Das 7,8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ5-phosphaspiro[4.4]nonanyl-Kation: Röntgenstrukturanalyse und temperaturabhängige 1H-NMR-Spektren: The 7, 8-Benzo-5-chloro-1,4,4-trimethyl-1-aza-4-azonia-6,9-dioxa-5 λ).5-phosphaspiro[4.4]nonanyl Cation: X-Ray Crystal Structure Determination and Variable 1H NMR Spectra

1992 ◽  
Vol 47 (6) ◽  
pp. 755-759 ◽  
Author(s):  
Thomas Kaukorat ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crystal Structure ◽  
1H Nmr ◽  
Nmr Spectra ◽  
Crystal Structure Analysis ◽  
Acceptor Interaction ◽  
Nmr Spectrum ◽  
X Ray ◽  
H Nmr ◽  
Trigonal Bipyramidal ◽  
Donor Acceptor

The 1H NMR spectrum of the spirophosphorane 3 at room temperature indicates dynamic behaviour of the cation. The low-temperature 1H NMR spectra of 3 exhibit two sets of doublets for the protons of the diastereotopic N(CH3)2 groups. The free enthalpy of activation for the dynamic process was determined (58.6 KJ/mole). In the reaction of 3 with sodium tetraphenylborate the crystalline compound, 4, involving the non-coordinating anion, [B(C6H5)4]-, was obtained. The X-ray crystal structure analysis of 4 reveals the presence of a five-membered ring, formally as a result of intramolecular donor-acceptor interaction between the nitrogen atom of the N(CH3)2 group and phosphorus. The geometry at phosphorus deviates somewhat from ideal trigonal bipyramidal.

119Sn, 15N, 13C, and 1H NMR Study of the Intramolecular Sn-N Donor-Acceptor Interaction in [2-(Dimethylaminomethyl)phenyl]stannanes

1998 ◽  
Vol 63 (7) ◽  
pp. 977-989 ◽  
Author(s):  
Aleš Růžička ◽  
Vladimír Pejchal ◽  
Jaroslav Holeček ◽  
Antonín Lyčka ◽  
Klaus Jacob
Keyword(s):  
1H Nmr ◽  
Nmr Spectra ◽  
Intramolecular Interaction ◽  
Coupling Constants ◽  
Acceptor Interaction ◽  
H Nmr ◽  
Nmr Parameters ◽  
Nmr Study ◽  
Donor Acceptor ◽  
Characteristic Values

119Sn, 15N, 13C, and 1H NMR spectra were studied for [2-(dimethylaminomethyl)phenyl]stannanes, R1R2R3R4Sn or R1R2R24Sn, where R1, R2, and R3 are 1-butyl, Cl or Br, the same or different, and R4 is 2-(dimethylaminomethyl)phenyl. The occurrence of intramolecular interaction between the nitrogen and tin atoms was demonstrated based on changes in the characteristic values of the NMR parameters of these nuclides (δ(15N), δ(119Sn), J(119Sn,15N), and their interrelations, as well as on the relatively high values of the coupling constants 3J(119Sn,13C(CH2)).

scholarly journals Stereoregular Oligomers of Methyl Methacrylate: X-Ray Crystal Structure Analysis and 1H NMR Spectrum of the Trimer

1989 ◽  
Vol 21 (3) ◽  
pp. 231-240 ◽  
Author(s):  
Koichi Ute ◽  
Tohru Nishimura ◽  
Yoshiki Matsuura ◽  
Koichi Hatada
Keyword(s):  
Crystal Structure ◽  
Methyl Methacrylate ◽  
Structure Analysis ◽  
1H Nmr ◽  
Crystal Structure Analysis ◽  
Nmr Spectrum ◽  
X Ray

Organometallic oxides: preparation of the cluster [(η-C5Me5)Mo]4O7 by reduction of [(η-C5Me5)MoCl(O)]2(μ-O) or (η-C5Me5)MoCl2(O)

2000 ◽  
Vol 78 (3) ◽  
pp. 383-394
Author(s):  
Frank Bottomley ◽  
Victor Sanchez ◽  
Robert C Thompson ◽  
Olusola O Womiloju ◽  
Zhiqiang Xu
Keyword(s):  
Nmr Spectra ◽  
Chloroform Solution ◽  
X Ray Diffraction ◽  
Broad Resonance ◽  
Nmr Spectrum ◽  
X Ray ◽  
Temperature Range ◽  
H Nmr ◽  
Tributyltin Hydride ◽  
Effective Moment

