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  • Essen : Verl. Glückauf
  • International Union of Crystallography (IUCr)
  • Krefeld : Geologischer Dienst Nordhein-Westfalen
  • 2010-2014  (32)
  • 2005-2009  (3)
  • 1970-1974  (4,538)
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  • 1
    Publication Date: 2014-04-08
    Description: Human carbonic anhydrases (CAs) are zinc metalloenzymes that catalyze the hydration and dehydration of CO2 and HCO3−, respectively. The reaction follows a ping-pong mechanism, in which the rate-limiting step is the transfer of a proton from the zinc-bound solvent (OH−/H2O) in/out of the active site via His64, which is widely believed to be the proton-shuttling residue. The decreased catalytic activity (∼20-fold lower with respect to the wild type) of a variant of CA II in which His64 is replaced with Ala (H64A CA II) can be enhanced by exogenous proton donors/acceptors, usually derivatives of imidazoles and pyridines, to almost the wild-type level. X-ray crystal structures of H64A CA II in complex with four imidazole derivatives (imidazole, 1-methylimidazole, 2-methylimidazole and 4-methylimidazole) have been determined and reveal multiple binding sites. Two of these imidazole binding sites have been identified that mimic the positions of the `in' and `out' rotamers of His64 in wild-type CA II, while another directly inhibits catalysis by displacing the zinc-bound solvent. The data presented here not only corroborate the importance of the imidazole side chain of His64 in proton transfer during CA catalysis, but also provide a complete structural understanding of the mechanism by which imidazoles enhance (and inhibit when used at higher concentrations) the activity of H64A CA II.
    Keywords: human carbonic anhydraseH64Aactivity enhancementrescueactivationimidazole
    Electronic ISSN: 2052-2525
    Topics: Geosciences , Physics
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  • 2
    Publication Date: 2014-04-08
    Description: Phosphatases function in the production, transport and recycling of inorganic phosphorus, which is crucial for cellular metabolism and bioenergetics, as well as in bacterial killing, since they are able to generate reactive oxygen species via Fenton chemistry. Diphosphonucleotide phosphatase/phosphodiesterase (PPD1), a glycoprotein plant purple acid phosphatase (PAP) from yellow lupin seeds, contains a bimetallic Fe–Mn catalytic site which is most active at acidic pH. Unlike other plant PAPs, PPD1 cleaves the pyrophosphate bond in diphosphonucleotides and the phosphodiester bond in various phosphodiesters. The homohexameric organization of PPD1, as revealed by a 1.65 Å resolution crystal structure and confirmed by solution X-ray scattering, is unique among plant PAPs, for which only homodimers have previously been reported. A phosphate anion is bound in a bidentate fashion at the active site, bridging the Fe and Mn atoms in a binding mode similar to that previously reported for sweet potato PAP, which suggests that common features occur in their catalytic mechanisms. The N-terminal domain of PPD1 has an unexpected and unique fibronectin type III-like fold that is absent in other plant PAPs. Here, the in vitro DNA-cleavage activity of PPD1 is demonstrated and it is proposed that the fibronectin III-like domain, which `overhangs' the active site, is involved in DNA selectivity, binding and activation. The degradation of DNA by PPD1 implies a role for PPD1 in plant growth and repair and in pathogen defence.
    Keywords: purple acid phosphatasediphosphonucleotide phosphatasephosphodiesterasePPD1bimetallic Fe–Mnfibronectin type III domaincrystal structureSAXS
    Electronic ISSN: 2052-2525
    Topics: Geosciences , Physics
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  • 3
    Publication Date: 2014-04-08
    Description: Acemetacin (ACM) is a non-steroidal anti-inflammatory drug (NSAID), which causes reduced gastric damage compared with indomethacin. However, acemetacin has a tendency to form a less soluble hydrate in the aqueous medium. We noted difficulties in the preparation of cocrystals and salts of acemetacin by mechanochemical methods, because this drug tends to form a hydrate during any kind of solution-based processing. With the objective to discover a solid form of acemetacin that is stable in the aqueous medium, binary adducts were prepared by the melt method to avoid hydration. The coformers/salt formers reported are pyridine carboxamides [nicotinamide (NAM), isonicotinamide (INA), and picolinamide (PAM)], caprolactam (CPR), p-aminobenzoic acid (PABA), and piperazine (PPZ). The structures of an ACM–INA cocrystal and a binary adduct ACM–PABA were solved using single-crystal X-ray diffraction. Other ACM cocrystals, ACM–PAM and ACM–CPR, and the piperazine salt ACM–PPZ were solved from high-resolution powder X-ray diffraction data. The ACM–INA cocrystal is sustained by the acid...pyridine heterosynthon and N—H...O catemer hydrogen bonds involving the amide group. The acid...amide heterosynthon is present in the ACM–PAM cocrystal, while ACM–CPR contains carboxamide dimers of caprolactam along with acid–carbonyl (ACM) hydrogen bonds. The cocrystals ACM–INA, ACM–PAM and ACM–CPR are three-dimensional isostructural. The carboxyl...carboxyl synthon in ACM–PABA posed difficulty in assigning the position of the H atom, which may indicate proton disorder. In terms of stability, the salts were found to be relatively stable in pH 7 buffer medium over 24 h, but the cocrystals dissociated to give ACM hydrate during the same time period. The ACM–PPZ salt and ACM–nicotinamide cocrystal dissolve five times faster than the stable hydrate form, whereas the ACM–PABA adduct has 2.5 times faster dissolution rate. The pharmaceutically acceptable piperazine salt of acemetacin exhibits superior stability, faster dissolution rate and is able to overcome the hydration tendency of the reference drug.
    Keywords: cocrystalhydratemelt crystallizationpiperazinepowder X-ray diffractionstructure determination from powder data (SDPD)
    Electronic ISSN: 2052-2525
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  • 4
    Publication Date: 2014-04-08
    Description: Crystal structure determinations of biological macromolecules are limited by the availability of sufficiently sized crystals and by the fact that crystal quality deteriorates during data collection owing to radiation damage. Exploiting a micrometre-sized X-ray beam, high-precision diffractometry and shutterless data acquisition with a pixel-array detector, a strategy for collecting data from many micrometre-sized crystals presented to an X-ray beam in a vitrified suspension is demonstrated. By combining diffraction data from 80 Trypanosoma brucei procathepsin B crystals with an average volume of 9 µm3, a complete data set to 3.0 Å resolution has been assembled. The data allowed the refinement of a structural model that is consistent with that previously obtained using free-electron laser radiation, providing mutual validation. Further improvements of the serial synchrotron crystallography technique and its combination with serial femtosecond crystallography are discussed that may allow the determination of high-resolution structures of micrometre-sized crystals.
    Keywords: protein microcrystallographyserial crystallographyin vivo grown microcrystals
    Electronic ISSN: 2052-2525
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  • 5
    Publication Date: 2014-04-08
    Description: X-ray diffraction patterns from two-dimensional (2-D) protein crystals obtained using femtosecond X-ray pulses from an X-ray free-electron laser (XFEL) are presented. To date, it has not been possible to acquire transmission X-ray diffraction patterns from individual 2-D protein crystals due to radiation damage. However, the intense and ultrafast pulses generated by an XFEL permit a new method of collecting diffraction data before the sample is destroyed. Utilizing a diffract-before-destroy approach at the Linac Coherent Light Source, Bragg diffraction was acquired to better than 8.5 Å resolution for two different 2-D protein crystal samples each less than 10 nm thick and maintained at room temperature. These proof-of-principle results show promise for structural analysis of both soluble and membrane proteins arranged as 2-D crystals without requiring cryogenic conditions or the formation of three-dimensional crystals.
