Expanding the Chemistry of Rhenium Metal–Metal Bonded Fluoro Complexes: Facile Preparation and Characterization of Paddlewheel Complexes

Balasekaran, Samundeeswari Mariappan; Sattelberger, Alfred P.; Hagenbach, Adelheid; Poineau, Frederic

doi:10.1021/acs.inorgchem.7b02519

Title: Expanding the Chemistry of Rhenium Metal–Metal Bonded Fluoro Complexes: Facile Preparation and Characterization of Paddlewheel Complexes

Abstract

Quadruply bonded rhenium(III) dimers with the stoichiometry Re₂L₄F₂ (1, L = hexahydro-2H-pyrimido[1,2a]pyrimidinate (hpp^–); 2, L = diphenyl formamidinate (dpf^–)) were prepared from the solid-state melt reactions (SSMRs) between (NH₄)₂[Re₂F₈]·2H₂O and HL. Then those compounds were characterized in the solid state by single-crystal X-ray diffraction and in solution by UV–visible spectroscopy and cyclic voltammetry. The compound [Re₂(hpp)₄F₂]PF₆ (3) was prepared from the one-electron oxidation of Re₂(hpp)₄F₂ with [Cp₂Fe]PF₆. Compounds 1–3 are isostructural with the corresponding chloro derivatives. In summation, compound 1 undergoes two one-electron oxidations. Comparison with its higher halogen homologues reveals that Re₂(hpp)₄F₂ (1) is more easily oxidized than its chloro and bromo analogues.

Authors:

^[1]; Sattelberger, Alfred P. ^[2]; Hagenbach, Adelheid ^[3]; Poineau, Frederic ^[1]

Univ. of Nevada, Las Vegas, NV (United States). Dept. of Chemistry and Biochemistry
Univ. of Nevada, Las Vegas, NV (United States). Dept. of Chemistry and Biochemistry; Argonne National Lab. (ANL), Argonne, IL (United States). Chemical Sciences and Engineering Division
Freie Univ., Berlin (Germany). Dept. of Chemistry and Biochemistry

Publication Date:: Fri Dec 08 00:00:00 EST 2017

Research Org.:: Univ. of Nevada, Las Vegas, NV (United States)

Sponsoring Org.:: USDOE National Nuclear Security Administration (NNSA)

OSTI Identifier:: 1413997

Grant/Contract Number:: NA0003180; NA0000979

Resource Type:: Accepted Manuscript

Journal Name:: Inorganic Chemistry

Additional Journal Information:: Journal Volume: 57; Journal Issue: 1; Journal ID: ISSN 0020-1669

Publisher:: American Chemical Society (ACS)

Country of Publication:: United States

Language:: English

Subject:: 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats


                    Balasekaran, Samundeeswari Mariappan, Sattelberger, Alfred P., Hagenbach, Adelheid, and Poineau, Frederic. Expanding the Chemistry of Rhenium Metal–Metal Bonded Fluoro Complexes: Facile Preparation and Characterization of Paddlewheel Complexes.  United States: N. p., 2017. 
Web.  doi:10.1021/acs.inorgchem.7b02519.

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                    Balasekaran, Samundeeswari Mariappan, Sattelberger, Alfred P., Hagenbach, Adelheid, & Poineau, Frederic. Expanding the Chemistry of Rhenium Metal–Metal Bonded Fluoro Complexes: Facile Preparation and Characterization of Paddlewheel Complexes.  United States.  https://doi.org/10.1021/acs.inorgchem.7b02519

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                    Balasekaran, Samundeeswari Mariappan, Sattelberger, Alfred P., Hagenbach, Adelheid, and Poineau, Frederic. Fri .  
"Expanding the Chemistry of Rhenium Metal–Metal Bonded Fluoro Complexes: Facile Preparation and Characterization of Paddlewheel Complexes".  United States.  https://doi.org/10.1021/acs.inorgchem.7b02519.  https://www.osti.gov/servlets/purl/1413997.

