Institut für Anorganische Chemie, Universität zu Köln, Greinstrasse 6, D-50939, Köln, Germany.
Dalton Trans. 2010 Dec 28;39(48):11577-86. doi: 10.1039/c0dt00866d. Epub 2010 Nov 4.
Deprotonation of the N-thiophosphorylated thioureas RC(S)NHP(S)(OiPr)(2) (R = Me(2)N, HL(I); iPrNH, HL(II); 2,6-Me(2)C(6)H(3)NH, HL(III), 2,4,6-Me(3)C(6)H(2)NH, HL(IV), aza-15-crown-5, HL(V)) and reaction with CuI or Cu(NO(3))(2) in aqueous EtOH leads to the polynuclear complexes [Cu(4)(L(I)-S,S')(4)], [Cu(8)(L(II)-S,S')(8)], and [Cu(3)(L(III-V)-S,S')(3)]. The structures of these compounds were investigated by IR, (1)H, (31)P{(1)H} NMR, UV-vis spectroscopy and elemental analyses. The crystal structures of [Cu(4)L(I)(4)], [Cu(8)L(II)(8)], [Cu(3)L(III,IV)(3)] were determined by single-crystal X-ray diffraction. Reaction of the deprotonated ligands (L(I-V))(-) with a mixture of CuI and 1,10-phenanthroline (phen) or PPh(3) leads to the mixed-ligand mononuclear complexes [Cu(phen)L(I-V)], [Cu(PPh(3))L(I-V)] or [Cu(PPh(3))(2)L(I-V)]. The same mixed-ligand complexes were obtained from the reaction of [Cu(4)L(I)(4)], [Cu(8)L(II)(8)], [Cu(3)L(III-V)(3)] with phen or PPh(3).
脱质子化的 N-硫代膦酰基硫脲 RC(S)NHP(S)(OiPr)(2)(R = Me(2)N,HL(I);iPrNH,HL(II);2,6-Me(2)C(6)H(3)NH,HL(III),2,4,6-Me(3)C(6)H(2)NH,HL(IV),氮杂-15-冠-5,HL(V))与 CuI 或 Cu(NO(3))(2)在水-乙醇中反应,生成多核配合物 [Cu(4)(L(I)-S,S')(4)]、[Cu(8)(L(II)-S,S')(8)]和[Cu(3)(L(III-V)-S,S')(3)]。这些化合物的结构通过红外光谱、(1)H、(31)P{(1)H}NMR、UV-vis 光谱和元素分析进行了研究。[Cu(4)L(I)(4)]、[Cu(8)L(II)(8)]、[Cu(3)L(III,IV)(3)]的晶体结构通过单晶 X 射线衍射确定。脱质子化配体(L(I-V))(-)与 CuI 和 1,10-邻菲啰啉(phen)或 PPh(3)的混合物反应,生成单核配合物[Cu(phen)L(I-V)]、[Cu(PPh(3))L(I-V)]或[Cu(PPh(3))(2)L(I-V)]。同样的混合配体配合物也可以通过[Cu(4)L(I)(4)]、[Cu(8)L(II)(8)]、[Cu(3)L(III-V)(3)]与 phen 或 PPh(3)的反应得到。