Crystal structure of μ3-tetrathioantimonato-tris[(cyclam)zinc(II)] tetrathioantimonate acetonitrile disolvate dihydrate showing Zn disorder over the cyclam ring planes (cyclam = 1,4,8,11-tetraazacyclotetradecane)
Reaction of Zn(ClO4)2·6H2O with cyclam (cyclam = 1,4,8,11-tetraazacyclotetradecane, C10H24N4) and Na3SbS4 in an acetonitrile/water mixture led to the formation of crystals of the title compound, [Zn3(SbS4)(C10H24N4)3](SbS4)·2CH3CN·2H2O or [(Zn-cyclam)3(SbS4)2](H2O)2(acetonitrile)2. The set-up of the...
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| Language: | English |
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International Union of Crystallography
2022-05-01
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| Series: | Acta Crystallographica Section E: Crystallographic Communications |
| Subjects: | |
| Online Access: | http://scripts.iucr.org/cgi-bin/paper?S2056989022003759 |
| _version_ | 1818029258242523136 |
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| author | Christian Näther Felix Danker Wolfgang Bensch |
| author_facet | Christian Näther Felix Danker Wolfgang Bensch |
| author_sort | Christian Näther |
| collection | DOAJ |
| description | Reaction of Zn(ClO4)2·6H2O with cyclam (cyclam = 1,4,8,11-tetraazacyclotetradecane, C10H24N4) and Na3SbS4 in an acetonitrile/water mixture led to the formation of crystals of the title compound, [Zn3(SbS4)(C10H24N4)3](SbS4)·2CH3CN·2H2O or [(Zn-cyclam)3(SbS4)2](H2O)2(acetonitrile)2. The set-up of the crystal structure is similar to that of [(Zn-cyclam)3(SbS4)2].8H2O reported recently [Danker et al. (2021). Dalton Trans. 50, 18107–18117]. The crystal structure of the title compound consists of three crystallographically independent ZnII cations (each disordered around centers of inversion), three centrosymmetric cyclam ligands, one SbS43– anion, one water and one acetonitrile molecule occupying general positions. The acetonitrile molecule is equally disordered over two sets of sites. Each Zn2+ cation is bound to four nitrogen atoms of a cyclam ligand and one sulfur atom of the SbS43– anion within a distorted square-pyramidal coordination. The cation disorder of the [Zn(cyclam)]2+ complexes is discussed in detail and is also observed in other compounds, where identical ligands are located above and below the [Zn(cyclam)]2+ plane. In the title compound, the building units are arranged in layers parallel to the bc plane forming pores in which the acetonitrile solvate molecules are located. Intermolecular C—H...S hydrogen bonding links these units to the SbS43– anions. Between the layers, additional water solvate molecules are present that act as acceptor and donor groups for intermolecular N—H...O and O—H...S hydrogen bonding. |
| first_indexed | 2024-12-10T05:16:50Z |
| format | Article |
| id | doaj.art-38c2b60cdfec457a8cb60a672d4c5c7b |
| institution | Directory Open Access Journal |
| issn | 2056-9890 |
| language | English |
| last_indexed | 2024-12-10T05:16:50Z |
| publishDate | 2022-05-01 |
| publisher | International Union of Crystallography |
| record_format | Article |
| series | Acta Crystallographica Section E: Crystallographic Communications |
| spelling | doaj.art-38c2b60cdfec457a8cb60a672d4c5c7b2022-12-22T02:00:56ZengInternational Union of CrystallographyActa Crystallographica Section E: Crystallographic Communications2056-98902022-05-0178549049510.1107/S2056989022003759wm5639Crystal structure of μ3-tetrathioantimonato-tris[(cyclam)zinc(II)] tetrathioantimonate acetonitrile disolvate dihydrate showing Zn disorder over the cyclam ring planes (cyclam = 1,4,8,11-tetraazacyclotetradecane)Christian Näther0Felix Danker1Wolfgang Bensch2Institut für Anorganische Chemie, Universität Kiel, Max-Eyth. Str. 2, 241128 Kiel, GermanyInstitut für Anorganische Chemie, Universität Kiel, Max-Eyth. Str. 2, 241128 Kiel, GermanyInstitut für Anorganische Chemie, Universität Kiel, Max-Eyth. Str. 2, 241128 Kiel, GermanyReaction of Zn(ClO4)2·6H2O with cyclam (cyclam = 1,4,8,11-tetraazacyclotetradecane, C10H24N4) and Na3SbS4 in an acetonitrile/water mixture led to the formation of crystals of the title compound, [Zn3(SbS4)(C10H24N4)3](SbS4)·2CH3CN·2H2O or [(Zn-cyclam)3(SbS4)2](H2O)2(acetonitrile)2. The set-up of the crystal structure is similar to that of [(Zn-cyclam)3(SbS4)2].8H2O reported recently [Danker et al. (2021). Dalton Trans. 