Synthesis of chloro(2-methylimidazole) ruthenium(III) complexes and their aqueous solution chemistry, and the crystal structure of [2-MeImH]2[RuCl52-MeIm]

2001 ◽  
Vol 79 (10) ◽  
pp. 1477-1482 ◽  
Author(s):  
Craig Anderson
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Solution Chemistry ◽  
Proton Nmr Spectroscopy ◽  
Line Broadening ◽  
Reaction Conditions ◽  
H Nmr ◽  
Paramagnetic Complexes

2-Methylimidazole (2-MeIm) reacts with RuCl3 in aqueous acidic ethanolic medium to give (2-MeImH)2[RuCl5(2-MeIm)] (1) and (2-MeImH)[RuCl4(2-MeIm)2] (2) (2-MeImH = protonated 2-methylimidazole), the ratio depending on reaction conditions used. Molecule 1 crystallizes in the space group Pnma: a = 14.046(2), b = 17.294(2), and c = 8.2778(12) Å. The 1H NMR spectra of these ruthenium(III) complexes have been measured and show peaks with large isotropic shifts and large line broadening characteristic of such paramagnetic complexes. The aquation of complexes 1 and 2 were followed by proton NMR spectroscopy. 1,2-Dimethyl imidazole (1,2-diMeIm) reacts with RuCl3 in methanolic solution to give [RuCl3(1,2-diMeIm)(H2O)S] (S=H2O (3a) or CH3OH (3b)). The aquation reactions of complexes 3a and 3b were followed by 1H NMR.Key words: ruthenium, paramagnetic, antitumour, NMR.

Crystal structure of methyl,2-mercaptopyrimidinatomercury(II)

1978 ◽  
Vol 56 (4) ◽  
pp. 560-563 ◽  
Author(s):  
Chung Chieh
Keyword(s):  
Crystal Structure ◽  
Aqueous Solution ◽  
Nmr Spectra ◽  
Heavy Atom ◽  
Pyrimidine Ring ◽  
Optically Active ◽  
Hydrogen Atoms ◽  
H Nmr ◽  
R Factor ◽  
Heavy Atom Method

Methyl,2-mercaptopyrimidinatomercury(II) was synthesized from methylmercuric hydroxide and 2-mercaptopyrimidine in aqueous solution. The crystal is orthorhombic with a = 4.063(2), b = 9.901(4), c = 18.808(15) Å, Dm = 2.88(1), Z = 4, Dc = 2.867 g cm−3, space group P212121. The structure was solved by the heavy atom method using 605 diffractometer measured reflections. The final R factor was 0.069. The key bond lengths and angles are: Hg—S, 2.39(2) Å, Hg—CH3, 2.13(6) Å, [Formula: see text] 174°. The CH3HgS— group bends out of the plane of the pyrimidine ring and the Hg atom interacts rather strongly with one of the ring nitrogens with an Hg—N distance of 2.83 Å. However, the Hg … N interaction is very labile in solution, since the two hydrogen atoms in the meta positions are equivalent from the 1H nmr spectra in both CDCl3 and DMSO solutions. The solution of the compound is not optically active.

Magnetic resonance imaging (1H) and spectroscopy (1H, 31P) of growing chicken embryos

1993 ◽  
Vol 73 (4) ◽  
pp. 953-965 ◽  
Author(s):  
A. Lirette ◽  
Z. Liu ◽  
D. C. Crober ◽  
R. A. Towner ◽  
U. M. Oehler ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Magnetic Resonance ◽  
Nmr Spectra ◽  
Surface Coil ◽  
Nmr Imaging ◽  
Chicken Embryos ◽  
H Nmr ◽  
Imaging And Spectroscopy ◽  
Two Peaks

