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Title: Electronic Structure and Magnetic Properties of a Titanium(II) Coordination Complex

Abstract

Stable coordination complexes of TiII (3d2) are relatively uncommon, but are of interest as synthons for low oxidation state titanium complexes for application as potential catalysts and reagents for organic synthesis. Specifically, high-spin TiII ions supported by redox-inactive ligands are still quite rare due to the reducing power of this soft ion. Among such TiII complexes is trans-[TiCl2(tmeda)2], where tmeda = N,N,N',N'-tetramethylethane-1,2-diamine. This complex was first reported by Gambarotta and co-workers almost 30 years ago, but it was not spectroscopically characterized and theoretical investigation by quantum chemical theory (QCT) was not feasible at that time. As part of our interest in low oxidation state early transition metal complexes, we have revisited this complex and report a modified synthesis and a low temperature (100 K) crystal structure that differs slightly from that originally reported at ambient temperature. We have used magnetometry, high-frequency and -field EPR (HFEPR), and variable-temperature variable-field magnetic circular dichroism (VTVH-MCD) spectroscopies to characterize trans-[TiCl2(tmeda)2]. These techniques yield the following S = 1 spin Hamiltonian parameters for the complex: D = -5.23(1) cm–1, E = -0.88(1) cm–1, (E/D = 0.17), g = [1.86(1), 1.94(2), 1.77(1)]. This information, in combination with electronic transitions from MCD, was used as input formore » both classical ligand-field theory (LFT) and detailed QCT studies, the latter including both density functional theory (DFT) and ab initio methods. These computational methods are seldom applied to paramagnetic early transition metal complexes, particularly those with S > 1/2. Our studies provide a complete picture of the electronic structure of this complex that can be put into context with the few other high-spin and mononuclear TiII species characterized to date.« less

Authors:
 [1]; ORCiD logo [2]; ORCiD logo [2]; ORCiD logo [3]; ORCiD logo [1]; ORCiD logo [1]; ORCiD logo [4]; ORCiD logo [4]; ORCiD logo [5]; ORCiD logo [6]
+ Show Author Affiliations
  1. Department of Chemistry and Pharmacy, Inorganic Chemistry, Friedrich-Alexander University Erlangen-Nürnberg (FAU), 91058 Erlangen, Germany
  2. Department of Chemistry, University of Kansas, 1567 Irving Hill Road, Lawrence, Kansas 66045, United States
  3. Department of Chemistry and Molecular Structure Center, Indiana University, Bloomington, Indiana 47405, United States
  4. National High Magnetic Field Laboratory, Florida State University, Tallahassee, Florida 32310, United States
  5. Department of Chemistry, University of Pennsylvania, Philadelphia, Pennsylvania 19104, United States
  6. Department of Biological, Physical and Health Sciences, Roosevelt University, Chicago, Illinois 60605, United States
Publication Date:
Research Org.:
Indiana Univ., Bloomington, IN (United States); Roosevelt Univ., Chicago, IL (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences, and Biosciences Division; National Science Foundation (NSF)
OSTI Identifier:
1614801
Alternate Identifier(s):
OSTI ID: 1617124
Grant/Contract Number:  
FG02-07ER15893; CHE-1565661; CHE-1900384; DMR-1644779
Resource Type:
Published Article
Journal Name:
Inorganic Chemistry
Additional Journal Information:
Journal Name: Inorganic Chemistry Journal Volume: 59 Journal Issue: 9; 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

Zolnhofer, Eva M., Wijeratne, Gayan B., Jackson, Timothy A., Fortier, Skye, Heinemann, Frank W., Meyer, Karsten, Krzystek, J., Ozarowski, Andrew, Mindiola, Daniel J., and Telser, Joshua. Electronic Structure and Magnetic Properties of a Titanium(II) Coordination Complex. United States: N. p., 2020. Web. doi:10.1021/acs.inorgchem.0c00311.
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Zolnhofer, Eva M., Wijeratne, Gayan B., Jackson, Timothy A., Fortier, Skye, Heinemann, Frank W., Meyer, Karsten, Krzystek, J., Ozarowski, Andrew, Mindiola, Daniel J., & Telser, Joshua. Electronic Structure and Magnetic Properties of a Titanium(II) Coordination Complex. United States. https://doi.org/10.1021/acs.inorgchem.0c00311
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Zolnhofer, Eva M., Wijeratne, Gayan B., Jackson, Timothy A., Fortier, Skye, Heinemann, Frank W., Meyer, Karsten, Krzystek, J., Ozarowski, Andrew, Mindiola, Daniel J., and Telser, Joshua. Sat . "Electronic Structure and Magnetic Properties of a Titanium(II) Coordination Complex". United States. https://doi.org/10.1021/acs.inorgchem.0c00311.
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@article{osti_1614801,
title = {Electronic Structure and Magnetic Properties of a Titanium(II) Coordination Complex},
author = {Zolnhofer, Eva M. and Wijeratne, Gayan B. and Jackson, Timothy A. and Fortier, Skye and Heinemann, Frank W. and Meyer, Karsten and Krzystek, J. and Ozarowski, Andrew and Mindiola, Daniel J. and Telser, Joshua},
abstractNote = {Stable coordination complexes of TiII (3d2) are relatively uncommon, but are of interest as synthons for low oxidation state titanium complexes for application as potential catalysts and reagents for organic synthesis. Specifically, high-spin TiII ions supported by redox-inactive ligands are still quite rare due to the reducing power of this soft ion. Among such TiII complexes is trans-[TiCl2(tmeda)2], where tmeda = N,N,N',N'-tetramethylethane-1,2-diamine. This complex was first reported by Gambarotta and co-workers almost 30 years ago, but it was not spectroscopically characterized and theoretical investigation by quantum chemical theory (QCT) was not feasible at that time. As part of our interest in low oxidation state early transition metal complexes, we have revisited this complex and report a modified synthesis and a low temperature (100 K) crystal structure that differs slightly from that originally reported at ambient temperature. We have used magnetometry, high-frequency and -field EPR (HFEPR), and variable-temperature variable-field magnetic circular dichroism (VTVH-MCD) spectroscopies to characterize trans-[TiCl2(tmeda)2]. These techniques yield the following S = 1 spin Hamiltonian parameters for the complex: D = -5.23(1) cm–1, E = -0.88(1) cm–1, (E/D = 0.17), g = [1.86(1), 1.94(2), 1.77(1)]. This information, in combination with electronic transitions from MCD, was used as input for both classical ligand-field theory (LFT) and detailed QCT studies, the latter including both density functional theory (DFT) and ab initio methods. These computational methods are seldom applied to paramagnetic early transition metal complexes, particularly those with S > 1/2. Our studies provide a complete picture of the electronic structure of this complex that can be put into context with the few other high-spin and mononuclear TiII species characterized to date.},
doi = {10.1021/acs.inorgchem.0c00311},
journal = {Inorganic Chemistry},
number = 9,
volume = 59,
place = {United States},
year = {Sat Apr 11 00:00:00 EDT 2020},
month = {Sat Apr 11 00:00:00 EDT 2020}
}
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