Structure of N-[bis(methylthio)methylene]cinnamamide, C12H13NOS2

M r = 251.34, monoclinic, P21/n, a =14.626 (3), b= 7.144 (1), c= 11.996 (2)\AA \betat=90.03 (2) °, V= 1253.4 (6) \AA 3, Z = 4, Dm= 1.326 (3),Dx=1.331(3)gcm -3, MoKat, \lambda = 0.7107 )\AA , \mu=3.51 cm -3, F(000) = 528.0, T-- 293 K, R -- 3.5% for1455 significant reflections. Of particular interest is an intramolecular attractive interaction between the sulphur and oxygen atoms with an S...O distance of 2.658 (3)\AA, in which the oxygen atom appears to actas a nucleophile.

3,3',5,5'-Tetrabromophenolsulfonphthalein (bromphenol blue), C19H10Br4O5S

M r=670.02, monoclinic, C2/c, a= 31.003(4), b=11.037(2), c=21.183(3)A, fl= 143.7 (1) °, V= 4291.2/k 3, D,n = 2.06, D x = 2.07Mgm -3, Z=8, MoKa, 2=0.7107/k, /~=7.45 mm -1, F(000) = 2560, T= 293 K, R = 0.061 for 1697 observed reflections. The bromphenol blue molecule consists essentially of three planar groupings: the sulfonphthalein ring system and two dibromophenol rings attached to the tetrahedral C atom of the five-membered ring of the sulfonphthalein system. The dibromophenol rings are inclined with resPect to each other at 73 ° whereas they make angles of 85 and 68 ° with respect to the sulfonphthalein system. The molecules aggregate into helical columns with the non-polar regions of the molecules in the interior and the polar regions on the surface. The columns are held together by a network of hydrogen bonds.

4-Biphenylyl phenyl thioketone (I), C19H14S, and 1-naphthyl phenyl thioketone (II), C17H12S

(I): Mr=274"39, orthorhombic, Pbca, a = 7.443 (1), b= 32.691 (3), c= 11.828 (2)A, V= 2877.98A 3, Z=8, Din= 1.216 (flotation in KI), D x = 1.266 g cm -3, /~(Cu Ka, 2 = 1.5418 A) = 17.55 cm -1, F(000) = li52.0, T= 293 K, R = 6.8%, 1378 significant reflections. (II): M r = 248.35, orthorhombic, P212~21, a = 5.873 (3), b = 13.677 (3), c = 15-668 (5) A, V = 1260.14 A 3, Z = 4, D,n = 1.297 (flotation in KI), Dx= 1.308 g cm -a, /t(CuKa, 2=1.5418 A) = 19.55 cm -~, F(000) = 520.0, T= 293 K, R = 6.9%, 751 significant reflections. Crystals of (I) and (II) undergo photo-oxidation in the crystallinestate. In (I) the dihedral angle between the phenyl rings of the biphenyl moiety is 46 (1) °. The C=S bond length is 1.611(5) A in (I) and 1.630 (9)/~ in (II). The correlation between molecular packing and reactivity is discussed.

The Structure of Monosodium Phosphoenolpyruvate

CDH406P-.Na +.H20 , M r = 208.0, is monoclinic, Cc, a = 11.423 (2), b = 23.253 (5), c - 6.604 (1) A, fl = 123.63 (1) °, U = 1460.6 A 3, D x =. 1.89 Mg m -a, Z = 8, 2(Mo Ka) = 0.7107 A, p(Mo Ka) = 0.44 mm -~, F(000) = 840. Final R = 0.063 for 1697 reflections.The two crystallographically independent molecules of phosphoenolpyruvate (PEP) (A and B) are almost mirror images of each other, the mirror being the planar enolpyruvate group. The torsion angle C(3)-C(2)- O(1)-P(1) is 122.6 in A and -112.0 ° in B, in contrast to -209.1 ° in PEP.K. The enolic C(2)-O(1) has a partial double-bond character [1.401 (A), 1.386A (B)]. The high-energy P~O bond (1.595 and 1.610A) is comparable to that in PEP.K (1.612 A). Na(1) has six nearest neighbours while Na(2) has only five. The Na + ions are involved in binding only the phosphates of different molecules, in contrast to the K ÷ ion in PEP. K, which binds to both the phosphate and carboxyl ends of the same molecule. The planar carboxyl groups stack on each other at an average distance of 3.2 A instead of forming hydrogen-bonded dimers usually found in carboxylate structures.