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@article{osti_1413997,

  title        = {Expanding the Chemistry of Rhenium Metal–Metal Bonded Fluoro Complexes: Facile Preparation and Characterization of Paddlewheel Complexes},

  author       = {Balasekaran, Samundeeswari Mariappan and Sattelberger, Alfred P. and Hagenbach, Adelheid and Poineau, Frederic},

  abstractNote = {Quadruply bonded rhenium(III) dimers with the stoichiometry Re2L4F2 (1, L = hexahydro-2H-pyrimido[1,2a]pyrimidinate (hpp–); 2, L = diphenyl formamidinate (dpf–)) were prepared from the solid-state melt reactions (SSMRs) between (NH4)2[Re2F8]·2H2O and HL. Then those compounds were characterized in the solid state by single-crystal X-ray diffraction and in solution by UV–visible spectroscopy and cyclic voltammetry. The compound [Re2(hpp)4F2]PF6 (3) was prepared from the one-electron oxidation of Re2(hpp)4F2 with [Cp2Fe]PF6. Compounds 1–3 are isostructural with the corresponding chloro derivatives. In summation, compound 1 undergoes two one-electron oxidations. Comparison with its higher halogen homologues reveals that Re2(hpp)4F2 (1) is more easily oxidized than its chloro and bromo analogues.},

  doi          = {10.1021/acs.inorgchem.7b02519},

  journal      = {Inorganic Chemistry},

  number       = 1,

  volume       = 57,

  place        = {United States},

  year         = {Fri Dec 08 00:00:00 EST 2017},

  month        = {Fri Dec 08 00:00:00 EST 2017}

}

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https://doi.org/10.1021/acs.inorgchem.7b02519

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Cited by: 4 works

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Figure 1: Ball and stick representation of the Re₂(hpp)₄F₂ molecule in 1: (a) view perpendicular to the Re−Re bond; (b) view along the Re−Re bond. H atoms have been omitted for clarity. Color code: Re in turquoise, N in blue, F in green, and C in gray.

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Works referenced in this record:

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Works referencing / citing this record:

Difluorotetrakis(2-oxypyridine)dirhenium(III) - Preparation, Crystallographic Structure, and Electrochemical Properties: Difluorotetrakis(2-oxypyridine)dirhenium(III) - Preparation, Crystallographic Structure, and Electrochemical Properties
journal, December 2018

Balasekaran, Samundeeswari Mariappan; Sattelberger, Alfred Peter; Noll, Bruce
Zeitschrift für anorganische und allgemeine Chemie, Vol. 645, Issue 1
DOI: 10.1002/zaac.201800414

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Title: Expanding the Chemistry of Rhenium Metal–Metal Bonded Fluoro Complexes: Facile Preparation and Characterization of Paddlewheel Complexes

Abstract

Citation Formats

Figures / Tables:

Structure of hexafluorotetrapyridine dimolybdenum(III) journal, March 1991

Mo2F4(PR3)4 compounds and a comparison of their properties with those of other Mo2X4(PR3)4 compounds. A new synthetic route to metal fluorides by the reaction of alkyl species with Olah's reagent journal, March 1992

Notizen: Synthese und Eigenschaften des Oktafluorodirhenat(III) -anions, [Re2F8]2- / Synthesis and Properties of the Octafluorodirhenate(III) Anion, [Re2F8]2- journal, December 1979

Better Understanding of the Species with the Shortest Re 2 6+ Bonds and Related Re 2 7+ Species with Tetraguanidinate Paddlewheel Structures journal, March 2007

Molecular Engineering of Redox Rich Diruthenium Compounds: Further Investigation of Ru2(Yap)4X Type Compounds journal, December 2004

Octafluorodirhenate(III) Revisited: Solid-State Preparation, Characterization, and Multiconfigurational Quantum Chemical Calculations journal, May 2016

Formamidinate complexes of dirhenium, Re2n+, cores with n = 4, 5, and 6 journal, March 1992

A very short Re26+ quadruple bond: first DFT calculations on a paddlewheel complex with an element of the third transition series journal, January 1999

The Synthesis and Characterization of Re2(Xap)4Cl2 Compounds journal, July 2006

Preparation and structure of dichlorotetrakis(o-oxypyridine)dirhenium(III) journal, June 1979

Resolving conformational ambiguities in M2(hpp)4Cl2 paddlewheel compounds: M=Mo, W, Re, Ru, Os, Ir, Pd, Pt journal, July 2003

Fluoridonitrosyl Complexes of Technetium(I) and Technetium(II). Synthesis, Characterization, Reactions, and DFT Calculations journal, May 2014

Crystallographic and Spectroscopic Characterization of Tetrakis(μ-N,N′-diarylformamidinato)dichlorodirhenium(III,III) Compounds journal, November 1999

A highly oxidized Re27+ species with an electron-poor bond of order 3.5 journal, March 2003

An uncommon highly oxidized multiple bonded Re28+ species journal, January 2011

New multiply-bonded dimetal compounds containing bridging 1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidinato groups—I. The V24+, Cr24+ and Mo24+ compounds and some salts of the protonated ligand journal, January 1998

