CO-ORDINATION COMPLEXES OF NIOBIUM AND TANTALUM. I. COMPLEX FORMATION OF NIOBIUM AND TANTALUM PENTAHALIDES AND NIOBIUM(V) OXYCHLORIDE WITH ACETYLACETONE IN ALCOHOL SOLUTIONS AND FORMATION OF OXO-DICHLORO-ACETYLACETONATO NIOBIUM(V)
Complexes of the type MX/sub 2/AcAc(OR)/sub 2/, where M = Nb(V), Ta(V); X = Cl,Br; AcAc = acetylacetone; and R == CH/sub 5/, C/sub 2/H/sub 5/ were prepared from the metal pentahalides and acetylacetone in the parent alcoholic solutions. They are stable crystalline substances, but in solutions in alcohols interactions with solvent molecules occur, as is evident from conductivity and molecular weight studies. Powder x-ray diffraction photographs showed that the methoxo chloro and bromo derivatives of niobium and tantalum are isomorphous and that the analogous ethoxo complexes form another isomorphous group. Infrared spectra were analyzed and a tentative assignment of some characteristic vibrational modes is given. Metal-ligand vibrational modes appear at frequencies close to those in other metal acetylacetonates and metal alkoxides. Under similar experimental conditions, starting from NbOCl/sub 3/ and acetylacetone in methyl and ethyl alcohol solutions, complex derivatives of the same type, NbCl/ sub 2/AcAc(OR)/sub 2/, were isolated. These results imply the unexpected solvolysis of the niobiumoxygen bond in alcohol solutions. A compound of the formula STANbOCl/sub 2/AcAc!/sub x/ was isolated from the reaction of NbOCl/sub 3/ with acetylacetone. Infrared spectrum of this oxodichloro-acetylacetonato- niobium (V) revealed the presence of co-ordinated acetylacetone and the vibrational modes of the niobium-oxygen double bond. Deuteration studies permitted the assignment of some bands. (auth)
- Research Organization:
- Univ. of Zagreb; Rudjer Boskovic Inst., Zagreb
- NSA Number:
- NSA-17-037192
- OSTI ID:
- 4636661
- Journal Information:
- Journal of Inorganic and Nuclear Chemistry (England) Merged with Inorg. Nucl. Chem. Lett. to form Polyhedron, Vol. Vol: 25; Other Information: Orig. Receipt Date: 31-DEC-63
- Country of Publication:
- Country unknown/Code not available
- Language:
- English
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Related Subjects
ACETONE
ALCOHOLS
CHEMICAL REACTIONS
CRYSTALS
DIFFRACTION
ELECTRIC CONDUCTIVITY
FREQUENCY
HALIDES
INFRARED RADIATION
MOLECULES
NIOBIUM CHLORIDES
NIOBIUM COMPLEXES
OXYGEN COMPOUNDS
PHOTOGRAPHY
POWDERS
PRODUCTION
SOLUTIONS
SOLVENTS
SPECTRA
STABILITY
TANTALUM CHLORIDES
TANTALUM COMPLEXES
VIBRATIONS
WEIGHT
X RADIATION