    Keywords: two-dimensional protein crystalfemtosecond crystallographysingle layer X-ray diffractionmembrane protein
    Electronic ISSN: 2052-2525
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  • 6
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-04-08
    Keywords: biological crystallographyeditorialIUCrJ
    Electronic ISSN: 2052-2525
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  • 7
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-04-08
    Keywords: protein microcrystallographyserial crystallographyin vivo-grown microcrystals
    Electronic ISSN: 2052-2525
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  • 8
    Publication Date: 2014-04-08
    Description: The harmonic model of atomic nuclear motions is usually enough for multipole modelling of high-resolution X-ray diffraction data; however, in some molecular crystals, such as 1-(2′-aminophenyl)-2-methyl-4-nitro-1H-imidazole [Paul, Kubicki, Jelsch et al. (2011). Acta Cryst. B67, 365–378], it may not be sufficient for a correct description of the charge-density distribution. Multipole refinement using harmonic atom vibrations does not lead to the best electron density model in this case and the so-called `shashlik-like' pattern of positive and negative residual electron density peaks is observed in the vicinity of some atoms. This slight disorder, which cannot be modelled by split atoms, was solved using third-order anharmonic nuclear motion (ANM) parameters. Multipole refinement of the experimental high-resolution X-ray diffraction data of 1-(2′-aminophenyl)-2-methyl-4-nitro-1H-imidazole at three different temperatures (10, 35 and 70 K) and a series of powder diffraction experiments (20 ≤ T ≤ 300 K) were performed to relate this anharmonicity observed for several light atoms (N atoms of amino and nitro groups, and O atoms of nitro groups) to an isomorphic phase transition reflected by a change in the b cell parameter around 65 K. The observed disorder may result from the coexistence of domains of two phases over a large temperature range, as shown by low-temperature powder diffraction.
    Keywords: anharmonicityisomorphic phase transitionexperimental charge densityX-ray closed-circuit helium cryostatHansen–Coppens modelmultiple-temperature powder diffraction
    Electronic ISSN: 2052-2525
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  • 9
    Publication Date: 2014-04-08
    Description: The partitioning of space with Hirshfeld surfaces enables the analysis of fingerprint molecular interactions in crystalline environments. This study uses the decomposition of the crystal contact surface between pairs of interacting chemical species to derive an enrichment ratio. This quantity enables the analysis of the propensity of chemical species to form intermolecular interactions with themselves and other species. The enrichment ratio is obtained by comparing the actual contacts in the crystal with those computed as if all types of contacts had the same probability to form. The enrichments and contact tendencies were analyzed in several families of compounds, based on chemical composition and aromatic character. As expected, the polar contacts of the type H...N, H...O and H...S, which are generally hydrogen bonds, show enrichment values larger than unity. O...O and N...N contacts are impoverished while H...H interactions display enrichment ratios which are generally close to unity or slightly lower. In aromatic compounds, C...C contacts can display large enrichment ratios due to extensive π...π stacking in the crystal packings of heterocyclic compounds. C...C contacts are, however, less enriched in pure (C,H) hydrocarbons as π...π stacking is not so favourable from the electrostatic point of view compared with heterocycles. C...H contacts are favoured in (C,H) aromatics, but these interactions occur less in compounds containing O, N or S as some H atoms are then involved in hydrogen bonds. The study also highlights the fact that hydrogen is a prefered interaction partner for fluorine.
    Keywords: enrichment ratioHirshfeld surface analysiscrystal packingfingerprint plots
    Electronic ISSN: 2052-2525
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  • 10
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Keywords: Editorialchemical crystallographycrystal engineering
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  • 11
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Description: The crystallographic structure solution of nucleotides and nucleotide complexes is now commonplace. The resulting electron-density maps are often poorer than for proteins, and as a result interpretation in terms of an atomic model can require significant effort, particularly in the case of large structures. While model building can be performed automatically, as with proteins, the process is time-consuming, taking minutes to days depending on the software and the size of the structure. A method is presented for the automatic building of nucleotide chains into electron density which is fast enough to be used in interactive model-building software, with extended chain fragments built around the current view position in a fraction of a second. The speed of the method arises from the determination of the `fingerprint' of the sugar and phosphate groups in terms of conserved high-density and low-density features, coupled with a highly efficient scoring algorithm. Use cases include the rapid evaluation of an initial electron-density map, addition of nucleotide fragments to prebuilt protein structures, and in favourable cases the completion of the structure while automated model-building software is still running. The method has been incorporated into the Coot software package.
    Keywords: nucleic acid chain tracingCoot
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  • 12
    Publication Date: 2014-11-12
    Description: Accurate structural models of reaction centres in zeolite catalysts are a prerequisite for mechanistic studies and further improvements to the catalytic performance. The Rietveld/maximum entropy method is applied to synchrotron powder X-ray diffraction data on fully dehydrated CHA-type zeolites with and without loading of catalytically active Cu2+ for the selective catalytic reduction of NOx with NH3. The method identifies the known Cu2+ sites in the six-membered ring and a not previously observed site in the eight-membered ring. The sum of the refined Cu occupancies for these two sites matches the chemical analysis and thus all the Cu is accounted for. It is furthermore shown that approximately 80% of the Cu2+ is located in the new 8-ring site for an industrially relevant CHA zeolite with Si/Al = 15.5 and Cu/Al = 0.45. Density functional theory calculations are used to corroborate the positions and identity of the two Cu sites, leading to the most complete structural description of dehydrated silicoaluminate CHA loaded with catalytically active Cu2+ cations.
    Keywords: CHA zeolitescatalytic activitylocation of Cu2+synchrotron powder X-ray diffractionRietveld/maximum entropy method
    Electronic ISSN: 2052-2525
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  • 13
    Publication Date: 2014-11-12
    Description: Crystallographic auto-indexing algorithms provide crystal orientations and unit-cell parameters and assign Miller indices based on the geometric relations between the Bragg peaks observed in diffraction patterns. However, if the Bravais symmetry is higher than the space-group symmetry, there will be multiple indexing options that are geometrically equivalent, and hence many ways to merge diffraction intensities from protein nanocrystals. Structure factor magnitudes from full reflections are required to resolve this ambiguity but only partial reflections are available from each XFEL shot, which must be merged to obtain full reflections from these `stills'. To resolve this chicken-and-egg problem, an expectation maximization algorithm is described that iteratively constructs a model from the intensities recorded in the diffraction patterns as the indexing ambiguity is being resolved. The reconstructed model is then used to guide the resolution of the indexing ambiguity as feedback for the next iteration. Using both simulated and experimental data collected at an X-ray laser for photosystem I in the P63 space group (which supports a merohedral twinning indexing ambiguity), the method is validated.
    Keywords: indexing ambiguityserial femtosecond crystallography (SFX)XFELsprotein crystallographyexpectation maximization algorithm
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  • 14
    Publication Date: 2014-11-12
    Description: The time evolution of the electron density and the resulting time dependence of Fourier components of the X-ray polarizability of a crystal irradiated by highly intense femtosecond pulses of an X-ray free-electron laser (XFEL) is investigated theoretically on the basis of rate equations for bound electrons and the Boltzmann equation for the kinetics of the unbound electron gas. The photoionization, Auger process, electron-impact ionization, electron–electron scattering and three-body recombination have been implemented in the system of rate equations. An algorithm for the numerical solution of the rate equations was simplified by incorporating analytical expressions for the cross sections of all the electron configurations in ions within the framework of the effective charge model. Using this approach, the time dependence of the inner shell populations during the time of XFEL pulse propagation through the crystal was evaluated for photon energies between 4 and 12 keV and a pulse width of 40 fs considering a flux of 1012 photons pulse−1 (focusing on a spot size of ∼1 µm). This flux corresponds to a fluence ranging between 0.8 and 2.4 mJ µm−2. The time evolution of the X-ray polarizability caused by the change of the atomic scattering factor during the pulse propagation is numerically analyzed for the case of a silicon crystal. The time-integrated polarizability drops dramatically if the fluence of the X-ray pulse exceeds 1.6 mJ µm−2.
    Keywords: femtosecond pulseX-ray diffractionpolarizabilityelectron densityrate equations
    Electronic ISSN: 2052-2525
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  • 15
    Publication Date: 2014-11-12
    Description: Melting of native tapioca starch granules in aqueous pastes upon heating is observed in situ using simultaneous small- and wide-angle X-ray scattering (SAXS/WAXS) and solution viscometry. Correlated structure and viscosity changes suggest closely associated amylose and amylopectin chains in the semicrystalline layers, and the release of amylose chains for enhanced solution viscosity occurs largely after melting of the semicrystalline structure. Before melting, WAXS results reveal mixed crystals of A- and B-types (∼4:1 by weight), whereas SAXS results indicate that the semicrystalline layers are composed of lamellar blocklets of ca 43 nm domain size, with polydisperse crystalline (≃7.5 nm) and amorphous (≃1.1 nm) layers alternatively assembled into a lamellar spacing of ≃8.6 nm with 20% polydispersity. Upon melting, the semicrystalline lamellae disintegrate into disperse and molten amylopectin nanoclusters with dissolved and partially untangled amylose chains in the aqueous matrix which leads to increased solution viscosity. During subsequent cooling, gelation starts at around 347 K; successively increased solution viscosity coincides with the development of nanocluster aggregation to a fractal dimension ≃2.3 at 303 K, signifying increasing intercluster association through collapsed amylose chains owing to decreased solvency of the aqueous medium with decreasing temperature.
