Structure of the disodium salt of glucose 1-phosphate hydrate, 2Na+.C6H11O9P2-.3.5H2O

Mr= 367.2, monoclinic, C2, a = 8.429 (1),b= 10.184(2), c= 16.570(2)A, /~= 99.18 (1) °, U= 1404.2 A 3, z = 4, D m = 1.73, D x = 1.74 Mg m -3,Cu K~, 2 = 1.5418 A, g = 2.99 mm -1, F(000) = 764,T= 300K, final R for 1524 observed reflections is0.069. The endocyclic C-O bonds in the glucose ring are nearly equal with C(5)-O(5)= 1.445 (10) and C(1)-O(5)= 1.424(10). The pyranose sugar ring adopts a 4C 1 chair conformation. The conformation about the exocyclic C(5)-C(6) bond is gauche-gauche, in contrast to gauche-trans observed in the structure of the dipotassium salt of glucose 1-phosphate. The phosphate ester bond, P-O(1), is 1.641 (6)A, slightly longer than the 'high-energy' P-,.O bond in the monopotassium salt of phosphoenolpyruvate [1.612 (6)A]. Two sodium ions are six coordinated while the third has only five neighbours.

Low temperature synthesis and hcaracterization of Ag2S1-x Tez(O

A low-temperature route for the synthesis of Ag2S,Ag2Te and their solid solutions Ag2S1-xTex(0 less-than-or-equal-to x less-than-or-equal-to 1) is reported. Ag2S is prepared by the direct addition of silver nitrate solution to thiourea, while Ag2Te is prepared by reacting silver nitrate solution with tellurium in nitric acid and subsequently reducing it with hydrazine hydrate. The solid solutions of Ag2S and Ag2Te are obtained by the addition of nitrate solutions of silver and tellurium to thiourea followed by its reduction with hydrazine hydrate. The method enables the synthesis of low-temperature crystalline phase of Ag2S1-xTex solid solutions. The powder X-ray diffraction studies suggest that the solid solutions of compositions x < 0.3 have a phase akin to alpha-Ag2S and those with compositions x > 0.6 are similar to alpha-Ag2Te. In the intermediate range of compositions (x = 0.4 and 0.5), the solid solutions are found to be mixtures of alpha-Ag2S and alpha-Ag2Te phases which transform totally to alpha-Ag2S phase on prolonged annealing at about 473 K.

Crystal Structure, Thermal Expansion and ElectricaH Conductivity of Yo.sCao.2Fel-x Mnx03+o (0 < x < 1.0)

The crystal structure, thennal expansion and electrical conductivity of the solid solutions YOgCao.2Fel-x MnxOJ+c5 (0 ~ x ~ 1.0) were investigated. All compositions had the GdFeOrtype orthorhombic perovskite structure with trace amounts of a second phase present in case of x = 0.8 and 1.0. The lattice parameters were detennined at room tempe'rature by using X-ray powder diffraction (XRPD). The pseudocubic lattice constant decreased with increasing x. The average I inear thermal expansion coefficient (anv) in the temperature range from 673 to 973 K showed negligible change with x up to x = 0.4. The thennal expansion curve for x = I had a slope approaching zero in the temperature range from 648 to 948 K. The calculated activation energy values for electrical conduction indicate that conduction occurs primarily by the small polaron hopping mechanism. The drastic drop in electrical conductivity for a small addition of Mn (0 ~ x ~ 0.2) is caused by the preferential fonnation of Mn4t ion~ (rather than Fe4 +) which act as carrier traps. This continues till the charge compensation for the divalent ions on the A-site is complete. The results indicate that with further increase in manganese content (beyond x =0.4) in the solid solutions, there is an increase in exc :::ss oxygen and consequently, a small increase in Mn'll il>I1~, which are charge compensated by the formation of cation vancancies.

