Tetrahydrofuran Complexes of Rhenium(I)

Storhoff, Bruce N.; Lewis, Huntley C.

doi:10.1080/00945717408069677

Cited by 19 publications

(5 citation statements)

References 13 publications

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“…It is worth noting that a similar route was also attempted in which Re(CO) 3 (THF) 2 Br was prepared by heating Re(CO) 5 Br in THF at reflux according to a report by Storhoff and Lewis . Unfortunately, after several trials, the reaction of this adduct failed to yield the desired complex.…”

Section: Resultsmentioning

confidence: 99%

Bitopic Phenylene-Linked Bis(pyrazolyl)methane Ligands: Preparation and Supramolecular Structures of Hetero- and Homobimetallic Complexes Incorporating Organoplatinum(II) and Tricarbonylrhenium(I) Centers

et al. 2005

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The new fixed-geometry, phenylene-linked bis(pyrazolyl)methane ligands α,α,α‘,α‘-tetra(1-pyrazolyl)-m-xylene (m-[CH(pz)2]2C6H4, L m ), α,α,α‘,α‘-tetra(1-pyrazolyl)-p-xylene (p-[CH(pz)2]2C6H4, L p ), and α,α,α‘,α‘-tetrakis(4-benzylpyrazol-1-yl)-p-xylene (p-[CH(4Bnpz)2]2C6H4, 4Bn L p ) have been synthesized in order to prepare hetero- and homobimetallic complexes incorporating tricarbonylrhenium(I) and bis(p-tolyl)platinum(II) fragments. Coordination of one rhenium center to L m was achieved to yield the monometallic rhenium complex {m-[CH(pz)2]2C6H4}Re(CO)3Br, which then incorporated a second metal center to give the heterobimetallic complex {μ-m-[CH(pz)2]2C6H4}[Re(CO)3Br][Pt(p-tolyl)2]. The homobimetallic rhenium complexes of each ligand, {μ-m-[CH(pz)2]2C6H4}[Re(CO)3Br]2, {μ-p-[CH(pz)2]2C6H4}[Re(CO)3Br]2, and {μ-p-[CH(4Bnpz)2]2C6H4}[Re(CO)3Br]2, were also prepared. The crystalline structure of each complex shows extensive noncovalent interactions, including weak hydrogen bonds and π···π and CH···π interactions, that organize the molecules into complex supramolecular structures.

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Section: Resultsmentioning

confidence: 99%

Bitopic Phenylene-Linked Bis(pyrazolyl)methane Ligands: Preparation and Supramolecular Structures of Hetero- and Homobimetallic Complexes Incorporating Organoplatinum(II) and Tricarbonylrhenium(I) Centers

et al. 2005

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“…An alternative synthetic approach to 2 was explored briefly. A solution of Re(CO) 5 Br was heated under reflux for 18 h in THF to give a solution containing Re 2 (CO) 6 (THF) 2 (μ-Br) 2 . Then 1,2-bis(indenyl)ethane in THF was treated with 2 equiv of n -butyllithium, and this solution was added to the previous one, followed by heating the mixture under reflux.…”

Section: Resultsmentioning

confidence: 99%

“…A solution of Re(CO) 5 Br was heated under reflux for 18 h in THF to give a solution containing Re 2 (CO) 6 -(THF) 2 (µ-Br) 2 . 7 Then 1,2-bis(indenyl)ethane in THF was treated with 2 equiv of n-butyllithium, and this solution was added to the previous one, followed by heating the mixture under reflux. However, the yields of 1 and 2 obtained following chromatographic workup (25% and 24%, respectively) were comparable with those obtained by the direct reaction method.…”

Section: Synthesis Ofmentioning

confidence: 99%

“…The Re-Re bond distance of 2.9843(6) Å in 7 is longer than that in related compounds containing a Re-Re bond and a bridging η 1 :η 2 -vinyl group. For example, this distance is 2.881(1) Å in Re 2 (CO) 7 (C 8 H 2 Ph 2 Fc 2 ), 14 2.8868 (7) Å in Re 2 (CO) 7 [µ-C(Me)C(NMe 2 )C(NMe 2 )-C(Me)], 15 2.878(1) Å in Re 2 (CO) 5 (C 4 Ph 4 )(C 2 Ph 2 ), 16 and 2.874(1) Å in Re 2 (µ-η 1 :η 1 :η 4 -C 4 Ph 4 )(CO) 7 . 17 It is also somewhat longer than the value of 2.928(1) Å in the R,βunsaturated bimetallic compound Cp*(CO) 2 Re{µ-η 1 :η 3 -CHdC[C(CH 3 )dCH 2 ]CO}Re(CO)Cp*.…”

