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Aspects of the Inorganic Chemistry of Rubber Vulcanisation. Part 4. Dialkyl- and Diaryl-dithiophosphate and -dithiophosphinate Complexes of Zinc: Phosphorus-31 Nuclear Magnetic Resonance Spectral Studies and Structures of 4>2P(OC6H4Me-p)2)3> and 4>2PPh2

DOI: 10.1039/DT9830000627

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 627 - 634 (1983)

Update date:2022-08-05

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Authors:

McCleverty, Jon A.McCleverty, Jon A.

Kowalski, Rick S. Z.Kowalski, Rick S. Z.

Bailey, Neil A.Bailey, Neil A.

Mulvaney, RobertMulvaney, Robert

O'Cleirigh, Donal A.O'Cleirigh, Donal A.

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Article abstract of DOI:10.1039/DT9830000627

The complexes 4>2P(OC6H4Me-p)2)3> and 4>2PPh2)3> have been prepared by treatment of 2PR2)2> with (NR'4>2PR2> (R=OC6H4Me-p or Ph, R'=Me or Et).Preparation of 2(S2P(OPri)2)>- and 2PR2)2(S2CNMe2)>- (R=OC6H4Me-p or Ph) is also described.From reactions of 2P(OR)2)2> (R=Pri or C6H4Me-p) with H2O2 or ButO(OH), zinc phosphates and ZnSO4 have been obtained, and 2P(OPh)2)2> and 2P(OPh)2)3>- react with ROH (R=Et or Pri) in solution to give amongst other products 2P(OR)2)2> and 2P(OR)2>- with loss of phenol.The 31P n.m.r. spectra of a series of dialkyl- and diaryl-dithiophosphate and -phosphinate complexes have been recorded and used to establish rapid exchange within the equilibrium 2P(OR)2)3>- <*> 2P(OR)2)2> + 2P(OR)2>-.The structures of the title compounds have been determined crystallographically: 4>2P(OC6H4Me-p)2)3> is monoclinic with a=29.311(9), b=11.032(3), c=17.515(5) Angstroem, β=106.83(2) deg, space group P21/a, Z=4, and 2490 reflections give R 0.0532; 4>2PPh2)3> is monoclinic with a=11.160(6), b=9.962(5), c=43.11(3) Angstroem, β=104.73(5) deg, space group P21/c, Z=4, and 3304 reflections give R 0.0411.Both have slightly distorted tetrahedral geometries in which one S2PR2 ligand is bidentate, and the other two are unidentate.

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Product name:(Zn(S2P(OC6H4Me-p)2)2)

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