    Keywords: tapioca starch granulesgelatinizationgelationSAXS/WAXSviscosity
    Electronic ISSN: 2052-2525
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  • 16
    Publication Date: 2014-11-12
    Description: Molecular self-assembly of nylon-12 rods in self-organized nanoporous alumina cylinders with two different diameters (65 and 300 nm) is studied with transmission electron microscopy (TEM) and wide-angle X-ray diffraction (WAXD) in symmetrical reflection mode. In a rod with a 300 nm diameter, the tendency of the hydrogen-bonding direction of a γ-form crystal parallel to the long axis of the rod is not clear because of weak two-dimensional confinement. In a rod with a diameter of 65 nm, the tendency of the hydrogen-bonding direction of a γ-form crystal parallel to the long axis of the rod is more distinct because of strong two-dimensional confinement. For the first time, selected-area electron diffraction (SAED) is applied in a transmission electron microscope to a polymer nanorod in order to determine the hydrogen-bond sheet and lamellar orientations. Results of TEM–SAED and WAXD showed that the crystals within the rod possess the γ-form of nylon-12 and that the b axis (stem axis) of the γ-form crystals is perpendicular to the long axis of the rod. These results revealed that only lamellae with 〈h0l〉 directions are able to grow inside the nanopores and the growth of lamellae with 〈hkl〉 (k ≠ 0) directions is stopped owing to impingements against the cylinder walls. The dominant crystal growth direction of the 65 nm rod in stronger two-dimensional confinement is in between the [−201] and [001] directions due to the development of a hydrogen-bonded sheet restricted along the long axis of the rod.
    Keywords: molecular self-assemblynanorodsselected-area electron diffractioncylindrical confinement
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  • 17
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Description: For more than 30 years X-ray crystallography has been by far the most powerful approach for determining the structures of viruses and viral proteins at atomic resolution. The information provided by these structures, which covers many important aspects of the viral life cycle such as cell-receptor recognition, viral entry, nucleic acid transfer and genome replication, has extensively enriched our vision of the virus world. Many of the structures available correspond to potential targets for antiviral drugs against important human pathogens. This article provides an overview of the current knowledge of different structural aspects of the above-mentioned processes.
    Keywords: bacteriophagesgenome deliveryfusion proteinsRNA-dependent RNA polymerasesviral proteasesviral receptorsviruses
    Electronic ISSN: 2052-2525
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  • 18
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Description: This article reviews efforts in accurate experimental charge-density studies with relevance to medicinal chemistry. Initially, classical charge-density studies that measure electron density distribution via least-squares refinement of aspherical-atom population parameters are summarized. Next, interaction density is discussed as an idealized situation resembling drug–receptor interactions. Scattering-factor databases play an increasing role in charge-density research, and they can be applied both to small-molecule and macromolecular structures in refinement and analysis; software development facilitates their use. Therefore combining both of these complementary branches of X-ray crystallography is recommended, and examples are given where such a combination already proved useful. On the side of the experiment, new pixel detectors are allowing rapid measurements, thereby enabling both high-throughput small-molecule studies and macromolecular structure determination to higher resolutions. Currently, the most ambitious studies compute intermolecular interaction energies of drug–receptor complexes, and it is recommended that future studies benefit from recent method developments. Selected new developments in theoretical charge-density studies are discussed with emphasis on its symbiotic relation to crystallography.
    Keywords: charge-density researchmedicinal chemistrydrug designinvariomHansen–Coppens multipole modelquantum theory of atoms in molecules
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  • 19
    Publication Date: 2014-11-12
    Description: Metastable phases are often used to design materials with outstanding properties, which cannot be achieved with thermodynamically stable compounds. In many cases, the metastable phases are employed as precursors for controlled formation of nanocomposites. This contribution shows how the microstructure of crystalline metastable phases and the formation of nanocomposites can be concluded from X-ray diffraction experiments by taking advantage of the high sensitivity of X-ray diffraction to macroscopic and microscopic lattice deformations and to the dependence of the lattice deformations on the crystallographic direction. The lattice deformations were determined from the positions and from the widths of the diffraction lines, the dependence of the lattice deformations on the crystallographic direction from the anisotropy of the line shift and the line broadening. As an example of the metastable system, the supersaturated solid solution of titanium nitride and aluminium nitride was investigated, which was prepared in the form of thin films by using cathodic arc evaporation of titanium and aluminium in a nitrogen atmosphere. The microstructure of the (Ti,Al)N samples under study was tailored by modifying the [Al]/[Ti] ratio in the thin films and the surface mobility of the deposited species.
    Keywords: metastable thin filmsmicrostructureX-ray diffraction
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  • 20
    Publication Date: 2014-11-12
    Description: Human transthyretin has an intrinsic tendency to form amyloid fibrils and is heavily implicated in senile systemic amyloidosis. Here, detailed neutron structural studies of perdeuterated transthyretin are described. The analyses, which fully exploit the enhanced visibility of isotopically replaced hydrogen atoms, yield new information on the stability of the protein and the possible mechanisms of amyloid formation. Residue Ser117 may play a pivotal role in that a single water molecule is closely associated with the γ-hydrogen atoms in one of the binding pockets, and could be important in determining which of the two sites is available to the substrate. The hydrogen-bond network at the monomer–monomer interface is more extensive than that at the dimer–dimer interface. Additionally, the edge strands of the primary dimer are seen to be favourable for continuation of the β-sheet and the formation of an extended cross-β structure through sequential dimer couplings. It is argued that the precursor to fibril formation is the dimeric form of the protein.
    Keywords: transthyretinamyloid assemblyneutron crystallographydeuteration
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  • 21
    Publication Date: 2014-11-12
    Description: The Mars Science Laboratory landed in Gale crater on Mars in August 2012, and the Curiosity rover then began field studies on its drive toward Mount Sharp, a central peak made of ancient sediments. CheMin is one of ten instruments on or inside the rover, all designed to provide detailed information on the rocks, soils and atmosphere in this region. CheMin is a miniaturized X-ray diffraction/X-ray fluorescence (XRD/XRF) instrument that uses transmission geometry with an energy-discriminating CCD detector. CheMin uses onboard standards for XRD and XRF calibration, and beryl:quartz mixtures constitute the primary XRD standards. Four samples have been analysed by CheMin, namely a soil sample, two samples drilled from mudstones and a sample drilled from a sandstone. Rietveld and full-pattern analysis of the XRD data reveal a complex mineralogy, with contributions from parent igneous rocks, amorphous components and several minerals relating to aqueous alteration. In particular, the mudstone samples all contain one or more phyllosilicates consistent with alteration in liquid water. In addition to quantitative mineralogy, Rietveld refinements also provide unit-cell parameters for the major phases, which can be used to infer the chemical compositions of individual minerals and, by difference, the composition of the amorphous component.
    Keywords: X-ray diffractionMarsextraterrestrial mineralogyCuriosity rover
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  • 22
    Publication Date: 2014-11-12
    Description: Small- and wide-angle X-ray scattering (SAXS, WAXS) are standard tools in materials research. The simultaneous measurement of SAXS and WAXS data in time-resolved studies has gained popularity due to the complementary information obtained. Furthermore, the combination of these data with non X-ray based techniques, via either simultaneous or independent measurements, has advanced understanding of the driving forces that lead to the structures and morphologies of materials, which in turn give rise to their properties. The simultaneous measurement of different data regimes and types, using either X-rays or neutrons, and the desire to control parameters that initiate and control structural changes have led to greater demands on sample environments. Examples of developments in technique combinations and sample environment design are discussed, together with a brief speculation about promising future developments.
