Synthesis and Characterization of Rhenium Phosphinothiolate Complexes. Crystal and Molecular Structures of [HNEt3][Re{P(C6H4S)3}2], ReOCl{OP(C6H5)2(C6H 4S)}{P(C6H5)2(C6H 4S)}

Paulo Perez-Lourido; J. Romero; J. Garcia-Vazquez; Antonio Sousa; Kevin P. Maresca; David J. Rose; Jon Zubieta

doi:10.1021/ic9715299

Synthesis and Characterization of Rhenium Phosphinothiolate Complexes. Crystal and Molecular Structures of [HNEt₃][Re{P(C₆H₄S)₃}₂], ReOCl{OP(C₆H₅)₂(C₆H ₄S)}{P(C₆H₅)₂(C₆H ₄S)}

Paulo Perez-Lourido, J. Romero, J. Garcia-Vazquez, Antonio Sousa, Kevin P. Maresca, David J. Rose, Jon Zubieta

Department of Chemistry

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Abstract

The reactions of ammonium perrhenate, HCl(aq), and the phosphinothiol ligands (2-HSC₆H₄)P(C₆H₄X)₂, where X = H or SH [abbreviated P-(SH),_x (x = 1, 3)], in alcohol have led to the isolation of a series of rhenium complexes containing the {M(P-S_x)₂} core, represented by [Re{P(C₆H₄S)₃}{P(C₆H ₄S)₂(C₆H₄SH)}] (1), [ReOCl{OP(C₆H₅)₂(C₆H ₄S)}{P(C₆H₅)₂(C₆H ₄S)}] (3), and [ReOCl{OP(C₆H₅)₂(2-SC₆H ₃-3-SiMe₃)}₂] (5). The reaction of 1 with NEt₃ results in the formation of [HNEt₃][Re{P(C₆H₄S)₃}₂] (2) by deprotonation of a thiol ligand. The reaction of ammonium perrhenate with P-(SH) also led to the isolation of the binuclear species [ReOCl{OP- (C₆H₅)₂(2-SC₆H ₃-3-SiMe₃)}₂] (4). Crystal data: 2, C₄₃H₄₂NP₂S₆Cl₂Re, monoclinic, P2₁/c, a = 14.2484(2) Å, b = 15.3108(1) Å, c = 19.5121(2) Å, β= 90.366(1)°, V = 4256.56(8) Å³, Z = 2, 26 410 reflections, R = 0.0605; 3, C₃₆H₂₈O₂P₂S ₂ClRe,triclinic, P1̄, a = 9.3427(1) Å, b = 11.9075(1) Å, c = 16.8504(1) Å, α = 98.177(1)°, β= 104.132(1)°, y = 109.000(1)°, V = 1667.79(2) Å³, Z = 2, 7567 reflections, R = 0.0333; 4, C₃₆H₂₈O₅P₂S₂Re ₂, monoclinic, P2₁/n, a = 10.6714(1) Å, b = 24.0076(2) Å, c = 13.3610(1) Å, β= 93.65(1)°, V = 3416.51(4) Å³, Z = 4, 8073 reflections, R = 0.0469; 5, C₄₄H₄₇NO₃Si₂P₂S ₂ClRe, triclinic, P1̄, a = 10.1616(2) Å, b = 14.7095(3) Å, c = 17.0744(3) Å, α = 89.108(1)°, β= 83.634(1)°, γ = 70.901(1)°, V = 2396.21(8) Å³, Z = 2, 6175 reflections, R = 0.0837.

Original language	English (US)
Pages (from-to)	3331-3336
Number of pages	6
Journal	Inorganic Chemistry
Volume	37
Issue number	13
DOIs	https://doi.org/10.1021/ic9715299
State	Published - 1998

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Physical and Theoretical Chemistry
Inorganic Chemistry

