Novel approach to the synthesis of ring systems containing phosphorus, nitrogen and sulfur or selenium

Solid-state C P W A S 'P NMR spectra were measured for the following unsaturated phosphorusnitroge-ulfur ring systems: l,S-R,P,N,S, (R = Me, Et, Ph), l,S-Ph,P,N,S,Ph,, Ph,PN,S,NPPh, and Ph,PN,S,. The ¡so-tropic solid-state shifts correlate well with the corresponding shifts in solution, the largest difference being 9.0 ppm, indicating that there are no phase-dependent structural features. Analysis of the principal elements of the shielding tensor by the spinning side band method showed that one of these elements is primarily responsible for the anomalousiy iow-field isotropic chernical shifts of 1,5-R,P,N,Sz , but no correlation was found between this individual tensor component and any of the structural parameters of these folded eight-membered rings. Two isotropic shifts were observed for the crystallographically inequivalent phosphorus atoms of 1,5-Et,PZN,S2 , hut the individual 31P isotropic shifts of 1,s-Me,P,N,S2 were not resolved.

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“…(2), 6 Ph,PN,S, (3)5 and Ph,PN,S,NPPh, (4). 12 The identity and purity of the products were established by 'P NMR spectroscopy.…”

Section: Methodsmentioning

confidence: 99%

Solid‐state ³¹P NMR investigations of unsaturated phosphorus–nitrogen–sulfur rings

Chivers

Edwards

Fyfe

et al. 1992

Magnetic Reson in Chemistry

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“…4 (3) C( 22) 0.187 (1) 0.6217 (9) 0.016 (1) 6.8 (3) C( 23) 0.151 (1) 0.562 (1) -0.0383 (9) 7. 6 (3) C( 24) 0.203 (1) 0.4411 (9) -0.0164 (8) 7.0 (3)…”

Section: Table IV Positional and Isotropic Equivalent Displacementunclassified

New halogen-bridged dinuclear edge-sharing and face-sharing bioctahedral tungsten(III) complexes, W2X6(PR3)n, where X = Cl or Br, PR3 = PMe3, PMe2Ph, PBu3, and n = 4 or 3: crystal structures of W2Cl6(PMe2Ph)4, W2Cl6(PMe2Ph)3 and W2Br6(PMe2Ph)3

Cotton¹,

Mandal²

1992

Inorg. Chem.

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“…The S,St-and Se,Sel-diorgano derivatives of these eightmembered rings, 3 and 4, are readily prepared (9,10). The P2N4E2 ring in 3 and 4 adopts a chair conformation with the two chalcogen atoms disposed on either side of the P2N4 plane and the exocyclic substituents on S or Se occupying axial positions (9,10).…”

Section: Introductionmentioning

confidence: 99%

“…The P2N4E2 ring in 3 and 4 adopts a chair conformation with the two chalcogen atoms disposed on either side of the P2N4 plane and the exocyclic substituents on S or Se occupying axial positions (9,10). These ring systems are potential precursors of hybrid inorganic polymers containing alternating PN and EN (E = S, Se) units.…”

Section: Introductionmentioning

confidence: 99%

“…The compounds 1 ,5-Ph4P,N4Se2R2 (R = Me, Et, Ph) (9), Ph4P,N3SPh (13), and [PtCl,(PEt,)], (14) were prepared by the literature procedures. The compound 1 ,5-Ph4P2N4S,Ph, was obtained in 59% yield from Ph,PN2(SiMe3), and three molar equivalents of PhSCl by a modification of the literature method (10) in which acetonitrile was used as a solvent instead of CH,Cl,. The solubility of the Ph2SZ by-product in acetonitrile facilitates the purification of the product by obviating the need to wash it with n-pentane.…”

Section: Introductionmentioning

confidence: 99%

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Preparation and nuclear magnetic resonance characterization of N-bonded complexes of platinum(II) with phosphorus-nitrogen rings containing three-coordinate chalcogens: X-ray structure of [PtCl₂(PEt₃)]₂(Ph₄P₂N₄Se₂Et₂)

Chivers¹,

Doxsee²,

Hilts³

et al. 1993

Can. J. Chem.