    Keywords: SAXSWAXSSANScomplementary techniquessample environment
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  • 23
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Description: Membranes are amongst the most important biological structures; they maintain the fundamental integrity of cells, compartmentalize regions within them and play an active role in a wide range of cellular processes. Pressure can play a key role in probing the structure and dynamics of membrane assemblies, and is also critical to the biology and adaptation of deep-sea organisms. This article presents an overview of the effect of pressure on the mesostructure of lipid membranes, bilayer organization and lipid–protein assemblies. It also summarizes recent developments in high-pressure structural instrumentation suitable for experiments on membranes.
    Keywords: biological membraneslipidsbilayerslipid–protein assemblieshigh-pressure studies
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  • 24
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Description: Most properties of nanocrystalline materials are shape-dependent, providing their exquisite tunability in optical, mechanical, electronic and catalytic properties. An example of the former is localized surface plasmon resonance (LSPR), the coherent oscillation of conduction electrons in metals that can be excited by the electric field of light; this resonance frequency is highly dependent on both the size and shape of a nanocrystal. An example of the latter is the marked difference in catalytic activity observed for different Pd nanoparticles. Such examples highlight the importance of particle shape in nanocrystalline materials and their practical applications. However, one may ask `how are nanoshapes created?', `how does the shape relate to the atomic packing and crystallography of the material?', `how can we control and characterize the external shape and crystal structure of such small nanocrystals?'. This feature article aims to give the reader an overview of important techniques, concepts and recent advances related to these questions. Nucleation, growth and how seed crystallography influences the final synthesis product are discussed, followed by shape prediction models based on seed crystallography and thermodynamic or kinetic parameters. The crystallographic implications of epitaxy and orientation in multilayered, core-shell nanoparticles are overviewed, and, finally, the development and implications of novel, spatially resolved analysis tools are discussed.
    Keywords: nanocrystalline materialsplasmonicsshape prediction models
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  • 25
    Publication Date: 2014-11-12
    Description: Membrane fusion is essential for human health, playing a vital role in processes as diverse as neurotransmission and blood glucose control. Two protein families are key: (1) the Sec1p/Munc18 (SM) and (2) the soluble N-ethylmaleimide-sensitive attachment protein receptor (SNARE) proteins. Whilst the essential nature of these proteins is irrefutable, their exact regulatory roles in membrane fusion remain controversial. In particular, whether SM proteins promote and/or inhibit the SNARE-complex formation required for membrane fusion is not resolved. Crystal structures of SM proteins alone and in complex with their cognate SNARE proteins have provided some insight, however, these structures lack the transmembrane spanning regions of the SNARE proteins and may not accurately reflect the native state. Here, we review the literature surrounding the regulatory role of mammalian Munc18 SM proteins required for exocytosis in eukaryotes. Our analysis suggests that the conflicting roles reported for these SM proteins may reflect differences in experimental design. SNARE proteins appear to require C-terminal immobilization or anchoring, for example through a transmembrane domain, to form a functional fusion complex in the presence of Munc18 proteins.
    Keywords: SM proteinsSNARE proteinssyntaxinMunc18membrane trafficking
    Electronic ISSN: 2052-2525
    Topics: Geosciences , Physics
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  • 26
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Description: The biological solution small-angle X-ray scattering (BioSAXS) field has undergone tremendous development over recent decades. This means that increasingly complex biological questions can be addressed by the method. An intricate synergy between advances in hardware and software development, data collection and evaluation strategies and implementations that readily allow integration with complementary techniques result in significant results and a rapidly growing user community with ever increasing ambitions. Here, a review of these developments, by including a selection of novel BioSAXS methodologies and recent results, is given.
    Keywords: biological solution small-angle X-ray scattering (BioSAXS)synchrotron radiationbeamlinesstructural complexitybiostructural research
    Electronic ISSN: 2052-2525
    Topics: Geosciences , Physics
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  • 27
    facet.materialart.
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Description: The study of single-crystal diffuse scattering (SCDS) goes back almost to the beginnings of X-ray crystallography. Because SCDS arises from two-body correlations, it contains information about local (short-range) ordering in the sample, information which is often crucial in the attempt to relate structure to function. This review discusses the state of the field, including detectors and data collection and the modelling of SCDS using Monte Carlo and ab initio techniques. High-quality, three-dimensional volumes of SCDS data can now be collected at synchrotron light sources, allowing ever more detailed and quantitative analyses to be undertaken, and opening the way to approaches such as three-dimensional pair distribution function studies (3D-PDF) and automated refinement of a disorder model, powerful techniques that require large volumes of low-noise data.
    Keywords: single-crystal diffuse scatteringdisordersynchrotron light sources
    Electronic ISSN: 2052-2525
    Topics: Geosciences , Physics
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  • 28
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Description: The smart specialization declared in the European program Horizon 2020, and the increasing cooperation between research and development found in companies and researchers at universities and research institutions have created a new paradigm where many calls for proposals require participation and funding from public and private entities. This has created a unique opportunity for large-scale facilities, such as synchrotron research laboratories, to participate in and support applied research programs. Scientific staff at synchrotron facilities have developed many advanced tools that make optimal use of the characteristics of the light generated by the storage ring. These tools have been exceptionally valuable for materials characterization including X-ray absorption spectroscopy, diffraction, tomography and scattering, and have been key in solving many research and development issues. Progress in optics and detectors, as well as a large effort put into the improvement of data analysis codes, have resulted in the development of reliable and reproducible procedures for materials characterization. Research with photons has contributed to the development of a wide variety of products such as plastics, cosmetics, chemicals, building materials, packaging materials and pharma. In this review, a few examples are highlighted of successful cooperation leading to solutions of a variety of industrial technological problems which have been exploited by industry including lessons learned from the Science Link project, supported by the European Commission, as a new approach to increase the number of commercial users at large-scale research infrastructures.
    Keywords: X-ray techniquesindustryinnovation
    Electronic ISSN: 2052-2525
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  • 29
    Publication Date: 2014-11-12
    Description: Iron(II) and 2-oxoglutarate (2OG)-dependent dioxygenases involved in histone and DNA/RNA demethylation convert the cosubstrate 2OG and oxygen to succinate and carbon dioxide, resulting in hydroxylation of the methyl group of the substrates and subsequent demethylation. Recent evidence has shown that these 2OG dioxygenases play vital roles in a variety of biological processes, including transcriptional regulation and gene expression. In this review, the structure and function of these dioxygenases in histone and nucleic acid demethylation will be discussed. Given the important roles of these 2OG dioxygenases, detailed analysis and comparison of the 2OG dioxygenases will guide the design of target-specific small-molecule chemical probes and inhibitors.
    Keywords: dioxygenaseshistone demethylationDNA/RNA demethylationN6-methyladenosineALKBH5
    Electronic ISSN: 2052-2525
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  • 30
    facet.materialart.
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Description: Worldwide research activity at the nanoscale is triggering the appearance of new, and frequently surprising, materials properties in which the increasing importance of surface and interface effects plays a fundamental role. This opens further possibilities in the development of new multifunctional materials with tuned physical properties that do not arise together at the bulk scale. Unfortunately, the standard methods currently available for solving the atomic structure of bulk crystals fail for nanomaterials due to nanoscale effects (very small crystallite sizes, large surface-to-volume ratio, near-surface relaxation, local lattice distortions etc.). As a consequence, a critical reexamination of the available local-structure characterization methods is needed. This work discusses the real possibilities and limits of X-ray absorption spectroscopy (XAS) analysis at the nanoscale. To this end, the present state of the art for the interpretation of extended X-ray absorption fine structure (EXAFS) is described, including an advanced approach based on the use of classical molecular dynamics and its application to nickel oxide nanoparticles. The limits and possibilities of X-ray absorption near-edge spectroscopy (XANES) to determine several effects associated with the nanocrystalline nature of materials are discussed in connection with the development of ZnO-based dilute magnetic semiconductors (DMSs) and iron oxide nanoparticles.
    Keywords: EXAFSXANESoxide nanomaterialsnanocrystalline materials
    Electronic ISSN: 2052-2525
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  • 31
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Description: The community of material scientists is strongly committed to the research area of multiferroic materials, both for the understanding of the complex mechanisms supporting the multiferroism and for the fabrication of new compounds, potentially suitable for technological applications. The use of high pressure is a powerful tool in synthesizing new multiferroic, in particular magneto-electric phases, where the pressure stabilization of otherwise unstable perovskite-based structural distortions may lead to promising novel metastable compounds. The in situ investigation of the high-pressure behavior of multiferroic materials has provided insight into the complex interplay between magnetic and electronic properties and the coupling to structural instabilities.