Reduction of [(η-C5Me5)MoCl(O)]2(μ-O) or (η-C5Me5)MoCl2(O) with sodium or magnesium amalgam, magnesium turnings, or tributyltin hydride produced [(η-C5Me5)Mo]4O7, with [(η-C5Me5)Mo(O)(μ-O)]2 as a co-product. [(η-C5Me5)Mo]4O7 was characterized by X-ray diffraction, mass spectrometry, 1H NMR and IR spectroscopies, and magnetism. Crystals of [(η-C5Me5)Mo]4O7 contained a tetrahedral [(η-C5Me5)Mo]4 unit (Mo-Mo = 2.909 (3) Å) with the Mo4O7 core having the structure Mo4(μ2-O(b))3(µ2-O(c))3(µ3-O(a)) (3). Microcrystalline samples of [(η-C5Me5)Mo]4O7 were paramagnetic over the temperature range 2-300 K, with an effective moment of 1.26 μB at 300 K. [(η-C5Me5)Mo]4O7 was also paramagnetic in chloroform solution, over the temperature range 223-298 K, with an effective moment of 1.43 µB at 298 K. The 1H NMR spectrum showed a broad resonance at 16.3 ppm (Δν 1/2 = 113 Hz) and two narrow resonances at 1.89 ppm and 1.69 ppm (Δν 1/2 = 5 Hz). The magnetism and NMR spectra showed that [(η-C5Me5)Mo]4O7 existed in two forms which were in equilibrium in solution. One form was paramagnetic (S = 1), with the Mo4O7 core having the geometry 3, and the other was diamagnetic (S = 0), with the Mo4O7 core having the geometry 4.Key words: cluster, cyclopentadienyl, molybdenum, oxide, paramagnetism.

η3-Allylmeta]l-Schwefel-Komplexe, VI. Anionische η3-Allylnickel- und -palladium-Schwefel-Cluster/ η3-Allylmetal-Sulfur-Complexes, VI. Anionic η3-Allylnickel- and -palladium-Sulfur-Clusters

1983 ◽  
Vol 38 (5) ◽  
pp. 604-610 ◽  
Author(s):  
Reinhard Benn ◽  
Borislav Bogdanović ◽  
Peter Göttsch ◽  
Martin Rubach
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra ◽  
Ionic Structure ◽  
Butyl Lithium ◽  
Sulfur Cluster ◽  
Anionic Clusters ◽  
H Nmr ◽  
Trigonal Bipyramidal ◽  
Lithium Sulfide

Abstractη3-Allylhydrogensulfidonickel (2) reacts with n-butyllithium with elimination of lithium sulfide and formation of the ionic η3-allylnickel-sulfur-cluster [(η3-C3H5Ni)3S2]+[Li(THF)2]- (4). The crystal structure of the analogous THF-TMEDA-adduct (4′) indicates that the nickel and sulfur atoms of the anion adopt a trigonal bipyramidal arrangement, in which the sulfur atoms are at the apices of the bipyramid. The Li(THF)2+ cation in 4 can be replaced by the (n-C4H9)4N+ cation (5). The 1H NMR spectra suggest the presence of two stereoisomers of the anionic clusters in 4 and 5 having C3h and Cs symmetry. In the reaction of η3-allyl- or η3-methallylhydrogensulfidopalladium (6, 6 a) with n-butyl-lithium crystalline compounds having the composition RC3H4PdSLi(THF)≈4, R = H, CH3 (7, 7 a) are obtained; their 1H NMR spectra also reveal the existence of the two stereoisomers having C3h and Cs symmetry. The same type of stereoisomerism is observed with the crystalline [(n-C4H9)4N]+[(η3-C3H5Pd)3S2]- (8) obtained from 7 and (n-C4H9)4N+ClO4-. For 7 and 7 a an ionic structure consisting of trigonal bipyramidal (η3-RC3H4Pd)3S2- anions and Li3S(THF)4+ cations is proposed.

Electron Donor-Acceptor Compounds. Synthesis and Structure of 5-(1,4-Benzoquinone-2-yl)-10,15,20-trialkylporphyrins

1998 ◽  
Vol 53 (9) ◽  
pp. 1021-1030 ◽  
Author(s):  
Steffen Runge ◽  
Mathias O. Senge
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Supramolecular Structure ◽  
Crystal Structure Analysis ◽  
Free Base ◽  
X Ray ◽  
X Ray Crystallography ◽  
New Methods ◽  
Polymeric Chains ◽  
Donor Acceptor

