Dias H V Rasika, Alidori Simone, Lobbia Giancarlo Gioia, Papini Grazia, Pellei Maura, Santini Carlo
Department of Chemistry and Biochemistry, Box 19065, The University of Texas at Arlington, Arlington, Texas 76019-0065, USA.
Inorg Chem. 2007 Nov 12;46(23):9708-14. doi: 10.1021/ic701041k. Epub 2007 Oct 9.
The first 5-substituted trihydro(azolyl)borate system, the sodium trihydro(5-CF3-pyrazol-1-yl)borate, Na[H3B(5-(CF3)pz)], has been synthesized by the reaction of 3-trifuoromethyl-pyrazole with NaBH4 in high yield. Na[H3B(5-(CF3)pz)] reacts with AgNO3 in the presence of monodentate tertiary phosphanes PR3 (PR3=P(C6H5)3, P(p-C6H4CH3)3, P(m-C6H4CH3)3, P(o-C6H4CH3)3, or PCH3(C6H5)2) to afford silver(I) bis(phosphane) adducts. These compounds have been characterized by elemental analyses, FTIR, ESI-MS, and multinuclear (1H, 19F, and 31P) NMR spectroscopy. Solid-state structures of {[H3B(5-(CF3)pz)]Ag[P(C6H5)3]2} and {[H3B(5-(CF3)pz)]Ag[P(p-C6H4CH3)3]2} are also reported. They feature kappa2-N,H-bonded trihydro(pyrazolyl)borate ligands and pseudo-tetrahedral silver atoms.
首个5-取代三氢（唑基）硼酸盐体系，即三氢（5-三氟甲基-吡唑-1-基）硼酸钠，Na[H3B(5-(CF3)pz)]，已通过3-三氟甲基-吡唑与硼氢化钠反应以高产率合成。Na[H3B(5-(CF3)pz)]在单齿叔膦PR3（PR3 = 三苯基膦、对甲基三苯基膦、间甲基三苯基膦、邻甲基三苯基膦或甲基二苯基膦）存在下与硝酸银反应，得到银（I）双（膦）加合物。这些化合物已通过元素分析、傅里叶变换红外光谱、电喷雾电离质谱和多核（1H、19F和31P）核磁共振光谱进行了表征。还报道了{[H3B(5-(CF3)pz)]Ag[P(C6H5)3]2}和{[H3B(5-(CF3)pz)]Ag[P(p-C6H4CH3)3]2}的固态结构。它们具有κ2-N，H键合的三氢（吡唑基）硼酸盐配体和伪四面体银原子。
Zotero 插件