Claims
- 1. A metal complex represented by the formula [(L).sub.a (NO).sub.b M.sub.c Z.sub.d ].sub.x wherein M is niobium or vanadium; each Z is a halogen, CN, SCN, OCN, or SnCl.sub.3 radical; each (L) is a ligand represented by the formula R.sub.3 QO, O, [(RCO).sub.2 CH--, R--S--R, R.sup.5 (CN).sub.b, R.sup.5 (COO--.sub.b, (R.sup.5 COR.sup.2 COO--, or ##STR6## wherein a, b, c, and d, are integers wherein a is 1-6, b is 1-2, c is 1-4, d is 0-6, and the number of Z, (L), and NO groups in the complex is not greater than the number required for the metal to achieve the closed shell electronic configuration of the next higher atomic number inert gas; x is the number of the polymeric state of the complex; Q is phosphorus, arsenic, or antimony; R is an aromatic or saturated aliphatic hydrocarbon radical having up to 20 carbon atoms per molecule; R.sup.2 is a divalent R radical; R.sup.3 is a divalent saturated or ethylenically unsaturated aliphatic radical having from 4 to 10 carbon atoms; and R.sup.5 is an aromatic, saturated aliphatic, or ethylenically unsaturated aliphatic radical having up to 30 carbon atoms.
- 2. The metal complex of claim 1 wherein said M is vanadium.
- 3. The complex of claim 1 wherein said metal complex is NOBr-treated (ethylenedinitrile)O.sub.2 V.sub.2 (acetate).sub.4, NOCl-treated VO(lactate).sub.2, NOI-treated (2,4-pentanedionate).sub.2 O.sub.V, NOCl-treated ( 2,4-pentanedionate).sub.2 (triphenylphosphine oxide)V, NOBr-treated (1-phenyl-1,3-butanedionate).sub.2 V, NO-treated (2,4-pentanedionate)OVCl.sub.2, NO-treated (acetate).sub.2 VCl.sub.4, NOCl-treated (2,4-pentanedionate).sub.3 V, or NOBr-treated (1-phenyl-1,3-butanedionate).sub.3 V.
- 4. The metal complex of claim 1 wherein M is niobium.
- 5. The metal complex of claim 1 further including a diluent in which said complex is at least partially soluble.
- 6. The metal complex of claim 5 wherein said diluent is carbon tetrachloride, methylene chloride, benzene, cyclohexane, xylene, isooctane, or chlorobenzene.
- 7. The metal complex of claim 1 wherein said complexing agent is triphenylphosphine oxide, tribenzylphosphine oxide, trimethylarsine oxide, tributylstibine oxide, tricyclopentylarsine oxide, tricyclohexylphosphine oxide, trieicosylstibine oxide, tridecylphosphine oxide, tri-p-tolylphosphine oxide, acetic acid, propionic acid, butanoic acid, 2-methylpropionic acid, pentanoic acid, hexanoic acid, octanoic acid, dodecanoic acid, hexadecanoic acid, octadecanoic acid, triacontanoic acid, benzoic acid, phenylacetic acid, oxalic acid, malonic acid, acetoacetic acid, benzoylacetic acid, .beta.-acetylpropionic acid, .delta.-acetobutyric acid, acetonitrile, butyronitrile, 1,2-cyclohexylenedinitrile, ethylenedinitrile, acrylonitrile, 2,4-pentanedione, 1,3-diphenyl-1,3-pentanedione, 3,5-heptanedione, 4-cyclohexyl-2,4-butanedione, ethylsulfide, phenylsulfide, methylethyl sulfide, thiophene, or tetrahydrothiophene.
- 8. A metal complex represented by [(L).sub.a (NO).sub.b M.sub.c Z.sub.d ].sub.x consisting essentially of a product formed by the admixture, under complex forming conditions, of (A) a niobium or vanadium compound which is the niobium or vanadium halide, oxyhalide, cyanide, thiocyanate, cyanate, trichlorostannate, or salt of a hydrocarbon organic acid having up to 30 carbon atoms per molecule, (B) NO or a nitrosyl halide, and (C) a complexing agent capable of complexing with said niobium or vanadium,
- wherein in said metal complex M is niobium or vanadium, Z is halogen, CN, SCN, OCN, or SnCl.sub.3 radical, L is a ligand represented by the formula O, [(RCO).sub.2 CH--, R--S--R, R.sup.5 (CN).sub.b, R.sup.5 (COO--.sub.b, (R.sup.5 COR.sup.2 COO--, or ##STR7## a, b, c, and d are integers wherein a is 1-6, b is 1-2, c is 1-4, d is 0-6, and x is a number representative of the polymeric state of the complex, R is an aromatic or saturated aliphatic hydrocarbon radical of up to 20 carbon atoms R.sup.2 is a divalent R radical, R.sup.3 is a divalent saturated or ethylenically unsaturated aliphatic radical of 4 to 10 carbon atoms, and R.sup.5 is an aromatic, saturated aliphatic, or ethylenically unsaturated aliphatic radical of up to 30 carbon atoms,
- and wherein said (C) complexing agent is represented by the formula: RCOCH.sub.2 COR; R.sup.5 (CN).sub.b ; R--S--R; ##STR8## acids of the formula R.sup.5 (COOH).sub.b ; or ketoacids of the formula R.sup.5 COR.sup.2 COOH,
- employing a molar proportion of vanadium or niobium compound to complexing agent in the range of about 0.1:1 to 10:1.