Nuclear magnetic resonance (NMR) imaging and spectroscopy techniques were used to observe in vivo anatomical and metabolite changes, respectively, in developing chicken embryos. Proton (1H) NMR images of the eggs revealed major changes in yolk shape from day 2 to day 6. Embryos were visible from day 6 to hatching, and good embryonic anatomical images were obtained. Two peaks were observed from 1H-NMR spectroscopy of fertilized eggs: one for lipid methylene protons, and one for water protons. Water peak to lipid peak ratios did not vary significantly (P > 0.05) from day 2 to day 21 of incubation. Localized 31P-NMR spectra of developing embryos were obtained with either a 31P surface coil or a double-tuned 31P/1H volume coil. The surface-coil method gave a greater signal to noise ratio by a factor of four. The 31P-NMR spectra indicated two peaks at day 2; these were attributed to phosphomonoesters and phosphodiesters. The three peaks characteristic of ATP appeared on day 11 and increased in size until hatching. From day 19, phosphocreatine was detectable. There appeared to be a good correlation between 31P-metabolite changes detected by in vivo 31P-NMR spectroscopy and literature values for biochemical analyses of developing chicken embryos. The advantage in using NMR imaging and spectroscopy techniques is that anatomical and metabolic changes can be obtained in vivo, non-invasively and repeatedly as an embryo develops. Key words: NMR, MRI, embryo, poultry

scholarly journals Metallkomplexe mit Tetrapyrrol-Liganden, XXXVIII [1]. Zur Kenntnis der Alkyl- und Arylimidovanadium(IV)-Porphyrine / Metal Complexes with Tetrapyrrole Ligands, XXXVIII [1]. On the Knowledge of Alkyl- and Arylimidovanadium(IV) Porphyrins

1985 ◽  
Vol 40 (10) ◽  
pp. 1362-1370 ◽  
Author(s):  
Johann W. Buchler ◽  
Stefan Pfeifer
Keyword(s):  
Mass Spectra ◽  
Nmr Spectra ◽  
Primary Amines ◽  
Reactive Intermediate ◽  
H Nmr ◽  
Vanadyl Complex ◽  
Elemental Analyses ◽  
Paramagnetic Metal ◽  
Paramagnetic Complexes ◽  
Proton Resonances

A series of novel alkyl or aryiimidovanadium(IV) 5,10,15,20-tetra(p-tolyl)porphyrinates, VNR(TTP) (4a-4g), is described. They are obtained from the vanadyl complex, VO(TTP) (2a) via the reactive intermediate VCl2(TTP) (3b) which undergoes aminolysis with the respective primary amines RNH2 (R = tBu, Ph, pTol, pClPh, pAnis, pBiph, ptBuPh)**. The formulae are proved by elemental analyses and mass spectra. The paramagnetic complexes are stable to water and may thus be purified by chromatography but are hydrolyzed to give 2 a on treatment with acetic acid. The UV/VIS and 1H NMR spectra of 4a-4g are of the same type as 2a, but the former are slightly hypsochromically shifted, and the latter do not show the proton resonances of the organylimide ligands due to the proximity of the paramagnetic metal center.

Nuclear magnetic resonance studies on the anions [M(SnCl3)5Cl]4− (M = Ru, Os) and [Ru(SnCl3)5(MeCN)]3−: the X-ray crystal structure of [N(C2H5)4]4[Ru(SnCl3)5Cl]

1982 ◽  
Vol 60 (11) ◽  
pp. 1304-1316 ◽  
Author(s):  
Louis J. Farrugia ◽  
Brian R. James ◽  
Claude R. Lassigne ◽  
Edward J. Wells
Keyword(s):  
Crystal Structure ◽  
Nuclear Magnetic Resonance ◽  
Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Octahedral Geometry ◽  
Coupling Constants ◽  
Order Effects ◽  
Magnetic Resonance Studies ◽  
X Ray ◽  
Crystallographic Study

The octahedral anions [M(SnCl3)5Cl]4− (M = Ru, Os) have been fully characterized by 119Sn FT nmr spectroscopy. For M = Ru, 117Sn and 115Sn nmr spectra were also recorded, and an X-ray crystallographic study was carried out on the tetraethylammonium salt, isolated as a disolvate from acetonitrile. The Ru—Sn bond lengths indicate some degree of dπ–dπ interactions. The slight distortions from octahedral geometry are discussed in connection with the packing of the chlorine atoms. The Sn nmr spectra reveal the first observed coupling to a 99Ru nucleus (I = 5/2, 12.7% natural abundance), very large 2J(119Sn—117Sn) coupling constants, and the first observed second-order effects on a heteronuclear system. The octahedral anion [Ru(SnCl3)5(MeCN)]3− was also synthesized as the tetraethylammonium salt and characterized spectroscopically.

