Synthesis and late transition metal complexes of the heterofunctional phosphane o-Ph2PNHC6H4P(S)Ph-2
The difunctional ligand o-Ph2PNHC6H4P(S)Ph-2 (PS) has been prepared by treatment of the lithium amide salt of 2-(diphenylthiophosphanyl) aniline {2-[Ph2P(S)]C6H4NH2} with Ph2PCl. The new ligand was oxidised to give the mixed chalcogen species Ph2P(E)NHC6H4P(S)Ph-2, by treatment with H2O2 (where E =...
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Published in | European journal of inorganic chemistry no. 9; pp. 2408 - 2418 |
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Main Authors | , , |
Format | Journal Article |
Language | English |
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Wiley
01.09.2002
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Abstract | The difunctional ligand o-Ph2PNHC6H4P(S)Ph-2 (PS) has been prepared by treatment of the lithium amide salt of 2-(diphenylthiophosphanyl) aniline {2-[Ph2P(S)]C6H4NH2} with Ph2PCl. The new ligand was oxidised to give the mixed chalcogen species Ph2P(E)NHC6H4P(S)Ph-2, by treatment with H2O2 (where E = O) or aerial oxidation by recrystallisation from MeOH, and by reaction with Se-8 (where E = Se) in warm toluene. The complexes [MCl(eta(3)-C3H5)(PS)] (M = Pt or Pd), CiS-[PtCl2(PS)(PMe2Ph)], [(AuCl)(PS)], CiS-[MCl2(PS)(2)] (M = Pt or Pd), cis-[PtMe2(PS)(2)] and trans-[PtMeCl(PS)(2)] have been synthesised by reaction of either [Pt(mu-Cl)(mu-eta(2):eta(1)-C3H5)](4), [Pd(mu-Cl)(eta(3)-C3H5)](2), [{PtCl(mu-Cl)(PMe2Ph)}(2)], [AuCl(tht)] (tht = tetrahydrothiophene), [PdCl2(cod)] or [PtX2(cod)] (X = Me or Cl; cod = cycloocta-1,5-diene) with (PS). In all these complexes the ligand (PS) is monodentate P-bound. Chloride abstraction from [MCl(eta(3)-C3H5)(PS)] (M = Pt or Pd), CiS-[PtCl2(PS)(PMe2Ph)], cis-[PtCl2(PS)(2)] and trans[PtMeCl(PS)(2)], using Ag[ClO4], gave the monocationic [M(eta(3)-C3H5)(PS)][ClO4] (M = Pt or Pd), cis-[PtCl(PS)(PMe2Ph)][ClO4], trans-[PtMe(PS)(2)] [ClO4] or dicationic [Pt(PS)(2)][ClO4](2) compounds in which the ligand (PS) is kappa(2)-P, S-bound. All compounds described here have been characterised by a combination of P-31{H-1} and H-1 NMR spectroscopy, microanalyses, FAB mass spectrometry and IR spectroscopy. The molecular structures of [AuCl(Ph2PNHC6H4P-(S)Ph-2-P)] in which there is an intramolecular hydrogen-onding interaction between the amine proton and the sulfur atom of the thiophosphoryl group and transt-[Pt(Ph2PNHC6H4P(S)Ph-2-kappa(2)-P,S)(2)][ClO4](2).CH2Cl2.2H(2)O in which the perchlorate counterions are associated by hydrogen-bonding interactions to the amine protons of the kappa(2)-P,S ligands have been determined by single-crystal X-ray diffraction. |
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AbstractList | The difunctional ligand o-Ph2PNHC6H4P(S)Ph-2 (PS) has been prepared by treatment of the lithium amide salt of 2-(diphenylthiophosphanyl) aniline {2-[Ph2P(S)]C6H4NH2} with Ph2PCl. The new ligand was oxidised to give the mixed chalcogen species Ph2P(E)NHC6H4P(S)Ph-2, by treatment with H2O2 (where E = O) or aerial oxidation by recrystallisation from MeOH, and by reaction with Se-8 (where E = Se) in warm toluene. The complexes [MCl(eta(3)-C3H5)(PS)] (M = Pt or Pd), CiS-[PtCl2(PS)(PMe2Ph)], [(AuCl)(PS)], CiS-[MCl2(PS)(2)] (M = Pt or Pd), cis-[PtMe2(PS)(2)] and trans-[PtMeCl(PS)(2)] have been synthesised by reaction of either [Pt(mu-Cl)(mu-eta(2):eta(1)-C3H5)](4), [Pd(mu-Cl)(eta(3)-C3H5)](2), [{PtCl(mu-Cl)(PMe2Ph)}(2)], [AuCl(tht)] (tht = tetrahydrothiophene), [PdCl2(cod)] or [PtX2(cod)] (X = Me or Cl; cod = cycloocta-1,5-diene) with (PS). In all these complexes the ligand (PS) is monodentate P-bound. Chloride abstraction from [MCl(eta(3)-C3H5)(PS)] (M = Pt or Pd), CiS-[PtCl2(PS)(PMe2Ph)], cis-[PtCl2(PS)(2)] and trans[PtMeCl(PS)(2)], using Ag[ClO4], gave the monocationic [M(eta(3)-C3H5)(PS)][ClO4] (M = Pt or Pd), cis-[PtCl(PS)(PMe2Ph)][ClO4], trans-[PtMe(PS)(2)] [ClO4] or dicationic [Pt(PS)(2)][ClO4](2) compounds in which the ligand (PS) is kappa(2)-P, S-bound. All compounds described here have been characterised by a combination of P-31{H-1} and H-1 NMR spectroscopy, microanalyses, FAB mass spectrometry and IR spectroscopy. The molecular structures of [AuCl(Ph2PNHC6H4P-(S)Ph-2-P)] in which there is an intramolecular hydrogen-onding interaction between the amine proton and the sulfur atom of the thiophosphoryl group and transt-[Pt(Ph2PNHC6H4P(S)Ph-2-kappa(2)-P,S)(2)][ClO4](2).CH2Cl2.2H(2)O in which the perchlorate counterions are associated by hydrogen-bonding interactions to the amine protons of the kappa(2)-P,S ligands have been determined by single-crystal X-ray diffraction. |
