作者:Q. Wang、P. V. Gushchin、N. A. Bokach、M. Haukka、V. Yu. Kukushkin
DOI:10.1007/s11172-012-0115-5
日期:2012.4
The replacement of the iodide ligands in the complex [PtI2(dpa)] (1) (dpa is 2,2′-dipyridylamine) by silver triflate in acetonitrile afforded the compound [Pt(dpa)(MeCN)2](SO3CF3)2 (2). Homoleptic complexes [Pt(dpa)2](X)2 (3·(X)2) were synthesized by the treatment of [PtI2(dpa)] (1) with 2,2′-dipyridylamine in the presence of silver salts AgX in methanol (X = NO3) or acetonitrile (X = SO3CF3). The deprotonation of the complex [3](SO3CF3)2 to give the homoleptic complex [Pt(dpa-H)2] (4) was performed by two methods, e.g., by the treatment of [3](SO3CF3)2 with 2 equiv. of NaOH in methanol or by the addition of excess Et3N to a suspension of [3](SO3CF3)2 in methanol. The structures of compounds 1–4 were established by elemental analyses, high resolution electrospray ionization mass spectrometry, IR and NMR spectroscopy; the crystal structure of complexes [2](SO3CF3)2, [3](NO3)2·H2O, [3](SO3CF3)2·2H2O, and 4 were determined by single-crystal X-ray diffraction.
在乙腈中用三酸银取代[PtI2(dpa)](1)复合物(dpa 是 2,2′-二吡啶基胺)中的碘配体,得到了[Pt(dpa)(MeCN)2](SO3CF3)2 (2)。在甲醇(X = NO3)或乙腈(X = SO3CF3)中,在银盐 AgX 的存在下,用 2,2′-二吡啶胺处理[PtI2(dpa)](1),合成了均质配合物[Pt(dpa)2](X)2 (3-(X)2)。复合物[3](SO3CF3)2 的去质子化得到同质复合物[Pt(dpa-H)2](4)的方法有两种,例如在甲醇中用 2 等量的 NaOH 处理[3](SO3CF3)2,或在甲醇中向[3](SO3CF3)2 的悬浮液中加入过量 Et3N。化合物 1-4 的结构是通过元素分析、高分辨率电喷雾电离质谱、红外光谱和核磁共振光谱确定的;复合物 [2](SO3CF3)2、[3](NO3)2-H2O、[3](SO3CF3)2-2H2O 和 4 的晶体结构是通过单晶 X 射线衍射确定的。