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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...
Autores principales: | , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
International Union of Crystallography
2020
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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. |
format | Online Article Text |
id | pubmed-7057377 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2020 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
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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