Komplexbildung von Rhodium mit 6.6-Dimethylfulven / Complex Formation of Rhodium with 6.6-Dimethylfulvene

1983 ◽  
Vol 38 (11) ◽  
pp. 1454-1459 ◽  
Author(s):  
Jörn Müller ◽  
Rainer Stock ◽  
Joachim Pickardt
Keyword(s):  
Complex Formation ◽  
Diffraction Analysis ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
X Ray

Abstract Reaction of [(nbd)RhCl]2 (nbd = nor bornadiene) with CH3Li and 6.6-dimethylfulvene yields (nbd)Rh(2-propenylcyclopentadienyl). (cod)Rh(Cl)P(CH3)3 (cod = 1.5-cyclooctadiene), obtained by cleavage of [(cod)RhCl]2 with P(CH3)3, reacts with 6.6-dimethyl-fulvene and CH3Li or i-C3H7MgBr with substitution of cod by dimeric fulvene ligands the nature of which depends on the alkyl reagent. The new complexes were characterized by NMR spectra and in one case by X-ray diffraction analysis.

Degradation-insertion reactions of decaborane(14) with inorganic salts

1983 ◽  
Vol 48 (9) ◽  
pp. 2593-2603 ◽  
Author(s):  
Karel Baše
Keyword(s):  
Diffraction Analysis ◽  
Nmr Spectra ◽  
Inorganic Salts ◽  
Analogous Reaction ◽  
X Ray Diffraction ◽  
Insertion Reactions ◽  
X Ray ◽  
Lewis Bases ◽  
H Nmr

Decaborane(14) reacts with NaNO2 in tetrahydrofuran forming the [9-tetrahydrofuran-6-NO2B10H12]- salt which after protonization with concentrated H2SO4 or diluted HCl affords azaboranes 6-NB9H12 and 4-NB8H13, respectively. The 6-NB9H12 azaborane is hydrolyzed to the 4-NB8H13 azaborane and reacts with Lewis bases under the formation of the 9-L-6-NB9H12 ligand derivatives (L = (CH)S, CHCN, (CH)P). By the reduction of 9-CHCN-6-NBH with LiAlH4 in tetrahydrofuran the 6-NB9H13- anion was prepared. By an analogous reaction of decaborane(14) with KHSO3 in water and by a subsequent protonization of the formed intermediate with concentrated H2SO4 or diluted HCl the thiaboranes 6-SB9H11 and 4-SB8H12, respectively, were prepared. The reaction of decaborane(14) with Na2SeO3 in tetrahydrofuran followed by the protonization of the intermediate with diluted HCl afforded the 7,8-Se2B9H9 species. Structures of all compounds were proposed on the basis of the 11B and 1H NMR spectra; in the case of 4-NB8H13, the structure was determined by the X-ray diffraction analysis.

Electronic Structure of 2,6-Bis{.N-(2-hydroxyphenyl)immoinethyl}-4-methylphenol

1999 ◽  
Vol 54 (7) ◽  
pp. 929-939 ◽  
Author(s):  
Miki Hasegawa ◽  
Yasunori Yamada ◽  
Ken-ichi Kumagai ◽  
Toshihiko Hoshi
Keyword(s):  
Diffraction Analysis ◽  
Electronic Absorption ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
Mo Calculations ◽  
Absorption Bands ◽  
Polar Solvents ◽  
Additional Band ◽  
X Ray ◽  
H Nmr

The electronic and molecular structure of 2,6-bis{N-(2-hydroxyphenyl)iminomethyl}-4- methylphenol (hpimp) is clarified from the measurements of electronic absorption and 1H NMR spectra in various solvents and an X-ray diffraction analysis, together with MO calculations. Electronic absorption bands of hpimp are at 422, 397.9, 359, 341, 294.3, 265.8, and 224 nm in the non-polar solvent cyclohexane. In polar solvents, such as methanol, an additional band which is assigned to a partly formed keto-amine hpimp, is observed at 499 nm. From the 1H NMR spectra it is seen that hpimp exists in the enol-imine form in non-polar solvents, and as an equilibrium mixture of enol-imine and keto-amine forms in polar solvents. Each electronic absorption band of solid hpimp in a KBr disk is broadened compared with the solution state, and an additional band, again assigned to the keto-amine form, appears around 499 nm. An X-ray diffraction analysis shows that hpimp assumes a keto-amine structure in the solid state, and forms a column structure along the c-axis. MO calculations suggest that the enol-imine hpimp has a twist structure around the two C−C single bonds, the twist angle being 100° to 120°.

Structural organization of mercury(II) and copper(II) dithiocarbamates from EPR and 13C and 15N MAS NMR spectra and X-ray diffraction analysis

2008 ◽  
Vol 34 (1) ◽  
pp. 59-69 ◽  
Author(s):  
A. V. Ivanov ◽  
E. V. Korneeva ◽  
B. V. Bukvetskii ◽  
A. S. Goryan ◽  
O. N. Antzutkin ◽  
...  
Keyword(s):  
Diffraction Analysis ◽  
Nmr Spectra ◽  
Structural Organization ◽  
Mas Nmr ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals π-Olefin-Iridium-Komplexe, VII [1] Komplexbildung von Iridium mit Fulvenen / π-Oefin Iridium Complexes, VII [1] Complex Formation of Iridium with Fulvenes

