near-ultraviolet, the visible, and the near-infrared spectral regions and giving rise to a very wide and continuous optical window, which is useful for many frequency conversion applications. Both 1 and 2 exhibit highly efficient second harmonic generation (SHG) as measured via the Kurtz-Perry method. The corresponding [Me4N]+ salts, [Me4N][Cd(XCN)3 where X = S (3) and Se (4), show no SHG effects. All four structures adopt noncentrosymmetric space groups (Cmc2(1) for 1 and 2 and Pna2(1) for 3 and presumably 4) and are based on one-dimensional anionic [Cd(XCN)3-] infinity zigzag chains. However, a detailed analysis of the structures of [R4N][Cd(XCN)3], where R = Et, Me and X = S, Se revealed that the difference in the second-order nonlinear responses of the Et4N+ salts (1 and 2) and the Me4N+ salts (3 and 4) is attributable to the relative alignment of the [Cd(XCN)3-] infinity zigzag chains, being parallel in the crystals of 1 and 2 but antiparallel in the crystals of 3 and 4. Also reported, for the first time, are the synthesis and crystal structure of [Et4N][Cd(SeCN)3] (2). Compound 2 crystallizes in an orthorhombic unit cell of Cmc21 space group symmetry with lattice parameters of 9.938(1) A, 16.868(2) A, 11.054(1) A, and Z = 4. Other issues related to the molecular and crystal engineering of this class of NLO materials are also discussed.

Journal Article↗
PubMed1986

Dependence of the coincidence aperture function of narrow BGO crystals on crystal shape and light encoding schemes.

Although the spatial resolution in positron emission tomography is improved by reducing the crystal width, the resolution becomes increasingly non-uniform towards the edges of the field of view. This is mainly due to penetration of the gamma rays through one or more crystals before detection and the inability of current systems to resolve the depth of interaction within the crystal. This paper compares crystals with straight and pointed tips with and without tungsten septa to determine the effects of pointed tips and septa on spatial resolution and efficiency. Monte Carlo calculations are compared with extensive experimental results obtained from 16 coincidence lines between two four-BGO crystal/dual PMT detector assemblies. The spectral efficiencies for the different combinations are compared. A modest improvement in signal-to-noise ratio at the maximum resolvable frequency is demonstrated when using tungsten septa and pointed crystals. The effects of the optical coding scheme used are discussed and it is shown that most coding schemes cause diminishment of spatial resolution even at the centre of the field of view, resulting from Compton scattering to adjacent crystals.

Electrons↗
PubMed2003

Tunable refraction effects in two-dimensional photonic crystals utilizing liquid crystals.

Tunable refraction effects in two-dimensional photonic crystals utilizing liquid crystals are theoretically demonstrated. Due to liquid crystals with anisotropies, the incident light propagates in photonic crystals at refractive angles different from those in photonic crystals composed of isotropic materials. Moreover, refractive angles can be changed by rotating the directors of liquid crystals. Tunable refraction effects are also discussed for the light with two kinds of frequencies: one is a frequency at the edge of a band gap, and the other is a frequency a little far from the edge of a band gap.

Journal Article↗
PubMed2005

Effect of pressure on the crystal structure of L-serine-I and the crystal structure of L-serine-II at 5.4 GPa.

The crystal structure of L-serine has been determined at room temperature at pressures between 0.3 and 4.8 GPa. The structure of this phase (hereafter termed L-serine-I), which consists of the molecules in their zwitterionic tautomer, is orthorhombic, space group P212121. The least compressible cell dimension (c), corresponds to chains of head-to-tail NH...carboxylate hydrogen bonds. The most compressible direction is along b, and the pressure-induced distortion in this direction takes the form of closing up voids in the middle of R-type hydrogen-bonded ring motifs. This occurs by a change in the geometry of hydrogen-bonded chains connecting the hydroxyl groups of the -CH2OH side chains. These hydrogen bonds are the longest conventional hydrogen bonds in the system at ambient pressure, having an O...O separation of 2.918 (4) A and an O...O...O angle of 148.5 (2) degrees ; at 4.8 GPa these parameters are 2.781 (11) and 158.5 (7) degrees . Elsewhere in the structure one NH...O interaction reaches an N...O separation of 2.691 (13) A at 4.8 GPa. This is amongst the shortest of this type of interaction to have been observed in an amino acid crystal structure. Above 4.8 GPa the structure undergoes a single-crystal-to-single-crystal phase transition to a hitherto uncharacterized polymorph, which we designate L-serine-II. The OH...OH hydrogen-bonded chains of L-serine-I are replaced in L-serine-II by shorter OH...carboxyl interactions, which have an O...O separation of 2.62 (2) A. This phase transition occurs via a change from a gauche to an anti conformation of the OH group, and a change in the NCalphaCO torsion angle from -178.1 (2) degrees at 4.8 GPa to -156.3 (10) degrees at 5.4 GPa. Thus, the same topology appears in both crystal forms, which explains why it occurs from one single-crystal form to another. The transition to L-serine-II is also characterized by the closing-up of voids which occur in the centres of other R-type motifs elsewhere in the structure. There is a marked increase in CH...O hydrogen bonding in both phases relative to L-serine-I at ambient pressure.