Abstract A series of 5-(benzoquinone)-10,15,20-trialkylporphyrins was synthesized via cross condensation of the respective aldehydes, 2,5-dimethoxybenzaldehyde and pyrrole followed by demethylation with BBr3 and oxidation with PbO2. This method worked reasonably well for compounds bearing the benzoquinone substituent and butyl, isopropyl, 1 -methylpropyl and 2-ethylpropyl residues (2a-d). The free base porphyrin quinones were converted into the zinc(II) complexes (3a-d) all of which showed remarkable stability for porphyrin quinones. The zinc(II) complex 3c bearing isopropyl residues was investigated by X-ray crystallography and showed a supramolecular structure consisting of polymeric chains facilitated by coordina­tion of a benzoquinone oxygen to a neighboring zinc(II) center. Attempts to synthesize a 5-(benzoquinone)-10,15,20-tris(terr-butylporphyrin) resulted in the formation of a yellow porphomethene (4), which could not be oxidized further. A crystal structure analysis of 4, the first for a free base porphomethene, shows an extremely twisted conformation with syn-orientation of the three tert-butyl groups. The results indicate that new methods will have to be developed for the synthesis of nonplanar porphyrin quinones.

Complexes of N-Aryltriphenylphosphinimines with Mercury(II) Halides

1999 ◽  
Vol 54 (7) ◽  
pp. 858-862 ◽  
Author(s):  
Thomas P. Braun ◽  
Paul A. Gutsch ◽  
Hans Zimmer
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Structure Analysis ◽  
Nmr Spectra ◽  
Crystal Structure Analysis ◽  
Phosphonium Salts ◽  
X Ray

The synthesis, IR and 31P NMR spectra of the complexes of various N-aryltriphenylphosphinimines with some mercury dihalides as well as the corresponding phosphonium salts are reported. It is shown by an X-ray crystal structure analysis of the complex of the unsubstituted phosphinimine with HgCl2 that in the solid state these complexes form dimers via two Hg ∙∙∙ μ2- Cl ∙∙∙ Hg bridges.

Darstellung, 11B-und 19F-NMR-Spektren des Monofluoropentaiodo- closo-hexaboratanions sowie Kristallstruktur von (CH2Py2)[B6FI5]/ Synthesis, 11B and 19F NMR Spectra of the Monofluoropentaiodo-closo-hexaborate Anion and the Crystal Structure of (CH2Py2)[B6FI5]

1998 ◽  
Vol 53 (8) ◽  
pp. 829-832 ◽  
Author(s):  
H. Thomsen ◽  
W. Preetz
Keyword(s):  
Crystal Structure ◽  
Nmr Spectra ◽  
19F Nmr ◽  
Coupling Constant ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
19F Nmr Spectra ◽  
Nmr Spectrum ◽  
X Ray ◽  
Excess Iodine

Abstract By reaction of closo-[B6H5F]2- in alkaline solution with excess iodine the monofluoropentaiodo- closo-hexaborate anion [B6FI5]2- is formed in good yield. The crystal structure of (CH2Py2)[B6FI5] has been determined by single crystal X-ray diffraction analysis (orthorhombic, space group Pnma, a = 13.803(2), b = 11.759(2), c = 13.936(2) Å, Z = 4). The B-F-bond length is 1.41 Å, the B-I distances range from 2.13 to 2.17 Å, the B-B distances from 1.69 to 1.76 A. According to the C4v point symmetry the 11B NMR spectrum of the anion exhibits three singlets at +3.8,-30.1 and-33.3 ppm with the intensity ratio 1:4:1, the 19F NMR spectrum one quartet at -247.6 ppm with the coupling constant 1J (19F, 11B) = 54 Hz.

Preparation and Crystal Structure of Genistein Benzenesulfonate Prodrugs

2008 ◽  
Vol 2008 (10) ◽  
pp. 555-558 ◽  
Author(s):  
You Peng ◽  
Zeyuan Deng ◽  
Shaojie Lang ◽  
Yawei Fan
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Sulfonic Acid ◽  
Nmr Spectra ◽  
High Yield ◽  
X Ray Diffraction ◽  
Aromatic Rings ◽  
X Ray ◽  
H Nmr ◽  
Ester Prodrugs

In order to improve bioavailability and anticancer activity of genistein, a series of novel sulfonic acid ester prodrugs of the isoflavone genistein were synthesised in high yield with excellent regioselectivity. Their structures were characterised by IR, MS, elemental analysis and 1H NMR spectra. The crystal structure was examined by X-ray diffraction. X-ray structure determination revealed that all the aromatic rings in the compound are not coplanar. In the crystal structure, molecules are linked through intermolecular C-H···O hydrogen bonds, forming layers parallel to the ab plane.

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