Search results for "Proton NMR"

2017

The energy levels of the HOMO/LUMO Frontier orbitals and the electronic properties of phthalocyanine macrocycles can be tuned by the introduction of substituents. Starting from tetrafluorophthalonitrile, we studied the substitution of fluorine atoms by (2-thienyl)ethoxy moieties. An optimization of the experimental conditions (nature and stoichiometry of the alcohol and base, temperature) allowed us to obtain the monoalkoxy derivative with a very good yield. It was fully characterized using 19F and 1H NMR spectroscopies, thermal analysis and X-ray diffraction on single crystals. Then, the corresponding zinc phthalocyanine was synthesized, characterized by means of 19F and 1H NMR spectroscop…

Synthesis and spectroscopic characterization of dimethyl-, di-n-butyl-, di-t-butyl-and diphenyl-tin(iv) derivatives of dipeptides: Crystal and molecu…

1992

The dipeptide complexes R2SnL listed below have been synthesized: (a) Me2SnL; H2L = glycylalanine (H2GlyAla), glycylvaline (H2GlyVal), glycylmethionine (H2GlyMet), glycyltryptophan (H2GlyTrp), glycyltyrosine (H2GlyTyr); (b) nBu2SnL; H2L = H2GlyAla, H2GlyVal; (c) nBu2SnL.H2O; H2L = glycylglycine (H2GlyGly), H2GlyAla; (d) tBu2SnL; H2L = H2GlyAla, H2GlyVal; (e) tBu2SnGlyGly. H2O; (f) Ph2SnL; H2L = H2GlyAla, H2GlyVal, H2GlyTyr, H2GlyTrp; (g) Ph2Sn(HGlyVal)2. The crystal and molecular structures of nBu2SnGl Val have been determined by single-crystal X-ray diffraction. The polyhedron around tin is a distorted trigonal bipyramid, analogous to that of Et2SnGlyTyr (see Vornefeld et al., Appl. Organo…

119Sn mössbauer, IR, 1H NMR spectroscopic and thermal decomposition studies on organotin(IV) adducts with glycylglycine

1985

Abstract The complexes R2SnCl2·(H2glygly), (H2glygly = glycylglycine) (R = Me, Bun, Octn, Ph) and RSnCl3·(H2glygly)

Electronic characterisation of the oxidized state of the blue copper protein Rusticyanin by 1 H NMR: Is the axial methionine the dominant influence f…

2001

The oxidized state of rusticyanin, the blue copper protein with the highest redox potential in its class, has been investigated through (1)H nuclear magnetic resonance applied to its cobalt(II) derivative. The assignment of the protons belonging to the coordinated residues has been performed. Many other amino acids situated in the vicinity of the metal ion, including six hydrophobic residues (isoleucine140 and five phenylalanines) have also been identified. The orientation of the main axes of the magnetic susceptibility tensor for the cobalt(II)-rusticyanin as well as its axial, Deltachi(ax), and rhombic, Deltachi(rh), magnetic susceptibility anisotropy components have been determined. A co…

A theoretical and experimental study of the racemization process of hexaaza[5]helicenes

2014

A dynamic 1H NMR study, together with DFT calculations, of bis-([1,2,3]triazolo)[1,5-a:5′,1′-k][1,10]phenanthroline 2 has allowed to identify the ring and open forms of a new example of ring/chain tautomerism, as well as their interconversion barriers (ring/ring and ring/open). The barrier of the exchange process between the chain forms and the ring form was found higher than the 'racemization' process in the closed form, so the ring opening does not contribute to the 'racemization'. The di-1,10-methyl and di-1,10-iodo derivatives have been prepared and their properties calculated.

Conformational mobility of thianthrene-5-oxide.

2005

[reaction: see text] Data on the apparent dipole moment of thianthrene-5-oxide (1) and (1)H NMR spectra in different solvents support the conformational mobility of 1, which flaps between two limit boat conformations with the sulfinyl group in pseudoequatorial and pseudoaxial positions, respectively. The conformational equilibrium of 1 occurs too fast for the (1)H NMR (500 MHz) time-scale even at -130 degrees C, and the equilibrium constant has not been determined. The apparent dipole moments of 1 in n-hexane and 1,4-dioxane and the (1)H NMR spectra of 1 and the model compounds cis- and trans-thianthrene-5,10-dioxides (2) and thianthrene (5) in different solvents and at various temperatures…

13C NMR, 1H NMR and IR spectra of a series of monochloroesters of aliphatic short chain carboxylic acids

1981

Abstract 13 C chemical shifts for 14 isomeric monochloroesters of aliphatic carboxylic acids from propanoic acid to hexanoic acid have been determined. Comparisons are made with the literature values for methyl monochloro-octanoate isomers. Substituent effects for all positions are given. Characteristic IR absorption bands are presented and comparisons are made with regard to the isomeric structure. Connections are suggested between observed trends in IR absorption frequencies and some “abnormal” chlorine substituent effects on 13 C chemical shifts. 1 H NMR spectra of these compounds are considered.

Spektroskopische analyse mehrfacher methacrylsäureester von oligo[(2-hydroxy-1,3-phenylen)methylen]en mittels UV-, IR-, 1H NMR- und massenspektren

1977

The structures of two homologous series of oligo[(2-hydroxy-1,3-phenylene)methylene]s completely esterified with methacrylic acid, were spectroscopically analysed. The molar decadal absorption coefficients of ultraviolet absorption maxima of the two homologous series confirm Hunter's relation. The vinylidene, ester, and substitution bands of the infrared spectra as well as the mass spectra agree with the accepted structures. The 1H NMR spectra permit to differentiate between exterior and interior groups of the molecules.

Combined study of anion recognition by a carbazole-based neutral tripodal receptor in a competitive environment

2012

Anion recognition studies have been carried out on a series of neutral synthetic receptors in which carbazole-2-carboxamide has been used as building block. Different ligands which include one to three carbazole units in their structure have been prepared. Binding experiments have been performed under competitive conditions in DMSO and DMSO-water solutions. The tripodal receptor offered a better host-guest association due to the synergistic effect of a well arranged set of hydrogen bonds. A selective response towards the biologically important pyrophosphate anion has been achieved. This selectivity is enhanced when studies are carried out with an increasing water content, which gets as high…

NMR spectral and X-ray structural investigation of 1,3-bis(2-quinolyl)-2-(p-chlorophenyl)-2-propanol

2000

Abstract 1,3-Bis(2-quinolyl)-2-(p-chlorophenyl)-2-propanol (BQCP) has been prepared and characterised by 1H, 13C, 15N NMR spectral and X-ray structural parameters. The methylene protons of BQCP are diastereotopic in solution (CDCl3) as revealed by 1H NMR. In crystalline state there exists an intramolecular hydrogen bond O–H⋯N with one of two nitrogen atoms in BQCP. Variable temperature 1H NMR and PFG 1H, 15N HMBC runs show that in solution BQCP shows C2v-symmetry (both CH2-2-quinolyl fragments are equivalent) in NMR-time scale due to a fast exchange of the hydrogen bond from one nitrogen to the other even at 223 K.