Preparation of iron carbonyl complexes of germanium(II) and tin(II) each with a terminal fluorine atom

Jana, Anukul; Samuel, Prinson P.; Roesky, Herbert W.; Schulzke, Carola

doi:10.1016/j.jfluchem.2010.03.011

Cited by 23 publications

(11 citation statements)

References 26 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The 119 Sn NMR spectrum of 2 shows a single resonance at 89 ppm, which is downfield shifted compared to 1 (–224 ppm),10 due to the coordination of the iron atom to tin. This chemical shift is pertinent to the reported values 8b. The C H 3 protons for compound 2 in the 1 H NMR spectrum show a single resonance at 1.52 ppm.…”

Section: Resultssupporting

confidence: 52%

Syntheses of Iron Carbonyl N‐Heterocyclic Stannylene Complexes

Jana

Azhakar

Roesky

et al. 2011

Zeitschrift anorg allge chemie

Self Cite

View full text Add to dashboard Cite

The reaction of the β-diketiminato tin(II) compound LSnCl (1) [L = CH{CMe(NAr)} 2 , Ar = 2,6-iPr 2 C 6 H 3 ] with diiron nonacarbonyl, Fe 2 (CO) 9 , at room temperature led to the iron carbonyl complex LSn(Cl)Fe(CO) 4 (2). Complex 2 reacted with AgOSO 2 CF 3 (AgOTf) to yield LSn(OTf)Fe(CO) 4 (3). Complex 3 could also be prepared by 1795 the reaction of LSnOTf (4) with Fe 2 (CO) 9 at room temperature. Compounds 2 and 3 were characterized by elemental analysis, NMR spectroscopy, and mass spectrometry. Both complexes were unambiguously established by single-crystal X-ray structural analysis. Results and DiscussionThe reaction of 1 with Fe 2 (CO) 9 in a 1:1 ratio afforded complex 2 in good yield, which further reacted with AgOSO 2 CF 3 (AgOTf) to give complex 3 in quantitative yield (Scheme 1). Complex 3 could also be prepared by treating 4 [10] in 1:1 ratio with Fe 2 (CO) 9 (Scheme 1). Both complexes 2 and 3 are soluble in common organic solvents. Furthermore, they are stable both in solution and the solid state for a long period of time without any decomposition in an inert gas atmosphere. Complexes 2 and 3 were fully characterized by NMR spectroscopy, EI-MS spectrometry, elemental analysis, and unambiguously by single-crystal X-ray structural analysis. Scheme 1. Synthesis of 2 and 3.

show abstract

Section: Resultssupporting

confidence: 52%

Syntheses of Iron Carbonyl N‐Heterocyclic Stannylene Complexes

Jana

Azhakar

Roesky

et al. 2011

Zeitschrift anorg allge chemie

Self Cite

View full text Add to dashboard Cite

show abstract

“…In principle, three groups of stannylene complexes with Fe(CO) 5 , Fe 2 (CO) 9 , or their fragments have been described in the literature (Figure ). − The first group consists of two possible isomers of L 2 SnFe(CO) 4 complexes, where the first one can be described as the equatorial type A − and the second one as the axial type B . − Khrustalev found both isomers with a common stannylene type for such Fe(CO) 4 complexes. The β-diketiminato tin(II) hydroxide–Fe(CO) 4 complex reveals a crystal structure of type A , but the Fe(CO) 4 complex obtained from a stannylene with a dimethylamido instead of a hydroxy moiety crystallizes according to a type B structure.…”

Section: Resultsmentioning

confidence: 99%

Combined NMR and DFT Study on the Complexation Behavior of Lappert’s Tin(II) Amide

