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
No coin nor oath required. For personal study only.
✦ 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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