TITLE

Synthesis, spectroscopic characterization, and structural studies of new Cu(I) and Cu(II) complexes containing organophosphorus ligands, and crystal structures of (Ph[sub 3] P)[sub 2] Cu[S[sub 2] PMe[sub 2] ], (Ph[sub 3] P)[sub 2] Cu[(OPPh[sub 2] )[sub 2] N], Cu[(OPPh[sub 2] )[sub 2] N][sub 2] , and Cu[(OPPh[sub 2] )(SPPh[sub 2] )N][sub 2]

AUTHOR(S)
Silvestru, Anca; Rotar, Adina; Drake, John E; Hursthouse, Michael B; Light, Mark E; Farcas, Sorin I; Rösler, Roland; Silvestru, Cristian
PUB. DATE
May 2001
SOURCE
Canadian Journal of Chemistry;May2001, Vol. 79 Issue 5/6, p983
SOURCE TYPE
Academic Journal
DOC. TYPE
Article
ABSTRACT
The Cu(I) complexes, (Ph[sub 3] P)[sub 2] CuL (L = [S[sub 2] PMe[sub 2] ][sup -] , [OSPR[sub 2] ][sup -] (R = Me, Ph), [(XPR[sub 2] )(YPR'[sub 2] )N][sup -] (X, Y, R, R' = O, O, Ph, Ph; O, S, Ph, Ph; O, S, OEt, Ph; S, S, Me, Me)) and Cu(II) complexes, CuL[sub 2] (L = [(XPR[sub 2] )(YPR'[sub 2] )N][sup -] (X, Y, R, R' = O, O, Ph, Ph; O, S, Ph, Ph)), have been prepared. The Cu(I) derivatives were characterized by multinuclear NMR spectroscopy and in two cases by X-ray crystallography. (Ph[sub 3] P)[sub 2] Cu[S[sub 2] PMe[sub 2] ] (1) crystallizes in the orthorhombic space group P2[sub 1] 2[sub 1] 2[sub 1] (No. 19) with cell parameters a = 9.782(2), b = 17.808(4), c = 20.216(4) Å, V = 3521(6) Å[sup 3] and Z = 4, and (Ph[sub 3] P)[sub 2] Cu[(OPPh[sub 2] )[sub 2] N] (4) in the triclinic space group P (No. 2) with cell parameters a = 9.8079(2), b = 12.9141(3), c = 22.5666(5) Å, α = 75.714(2), β = 79.465(2), γ = 68.2770(8)°, V = 2559.9(1) Å[sup 3] and Z = 2. In both cases the phosphorus ligands are bidentate, thus resulting in monomeric molecules that contain tetrahedral CuP[sub 2] S[sub 2] and CuP[sub 2] O[sub 2] cores. The molecular structures of two of the Cu(II) derivatives were also determined. Cu[(OPPh[sub 2] )[sub 2] N][sub 2] (8) and Cu[(OPPh[sub 2] )(SPPh[sub 2] )N][sub 2] (9) crystallize in the triclinic space group P (No. 2) with cell parameters a = 8.887(2), b = 10.739(2), c = 12.477(3) Å, α = 77.61(3), β = 76.15(5), γ = 79.46(3)°, V = 1118.3(4) Å[sup 3] and Z = 1 for 8, and a = 9.626(2), b = 14.151(3), c = 24.752(5) Å, α = 88.23(3), β = 79.93(3), γ = 89.77(3)°, V = 3181(1) Å[sup 3] and Z = 3 for 9. The molecule of Cu[(OPPh[sub 2] )[sub 2] N][sub 2] (8) has a planar CuO[sub 4] core, while in Cu[(OPPh[sub 2] )(SPPh[sub 2] )N][sub 2] (9) both planar and tetrahedral copper cores are observed in a ratio of 1:2.Key words: structure, copper, thiophosphinates, oxo- and thio-imidodiphosphinatesOn a préparé les complexes suivants du Cu(I), (Ph[sub 3] P)[sub 2] CuL (L = [S[sub 2] PMe[sub 2] ][sup -] , [OSPR[sub 2] ][sup -] (R = Me, Ph), [(XPR[sub 2] )(YPR'[sub 2] )N][sup -] (X, Y, R, R' = O, O, Ph, Ph; O, S, Ph, Ph; O, S, OEt, Ph; S, S, Me, Me)) et du Cu(II), CuL[sub 2] (L = [(XPR[sub 2] )(YPR'[sub 2] )N][sup -] (X, Y, R, R' = O, O, Ph, Ph; O, S, Ph, Ph)). On a caractérisé les dérivés du Cu(I) par spectroscopie RMN multinucléaire et, dans deux cas, par diffraction des rayons X. Les cristaux de (Ph[sub 3] P)[sub 2] Cu[S[sub 2] PMe[sub 2] ] (1) sont orthorhombiques, groupe d'espace P2[sub 1] 2[sub 1] 2[sub 1] (No. 19) avec a = 9,782(2), b = 17,808(4) et c = 20,216(4) Å, V = 3521(6) Å[sup 3] et Z = 4; ceux du (Ph[sub 3] P)[sub 3] Cu[OPPh[sub 2] )[sub 2] N] (4) sont tricliniques, groupe d'espace P (No. 2) avec a = 9,08079(2), b = 12,9141(3) et c = 22,5666(5) Å, α = 75,714(2), β = 79,465(2) et γ = 68,2770(8)°, V = 2559,9(1) Å[sup 3] et Z = 2. Dans les deux cas, les ligands phosphorés sont bidentates ce qui conduit à des molécules monomères qui comportent des unités centrales CP[sub 2] S[sub 2] et CP[sub 2] O[sub 2] tétraédriques. On a aussi déterminé les structures moléculaires de deux des dérivés du Cu(II). Les cristaux de Cu[(OPPh[sub 2] )[sub 2] N][sub 2] (8) et de Cu[(OPPh[sub 2] )(SPPh[sub 2] )N][sub 2] (9) sont tous les deux tricliniques, groupe d'espace P (No. 2) avec a = 8,887(2), b = 10,739(3) et c = 12,477(3) Å, α = 77,61(3), β = 76,15(5) et γ = 79,46(3)°, V = 1118,3(1) Å[sup 3] et Z = 1, pour le composé 8, et avec a = 9,626(2), b = 14,151(3) et c = 24,752(5) Å, α = 88,23(3), β = 79,93(3) et γ = 89,77(3)°, V = 3181(1) Å[sup 3] et Z = 3, pour le composé 9. La molécule de Cu[(OPPh[sub 2] )[sub 2] N][sub 2] (8) comporte une unité centrale de CuO[sub 4] qui est plane alors que dans la molécule de Cu[(OPPh[sub 2] )(SPPh[sub 2] )N][sub 2] (9), on observe la présence d'unités de cuivre planes et tétraédriques dans un rapport de 1:2.Mots clés : structure, cuivre, thiophosphinates, oxo- et thio-imidodiphosphinates.[Traduit par la Rédaction]
ACCESSION #
10580647

 

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