Broeckaert¹,

Turek

Olejník

et al. 2013

Organometallics

View full text Add to dashboard Cite

The complexation chemistry of the stannylene Sn{N[Si(CH3)3]2}2, first reported by Lappert in the 1970s, was investigated by 119Sn NMR chemical shift measurements. To this end, experimental NMR data and theoretical density functional theory (DFT) calculations were combined to get an insight into the interaction between the stannylene and various solvent molecules with σ- and/or π-coordinating power. Small variations in the measured 119Sn chemical shifts revealed a donor–acceptor interaction with the solvent molecules. In comparison to the noncoordinating solvent cyclohexane taken as a reference, a weak coordination was observed with aromatic solvent molecules (benzene and toluene) and a much stronger coordination with the σ-donors THF and pyridine. Pyridine was confirmed to be the strongest donor, as evidenced by its large upfield chemical shift Δδ(119Sn) of 635 ppm. The experimental chemical shifts were reproduced by DFT (NMR) calculations, demonstrating similar trends in the interaction strength with the σ- and π-donors. The stannylene Sn{N[Si(CH3)3]2}2 showed the ability to react with Fe(CO)5 and Fe2(CO)9 in the molar ratio 1/1 to provide L2SnFe(CO)4 complexes. With a molar excess of Fe2(CO)9, L2Sn[Fe(CO)4]2 was generated irreversibly. Upon prolonged UV irradiation in the presence of W(CO)6, in the molar ratio 1/1, a mixture of L2SnW(CO)5 and two (L2Sn)2W(CO)4 complexes was generated.

show abstract

“…We thus focused on the synthesis of a FeGe system devoid of the Si(II) fragment . Iron germanide in the bulk and nanoparticular state has received considerable attention as a magnetic semiconductor .…”

mentioning

confidence: 99%

A Molecular Complex with a Formally Neutral Iron Germanide Motif (Fe₂Ge₂)

et al. 2014

Self Cite

View full text Add to dashboard Cite

We report the synthesis and isolation of a stable complex containing the formally neutral Fe2Ge2 motif, which is stabilized by the coordination of an N-heterocyclic carbene to the germanium and of carbon monoxide to the iron center. [(NHC iPr2Me2 )GeFe(CO)4]2 is obtained by reduction of the NHC iPr2Me2 -coordinated dichlorogermylene adduct of Fe(CO)4, which in turn is obtained from the reaction of Fe2(CO)9 with GeCl2·NHC iPr2Me2 (NHC iPr2Me2 = 1,3-diisopropyl-4,5-dimethylimidazol-2-ylidene). The solid-state structure of the title compound reveals two distinct coordination modes for the Fe(CO)4 fragments: bridging (π-type) and terminal (σ-type). In solution, the rapid equilibrium between the two modes was resolved by NMR at −35 °C. Reaction with propylene sulfide at room temperature affords the sulfide-bridged digermanium complex with two terminal Fe(CO)4 moieties.

show abstract

Preparation of iron carbonyl complexes of germanium(II) and tin(II) each with a terminal fluorine atom

Cited by 23 publications

References 26 publications

Syntheses of Iron Carbonyl N‐Heterocyclic Stannylene Complexes

Syntheses of Iron Carbonyl N‐Heterocyclic Stannylene Complexes

Combined NMR and DFT Study on the Complexation Behavior of Lappert’s Tin(II) Amide

A Molecular Complex with a Formally Neutral Iron Germanide Motif (Fe₂Ge₂)

Contact Info

Product

Resources

About

Preparation of iron carbonyl complexes of germanium(II) and tin(II) each with a terminal fluorine atom

Cited by 23 publications

References 26 publications

Syntheses of Iron Carbonyl N‐Heterocyclic Stannylene Complexes

Syntheses of Iron Carbonyl N‐Heterocyclic Stannylene Complexes

Combined NMR and DFT Study on the Complexation Behavior of Lappert’s Tin(II) Amide

A Molecular Complex with a Formally Neutral Iron Germanide Motif (Fe2Ge2)

Contact Info

Product

Resources

About

A Molecular Complex with a Formally Neutral Iron Germanide Motif (Fe₂Ge₂)