Some reactions of the octahalodirhenate(III) ions. 10. Further study of the tetrakis(pivalato)dirhenium dihalides journal, June 1979

Studies on metal carboxylates. 16. Electrochemical generation and solution properties of the [Re2(O2CR)4X2]- anions (X = chlorine, bromine, iodine) journal, June 1980

Cobaltocene reductions of multiply bonded dirhenium complexes. II. The isolation of the paramagnetic species [(η5-C5H5)2Co][Re2(hp)4X2] (hp = anion of 2-hydroxypyridine; X = Cl, Br, or I) journal, December 1985

Octachloro- and Octabromoditechnetate(III) and Their Rhenium(III) Congeners journal, February 2008

Difluorotetrakis(2-oxypyridine)dirhenium(III) - Preparation, Crystallographic Structure, and Electrochemical Properties: Difluorotetrakis(2-oxypyridine)dirhenium(III) - Preparation, Crystallographic Structure, and Electrochemical Properties journal, December 2018

Structure of hexafluorotetrapyridine dimolybdenum(III)
journal, March 1991

Mo2F4(PR3)4 compounds and a comparison of their properties with those of other Mo2X4(PR3)4 compounds. A new synthetic route to metal fluorides by the reaction of alkyl species with Olah's reagent
journal, March 1992

Notizen: Synthese und Eigenschaften des Oktafluorodirhenat(III) -anions, [Re2F8]2- / Synthesis and Properties of the Octafluorodirhenate(III) Anion, [Re2F8]2-
journal, December 1979

Better Understanding of the Species with the Shortest Re ₂ ⁶⁺ Bonds and Related Re ₂ ⁷⁺ Species with Tetraguanidinate Paddlewheel Structures
journal, March 2007

Molecular Engineering of Redox Rich Diruthenium Compounds: Further Investigation of Ru2(Yap)4X Type Compounds
journal, December 2004

Octafluorodirhenate(III) Revisited: Solid-State Preparation, Characterization, and Multiconfigurational Quantum Chemical Calculations
journal, May 2016

Formamidinate complexes of dirhenium, Re2n+, cores with n = 4, 5, and 6
journal, March 1992

A very short Re26+ quadruple bond: first DFT calculations on a paddlewheel complex with an element of the third transition series
journal, January 1999

The Synthesis and Characterization of Re2(Xap)4Cl2 Compounds
journal, July 2006

Preparation and structure of dichlorotetrakis(o-oxypyridine)dirhenium(III)
journal, June 1979

Resolving conformational ambiguities in M2(hpp)4Cl2 paddlewheel compounds: M=Mo, W, Re, Ru, Os, Ir, Pd, Pt
journal, July 2003

Fluoridonitrosyl Complexes of Technetium(I) and Technetium(II). Synthesis, Characterization, Reactions, and DFT Calculations
journal, May 2014

Crystallographic and Spectroscopic Characterization of Tetrakis(μ-N,N′-diarylformamidinato)dichlorodirhenium(III,III) Compounds
journal, November 1999

A highly oxidized Re27+ species with an electron-poor bond of order 3.5
journal, March 2003

An uncommon highly oxidized multiple bonded Re28+ species
journal, January 2011

New multiply-bonded dimetal compounds containing bridging 1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidinato groups—I. The V24+, Cr24+ and Mo24+ compounds and some salts of the protonated ligand
journal, January 1998

Some reactions of the octahalodirhenate(III) ions. 10. Further study of the tetrakis(pivalato)dirhenium dihalides
journal, June 1979

Studies on metal carboxylates. 16. Electrochemical generation and solution properties of the [Re2(O2CR)4X2]- anions (X = chlorine, bromine, iodine)
journal, June 1980

Cobaltocene reductions of multiply bonded dirhenium complexes. II. The isolation of the paramagnetic species [(η5-C5H5)2Co][Re2(hp)4X2] (hp = anion of 2-hydroxypyridine; X = Cl, Br, or I)
journal, December 1985

Octachloro- and Octabromoditechnetate(III) and Their Rhenium(III) Congeners
journal, February 2008

Difluorotetrakis(2-oxypyridine)dirhenium(III) - Preparation, Crystallographic Structure, and Electrochemical Properties: Difluorotetrakis(2-oxypyridine)dirhenium(III) - Preparation, Crystallographic Structure, and Electrochemical Properties
journal, December 2018