Search results for "Proton NMR"

η⇌μ exchange bonding mode of bidentate tmeda ligand. Molecular structure of [Y(tmhd)3]2(μ-tmeda)

2003

Abstract The reaction between the yttrium β-diketonate complexes Y(tmhd)3(H2O)x (x=0 or 1) and 0.5 or 1 equivalent of N,N,N′,N′-tetramethylethylenediamine (tmeda=Me2NCH2CH2NMe2) in hexane at room temperature afforded [Y(tmhd)3]2(tmeda) (1) and Y(tmhd)3(tmeda) (2) derivatives, respectively. They have been characterized by FT-IR, 1H NMR spectroscopy and by single crystal X-ray diffraction for 1. Variable temperature 1H NMR experiments indicated an equilibrium between 1 and 2. Their thermal behaviors were characterized by TGA and sublimation experiments. 2 is converted into compound 1 by heating over 100 °C. These precursors were used for the growth of Y2O3 and YBa2Cu3O7 − x films by pulsed in…

Designing dicyanamide bridged 1D molecular architecture from a mononuclear copper(II) Schiff base precursor: Syntheses, structural variations and mag…

2009

International audience; A new tridentate N2O donor Schiff base ligand [(C6H5C(OH)CHC(CH3)NCH2C5H4N)LH] was obtained by 1:1 condensation of benzoylacetone with 2-picolylamine and has been used to synthesise a mononuclear [CuLCl] (1) and an end-to-end dicyanamide bridged polynuclear {[Cu2(μ-L)2(μ2-1,5-(CN)2N)]ClO4}n (2) copper(II) complexes. The ligand, 1 and 2 were clearly characterised by elemental analysis, FT-IR, 1H NMR, UV–Vis spectral studies, electrochemical studies and in addition single crystal X-ray diffraction studies were performed for 1 and 2. The Schiff base ligand [LH] shows a significant variation in its coordination behaviour with copper(II) ion in absence and in presence of …

A conjugated polymer with ethyl 2-(2-(pyridin-2-yl)-1H-benzo[d]imidazol-1-yl) acetate units as a novel fluorescent chemosensor for silver(I) detection

2013

Abstract A novel conjugated polymer ( P1 ) containing fluorene and ethyl 2-(2-(pyridin-2-yl)-1 H -benzo[ d ]imidazol-1-yl)acetate (PBMA) was designed and successfully synthesized through the Sonogashira coupling reaction. P1 shows high sensitivity and selectivity for Ag + detection in comparison to other metal cations. Upon addition of Ag + , the fluorescent emission of the polymer solution in THF was quenched dramatically, accompanying the color changed from blue to green. The detection limit for Ag + was 5 × 10 −8  mol L −1 . However, the similar copolymers P2 and P3 containing 2-(pyridin-2-yl)-1 H -benzo[ d ]imidazole and 2-(thiophen-2-yl)-1 H -benzo[ d ]imidazole, respectively, did not …

1H,13C and19F NMR spectroscopy of polyfluorinated ureas. Correlations involving NMR chemical shifts and electronic substituent effects

2005

Seventeen N-(mono-, di-, tri-, tetra- and penta-fluorophenyl)-N′-(3-nitrophenyl)ureas were prepared and characterized. Complete assignment of their 1H, 13C and 19F NMR data was undertaken and the correlation of the chemical shifts of the ureido protons with field-inductive and mesomeric electronic substituent parameters was studied using the Swain–Lupton model. The best correlations were obtained when the study was limited to certain substitution patterns, e.g. non-ortho, mono-ortho- and di-ortho-fluorinated ureas, which reveal probable changes in conformations caused by the degree of ortho fluorination at the phenyl ring. Additionally, there is an excellent linear cross-correlation between…

1H, 13C and 17O NMR spectral study of chlorinated 3,4-dihydroxybenzaldehydes (protocatechualdehydes)

1995

Abstract Chlorinated 3,4-dihydroxybenzaldehydes have been studied by means of 1 H, 13 C and 17 O NMR spectroscopy. The 1 H and 13 C NMR spectral assignments are based on 2-dimensional 13 C- 1 H chemical shift correlation spectroscopy (COSY). The 17 O NMR measurements at natural isotope content in organic solvents are problematic owing to the poor solubility of the compounds and/or broadness of the resonance lines. In aqueous alkaline solutions, however, all protocatechualdehydes exhibit “easy-to-detect” 17 O NMR spectral characteristics. The 17 O NMR chemical shifts in the range of 140–480 p.p.m. are interpreted as arising from the different canonical structures of formyl substituted phenol…

13C and15N NMR study of substituted 1,2,4-triazines

1995

13C and 15N NMR spectra of eight substituted 1,2,4-triazines were measured and assigned. The assignments of the 13C NMR spectra were based on the substituent chemical shifts and nJ(C,H) coupling constants. 15N NMR chemical shifts generally showing well separated ranges were assigned by the proton coupled 15N NMR spectra. 15N NMR chemical shifts of N-4 in 3- and 5-methoxy or -thiomethyl-substituted 1,2,4-triazines were found to be related significantly (confidence level >99%) with the π-charge at N-4 calculated by a semi-empirical molecular orbital (AM1) procedure. For the 15N NMR chemical shifts of N-1 and N-2, no reliable correlations with the molecular electronic properties such as AM1 π-…

?-Phenylsulfonyl-N-arylacetamides (?-phenylsulfonylacetanilides):1H,13C and15N NMR spectral characterization

2000

Combined proton NMR wideline and NMR relaxometry to study SOM-water interactions of cation-treated soils

2013

Abstract Focusing on the idea that multivalent cations affect SOM matrix and surface, we treated peat and soil samples by solutions of NaCl, CaCl2 or AlCl3. Water binding was characterized with low field 1H-NMR-relaxometry (20 MHz) and 1H wideline NMR spectroscopy (400 MHz) and compared to contact angles. From 1H wideline, we distinguished mobile water and water involved in water molecule bridges (WaMB). Large part of cation bridges (CaB) between SOM functional groups are associated with WaMB. Unexpectedly, 1H NMRrelaxometry relaxation rates suggest that cross-linking in the Al-containing peat is not stronger than that by Ca. The relation between percentage of mobile water and WaMB water in…

Crystal structure of 4,6-O-ethylidene-N-(2-hydroxybenzylidene)-β-D-glucopyranosylamine

2002

4,6-O-Ethylidene-N-(2-hydroxybenzylidene)-β-D-glucopyranosylamine was synthesized and characterized using analytical, spectral and single-crystal X-ray diffraction methods. The anomeric nature of the saccharide moiety was proposed based on 1H NMR studies and was confirmed by the crystal structure. The lattice structure of this compound was compared with that of its analogues.

Effect of Substituents on the Molecular Shapes of π-Basic Macrotricyclic Receptors

2010

Molecular recognition between receptor and substrate is optimized when these compounds show complementary shapes, sizes, and interacting moieties. A family of C3v-symmetric macrotricycles 1–4 is presented that incorporate resorcinol- and mesitylene-derived “walls” and “cap”, respectively. These compounds feature, in principle, a tetrahedral π-basic cavity. This paper reports the effect of substituents in the “walls” and the “cap” on the shapes of the macrotricycles in solution (1H NMR), the solid state (X-ray diffraction), and gas phase (calculations). Substitution of the lower position of the “walls” by Br (in 3) or MeS (in 4) has the same effect as ethyl substitution of the “cap” (in 2), …