Synthesis and X-ray and Neutron Structures of Zr{(-H)2BC8H14}4
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- 作者：Errun Ding ; Bin Du ; Edward A. Meyers ; Sheldon G. Shore ; Muhammed Yousufuddin ; Robert Bau ; and Garry J. McIntyre
- 刊名：Inorganic Chemistry
- 出版年：2005
- 出版时间：April 4, 2005
- 年：2005
- 卷：44
- 期：7
- 页码：2459 - 2464
- 全文大小：122K
- 年卷期：v.44,no.7(April 4, 2005)
- ISSN：1520-510X
文摘
The complex Zr(9-BBN)4 [9-BBN = (
-H)2BC8H14] has been synthesized via the reaction of K(9-BBN) with ZrCl4in diethyl ether. The structure of the title compound has been determined by X-ray and neutron single-crystaldiffraction techniques. Each 9-BBN ligand is coordinated to the Zr atom via two B-H-Zr bridges, and these metal-ligand bonding interactions are further augmented by three prominent C-H···Zr agostic interactions. Average molecularparameters derived from the neutron analysis: Zr-H = 2.051(8) Å, B-H = 1.286(7) Å, Zr···B = 2.409(6) Å,Zr-H-B = 87.7(4)
, H-Zr-H = 58.9(3). The Zr···H distances corresponding to the three C-H···Zr agosticinteractions are 2.424(7), 2.663(8), and 2.551(7) Å. The fourth potential C-H···Zr interaction has a Zr···H distance[3.146(7) Å] that is too long to be considered in the agostic range. Single-crystal X-ray diffraction data were collectedon an Enraf-Nonius Kappa CCD diffraction system, and neutron diffraction data were collected on the quasi-Lauediffractometer VIVALDI at the Institut Laue-Langevin; the final agreement factor for the neutron analysis is 6.52%for 2557 reflections with I > 2
(I).
-H)2BC8H14] has been synthesized via the reaction of K(9-BBN) with ZrCl4in diethyl ether. The structure of the title compound has been determined by X-ray and neutron single-crystaldiffraction techniques. Each 9-BBN ligand is coordinated to the Zr atom via two B-H-Zr bridges, and these metal-ligand bonding interactions are further augmented by three prominent C-H···Zr agostic interactions. Average molecularparameters derived from the neutron analysis: Zr-H = 2.051(8) Å, B-H = 1.286(7) Å, Zr···B = 2.409(6) Å,Zr-H-B = 87.7(4), H-Zr-H = 58.9(3). The Zr···H distances corresponding to the three C-H···Zr agosticinteractions are 2.424(7), 2.663(8), and 2.551(7) Å. The fourth potential C-H···Zr interaction has a Zr···H distance[3.146(7) Å] that is too long to be considered in the agostic range. Single-crystal X-ray diffraction data were collectedon an Enraf-Nonius Kappa CCD diffraction system, and neutron diffraction data were collected on the quasi-Lauediffractometer VIVALDI at the Institut Laue-Langevin; the final agreement factor for the neutron analysis is 6.52%for 2557 reflections with I > 2(I).