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

Producción científica: Article › revisión exhaustiva

20 Citas (Scopus)

Resumen

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.

Idioma original	English
Páginas (desde-hasta)	133-143
Número de páginas	11
Publicación	Journal of Organometallic Chemistry
Volumen	578
N.º	1-2
DOI	https://doi.org/10.1016/S0022-328X(98)01115-2
Estado	Published - abr 22 1999

Nota bibliográfica

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.

Financiación

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.

Financiadores	Número del financiador
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
U.S. Department of Energy Oak Ridge National Laboratory U.S. Department of Energy National Science Foundation National Energy Research Scientific Computing Center	DE-FG02-91ER75657, DE-FG05-85ER13432
U.S. Department of Energy Oak Ridge National Laboratory U.S. Department of Energy National Science Foundation National Energy Research Scientific Computing Center

ASJC Scopus subject areas

Biochemistry
Physical and Theoretical Chemistry
Organic Chemistry
Inorganic Chemistry
Materials Chemistry

Acceder al documento

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

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@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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