Author | Aucott, SM Slawin, AMZ Woollins, JD |
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Keywords | COORDINATION CHEMISTRY PLATINUM(II) COMPLEXES MOLECULAR-STRUCTURE chelate complexes NUCLEAR-MAGNETIC-RESONANCE phosphorus-sulfur ligands ORGANOMETALLIC COMPLEXES TRIDENTATE LIGAND monodentate complexes BONDING PROPERTIES SULFUR PALLADIUM(II) |
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DIAMAGNETIC NICKEL(2) COMPLEXES WITH POLYDENTATE PHOSPHINES CONTAINING SULFUR AND SELENIUM DONOR ATOMS publication-title: INORGANIC CHEMISTRY contributor: fullname: WORKMAN, MO – volume: 98 start-page: 6521 year: 1976 ident: WOS:A1976CG22700018 article-title: THERMAL-DECOMPOSITION OF BIS(PHOSPHINE)PLATINUM(II) METALLOCYCLES publication-title: JOURNAL OF THE AMERICAN CHEMICAL SOCIETY contributor: fullname: MCDERMOTT, JX – volume: 20 start-page: 2516 year: 1981 ident: WOS:A1981LZ96700029 article-title: UNSYMMETRICAL BISPHOSPHORUS LIGANDS .14. MULTI-NUCLEAR MAGNETIC-RESONANCE STUDIES OF GROUP-6 METAL-CARBONYL-COMPLEXES OF UNSYMMETRICAL BISPHOSPHORUS LIGANDS publication-title: INORGANIC CHEMISTRY contributor: fullname: COLQUHOUN, IJ – volume: 95 start-page: 1102 year: 1973 ident: WOS:A1973O920600018 article-title: MECHANISM OF TERTIARY PHOSPHINE CATALYZED ISOMERIZATION OF TETRAGONAL PLANAR PLATINUM(II) COMPLEXES publication-title: JOURNAL OF THE AMERICAN CHEMICAL SOCIETY contributor: fullname: COOPER, DG – volume: 475 start-page: 116 year: 1981 ident: WOS:A1981LQ21700012 article-title: ON THE COORDINATION CHEMISTRY OF PHOSPHINES AND PHOSPHINOXIDES .30. NICKEL, PALLADIUM, AND PLATINUM COMPLEXES OF PRIMARY MERCAPTOALKYLPHOSPHINES publication-title: ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE contributor: fullname: ISSLEIB, K – volume: 19 start-page: 3195 year: 1980 ident: WOS:A1980KK17200079 article-title: UNSYMMETRICAL BIS-PHOSPHORUS LIGANDS .13. BIS(TERT-BUTYLPHOSPHINO)(DIPHENYLPHOSPHINO)METHANE AND SOME DERIVATIVES publication-title: INORGANIC CHEMISTRY contributor: fullname: GRIM, SO – volume: 31 start-page: 1406 year: 1992 ident: WOS:A1992HP28800021 article-title: RESOLUTIONS INVOLVING METAL COMPLEXATION - OPTICAL RESOLUTION AND PHOTOCHEMICAL-REARRANGEMENT OF (+/-)-(2-MERCAPTOETHYL)METHYLPHENYLPHOSPHINE publication-title: INORGANIC CHEMISTRY contributor: fullname: LEUNG, PH – volume: 312 start-page: 67 year: 1986 ident: WOS:A1986E069200008 article-title: PHOSPHINE-SUBSTITUTED CHELATE LIGANDS .21. REVERSIBLE SUBSTITUTION OF TETRACARBONYL(PHOSPHINOTHIOFORMAMID)-COMPLEXES, (CO)4M(PS) (M=CR, MO, W), WITH TRIORGANOPHOSPHINES, TRIORGANOARSINES AND TRIORGANOSTIBINES publication-title: JOURNAL OF ORGANOMETALLIC CHEMISTRY contributor: fullname: KUNZE, U – volume: 467 start-page: 85 year: 1994 ident: WOS:A1994MY33300012 article-title: SOME TRANSITION-METAL COMPLEXES OF PH2P(CH2)NP(O)PH2 (N=1, 2) AND PH2P(CH2)P(S)PH2 publication-title: JOURNAL OF ORGANOMETALLIC CHEMISTRY contributor: fullname: BLAGBOROUGH, TC |
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Snippet | The difunctional ligand o-Ph2PNHC6H4P(S)Ph-2 (PS) has been prepared by treatment of the lithium amide salt of 2-(diphenylthiophosphanyl) aniline... |
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SubjectTerms | Chemistry Chemistry, Inorganic & Nuclear Physical Sciences Science & Technology |
Title | Synthesis and late transition metal complexes of the heterofunctional phosphane o-Ph2PNHC6H4P(S)Ph-2 |
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