USRE27467E - Complexes of - Google Patents
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- USRE27467E USRE27467E US27467DE USRE27467E US RE27467 E USRE27467 E US RE27467E US 27467D E US27467D E US 27467DE US RE27467 E USRE27467 E US RE27467E
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- phosphine
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- 229910052751 metal Inorganic materials 0.000 abstract description 9
- 239000002184 metal Substances 0.000 abstract description 9
- 150000003839 salts Chemical class 0.000 abstract description 9
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 abstract description 8
- 150000001875 compounds Chemical class 0.000 abstract description 8
- 239000010949 copper Substances 0.000 abstract description 5
- 229910000073 phosphorus hydride Inorganic materials 0.000 abstract description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract description 3
- 238000000151 deposition Methods 0.000 abstract description 2
- 239000012442 inert solvent Substances 0.000 abstract description 2
- CIUQDSCDWFSTQR-UHFFFAOYSA-N [C]1=CC=CC=C1 Chemical group [C]1=CC=CC=C1 CIUQDSCDWFSTQR-UHFFFAOYSA-N 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 239000000243 solution Substances 0.000 description 9
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000000376 reactant Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 4
- 238000000862 absorption spectrum Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical group 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 150000003003 phosphines Chemical class 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- QJIMTLTYXBDJFC-UHFFFAOYSA-N (4-methylphenyl)-diphenylphosphane Chemical compound C1=CC(C)=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 QJIMTLTYXBDJFC-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- RRQYJINTUHWNHW-UHFFFAOYSA-N 1-ethoxy-2-(2-ethoxyethoxy)ethane Chemical compound CCOCCOCCOCC RRQYJINTUHWNHW-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 description 1
- XOBKSJJDNFUZPF-UHFFFAOYSA-N Methoxyethane Chemical compound CCOC XOBKSJJDNFUZPF-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- VPEPTFVFITUGAD-UHFFFAOYSA-N bis(4-methylphenyl)-phenylphosphane Chemical compound C1=CC(C)=CC=C1P(C=1C=CC(C)=CC=1)C1=CC=CC=C1 VPEPTFVFITUGAD-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 150000004292 cyclic ethers Chemical class 0.000 description 1
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-O tert-butylammonium Chemical compound CC(C)(C)[NH3+] YBRBMKDOPFTVDT-UHFFFAOYSA-O 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- ZMANZCXQSJIPKH-UHFFFAOYSA-O triethylammonium ion Chemical compound CC[NH+](CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-O 0.000 description 1
- DMEUUKUNSVFYAA-UHFFFAOYSA-N trinaphthalen-1-ylphosphane Chemical compound C1=CC=C2C(P(C=3C4=CC=CC=C4C=CC=3)C=3C4=CC=CC=C4C=CC=3)=CC=CC2=C1 DMEUUKUNSVFYAA-UHFFFAOYSA-N 0.000 description 1
- IDXDWPWXHTXJMZ-UHFFFAOYSA-N tris(2,4,6-trimethylphenyl)phosphane Chemical compound CC1=CC(C)=CC(C)=C1P(C=1C(=CC(C)=CC=1C)C)C1=C(C)C=C(C)C=C1C IDXDWPWXHTXJMZ-UHFFFAOYSA-N 0.000 description 1
- KAAYGTMPJQOOGY-UHFFFAOYSA-N tris(2,5-dimethylphenyl)phosphane Chemical compound CC1=CC=C(C)C(P(C=2C(=CC=C(C)C=2)C)C=2C(=CC=C(C)C=2)C)=C1 KAAYGTMPJQOOGY-UHFFFAOYSA-N 0.000 description 1
- COIOYMYWGDAQPM-UHFFFAOYSA-N tris(2-methylphenyl)phosphane Chemical compound CC1=CC=CC=C1P(C=1C(=CC=CC=1)C)C1=CC=CC=C1C COIOYMYWGDAQPM-UHFFFAOYSA-N 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/50—Organo-phosphines
- C07F9/5045—Complexes or chelates of phosphines with metallic compounds or metals
Definitions
- ABSTRACT OF THE DISCLOSURE Complexes selected from those represented by the formulas wherein M is either copper or gold and each R' is phenyl. [aryl or a1karyl.]
- the compotmds are prepared by reacting a salt of B H with a salt of the metal M. in the presence of the phosphine and an inert solvent. The compounds are useful in depositing metal films on substrate surfaces.
- This invention relates to novel metal-organic compounds. More specifically, it concerns complexes of B ll or B iH with selected metals and phosphines, and to a method for their preparation.