Crystallography↗
PubMed2005

The determination of the optimal length of crystal blanks in quartz crystal resonators.

It is well understood that the strong coupling of thickness-shear and flexural vibrations in piezoelectric crystal plates only occurs at specific length at which the vibration mode conversion, like the flexural mode gradually converting to thickness-shear mode while the thickness-shear mode converting to higher-order flexural mode, happens. It is important to avoid the strong coupling of modes in a crystal resonator that uses thickness-shear vibrations to enhance the energy trapping. To achieve such a design goal, the length of a crystal blank should be carefully chosen such that the coupling is at its weakest, which usually is in the middle of two strong coupling points. Through a closer examination of the frequency spectra, or the frequency-length relationship in this study, we can see that the strong coupling points appear periodically. This implies that we can find exact locations with the plate theory that predicts the resonance frequency. Based on this observation, we first use the first-order Mindlin plate theory with the precise thickness-shear frequency, which is normalized to one, to find corresponding wavenumbers. Then the length as a variable is solved from the coupled frequency equation for exact coupling points in a crystal plate of AT-cut quartz. The optimal length of a crystal blank in the simplest resonator model is calculated for the coupled thickness-shear, flexural, and extensional vibrations. The solutions and the method will be important in the determination of optimal length of a crystal blank in the resonator design process.

Computer Simulation↗
PubMed2005

Stress-induced crystal-to-crystal transformations in high-density polyethylene-layered silicate nano-composites: a spectroscopic study.

High-density polyethylene (HDPE)-clay nano-composites have been prepared using the melt intercalation technique. Organically modified montmorillonite at various loadings (0.5--7%) was used as a nano-additive. Fourier transform infrared spectroscopy (FT-IR) was utilized for the first time to monitor the stress-induced crystal-to-crystal transformations of the polyethylene matrix with respect to the clay loading as well as to the degree of mechanical strain. In addition, polarized infrared measurements revealed information on both the orientation and the stress-induced distortion of the crystals. It was concluded that the crystal-to-crystal transformations are hindered by the presence of the clay, which also prevented the crystals from orienting even at low clay loadings (1%). Finally, X-ray diffraction (XRD) and differential scanning calorimetry (DSC) measurements confirmed the presence of the stress-induced crystalline structures in agreement with the infrared measurements.

Hydrogen Bonding↗
PubMed1992

Observations on the structural features and characteristics of biological apatite crystals. 2. Observation on the ultrastructure of human enamel crystals.

In a series of studies to investigate the structural features of biological crystals, using an electron microscope, we examined the ultrastructure of human enamel crystals at near atomic resolution through the cross and longitudinal sections of the crystals. The materials used for this study were the middle layer of the noncarious enamel from freshly extracted human erupted permanent molars. The small cubes of the enamel were fixed in glutaraldehyde and osmium tetroxide and embedded in epoxy resin using the routine methods. The ultrathin sections were cut with a diamond knife without decalcification. The sections were examined with HITACHI H-500 and H-700 types of transmission electron microscopes operated at 125-200 kV. Each crystal was observed at the initial magnification of 300,000 times and at the final magnification of 10,000,000 times and over. Using this approach, the authors have been able to show the configuration of the hydroxyapatite in the cross and longitudinal sections of the enamel crystals and observe the basic hexagonal pattern of the unit cell viewed down the c-axis. The authors sincerely believe that the electron micrograph shown in this report is the first atomic image to be obtained from a hydroxyapatite crystal from the human enamel, using the sections.

