Synthesis and crystal structures of 5-amino-1-(2-hydroxyethyl)imidazole-4-carboxamide and 5-amino-1-(2-chloroethyl)-4-cyanoimidazole

Both 5-amino-1-(2-hydroxyethyl)imidazole-4-carboxamide (AHIC) and 5-amino-1-(2-chloroethyl)-4-cyanoimidazole (ACCI) have been synthesized and crystallized in the monoclinic space group P2₁/c, Z = 4, with a = 8.420(2), b = 9.759(2), c = 10.583(2) Å, = 111.80(2)° for AHIC and a = 6.139(1), b = 8.522(2), c = 15.156(3) Å, = 96.71(2)° for ACCI. Differences in the molecular geometries of the two compounds are attributed to the differences in the substituents at the 1- and 4-positions of the imidazole ring. The molecular conformation of AHIC is stabilized by intramolecular hydrogen bonding between the 5-amino and the vicinal carboxamide moiety, resulting in an extended planar structural pattern. The presence of the cyano group in the 4-position of ACCI prevents the formation of such an intramolecular hydrogen bond. Both the crystal structures are stabilized by networks of intermolecular hydrogen bonds.     

Tests of QCD at LEP

The four experiments, ALEPH, DELPHI, L3 and OPAL at LEP, have performed a large number of precise measurements to test Quantum Chromodynamics. The strong coupling constant has been measured with high precision:α _s (M_z) = 0.123±0.004. The coupling constant has been found to be independent of quark flavour. The running ofα _s has been demonstrated by the data. Second order QCD matrix element calculations have been tested from several measured distributions in 3-jet and 4-jet events. These distributions give evidence of the vector nature of the gluon and provide measurements of the QCD colour factors. The hadronic distributions are well reproduced by QCD Monte Carlo programs as well as by analytical calculations with soft gluon coherence effects.     

Hydroxamic acid dinuclear complexes of molybdenum(V) and molybdenum(III)

Summary Molybdenum(V) and molybdenum(III) complexes [Mo₂O₃L₄] and [Mo₂L₆] derived from hydroxamic acids (HL) were prepared and identified by Raman, i.r., e.s.r., electronic spectra and analytical data. The low magnetic moments of the dinuclear complexes are due to in part to intramolecular interactions. Electronic spectra and vibrational studies indicate the presence of a Mo₂O₃ core in the molybdenum(V) complexes. The relative intensities of the, main and satellite peaks in e.s.r. spectra indicate the dinulcear nature of molybdenum(III) hydroxamates.     

Alternative Procedure for the Synthesis of (+)-Tavacpallescencine Precursor

A conversion of dimethylbenzo[d]suberone prepared from 5-chlorovaleric acid into butenolide, a precursor of tavacpallescencine, was described.     

Synthesis and Characterization of Nano-Crystalline Fluorine-Doped Tin Oxide Thin Films by Sol-Gel Method

Thin films of fluorine-doped tin-oxide (FTO) were prepared by sol-gel dip-coating technique. Stannous chloride (SnCl₂2H₂O) and hydrogen fluoride (HF) were mixed with isopropyl alcohol to serve as source solution. X-ray diffraction (XRD) spectrum showed all the peaks of the crystalline SnO₂. Analysis of XRD spectrum showed the particle size to be nearly 6 nm, which indicated the nanocrystalline structure of the films. Strain calculation by integral breadth (IB) method from XRD data showed a value of 0.010. UV-Visible spectrophotometric measurement showed high transparency of the films in the visible region and the band gap was calculated to be 3.34 eV. The room temperature resistivity of the films were of the order of 1 cm. Fluorine concentration in the films was determined from energy dispersive X-ray (EDX) study. Current-voltage (I-V) characteristics at high temperatures showed the Poole-Frenkel effect of thermionic emission. SEM study indicated the existence of fine grains in the film. FT-IR spectroscopy showed strong Sn—O and Sn—O—Sn bonding.     

