Revisiting the structure of a synthetic somatostatin analogue for peptide drug design

Natural or artificially manufactured peptides attract scientific interest worldwide owing to their wide array of pharmaceutical and biological activities. X-ray structural studies are used to provide a precise extraction of information, which can be used to enable a better understanding of the function and physicochemical characteristics of peptides. Although it is vulnerable to disassociation, one of the most vital human peptide hormones, somatostatin, plays a regulatory role in the endocrine system as well as in the release of numerous secondary hormones. This study reports the successful crystallization and complete structural model of octreotide, a stable octapeptide analogue of somatostatin. Common obstacles in crystallographic studies arising from the intrinsic difficulties of obtaining a suitable single-crystal specimen were efficiently overcome as polycrystalline material was employed for synchrotron and laboratory X-ray powder diffraction (XPD) measurements. Data collection and preliminary analysis led to the identification of unit-cell symmetry [orthorhombic, P212121, a = 18.5453 (15), b = 30.1766 (25), c = 39.798 (4) Å], a process which was later followed by complete structure characterization and refinement, underlying the efficacy of the suggested (XPD) approach.

Reexamination of the crystal structure of semseyite, Pb9Sb8S21

The crystal structure of semseyite, Pb9Sb8S21was successfully refined using a single-crystal specimen from Wolfsberg, Harz, Germany, having chemical composition (EPMA) Pb9.01(1)Sb8.00(3)S21.05(5). The structure belongs to the monoclinicC2/cspace group (a=13.6267(10) Å,b=11.9742(9) Å,c=24.5891(18) Å,β=105.997(3)°,V=3856.8(5) Å3,Z=4,Dc=6.048 g/cm3). Crystal structure refinement with all atoms refined anisotropically converged toR1=4.64% (I>2σ(I)). The crystal structure is built of two subunits (A and B) showing TlSbS2-like topology. Each of them stacks parallel to (001), andc/2 in thickness. Two cation sites (Pb1 and Sb5) located at central part of the subunit, show mixed occupancy behavior as 95% Pb and 5% Sb at the Pb5 site, and 95% Sb and 5% Pb at the Sb1 site, respectively. Each of subunits are related by unit cell-level twinning mechanism “tropochemical cell twinning” with the TlSbS2-like subunits alternatively parallel to (1 1 −4) and (−1 1 4) planes.

Connecting heterogeneous single slip to diffraction peak evolution in high-energy monochromatic X-ray experiments

A forward modeling diffraction framework is introduced and employed to identify slip system activity in high-energy diffraction microscopy (HEDM) experiments. In the framework, diffraction simulations are conducted on virtual mosaic crystals with orientation gradients consistent with Nye's model of heterogeneous single slip. Simulated diffraction peaks are then compared against experimental measurements to identify slip system activity. Simulation results compared against diffraction data measuredin situfrom a silicon single-crystal specimen plastically deformed under single-slip conditions indicate that slip system activity can be identified during HEDM experiments.

Influence of Biaxial Magnetic Field on Martensite Reorientation in Magnetic Shape Memory Alloy

Based on thermodynamics, a constitutive model for magnetic shape memory alloy (MSMA) is developed under biaxial magnetic field. Considering the driving force provided by Gibbs free energy and resistive force during martensite reorientation, a kinetic equation is got. Of special concern is the influence of biaxial magnetic field on martensite reorientation for a Ni2MnGa single-crystal specimen. The theoretical results are in agreement with experimental data. Some useful conclusions can be obtained.

Crystal growth and twinned crystal structure of Sr2CaWO6

Single crystals of Sr2CaWO6 have been prepared by sintering at high temperature. Powder samples were compressed into rods and heated up to 1953 K. This seems a promising new route for further studies of the structure and physical properties of double perovskites. The structural model of Sr2CaWO6 includes a quantitative description of the twinning shown by the diffraction pattern that should be present in almost any single-crystal specimen for this type of compound.

Influence of Temperature on Field-Induced Reorientation Strain in Magnetic Shape Memory Alloy

A constitutive model for magnetic shape memory alloys is developed through a combined consideration of micromechanical and thermodynamic theories. Of special concern is the influence of different temperatures on field-induced reorientation strain for a NiMnGa single-crystal specimen. The theoretical results are found to be in general agreement with experimental data. It is shown that the method is accurate and simple.

Crack Tip Fields in a Single Edge Notched Aluminum Single Crystal Specimen

We report a combined experimental and computational study of a low constraint aluminum single crystal fracture geometry and investigate the near-tip stress and strain fields. To this end, a single edge notched tensile (SENT) specimen is considered. A notch, with a radius of 50μm, is taken to lie in the (010) plane and its front is aligned along the [101] direction. Experiments are conducted by subjecting the specimen to tensile loading using a special fixture inside a scanning electron microscope chamber. Both SEM micrographs and electron back-scattered diffraction (EBSD) maps are obtained from the near-tip region. The experiments are complemented by performing 3D and 2D plane strain finite element simulations within a continuum crystal plasticity framework assuming an isotropic hardening response characterized by the Pierce–Asaro–Needleman model. The simulations show a distinct slip band forming at about 55deg with respect to the notch line corresponding to slip on (11¯1)[011] system, which corroborates well with experimental data. Furthermore, two kink bands occur at about 45deg and 90deg with respect to the notch line within which large rotations in the crystal orientation take place. These predictions are in good agreement with the EBSD observations. Finally, the near-tip angular variations of the 3D stress and plastic strain fields in the low constraint SENT fracture geometry are examined in detail.