X-Ray Structure Analysis and Spectroscopic Data of the Antibiotic 8-(Dichloroacetyl)-5-hydroxy-2,7-dimethyl-1,4-naphthoquinone from the Fungus Mollisia sp.*

1987 ◽  
Vol 42 (1-2) ◽  
pp. 1-3 ◽  
Author(s):  
Gabriela Weber ◽  
Thomas Hübner ◽  
Alfred Gieren ◽  
Johann Sonnenbichler ◽  
Tadeusz Kowalski ◽  
...  
Keyword(s):  
High Resolution ◽  
Structure Analysis ◽  
Spectroscopic Data ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
X Ray ◽  
H Nmr

Abstract Mass spectra, X-ray data and high resolution 13C and 1H NMR spectra of 8-(dichloroacetyl)-5-hydroxy-2,7-dim ethyl-1,4-naphthoquinone are reported. The antibiotic active com pound was isolated from the fungus Mollisia sp.

scholarly journals Atran-analoge Verbindungen des Typs / Atrane Analogous Compounds of the Type

1984 ◽  
Vol 39 (3) ◽  
pp. 341-351 ◽  
Author(s):  
Joseph Grobe ◽  
Gerald Henkel ◽  
Bernt Krebs ◽  
Nikolaos Voulgarakis
Keyword(s):  
Structure Analysis ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Trigonal Bipyramid ◽  
Angular Distortion ◽  
Type I ◽  
Tetrahedral Coordination ◽  
Cage Compounds ◽  
X Ray ◽  
H Nmr

Heterocyclic cage compounds of type I (compounds 8-10) have been prepared by condensation reactions of 1,2,2-trifunctional disilanes Me(R)XSiSiMeX2 (R = Me, Ph, OEt; X = NMe2, OEt) with triethanolamine using the “Dilution Principle”. The starting compounds are obtained by Si-Me cleavage of Si2Me6 with acetylchloride/AlCl3 followed by either aminolysis with HNMe2 or alcoholysis with EtOH. 1H NMR spectra indicate N→Si(1) intraction with the more acidic Si atom in 8 and 9. This result is proved by the X-ray structure analysis of 8 (monoclinic, P21/c; a = 7,088(2), b = 15,070(4), c = 12,701(4) Å, β = 104,96(2) at -130 °C, Z = 4); the Si(1)···N distance is found to be 2,768 Å , connected with a significant angular distortion of the tetrahedral coordination around Si(1) towards a trigonal bipyramid. In compound 10, too, N→Si(1) coordination is observed at room temperature in spite of almost equal acidity for both Si atoms. This can be explained by the preference of 5- over 6-membered chelating ring systems. At higher temperatures the 1H NMR spectra show a fluctuation of the N-donor between the two Si centres.

Pentamethylcyclopentadienyl Halfsandwich Complexes of Rhodium and Iridium Containing 1,1′-Ferrocene Dichalcogenido Ligands

1992 ◽  
Vol 47 (8) ◽  
pp. 1091-1098 ◽  
Author(s):  
Max Herberhold ◽  
Guo-Xin Jin ◽  
Arnold L. Rheingold ◽  
George F. Sheats
Keyword(s):  
Electron Impact ◽  
Structure Analysis ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
Direct Interaction ◽  
Bimetallic Complexes ◽  
X Ray ◽  
New Compounds

A series of 12 bimetallic complexes Cp M(L)[(EC5H4)2Fe] (M(L) = Rh(PMe3), Ir(PMe3), Ir(PPh3) and Ir(CNtBu); E = S, Se, Te) has been synthesized from the dichlorides Cp M(L)Cl2. The new compounds have been characterized by their 1H, 13C and 31P NMR spectra in solution. The mass spectra indicate that the two-electron ligand L is preferentially eliminated upon electron-impact. Oxidation by AgBF4 to give ferrocenium-type cations also occurs readily. An X-ray structure analysis of CpRh(PMe3)[(SC5H4)2Fe] (la) confirms the presence of a 1,1′-ferrocene dithiolate ligand with parallel and ecliptic cyclopentadienyl rings. The long Rh ... Fe (430.4(1) pm) distance rules out any direct interaction between the rhodium center and the iron in the cavity of the ferrocene sandwich.

Zur Chemie der 1,3,5-Triaza-2-phosphorinan-4,6-dione. Teil X. Umsetzungen von 2-Hydro-1,3,5-trimethyl-1,3,5-triaza-2-oxo-2λ4- phosphorinan-4,6-dion mit Triazin-Derivaten sowie mit einigen Aldehyden / Chemistry of the 1,3,5-Triaza-2-phosphorinan-4,6-diones. Part X. Reactions of 2-Hydro-1,3,5-trimethyl-1,3,5-triaza-2-oxo-2λ4 -phosphorinan-4,6-dione with Triazine Derivatives and with Some Aldehydes

1995 ◽  
Vol 50 (12) ◽  
pp. 1833-1838 ◽  
Author(s):  
Ion Neda ◽  
Michael Farkens ◽  
Holger Thönnessen ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Structure Analysis ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
Glyoxylic Acid ◽  
Crystal Structure Analysis ◽  
Membered Ring ◽  
X Ray ◽  
Triazine Derivatives