Dental Enamel↗
PubMed1976

[Protein crystals and tubuli bundles in yeast cells. IV. Biochemical and electron microscopic studies of the induction of alcohol dehydrogenase (ADH) crystals].

Cells of Saccharomyces carlsbergensis H 60 synthesize alcohol dehydrogenase (ADH) in media containing 2% lactat, 1% ethanol or 0.1% glucose. Crystals may be induced in protoplasts of these cells. Increase of glucose concentration in the medium results in diminished ADH synthesis and decreased tendency for crystal formation. Repression of ADH synthesis by glucose results in the formation of a protein (MG 110000 D), the significance of which is discussed. Early stages of crystal formation inside the cell are demonstrated electronmicroscopically. At first dense material accumulates between opposite membranes of neighbouring mitochondria. Within mitochondria frequently membrane bundles occur in close vicinity to crystals. These ADH-crystals arise from this material.

Alcohol Oxidoreductases↗
PubMed2004

Thermodynamics of sublimation, crystal lattice energies, and crystal structures of racemates and enantiomers: (+)- and (+/-)-ibuprofen.

Thermodynamic differences between ibuprofen (IBP) racemate and the (+)-enantiomer were studied by X-ray diffraction, thermoanalysis, and crystal energy calculations. The thermodynamic functions of sublimation (as a measure of crystal lattice energy) were obtained by the transpiration method. The sublimation enthalpies (DeltaH(sub)) of (+/-)-IBP and (+)-IBP are 115.8 +/- 0.6 and 107.4 +/- 0.5 kJ. mol(-1), respectively. Using the temperature dependency of the saturated vapor pressure, the relative fractions of enthalpy and entropy of the sublimation process were calculated, and the sublimation process for both the racemate and the enantiomer was found to be enthalpy driven (62%). Two different force fields, Mayo et al. (M) and Gavezzotti (G), were used for comparative analysis of crystal lattice energies. Both force fields revealed that the van der Waals term contributes more to the packing energy in (+)-IBP than in (+/-)-IBP. The hydrogen bonding energy, however, contributes at 29.7 and 32.3% to the total crystal lattice energy in (+)-IBP and (+/-)-IBP (M), respectively. Furthermore, different structure fragments of the IBP molecule were analyzed with respect to their contribution to nonbonded van der Waals interactions. The effect of the C-H distance on the van der Waals term of the crystal lattice energy was also studied.

Crystallization↗
PubMed1981

Crystal structure and solid-state behavior of aspirin anhydride crystals.

The crystal structure and solid-state behavior of aspirin anhydride were determined using single-crystal X-ray techniques and microscopic examination of the reacting crystals. The crystal structure and solid-state conformation of aspirin anhydride were similar to those of related compounds. The crystal packing of aspirin anhydride allows the initial product of the solid-state reaction to be predicted; however, this prediction could not be tested because the thermal degradation products reported in the literature appear to be those obtained from reaction in a liquid state.

Anhydrides↗
PubMed2005

Crystal structure and morphology of poly(16-hexadecalactone) chain-folded lamellar crystals.

Solution-grown, chain-folded lamellar crystals of poly(16-hexadecalactone) (PHDL) were crystallized isothermally from 1-hexanol at 70 degrees C. The morphology of lozenge-shaped crystals was studied by TEM and AFM. The lamellae are ca. 10 nm thick and the chains run orthogonal to the lamellar surface with folding along (110) and (110) planes. The crystal structure of PHDL was determined by XRD and election diffraction of single crystals. The chains are in the 2(1) helix conformation close to all-trans and the structure consists of an orthorhombic unit cell with a P2(1)2(1)2(1) space group with the lattice constants a = 0.746 +/- 0.001 nm, b = 0.504 +/- 0.001 nm, and c (chain axis) = 4.116 +/- 0.003 nm. There are two chains per unit cell, which exist in an antiparallel arrangement. Molecular packing structure has been studied in detail, taking into account both diffraction data and energy calculations. The setting angles, with respect to a axis, were +/-40 degrees for the corner and center chains, respectively. By using the electron and XRD data, the best molecular packing model was refined to R-factors of 0.168 and 0.196, respectively. A brief comparison of chain-packing structure is also made with related polymer structures.

Crystallization↗
PubMed1998

Cadmium-induced crystallization of proteins: II. Crystallization of the Salmonella typhimurium histidine-binding protein in complex with L-histidine, L-arginine, or L-lysine.

