Synthesis and characterization of oxorhenium(V)-'3+1' mixed thiolate [SNS]/[S] and [ONS]/[S] complexes. Crystal and molecular structures of [ReO(eta (3)-SCH2C5H3NCH2S)(eta(1)-C6H4Br-4-S)], [ReO(eta(3)-SCH2C5H3NCH2O)(eta(1)-C6H4X-4-S)] (X = Cl, OMe),

摘要

The reaction of [ReOCl3(Ph-3)(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(eta(3)-SCH2C5H3NCH2S)(eta(1)-C5H4NH-2-S)][Cl] (22). Crystal data for 10, C13H11BrNOS3Re: triclinic, P1, a = 7.2909(5), b = 14.1978(9), c = 15.991(1) Angstrom, alpha = 77.184(1), beta = 86.588(1), gamma = 75.507(1)degrees, V = 1562.69(18) Angstrom(3), Z = 4. For 16, C13H11ClNO2S2Re: orthorhombic, P2(1)2(1)2(1), a = 6.9728(6), b = 13.477(1), c = 15.761(1) Angstrom, V = 1481.1(2) Angstrom(3), Z = 4. For 18, C14H14NO3S2Re: monoclinic, P2(1)/c, a = 15.6512(14), b = 7.6678(7), c = 13.732(1) Angstrom, beta = 112.489(1)degrees, V = 1522.7(2) Angstrom(3), Z = 4. For 21, C15H16NO3S2Re: monoclinic, P2(1)/c, a = 13.929(1), b = 7.741(1), c = 15.583(2) Angstrom, beta = 103.600(2)degrees, V = 1633.1(3) Angstrom(3), Z = 4. For 22, C12H11ClN2OS3Re: monoclinic, C2(1)/c, a = 27.827(3), b = 8.529(1), c = 14.957(2) Angstrom, beta = 119.314(2)degrees, V = 3095.3(6) Angstrom(3), Z = 8, (C) 2000 Elsevier Science S.A. All rights reserved. [References: 43]