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Title: Cyanate groups in higher oxidation state metal cluster chemistry: Mixed-valence (II/III) Mn16 and Mn18 clusters

Abstract

Here, the employment of cyanato (OCN-) group in high oxidation state manganese cluster chemistry, in conjunction with carboxylate ions and the organic chelating/bridging ligand 2-(hydroxymethyl)pyridine (hmpH), is reported. The syntheses, crystal structures, and magnetochemical characterization are described for [Mn16O8(OR)4(OCN)4(O2CMe)12(hmp)6(ROH)2] (R = Me (1), Et (2)) and [Mn18O14(O2CR)18(hmp)4(hmpH)2(H2O)2] (R = Me (3), Et (4)). The 2:1:1:1 reactions of Mn(O2CMe)2·4H2O, hmpH, NaOCN and NEt3 in solvent MeOH or EtOH afford the isostructural complexes [Mn16O8(OR)4(OCN)4(O2CMe)12(hmp)6(ROH)2] (R = Me (1), Et (2)). The [Mn16(μ4-O)4(μ3-O)4(μ-OMe)4(μ3-OR)6(μ-OR)6]10+ core of representative complex 1 comprises a MnII4MnIII4 double-cubane subunit attached on either side to two symmetry-related MnIIMnIII3 defective dicubanes. A similar reaction of Mn(O2CR)2·4H2O, hmpH, NaOCN and NEt3, but in solvent MeCN, led instead to the formation of [Mn18O14(O2CR)18(hmp)4(hmpH)2(H2O)2] (R = Me (3), Et (4)). Compounds 3 and 4 are very similar to each other and can be described as a central [MnIII4(μ-O)6] rodlike subunit attached on either side to two symmetry-related [Mn7O9] subunits. Variable-temperature, solid-state dc and ac magnetic susceptibility studies revealed the presence of predominant antiferromagnetic exchange interactions in all compounds, and possible S = 2 or 1 (for 1 and 2) and S = 0 (for 3 and 4) ground state spin values. The combined resultsmore » demonstrate the ability of cyanato groups to facilitate the formation of new polynuclear MnII/III complexes with structures different than these obtained from the use of the related azides.« less

Authors:
 [1];  [2];  [3];  [4];  [4];  [2];  [5];  [1]
+ Show Author Affiliations
  1. Brock Univ., St. Catharines, ON (Canada). Dept. of Chemistry
  2. Univ. of Cyprus, Nicosia (Cyprus). Dept. of Chemistry
  3. Univ. of Cyprus, Nicosia (Cyprus). Dept. of Chemistry; Univ. of Florida, Gainesville, FL (United States). Dept. of Chemistry
  4. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source (ALS)
  5. Univ. of Florida, Gainesville, FL (United States). Dept. of Chemistry
Publication Date:
Research Org.:
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES); Brock Univ., St. Catharines, ON (Canada); Natural Sciences and Engineering Research Council of Canada (NSERC); European Research Area (ERA); Ontario Trillium Foundation; National Science Foundation (NSF)
OSTI Identifier:
1439196
Alternate Identifier(s):
OSTI ID: 1250199
Grant/Contract Number:  
AC02-05CH11231; DMR-1213030
Resource Type:
Accepted Manuscript
Journal Name:
Polyhedron
Additional Journal Information:
Journal Volume: 108; Journal Issue: C; Related Information: © 2015 Elsevier Ltd. All rights reserved.; Journal ID: ISSN 0277-5387
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Manganese; Cyanates; 2-(Hydroxymethyl)pyridine; Crystal structures; Magnetism