Peptide-lanthanide interactions. Crystal structure of a europium(III)-triglycine complex

Crystals of Eu-(Gly-Gly-Gly).(H2O)5.(ClO4)3 are triclinic, spacegroup P1BAR with a = 9.123 (2), b = 11.185 (5), c = 11.426 (2) angstrom; alpha = 90.79 (2), beta = 98.08 (1), gamma = 98.57 (2)-degrees; Z = 2. The europium cation is surrounded by four oxygens from three different peptide units and four oxygens from water molecules. The geometry around the metal is a distorted bi-capped trigonal prism. The peptide backbone conformation in this complex is compared with those in the free peptide and in various metal complexes. Considerable differences are observed between Eu(III) and Ca(II) complexes of triglycine. (C) Munksgaard 1994.

Crystal structure of 8-methoxy-3-dibromoacetylcoumarin, C12H8Br2O4

C12H8BT2O4. monoclinic, P12(1)/cl (No. 14), a = 11.546(2) Angstrom, b = 6.885(4) Angstrom,= 15.949(3) Angstrom, beta = 101.75(2)degrees, V= 1241.3 Angstrom(3), Z = 4, p(m) = 2.040 g.cm(-3), R-all(F) = 0.039, wR(all)(F) = 0.043, T = 300 K.

Crystal structure of cadaverine dihydrochloride monohydrate

The structure of cadaverine dihydrochloride monohydrate has been determined by X-ray crystallography with the following features: NH3+(CH2)5NH3+.2Cl-.H2O, formula weight 191.1, monoclinic, P2, a = 11.814(2) angstrom, b = 4.517(2) angstrom, c = 20.370(3) angstrom, beta = 106.56-degrees(1): V = 1041.9(2) angstrom3, lambda = 1.541 angstrom; mu = 53.4 1; T = 296-degrees; Z = 4, D(x) = 1.218 g.cm-3, R = 0.101 for 1383 observed reflections. The crystal is highly pseudosymmetric with 2 molecules of cadaverine, 4 chloride ions and 2 partially disordered water molecules present in the asymmetric unit. Though both the cadaverine molecules in the asymmetric unit have an all trans conformation, the carbon backbones are slightly bent. Between the concave surfaces of two bent cadaverine molecules exists water channels all along the short b axis. The water molecules present in the channels are partially disordered

Synthesis, spectral and structural studies on metal complexes of Schiff bases involving vitamin B6 and histamine

Six metal complexes of Schiff bases involving Vitamin B6 and the decarboxylated amino acid histamine have been synthesised and characterized. Crystal structures have been determined for [CuL1(H2O)Br]-NO31(L1= pyridoxylidenehistamine) and [Cu2L22(NO3)2]·6H2O 2(L2= 5′-phosphopyridoxylidenehistaminate). The crystal structure of complex 1[space group P[1 with combining macron], a= 8.161(2), b= 10.368(2), c= 11.110(2)Å, α= 105.18(1), β= 102.12(1), γ= 72.10(1)° and Z= 2; R= 0.072, R′= 0.083] consists of square-pyramidally co-ordinated copper with the tridentate Schiff base in the zwitterionic form, whereas in 2[space group P[1 with combining macron], a= 8.727(1), b= 10.308(1), c= 12.845(2)Å, α= 110.00(1), β= 78.94(1), γ= 114.35(1)° and Z= 1; R= 0.035, R′= 0.034] the copper has the same co-ordination geometry but the tetradentate Schiff-base ligand exists as a monoanion. The conformational parameters deduced from such structures are important for understanding the stereochemical aspects of Vitamin B6-catalysed model reactions involving histidine.