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confidence: 99%

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Mono- and Bimetalated Rhenium and Manganese Carbonyl Derivatives of 1,2-Bis(indenyl)ethane

and

Shapley

2000

Organometallics

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Heating a mixture of M 2 (CO) 10 (M ) Re, Mn) with 1,2-bis(indenyl)ethane in Decalin at ca. 180 °C provided both monometalated M(CO) 3 {(η 5 -C 9 H 6 )C 2 H 4 C 9 H 7 )} (1, M ) Re; 3, M ) Mn) and bimetalated (M(CO) 3 ) 2 {µ-(η 5 -C 9 H 6 )C 2 H 4 (η 5 -C 9 H 6 )} (2, M ) Re; 4, M ) Mn) products, which were separated by chromatography, isolated as pure solids, and characterized by a combination of analytical and spectroscopic methods. The bimetalated compounds 2 and 4 were formed as a mixture of meso and rac diastereomers; the rac form of 2 crystallized selectively, and its structure was determined by X-ray crystallography. UV photolysis of 1 and 3 (or 4) yielded the compounds M(CO) 2 {(η 5 -C 9 H 6 )C 2 H 4 (η 2 -C 9 H 7 )} (5, M ) Re; 6, M ) Mn), in which a carbonyl ligand is replaced by the η 2 coordination of the pendant indene group. UV photolysis of 2 gave primarily the rearranged isomer Re 2 (CO) 6 {µ-(η 1 :η 2 -C 9 H 6 )-C 2 H 4 (η 5 -C 9 H 6 )} ( 7), in which one indenyl group bridges the two Re centers as an η 1 :η 2 -vinyl moiety. The molecular structures of compounds 6 and 7 also were determined by X-ray crystallography.

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“…Cycloheptatriene (90%), bromoform (96%), potassium tert -butoxide (95%), methyllithium (complex with lithium bromide, 1.5 M in Et 2 O), n -butyllithium (2.5 M in hexanes), and thallium ethoxide (98%) were supplied by Aldrich and used without further purification. 7-Alkylcycloheptatrienes (R = methyl, ethyl, isopropyl, tert -butyl), 8,8-dibromobicyclo[5.1.0]octa-2,4-diene, [Re(CO) 3 (THF)Br] 2 and Mn(CO) 3 (py) 2 Br were prepared by the literature procedures.…”

Section: Methodsmentioning

confidence: 99%

Convenient Solution Route To Alkylated Pentalene Ligands: New Metal Monoalkylpentalenyl Complexes

et al. 2005

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Carbene-induced rearrangement of 8,8-dibromobicyclo[5.1.0]octa-2,4-dienes and subsequent in situ deprotonation of the dihydropentalenes formed represents a straightforward and versatile solution route to pentalene ligands for use in organometallic chemistry. We report here the synthesis of 6-alkyl-substituted 8,8-dibromobicyclo[5.1.0]octa-2,4-dienes and their rearrangement to give correspondingly substituted pentalene ligands. Generation of methyl-substituted dihydropentalenes from 8,8-dibromo-6-methylbicyclo-[5.1.0]octa-2,4-diene followed by monodeprotonation with TlOEt gives methylhydropentalenyl salts, Tl-(C 8 H 6 Me), as a mixture of isomers. Formation of both 1-Me and 3-Me isomers of Re(C 8 H 6 Me)(CO) 3 from these Tl species shows that monodeprotonation of the dihydropentalenes occurs at the unsubstituted ring. No evidence for the 2-Me isomer is observed, consistent with the rearrangement mechanism reported in the literature. Likewise, rearrangement of 8,8-dibromo-6-alkylbicyclo[5.1.0]octa-2,4-dienes (R ) Me, Et, i Pr) and subsequent double deprotonation with n BuLi in the presence of DME affords the pentalenyl salts Li 2 (C 8 H 5 R)‚xDME. X-ray crystallographic studies of the dinuclear Mn organometallics anti-[Mn-(CO) 3 ] 2 (C 8 H 5 R) synthesized from the Li salts confirm that these alkylated pentalene ligands are substituted at the 1-position exclusively. The crystal structure of a model hydropentalenyl complex, Re(C 8 H 7 )(CO) 3 , is also reported.

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Tetrahydrofuran Complexes of Rhenium(I)

Cited by 19 publications

References 13 publications

Bitopic Phenylene-Linked Bis(pyrazolyl)methane Ligands: Preparation and Supramolecular Structures of Hetero- and Homobimetallic Complexes Incorporating Organoplatinum(II) and Tricarbonylrhenium(I) Centers

Bitopic Phenylene-Linked Bis(pyrazolyl)methane Ligands: Preparation and Supramolecular Structures of Hetero- and Homobimetallic Complexes Incorporating Organoplatinum(II) and Tricarbonylrhenium(I) Centers

Mono- and Bimetalated Rhenium and Manganese Carbonyl Derivatives of 1,2-Bis(indenyl)ethane

Convenient Solution Route To Alkylated Pentalene Ligands: New Metal Monoalkylpentalenyl Complexes

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