Citation Formats

Alexandropoulos, Dimitris I., Moushi, Eleni E., Papatriantafyllopoulou, Constantina, Beavers, Christine M., Teat, Simon J., Tasiopoulos, Anastasios J., Christou, George, and Stamatatos, Theocharis C. Cyanate groups in higher oxidation state metal cluster chemistry: Mixed-valence (II/III) Mn16 and Mn18 clusters. United States: N. p., 2015. Web. doi:10.1016/j.poly.2015.11.031.
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Alexandropoulos, Dimitris I., Moushi, Eleni E., Papatriantafyllopoulou, Constantina, Beavers, Christine M., Teat, Simon J., Tasiopoulos, Anastasios J., Christou, George, & Stamatatos, Theocharis C. Cyanate groups in higher oxidation state metal cluster chemistry: Mixed-valence (II/III) Mn16 and Mn18 clusters. United States. https://doi.org/10.1016/j.poly.2015.11.031
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Alexandropoulos, Dimitris I., Moushi, Eleni E., Papatriantafyllopoulou, Constantina, Beavers, Christine M., Teat, Simon J., Tasiopoulos, Anastasios J., Christou, George, and Stamatatos, Theocharis C. Wed . "Cyanate groups in higher oxidation state metal cluster chemistry: Mixed-valence (II/III) Mn16 and Mn18 clusters". United States. https://doi.org/10.1016/j.poly.2015.11.031. https://www.osti.gov/servlets/purl/1439196.
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@article{osti_1439196,
title = {Cyanate groups in higher oxidation state metal cluster chemistry: Mixed-valence (II/III) Mn16 and Mn18 clusters},
author = {Alexandropoulos, Dimitris I. and Moushi, Eleni E. and Papatriantafyllopoulou, Constantina and Beavers, Christine M. and Teat, Simon J. and Tasiopoulos, Anastasios J. and Christou, George and Stamatatos, Theocharis C.},
abstractNote = {Here, the employment of cyanato (OCN-) group in high oxidation state manganese cluster chemistry, in conjunction with carboxylate ions and the organic chelating/bridging ligand 2-(hydroxymethyl)pyridine (hmpH), is reported. The syntheses, crystal structures, and magnetochemical characterization are described for [Mn16O8(OR)4(OCN)4(O2CMe)12(hmp)6(ROH)2] (R = Me (1), Et (2)) and [Mn18O14(O2CR)18(hmp)4(hmpH)2(H2O)2] (R = Me (3), Et (4)). The 2:1:1:1 reactions of Mn(O2CMe)2·4H2O, hmpH, NaOCN and NEt3 in solvent MeOH or EtOH afford the isostructural complexes [Mn16O8(OR)4(OCN)4(O2CMe)12(hmp)6(ROH)2] (R = Me (1), Et (2)). The [Mn16(μ4-O)4(μ3-O)4(μ-OMe)4(μ3-OR)6(μ-OR)6]10+ core of representative complex 1 comprises a MnII4MnIII4 double-cubane subunit attached on either side to two symmetry-related MnIIMnIII3 defective dicubanes. A similar reaction of Mn(O2CR)2·4H2O, hmpH, NaOCN and NEt3, but in solvent MeCN, led instead to the formation of [Mn18O14(O2CR)18(hmp)4(hmpH)2(H2O)2] (R = Me (3), Et (4)). Compounds 3 and 4 are very similar to each other and can be described as a central [MnIII4(μ-O)6] rodlike subunit attached on either side to two symmetry-related [Mn7O9] subunits. Variable-temperature, solid-state dc and ac magnetic susceptibility studies revealed the presence of predominant antiferromagnetic exchange interactions in all compounds, and possible S = 2 or 1 (for 1 and 2) and S = 0 (for 3 and 4) ground state spin values. The combined results demonstrate the ability of cyanato groups to facilitate the formation of new polynuclear MnII/III complexes with structures different than these obtained from the use of the related azides.},
doi = {10.1016/j.poly.2015.11.031},
journal = {Polyhedron},
number = C,
volume = 108,
place = {United States},
year = {Wed Dec 02 00:00:00 EST 2015},
month = {Wed Dec 02 00:00:00 EST 2015}
}
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