- novel complexes of this invention are compounds selected from those represented by the formulas wherein M is a metal selected from the group consisting of copper and gold; and each R is [of 6-12 carbon atoms selected from the class consisting of aryl and alkaryL] phenyl.
- novel complexes of this invention are prepared by reacting a soluble polyboron salt of the formula MB H wherein M is alkali metal or R,,NH wherein n is a cardinal number of 0-4 inclusive and R is lower alkyl, with a soluble salt of the metal M in the presence of the phosphine, R P, and an inert medium.
- the salt of the metal M can be represented by the formulas CuX AgX, AuX and M'AuX," wherein X is one equivalent of an anion selected from the class consisting of chloride, bromide, nitrate, sulfate, formate, acetate, lactate and tartrate; X is selected from the class consisting of acetate, nitrate and fluoride, and X" is selected from the class consisting of chloride and bromide.
- the process is usually carried out at room temperatures, e.g. 20-30" C., or slightly higher temperatures, e.g., up to 50 C.
- room temperatures e.g. 20-30" C.
- slightly higher temperatures e.g., up to 50 C.
- the latter range is sometimes useful for effecting increased dissolution of some of the reactants.
- the temperature range is not critical and higher or lower temperatures may be used, but present no advantage.
- the R groups in the cation R,,'NH.; can be the same or different and the cations are represented by tert-butylammonium, diisopropylammonium, triethylammonium, tetramethylammonium, and the like.
- Pressure is not critical and solely for convenience, atmospheric pressure is ordinarily employed.
- Operable solvents include water, polar organic solvents that are at least partially miscible with water, and mixtures of the two.
- polar solvents include lower alkanols such as methanol, ethanol and isopropyl alcohol; cyclic ethers such as dioxane and tetrahydro furan; open-chain polyethers such as [1,2-dimethoxymethane] 1,2-dz'methoxyethane and di(2-ethoxyethyl) ether; and lower alkanenitriles such as acetonitrile and propionitrile.
- the reactants CsB Hw RbB l-l (CH NHB H and (C'H NHB H can be prepared as described in Aftanclilian et al., Inorg. Chem. 1, 736 (1962).
- Ammonium, other alkali-metal, and other substituted ammonium B 11 salts which make up the reactants in the process of this invention are prepared from the cesium or rubidium B H salt by conventional cation exchange techniques.
- R P representsative phosphines (R P), both as reactants and complexed ligand groups in the compounds of the invention, include triphenylphosphine, tritolylphosphine (0-, mand p-), tris(2,5-xylyl)phosphine, tris(2,4,6-trimethylphenyl) phosphine, phenyldi-p-tolylphosphine, diphenyl-p-tolylphosphine, tris(1-naphthyl)phosphine, tris- (biphenyl)phosphine, and the like]
- the novel complexes of this invention are crystalline solids. Their infrared absorption spectra indicate that the metal M is bonded directly to boron of the polyboron nucleus, and is not bonded to the hydrogen of the polyboron nucleus.
- the infrared absorption (KBr wafer) showed one B-d-I absorption band at 2550 cm.- (terminal hydrogen).
- the infrared absorption spectrum showed one B-H absorption band at 2515 cm.- (terminal hydrogen).
- the compounds of this invention are useful in the depsition of metal films on a substrate surface.
- metal films on a substrate surface.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
Abstract
COMPLEXES SELECTED FROM THOSE REPRESENTED BY THE FORMULAS
(1) (R3P)3MB11H14
AND
(2) ((R3P)4AG)2B11H13
WHEREIN M IS EITHER COPPER OR GOLD AND EACH R IS PHENYL, (ARYL OR ALKARYL). THE COMPOUNDS ARE PREPARED BY REACTING A SALT OF B11H14- WITH A SALT OF THE METAL M IN THE PRESENCE OF THE PHOSPHINE AND IN INERT SOLVENT. THE COMPOUNDS ARE USEFUL IN DEPOSITING METAL FILMS ON SUBSTRATE SURFACES.
(1) (R3P)3MB11H14
AND
(2) ((R3P)4AG)2B11H13
WHEREIN M IS EITHER COPPER OR GOLD AND EACH R IS PHENYL, (ARYL OR ALKARYL). THE COMPOUNDS ARE PREPARED BY REACTING A SALT OF B11H14- WITH A SALT OF THE METAL M IN THE PRESENCE OF THE PHOSPHINE AND IN INERT SOLVENT. THE COMPOUNDS ARE USEFUL IN DEPOSITING METAL FILMS ON SUBSTRATE SURFACES.