Synthesis and Antileukemic Activity of Novel 2-(4-(2,4-dimethoxybenzoyl)phenoxy)-1-(4-(3-(piperidin-4-yl)propyl)piper idin-1-yl)ethanone Derivatives

A series of novel 2-(4-(2,4-dimethoxybenzoyl)phenoxy)-1-(4-(3-(piperidin-4-yl)propyl) piperidin-1-yl)ethanone derivatives 9(ae) and 10(ag) were synthesized and characterized by 1H NMR, IR, mass spectral, and elemental analysis. These novel compounds were evaluated for their antileukemic activity against two human leukemic cell lines (K562 and CEM) by using the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazoliumbromide assay. Some of the tested compounds showed good antiproliferative activity with IC50 values ranging from 1.6 to 8.0 mu m. Compound 9c, 9e, and 10f with an electron-withdrawing halogen substituent at the para position on the phenyl ring showed excellent in vitro potency against tested human leukemia cells (K562 and CEM).

X-ray Structure of Gelonin at 1.8 Å Resolution

Gelonin is a single chain ribosome inactivating protein (RIP) with potential application in the treatment of cancer and AIDS. Diffraction quality crystals grown using PEG3350, belong to the space group P2(1), with it a = 49.4 Angstrom b = 44.9 Angstrom, c = 137.4 Angstrom and beta = 98.4 degrees, and contain two molecules in the asymmetric unit. Diffraction data collected to 1.8 Angstrom resolution has a R(m) value of 7.3%. Structure of gelonin has been solved by the molecular replacement method, using ricin A chain as the search model. Crystallographic refinement using X-PLOR resulted in a model for which the r.m.s deviations from ideal bond lengths and bond angles are 0.012 Angstrom and 2.7 degrees, respectively The final R-factor is 18.4% for 39,806 reflections for which I > 1.0 sigma(I).The C-alpha atoms of the two molecules in the asymmetric unit superpose to within 0.38 Angstrom for 247 atom pairs. The overall fold of gelonin is similar to that of other RIPs such as ricin A chain and alpha-momorcharin, the r.m.s.d. for C-alpha superpositions being 1.3 and 1.4 Angstrom, respectively The-catalytic residues (Glu166, Arg169 and Tyr113) in the active site form a hydrogen bond scheme similar to that observed in other RIPs. The conformation of Tyr74 in the active site, however, is significantly different from that in alpha-momorcharin. Three well defined water molecules are located in the active site cavity and one of them, X319, superposes to within 0.2 Angstrom of a corresponding water molecule in the structure of alpha-momorcharin. Any of the three could be the substrate water molecule in the hydrolysis reaction catalysed by gelonin.Difference electron density for a N-linked sugar moiety has been observed near only one of the two potential glycosylation sites in the sequence. The amino acid at position 239 has been established as Lys by calculation of omit electron density maps.The two cysteine residues in the sequence, Cys44 and Cys50, form a disulphide bond, and are therefore not available for disulphide conjugation with antibodies. Based on the structure, the region of the molecule that is involved in intradimer interactions is suggested to be suitable for introducing a Cys residue for purposes of conjugation with an antibody to produce useful immunotoxins.

Exact N-wave solutions of generalized Burgers equations

Exact N-wave solutions for the generalized Burgers equation u(t) + u(n)u(x) + (j/2t + alpha) u + (beta + gamma/x) u(n+1) = delta/2u(xx),where j, alpha, beta, and gamma are nonnegative constants and n is a positive integer, are obtained. These solutions are asymptotic to the (linear) old-age solution for large time and extend the validity of the latter so as to cover the entire time regime starting where the originally sharp shock has become sufficiently thick and the viscous effects are felt in the entire N wave.

