Search results for "Proton NMR"

1H NMR, DSC, dielectric, and dilatometric studies of phase transitions and molecular dynamics in N (C2H5)4SbCl4

1994

The results of dielectric, dilatometric, 1H NMR, and DSC studies on N(C2H5)4SbCl4 crystals are presented. The title compound undergoes two phase transitions at Tc1 = 272 K reversible of first order and at Tc2 = 393 K irreversible. The values of transition entropies and enthalpies are compared with those of other tetraethylammonium halogenoantimonates and bismuthates (III). The spin-lattice relaxation times and the values of the second moments of the 1H NMR line for the N(C2H5)4SbCl4 crystal are measured in the temperature range of 70 to 400 K. Two minima of T1 are observed. They are attributed to CH3 group reorientations. The activation energies for the processes are determined.

Synthesis and Electrochemistry of Aluminum Porphycenes. Crystal and Molecular Structure of Methyl-σ-Bonded Aluminum Etioporphycene

1997

The synthesis and characterization of three monomeric aluminum porphycenes with anionic or σ-bonded axial ligands is reported. The investigated compounds are represented as ( EtioPc ) Al ( CH 3) and ( EtioPc ) AlX where EtioPc represents the dianion of etioporphycene and X = Cl − or OH −. Each synthesized complex was characterized by mass spectrometry. 1 H NMR, IR and UV-visible spectroscopies as well as by electrochemistry. Comparisons are made between the properties of complexes in the aluminum etioporphycene series and related chloro- or methyl σ-bonded Al ( III ) porphyrins containing octaethylporphyrin ( OEP ) or tetraphenylporphyrin ( TPP ) macrocycles. Comparisons are also made betw…

Complete assignments of1H and13C NMR spectra of four hispanane diterpenoids

2000

An NMR study of four hispanane diterpenoids is described. In addition to conventional 1D NMR methods, 2D shift-correlated experiments [1H,1H-COSY, 1H,1H-TOCSY, 1H,13C-HSQC-1J(C,H). 1H,13C-HMBC-nJ(C,H) (n = 2 and 3)] and 2D 1H,1H-NOESY were used for the complete and unambiguous 1H and 13C chemical shift assignments of these diterpenoids. Copyright © 2000 John Wiley & Sons, Ltd.

1H,13C and15N NMR chemical shifts of substituted pyrazolo[1,5-a]pyrimidines

2002

1H NMR study of dynamical inequivalence of cations in [C(NH2)3]3Sb2Cl9

2001

Abstract The proton NMR second moment and spin–lattice relaxation time have been studied for polycrystalline tris-guanidinium nonachlorodiantimonate(III) in a wide temperature range. The C 3 reorientation of two types of the cations, hindered by very different potential barriers (20.5 and 54.5 kJ/mol) has been revealed. An unusually large dynamical inequivalence of two cations evidently reflects their different crystalline environments.

ChemInform Abstract: Asymmetrically Substituted Calix(4)arenes. A Two-Dimensional 1H NMR Study of a Tetraester Derivative in the cone-Conformation.

2010

1977

Solutions of chain- (PS-d3) and phenyl ring (PS-d5) deuterated polystyrenes in perdeuterated PS-d8 have been investigated with 1H and 2D NMR relaxation and wide line methods. The intra- and intermolecular parts of the 1H second moments at −100°C are 3,7 G2 and 2,0 G2, respectively, for PS-d3, and 14,7 G2 and ca. 0 G2, respectively, for PS-d5. The intermolecular contribution to the 1H spin lattice relaxation rate, determined at 55 MHz between 150°C and 250°C, is about one third of the total rate in PS-d3, and negligible in PS-d5. We suggest that this contribution is caused by rotational fluctuations of the intermolecular H H vectors. The intramolecular 1H- and 2D-relaxation rates indicate th…

Synthesis, spectroscopic, cyclic voltammetry properties and molecular structure of the thiocyanato-N meso-tetratolylporphyrinato zinc(II) ion complex

2017

International audience; This paper describes the synthesis of the (thiocyanato-N)(meso-tetratolylporphyrinato)zinc(II) chlorobenzene monosolvate complex with the formula [K(2,2,2-crypt)][Zn(TTP)(NCS)]·C6H5Cl (I) using the cryptand-222 to solubilize potassium thiocyanate in chlorobenzene solvent. Complex (I) has been characterized by elementary analysis, IR, UV–vis, 1H NMR and MS, and the structure of this new zinc(II) metalloporphyrin been examined crystallographically. A cyclic voltammetry investigation was also carried out on this species. The title compound crystallizes in the triclinic, space group P-1, with a = 11.5151(7) Å, b = 15.212(10) Å, c = 20.1093(12) Å, α = 80.428(4)°, β = 74.9…

Self-assembled dendrimers with uniform structure

2008

Calix[4]arenes substituted at their wide rim by four aryl urea residues (1) form hydrogen-bonded dimers in apolar solvents. Replacement of one urea residue by an acetamido moiety leads to calix[4]arene derivatives (5) which form hydrogen-bonded tetramers under the same conditions. Both self-assembly processes occur independently. Therefore, molecules have been prepared in which a tetra-urea calix[4]arene and a tri-urea mono acetamide derivative are covalently connected between their narrow rims by a long, mainly aliphatic chain [-O-(CH(2))(n)-C(O)-NH-(CH(2))(m)-O-] (7). In the presence of an equimolar amount of tetra-tosyl urea calix[4]arene () they form dendritic assemblies since the well …

Synthesis and structural characterization of new transition metal complexes of a highly luminescent amino-terpyridine ligand

2020

Abstract The synthesis, NMR and UV–Vis spectroscopy measurements and X-ray diffraction analysis of four new metal complexes of the amino terpyridine ligand 4′-[4-(4-aminophenyl)phenyl]-2,2′:6′,2″-terpyridine L, namely [FeL2](ClO4)2 (1), [ZnL2](ClO4)2 (2), [CdL2](ClO4)2 (3) and [PtMe3IL] (4), are reported. The X-ray crystal structures of complexes 1–3 are 1:2 metal:ligand structures with tridentate ligands decorated around the octahedral metal centers. In complex 4, with L in a bidentate coordination mode, the Pt(IV) coordinated methyl and iodine groups form a fac-arrangement. The 1H NMR spectrum of 4 shows three 195Pt-1H resonances for the methyl groups incorporating the fac-arrangement, wh…