X-ray crystallographic structures of two lamotrigine analogues: (I) 3,5-diamino-6-(2-chlorophenyl)-1,2,4-triazine water solvate and (II) 3,5-diamino-6-(3,6-dichlorophenyl)-1,2,4-triazine methanol solvate

The X-ray crystal structures of two lamotrigine derivatives (I) 3,5-diamino-6-(2-chlorophenyl)-1,2,4-triazine, C9H8ClN5, (465BL) as a hydrate, and (II) 3,5-diamino-6-(3,6-dichlorophenyl)-1,2,4-triazine, C9H7Cl2N5, (469BR) as a methanol solvate, have been carried out at liquid nitrogen temperature and room temperature, respectively. A detailed comparison of the two structures is given. Both are centrosymmetric with (I) in the orthorhombic space group Pbca, a = 12.2507(3), b = 15.7160(6), c = 21.71496(9) angstrom, Z = 16, and (II) in the monoclinic space group C2/c, a = 38.553(3), b = 4.9586(2), c = 14.546(2) angstrom, beta = 111.59(1)degrees, Z = 8. Final R indices [I > 2sigma(I)] for (I) are R1 = 0.0670, wR2 = 0.1515 and for (II) R1 = 0.0434, wR2 = 0.1185. Structure (I) has water of crystallization in the lattice and (II) includes a solvated CH3OH. Structure (I) is characterized by having two crystallographically independent molecules, A and B, of 465BL, per asymmetric unit. Molecule B has a very unusual feature in that the 2-chlorophenyl ring is statistically disordered, occupying site (1) in 87.5% of the structure and site (2) in 12.5% of the structure. Sites (1) and (2) are related by an exact 180 degrees pivot of the phenyl ring about the ring linkage bond. The presence of two independent molecules per asymmetric unit provides an ideal opportunity for the conformational flexibility of the molecule 465BL to be studied. Structure (I) also includes a further unusual feature in that the lattice contains one fully occupied water molecule and an additional solvated water which is only 33% occupied.

Low temperature X-ray crystallographic structures of two lamotrigine analogues: (I) 2-methyl,3-amino, 5-imino-6-(2,3-dichlorophenyl)-1,2,4-triazine water solvate and (II) 2-methyl,3,5-diamino-6-(2,3-dichlorophenyl)-1,2,4-triazine isethionate, hemi-hydrate

The X-ray crystal structures of two lamotrigine derivatives (I) 2-methyl, 3-amino, 5-imino-6-(2, 3-dichlorophenyl)-1,2,4-triazine, C10H9Cl2N5, as the hemi hydrate and (II) 2-methyl,3,5-diamino-6-(2,3-dichlorophenyl)-1,2,4-triazine, C10H10Cl2N5, as the isethionate-water solvate, have been carried out at liquid nitrogen temperature. A detailed comparison of the two structures is given. Both are monoclinic and centrosymmetric, with (I) in space group C2/c, and (II) in space group P2(1)/n. For (I) the unit cell dimensions are a = 19.5466(10), b = 7.5483(4), c = 15.7861(8) angstrom, beta = 91.458(3)degrees, volume = 2328.4(2) angstrom(3), Z = 8, density = 1.590 Mg/m(3); for (II). For (II) the unit cell dimensions are a = 6.0566(2), b = 11.0084(4) c = 23.9973(9) angstrom, beta = 92.587(3)degrees, volume = 1598.35(10) angstrom(3), Z = 4, density = 1.597 Mg/m(3). For (I) final R indices [I > 2sigma(I)] are R1 = 0.0356, wR2 = 0.0782 and R indices (all data) are R1 = 0.0424, wR2 = 0.0817. For (II) final R indices [I > 2sigma(I)] are R1 = 0.0380, wR2 = 0.0871 and R indices (all data) R1 = 0.0558, wR2 = 0.0949. Both structures have a molecule of water of crystallization and (II) also includes a solvated CH3SO3. Comparisons are made between the two structures. Structure (I) is very unusual in having a = NH group at position C5' on the triazine ring. No other examples of this particular substitution, which is usually -NH2, have been reported.

X-ray crystallographic structures of neuroprotective pyrimidine derivatives: (I) the mesylate salt of BW1003C87 and (II) sipatrigine base

Drugs based on 5-phenyl-2,4 diamino pyrimidine and 6-phenyl-1,2,4 triazine derivatives are well known for their effects on the central nervous system. The study presented here provides detailed crystal structures of two pyrimidine derivatives which have neuroprotective properties in models of both grey and white matter ischemia. Recently published studies suggest that the compounds lamotrigine (a triazine derivative), and the two pyrimidines BW1003C87 (I) and sipatrigine (II) mediate their primary in vivo mode of action by inhibiting voltage-gated Na+ channels. The X-ray crystal structures will contribute valuable data for applications involving binding and modelling studies of the biological actions of these drugs.

