一种二价铕单（螯合配体）配合物和一种空间位阻较大的吡唑硼烷的形成与结构表征
Formation and structural characterization of a europium(II) mono(scorpionate) complex and a sterically crowded pyraza-bole.
作者信息
Liebing Phil, Kühling Marcel, Takats Josef, Hilfert Liane, Edelmann Frank T
机构信息
ETH Zürich, Laboratorium für Anorganische Chemie, Vladimir-Prelog-Weg 2, 8093 Zürich, Switzerland.
Chemisches Institut der Otto-von-Guericke-Universität Magdeburg, Universitätsplatz 2, 39106 Magdeburg, Germany.
出版信息
Acta Crystallogr E Crystallogr Commun. 2017 Nov 21;73(Pt 12):1921-1925. doi: 10.1107/S2056989017016498. eCollection 2017 Dec 1.
The reaction of EuI(THF) with potassium hydro-tris-(3,5-diiso-propyl-pyrazol-yl)borate (K[HB(3,5- pz)] (= KTp , pz = pyrazol-yl) in a molar ratio of 1:1.5 resulted in extensive ligand fragmentation and formation of the europium(II) mono(scorpionate) complex bis-(3,5-diisopropyl-1-pyrazole)[hydro-tris-(3,5-diiso-propyl-pyrazol-yl)borato]iodido-europium(II), [Eu(CHBN)I(CHN)] or (Tp )(3,5- pzH)EuI, , in high yield (78%). As a typical by-product, small amounts of the sterically crowded pyraza-bole derivative -4,8-bis-(3,5-diiso-propyl-pyrazol-1-yl)-1,3,5,7-tetra-iso-propyl-pyraza-bole, CHBH or -{(3,5- pz)HB(μ-3,5- pz)}, , were formed. Both title compounds have been structurally characterized through single-crystal X-ray diffraction. In , two isopropyl groups are each disordered over two orientations with occupancy ratios of 0.574 (10):0.426 (10) and 0.719 (16):0.281 (16). In , one isopropyl group is similarly disordered, occupancy ratio 0.649 (9):0.351 (9).
碘化铕（II）（四氢呋喃）与氢化三（3,5-二异丙基吡唑基）硼酸钾（K[HB(3,5-pz)]，即KTp，pz = 吡唑基）以1:1.5的摩尔比反应，导致大量配体断裂，并形成了高产率（78%）的铕（II）单（螯合配体）配合物双（3,5-二异丙基-1-吡唑）[氢化三（3,5-二异丙基吡唑基）硼酸盐]碘铕（II），[Eu(CHBN)I(CHN)]或(Tp)(3,5-pzH)EuI。作为典型的副产物，生成了少量空间位阻较大的吡唑硼烷衍生物-4,8-双（3,5-二异丙基吡唑-1-基）-1,3,5,7-四异丙基吡唑硼烷，CHBH或-{(3,5-pz)HB(μ-3,5-pz)}。两种标题化合物均通过单晶X射线衍射进行了结构表征。在[Eu(CHBN)I(CHN)]中，两个异丙基各自在两个取向上无序，占有率分别为0.574 (10):0.426 (10)和0.719 (16):0.281 (16)。在(Tp)(3,5-pzH)EuI中，一个异丙基同样无序，占有率为0.649 (9):0.351 (9)。
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