The cyclo-C3 ligand: Trimetallic cyclopropenium complexes of Group 6-8 metals, including the X-ray crystal structure of [{Fe(CO)2(Cp)}3(μ3-C3)][SbF 6]

Michael S. Morton; John P. Selegue

doi:10.1016/S0022-328X(98)01115-2

The cyclo-C₃ ligand: Trimetallic cyclopropenium complexes of Group 6-8 metals, including the X-ray crystal structure of [{Fe(CO)₂(Cp)}₃(μ₃-C₃)][SbF ₆]

Michael S. Morton, John P. Selegue

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

20 Scopus citations

Abstract

Several trimetallic cyclopropenium cations have been prepared via reactions of three equivalents of a metallate anion with [C₃Cl₃][SbF₆]. The X-ray crystal structure of [{Fe(CO)₂(Cp)}₃(μ₃-C₃)][SbF ₆] (1) shows a nearly equilateral C₃ ring with an iron center bonded to each vertex. The cyclopropenium complexes [{Ru(CO)₂(Cp)}₃(μ₃-C₃)][SbF ₆] (2), [{Mo(CO)₃(Cp)}₃(μ₃-C₃)][SbF ₆] (3), [{W(CO)₃(Cp)}₃(μ₃-C₃)][SbF ₆] (4), and [{Re(CO)₅}₃(μ₃-C₃)][SbF ₆] (5) were spectroscopically characterized. Because of the 3-fold symmetrical nature of these complexes, their NMR spectra display a single cyclo-C₃ ring carbon resonance and a single set of resonances for the metal moiety. Compound 1 reacts with Li[BHEt₃] and LiMe to give complex reaction mixtures. We were not able to add a fourth metal center to the C₃ ring of 1. The spectroscopically characterized C₉ complex [{Fe(CO)₂(Cp)}₃{μ₃-C ₃(C≡C)₃}][SbF₆] (6), prepared by the reaction of three equivalents of [Fe(C≡CSiMe₃)(CO)₂(Cp)] with [C₃Cl₃][SbF₆], was not stable enough to isolate in analytically pure form.

Original language	English
Pages (from-to)	133-143
Number of pages	11
Journal	Journal of Organometallic Chemistry
Volume	578
Issue number	1-2
DOIs	https://doi.org/10.1016/S0022-328X(98)01115-2
State	Published - Apr 22 1999

Bibliographical note

Funding Information:
We thank the Kentucky National Science Foundation EPSCOR program (EPS-9452895) and the U.S. Department of Energy (DE-FG05-85ER13432 and EPSCOR Traineeship DE-FG02-91ER75657) for financial support, the University of Kentucky Major Research Instrumentation Bond Program (ID# 7E-8E48-25) for equipment used in this study, the University of Kentucky Mass Spectrometry Center for mass spectra and Professor Carolyn P. Brock and Michael Lloyd for X-ray crystallographic assistance.

Funding

We thank the Kentucky National Science Foundation EPSCOR program (EPS-9452895) and the U.S. Department of Energy (DE-FG05-85ER13432 and EPSCOR Traineeship DE-FG02-91ER75657) for financial support, the University of Kentucky Major Research Instrumentation Bond Program (ID# 7E-8E48-25) for equipment used in this study, the University of Kentucky Mass Spectrometry Center for mass spectra and Professor Carolyn P. Brock and Michael Lloyd for X-ray crystallographic assistance.

Funders	Funder number
National Science Foundation NNCI Kentucky Multiscale Manufacturing	EPS-9452895
University of Kentucky Major Research Instrumentation Bond Program	7E-8E48-25
University of Kentucky Mass Spectrometry Center
Michigan State University-U.S. Department of Energy (MSU-DOE) Plant Research Laboratory	DE-FG02-91ER75657, DE-FG05-85ER13432

Keywords

Carbide
Cyclopropenium
Iron
Molybdenum
Rhenium
Ruthenium
Tungsten

ASJC Scopus subject areas

Biochemistry
Physical and Theoretical Chemistry
Organic Chemistry
Inorganic Chemistry
Materials Chemistry

Access to Document

10.1016/S0022-328X(98)01115-2

Cite this

@article{a49febc7c6f4409793dc9b5974dbf283,

title = "The cyclo-C3 ligand: Trimetallic cyclopropenium complexes of Group 6-8 metals, including the X-ray crystal structure of [{Fe(CO)2(Cp)}3(μ3-C3)][SbF 6]",

abstract = "Several trimetallic cyclopropenium cations have been prepared via reactions of three equivalents of a metallate anion with [C3Cl3][SbF6]. The X-ray crystal structure of [{Fe(CO)2(Cp)}3(μ3-C3)][SbF 6] (1) shows a nearly equilateral C3 ring with an iron center bonded to each vertex. The cyclopropenium complexes [{Ru(CO)2(Cp)}3(μ3-C3)][SbF 6] (2), [{Mo(CO)3(Cp)}3(μ3-C3)][SbF 6] (3), [{W(CO)3(Cp)}3(μ3-C3)][SbF 6] (4), and [{Re(CO)5}3(μ3-C3)][SbF 6] (5) were spectroscopically characterized. Because of the 3-fold symmetrical nature of these complexes, their NMR spectra display a single cyclo-C3 ring carbon resonance and a single set of resonances for the metal moiety. Compound 1 reacts with Li[BHEt3] and LiMe to give complex reaction mixtures. We were not able to add a fourth metal center to the C3 ring of 1. The spectroscopically characterized C9 complex [{Fe(CO)2(Cp)}3{μ3-C 3(C≡C)3}][SbF6] (6), prepared by the reaction of three equivalents of [Fe(C≡CSiMe3)(CO)2(Cp)] with [C3Cl3][SbF6], was not stable enough to isolate in analytically pure form.",