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10.1021/ic9715299

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@article{0e9e854c219b4a3b91e473e7e89db4d5,

title = "Synthesis and Characterization of Rhenium Phosphinothiolate Complexes. Crystal and Molecular Structures of [HNEt3][Re{P(C6H4S)3}2], ReOCl{OP(C6H5)2(C6H 4S)}{P(C6H5)2(C6H 4S)}",

abstract = "The reactions of ammonium perrhenate, HCl(aq), and the phosphinothiol ligands (2-HSC6H4)P(C6H4X)2, where X = H or SH [abbreviated P-(SH),x (x = 1, 3)], in alcohol have led to the isolation of a series of rhenium complexes containing the {M(P-Sx)2} core, represented by [Re{P(C6H4S)3}{P(C6H 4S)2(C6H4SH)}] (1), [ReOCl{OP(C6H5)2(C6H 4S)}{P(C6H5)2(C6H 4S)}] (3), and [ReOCl{OP(C6H5)2(2-SC6H 3-3-SiMe3)}2] (5). The reaction of 1 with NEt3 results in the formation of [HNEt3][Re{P(C6H4S)3}2] (2) by deprotonation of a thiol ligand. The reaction of ammonium perrhenate with P-(SH) also led to the isolation of the binuclear species [ReOCl{OP- (C6H5)2(2-SC6H 3-3-SiMe3)}2] (4). Crystal data: 2, C43H42NP2S6Cl2Re, monoclinic, P21/c, a = 14.2484(2) {\AA}, b = 15.3108(1) {\AA}, c = 19.5121(2) {\AA}, β= 90.366(1)°, V = 4256.56(8) {\AA}3, Z = 2, 26 410 reflections, R = 0.0605; 3, C36H28O2P2S 2ClRe,triclinic, P{\=1}, a = 9.3427(1) {\AA}, b = 11.9075(1) {\AA}, c = 16.8504(1) {\AA}, α = 98.177(1)°, β= 104.132(1)°, y = 109.000(1)°, V = 1667.79(2) {\AA}3, Z = 2, 7567 reflections, R = 0.0333; 4, C36H28O5P2S2Re 2, monoclinic, P21/n, a = 10.6714(1) {\AA}, b = 24.0076(2) {\AA}, c = 13.3610(1) {\AA}, β= 93.65(1)°, V = 3416.51(4) {\AA}3, Z = 4, 8073 reflections, R = 0.0469; 5, C44H47NO3Si2P2S 2ClRe, triclinic, P{\=1}, a = 10.1616(2) {\AA}, b = 14.7095(3) {\AA}, c = 17.0744(3) {\AA}, α = 89.108(1)°, β= 83.634(1)°, γ = 70.901(1)°, V = 2396.21(8) {\AA}3, Z = 2, 6175 reflections, R = 0.0837.",

author = "Paulo Perez-Lourido and J. Romero and J. Garcia-Vazquez and Antonio Sousa and Maresca, {Kevin P.} and Rose, {David J.} and Jon Zubieta",

year = "1998",

doi = "10.1021/ic9715299",

language = "English (US)",

volume = "37",

pages = "3331--3336",

journal = "Inorganic Chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "13",

}

TY - JOUR

T1 - Synthesis and Characterization of Rhenium Phosphinothiolate Complexes. Crystal and Molecular Structures of [HNEt3][Re{P(C6H4S)3}2], ReOCl{OP(C6H5)2(C6H 4S)}{P(C6H5)2(C6H 4S)}

AU - Perez-Lourido, Paulo

AU - Romero, J.

AU - Garcia-Vazquez, J.

AU - Sousa, Antonio

AU - Maresca, Kevin P.

AU - Rose, David J.

