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Organometallic Zirconium Compounds in an Oxygen-Rich Coordination Environment: Synthesis and Structural Characterization of Tris(oxoimidazolyl)hydroboratozirconium Compounds
Inorganic Chemistry ( IF 4.3 ) Pub Date : 2018-01-09 00:00:00 , DOI: 10.1021/acs.inorgchem.7b02832 Ahmed Al-Harbi 1 , Matthew J. Hammond 1 , Gerard Parkin 1
Inorganic Chemistry ( IF 4.3 ) Pub Date : 2018-01-09 00:00:00 , DOI: 10.1021/acs.inorgchem.7b02832 Ahmed Al-Harbi 1 , Matthew J. Hammond 1 , Gerard Parkin 1
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A series of tris(oxoimidazolyl)hydroborato ligands, which serve as L2X [O3] donors, have been employed to obtain organometallic zirconium compounds in an uncommon oxygen-rich coordination environment. For example, Cp[ToMeBenz]ZrCl2 has been synthesized via the reaction of [ToMeBenz]Na with CpZrCl3 and bears a structural resemblance to the bent metallocene dichloride derivative Cp2ZrCl2. In addition, the half-sandwich counterparts [ToMeBenz]ZrCl3 and [ToBut]ZrCl3 have been obtained by metathesis of ZrCl4 with [ToMeBenz]Na and [ToBut]Na, respectively. The structurally related zirconium benzyl compounds [ToRBenz]Zr(CH2Ph)3 (R = Me, But, 1-Ad) have also been synthesized via the reactions of [ToRBenz]Tl with Zr(CH2Ph)4, and X-ray diffraction studies demonstrate that the benzyl ligands in these compounds are conformationally flexible and exhibit a large range of Zr–CH2–Ph bond angles (94.7–131.7°). Protolytic cleavage of one of the benzyl ligands of [ToRBenz]Zr(CH2Ph)3 (R = But, 1-Ad) may be achieved by treatment with [PhNHMe2][B(C6F5)4] to generate {[ToRBenz]Zr(CH2Ph)2}[B(C6F5)4], which are catalysts for the polymerization of ethylene. The molecular structure of the ether adduct, {[ToButBenz]Zr(CH2Ph)2(OEt2)}[B(C6F5)4], has been determined by X-ray diffraction. In addition to the use of tris(oxoimidazolyl)hydroborato ligands, bis(oxoimidazolyl)hydroborato ligands have also been used to obtain zirconium benzyl compounds in oxygen-rich environments, namely, [BoMeBenz]2Zr(CH2Ph)2 and [BoAdBenz]2Zr(CH2Ph)2.
中文翻译：
富氧配位环境中的有机金属锆化合物：三（氧代咪唑基）氢硼酸锆化合物的合成与结构表征
用作L 2 X [O 3 ]供体的一系列三（氧代咪唑基）氢硼酸盐配体已用于在罕见的富氧配位环境中获得有机金属锆化合物。例如，通过[To MeBenz ] Na与CpZrCl 3的反应已经合成了Cp [ ToMeBenz ] ZrCl 2，并且其结构类似于弯曲的茂金属二氯化物衍生物Cp 2 ZrCl 2。另外，通过ZrCl 4的复分解获得了半三明治的[To MeBenz ] ZrCl 3和[To Bu t ] ZrCl 3。分别使用[To MeBenz ] Na和[To Bu t ] Na。与结构相关的苄基锆化合物[To RBenz ] Zr（CH 2 Ph）3（R = Me，Bu t，1-Ad）也已经通过[To RBenz ] Tl与Zr（CH 2 Ph）4的反应合成。和X射线衍射研究表明，这些化合物中的苄基配体具有构象柔性，并表现出大范围的Zr–CH 2 –Ph键角（94.7–131.7°）。[To RBenz ] Zr（CH 2 Ph）3（R = Bu t）的苄基配体之一的蛋白水解裂解，1-Ad）可以通过用[PhNHMe 2 ] [B（C 6 F 5）4 ]处理以生成{[To RBenz ] Zr（CH 2 Ph）2 } [B（C 6 F 5）4 ]来实现。 ，它们是乙烯聚合的催化剂。醚加合物的分子结构，{[为了卜吨奔驰]的Zr（CH 2 PH）2（OET 2）} [B（C 6 ˚F 5）4通过X射线衍射测定。除了使用三（氧代咪唑基）氢硼酸盐配体之外，双（氧代咪唑基）氢硼酸盐配体也已用于在富氧环境中获得[苄基] [ Z ]苯并[ 2 ] Zr（CH 2 Ph）2和[[ Bo AdBenz ] 2 Zr（CH 2 Ph）2。
更新日期：2018-01-09
中文翻译：
富氧配位环境中的有机金属锆化合物：三（氧代咪唑基）氢硼酸锆化合物的合成与结构表征
用作L 2 X [O 3 ]供体的一系列三（氧代咪唑基）氢硼酸盐配体已用于在罕见的富氧配位环境中获得有机金属锆化合物。例如，通过[To MeBenz ] Na与CpZrCl 3的反应已经合成了Cp [ ToMeBenz ] ZrCl 2，并且其结构类似于弯曲的茂金属二氯化物衍生物Cp 2 ZrCl 2。另外，通过ZrCl 4的复分解获得了半三明治的[To MeBenz ] ZrCl 3和[To Bu t ] ZrCl 3。分别使用[To MeBenz ] Na和[To Bu t ] Na。与结构相关的苄基锆化合物[To RBenz ] Zr（CH 2 Ph）3（R = Me，Bu t，1-Ad）也已经通过[To RBenz ] Tl与Zr（CH 2 Ph）4的反应合成。和X射线衍射研究表明，这些化合物中的苄基配体具有构象柔性，并表现出大范围的Zr–CH 2 –Ph键角（94.7–131.7°）。[To RBenz ] Zr（CH 2 Ph）3（R = Bu t）的苄基配体之一的蛋白水解裂解，1-Ad）可以通过用[PhNHMe 2 ] [B（C 6 F 5）4 ]处理以生成{[To RBenz ] Zr（CH 2 Ph）2 } [B（C 6 F 5）4 ]来实现。 ，它们是乙烯聚合的催化剂。醚加合物的分子结构，{[为了卜吨奔驰]的Zr（CH 2 PH）2（OET 2）} [B（C 6 ˚F 5）4通过X射线衍射测定。除了使用三（氧代咪唑基）氢硼酸盐配体之外，双（氧代咪唑基）氢硼酸盐配体也已用于在富氧环境中获得[苄基] [ Z ]苯并[ 2 ] Zr（CH 2 Ph）2和[[ Bo AdBenz ] 2 Zr（CH 2 Ph）2。
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