To further investigate favorable effects of divalent cations on the formation of protein crystals, three complexes of Salmonella typhimurium histidine-binding protein were crystallized with varying concentrations of cadmium salts. For each of the three histidine-binding protein complexes, cadmium cations were found to promote or improve crystallization. The optimal cadmium concentration is ligand specific and falls within a narrow concentration range. In each case, crystals grown in the presence of cadmium diffract to better than 2.0 angstroms resolution and belong to the orthorhombic space group P2(1)2(1)2(1). From our results and from the analysis of cadmium sites in well-refined protein structures, we propose that cadmium addition provides a generally useful technique to modify crystal morphology and to improve diffraction quality.

Arginine↗
PubMed2001

Crystal structures of the peanut lectin-lactose complex at acidic pH: retention of unusual quaternary structure, empty and carbohydrate bound combining sites, molecular mimicry and crystal packing directed by interactions at the combining site.

The crystal structures of a monoclinic and a triclinic form of the peanut lectin-lactose complex, grown at pH 4.6, have been determined. They contain two and one crystallographically independent tetramers, respectively. The unusual "open" quaternary structure of the lectin, observed in the orthorhombic complex grown in neutral pH, is retained at the acidic pH. The sugar molecule is bound to three of the eight subunits in the monoclinic crystals, whereas the combining sites in four are empty. The lectin-sugar interactions are almost the same at neutral and acidic pH. A comparison of the sugar-bound and free subunits indicates that the geometry of the combining site is relatively unaffected by ligand binding. The combining site of the eighth subunit in the monoclinic crystals is bound to a peptide stretch in a loop from a neighboring molecule. The same interaction exists in two subunits of the triclinic crystals, whereas density corresponding to sugar exists in the combining sites of the other two subunits. Solution studies show that oligopeptides with sequences corresponding to that in the loop bind to the lectin at acidic pH, but only with reduced affinity at neutral pH. The reverse is the case with the binding of lactose to the lectin. A comparison of the neutral and acidic pH crystal structures indicates that the molecular packing in the latter is directed to a substantial extent by the increased affinity of the peptide loop to the combining site at acidic pH.

Carbohydrates↗
PubMed2000

Magnet used for protein crystallization: novel attempts to improve the crystal quality.

The accuracy of the structures of biological macromolecules determined by X-ray crystallography is of fundamental importance, both for the understanding of life processes and for medical applications. The resolution of the structure is thus critical, and is largely determined by the quality of single crystals. Here we report the results of applying a magnetic field and a magnetization force during growth of the snake muscle fructose-1,6-bisphosphatase and human estrogenic 17beta-hydroxysteroid dehydrogenase crystals. For both enzyme proteins, the quality of the crystals improved with repeated assay, and their data sets were collected at significantly higher resolutions. These results coincide with a mechanism involving the reduction of convection, due to both the hydrodynamics within a magnet and the partially reduced gravity induced by a magnetization force. The density difference between the crystal and solution becomes less significant, and the sedimentation speed of the crystals is also reduced in the presence of the magnetization force.

17-Hydroxysteroid Dehydrogenases↗
PubMed1994

Isolation and partial characterization of crystal matrix protein as a potent inhibitor of calcium oxalate crystal aggregation: evidence of activation peptide of human prothrombin.

In order to clarify the characteristics of crystal matrix protein (CMP), which exhibits a remarkable affinity for calcium oxalate crystals and may be important in stone pathogenesis, we have isolated CMP from macromolecular matrix substances of newly-formed calcium oxalate crystals. Purification of CMP consisted of calcium oxalate crystal formation, dissolution of crystals, electrodialysis, anion exchange chromatography and high-performance liquid chromatography. CMP showed the protein band of 31 kDa in sodium dodecyl sulfate-polyacrylamide gel electrophoresis. The N-terminal amino acid sequence of CMP was identical to that of human prothrombin. Both anti-CMP polyclonal antibody and anti-human prothrombin antibody cross-reacted well with human prothrombin and CMP in Western blotting. Its amino acid composition and its molecular weight of 31 kDa strongly suggest that CMP is the activation peptide of human prothrombin.

Adult↗
PubMedDate not supplied

Computer image analysis of two-dimensional crystals of beef heart NADH: ubiquinone oxidoreductase fragments. I. Comparison of crystal structures in various negative stains.

