NDLI: Synthesis and Structure of Amido- and Imido(pentafluorophenyl)borane Zirconocene and Hafnocene Complexes: NH and BH Activation

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Synthesis and Structure of Amido- and Imido(pentafluorophenyl)borane Zirconocene and Hafnocene Complexes: NH and BH Activation

Content Provider	World Health Organization (WHO)-Global Index Medicus
Author	Jones, Garth A. Tizzard, Graham J. Fuller, Anna Lancaster, Simon J. Jacobs, Elizabeth A. Coles, Simon J. Wright, Joseph A.
Description	Author Affiliation: Jacobs EA ( Energy Materials Laboratory, School of Chemistry, University of East Anglia, Norwich Research Park, Norwich, NR4 7TJ, UK.)
Abstract	Treatment of $Me_{2}S⋅B(C_{6}F_{5})_{n}H_{3−n}$ (n=1 or 2) with ammonia yields the corresponding adducts. $H_{3}N⋅B(C_{6}F_{5})H_{2}$ dimerises in the solid state through NH⋅⋅⋅HB dihydrogen interactions. The adducts can be deprotonated to give lithium amidoboranes $Li[NH_{2}B(C_{6}F_{5})_{n}H_{3−n}].$ Reaction of the n=2 reagent with $[Cp_{2}ZrCl_{2}]$ leads to disubstitution, but $[Cp_{2}Zr\{NH_{2}B(C_{6}F_{5})_{2}H\}_{2}]$ is in equilibrium with the product of β-hydride elimination $[Cp_{2}Zr(H)\{NH_{2}B(C_{6}F_{5})_{2}H\}],$ which proves to be the major isolated solid. The analogous reaction with $[Cp_{2}HfCl_{2}]$ gives a mixture of $[Cp_{2}Hf\{NH_{2}B(C_{6}F_{5})_{2}H\}_{2}]$ and the NH activation product $[Cp_{2}Hf\{NHB(C_{6}F_{5})_{2}H\}].$ $[Cp_{2}Zr\{NH_{2}B(C_{6}F_{5})_{2}H\}_{2}]⋅PhMe$ and $[Cp_{2}Hf\{NH_{2}B(C_{6}F_{5})_{2}H\}_{2}]⋅4(thf)$ exhibit β-B-agostic chelate bonding of one of the two amidoborane ligands in the solid state. The agostic hydride is invariably coordinated to the outside of the metallocene wedge. Exceptionally, $[Cp_{2}Hf\{NH_{2}B(C_{6}F_{5})_{2}H\}_{2}]⋅PhMe$ has a structure in which the two amidoborane ligands adopt an intermediate coordination mode, in which neither is definitively agostic. $[Cp_{2}Hf\{NHB(C_{6}F_{5})_{2}H\}]$ has a formally dianionic imidoborane ligand chelating through an agostic interaction, but the bond-length distribution suggests a contribution from a zwitterionic amidoborane resonance structure. Treatment of the zwitterions $[Cp_{2}MMe(μ-Me)B(C_{6}F_{5})_{3}]$ (M=Zr, Hf) with $Li[NH_{2}B(C_{6}F_{5})_{n}H_{3−n}]$ (n=2) results in $[Cp_{2}MMe\{NH_{2}B(C_{6}F_{5})_{2}H\}]$ complexes, for which the spectroscopic data, particularly $^{1}J(B,H),$ again suggest β-B-agostic interactions. The reactions proceed similarly for the structurally encumbered $[Cp′′_{2}ZrMe(μ-Me)B(C_{6}F_{5})_{3}]$ precursor $(Cp′′=1,3-C_{5}H_{3}(SiMe_{3})_{2},$ n=1 or 2) to give $[Cp′′_{2}ZrMe\{NH_{2}B(C_{6}F_{5})_{n}H_{3−n}\}],$ both of which have been structurally characterised and show chelating, agostic amidoborane coordination. In contrast, the analogous hafnium chemistry leads to the recovery of $[Cp′′_{2}HfMe_{2}]$ and the formation of $Li[HB(C_{6}F_{5})_{3}]$ through hydride abstraction.
ISSN	09476539
e-ISSN	15213765
Journal	Chemistry - A European Journal
Issue Number	28
Volume Number	18
Language	English
Publisher	Wiley-VCH;ChemPubSoc Europe
Publisher Date	2012-07-09
Publisher Place	Germany
Access Restriction	Open
Subject Keyword	Chemistry
Content Type	Text
Resource Type	Article
Subject	Organic Chemistry Catalysis

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