1981 ◽  
Vol 36 (10) ◽  
pp. 1219-1224 ◽  
Author(s):  
Jörn Müller ◽  
Rainer Stock ◽  
Joachim Pickardt
Keyword(s):  
Complex Formation ◽  
Diffraction Analysis ◽  
Mass Spectra ◽  
Iridium Complexes ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cyclopentadienyl Ligand

Abstract Reactions of [Ir(COD)Cl]2 (COD = 1,5-cyclooctadiene) with either i-C3H7MgBr or CH3Li in the presence of dimethyl-and diethylfulvene, respectively, yield complexes of the type [Ir(COD)(C5H4R)] where C5H4R is a cyclopentadienyl ligand. The nature of the substituent R depends on the fulvene as well as on the alkyl reagent. The compounds were characterized by NMR and mass spectra and in one case by X-ray diffraction analysis.

Reactions of PO(NCS)3 with 4-Hydroxy-1,3-dioxanes. Crystal Structure of rel-(2S,4R,5S,6S)-2,6-Diethyl-5-methyl-4-(N'-benzylthioureido)-1,3-dioxane

1992 ◽  
Vol 57 (6) ◽  
pp. 1299-1313 ◽  
Author(s):  
Juraj Bernát ◽  
Ladislav Kniežo ◽  
Gabriela Birošová ◽  
Miloš Buděšínský ◽  
Jaroslav Podlaha ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Diffraction Analysis ◽  
Nmr Spectra ◽  
Crystalline Form ◽  
The Other ◽  
Axial Position ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Alkyl Groups

Substituted 4-hydroxy-1,3-dioxanes II react rapidly with PO(NCS)3 to give 4-isothiocyanato-1,3-dioxanes III. The 1H NMR spectra showed that in the isothiocyanate IIIa the predominant stereoisomer has its NCS group in axial position. The addition of benzylamine to the isothiocyanates IIIa and IIIb gave uniform thioureas IVa and IVb with equatorial alkyl groups at 2 and 6 positions and axial thioureido group at 4 position. On the other hand, the isothiocyanate IIIc reacts with benzylamine to give a mixture of three stereoisomeric thioureas V,VI, and VIII. The structure of VI was proved by means of X-ray diffraction analysis; in crystalline form the molecules of VI are present as H-bonded dimers (N-H...O).

scholarly journals Synthesis of 4-(2H-[1,2,4]-Triazol-5-ylsulfanyl)-1,2-dihydropyrazol-3-one via Ring-Switching Hydrazinolysis of 5-Ethoxymethylidenethiazolo [3,2-b][1,2,4]triazol-6-one

Molbank ◽  
10.3390/m1022 ◽  
2018 ◽  
Vol 2018 (4) ◽  
pp. M1022 ◽  
Author(s):  
Serhii Holota ◽  
Yaroslav Shylych ◽  
Halyna Derkach ◽  
Olexandr Karpenko ◽  
Andrzej Gzella ◽  
...  
Keyword(s):  
Acetic Anhydride ◽  
Diffraction Analysis ◽  
Nmr Spectra ◽  
Chloroacetic Acid ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
One Pot ◽  
X Ray ◽  
Ethanol Medium ◽  
Williamson Reaction

4-(1H-[1,2,4]-Triazol-5-ylsulfanyl)-1,2-dihydropyrazol-3-one (4) was synthesized with a yield of 55% via ring-switching hydrazinolysis of 5-ethoxymethylidenethiazolo[3,2-b][1,2,4] triazol-6-one (3) in ethanol medium. The initial 1H-[1,2,4]-triazole-3-thiol (1) was modified via a two-step reaction: S-alkylation with chloroacetic acid under Williamson reaction conditions, and further one-pot cyclization–condensation with triethylorthoformate in the acetic anhydride medium, yielding compound 3. The structures of compounds 3 and 4 were confirmed by LC-MS, NMR spectra and a single X-ray diffraction analysis (for compound 4).

tert-Butylimino-cyclopentadienyIvanadiuni(V)-Verbindungen Darstellung, Struktur und NMR-spektroskopische Untersuchungen

1987 ◽  
Vol 42 (7) ◽  
pp. 881-888 ◽  
Author(s):  
Fritz Preuss ◽  
Harald Becker ◽  
Hans-Joachim Häusler
Keyword(s):  
Molecular Structure ◽  
Diffraction Analysis ◽  
Temperature Dependence ◽  
Metal Atom ◽  
Nmr Spectra ◽  
X Ray Diffraction ◽  
Nmr Spectrum ◽  
X Ray ◽  
H Nmr ◽  
Intramolecular Rearrangements

Abstract The cyclopentadienyl compounds tC4R9N = VCpCl2 (2). tC4H9N = VCp(OtC4H9)Cl, tC4H9N = VCp(OtC4H9)(R) (R = CH3, "C4H9, CH2SiMe3), tC4H9N = VCp2(OtC4H9) (5) and ,tC4H9N = VCp(OtC4H9)2 have been prepared starting from tC4H9N = VCl31H and 51V NMR spectra are discussed; except for 5, the C5H5 rings are η5-coordinated to the metal atom. The temperature dependence of the 1H NMR spectrum of 5 indicates two types o f intramolecular rearrangements: η1/η5-Interchange of the C5H5 rings and fluxional behavior of the η1-C5H5 ring. The molecular structure of 2 has been investigated by X-ray diffraction analysis.

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