Studies on ß-arylhydrazone-imine nickel(II) complexes—Examples of metal template syntheses

ß-arylhydrazone-imine ligand complexes of nickel(II), namely, 4,10-dimethyl-5,9-diazatrideca-4,9-diene-2,12-dione-3,11-diphenylhydrazonato nickel(II), Ni(acacpn)(N2Ph-R)2 and 1,11-diphenyl-3,9-dimethyl-4,8-diazaun-deca-3,8-diene,1,11-dione-2,10-diphenyl hydrazonato nickel(II), Ni (beacpn) (N2Ph-R)2, [R = H, o-CH3p-CH3] have been prepared by metal template reactions and characterized. Both the azomethine nitrogens and α-nitrogens of bis-hydrazone form the coordination sites of the square-planar geometry around the nickel(II) ion. Loss of CO from the molecule and subsequently an interesting methyl group migration to the nucleus of the chelate ring have been observed in the mass spectrum. Structures are proposed based on the spectral and magnetic properties.

Crystal and molecular structure of Boc-Phe-Val-OMe; comparison of the peptide conformation with its dehydro analogue

The crystal structure of the peptide Boc-Phe-Val-OMe determined by X-ray diffraction methods is reported in this paper. The crystals grown from aqueous methanol are orthorhombic, space group P2(1)2(1)2(1), a = 11.843(2), b = 21.493(4), c = 26.676(4)Angstrom and V = 6790 Angstrom(3). Data were collected on a CAD4 diffractometer using MoK2 radiation (lambda = 0.7107 Angstrom) up to Bragg angle theta = 26 degrees. The structure was solved by direct methods and refined by a least-squares procedure to an R value of 6.8% for 3288 observed reflections. There are three crystallographically independent peptide molecules in the asymmetric unit. All the three molecules exhibit extended conformation. The sidechain of the Val(2) residue shows two different conformations. The conformation of the peptide Boc-Phe-Val-OMe is compared with the conformation of Ac-Delta Phe-Val-OH. It is observed that while Boc-Phe-Val-OMe exhibits an extended conformation, Ac-Delta Phe-Val-OH shows a folded conformation. The results of this comparison highlight the conformation constraining property of the Delta Phe residue. Interestingly, even though Boc-Phe-Val-OMe and Ac-Delta Phe-Val-OH are conformationally different, they exhibit similar packing patterns in the solid state. (C) Munksgaard 1995.

Structure of 7-ethylamino-6-methyl-4-trifluoromethylcoumarin

C13H12F3NO2, M(r) = 271.2, triclinic, P1BAR, a = 5.029 (2), b = 7.479 (2), c = 17.073 (5) angstrom, alpha = 97.98 (2), beta = 95.54 (3), gamma = 103.62 (3)-degrees, V = 612.4 (4) angstrom 3, Z = 2, D(m) = 1.463, D(x) = 1.471 g cm-3, lambda(Mo K-alpha) = 0.71069 angstrom, mu = 1.23 cm-1, F(000) = 280, T = 298 K, final R value is 0.041 for 2047 observed reflections with \F(omicron)\ greater-than-or-equal-to 6-sigma(\F(omicron)\). The N-C(sp2) bond length is 1.356 (2) angstrom. The N and C atoms of the ethylamino group deviate by < 0.15 angstrom from the plane of the aromatic ring. Short intramolecular contacts, C(3)...F(17) 2.668 (3) angstrom [H(3)...F(17) 2.39 (2) angstrom, C(3)-H(C3)...F(17) 98 (1)-degrees], C(5)...F(18) 3.074 (3) and C(5)...F(19) 3.077 (3) angstrom exist in the structure. The crystal structure is stabilized by intermolecular N-H...O hydrogen bonds with N(12)-H(N12) 0.79 (3), H(N12)...O(11)' 2.36 (3), N(12)...O(11)' (x - 1, y + 1, z) 3.105 (3) angstrom and N(12)-H(N12)...O(11)' 155 (2)-degrees.