    Keywords: high pressuremultiferroicsmaterials science
    Electronic ISSN: 2052-2525
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  • 32
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    International Union of Crystallography (IUCr)
    In: IUCrJ
    Publication Date: 2014-11-12
    Description: Metal–organic frameworks (MOFs) are one of the most intensely studied material types in recent times. Their networks, resulting from the formation of strong bonds between inorganic and organic building units, offer unparalled chemical diversity and pore environments of growing complexity. Therefore, advances in single-crystal X-ray diffraction equipment and techniques are required to characterize materials with increasingly larger surface areas, and more complex linkers. In addition, whilst structure solution from powder diffraction data is possible, the area is much less populated and we detail the current efforts going on here. We also review the growing number of reports on diffraction under non-ambient conditions, including the response of MOF structures to very high pressures. Such experiments are important due to the expected presence of stresses in proposed applications of MOFs – evidence suggesting rich and complex behaviour. Given the entwined and inseparable nature of their structure, properties and applications, it is essential that the field of structural elucidation is able to continue growing and advancing, so as not to provide a rate-limiting step on characterization of their properties and incorporation into devices and applications. This review has been prepared with this in mind.
    Keywords: MOFsnon-ambient crystallographycrystal growth
    Electronic ISSN: 2052-2525
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  • 33
    Call number: K 06.0479 / Fach 26
    Type of Medium: Map available for loan
    Pages: 1 Kt. , mehrfarb. ; 54 x 54 cm, gefaltet
    Edition: Bearbeitungstand: Juni 2006
    Location: Upper compact magazine
    Branch Library: GFZ Library
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  • 34
    Call number: K 06.0161 / Fach 112
    Type of Medium: Map available for loan
    Pages: 1 Kt. : mehrfarb. : 53 x 75 cm
    ISBN: 3773912706
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  • 35
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    Essen : Verl. Glückauf | Wuppertal : Wuppertal Institut für Klima, Umwelt, Energie
    Publication Date: 2016-08-23
    Keywords: ddc:600
    Repository Name: Wuppertal Institut für Klima, Umwelt, Energie
    Language: English
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  • 36
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 399-400 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A new method for the phase control in an optical diffractometer is described. A photographic negative of the weighted reciprocal net is used as the mask of the diffractometer. The phase of each reciprocal point is represented by the shift of the position in the reciprocal plane. Although this method cannot reproduce the periodic image of a crystal, it is particularly suitable for reconstructing the image of a molecule in a crystal.
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  • 37
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 408-408 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
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  • 38
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 404-405 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Unit-cell parameters and space groups have been determined on four ammonium polyphosphate salts. (NH4)5P3O10.2H2O is monoclinic with space group P21/n, a = 16.643, b = 6.719, c = 13.843, β = 98.61. (NH4)5P3O10.H2O is monoclinic, space group P2/n or Pn, a = 10.949, b = 10.377, c = 6.426, β = 91.06. (NH4)6P4O13.2H2O is triclinic, a =13.426, b = 11.874, c = 6.524, α = 93.80, β = 84.78, γ = 106.97. (NH4)4 H2P4O13 is orthorhombic, space group P22121, a = 13.359, b = 13.244, c = 8.214.
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  • 39
    Electronic Resource
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 406-406 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
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  • 40
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 408-408 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
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  • 41
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 511-512 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Crystal data for Zn(H2PO4)2. 2H2O and ZnH2P2O7 are given. The two compounds crystallize in the monoclinic system. The monophosphate is isotypic with Cd(H2PO4)2.2H2O.
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  • 42
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 513-513 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
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  • 43
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 515-518 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Unusual SiC polytypic features have been studied by X-ray diffraction and chemical etching to increase understanding of their growth mechanism. The feasibility of periodic slip as a possible mode of growth of SiC polytypes has been examined. It is proposed that island formation on the helicoidal growth surface is responsible for most of the unusual SiC polytypes not explicable purely in terms of a screw-dislocation mechanism.
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  • 44
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 526-531 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: All the information relating to the quantitative composition of a mixture is coded and stored in its X-ray diffraction pattern. It has been the goal of X-ray diffraction analysts since the discovery of X-rays to retrieve and decode this information directly from the X-ray diffraction pattern rather than resort to calibration curves or internal standards. This goal appears to be attained by the application of the `matrix-flushing theory' and the now-proposed `adiabatic principle' in applied X-ray diffraction analysis. The matrix-flushing theory offers a simple intensity-concentration equation free from matrix effects which degenerates to `auto-flushing' for binary systems. The adiabatic principle establishes that the intensity–concentration relationship between each and every pair of components in a multi component system is not perturbed by the presence or absence of other components. A key equation is derived which conducts the decoding process. Both the matrix-flushing theory and the adiabatic principle are experimentally verified.
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  • 45
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 535-540 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: X-ray diffraction topography using transmission geometry has revealed an interesting array of extremely straight and narrow long-line images in sizeable copper single crystals grown under particular growth conditions by the Czochralski technique. These images are analyzed and elucidated by a model of Lomer–Cottrell dislocations. The formation of these sessile dislocations usually aids the growth of large copper crystals of high perfection. The high degree of perfection over the entire volume of the crystals accounts for macroscopic arrangements of Lomer–Cottrell dislocations which have not previously been observed by electron microscopic techniques.
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  • 46
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 547-554 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Investigations of many imperfect single crystals of different materials by means of a γ-diffractometer show that the mosaic structure of large single crystals is often very inhomogeneous: the mosaic distribution function has neither a Gaussian nor a Lorentzian shape and the shapes differ remarkably for different volume elements in the sample. Current extinction theories must be considered with reservation because Darwin's intensity transport equations are solved assuming the scattering length for a given angle of incidence to be constant all over the irradiated crystal volume. This is not true for samples with inhomogeneous mosaic structure.
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  • 47
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 577-585 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Superlattice formation in thin films of copper–gold alloys has been studied by the use of optical-diffraction analogues. Fraunhofer diffraction patterns of arrangements of holes in opaque screens have been compared with electron-diffraction patterns of the alloy films. It has been found possible to draw some general conclusions about the ways in which the antiphase domains fit together to produce certain characteristics of the electron-diffraction patterns. Some ideas are put forward about the growth of superlattices.
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  • 48
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 599-603 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A drum-scanning microdensitometer has been automated with a minicomputer equipped with a magnetic disk memory. Part of the disk is used for temporary data storage, in a manner allowing rapid retrieval. X-ray diffraction photographs from macromolecular crystals can be measured at rates up to about 25 reflections per second, with the flexibility of an `on-line' system. The method can also be used when the computer is time-shared, but with lowered film-processing rates dependent on the number of `simultaneous' (time-sharing) users.
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  • 49
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 555-564 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A profile-fitting algorithm has been applied to the determination of X-ray diffraction intensities from precession photographs. It is assumed that each reflection on the film has the same profile or scaled intensity distribution, over a two-dimensional array of points about its center. The integrated intensity of a reflection is that scale factor which gives the best fit between a scaled model profile and the optical density measurements of the reflection. The systematic error in the calculated intensity was evaluated from the discrepancy between the model and observed profiles and was about 2% for strong reflections (about 1.5 OD units). Profile fitting reduced the likely random error in the intensity, produced by errors in optical density measurements, to half the value given by conventional integration. This gain is especially significant for weak reflections which form the bulk of protein data sets. A comparison between film data processed by this method and diffractometer data for the protein lactate dehydrogenase, (34000 Dalton in asymmetric unit), showed that film data agreed with diffractometer data as well as diffractometer data sets agreed among themselves. Film data for glyceraldehyde-3-phosphate dehydrogenase (144000 Dalton in asymmetric unit) had a reliability index of 6% and significant Bijvoet differences were measured for mercury derivatives of the protein. Methods for the correction for non-linear effects in film data are evaluated for model data. It is shown that these corrections give significant improvement only when the data satisfy two conditions: they extend over a wide range of optical densities (at least 20D units) and they are reliable (better than 4% reliability index). Under these conditions an extended version of the Hamilton, Rollett and Sparks scaling algorithm performs better than the other methods considered.
