TY - JOUR
T1 - Synthesis and characterization of oxorhenium(V)-'3 + 1' mixed thiolate [SNS]/[S] and [ONS]/[S] complexes
AU - Chen, Xiaoyuan
AU - Femia, Frank J.
AU - Babich, John W.
AU - Zubieta, Jon
N1 - Funding Information:
This work was supported by a grant from the Department of Energy (DOE), Office of Health and Environmental Research D2-FG02-99ER62791.
PY - 2000/9/11
Y1 - 2000/9/11
N2 - The reaction of [ReOCl3(PPh3)2] with the tridentate ligands 2,6-dithiomethylpyridine (4) or 6-thiomethyl-2-pyridinemethanol (5) and the appropriate monothiols, such as para-substituted benzenethiols (C6H4X-4-SH) (where X = F, Cl, Br and OCH3) and para-substituted benzylmercaptans (C6H4X-4-CH2SH) (where X = F, Cl and OCH3) in the presence of Et3N leads to the isolation of a series of integrated '3 + 1' oxorhenium(V) complexes. Similarly, reaction of [ReOCl3(PPh3)2] with 2-mercaptopyridine and 4 afforded a cationic oxorhenium(V) complex, [ReO(η3-SCH2C5H3NCH2S)(η1-C5H4NH-2-S)][Cl] (22). Crystal data for 10. C13H11BrNOS3Re: triclinic, P1, a = 7.2909(5), b = 14.1978(9), c = 15.991(1) Å, α = 77.184(1), β = 86.588(1), γ = 75.507(1)°, V = 1562.69(18) Å3, Z = 4. For 16, C13H11ClNO2S2Re: orthorhombic, P212121, a = 6.9728(6), b = 13.477(1), c = 15.761(1) Å, V = 1481.1(2) Å3, Z = 4. For 18, C14H14NO3S2Re: monoclinic, P21/c, a = 15.6512(14), b = 7.6678(7), c = 13.732(1) Å, β = 112.489(1)°, V = 1522.7(2) Å3, Z = 4. For 21, C15H16NO3S2Re: monoclinic, P21/c, a = 13.929(1), b = 7.741(1), c = 15.583(2) Å, β = 103.600(2)°, V = 1633.1(3) Å3, Z = 4. For 22, C12H11ClN2OS3Re: monoclinic, C21/c, a = 27.827(3), b = 8.529(1), c = 14.957(2) Å, β = 119.314(2)°, V = 3095.3(6) Å3, Z = 8. (C) 2000 Elsevier Science S.A.
AB - The reaction of [ReOCl3(PPh3)2] with the tridentate ligands 2,6-dithiomethylpyridine (4) or 6-thiomethyl-2-pyridinemethanol (5) and the appropriate monothiols, such as para-substituted benzenethiols (C6H4X-4-SH) (where X = F, Cl, Br and OCH3) and para-substituted benzylmercaptans (C6H4X-4-CH2SH) (where X = F, Cl and OCH3) in the presence of Et3N leads to the isolation of a series of integrated '3 + 1' oxorhenium(V) complexes. Similarly, reaction of [ReOCl3(PPh3)2] with 2-mercaptopyridine and 4 afforded a cationic oxorhenium(V) complex, [ReO(η3-SCH2C5H3NCH2S)(η1-C5H4NH-2-S)][Cl] (22). Crystal data for 10. C13H11BrNOS3Re: triclinic, P1, a = 7.2909(5), b = 14.1978(9), c = 15.991(1) Å, α = 77.184(1), β = 86.588(1), γ = 75.507(1)°, V = 1562.69(18) Å3, Z = 4. For 16, C13H11ClNO2S2Re: orthorhombic, P212121, a = 6.9728(6), b = 13.477(1), c = 15.761(1) Å, V = 1481.1(2) Å3, Z = 4. For 18, C14H14NO3S2Re: monoclinic, P21/c, a = 15.6512(14), b = 7.6678(7), c = 13.732(1) Å, β = 112.489(1)°, V = 1522.7(2) Å3, Z = 4. For 21, C15H16NO3S2Re: monoclinic, P21/c, a = 13.929(1), b = 7.741(1), c = 15.583(2) Å, β = 103.600(2)°, V = 1633.1(3) Å3, Z = 4. For 22, C12H11ClN2OS3Re: monoclinic, C21/c, a = 27.827(3), b = 8.529(1), c = 14.957(2) Å, β = 119.314(2)°, V = 3095.3(6) Å3, Z = 8. (C) 2000 Elsevier Science S.A.
KW - Crystal structures
KW - Mixed thiolate complexes
KW - Oxorhenium complexes
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U2 - 10.1016/S0020-1693(00)00209-7
DO - 10.1016/S0020-1693(00)00209-7
M3 - Article
AN - SCOPUS:0034637860
SN - 0020-1693
VL - 307
SP - 88
EP - 96
JO - Inorganica Chimica Acta
JF - Inorganica Chimica Acta
IS - 1-2
ER -