Eine effiziente Synthesemethode für DiarylallenyIiden(pentacarbonyl)chrom- und -wolfram-Komplexe -Kristallstruktur von (CO)5Cr=C=C=CPh2 / An efficient Synthesis of Diarylallenylidene Pentacarbonyl Chromium and Tungsten Complexes - Crystal Structure of (CO)5Cr=C=C=CPh2

1994 ◽  
Vol 49 (9) ◽  
pp. 1207-1214 ◽  
Author(s):  
Helmut Fischer ◽  
David Reindl ◽  
Gerhard Roth
Keyword(s):  
Crystal Structure ◽  
Structure Analysis ◽  
Good Yield ◽  
Efficient Synthesis ◽  
X Ray ◽  
Tungsten Complexes ◽  
And Tungsten

An efficient synthesis of diarylallenylidene pentacarbonyl chromium and tungsten com­plexes is presented. Irradiation of M(CO)6 in THF affords (CO)sM[THF], Substitution of the THF ligand by diarylpropargylalcoholate and subsequent desoxygenation with COCF gives the title compounds in good yield. (The structure of diphenylallenylidene pentacarbonyl chromium has been determined by X-ray structure analysis

Übergangsmetallkomplexe mit Schwefelliganden, LXI / Transition Metal Complexes with Sulfur Ligands, LXI

1991 ◽  
Vol 46 (11) ◽  
pp. 1435-1448 ◽  
Author(s):  
Dieter Sellmann ◽  
Bernd Seubert ◽  
Wolfgang Kern ◽  
Falk Knoch ◽  
Matthias Moll
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Structure Analysis ◽  
Transition Metal Complexes ◽  
Coordination Geometry ◽  
X Ray ◽  
Tungsten Complexes ◽  
Reductive Nitrosylation ◽  
Hydrolysis Of ◽  
And Tungsten

In order to study the properties of sulfur coordinated metal centres, the chromium and tungsten complexes [Cr(NO)(µ-′S4′)]2 (4), (NR4)2[W(NO)2(′S2′)2] (1) (R = Me (la), n-Bu (lb)), [W(NO)2(′S4′)] (2), [µ-O{W(NO)(′S4′)}2] (3) and [W(NPR3)(NO)(′S4′)] (5) (R = Me (5a), Et (5 b)) were synthesized (′S2′2- = 1.2-benzenedithiolate(2-); ′S4′2- = 1.2-bis(2-mercaptophenylthio)ethane(2-)). la and lb result from the reductive nitrosylation of Li2[W(′S2′)3] which was prepared by reduction of [W(′S2′)3] with n-BuLi. la was also obtained from [W(NO)2(Cl)2]n, ′S2′2- and NMe4+. Alkylation of la or lb by 1.2-dibromoethane yields 2, whose X-ray structure analysis shows that W is pseudooctahedrally coordinated by two trans thiolato S, two cis thioether S and two cis N atoms of linear W-NO groups. 2 was also obtained from [W(NO)2(CH3CN)4](BF4)2 or [W(NO)2(Cl)2]n and ′S4′2--. The reaction of [W(NO)2(Cl)2]n yielded the dinuclear oxo-bridged complex 3 as a by-product in small amounts. In preparative amounts, 3 was synthesized by hydrolysis of [W(Cl)(NO)(′S4′)]. In contrast to the analogous Mo complex, 2 does not react with N2H4; with the ligands PMe3 and PEt3, it gives the corresponding phosphiniminato complexes 5 and free phosphineoxides OPR3. In order to compare the [M(NO)2(′S4′)] complexes (M = Cr, Mo, W), the structure of [Cr(NO)2(′S4′)] was determined by X-ray structure analysis. The Cr complex exhibits the same molecular coordination geometry as 2. While growing crystals of [Cr(NO)2(′S4′)], the dinuclear Cr complex 4 was also formed. Its X-ray structure analysis shows each of the Cr centres to be coordinated pseudooctahedrally by five sulfur donors and one nitrosyl N donor. 4 was also obtained by the reaction of [Cr(CO)4(nor)] with ′S4′2- and NOBF4.