AU - Zubieta, Jon

PY - 1998

Y1 - 1998

N2 - The reactions of ammonium perrhenate, HCl(aq), and the phosphinothiol ligands (2-HSC6H4)P(C6H4X)2, where X = H or SH [abbreviated P-(SH),x (x = 1, 3)], in alcohol have led to the isolation of a series of rhenium complexes containing the {M(P-Sx)2} core, represented by [Re{P(C6H4S)3}{P(C6H 4S)2(C6H4SH)}] (1), [ReOCl{OP(C6H5)2(C6H 4S)}{P(C6H5)2(C6H 4S)}] (3), and [ReOCl{OP(C6H5)2(2-SC6H 3-3-SiMe3)}2] (5). The reaction of 1 with NEt3 results in the formation of [HNEt3][Re{P(C6H4S)3}2] (2) by deprotonation of a thiol ligand. The reaction of ammonium perrhenate with P-(SH) also led to the isolation of the binuclear species [ReOCl{OP- (C6H5)2(2-SC6H 3-3-SiMe3)}2] (4). Crystal data: 2, C43H42NP2S6Cl2Re, monoclinic, P21/c, a = 14.2484(2) Å, b = 15.3108(1) Å, c = 19.5121(2) Å, β= 90.366(1)°, V = 4256.56(8) Å3, Z = 2, 26 410 reflections, R = 0.0605; 3, C36H28O2P2S 2ClRe,triclinic, P1̄, a = 9.3427(1) Å, b = 11.9075(1) Å, c = 16.8504(1) Å, α = 98.177(1)°, β= 104.132(1)°, y = 109.000(1)°, V = 1667.79(2) Å3, Z = 2, 7567 reflections, R = 0.0333; 4, C36H28O5P2S2Re 2, monoclinic, P21/n, a = 10.6714(1) Å, b = 24.0076(2) Å, c = 13.3610(1) Å, β= 93.65(1)°, V = 3416.51(4) Å3, Z = 4, 8073 reflections, R = 0.0469; 5, C44H47NO3Si2P2S 2ClRe, triclinic, P1̄, a = 10.1616(2) Å, b = 14.7095(3) Å, c = 17.0744(3) Å, α = 89.108(1)°, β= 83.634(1)°, γ = 70.901(1)°, V = 2396.21(8) Å3, Z = 2, 6175 reflections, R = 0.0837.

AB - The reactions of ammonium perrhenate, HCl(aq), and the phosphinothiol ligands (2-HSC6H4)P(C6H4X)2, where X = H or SH [abbreviated P-(SH),x (x = 1, 3)], in alcohol have led to the isolation of a series of rhenium complexes containing the {M(P-Sx)2} core, represented by [Re{P(C6H4S)3}{P(C6H 4S)2(C6H4SH)}] (1), [ReOCl{OP(C6H5)2(C6H 4S)}{P(C6H5)2(C6H 4S)}] (3), and [ReOCl{OP(C6H5)2(2-SC6H 3-3-SiMe3)}2] (5). The reaction of 1 with NEt3 results in the formation of [HNEt3][Re{P(C6H4S)3}2] (2) by deprotonation of a thiol ligand. The reaction of ammonium perrhenate with P-(SH) also led to the isolation of the binuclear species [ReOCl{OP- (C6H5)2(2-SC6H 3-3-SiMe3)}2] (4). Crystal data: 2, C43H42NP2S6Cl2Re, monoclinic, P21/c, a = 14.2484(2) Å, b = 15.3108(1) Å, c = 19.5121(2) Å, β= 90.366(1)°, V = 4256.56(8) Å3, Z = 2, 26 410 reflections, R = 0.0605; 3, C36H28O2P2S 2ClRe,triclinic, P1̄, a = 9.3427(1) Å, b = 11.9075(1) Å, c = 16.8504(1) Å, α = 98.177(1)°, β= 104.132(1)°, y = 109.000(1)°, V = 1667.79(2) Å3, Z = 2, 7567 reflections, R = 0.0333; 4, C36H28O5P2S2Re 2, monoclinic, P21/n, a = 10.6714(1) Å, b = 24.0076(2) Å, c = 13.3610(1) Å, β= 93.65(1)°, V = 3416.51(4) Å3, Z = 4, 8073 reflections, R = 0.0469; 5, C44H47NO3Si2P2S 2ClRe, triclinic, P1̄, a = 10.1616(2) Å, b = 14.7095(3) Å, c = 17.0744(3) Å, α = 89.108(1)°, β= 83.634(1)°, γ = 70.901(1)°, V = 2396.21(8) Å3, Z = 2, 6175 reflections, R = 0.0837.

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U2 - 10.1021/ic9715299

DO - 10.1021/ic9715299

M3 - Article

AN - SCOPUS:0000164783

SN - 0020-1669

VL - 37

SP - 3331

EP - 3336

JO - Inorganic Chemistry

JF - Inorganic Chemistry

IS - 13

ER -

Synthesis and Characterization of Rhenium Phosphinothiolate Complexes. Crystal and Molecular Structures of [HNEt₃][Re{P(C₆H₄S)₃}₂], ReOCl{OP(C₆H₅)₂(C₆H ₄S)}{P(C₆H₅)₂(C₆H ₄S)}

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