50, 18107–18117]. The crystal structure of the title compound consists of three crystallographically independent ZnII cations (each disordered around centers of inversion), three centrosymmetric cyclam ligands, one SbS43– anion, one water and one acetonitrile molecule occupying general positions. The acetonitrile molecule is equally disordered over two sets of sites. Each Zn2+ cation is bound to four nitrogen atoms of a cyclam ligand and one sulfur atom of the SbS43– anion within a distorted square-pyramidal coordination. The cation disorder of the [Zn(cyclam)]2+ complexes is discussed in detail and is also observed in other compounds, where identical ligands are located above and below the [Zn(cyclam)]2+ plane. In the title compound, the building units are arranged in layers parallel to the bc plane forming pores in which the acetonitrile solvate molecules are located. Intermolecular C—H...S hydrogen bonding links these units to the SbS43– anions. Between the layers, additional water solvate molecules are present that act as acceptor and donor groups for intermolecular N—H...O and O—H...S hydrogen bonding.http://scripts.iucr.org/cgi-bin/paper?S2056989022003759crystal structurezn-thioantimonatecation disorderhydrogen bonding |
| spellingShingle | Christian Näther Felix Danker Wolfgang Bensch Crystal structure of μ3-tetrathioantimonato-tris[(cyclam)zinc(II)] tetrathioantimonate acetonitrile disolvate dihydrate showing Zn disorder over the cyclam ring planes (cyclam = 1,4,8,11-tetraazacyclotetradecane) Acta Crystallographica Section E: Crystallographic Communications crystal structure zn-thioantimonate cation disorder hydrogen bonding |
| title | Crystal structure of μ3-tetrathioantimonato-tris[(cyclam)zinc(II)] tetrathioantimonate acetonitrile disolvate dihydrate showing Zn disorder over the cyclam ring planes (cyclam = 1,4,8,11-tetraazacyclotetradecane) |
| title_full | Crystal structure of μ3-tetrathioantimonato-tris[(cyclam)zinc(II)] tetrathioantimonate acetonitrile disolvate dihydrate showing Zn disorder over the cyclam ring planes (cyclam = 1,4,8,11-tetraazacyclotetradecane) |
| title_fullStr | Crystal structure of μ3-tetrathioantimonato-tris[(cyclam)zinc(II)] tetrathioantimonate acetonitrile disolvate dihydrate showing Zn disorder over the cyclam ring planes (cyclam = 1,4,8,11-tetraazacyclotetradecane) |
| title_full_unstemmed | Crystal structure of μ3-tetrathioantimonato-tris[(cyclam)zinc(II)] tetrathioantimonate acetonitrile disolvate dihydrate showing Zn disorder over the cyclam ring planes (cyclam = 1,4,8,11-tetraazacyclotetradecane) |
| title_short | Crystal structure of μ3-tetrathioantimonato-tris[(cyclam)zinc(II)] tetrathioantimonate acetonitrile disolvate dihydrate showing Zn disorder over the cyclam ring planes (cyclam = 1,4,8,11-tetraazacyclotetradecane) |
| title_sort | crystal structure of μ3 tetrathioantimonato tris cyclam zinc ii tetrathioantimonate acetonitrile disolvate dihydrate showing zn disorder over the cyclam ring planes cyclam 1 4 8 11 tetraazacyclotetradecane |
| topic | crystal structure zn-thioantimonate cation disorder hydrogen bonding |
| url | http://scripts.iucr.org/cgi-bin/paper?S2056989022003759 |
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