Synthesis and characterization of pentaphosphino zero-valent iron complexes and their corresponding iron(II)-chloride and -hydride complexes

Kristen A. Thoreson; Angela D. Follett; Kristopher McNeill

doi:10.1021/ic1003325

Synthesis and characterization of pentaphosphino zero-valent iron complexes and their corresponding iron(II)-chloride and -hydride complexes

Kristen A. Thoreson
, Angela D. Follett
, Kristopher McNeill

Research output: Contribution to journal › Article › peer-review

14 Scopus citations

Abstract

A pentaphosphino iron(II)-chloride species [^tSiP ₃(dmpm)FeCl][Cl] (1-Cl) (^tSiP₃ = ^tBuSi(CH₂PMe₂)₃, dmpm = Me ₂PCH₂PMe₂) was prepared from [( ^tSiP₃Fe)₂(μ-Cl)₃][Cl] and dmpm. This species was reduced to give the corresponding iron(0) complex, ^tSiP₃(dmpm)Fe (3), in near quantitative yield. Analogous complexes [SiP₃(dmpe)FeCl][Cl] (2-Cl) and SiP₃(dmpe)Fe (4) (SiP₃ = MeSi(CH₂PMe₂)₃, dmpe = Me₂PCH₂CH₂PMe₂) were prepared in the same manner as 1 and 3 but with lower yields because of competitive ligand rearrangement reactions that gave byproduct of trans-(dmpe)₂FeCl ₂ and (dmpe)₅Fe₂ (5). [^tSiP ₃(dmpm)FeH][A] (6) was prepared from the reaction of 3 with weak acids (HA), and the pK_a of 6 was established to be approximately 25. Attempts to prepare pentaphosphino-iron(0) complexes of the form SiP ₃(PR₃)₂Fe using PPh₃ and PMe ₃ resulted in cyclometalated products, SiP₃FeH((o-C ₆H₄)PPh₂) (7) and SiP₃FeH(CH ₂PMe₂) (8). Synthesis and characterization of these complexes, including crystal structures of 1-5, are reported.

Original language	English (US)
Pages (from-to)	3942-3949
Number of pages	8
Journal	Inorganic chemistry
Volume	49
Issue number	8
DOIs	https://doi.org/10.1021/ic1003325
State	Published - Apr 19 2010

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title = "Synthesis and characterization of pentaphosphino zero-valent iron complexes and their corresponding iron(II)-chloride and -hydride complexes",

abstract = "A pentaphosphino iron(II)-chloride species [tSiP 3(dmpm)FeCl][Cl] (1-Cl) (tSiP3 = tBuSi(CH2PMe2)3, dmpm = Me 2PCH2PMe2) was prepared from [( tSiP3Fe)2(μ-Cl)3][Cl] and dmpm. This species was reduced to give the corresponding iron(0) complex, tSiP3(dmpm)Fe (3), in near quantitative yield. Analogous complexes [SiP3(dmpe)FeCl][Cl] (2-Cl) and SiP3(dmpe)Fe (4) (SiP3 = MeSi(CH2PMe2)3, dmpe = Me2PCH2CH2PMe2) were prepared in the same manner as 1 and 3 but with lower yields because of competitive ligand rearrangement reactions that gave byproduct of trans-(dmpe)2FeCl 2 and (dmpe)5Fe2 (5). [tSiP 3(dmpm)FeH][A] (6) was prepared from the reaction of 3 with weak acids (HA), and the pKa of 6 was established to be approximately 25. Attempts to prepare pentaphosphino-iron(0) complexes of the form SiP 3(PR3)2Fe using PPh3 and PMe 3 resulted in cyclometalated products, SiP3FeH((o-C 6H4)PPh2) (7) and SiP3FeH(CH 2PMe2) (8). Synthesis and characterization of these complexes, including crystal structures of 1-5, are reported.",

author = "Thoreson, \{Kristen A.\} and Follett, \{Angela D.\} and Kristopher McNeill",

year = "2010",

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T1 - Synthesis and characterization of pentaphosphino zero-valent iron complexes and their corresponding iron(II)-chloride and -hydride complexes

AU - Thoreson, Kristen A.

AU - Follett, Angela D.

AU - McNeill, Kristopher

PY - 2010/4/19

Y1 - 2010/4/19

N2 - A pentaphosphino iron(II)-chloride species [tSiP 3(dmpm)FeCl][Cl] (1-Cl) (tSiP3 = tBuSi(CH2PMe2)3, dmpm = Me 2PCH2PMe2) was prepared from [( tSiP3Fe)2(μ-Cl)3][Cl] and dmpm. This species was reduced to give the corresponding iron(0) complex, tSiP3(dmpm)Fe (3), in near quantitative yield. Analogous complexes [SiP3(dmpe)FeCl][Cl] (2-Cl) and SiP3(dmpe)Fe (4) (SiP3 = MeSi(CH2PMe2)3, dmpe = Me2PCH2CH2PMe2) were prepared in the same manner as 1 and 3 but with lower yields because of competitive ligand rearrangement reactions that gave byproduct of trans-(dmpe)2FeCl 2 and (dmpe)5Fe2 (5). [tSiP 3(dmpm)FeH][A] (6) was prepared from the reaction of 3 with weak acids (HA), and the pKa of 6 was established to be approximately 25. Attempts to prepare pentaphosphino-iron(0) complexes of the form SiP 3(PR3)2Fe using PPh3 and PMe 3 resulted in cyclometalated products, SiP3FeH((o-C 6H4)PPh2) (7) and SiP3FeH(CH 2PMe2) (8). Synthesis and characterization of these complexes, including crystal structures of 1-5, are reported.

AB - A pentaphosphino iron(II)-chloride species [tSiP 3(dmpm)FeCl][Cl] (1-Cl) (tSiP3 = tBuSi(CH2PMe2)3, dmpm = Me 2PCH2PMe2) was prepared from [( tSiP3Fe)2(μ-Cl)3][Cl] and dmpm. This species was reduced to give the corresponding iron(0) complex, tSiP3(dmpm)Fe (3), in near quantitative yield. Analogous complexes [SiP3(dmpe)FeCl][Cl] (2-Cl) and SiP3(dmpe)Fe (4) (SiP3 = MeSi(CH2PMe2)3, dmpe = Me2PCH2CH2PMe2) were prepared in the same manner as 1 and 3 but with lower yields because of competitive ligand rearrangement reactions that gave byproduct of trans-(dmpe)2FeCl 2 and (dmpe)5Fe2 (5). [tSiP 3(dmpm)FeH][A] (6) was prepared from the reaction of 3 with weak acids (HA), and the pKa of 6 was established to be approximately 25. Attempts to prepare pentaphosphino-iron(0) complexes of the form SiP 3(PR3)2Fe using PPh3 and PMe 3 resulted in cyclometalated products, SiP3FeH((o-C 6H4)PPh2) (7) and SiP3FeH(CH 2PMe2) (8). Synthesis and characterization of these complexes, including crystal structures of 1-5, are reported.

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UR - https://www.scopus.com/pages/publications/77950985891#tab=citedBy

U2 - 10.1021/ic1003325

DO - 10.1021/ic1003325

M3 - Article

C2 - 20230063

AN - SCOPUS:77950985891

SN - 0020-1669

VL - 49

SP - 3942

EP - 3949

JO - Inorganic chemistry

JF - Inorganic chemistry

IS - 8

ER -

Synthesis and characterization of pentaphosphino zero-valent iron complexes and their corresponding iron(II)-chloride and -hydride complexes

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