Structure of diaquadichlorobis(hydrazinium)iron(II) dichloride

[Fe(N2H5)2(H2O)2Cl2].Cl2, M(r) = 299.65, monoclinic, P2(1)/c, a = 8.027 (1), b = 5.725 (2), c = 11.430 (2) angstrom, beta = 97.08 (1)-degrees, V = 521.3 (2) angstrom 3, Z = 2, D(m) = 1.92, D(x) = 1.910 g cm-3, lambda(Mo K-alpha) = 0.71069 angstrom, mu = 24.5 cm-1, F(000) = 304, T = 295 K, final R = 0.0242 and wR = 0.0292 for 1411 significant [F(o) > 5.0-sigma(F(o))] reflections. The crystal contains discrete Cl- ions and complex [Fe(N2H5)2(H2O)2Cl2]2+ cations. In the complex cation, the Fe atom is bonded to two hydrazinium cations, two Cl atoms and two water molecules. The coordinated atoms are trans to each other. The ions are connected by both N-H...Cl and O-H...Cl type hydrogen bonds.

Solid Oxide-Ion Electrolytes

Solid oxide-ion electrolytes find application in oxygen sensors, oxygen pumps and in high-temperature electrolyser-fuel-cell hybrid systems. All the solid electrolytes known so Qr, however, exhibit: tow oxide-ion conductivities below 973 K. Therefore, there is a need for fast oxide-ion conductors operative at temperatures around 673 K, Recently, efforts have been directed towards developing such materials. This article summarizes various type of oxide-ton electrolytes reported in literature and outlines a strategy for the identificatiom/synthesis of improved materials.

Role of two consecutive alpha,beta-dehydrophenylalanines in peptide structure: Crystal and molecular structure of Boc-Leu-Delta Phe-Delta Phe-Ala-Phe-NHMe

An N-alpha-protected model pentapeptide containing two consecutive Delta Phe residues, Boc-Leu-Delta Phe-Delta Phe-Ala-Phe-NHMe, has been synthesized by solution methods and fully characterized. H-1-nmr studies provided evidence for the occurrence of a significant population of a conformer having three consecutive, intramolecularly II-bonded beta-bends in solution. The solid state structure has been determined by x-ray diffraction methods. The crystals grown from aqueous methanol are orthorhombic, space group P2(1)2(1)2(1),, a = 11.503(2), b = 16.554(2), c = 22.107(3) Angstrom, V = 4209(1) Angstrom,(3) and Z = 4. The x-ray data were collected on a CAD4 diffractometer using CuKalpha radiation (lambda = 1.5418 Angstrom). The structure was determined using direct methods and refined by full-matrix least-squares procedure. The R factor is 5.3%. The molecule is characterized by a right handed 3(10)-helical conformation ((phi) = -68.2 degrees (psi) = -26.3 degrees), which is made up of two consecutive type III beta-bends and one type I beta-bend. In the solid state the helical molecules are aligned head-to-tail, thus forming long rod like structures. A comparison with other peptide structures containing consecutive Delta Phe residues is also provided. The present study confirms that the -Delta Phe-Delta Phe-sequence can be accommodated in helical structures. (C) 1997 John Wiley & Sons, Inc.

GC-MS study of Artabotrys odoratissimus fatty oil (leaves)

GC-MS study of two fatty oil fractions from Artabotrys odoratissimus (leaves) indicated the presence of fifteen compounds namely, nonanoic acid; methyl phenyl propanoate; decanoic acid; diethyl phthalate; dibutyl phthalate; 2 - amino-3-ethyl biphenyl; 5-methyl-9-phenylnonan-3-ol; hexadeca-2,7,11-triene; 2,6-dimethyl-1-phenylhepta-1-one; 2,5-dimethyltetradecahydrophenenthrene; 1-phenylundecane; 1-isopropyl-4,6-dimethyl naphthalene; 5-(2-butyl phenyl)pent-3-en-2-ol; 1-phenyideca-1-one and 1-phenylundecan-1-one. Some of the compounds are rare occurring and biologically active.