Crystal-Structure Determination of Powdered Paramagnetic Lanthanide Complexes by Proton NMR Spectroscopy

2009 ◽  
Vol 121 (17) ◽  
pp. 3128-3132 ◽  
Author(s):  
Gwendal Kervern ◽  
Anthony D'Aléo ◽  
Loïc Toupet ◽  
Olivier Maury ◽  
Lyndon Emsley ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Structure Determination ◽  
Lanthanide Complexes ◽  
Proton Nmr ◽  
Crystal Structure Determination ◽  
Proton Nmr Spectroscopy

scholarly journals Three-Dimensional Supramolecular Network Directed by Intermolecular Interactions in [Pb2(dmp)2(hfacac)4]

2009 ◽  
Vol 6 (4) ◽  
pp. 1085-1090
Author(s):  
Farzin Marandi ◽  
Lotfali Saghatforoush ◽  
Hossein Farzaneh
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Three Dimensional ◽  
Supramolecular Network ◽  
Stacking Interactions ◽  
H Nmr ◽  
Noncovalent Bond ◽  
Donor And Acceptor ◽  
Anionic Ligands ◽  
C Nmr

To investigate the interactions between noncovalent bond donor and acceptor giving rise to three dimensional networks, compound [Pb2(dmp)2(hfacac)2] (1) (dmp = 2,9-dimethyl-1,10-henanthroline and Hhfacac = hexafluoroacetylacetonate) has been prepared and characterized by elemental analysis, IR,1H NMR, and13C NMR spectroscopy and its crystal structures was investigated. The single crystal structure show the coordination number of Pb(II) to be eight with twoN-donor atoms from a “dmp” ligand and sixO-donors from the anionic ligands. The supramolecular structure of 1 is realized by weak directional C–H∙∙∙O–C, C–F∙∙∙F–C andπ–πstacking interactions.

scholarly journals Assessment of 1H NMR Spectroscopy for Specific Metabolite Fingerprinting of Angelica sinensis

2008 ◽  
Vol 3 (5) ◽  
pp. 1934578X0800300
Author(s):  
Dongmin Su ◽  
Jinglan Han ◽  
Shishan Yu ◽  
Hailin Qin
Keyword(s):  
Nmr Spectroscopy ◽  
1H Nmr ◽  
1H Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Authentic Sample ◽  
Angelica Sinensis ◽  
Metabolite Fingerprinting ◽  
H Nmr ◽  
Pure Compounds ◽  
Polar Extracts

The 1H NMR fingerprints of fractionated non-polar extracts (CSPD A) from the roots of Angelica sinensis of six different specimens were assigned by comparison with the 1H NMR spectra of the isolated pure compounds. The 1H NMR fingerprints showed exclusively characteristic resonance signals of the major constituents of the plant. The 1H NMR fingerprint established for an authentic sample of A. sinensis can be used for authenticating A. sinensis species.