We investigated the structure of two-dimensional crystals from bovine heart mitochondrial NADH: ubiquinone oxidoreductase. A detailed description of uranyl acetate-stained crystals demonstrated that they are composed of fragments in a spatial arrangement according to space group P4212 [J. Brink, S. Hovmöller, C.I. Ragan, M.W.J. Cleeter, E.J. Boekema and E.F.J. van Bruggen, European J. Biochem. 166 (1987) 287]. To gain more structural information on the crystal structure and to assess the effects of various negative stains on the structure preservation and appearance, we examined stained crystals by means of electron microscopy and image analysis. The space group P4212 appeared to be present for several stains tested, i.e. ammonium molybdate, uranyl acetate, uranyl nitrate and uranyl sulphate. Use of phosphotungstic acid and silicotungstate resulted in a reduction of symmetry to pseudo-P4212 or p4. Use of sodium tungstate led to a considerable loss of resolution to 3.8 nm at best, whereas otherwise 1.5 to 1.9 nm could be demonstrated. The lattice vectors were not affected by the stains; they were determined as a = b = 14.9 +/- 0.25 nm with gamma = 89.8 degrees +/- 0.6 degrees. Image analysis showed the presence of similar structures with the molybdate and uranyl compounds. Differences were observed in the case of the tungstate type of stains. Furthermore, the analysis revealed the complete absence of the four small pores of 2.0 nm diameter in the unit cell. This effect was observed irrespective of the type of stain and supporting film, and could be ascribed only to the glow-discharge treatment of the supporting film. The observed difference must be caused by changed interactions between the protein, stain and supporting film. Application of correspondence analysis and clustering algorithms to the various reconstructed images of the crystals showed that they could be separated into several clusters. Each of these clusters corresponded on the average to only one type of stain, whereas a further division according to the specific uranyl compounds was observed. This study therefore shows that under identical preparation conditions subtle differences between individual stains can be detected.

Animals↗
PubMed2004

High-throughput crystallization: polymorphs, salts, co-crystals and solvates of pharmaceutical solids.

The concepts of high-throughput (HT) screening and combinatorial synthesis have been integrated into the pharmaceutical discovery process, but are not yet commonplace in the pharmaceutical development arena. Emerging strategies to speed pharmaceutical development and capture solid form diversity of pharmaceutical substances have resulted in the emergence of HT crystallization technologies. The primary type of diversity often refers to polymorphs, which are different crystal forms of the same chemical composition. However, diverse salt forms, co-crystals, hydrates and solvates are also amenable to study in HT crystallization systems. The impact of form diversity encompasses issues of stability and bioavailability, as well as development considerations such as process definition, formulation design, patent protection and regulatory control. This review highlights the opportunities and challenges of HT crystallization technologies as they apply to pharmaceutical research and development.

Chemistry, Pharmaceutical↗
PubMed2004

Crystal structures of the group II chaperonin from Thermococcus strain KS-1: steric hindrance by the substituted amino acid, and inter-subunit rearrangement between two crystal forms.

The crystal structures of the group II chaperonins consisting of the alpha subunit with amino acid substitutions of G65C and/or I125T from the hyperthermophilic archaeum Thermococcus strain KS-1 were determined. These mutants have been shown to be active in ATP hydrolysis but inactive in protein folding. The structures were shown to be double-ring hexadecamers in an extremely closed form, which was consistent with the crystal structure of native alpha8beta8-chaperonin from Thermoplasma acidophilum. Comparisons of the present structures with the atomic structures of the GroEL14-GroES7-(ADP)7 complex revealed that the deficiency in protein-folding activity with the G65C amino acid substitution is caused by the steric hindrance of the local conformational change in an equatorial domain. We concluded that this mutant chaperonin with G65C substitution is deprived of the smooth conformational change in the refolding-reaction cycle. We obtained a new form of crystal with a distinct space group at a lower concentration of sulfate ion in the presence of nucleotide. The crystal structure obtained at the lower concentration of sulfate ion tilts outward, and has much looser inter-subunit contacts compared with those in the presence of a higher concentration of sulfate ion. Such subunit rotation has never been characterized in group II chaperonins. The crystal structure obtained at the lower concentration of sulfate ion tilts outward, and has much looser inter-subunit contacts compared with those in the presence of a higher concentration of sulfate ion.

Adenosine Triphosphate↗