An Electron-Microscope X-Ray-Diffraction And Amino-Acid-Analysis Study Of The Opercular Filament Cuticle Calcareous Opercular Plate And Habitation Tube Of Pomatoceros Lamarckii Quatrefages (Polychaeta Serpulidae)

The structure, X-ray diffraction and amino acid compositions of the opercular filament cuticle, calcareous opercular plate and habitation tube of the polychaete serpulid, Pomatoceros lamarckii quatrefages, are reported. The opercular filament cuticle is made up of protein and chitin. The chitin is probably in the crystallographic α form. The structure and amino acid composition of the organic components of the opercular filament cuticle and calcareous opercular plate have similarities but are distinctly different from those of the calcareous habitation tube. The opercular plate and habitation tube are composed of different polymorphs of calcium carbonate, aragonite and calcite respectively. Comparisons are made with other chitin-protein systems, structural and calcified proteins.

An investigation into the subambient behavior of aqueous mannitol solutions using differential scanning calorimetry, cold stage microscopy, and X-ray diffractometry

The subambient behavior of aqueous mannitol solutions is of considerable relevance to the preparation of freeze dried formulations. In this investigation the properties of 3% w/v mannitol solutions were investigated using differential scanning calorimetry (DSC), cold stage microscopy (CSM), and X-ray diffraction (XRD) to identify the thermal transitions and structural transformations undergone by this system. It was found that on cooling from ambient the system formed ice at circa -20°C while a further exotherm was seen at approximately -30°C. Upon reheating an endotherm was seen at circa -30°C followed immediately by an exotherm at circa -25°C. Temperature cycling indicated that the thermal transitions observed upon reheating were not reversible. Modulated temperature DSC (MTDSC) indicated that the transitions observed upon reheating corresponded to a glass transition immediately followed by recrystallization, XRD data showed that recrystallization was into the ß form. Annealing at -35°C for 40 min prior to cooling and reheating resulted in a maximum enthalpy being observed for the reheating exotherm. It is concluded that on cooling 3% w/v aqueous mannitol solutions an amorphous phase is formed that subsequently recrystallises into the ß form. The study has also shown that DSC, CSM, and XRD are useful complementary techniques for the study of frozen systems

Synchrotron X-ray diffraction study of the phase transformations in titanium alloys

High-resolution synchrotron X-ray diffraction was used to study the phase transformations in titanium alloys. Three titanium alloys were investigated: Ti-6Al-4V, Ti-6Al-2Sn-4Zr-2Mo-0.08Si and beta21s. Both room and high temperature measurements were performed. The room temperature experiments were performed to study the structure of the alloys after different heat treatments, namely as received (AR), furnace cooling (FC), water quenching (WQ) and water quenching followed by ageing. The alpha, alpha', alpha'' and beta phases were observed in different combinations depending on the heat treatment conditions and the alloy studied. A multicomponent hexagonal close packed (hcp) alpha phase, with different c and the same a lattice parameters, was detected in Ti-6Al-4V after FC. High temperature synchrotron X-ray diffraction was used for 'in situ' study of the transformations on the sample surface at elevated temperatures. The results were used to trace the kinetics of surface oxidation and the concurrent phase transformations taking place under different conditions. The influence of the temperature and oxygen content on the lattice parameters of the alpha phase was derived and new data obtained on the coefficients of thermal expansion in the different directions of the hcp alpha phase, for Ti-6Al-4V and Ti-6Al-2Sn-4Zr-2Mo-0.08Si.

An investigation into the use of atomic datasets in simulations of the Ni-like gadolinium x-ray laser

The effect of differing the datasets used in the modelling of the Ni-like Gd x-ray laser (XRL) is examined through the 1.50 hydro-atomic code, EHYBRID. Two atomic datasets, including energy levels and radiative and collisional excitation rates, are used as input data for the code. It is found that the behaviour of the XRL is somewhat different than might be expected from superficial examination of the atomic data. The similarities in the gain profiles at low densities are found to have encouraging implications. in our attempts to model XRLs.

Modeling X-ray photoionized plasmas produced at the Sandia Z-facility

In experiments at the high-power Z-facility at Sandia National Laboratory in Albuquerque, New Mexico, we have been able to produce a low density photoionized laboratory plasma of Fe mixed with NaF. The conditions in the experiment allow a meaningful comparison with X-ray emission from astrophysical sources. The charge state distributions of Fe, Na and F are determined in this plasma using high resolution X-ray spectroscopy. Independent measurements of the density and radiation flux indicate unprecedented values for the ionization parameter xi = 20-25 erg cm s(-1) under nearly steady-state conditions. First comparisons of the measured charge state distributions with X-ray photoionization models show reasonable agreement, although many questions remain.

Plasma-based studies with intense X-ray and particle beam sources

The construction of short pulse (

He-like x-ray line emission from laser irradiated sources

Photon yields for the 1s(2)-1s2p (He-alpha) transition of He- like ions have been measured for laser irradiated, thin foils of Ti, V and Fe. The laser pulses were of 0.527 mum wavelength and of either 80 or 300 ps duration. The data shows significant shot-to-shot variation but the Ti data is broadly consistent with previous results. In this work, we extend the previous results to include, new elements, longer pulse lengths and yields measured for emission from both surfaces of the foils. We compare our data to simulations using a hydrodynamic code and a collisional radiative model.