Morpholines-(IV)

1971 ◽  
Vol 26 (11) ◽  
pp. 1140-1143 ◽  
Author(s):  
Riaz F. Abdulla ◽  
Alok N. Bannerji
Keyword(s):  
Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Beta Lactams ◽  
Aryl Substituent ◽  
Open Chain ◽  
H Nmr

Cyclodehydrohalogenation-beta-Lactams-Morpholin-3-ones-H'-NMR SpectroscopyN-Aryl-N-chloroacetyl-2-chlorophenacylamines (2) give morpholinones 3, or beta-lactams 4, depending upon the N-aryl-substituent. N-Phenyl-N- (2,3-dibromo-3-phenylpropionyl) -4-nitrophenacylamine did not undergo base-catalysed cyclization but gave, instead, the α,β-unsaturated, open-chain amide 5. N-Aryl-N-chloroacetyl-aminomethyl-2-naphthylketones afford only beta-lactams. The first attempt at the synthesis of a 2-chloro-3-oxo-morpholine resulted in the isolation of the 2-hydroxyderivative. The H1-NMR spectra of some more 3-oxo-morpholines have been recorded.

Multiaxial Reorientationsof ND+4 Ions Studied by 2H-NMR Spectroscopy

1991 ◽  
Vol 46 (10) ◽  
pp. 829-840 ◽  
Author(s):  
Z. T. Lalowicz ◽  
S. F. Sagnowski
Keyword(s):  
Nmr Spectroscopy ◽  
Density Matrix ◽  
Nmr Spectra ◽  
Activation Energies ◽  
Matrix Formalism ◽  
2H Nmr ◽  
Jump Frequency ◽  
H Nmr ◽  
2H Nmr Spectroscopy ◽  
Density Matrix Formalism

AbstractThe density matrix formalism is used to simulate motional averaging in the 2H-NMR spectra of reorienting ND+4 ions. The development of the spectra under increasing jump frequency about a single C3 or C2 axis is followed. Next we assume a hierarchy of axes in terms of activation energies sufficient to reach extreme narrowing conditions for some axes before activating jumps about a next one. Primary reorientations about the fastest C3 or C2 symmetry axes define the shape of spectra, the width of which is then stepwise reduced by fast reorientations about the subsequent axes in a postulated sequence of statistically uncorrelated jumps.

Synthesis, Spectroscopic Properties, and Crystal Structure of the Oxonium Acid [H(OEt2)2]+[Ti2Cl9]–

2003 ◽  
Vol 58 (8) ◽  
pp. 745-750 ◽  
Author(s):  
Stefan Rannabauer ◽  
Tassilo Habereder ◽  
Heinrich Nöth ◽  
Wolfgang Schnick
Keyword(s):  
Crystal Structure ◽  
Ir Spectroscopy ◽  
Single Crystals ◽  
Nmr Spectra ◽  
Spectroscopic Properties ◽  
Partial Hydrolysis ◽  
Distorted Tetrahedron ◽  
Methyl Carbon ◽  
H Nmr ◽  
The Stability

The oxonium acid [H(OEt2)2]+[Ti2Cl9]− (1) was obtained by the reaction of TiCl4 with Et2O in n-pentane and subsequent partial hydrolysis. Suitable single crystals of 1 were obtained by sublimation at 5° C ([H(OEt2)2]+[Ti2Cl9]−, P212121 (no. 19), Z = 4, a = 1101.08(8), b = 1328.4(2), c = 1525.0(2) pm, T = 193(2) K, 4489 independent reflections, 197 parameters, R1 = 0.049). The cation is made up from two independent Et2O molecules and one disordered proton on two split positions. Both ether molecules exhibit a W form, and their molecular planes include an angle of 74.1(7)°. Thus a distorted tetrahedron is formed by the four methyl carbon atoms of the two ether molecules. The distance O···O amounts to 237.7(1) pm. The proton of the cation was characterized both by 1H NMR (CDCl3, T = 23 °C: δ = 11.7 ppm, w1/2 = 100 Hz) and IR spectroscopy (3120 cm−1, ν vbr). The [Ti2Cl9]− ion consists of two face sharing octahedra. 47Ti and 49Ti NMR spectra were recorded in solution (CH2Cl2, T = 23 °C: δ 49Ti = 137 ppm, w1/2 = 175 Hz; δ 47Ti = −124 ppm, w1/2 = 250 Hz). The absence of a signal for TiCl4 at δ 49Ti = 0 ppm indicates the stability of the dinuclear anion in solution.

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