Synthesis of [AsPh4][Fe3(CO)9(μ-CO)(μ3-HBCl)] by Oxidative Chloride Substitution of [Fe3(CO)9(μ3-HBCO)]2-

Louise E. Crascall; B. H.S. Thimmappa; Arnold L. Rheingold; Robert Ostrander; Thomas P. Fehlner

doi:10.1021/om00018a006

Synthesis of [AsPh₄][Fe₃(CO)₉(μ-CO)(μ₃-HBCl)] by Oxidative Chloride Substitution of [Fe₃(CO)₉(μ₃-HBCO)]^2-

Louise E. Crascall, B. H.S. Thimmappa, Arnold L. Rheingold^*, Robert Ostrander, Thomas P. Fehlner

^*Corresponding author for this work

Department of Chemistry, Manipal Institute of Technology, Manipal

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Abstract

The deprotonation of (μ-H)Fe₃(CO)₉(μ-CO)(μ₃-HBH) with n-butyllithium yields the dianionic complex [Li]₂[Fe₃(CO)₉(μ₃-HBCO)], which has been spectroscopically characterized. In contrast to the facile reprotonation of closely related ferraboranes, protonation of [Li]₂[Fe₃(CO)₉(μ₃-HBCO)] leads to decomposition. On the other hand, reaction of this dianionic complex with 2 equiv of FeCl₃ gives a good yield of [Li][Fe₃(CO)₉(μ-CO)(μ₃-HBCl). Metathesis with [AsPh₄][Cl] yields [AsPh₄][Fe₃(CO)₉(μ-CO)(μ₃-HBCl)], which has been crystallographically characterized (triclinic, P1, a = 9.534(3) Å, b = 13.305(4) Å, c = 15.225(4) Å, α = 104.39(2)°, β = 103.56(2)°, γ = 99.23(2)°, V = 1768.7(8) Å³, Z = 2). Comparison with the analogous osmium clusters, as well as isoelectronic organometallic clusters, reveals relationships among their structures, properties, and energetics.

Original language	English
Pages (from-to)	2153-2158
Number of pages	6
Journal	Organometallics
Volume	13
Issue number	6
DOIs	https://doi.org/10.1021/om00018a006
Publication status	Published - 01-06-1994

All Science Journal Classification (ASJC) codes

Physical and Theoretical Chemistry
Organic Chemistry
Inorganic Chemistry

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10.1021/om00018a006

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@article{570c4a2784c64178b6f2191a1b02e85d,

title = "Synthesis of [AsPh4][Fe3(CO)9(μ-CO)(μ3-HBCl)] by Oxidative Chloride Substitution of [Fe3(CO)9(μ3-HBCO)]2-",

abstract = "The deprotonation of (μ-H)Fe3(CO)9(μ-CO)(μ3-HBH) with n-butyllithium yields the dianionic complex [Li]2[Fe3(CO)9(μ3-HBCO)], which has been spectroscopically characterized. In contrast to the facile reprotonation of closely related ferraboranes, protonation of [Li]2[Fe3(CO)9(μ3-HBCO)] leads to decomposition. On the other hand, reaction of this dianionic complex with 2 equiv of FeCl3 gives a good yield of [Li][Fe3(CO)9(μ-CO)(μ3-HBCl). Metathesis with [AsPh4][Cl] yields [AsPh4][Fe3(CO)9(μ-CO)(μ3-HBCl)], which has been crystallographically characterized (triclinic, P1, a = 9.534(3) {\AA}, b = 13.305(4) {\AA}, c = 15.225(4) {\AA}, α = 104.39(2)°, β = 103.56(2)°, γ = 99.23(2)°, V = 1768.7(8) {\AA}3, Z = 2). Comparison with the analogous osmium clusters, as well as isoelectronic organometallic clusters, reveals relationships among their structures, properties, and energetics.",

author = "Crascall, \{Louise E.\} and Thimmappa, \{B. H.S.\} and Rheingold, \{Arnold L.\} and Robert Ostrander and Fehlner, \{Thomas P.\}",

year = "1994",

month = jun,

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doi = "10.1021/om00018a006",

language = "English",

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pages = "2153--2158",

journal = "Organometallics",

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publisher = "American Chemical Society",

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TY - JOUR

T1 - Synthesis of [AsPh4][Fe3(CO)9(μ-CO)(μ3-HBCl)] by Oxidative Chloride Substitution of [Fe3(CO)9(μ3-HBCO)]2-

AU - Crascall, Louise E.

AU - Thimmappa, B. H.S.

AU - Rheingold, Arnold L.

AU - Ostrander, Robert

AU - Fehlner, Thomas P.

PY - 1994/6/1

Y1 - 1994/6/1

N2 - The deprotonation of (μ-H)Fe3(CO)9(μ-CO)(μ3-HBH) with n-butyllithium yields the dianionic complex [Li]2[Fe3(CO)9(μ3-HBCO)], which has been spectroscopically characterized. In contrast to the facile reprotonation of closely related ferraboranes, protonation of [Li]2[Fe3(CO)9(μ3-HBCO)] leads to decomposition. On the other hand, reaction of this dianionic complex with 2 equiv of FeCl3 gives a good yield of [Li][Fe3(CO)9(μ-CO)(μ3-HBCl). Metathesis with [AsPh4][Cl] yields [AsPh4][Fe3(CO)9(μ-CO)(μ3-HBCl)], which has been crystallographically characterized (triclinic, P1, a = 9.534(3) Å, b = 13.305(4) Å, c = 15.225(4) Å, α = 104.39(2)°, β = 103.56(2)°, γ = 99.23(2)°, V = 1768.7(8) Å3, Z = 2). Comparison with the analogous osmium clusters, as well as isoelectronic organometallic clusters, reveals relationships among their structures, properties, and energetics.

AB - The deprotonation of (μ-H)Fe3(CO)9(μ-CO)(μ3-HBH) with n-butyllithium yields the dianionic complex [Li]2[Fe3(CO)9(μ3-HBCO)], which has been spectroscopically characterized. In contrast to the facile reprotonation of closely related ferraboranes, protonation of [Li]2[Fe3(CO)9(μ3-HBCO)] leads to decomposition. On the other hand, reaction of this dianionic complex with 2 equiv of FeCl3 gives a good yield of [Li][Fe3(CO)9(μ-CO)(μ3-HBCl). Metathesis with [AsPh4][Cl] yields [AsPh4][Fe3(CO)9(μ-CO)(μ3-HBCl)], which has been crystallographically characterized (triclinic, P1, a = 9.534(3) Å, b = 13.305(4) Å, c = 15.225(4) Å, α = 104.39(2)°, β = 103.56(2)°, γ = 99.23(2)°, V = 1768.7(8) Å3, Z = 2). Comparison with the analogous osmium clusters, as well as isoelectronic organometallic clusters, reveals relationships among their structures, properties, and energetics.

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Synthesis of [AsPh₄][Fe₃(CO)₉(μ-CO)(μ₃-HBCl)] by Oxidative Chloride Substitution of [Fe₃(CO)₉(μ₃-HBCO)]^2-

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