Description
United States Patent 27,467 COMPLEXES OF B H AND B H Frank K. Klanberg and George W. Parshall, by E. I. du Pont de Nemours and (10., assignee N0 Drawing. Original No. 3,455,977, dated July 15, 1969, Ser. No. 601,308, Dec. 13, 1966. Application for reissue Feb. 26, 1971, Ser. No. 119,423 Int. Cl. C07f 1/10, 1/12, 1/08 U.S. Cl. 260-430 4 Claims Matter enclosed in heavy brackets II] appears in the original patent but forms no part of this reissue specification; matter printed in italics indicates the additions made by reissue.
ABSTRACT OF THE DISCLOSURE Complexes selected from those represented by the formulas wherein M is either copper or gold and each R' is phenyl. [aryl or a1karyl.] The compotmds are prepared by reacting a salt of B H with a salt of the metal M. in the presence of the phosphine and an inert solvent. The compounds are useful in depositing metal films on substrate surfaces.
This invention relates to novel metal-organic compounds. More specifically, it concerns complexes of B ll or B iH with selected metals and phosphines, and to a method for their preparation.
The novel complexes of this invention are compounds selected from those represented by the formulas wherein M is a metal selected from the group consisting of copper and gold; and each R is [of 6-12 carbon atoms selected from the class consisting of aryl and alkaryL] phenyl.
The novel complexes of this invention are prepared by reacting a soluble polyboron salt of the formula MB H wherein M is alkali metal or R,,NH wherein n is a cardinal number of 0-4 inclusive and R is lower alkyl, with a soluble salt of the metal M in the presence of the phosphine, R P, and an inert medium.
The salt of the metal M can be represented by the formulas CuX AgX, AuX and M'AuX," wherein X is one equivalent of an anion selected from the class consisting of chloride, bromide, nitrate, sulfate, formate, acetate, lactate and tartrate; X is selected from the class consisting of acetate, nitrate and fluoride, and X" is selected from the class consisting of chloride and bromide.
For convenience, the process is usually carried out at room temperatures, e.g. 20-30" C., or slightly higher temperatures, e.g., up to 50 C. The latter range is sometimes useful for effecting increased dissolution of some of the reactants. The temperature range, however, is not critical and higher or lower temperatures may be used, but present no advantage.
The R groups in the cation R,,'NH.; can be the same or different and the cations are represented by tert-butylammonium, diisopropylammonium, triethylammonium, tetramethylammonium, and the like.
Pressure is not critical and solely for convenience, atmospheric pressure is ordinarily employed.
[Nor is the ratio of reactants critical] Usually, for
optimum results, approximately stoichiometric ratios are used. As seen in the examples, the order of addition of the reactants is not critical and they can be combined in any sequence or all mixed together simultaneously.
Operable solvents include water, polar organic solvents that are at least partially miscible with water, and mixtures of the two. Examples of such polar solvents include lower alkanols such as methanol, ethanol and isopropyl alcohol; cyclic ethers such as dioxane and tetrahydro furan; open-chain polyethers such as [1,2-dimethoxymethane] 1,2-dz'methoxyethane and di(2-ethoxyethyl) ether; and lower alkanenitriles such as acetonitrile and propionitrile.
All products of the invention are relatively insoluble in the reaction medium and usually precipitate immediately when all the reactants are in mutual contact. The product can then be isolated by filtration and purified by recrystallization as shown in the examples.
The reactants CsB Hw RbB l-l (CH NHB H and (C'H NHB H can be prepared as described in Aftanclilian et al., Inorg. Chem. 1, 736 (1962). Ammonium, other alkali-metal, and other substituted ammonium B 11 salts which make up the reactants in the process of this invention are prepared from the cesium or rubidium B H salt by conventional cation exchange techniques.
[Representative phosphines (R P), both as reactants and complexed ligand groups in the compounds of the invention, include triphenylphosphine, tritolylphosphine (0-, mand p-), tris(2,5-xylyl)phosphine, tris(2,4,6-trimethylphenyl) phosphine, phenyldi-p-tolylphosphine, diphenyl-p-tolylphosphine, tris(1-naphthyl)phosphine, tris- (biphenyl)phosphine, and the like] The novel complexes of this invention are crystalline solids. Their infrared absorption spectra indicate that the metal M is bonded directly to boron of the polyboron nucleus, and is not bonded to the hydrogen of the polyboron nucleus.
