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Synthesis of the Naphthol Skeleton from Pentacarbonyl-[methoxy(phenyl)carbene]chromium (O) and Tolan

✍ Scribed by Dr. Karl Heinz Dötz


Book ID
101546335
Publisher
John Wiley and Sons
Year
1975
Tongue
English
Weight
247 KB
Volume
14
Category
Article
ISSN
0044-8249

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✦ Synopsis


Thermal decomposition (1 10 "C) of ammonium heptamolybdate, (NH4)6M07024.4Hz0, affords 2(NH4)z0. 5M003"]. This product proved identical with an ammonium polymolybdate that crystallized during several days at ca. 80°C as colorless prisms from concentrated aqueous ammonium heptamolybdate solutions to which some ammonia had been addedrZ].

For determination of the structure, the intensities of 3356 reflections were measured on a Siemens four-circle diffractometer with CUK? radiation. The triclinic, centrosymmetrical cell with the lattice parameter! a= 10.996+0.002, p = 99.25 & 0.08, y = 107.13 $-0.08", contains five crystallographically independent molybdenum atoms whose positions were determined by Patterson methods. The coordinates of the oxygen and nitrogen atoms were obtained by a difference Fourier synthesis. The atomic parameters (except for H) were refined to an R value of 5.1 (anisotropic temperature factors, corrections for absorption and extinction).

Because of the very slow dissolution of the compound in water (with destruction of the structure) a high-polymeric anion structure was suspected. However, it was found that isolated decamolybdate ions, Mo, o054, were present in which one Mo8OZ8 unit built up of edge-bridged MOO, octahedra was connected at corners to two M o o 4 tetrahedra (Fig. 1). 6=10.921 f0.


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