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2
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3
A five-coordinate phosphino/acetate iron(II) scaffold that binds N2, N2H2, N2H4, and NH3 in the sixth site.一个五配位的膦/乙酸根铁(II)支架，可在第六位结合 N2、N2H2、N2H4 和 NH3。
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4
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单核五配位和六配位铁腙基和肼基物种。

Mononuclear five- and six-coordinate iron hydrazido and hydrazine species.

机构信息

Division of Chemistry and Chemical Engineering, California Institute of Technology, Pasadena, California 91125, USA.

出版信息

Inorg Chem. 2012 Sep 17;51(18):10043-54. doi: 10.1021/ic301704f. Epub 2012 Sep 5.

DOI:10.1021/ic301704f
PMID:22950847
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC4167049/
Abstract

This article describes the synthesis and characterization of several low-spin iron(II) complexes that coordinate hydrazine (N(2)H(4)), hydrazido (N(2)H(3)(-)), and ammonia. The sterically encumbered tris(di-meta-terphenylphosphino)borate ligand, PhBP(mter)(3), is introduced to provide access to species that cannot be stabilized with the PhBP(Ph)(3) ligand (PhBP(R)(3) = PhB(CH(2)PR(2))(3)(-)). Treatment of [PhBP(mter)(3)]FeMe with hydrazine generates the unusual 5-coordinate hydrazido complex [PhBP(mter)(3)]Fe(η(2)-N(2)H(3)) (1), in which the hydrazido serves as an L(2)X-type ligand. Upon coordination of an L-type ligand, the hydrazido shifts to an LX-type ligand, generating [PhBP(mter)(3)]Fe(L)(η(2)-N(2)H(3)) (L = N(2)H(4) (2) or NH(3) (3)). In contrast, treatment of [PhBP(Ph)(3)]FeMe with hydrazine forms the adduct [PhBP(Ph)(3)]Fe(Me)(η(2)-N(2)H(4)) (5). Complex 5 is thermally unstable to methane loss, generating intermediate [PhBP(Ph)(3)]Fe(η(2)-N(2)H(3)), which undergoes bimolecular coupling to produce {[PhBP(Ph)(3)]Fe}(2)(μ-η(1):η(1)-N(2)H(4))(μ-η(2):η(2)-N(2)H(2)). The oxidation of these and related hydrazine and hydrazido species is also presented. For example, oxidation of 1 or 5 with Pb(OAc)(4) results in disproportionation of the N(2)H(x) ligand (x = 3, 4), and formation of [PhBP(R)(3)]Fe(NH(3))(OAc) (R = Ph (9) and mter (11)).

摘要

本文描述了几种低自旋铁(II)配合物的合成和表征，这些配合物与肼（N(2)H(4)）、叠氮化物（N(2)H(3)(-)）和氨配位。引入位阻较大的三（二-间-三联苯膦基）硼酸盐配体[PhBP(mter)(3)]-，以提供无法用[PhBP(Ph)(3)]-稳定的物种。[PhBP(mter)(3)]FeMe 与肼反应生成不寻常的 5 配位叠氮化物配合物[PhBP(mter)(3)]Fe(η(2)-N(2)H(3))（1），其中叠氮化物充当 L(2)X 型配体。当配位一个 L 型配体时，叠氮化物迁移到 LX 型配体，生成[PhBP(mter)(3)]Fe(L)(η(2)-N(2)H(3))（L = N(2)H(4)（2）或 NH(3)（3））。相比之下，[PhBP(Ph)(3)]FeMe 与肼反应生成加合物[PhBP(Ph)(3)]Fe(Me)(η(2)-N(2)H(4))（5）。5 对甲烷失去不稳定，生成中间产物[PhBP(Ph)(3)]Fe(η(2)-N(2)H(3))，它经历双分子偶联，生成{[PhBP(Ph)(3)]Fe}(2)(μ-η(1)：η(1)-N(2)H(4))(μ-η(2)：η(2)-N(2)H(2))。还介绍了这些和相关的肼和叠氮化物物种的氧化。例如，用 Pb(OAc)(4)氧化 1 或 5 导致 N(2)H(x)配体（x = 3，4）的歧化，生成[PhBP(R)(3)]Fe(NH(3))(OAc)（R = Ph（9）和 mter（11））。