DOI: 10.1021/ja9715197. The First Binuclear Mn(IV) Complex Containing a Bridging Imidazolate Ligand Exhibits Unique EPR Spectral Features

The First Binuclear Mn(IV) Complex Containing a Bridging Imidazolate Ligand Exhibits Unique EPR Spectral Features

10.1021/ja9715197

Crossref journal-article

American Chemical Society (ACS)

Journal of the American Chemical Society (316)

Bibliography

Caudle, M. T., Kampf, J. W., Kirk, M. L., Rasmussen, P. G., & Pecoraro, V. L. (1997). The First Binuclear Mn(IV) Complex Containing a Bridging Imidazolate Ligand Exhibits Unique EPR Spectral Features. Journal of the American Chemical Society, 119(39), 9297â9298.

Authors 5

M. Tyler Caudle (first)
Jeff W. Kampf (additional)
Martin L. Kirk (additional)
Paul G. Rasmussen (additional)
Vincent L. Pecoraro (additional)

References 27 Referenced 55

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10.1021/ic00220a005 / Inorg. Chem. by Seela J. L. (1985)
The preparation and characterization of the [Mn(III)(dtbsalpn)]2HDCBI precursor will be detailed in a subsequent full paper. [Mn(III)(dtbsalpn)]2HDCBI (1.5 g, 1.2 mmol) was slurried in 120 mL of distilled CH3CN containing 0.10 M tetrabutylammonium hexafluorophosphate and was carefully reacted with 1 equiv of tetrabutylammonium hydroxide under anaerobic conditions. Bulk electrolysis of the solution at 500 mVvsAg wire on a Pt gauze under N2sparging gave a dark green solution after passage of 230 C. The CH3CN solvent was allowed to evaporate, and the green residue was extracted with CH2Cl2. Storage of the solution at −45 °C overnight gave 0.85 g (51% yield) of green microcrystalline [Mn(IV)(dtbsalpn)]2DCBI+PF6-. Anal. Found (calcd): C, 60.5 (60.1); H, 7.1(7.0); N, 5.6 (5.9); Mn, 7.3(7.8). IR: νCO1710 cm-1, νCN1603 cm-1. Visible: λmax682 nm, ε = 9500 M-1cm-1. χm= 5.4 μB(298 K). Vapor diffusion of benzene into an acetonitrile solution of [Mn(IV)(dtbsalpn)]2DCBI+PF6-yielded dark-green X-ray quality crystals with three benzene and two acetonitrile molecules of crystallization (Mn2C93F6H121N8O8P, orthorhombic, space groupPbca,a= 21.0211(3),b= 26.8006(2), andc= 32.6466(6) Å, α = β = γ = 90°,V= 18392.4(4) Å3,Z= 8. X-ray diffraction data was collected on a Siemens SMART CCD diffractometer and refined with full-matrix least-squares onF2using 21 826 independent reflections (R= 0.1188, GOF = 1.179).
10.1021/ja00367a014 / J. Am. Chem. Soc. by Kolks G. (1982)
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10.1021/ja00104a014 / J. Am. Chem. Soc. by Baldwin M. J. (1994)
10.1021/ja00052a044 / J. Am. Chem. Soc. by Kirk M. L. (1992)

Dates

Type	When
Created	23 years, 1 month ago (July 26, 2002, 1:09 a.m.)
Deposited	3 years, 11 months ago (Sept. 23, 2021, 12:45 a.m.)
Indexed	1 year, 7 months ago (Jan. 18, 2024, 1:24 p.m.)
Issued	27 years, 10 months ago (Oct. 1, 1997)
Published	27 years, 10 months ago (Oct. 1, 1997)
Published Online	27 years, 10 months ago (Oct. 1, 1997)
Published Print	27 years, 10 months ago (Oct. 1, 1997)

Funders 0

None

BibTeX

@article{Caudle_1997, title={The First Binuclear Mn(IV) Complex Containing a Bridging Imidazolate Ligand Exhibits Unique EPR Spectral Features}, volume={119}, ISSN={1520-5126}, url={http://dx.doi.org/10.1021/ja9715197}, DOI={10.1021/ja9715197}, number={39}, journal={Journal of the American Chemical Society}, publisher={American Chemical Society (ACS)}, author={Caudle, M. Tyler and Kampf, Jeff W. and Kirk, Martin L. and Rasmussen, Paul G. and Pecoraro, Vincent L.}, year={1997}, month=oct, pages={9297–9298} }

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      "unstructured": "The preparation and characterization of the [Mn(III)(dtbsalpn)]2HDCBI precursor will be detailed in a subsequent full paper. [Mn(III)(dtbsalpn)]2HDCBI (1.5 g, 1.2 mmol) was slurried in 120 mL of distilled CH3CN containing 0.10 M tetrabutylammonium hexafluorophosphate and was carefully reacted with 1 equiv of tetrabutylammonium hydroxide under anaerobic conditions. Bulk electrolysis of the solution at 500 mVvsAg wire on a Pt gauze under N2sparging gave a dark green solution after passage of 230 C. The CH3CN solvent was allowed to evaporate, and the green residue was extracted with CH2Cl2. Storage of the solution at \u221245 \u00b0C overnight gave 0.85 g (51% yield) of green microcrystalline [Mn(IV)(dtbsalpn)]2DCBI+PF6-. Anal. Found (calcd): C, 60.5 (60.1); H, 7.1(7.0); N, 5.6 (5.9); Mn, 7.3(7.8). IR:\u2009 \u03bdCO1710 cm-1, \u03bdCN1603 cm-1. Visible:\u2009 \u03bbmax682 nm, \u03b5 = 9500 M-1cm-1. \u03c7m= 5.4 \u03bcB(298 K). Vapor diffusion of benzene into an acetonitrile solution of [Mn(IV)(dtbsalpn)]2DCBI+PF6-yielded dark-green X-ray quality crystals with three benzene and two acetonitrile molecules of crystallization (Mn2C93F6H121N8O8P, orthorhombic, space groupPbca,a= 21.0211(3),b= 26.8006(2), andc= 32.6466(6) \u00c5, \u03b1 = \u03b2 = \u03b3 = 90\u00b0,V= 18392.4(4) \u00c53,Z= 8. X-ray diffraction data was collected on a Siemens SMART CCD diffractometer and refined with full-matrix least-squares onF2using 21\u2009826 independent reflections (R= 0.1188, GOF = 1.179)."
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