The reactions o f 2-hydro-1,3,5-trim ethyl-1,3,5-triaza-2-oxo-2λ4 -phosphorinan-4,6-dione 1 with the triazine derivatives, 1,3,5-trimethyl- and 1,3,5-tribenzyl-hexahydro-1,3,5-triazine, are described. The reaction of three equivalents of 1 with one equivalent of the triazine derivative gave 2 and 3. Both compounds were characterized via their 1H, 13C, and 31P NMR spectra, mass spectra and, in the case of 2, by an X-ray crystal structure analysis, which showed an almost planar six-membered ring; hydrogen bonds of the form N-H···O link the molecules in centrosymmetric pairs. The reactions of 1 with the aldehydes glyoxylic acid, 2-hydroxybenzaldehyde and 3,4,5-trimethoxybenzaldehyde gave addition products. The C (:O) group o f the aldehyde is inserted into the P -H bond o f 1. The resulting compounds 4 ,5 and 6 were characterized through their 1H, 13C, and 31P NMR spectra, and mass spectra.

scholarly journals Chemie polyfunktioneller Moleküle, 106. Kupfer(I)halogenid — Komplexe des Bis(diphenylphosphino)amins / Chemistry of Polyfunctional Molecules, 106. Copper(I) Halide Complexes of Bis(diphenylphosphino)amine

1990 ◽  
Vol 45 (12) ◽  
pp. 1657-1668 ◽  
Author(s):  
Jochen Ellermann ◽  
Falk A. Knoch ◽  
Klaus J. Meier
Keyword(s):  
Crystal Structure ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
Conductivity Data ◽  
Triclinic Space Group ◽  
X Ray ◽  
Lattice Constants ◽  
H Nmr ◽  
Nmr Data ◽  
Halide Complexes

Reaction of Copper(I) halides CuX (X = Cl, Br, I) in methanol with bis(diphenylphosphino)amine (dppa, 1) yields complexes [Cu3X2(dppa)3]X (X = Cl, Br, I: 2a–c). The derivates [Cu3X2(dppa)3]PF6 (2a′–c′) have been synthesized by metatheses of 2a–c with NH4PF6. The IR, Raman, 31P{1H} NMR, 1H{31Ρ} NMR, 13C{1H} NMR spectra, and FD mass spectra as well as the conductivity data are reported and discussed together with the X-ray crystal structure of 2a · 5 CH3OH. The structure consists of the trinuclear cations [Cu3Cl2(dppa)3]+, distorted tetrahedral anions [Cl( · · · HOCH3)4]- and molecules of methanol of crystallization, hydrogen bridged to the solvated anions. The Cu3Cl2 core of the cations corresponds closely to a trigonal bipyramid with the copper atoms in the equatorial and the chlorine atoms in the axial positions. The colourless prisms of 2a · 5 CH3OH crystallize in the triclinic space group P1̅, with the lattice constants a = 1368.0(4); b = 1486.7(4); c = 2036.8(10) pm; α = 74.52(3); β = 74.73(3); γ = 82.26(2)°. Raman and 31P{1H} NMR data of the complexes [Cu(X)dppm]4 (dppm = (C6H5)2PCH2P(C6H5)2; X = Br, I) described earlier suggest that these compounds should also be formulated as [Cu3X2(dppm)3]X (4b, c).The Raman spectra of the cations of 2a–c, 2a′–c′ and 4a–c show bands at 165 (X = Cl), 145 (X = Br) and 125 (X = I) cm-1, which can be assigned to the symmetric (XCu3X) stretching mode of the XCu3X unit.

N,N,N′,N′,N′,N″,N‴,N‴-Octamethyl-[bi-2,4,6-cycloheptatrien-1-yl]- 3,3′-dicarboxamidinium-Salze: Struktur der meso-Verbindung in Lösung und im Kristall [1] / N,N,N′,N′,N′,N″,N‴,N‴-Octamethyl-[bi-2,4,6-cycloheptatriene-1-yl]- 3,3′-dicarboxamidinium Salts: Structure of the meso-Compound in Solution and in Solid State [1]

1985 ◽  
Vol 40 (10) ◽  
pp. 1390-1397 ◽  
Author(s):  
Jörg Daub ◽  
Adelheid Hasenhündl ◽  
Erika Salbeck ◽  
Alfred Gieren ◽  
Thomas Hübner
Keyword(s):  
Solid State ◽  
Structure Analysis ◽  
Nmr Spectra ◽  
Oxidative Dimerization ◽  
Temperature Dependent ◽  
X Ray ◽  
H Nmr ◽  
Nmr Techniques ◽  
State 1 ◽  
Structure In Solution

3,3′-Bicycloheptatrienylamidinium salts 3 have been prepared by oxidative dimerization of 8 ,8 -bis(dimethylamino)heptafulvene (1). An X-ray structure analysis of the meso-octamethyl[bi-2,4,6-cycloheptatrienyl]3,3'-dicarboxamidinium-bis(triiodide) (3b) has been carried out. The dication 3 is centrosymmetric (Ci-symmetry) with boat shaped cycloheptatriene rings. The amidinium groups are twisted out of the plane of the C3(C3′)-C2(C2′) double bonds. The structure of the dication in the solid state is discussed in comparison with the structure in solution by aid of 1H NMR techniques. The N-methyls within one amidinium group show temperature dependent 1H NMR spectra and are chemically nonequivalent (anisochronous).