Ethyl 1-(2-cyanoethyl)-3,5-dimethyl-1H-indole-2-carboxylate

The title compound, C16H18N2O2, is an important precursor in the synthesis of 1,2,3,4-tetrahydropyrazinoindoles, which show excellent antihistamine, antihypertensive and central nervous system depressant properties. The carbethoxy group attached to C2 and the planar cyanoethyl group attached to N1 make dihedral angles of 11.0(4) and 75.0(3)degrees, respectively, with the mean plane of the indole ring, The C-C=N chain is linear with a bond angle of 179.3 (4)degrees.

3-Phenylisoquinolin-1(2H)-one

The title compound, C15H11NO, consists of a planar isoquinolinone group to which a phenyl ring is attached in a twisted fashion [dihedral angle = 39.44 (4)degrees]. The crystal packing is dominated by intermolecular N-H center dot center dot center dot O and C-H center dot center dot center dot O hydrogen bonds which define centrosymmetric dimeric entitities.

Methyl 1H-1,2,3-triazole-4-carboxylate

The title compound, C4H5N3O2, features an essentially planar molecule (r.m.s. deviation for all non-H atoms = 0.013 angstrom). The crystal structure is stabilized by intermolecular N-H center dot center dot center dot O hydrogen bonds and pi-pi stacking interactions (centroid centroid distance 3.882 angstrom).

1-(4-Chloro-3-fluorophenyl)-2-[(3-phenylisoquinolin-1-yl)sulfanyl]ethanone

In the title compound, C23H15ClFNOS, the isoquinoline system and the 4-chloro-3-fluorophenyl ring are aligned at 80.4 (1)degrees. The dihedral angle between the isoquinoline system and the pendant (unsubstituted) phenyl ring is 19.91 (1)degrees.

2-[2-(Hydroxymethyl)phenyl]-1-phenylethanol

The title compound, C15H16O2, has a dihedral angle of 19.10 (5)degrees between the mean planes of the two benzene rings. There is an intramolecular O-H center dot center dot center dot O hydrogen bond and the C-C-C-C torsion angle across the bridge between the two rings is 173.13 (14)degrees. The molecules form intermolecular O-H center dot center dot center dot O hydrogen-bonded chains extending along the a axis. C-H center dot center dot center dot pi contacts are also observed between molecules within the chains.

3-(1,3-Dioxolan-2-yl)-2-hydrazino-7-methylquinoline

In the title molecule, C13H15N3O2, the dihedral angle between the mean plane of the 1,3-dioxolane group and the 2-hydrazino-7-methylisoquinoline unit is 85.21 (5)degrees. The conformation of the molecule is influenced by bifurcated N-H center dot center dot center dot(O, O) and N-H center dot center dot center dot N intramolecular hydrogen bonds. In the crystal structure, molecules are linked via intermolecular N-H center dot center dot center dot O hydrogen bonds, forming extended chains along [001].

1,3-Dimethyl-2,6-diphenylpiperidin-4-one

In the title moleclue, C19H21NO, the 4-piperidone ring adopts a chair conformation in which the two benzene rings and the methyl group attached to C atoms all have equatorial orientations. In the crystal structure, centrosymmetric dimers are formed through weak intermolecular C-H center dot center dot center dot O hydrogen bonds [the dihedral angle between the aromatic rings is 58.51 (5)degrees].

Thermodynamics of ligand (substrate end product) binding to endoxylanase from Chainia sp. (NCL-82-5-1): isothermal calorimetry and fluorescence titration studies

The binding of xylo-oligosaccharides to Chainia endoxylanase resulted in a decrease in fluorescence intensity of the enzyme with the formation of 1:1 complex. Equilibrium and thermodynamic parameters of ligand binding were determined by fluorescence titrations and titration calorimetry. The affinity of xylanase for the oligosaccharides increases in the order X-2 < X-3 < X-4 less than or equal to X-5. Contributions from the enthalpy towards the free energy change decreased with increasing chain length from X-2 to X-4, whereas an increase in entropy was observed, the change in enthalpy and entropy of binding being compensatory. The entropically driven binding process suggested that hydrophobic interactions as well as hydrogen bonds play a predominant role in ligand binding.