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  • 50
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 593-598 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The construction and successful operation of a Laue-case skew-symmetric two-crystal X-ray interferometer is described. The alignment is accomplished with an auxiliary X-ray beam, which is multiply reflected by both interferometer parts. As expected, the skew-symmetric two-crystal interferometer is found to be considerably less affected by vibrations than is the symmetric two-crystal interferometer. [Bonse & te Kaat (1968), Z. Phys. 214, 16–21]. The dependence of the crystal lattice moiré pattern on rotations about the Δρ and Δ&thgr; axes are investigated.
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  • 51
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 19-21 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Precession X-ray films were scanned with a rotating-drum microdensitometer. It is necessary to correct for non-linearity between the scanner input and output. Reliability factors for estimating the precision of scanner measurements are compared. The values of the symmetry-averaged reliability factor, Rsym, vary between 3.9 and 12% and depend strongly on the quality of films, while the values of the scanning reproducibility factor, Rrept (3.5–4%), and the film-scaling reliability factor, Rscale (4.5–5.5%), depend more on the quality of scanner software and electronics than on films.
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  • 52
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 1-18 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: This article is the text of a general lecture given at the Ninth International Congress of Crystallography, September 1972, at Kyoto, Japan. The lecture begins with the famous experiment of Kikuchi and continues with results of work carried out under the leadership of Miyake and the author. The main topics in the former part are: anomalous enhancement and splitting of Bragg peaks, appearance of non-Bragg maxima, dynamical multiple refraction, etc. Dynamical theories including inelastic scattering are introduced, and the formation mechanism of Kikuchi bands and absorption effects are explained. Electron diffraction and electron microscopy, which were originally developed as different fields, have been unified after 1950. The development of high-voltage electron microscopy is emphasized. The reason for the enhancement of dynamical effects at very high voltages is explained in terms of relativistic diffraction theory. As an example of some most remarkable dynamical effects, the vanishing of the second-order reflexion is described. Finally, the findings and developments in moiré patterns and lattice images are reviewed briefly. The lecture is devoted to diffraction phenomena themselves and applications to structural studies are excluded.
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  • 53
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 22-24 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: X-ray divergent-beam anomalous-transmission patterns of [111] Gd3Ga5O12 crystal wafers cut from Czochralski-grown boules were obtained with Co radiation. The patterns contained {800} Kα transmission conics which just miss having a triple intersection. The intersection region was analyzed to determine the lattice parameter. The values of lattice parameter for wafers cut from several different boules ranged from 12.3807 to 12.383 Å with an estimated precision of ±0.0004 Å. The method is simple and non-destructive and offers sufficient precision to investigate compositional variations and to evaluate the crystals in terms of lattice parameter matching requirements for epitaxic film deposition.
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  • 54
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 25-36 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Measurements made by small-angle X-ray scattering on Al–Ag alloys aged at various temperatures have shown that the asymptotic Porod's law was obeyed except for a constant term. This additional term represents a Laue monotonic intensity, due mainly to atomic concentration fluctuations inside G.P. zones. The integrated intensity Q0 of the G.P. zones themselves can then be calculated, and the boundaries of the metastable miscibility gap estimated with more precision than previously. Furthermore, the integrated intensities in the first reciprocal-space shell make it possible to discuss the crystallographic structure of the G.P. zones. After quenching from 550 to −80°C, the measured intensities agree with the theoretical values, which implies that small G.P. zones ε′ are disordered. However, for aging above room temperature, there is no agreement between measured and theoretical values. When the aging temperature is increased from 140 to 190°C, an evolution towards a complex structure of G.P. zones is shown.
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  • 55
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 36-38 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Optical-transform methods remain useful aids in determining the structures of polymers, and other disordered materials, from X-ray scattering data. Hitherto a major difficulty has been the preparation of diffracting screens which contain sufficient information to specify adequately the material being studied. The Optronics P-1500 Photowrite system overcomes this difficulty. The equipment is described briefly and two examples of its use in optical transform methods are given.
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  • 56
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 38-41 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Absolute reflectivities, width of rocking curves and effective absorption coefficients for many pyrolytic graphite crystals at different wavelengths were measured. The results can be described within a few percent by the formulae for the ideal mosaic crystal with absorption. Effective absorption is caused by unavoidable parasitic reflections. The measured effective absorption coefficient is the same for different specimens; it does not depend on the mosaic width. By means of this effective absorption, the peak reflectivity decreases with increasing mosaic width.
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  • 57
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    Applied crystallography online 7 (1974), S. 41-44 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: A small, colorless, single-crystal with appreciable vapor pressure at room temperature was presumed to be a new oxyfluoride compound of osmium. An X-ray study on a precession camera at a variety of temperatures from 20 to −100°C with many recrystallizations of the material revealed that it was dimorphic. One structure is monoclinic in space group C2/c with a unit cell nearly identical to that reported for OsO4. The second structure is cubic, a = 8.595 Å, Z = 8, space group P\bar 43n, with an extraordinary assortment of systematic absences which yield the most remarkable diffraction patterns the writer has ever encountered. The observations are accounted for by a structure comprising 8 tetrahedral molecules with the anions in cubic close packing at an anion–anion distance of 3.04 Å and with an Os–anion distance of 1.86 Å. The most likely possibilities for the chemical composition appear to be OsO2F2 or OsO3F.
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    Applied crystallography online 7 (1974), S. 44-50 
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    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: An improved iterative deconvolution procedure is described which involves convolution of an assumed function, which represents the imperfectly known result, with the instrument function and operation on the differences between the convoluted function and the observed data function. Its advantage over the simple Fourier–Stokes treatment lies in improved resolution, its capability to handle functions with discontinuities in the function or in its derivative, and the possibility of using a variable instrument function.
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    Applied crystallography online 7 (1974), S. 50-59 
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    Notes: The ordered structures of Cu–Pt alloys containing 65–78 at. % Pt have been investigated by a combined technique of selected-area electron diffraction and dark-field electron microscopy using thin foils prepared from bulk specimens, and three different types of ordered structure have been observed. Below the order–disorder transformation temperatures, alloys containing less than about 70 at. % Pt have the rhombohedral superlattice of the Cu3Pt5 type and those with more than 70 at. % Pt, the CuPt3-type superlattice with cubic symmetry. At lower temperatures, however, the orthorhombic superlattice is stable in the composition range from about 68 to 75 at. % Pt. On the basis of the present observations, a partial phase diagram around the composition CuPt3 has been determined.
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    Applied crystallography online 7 (1974), S. 59-64 
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    Topics: Geosciences , Physics
    Notes: Neutron diffraction topography with thermal neutrons has been used to observe the three-dimensional strain fields in a hot-pressed germanium crystal 8 mm thick. In the stereo-paired and section topographs the strain fields were found to be columnar along the press direction. This result was confirmed by X-ray diffraction topography performed on slices cut from the same crystal.
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    Applied crystallography online 7 (1974), S. 65-66 
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    Notes: Gold films of several hundred Ångströms in thickness were evaporated on heated glass substrates. Fourier analysis of the 111 reflexion obtained with Cu Kα radiation showed that the thickness of the film must be fairly constant. After correction for instrumental broadening the 111 line profile was very similar to the theoretical profile of a reflexion from a plate of constant thickness. The thickness was measured in three different ways. It was shown that the first secondary maxima may be unreliable in the measurement of the thickness.
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  • 62
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    Applied crystallography online 7 (1974), S. 67-73 
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    Notes: The structure of the interstitially ordered lattice formed in zirconium–oxygen alloys has been studied with use of single-crystal data obtained by X-ray and neutron diffraction methods. The structure belongs to space group P312 and the lattice parameters a and c are related to a0 and c0 of the host hexagonal metal lattice by a = √3a0 and c = c0. The ordered arrangement of interstitial oxygen atoms is described as a regular stacking of layers parallel to the (00.1) plane with the sequence (AC)B(AC)B... which is of the same type as that of nitrogen atoms in ε-Fe2N. The occupancy probability of oxygen atoms is high for interstitial sites of the A and B types while it is low for sites of the C type. The host metal lattice is distorted in such a way that spacings of successive (00.2) planes are not the same and a hexagonal network of atoms in these planes is periodically deformed.
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    Applied crystallography online 7 (1974), S. 78-82 
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    Notes: Algebraic criteria are presented by means of which it can be decided whether a given zonal net can belong to a cubic, tetragonal, hexagonal or rhombohedral lattice or not. Methods of calculating the axes of the possible lattices from the nets are discussed.