scholarly journals Preparative-scale HPLC Resolution of Metallacyclic η3-Allyltricarbonyliron Complexes and Determination of the Absolute Configuration by X-Ray Crystal Structure Analysis

1999 ◽  
Vol 23 (9) ◽  
pp. 578-579
Author(s):  
Rainer Schobert ◽  
Hermann Pfab ◽  
Jutta Böhmer ◽  
Frank Hampel ◽  
Andreas Werner
Keyword(s):  
Crystal Structure ◽  
Silica Gel ◽  
Structure Analysis ◽  
Absolute Configuration ◽  
Crystal Structure Analysis ◽  
Preparative Scale ◽  
X Ray ◽  
The Absolute

Racemates of (η3-allyl)tricarbonyliron lactone complex Fe(CO)3{η1:η3-C(O)XCH2CHCMeCH2} 1a (X = O) and (η3-allyl)tricarbonyliron lactam complex 2a (X = NMe) are resolved on a preparative scale by HPLC on cellulose tris(3,5-dimethylphenyl)carbamate/silica gel RP-8 and the absolute configuration of (-)-2a is determined by X-ray crystal structure analysis.

Second-Generation Inhibitors for the Metalloprotease Neprilysin Based on Bicyclic Heteroaromatic Scaffolds: Synthesis, Biological Activity, and X-Ray Crystal-Structure Analysis

2005 ◽  
Vol 88 (4) ◽  
pp. 731-750 ◽  
Author(s):  
Stefan Sahli ◽  
Brian Frank ◽  
W. Bernd Schweizer ◽  
François Diederich ◽  
Denise Blum-Kaelin ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Biological Activity ◽  
Structure Analysis ◽  
Second Generation ◽  
Crystal Structure Analysis ◽  
X Ray

Regiospezifische Insertion von [SCN]- und [SeCN]- in die S – C- bzw. Se– C-Bindung Übergangsmetall-koordinierter Thietane und SelenetaneRegiospecific Insertion of [SCN]- and [SeCN]- in the S–C- and Se–C-Bond of Transition-Metal-Coordinated Thietanes and Selenetanes

1993 ◽  
Vol 48 (11) ◽  
pp. 1613-1620 ◽  
Author(s):  
Helmut Fischer ◽  
Claudia Kalbas ◽  
Carsten Troll ◽  
Klaus H. Fluck
Keyword(s):  
Nitrogen Atom ◽  
Transition Metal ◽  
Structure Analysis ◽  
Trans Isomer ◽  
X Ray ◽  
Tungsten Complexes ◽  
Membered Heterocycle

Pentacarbonyl(thietane)tungsten complexes react with thiocyanate, [SCN]-, and SiO2/H2O by insertion of the CN group into a S—C bond of the four-membered heterocycle, 1,3-migration of the pentacarbonyltungsten fragment and protonation of the nitrogen atom to give tungsten-coordinated thiazinthione complexes. Analogously, the reactions of a thietane tungsten complex with [SeCN]- and SiO2/H2O affords a thiazinselone complex. A selenazinthione complex is obtained from a selenetane complex and [SCN]- (+ SiO2/H2O). The insertions are regiospecific and stereoselective. The structure of the trans-isomer of a pentacarbonyl-(thiazinthione) complex has been established by X-ray structure analysis.

Imido complexes of molybdenum and tungsten(VI); X-ray crystal structure of cis-(η1-CF3SO3)2 W(NBut)2(NH2But)2

Polyhedron ◽  
1989 ◽  
Vol 8 (24) ◽  
pp. 2947-2949 ◽  
Author(s):  
Andreas A. Danopoulos ◽  
Geoffrey Wilkinson ◽  
Michael B. Hursthouse ◽  
Bilquis Hussain
Keyword(s):  
Crystal Structure ◽  
X Ray ◽  
Imido Complexes ◽  
And Tungsten
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