The products and process of this invention are illustrated in greater detail in the following examples:
A mixture of 7.8 g. of triphenylphosphine and 1.6 g. of copper sulfate in 180 ml. of ethanol and 50 ml. of water was stirred with a solution of 3 g. of CsB H in 70 ml. of a 1:1 by volume mixture of water and ethanol. A cream-co lored solid precipitate formed which was collected and taken up in ml. of tetrahydrofuran, with warming, to yield a yellow solution. Concentration of this solution gave 5.5 g. of a solid which was separated. The product was recrystallized three times from a 1:1 by volume mixture of benzene and 1,2-dimethoxyethane to give 1 g. of [(C H P] CuB H which decomposed between 205220 C.
Analysis.-Calcd. for C H B CuP C, 66.0; H, 6.1; B, 12.1; Cu, 6.5. Found: C, 65.1; H, 6.4; B, 12.3; Cu, 6.3.
The infrared absorption (KBr wafer) showed one B-d-I absorption band at 2550 cm.- (terminal hydrogen).
Examp s s)a ]s n 14 A solution of NaAuCl -2H O (3.3 g.) in 40 ml. of ethanol was added to a mixture of triphenylphosphine (6.5 g.) and CsB H (2.6 g.) in ml. of warm ethanol and 10 ml. of water. A solid precipitated. The solid was isolated by filtration and recrystallized three times from 1,2-dimethoxyethane. The final product consisted of white crystals of [(C H P] AuB H which yellowed at C. and decomposed at 217-218 C.
Analysis.Calcd. for C H AuB P C, 58.1; H, 5.3; P, 8.3; B, 10.7; An, 17.6. Found: C, 57.7; H, 5.7; P, 7.7; B, 10.2; An, 17.1.
The infrared absorption spectrum showed one B-H absorption band at 2515 cm.- (terminal hydrogen).
Solutions of 15 g. of triphenylphosphine in 150 ml. of :thanol and 2 g. of CsB H in 20 ml. of ethanol and 20 11. of water were combined, and the resulting mixture was added with stirring to a solution of 1.7 g. of silver iitrate in 10 ml. of ethanol and 10 ml. of water. A white olid precipitated. It was separated by filtration and disolved in 100 ml. of tetrahydrofuran. When this solution Ias chilled in ice, a crystalline solid precipitated. It was eparated by filtration and dried to give 3.6 g. of
he product decomposed at 180 C. after browning slightat 165-168 C.
Analysis.-Calcd. for C H ;,Ag B P C, 70.7; H, .5; Ag, 8.8; B, 4.9. Found: C, 68.8; H, 5.4; Ag, 8.2; i, 4.8.
he infrared absorption spectrum of the product (KBr rafer) showed one sharp band at 2550 cm.- (terminal .ydrogen).
An additional 4.0 g. of product was obtained when the iother liquor was concentrated to about one-half of its riginal volume. Its infrared absorption spectrum and ielting behavior were identical with those of the first frac- By employing the procedure set forth in the foregoing xamples, all the compounds of this invention can be preared.
The compounds of this invention are useful in the depsition of metal films on a substrate surface. For example,
glass vessel containing a solution of about 0.05 g. of
(C H P] AuB H in 5 ml. of dimethyl sulfoxide was varmed gently to about 100 C. A thin film of metallic ;old was deposited on the wall of the vessel that was in ontact with the solution.
The foregoing detailed description has been given for learness of understanding only and no unnecessary imitations are to be understood therefrom. The invention not limited to the exact details shown and described, or obvious modifications will occur to those skilled in he art.
The embodiments of the invention in which an exlusive property or privilege is claimed are defined as ollows:
, '4 1. Compounds represented by the formula selected from those of the class consisting of References Cited The following references, cited by the Examiner, are of record in the patented file of this patent or the original patent.
and
UNITED STATES PATENTS 3,217,023 11/1965 Miller 260430 X 3,296,260 3/1967 Knoth 260430 X 3,328,422 6/1967 Knoth 260430 X 3,418,346 12/1968 Parshall 260429 OTHER REFERENCES Cariati et al.: Gazz, Chim. Ital., vol. 95, pp. 3-5 (1965).
Davidson- Chem. & Ind., pp. 2021-22 (1964). Cariati et al.: Gazz, Chim. Ital., vol. 95, pp. 201-205 (1965).
TOBIAS E. LEVOW, Primary Examiner H. M. S. SNEED, Assistant Examiner US. Cl. X.R.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US11942371A | 1971-02-26 | 1971-02-26 |
Publications (1)
Publication Number | Publication Date |
---|---|
USRE27467E true USRE27467E (en) | 1972-09-05 |
Family
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Family Applications (1)
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US27467D Expired USRE27467E (en) | 1971-02-26 | 1971-02-26 | Complexes of |
Country Status (1)
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US (1) | USRE27467E (en) |
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1971
- 1971-02-26 US US27467D patent/USRE27467E/en not_active Expired
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