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    Applied crystallography online 7 (1974), S. 73-78 
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    Notes: An extensive computer program has been developed to check the internal consistency of published, numeric, crystallographic data prior to storage in the data files of the Cambridge Crystallographic Data Centre. The coding is in Fortran IV for an IBM 3701165 with 1 megabyte store. The atomic coordinates, constitution and connectivity of the unique bonded residue(s) are determined from the published asymmetric unit coordinates. Bond lengths are calculated and compared with published values, and any discrepancies are flagged. Checks are made to ensure that the valency requirements of certain elemental types are not violated. The connectivity of the system is expressed in a compact notation. Axial projection plots may optionally be produced on the line printer. The program is likely to be generally useful to individual crystallographers at various stages of an analysis as well as for checking of published data.
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    Applied crystallography online 7 (1974), S. 83-86 
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    Notes: Experimental measurements were performed on a 48.4 at. % Ni/51.6 at. % Pt alloy. The order parameter S in equilibrium was measured as a function of temperature T by means of X-ray diffraction. Up to 592±3°C the sample is a single-phase ordered alloy with an order parameter above 0.98. Between 592 and 625±3°C there exists a two-phase region in which the ordered and disordered phases are in equilibrium. Above 625±3°C a disordered f.c.c. structure exists. Diffuse X-ray intensity measurements were performed at T = 1.1 Tc and both the short-range parameters αi and the size-effect parameters βi were calculated. From the αi parameters so derived three ordering energies νi were determined. It was found that these energies were consistent with the symmetry of the ordered phase below the critical temperature.
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    Applied crystallography online 7 (1974), S. 87-88 
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    Notes: Crystal data at −17°C are reported for the two spectroscopically important title compounds. The experimental techniques used for the growth, mounting and preservation of the crystals in a cold room are described.
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    Applied crystallography online 7 (1974), S. 88-90 
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    Notes: Unit-cell parameters and indexed powder patterns are reported for mescaline sulfate dihydrate, hydrochloride, hydrobromide and hydroiodide. Mescaline (3,4,5-trimethoxyphenethylamine) is a hallucinogenic substance naturally occurring in the peyote cactus, Lophophora williamsii.
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    Applied crystallography online 7 (1974), S. 90-91 
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    Notes: The title compound, prepared by evaporation, is orthorhombic, Pcab, with a= 15.570 (6), b= 16.837 (7), c = 13.715 (4) Å. It appears to be isomorphous with previously reported forms of the iron(III) and vanadium(III) compounds.
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    Applied crystallography online 7 (1974), S. 91-91 
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    Applied crystallography online 7 (1974), S. 91-92 
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    Applied crystallography online 7 (1974), S. 92-92 
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    Applied crystallography online 7 (1974), S. 92-93 
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    Applied crystallography online 7 (1974), S. 93-93 
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    Applied crystallography online 7 (1974), S. 94-94 
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    Applied crystallography online 7 (1974), S. 94-94 
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    Applied crystallography online 7 (1974), S. 94-94 
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    Applied crystallography online 7 (1974), S. 95-95 
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    Applied crystallography online 7 (1974), S. 147-147 
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    Notes: The evaluation of the small-angle scattering of two-phase systems is greatly facilitated if Porod's law can be observed in the outer angular region.
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    Applied crystallography online 7 (1974), S. 147-153 
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    Notes: A new iterative procedure for desmearing small-angle scattering data including the three types of resolution errors and arbitrary weighting functions is presented. The statistical errors of the data are taken into account by a `weighted least-squares' approximation, i.e. the accuracy of the data controls the iterative process. The degree of smoothing is dependent on a free smoothing parameter and on the accuracy of the data. The method is not restricted to special types of scattering functions. The termination error is negligible; therefore it is possible to correct parts of scattering distributions. This is of importance for investigations in biological substances where the scattering distribution must be determined in parts with different slit widths. No artificial oscillations are generated in the solution of the integral equation. To ensure the stability of the procedure a criterion for uniform convergence of the iterative process is involved. The results of several numerical tests are shown in the figures. The Fortran program was tested for several months with very satisfactory results.
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    Applied crystallography online 7 (1974), S. 154-158 
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    Notes: An analytic expression for the power transmitted through a Kratky small-angle X-ray scattering collimation geometry has been derived which depends on the size and position of a uniformly intense focal spot relative to the entrance slit in the width direction. Complete details on the derivation of this power expression are available from the authors. The power expression can be optimized, subject to the constraint of a predetermined and fixed minimum angle, to yield the optimum values for the collimation system parameters. This paper discusses the optimum values of the entrance and receiving slits for a given minimum angle and describes the application of these results for the entrance slit either fully or not fully illuminated. A comparison of the analytical power expression with the experimental scattered power is also given.
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    Applied crystallography online 7 (1974), S. 131-146 
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    Notes: The relation between the form of the scattering particles and the outer part of the small-angle X-ray scattering curve has been studied. The particles are assumed to be independent, identical, and randomly oriented and to have a uniform electron density and a smooth, strictly convex boundary surface. The electron density of the solvent is also assumed to be uniform. As earlier calculations by the authors and others have shown, the effects of the particle shape on the scattered intensity can often be conveniently described by a function called the chord, or intersect, distribution G(M). A chord, or intersect, is a straight line that has both ends on the particle boundary surface, and G(M) is defined to have the property that G(M)dM is the probability that the chord length will lie between M and M+ dM. The outer part of the scattering curve is shown to depend on the form of G(M) only in the neighborhoods of M = 0 and of any M values at which G(M) or G′(M) are discontinuous. Methods are developed for finding where these discontinuities occur and for calculating the form of G(M) in the neighborhood of these M values. In the outer part of the scattering curve, the intensity I(h) is shown to have the limiting form I(h) = \pi I_{e}\rho^{2}h^{-4}\Bigg[2A+j_{-2}h^{-2}+ \sum_{i=0}^{N+1} j_{i} {{sin (hD_i + \phi _{i})}\over (hD_{i})^{\mu}_{\kern4pt i}}\Bigg] where h = 4πλ −1 sin (&thgr;/2), 2 is the X-ray wavelength, &thgr; is the scattering angle, Ie is the intensity scattered by a single electron, A is the particle surface area, the Di are the values of M at which G(M) or G′(M) is discontinuous, and j−2 and the ji, &phgr;i, and μi are quantities which can be calculated from the principal curvatures and other properties of the surface at the two points where it contacts the chord with length Di. The values of the μi are shown to lie in the interval 0 ≤ μi ≤ 1. In this equation the assumption is made that only the term or terms which vanish least rapidly as h increases are to be retained. In addition to the assumptions which conventionally are made in the analysis of the small-angle X-ray scattering from dilute suspensions, the limiting expression for the intensity for large h requires only that the particle boundary be smooth and strictly convex. This approximation is useful for determining the effect of the particle shape on the outer part of the scattering curve. In addition, the equation can be employed for numerical calculations for large h, where other methods of computation often are unwieldy or inapplicable.
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    Applied crystallography online 7 (1974), S. 159-163 
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    Notes: The unified theory of absolute intensity measurements in small-angle X-ray scattering has been experimentally verified by determining a collimation system and wavelength-independent calibration constant for polyethylene (Lupolen). Consistent values of this constant were determined for three X-ray wavelengths (Ag Kα, Mo Kα and Cu Kα by gas scattering and multiple-foil attenuator experiments. The agreement of the results implies that all of the experimentally significant parameters involved in these absolute intensity calibrations have been identified. In addition, they show Lupolen to be a more general secondary standard than had been previously recognized.
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    Applied crystallography online 7 (1974), S. 163-163 
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    Notes: The three years since the Second International Small-Angle X-ray Scattering Conference have seen a great many important applications of small-angle X-ray scattering to the determination of biological structures.
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    Applied crystallography online 7 (1974), S. 168-168 
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    Notes: SAXS was applied to the RNA from bacteriophage MS2.