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The reaction of 1,s-Ph,P2N,S2Ph2 with [PtC12(PEt3)], in chloroform at 60°C produces the 1: 1 adduct transPtC1,(PEt3)(PbP2N,S2Ph2) in which the platinum is attached to a nitrogen atom on the basis of 3 1~ nmr spectroscopy. By contrast, the corresponding reactions of 13-Ph,P2N4Se,R, (R = Me, Et, Ph) produce the 2: 1 adducts [PtCl2(PEt3)I2(Ph4P2N4Se2R2) (7a, R = Me; 7b, R = Et; 7c, R = Ph) which have been characterized by 'H, 3 1~ and 77Se nrnr spectroscopy an$, in the case of 76, by X-ray crystallography. Crystals of 7b are monoclinic, space group C2/c, with a = 27.803(7) A, b = 12.378(7) A, c = 15.752(8) A, P = 115.49(2)", V = 4893(3) A~, and Z = 4. The leastsquares refinement with anisotropic thermal parameters for all non-hydrogen atoms converged at R = 0.037 and R, = 0.022. The platinum centres in 7b are attached to distal nitrogen atoms of the disordered P,N,Se2 ring. The reaction of the six-membered ring PbP2N3SPh with [PtC12(PEt3)], in dichloromethane at 23'C occurs in a regiospecific manner to give the 1 : 1 adduct PtC1,(PEt3)(PbP,N3SPh) in which, on the basis of "P nmr spectroscopy, the platinum is coordinated to a nitrogen atom between phosphorus and sulfur.

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Novel approach to the synthesis of ring systems containing phosphorus, nitrogen and sulfur or selenium

Cited by 12 publications

References 1 publication

Solid‐state ³¹P NMR investigations of unsaturated phosphorus–nitrogen–sulfur rings

Solid‐state ³¹P NMR investigations of unsaturated phosphorus–nitrogen–sulfur rings

New halogen-bridged dinuclear edge-sharing and face-sharing bioctahedral tungsten(III) complexes, W2X6(PR3)n, where X = Cl or Br, PR3 = PMe3, PMe2Ph, PBu3, and n = 4 or 3: crystal structures of W2Cl6(PMe2Ph)4, W2Cl6(PMe2Ph)3 and W2Br6(PMe2Ph)3

Preparation and nuclear magnetic resonance characterization of N-bonded complexes of platinum(II) with phosphorus-nitrogen rings containing three-coordinate chalcogens: X-ray structure of [PtCl₂(PEt₃)]₂(Ph₄P₂N₄Se₂Et₂)

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Novel approach to the synthesis of ring systems containing phosphorus, nitrogen and sulfur or selenium

Cited by 12 publications

References 1 publication

Solid‐state 31P NMR investigations of unsaturated phosphorus–nitrogen–sulfur rings

Solid‐state 31P NMR investigations of unsaturated phosphorus–nitrogen–sulfur rings

New halogen-bridged dinuclear edge-sharing and face-sharing bioctahedral tungsten(III) complexes, W2X6(PR3)n, where X = Cl or Br, PR3 = PMe3, PMe2Ph, PBu3, and n = 4 or 3: crystal structures of W2Cl6(PMe2Ph)4, W2Cl6(PMe2Ph)3 and W2Br6(PMe2Ph)3

Preparation and nuclear magnetic resonance characterization of N-bonded complexes of platinum(II) with phosphorus-nitrogen rings containing three-coordinate chalcogens: X-ray structure of [PtCl2(PEt3)]2(Ph4P2N4Se2Et2)

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Solid‐state ³¹P NMR investigations of unsaturated phosphorus–nitrogen–sulfur rings

Solid‐state ³¹P NMR investigations of unsaturated phosphorus–nitrogen–sulfur rings

Preparation and nuclear magnetic resonance characterization of N-bonded complexes of platinum(II) with phosphorus-nitrogen rings containing three-coordinate chalcogens: X-ray structure of [PtCl₂(PEt₃)]₂(Ph₄P₂N₄Se₂Et₂)