Synthesis,characterisation and crystal structure analysis of bis (pyridine-2-carbaldehyde thiosemicarbazonato) cobalt(III) thio-cyanate monohydrate

The crystal structure of [CoL2](SCN)·H2O (L = pyridine-2-carbaldehyde thiosemicarbazonato) is reported. The structure, along with other physico-chemical studies, establishes that the compound is a low spin CoIII complex. This resolves confusion arising out of an e     

Chemistry of the rhenium-azopyridine family: an oxo parent and derivatives thereof including a novel oxo-imido dimer

The concerned azo ligands are 2-(phenylazo)pyridine (HL) and 2-((p-chlorophenyl)azo)pyridine (ClL). The reaction of KReO4 with HL in hot concentrated HCl is attended with metal reduction and ligand chlorination affording the oxo complex ReVOCl3(ClL), 2, which furnishes ReIII(OPPh3)Cl3(ClL), 3, upon treatment with PPh3. Aromatic amines, ArNH2, convert 2 to the imido complex ReV(NAr)Cl3(ClL), 5, and the unusual oxo-imido dimer (ClL)-Cl2(O)ReVOReV(NAr)Cl2(ClL), 7. The complex ReIII(OPPh3)Cl3(HL), 4, has been generated from ReVOCl3(PPh3)2 and HL. Reaction of 4 with HL has yielded ReV(NPh)Cl3(HL), 6, via azo splitting. The complexes have been characterized with the help spectral, magnetic, and X-ray structural data (2, 3, 5c (Ar = pClC6H4) and 7.CH2Cl2 (Ar = pMeC6H4)). In 2, 3, and 5c the ReCl3 fragment is meridionally disposed, and in 7 the ReCl2 fragments have a trans configuration. The Re-O(oxo) bond, 1.663(6) A, in 2 and Re-N(imido) bond, 1.719(5) A, in 5c are triple bonds. The corresponding bonds are slightly longer in 7 wherein the (O)Re(1)-O(2)-Re(2)(NAr) bridge is angular (151.0(5) degrees) and unsymmetrical, the Re(1)-O(2) bond, 1.849(7) A, having a large double-bond character (Re(2)-O(2), 1.954(7) A). In effect, cis-ReVO2 acts as a monodentate oxygen ligand toward ReVNAr in 7. In all cases the pyridine nitrogen binds trans to the oxo, OPPh3, or NAr donor. Bond length data are consistent with the presence of substantial d(Re)-pi*(azo) back-bonding. In acetonitrile solution the complexes display electrochemical one-electron metal (ReVI/ReV or ReIV/ReIII) and azo redox. The imido ligand in 5 stabilizes the ReVI state (E1/2 approximately 1.4 V) better than the oxo ligand in 2 (approximately 1.9 V). Parallely it is more difficult to reduce the azo group in 5 (approximately -0.4 V) than in 2 (approximately 0.0 V). In 7 the metal (approximately 1.0 V) and azo (approximately -0.4 V) couples correspond to the imido and oxo halves, respectively. The significantly higher (by 0.2-0.6 V) metal reduction potentials of the azopyridine compared to pyridine-2-aldimine complexes is ascribed to the superior pi-acidity and electron-withdrawing character of the azo function relative to the aldimine function. This also makes the transfer of the ReVO oxygen function much more facile under azopyridine chelation as in 2. For the same reason, ReOCl3(PPh3)2 reacts with HL affording only 4 while it reacts with pyridine-2-aldimines furnishing oxo species. Crystal data for the complexes are as follows: 2, empirical formula C11H8Cl4N3ORe, crystal system triclinic, space group P1, a = 7.118(4) A, b = 8.537(4) A, c = 13.231(9) A, alpha = 79.16(5) degrees, beta = 78.03(5) degrees, gamma = 70.96(4) degrees, V = 737.2(7) A3, Z = 2; 3, empirical formula C29H23Cl4N3OPRe, crystal system monoclinic, space group P2(1)/n, a = 11.264(2) A, b = 15.221(3) A, c = 17.628(4) A, beta = 94.21(3) degrees, V = 3014(1) A3, Z = 4; 5c, empirical formula C17H12Cl5N4Re, crystal system triclinic, space group P1, a = 9.683(3) A, b = 10.898(3) A, c = 11.522(3) A, alpha = 63.67(2) degrees, beta = 71.24(2) degrees, gamma = 86.79(2) degrees, V = 1026(1) A3, Z = 2; 7.CH2Cl2, empirical formula C30H25Cl8N7O2Re2, crystal system triclinic, space group P1, a = 12.522(6) A, b = 12.857(8) A, c = 13.182(7) A, alpha = 67.75(4) degrees, beta = 88.30(4) degrees, gamma = 82.09(4) degrees, V = 1945(2) A3, Z = 2.