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    Applied crystallography online 7 (1974), S. 173-178 
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    Notes: In order to get an idea of the possible neutron small-angle scattering experiments with solutions of macromolecules at the high-flux reactor of the Institut Max von Laue–Paul Langevin at Grenoble, aqueous solutions of molecules with molecular weights from about one hundred to several millions have been studied. Changing the contrast by using different H2O/D2O mixtures the basic scattering functions could be determined. Zero-angle scattering from neutron and X-ray small-angle scattering experiments are compared. In the case of ferritin the molecular-weight distribution could be determined from the dependence of zero-angle scattering on the solvent. A considerable variation of the square of the radius of gyration R at low contrast \bar \rho was observed. R2 turned out to be a linear function of 1/\bar \rho. The slope of the straight line is a measure of the homogeneity of the internal structure. Proton–deuteron exchange reactions have been studied. A time resolution of less than two seconds had been reached with myoglobin and other globular proteins.
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    Applied crystallography online 7 (1974), S. 169-173 
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    Notes: A model has been developed to calculate the diffraction given by a disordered set of thick coils of helical conformation. Double coils placed inside a cylinder of different density are considered. The cylinder accounts for the presence of substances which may interact with the double coil in a random manner. The thickness of each coil, pitch and radius of gyration, outer cylinder diameter and its density are the parameters that influence the diffraction maxima observed. It is demonstrated that when the parameter Z (pitch/radius) increases, the peaks tend to overlap. The relative position (α) of the two coils is also studied. When they are diametrically opposed, only even layer-line peaks are detected. At intermediate positions, other peaks appear, the intensity of which depends strongly on the precise value of α. An interesting result is that the relative position of the peaks for any single coil is constant and does not depend on the dimensions of the coil. The central scattering increases considerably if one of the two-component coils becomes a straight cylinder coaxial with the primitive coil. As a result the lower layer-line peaks do not show. On the other hand, the intensity due to the central equatorial peak diminishes when some packing order is introduced between coils. The model is suitable for interpreting the specific case of nucleohistone patterns.
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    Applied crystallography online 7 (1974), S. 188-188 
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    Notes: A comparative study of the dimensions of a flexible polymer (atactic polystyrene) in three environments has been undertaken.
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    Applied crystallography online 7 (1974), S. 189-189 
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    Notes: In the investigation of polymer solutions by small-angle neutron or X-ray scattering, the intermediate momentum range corresponds to the distance between the radius of gyration RG and the statistical subunit length l of the polymer chain. In this range, where the specific polymeric behaviour prevails, it can be shown, using the Debye relation, that the scattering curve presents a q−2 singularity, q being the momentum transfer.
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    Applied crystallography online 7 (1974), S. 190-190 
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    Notes: The radius of gyration, rg, of atactic polystyrene molecules in the bulk polymer has been measured by low-angle neutron scattering from dilute solid solutions of poly-proto-styrene in poly-deutero-styrene with concentrations of 5 % and 0.5 % tagged solute molecules.
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    Applied crystallography online 7 (1974), S. 190-190 
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    Notes: The small-angle scattering of polymers contains a component which is due to the statistical fluctuation of the density produced by imperfections in the long-range or short-range order. This fluctuation is entirely due to thermal motion and is related to the compressibility in the case of a one-component fluid system in thermodynamic equilibrium. In non-equilibrium one-component systems in the solid state, the statistical fluctuations of the density are, at least partly, due to frozen-in disordered structures.
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    Applied crystallography online 7 (1974), S. 191-191 
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    Notes: Deux types d'échantillons permettent la mesure de l'orientation des faces limites des lamelles et du rapport R de la longueur des plis à celle des monomères.
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    Applied crystallography online 7 (1974), S. 191-191 
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    Notes: The small-angle X-ray scattering from a dilute solution of the polystyrene/polybutadiene/polystyrene block copolymer in methyl ethyl ketone was measured.
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    Applied crystallography online 7 (1974), S. 207-210 
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    Notes: Small-angle scattering (SAS) of neutrons is applied to the investigation of the microinhomogeneous structure of glasses. The alumina–silica titania-containing systems are taken as the subject of the investigation. The negative sign of the Ti nuclear scattering amplitude sharply extends the sensitivity to fluctuations of the atomic density. The phase-segregation kinetics was studied in the temperature region 750–950°C. A comparison of neutron SAS data with the data from X-ray phase analysis and neutron diffraction has shown that the process of segregation into two amorphous phases is accompanied by the simultaneous ordering of the titania-rich phase up to the appearance of crystallites. The `glass-in-glass' state corresponds only to the initial stages of the decomposition.
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    Applied crystallography online 7 (1974), S. 218-218 
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    Notes: Small-angle X-ray scattering has been used to study early-stage spinodal decomposition in Al-base Zn and Al-base Ag alloys which were liquid-quenched at rates of the order of 106°C/sec.
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    Applied crystallography online 7 (1974), S. 222-222 
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    Notes: Boron carbide is a potential neutron-absorber material for fast-reactor control systems. It is, therefore, essential that its response to prolonged fast-neutron irradiation be well characterized.
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    Applied crystallography online 7 (1974), S. 222-222 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: In solid-state physics small-angle scattering near the reciprocal origin is a subcase of the more general situation of studying diffuse scattering at Bragg reflexions. In this work two difficulties connected with scattering studies on metal alloys near Bragg reflexion (Huang scattering) have been overcome.
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  • 97
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 219-221 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The small-angle neutron scattering from G. P. zones in aged Al–Mg alloys has been measured by the difference in intensity between the scattering before and after an anneal at 100°C sufficiently long for dissolving the zones. No zones have been found by this method in Al–7% Mg alloys. The scattering by zones found in Al–11.5% Mg alloys has been analysed with the help of a radial pair-correlation function written in the form of a sum of Gaussian distribution functions. Best fitting is obtained with a rather smooth function. The mean size of the zones has been determined: mean diameter of about 70 Å for an alloy aged one year at room temperature, and 110 Å, for an alloy aged the first three months at 40°C and then nine months at room temperature. The corresponding mean distance between the zones is found to be equal to about 130 and 200 Å, respectively. The concentration in Mg of the zones has been found to be of the order of magnitude of 20 to 25%.
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  • 98
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 233-236 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Small-angle scattering from an Fe65Ni35 single-crystal has been measured with the magnetic field applied parallel and perpendicular to the scattering vector κ. Scattering cross sections due to longitudinal and transverse fluctuations have been calculated. The transverse cross section consists mainly of spin-wave scattering and has a long tail up to κ = 0.2 Å−1. This suggests that there are spin-wave modes heavily damped by magnetic inhomogeneities. The longitudinal cross section can be described by a Guinier approximation (dσ/dΩ)0 exp (− κ2R2g/3) for the range 0.05 〈 κ 〈 0.2 Å−1. The forward-scattering cross section (dσ/dΩ)0 and the radius of gyration Rg obtained from experiment are compared with values calculated from Kachi's model. In this model the magnetization is zero for every cluster of 60 atoms with a concentration of nickel below 29%. The comparison shows that the observed value for Rg (= 7.7 Å) is about twice as large as the calculated one. The observed forward scattering (dσ/dΩ)0 has slightly different values for different crystal orientations and is on the average 75% of the calculated value. The agreement is remarkable with regard to the crudeness of the model.
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  • 99
    Electronic Resource
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 247-250 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: The superstructure of U4O9 above the transition was studied at 120 °C by single-crystal neutron diffraction. The space group I4132 is found not to change through the transition. The lattice constant of the superstructure is four times that of the fundamental fluorite-type UO2 mother structure. From difference Fourier synthesis for the superlattice reflections, the parameter in the special position 24(g) representing additional oxygen atoms in the fundamental structure was found to change a little at the transition.
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  • 100
    Electronic Resource
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    Copenhagen : International Union of Crystallography (IUCr)
    Applied crystallography online 7 (1974), S. 240-246 
    ISSN: 1600-5767
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Geosciences , Physics
    Notes: Certain aspects of phase transformations in cadmium iodide polytypic crystals have been studied for the first time. It has been shown that the transformation of an ordered polytypic structure into another ordered structure is possible. This fact has been elucidated from the transformation 14H → 4H and 18H → 4H. Electron-microscope evidence for the occurrence of such transformations has been obtained. The phase transformations have also been viewed in the light of the structural geometrical schemes and of the stacking-fault energies of initial and transformed structures. Polytypic transformation from a rhombohedral to a hexagonal type has been observed, 42R→ 12H. Transformations involving poly types having similar stacking-fault configurations in their layer sequences have also been studied. The observed transformations of this type are 28H → 4H and 36H → 4H.
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