- 9. The metal complex of claim 8 wherein said vanadium compound is VBr.sub.3, VCl.sub.2, VCl.sub.3, VCl.sub.4, VF.sub.3, VF.sub.5, VOCl, VOBr, VOBr.sub.2, VOBr.sub.3, VO.sub.2 Cl, VOCl.sub.2 or VOCl.sub.3.
- 10. The metal complex of claim 8 wherein said niobium compound is NbBr.sub.5, NbCl.sub.5, NbF.sub.5, NbOBr.sub.3, or NbOCl.sub.3.
- 11. The metal complex of claim 8 wherein said vanadium or niobium compound is niobium or vanadium halide or oxyhalide.
- 12. The metal complex of claim 8 wherein said niobium or vanadium compound is NbCl.sub.5, said complexing agent is benzoic acid, and said NO or nitrosyl halide is said NO.
- 13. A process for preparing a metal complex which comprises admixing under complexing conditions and in complex forming ratios
- (A) a niobium or vanadium compound which is the niobium or vanadium halide, oxyhalide, cyanide, thiocyanate, cyanate, trichlorostannate, or salt of a hydrocarbon acid having up to 30 carbon atoms per molecule,
- with (B) NO or a nitrosyl halide,
- and (C) with at least one complexing agent capable of complexing said niobium or vanadium wherein said ratio of said niobium or vanadium compound to said complexing agent is in the range of about 0.1:1 to about 10:1, and
- wherein said complexing agent is represented by the formula:
- Rcoch.sub.2 cor: r.sup.5 (cn).sub.b ; R--S--R; ##STR9## acids of the formula R.sup.5 (COOH).sub.b ; or ketoacids of the formula R.sup.5 COR.sup.2 COOH; wherein R is an aromatic or saturated aliphatic hydrocarbon radical having up to 20 carbon atoms; R.sup.2 is a divalent R radical, R.sup.3 is a divalent saturated or ethylenically unsaturated aliphatic radical having 4 to 10 carbon atoms, R.sup.5 is an aromatic, saturated aliphatic, or ethylenically unsaturated aliphatic radical having up to 30 carbon atoms, and b is an integer of 1 or 2.
- 14. The process for preparing the metal complex according to claim 13 wherein said niobium or vanadium compound is said halide or oxyhalide.
- 15. The process according to claim 13 wherein said niobium or vanadium compound is said vanadium compound, and is selected from the group consisting of VBr.sub.3, VCl.sub.2, VCl.sub.3, VCl.sub.4, VF.sub.3, VF.sub.5, VOCl, VOBr, VOBr.sub.2, VOBr.sub.3, VO.sub.2 Cl, VOCl.sub.2, and VOCl.sub.3.
- 16. The process according to claim 13 wherein said niobium or vanadium compound is said niobium compound and is selected from the group consisting of NbBr.sub.5, NbCl.sub.5, NbF.sub.5, NbOBr.sub.3, or NbOCl.sub.3.
- 17. The metal complex prepared by the process of reacting (a) niobium chloride with (b) NO and (c) benzoic acid, under complex-forming conditions employing a molar ratio of about 1:2 niobium chloride:benzoic acid.
- 18. The metal complex which is NO-treated benzoic acid NbCl.sub.5, NO-treated (tetrahydrothiophene) NbBr.sub.5 or NO-treated (tetrahydrothiophene) NbCl.sub.5.
Parent Case Info
This application is a continuation of copoending application Ser. No. 274,727, filed July 24, 1972, now abandoned which is a divisional application of Ser. No. 80,230, filed Oct. 12, 1970, now U.S. Pat. No. 3,691,253, issued Sept. 12, 1972, which is a divisional of copending application Ser. No. 694,875, filed Jan. 2, 1968, now U.S. Pat. No. 3,562,178 issued Feb. 9, 1971, which is a continuation-in-part of application Ser. No. 635,656, filed May 3, 1967, now abandoned.
US Referenced Citations (2)
Number |
Name |
Date |
Kind |
3294828 |
Werner |
Dec 1966 |
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3475471 |
Maxfield |
Oct 1969 |
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Divisions (2)
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Number |
Date |
Country |
Parent |
80230 |
Oct 1970 |
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Parent |
694875 |
Jan 1968 |
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Continuations (1)
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Number |
Date |
Country |
Parent |
274727 |
Jul 1972 |
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Continuation in Parts (1)
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Number |
Date |
Country |
Parent |
635656 |
May 1967 |
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