keywords = "Carbide, Cyclopropenium, Iron, Molybdenum, Rhenium, Ruthenium, Tungsten",

author = "Morton, {Michael S.} and Selegue, {John P.}",

note = "Funding Information: We thank the Kentucky National Science Foundation EPSCOR program (EPS-9452895) and the U.S. Department of Energy (DE-FG05-85ER13432 and EPSCOR Traineeship DE-FG02-91ER75657) for financial support, the University of Kentucky Major Research Instrumentation Bond Program (ID# 7E-8E48-25) for equipment used in this study, the University of Kentucky Mass Spectrometry Center for mass spectra and Professor Carolyn P. Brock and Michael Lloyd for X-ray crystallographic assistance.",

year = "1999",

month = apr,

day = "22",

doi = "10.1016/S0022-328X(98)01115-2",

language = "English",

volume = "578",

pages = "133--143",

number = "1-2",

}

TY - JOUR

T1 - The cyclo-C3 ligand

T2 - Trimetallic cyclopropenium complexes of Group 6-8 metals, including the X-ray crystal structure of [{Fe(CO)2(Cp)}3(μ3-C3)][SbF 6]

AU - Morton, Michael S.

AU - Selegue, John P.

N1 - Funding Information: We thank the Kentucky National Science Foundation EPSCOR program (EPS-9452895) and the U.S. Department of Energy (DE-FG05-85ER13432 and EPSCOR Traineeship DE-FG02-91ER75657) for financial support, the University of Kentucky Major Research Instrumentation Bond Program (ID# 7E-8E48-25) for equipment used in this study, the University of Kentucky Mass Spectrometry Center for mass spectra and Professor Carolyn P. Brock and Michael Lloyd for X-ray crystallographic assistance.

PY - 1999/4/22

Y1 - 1999/4/22

N2 - Several trimetallic cyclopropenium cations have been prepared via reactions of three equivalents of a metallate anion with [C3Cl3][SbF6]. The X-ray crystal structure of [{Fe(CO)2(Cp)}3(μ3-C3)][SbF 6] (1) shows a nearly equilateral C3 ring with an iron center bonded to each vertex. The cyclopropenium complexes [{Ru(CO)2(Cp)}3(μ3-C3)][SbF 6] (2), [{Mo(CO)3(Cp)}3(μ3-C3)][SbF 6] (3), [{W(CO)3(Cp)}3(μ3-C3)][SbF 6] (4), and [{Re(CO)5}3(μ3-C3)][SbF 6] (5) were spectroscopically characterized. Because of the 3-fold symmetrical nature of these complexes, their NMR spectra display a single cyclo-C3 ring carbon resonance and a single set of resonances for the metal moiety. Compound 1 reacts with Li[BHEt3] and LiMe to give complex reaction mixtures. We were not able to add a fourth metal center to the C3 ring of 1. The spectroscopically characterized C9 complex [{Fe(CO)2(Cp)}3{μ3-C 3(C≡C)3}][SbF6] (6), prepared by the reaction of three equivalents of [Fe(C≡CSiMe3)(CO)2(Cp)] with [C3Cl3][SbF6], was not stable enough to isolate in analytically pure form.

AB - Several trimetallic cyclopropenium cations have been prepared via reactions of three equivalents of a metallate anion with [C3Cl3][SbF6]. The X-ray crystal structure of [{Fe(CO)2(Cp)}3(μ3-C3)][SbF 6] (1) shows a nearly equilateral C3 ring with an iron center bonded to each vertex. The cyclopropenium complexes [{Ru(CO)2(Cp)}3(μ3-C3)][SbF 6] (2), [{Mo(CO)3(Cp)}3(μ3-C3)][SbF 6] (3), [{W(CO)3(Cp)}3(μ3-C3)][SbF 6] (4), and [{Re(CO)5}3(μ3-C3)][SbF 6] (5) were spectroscopically characterized. Because of the 3-fold symmetrical nature of these complexes, their NMR spectra display a single cyclo-C3 ring carbon resonance and a single set of resonances for the metal moiety. Compound 1 reacts with Li[BHEt3] and LiMe to give complex reaction mixtures. We were not able to add a fourth metal center to the C3 ring of 1. The spectroscopically characterized C9 complex [{Fe(CO)2(Cp)}3{μ3-C 3(C≡C)3}][SbF6] (6), prepared by the reaction of three equivalents of [Fe(C≡CSiMe3)(CO)2(Cp)] with [C3Cl3][SbF6], was not stable enough to isolate in analytically pure form.

KW - Carbide

KW - Cyclopropenium

KW - Iron

KW - Molybdenum

KW - Rhenium

KW - Ruthenium

KW - Tungsten

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U2 - 10.1016/S0022-328X(98)01115-2

DO - 10.1016/S0022-328X(98)01115-2

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