Synthese und Kristallstruktur von W2[OC(CF3)2NMe2]2(NMe2)4 / Synthesis and Crystal Structure of W2[OC(CF3)2NMe2]2(NMe2)4

1986 ◽  
Vol 41 (12) ◽  
pp. 1506-1508 ◽  
Author(s):  
Herbert W. Roesky ◽  
Norbert Bertel ◽  
Frank Edelmann ◽  
Regine Herbst ◽  
Ernst Egert ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Triple Bond ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
Synthesis And Crystal Structure ◽  
X Ray

AbstractThe reaction of W2(NMe2)6 with hexafluoroacetone (HFA) yields W2[OC(CF3)2NMe2]2(NMe2)4, an orange solid, which was characterized by mass spectra, 1H, 13C, 19F NMR spectra and an X-ray structure analysis. The compound contains a W=W triple bond of 230.1(1) pm.

Verbindungen mit dem 5,6-Benzo-l,3,2-diazaphosphorinan-4-on-Ringsystem: Synthese von 2-Chlor-, 2-N,N-dimethylamino-und 2-Bis-(2-chlorethyl)amino- substituierten Derivaten mit drei-und vierfach koordiniertem Phosphor / Compounds Involving the 5,6-Benzo-l,3,2-diazaphosphorinane-4-one Ring System: Synthesis of 2-Chloro-, 2-N,N-dimethylamino-and 2-Bis-(2-chloroethyl)amino- Substituted Derivatives with Three-and Four-Coordinated Phosphorus

1994 ◽  
Vol 49 (6) ◽  
pp. 788-800 ◽  
Author(s):  
Ralf Sonnenburg ◽  
Ion Neda ◽  
Axel Fischer ◽  
Peter G. Jones ◽  
Reinhard Schmutzler
Keyword(s):  
Nitrogen Atom ◽  
Mass Spectra ◽  
Nmr Spectra ◽  
Ring System ◽  
Phosphorus Trichloride ◽  
Amine Hydrochloride ◽  
Nmr Studies ◽  
X Ray ◽  
H Nmr ◽  
Structure Determinations

The reaction of methylisatoic anhydride with 2-(aminomethyl)pyridine, 3-(aminomethyl)- pyridine, 3-dimethylamino-1-propylamine, 3-diethylamino-1-propylamine and 3-dibutylamino- 1-propylamine furnished the N-substituted N'-methylanthranilic amides 1-5. In the reaction of 1-5 with phosphorus trichloride the 3-substituted 5,6-benzo-1-m ethyl-1,3,2-diazaphosphorinane- 4-one derivatives 6 to 10 were obtained. The possibility of intramolecular donoracceptor interaction between the nitrogen atom of the R2N group and the λ3P atom is suggested on the basis of 1H NMR studies. The reaction of 9 with dimethylamino-trimethylsilane furnished the 2-dimethylamino-substituted product 11. In the reaction of 6, 7 and 10 with bis-(2-chloroethyl)amine hydrochloride/triethylamine the expected substitution products 12 to 14 were obtained. 5,6-Benzo-2-[bis-(2-chloroethyl)amino]-1-methyl-3-(3-picolyl)-1,3,2-diazaphosphorinan- 4-one 13 reacted with (COD)PtCl2 to give the czs-dichloro-platinum(II) complex 15. The characterisation of 1-15 is based on the 1H-, 13C-, and 31P-NMR spectra, mass spectra and X-ray structure determinations of the precursor compounds 1 and 3

Preparation, properties and structure of some intermediate nido- and arachno-monocarbaboranes

1981 ◽  
Vol 46 (10) ◽  
pp. 2345-2353 ◽  
Author(s):  
Karel Baše ◽  
Bohumil Štíbr ◽  
Jiří Dolanský ◽  
Josef Duben
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Nmr Spectra ◽  
Liquid Ammonia ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Starting Compound

The 6-N(CH3)3-6-CB9H11 carbaborane reacts with sodium in liquid ammonia with the formation of 6-CB9H12- which was used as a starting compound for preparing the 4-CB8H14, 9-L-6-CB9H13 (L = (CH3)2S, CH3CN and P(C6H5)3), 1-(η5-C5H5)-1,2-FeCB9H10-, and 2,3-(η5-C5H5)2-2,31-Co2CB9H10- carboranes. The 4-CB8H14 compound was dehydrogenated at 623 K to give 4-(7)-CB8H12 carborane. Base degradation of 6-N(CH3)3-6-CB9H11 in methanol resulted in the formation of 3,4-μ-N(CH3)3CH-B5H10. The structure of all compounds was proposed on the basis of their 11B and 1H NMR spectra and X-ray diffraction was used in the case of the transition metal complexes.

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.

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.

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