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Synthesis and crystal structure of (1,4,7,10-tetra­aza­cyclo­dodecane-κ(4) N)(tetra­sulfido-κ(2) S (1),S (4))manganese(II)

The title compound, [Mn(S(4))(C(8)H(20)N(4))], was accidentally obtained by the hydro­thermal reaction of Mn(ClO(4))(2)·6H(2)O, cyclen (cyclen = 1,4,7,10-tetra­aza­cyclo­dodeca­ne) and Na(3)SbS(4)·9H(2)O in water at 413 K, indicating that polysulfide anions might represent inter­mediates in the synt...

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Detalles Bibliográficos
Autores principales: Danker, Felix, Näther, Christian, Bensch, Wolfgang
Formato: Online Artículo Texto
Lenguaje:English
Publicado: International Union of Crystallography 2020
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7057377/
https://www.ncbi.nlm.nih.gov/pubmed/32148894
http://dx.doi.org/10.1107/S2056989020002492
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author Danker, Felix
Näther, Christian
Bensch, Wolfgang
author_facet Danker, Felix
Näther, Christian
Bensch, Wolfgang
author_sort Danker, Felix
collection PubMed
description The title compound, [Mn(S(4))(C(8)H(20)N(4))], was accidentally obtained by the hydro­thermal reaction of Mn(ClO(4))(2)·6H(2)O, cyclen (cyclen = 1,4,7,10-tetra­aza­cyclo­dodeca­ne) and Na(3)SbS(4)·9H(2)O in water at 413 K, indicating that polysulfide anions might represent inter­mediates in the synthesis of thio­metallate compounds using Na(3)SbS(4)·9H(2)O as a reactant. X-ray powder diffraction proves that the sample is slightly contaminated with NaSb(OH)(6) and an unknown crystalline phase. The crystal investigated was twinned with a twofold rotation axis as the twin element, and therefore a twin refinement using data in HKLF-5 format was performed. The asymmetric unit of the title compound consists of one Mn(II) cation, one [S(4)](2−) anion and one cyclen ligand in general positions. The Mn(II) cation is sixfold coordinated by two cis-S atoms of the [S(4)](2−) anions, as well as four N atoms of the cyclen ligand within an irregular coordination. The complexes are linked via pairs of N—H⋯S hydrogen bonds into chains, which are further linked into layers by additional N—H⋯S hydrogen bonding. These layers are connected into a three-dimensional network by inter­molecular N—H⋯S and C—H⋯S hydrogen bonding. It is noted that only one similar complex with Mn(II) is reported in the literature.
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spelling pubmed-70573772020-03-06 Synthesis and crystal structure of (1,4,7,10-tetra­aza­cyclo­dodecane-κ(4) N)(tetra­sulfido-κ(2) S (1),S (4))manganese(II) Danker, Felix Näther, Christian Bensch, Wolfgang Acta Crystallogr E Crystallogr Commun Research Communications The title compound, [Mn(S(4))(C(8)H(20)N(4))], was accidentally obtained by the hydro­thermal reaction of Mn(ClO(4))(2)·6H(2)O, cyclen (cyclen = 1,4,7,10-tetra­aza­cyclo­dodeca­ne) and Na(3)SbS(4)·9H(2)O in water at 413 K, indicating that polysulfide anions might represent inter­mediates in the synthesis of thio­metallate compounds using Na(3)SbS(4)·9H(2)O as a reactant. X-ray powder diffraction proves that the sample is slightly contaminated with NaSb(OH)(6) and an unknown crystalline phase. The crystal investigated was twinned with a twofold rotation axis as the twin element, and therefore a twin refinement using data in HKLF-5 format was performed. The asymmetric unit of the title compound consists of one Mn(II) cation, one [S(4)](2−) anion and one cyclen ligand in general positions. The Mn(II) cation is sixfold coordinated by two cis-S atoms of the [S(4)](2−) anions, as well as four N atoms of the cyclen ligand within an irregular coordination. The complexes are linked via pairs of N—H⋯S hydrogen bonds into chains, which are further linked into layers by additional N—H⋯S hydrogen bonding. These layers are connected into a three-dimensional network by inter­molecular N—H⋯S and C—H⋯S hydrogen bonding. It is noted that only one similar complex with Mn(II) is reported in the literature. International Union of Crystallography 2020-02-28 /pmc/articles/PMC7057377/ /pubmed/32148894 http://dx.doi.org/10.1107/S2056989020002492 Text en © Danker et al. 2020 http://creativecommons.org/licenses/by/4.0/ This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.http://creativecommons.org/licenses/by/4.0/
spellingShingle Research Communications
Danker, Felix
Näther, Christian
Bensch, Wolfgang
Synthesis and crystal structure of (1,4,7,10-tetra­aza­cyclo­dodecane-κ(4) N)(tetra­sulfido-κ(2) S (1),S (4))manganese(II)
title Synthesis and crystal structure of (1,4,7,10-tetra­aza­cyclo­dodecane-κ(4) N)(tetra­sulfido-κ(2) S (1),S (4))manganese(II)
title_full Synthesis and crystal structure of (1,4,7,10-tetra­aza­cyclo­dodecane-κ(4) N)(tetra­sulfido-κ(2) S (1),S (4))manganese(II)
title_fullStr Synthesis and crystal structure of (1,4,7,10-tetra­aza­cyclo­dodecane-κ(4) N)(tetra­sulfido-κ(2) S (1),S (4))manganese(II)
title_full_unstemmed Synthesis and crystal structure of (1,4,7,10-tetra­aza­cyclo­dodecane-κ(4) N)(tetra­sulfido-κ(2) S (1),S (4))manganese(II)
title_short Synthesis and crystal structure of (1,4,7,10-tetra­aza­cyclo­dodecane-κ(4) N)(tetra­sulfido-κ(2) S (1),S (4))manganese(II)
title_sort synthesis and crystal structure of (1,4,7,10-tetra­aza­cyclo­dodecane-κ(4) n)(tetra­sulfido-κ(2) s (1),s (4))manganese(ii)
topic Research Communications
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7057377/
https://www.ncbi.nlm.nih.gov/pubmed/32148894
http://dx.doi.org/10.1107/S2056989020002492
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