Synthetic Access to a Novel Binaphthyl Ligand Bearing a Phosphine and a Triazole Donor Site

The combination of a diphenylphospinyl and a triazol-3-yl unit was realized for the first time at a 1,1'-binaphthyl backbone. This novel type of P,N-ligand is accessible as an enantiomerically pure compound in just a few steps. First experiments on the coordination chemistry with palladium(II) chloride have been carried out. A series of intermediates and a binuclear palladium(II) complex could be characterized by X-ray crystal structure analysis

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Zur Struktur und Komplexchemie von Phosphinoderivaten des 5-Methoxy-2(5H)-furanons / Structure and Coordination Chemistry of Phosphino Derivatives of 5-Methoxy-2(5H)-furanon

Zeitschrift für Naturforschung B ◽

10.1515/znb-1980-0904 ◽

1980 ◽

Vol 35 (9) ◽

pp. 1075-1082 ◽

Cited By ~ 3

Author(s):

D. Fenske ◽

H. Prokscha ◽

P. Stock ◽

H. J. Becher

Keyword(s):

Crystal Structure ◽

Coordination Chemistry ◽

Structure Analysis ◽

Model Compound ◽

Crystal Structure Analysis ◽

X Ray ◽

Derivatives Of ◽

Cl Atoms ◽

Cl Atom ◽

Similar Complex

With R2PSi(CH3)3 (R = C6H5, i-C3H7, t-C4H9) one Cl atom of 3,4-dichlor-5-methoxy-2(5 H)-furanon (1) is substituted by the R2P group. An x-ray crystal structure analysis of the phosphino derivative with R = C6H5 (2) it has shown that of the two Cl atoms in 1 only the β-position (to C= O) is substituted. The coordination chemistry of 2 and its bis- (diphenylphosphino) derivative (3) is studied by preparation of the compounds 2 · Mo(CO)5 and 3 · Mo(CO)4. With PdCl2 · 2 C6H5CN (2) gives a dinuclear complex [2 · PdCl2]2, with bridging Cl atoms. The structure is established by a comparison with the similar complex of PdCl2 and 2-chloro-diphenylphosphino-maleic acid dimethylestor, which was synthesized as a model compound and studied by x-ray crystal structure analysis.

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Synthesis and X-Ray Crystal Structure Analysis of 1,4-Epoxy-4-methyl- 1H,4H-2,3-benzodioxepin

Zeitschrift für Naturforschung B ◽

10.1515/znb-2011-0412 ◽

2011 ◽

Vol 66 (4) ◽

pp. 419-424

Author(s):

David S. Giera ◽

Lothar Hennig ◽

Thomas Gelbrich ◽

Christoph Schneider

Keyword(s):

Crystal Structure ◽

Structure Analysis ◽

Crystal Structure Analysis ◽

Acetate Solution ◽

Enantiomerically Pure ◽

X Ray ◽

Monoclinic Form ◽

Secondary Ozonide ◽

Orthorhombic Modification ◽

Polymorphic Forms

Ozonolysis of 2-methyl-1H-indene (1) afforded the stable secondary ozonide 1,4-epoxy-4-methyl- 1H,4H-2,3-benzodioxepin (2). This compound crystallizes in two polymorphic forms, depending on the solvent used. The monoclinic form 2a containing two symmetry-independent molecules (enantiomers) is obtained by crystallization from dichloromethane. In contrast, the orthorhombic modification 2b is obtained from ethyl acetate solution and crystallizes as a conglomerate of enantiomerically pure single crystals. Additionally, the ring-opened product 2-(2-oxopropyl)benzoic acid (3) was obtained and investigated by X-ray crystal structure analysis.

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

Journal of Chemical Research ◽

10.1177/174751989902300930 ◽

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.

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