Structure and Vibrational Spectra of Pyridine Solvated Solid Bis(Pyridine)silver(I) Perchlorate, [Agpy<sub>2</sub>ClO<sub>4</sub>]·0.5py
A hemipyridine solvate of bis(pyridine)silver(I) perchlorate, [Agpy<sub>2</sub>ClO<sub>4</sub>]·0.5py (compound <b>1</b>) was prepared and characterized by single crystal X-ray analysis and vibrational spectroscopy (R and low-temperature Raman). Compound <b>...
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MDPI AG
2022-08-01
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| Series: | Inorganics |
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| Online Access: | https://www.mdpi.com/2304-6740/10/9/123 |
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| author | Nóra V. May Niloofar Bayat Kende Attila Béres Petra Bombicz Vladimir M. Petruševski György Lendvay Attila Farkas László Kótai |
| author_facet | Nóra V. May Niloofar Bayat Kende Attila Béres Petra Bombicz Vladimir M. Petruševski György Lendvay Attila Farkas László Kótai |
| author_sort | Nóra V. May |
| collection | DOAJ |
| description | A hemipyridine solvate of bis(pyridine)silver(I) perchlorate, [Agpy<sub>2</sub>ClO<sub>4</sub>]·0.5py (compound <b>1</b>) was prepared and characterized by single crystal X-ray analysis and vibrational spectroscopy (R and low-temperature Raman). Compound <b>1</b> was prepared via the trituration of [Agpy<sub>2</sub>ClO<sub>4</sub>] and 4[Agpy<sub>2</sub>ClO<sub>4</sub>]·[Agpy<sub>4</sub>]ClO<sub>4</sub> (as the source of the solvate pyridine) in a mixed solvent of acetone:benzene =1:1 (v = v) at room temperature. The monoclinic crystals of compound <b>1</b> were found to be isomorphic with the analogous permanganate complex (a = 19.1093(16) Å, b = 7.7016(8) Å, c = 20.6915(19) Å, β = 105.515(7)°; space group: C2/c). Two [Agpy<sub>2</sub>]<sup>+</sup> cations formed a dimeric unit [Agpy<sub>2</sub>ClO<sub>4</sub>]<sub>2</sub>, and each silver ion was connected to two ClO<sub>4</sub><sup>−</sup> anions via oxygen atoms. The Ag∙∙∙Ag distance was 3.3873(5) Å, the perchlorate ions were coordinated to silver ions, and the Ag∙∙∙O distances were 2.840(2) Å and 2.8749(16) Å in the centrosymmetric rectangle of Ag-O-Ag-O. The stoichiometric ratio of the monomer [Agpy<sub>2</sub>ClO<sub>4</sub>] and the solvent pyridine was 1:0.5. The guest pyridine occupied 527.2 Å<sup>3</sup>, which was 18.0% of the volume of the unit cell. There was no additional residual solvent-accessible void in the crystal lattice. The solvate pyridine was connected via its a-CH to one of the O atoms of the perchlorate anion. Correlation analysis, as well as IR and low-temperature Raman studies, were performed to assign all perchlorate and pyridine vibrational modes. The solvate and coordinated pyridine bands in the IR and Raman spectra were not distinguishable. A perchlorate contribution via Ag-O coordination to low-frequency Raman bands was also assigned. |
| first_indexed | 2024-03-09T23:39:41Z |
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| spelling | doaj.art-28fcca97784c4a188e11e334c98be3f42023-11-23T16:53:53ZengMDPI AGInorganics2304-67402022-08-0110912310.3390/inorganics10090123Structure and Vibrational Spectra of Pyridine Solvated Solid Bis(Pyridine)silver(I) Perchlorate, [Agpy<sub>2</sub>ClO<sub>4</sub>]·0.5pyNóra V. May0Niloofar Bayat1Kende Attila Béres2Petra Bombicz3Vladimir M. Petruševski4György Lendvay5Attila Farkas6László Kótai7Research Centre for Natural Sciences, Hungarian Academy of Sciences, Magyar Tudósok krt. 2., 1117 Budapest, HungaryResearch Centre for Natural Sciences, Hungarian Academy of Sciences, Magyar Tudósok krt. 2., 1117 Budapest, HungaryResearch Centre for Natural Sciences, Hungarian Academy of Sciences, Magyar Tudósok krt. 2., 1117 Budapest, HungaryResearch Centre for Natural Sciences, Hungarian Academy of Sciences, Magyar Tudósok krt. 2., 1117 Budapest, HungaryFaculty of Natural Sciences and Mathematics, Ss. Cyril and Methodius University, 1000 Skopje, North MacedoniaResearch Centre for Natural Sciences, Hungarian Academy of Sciences, Magyar Tudósok krt. 2., 1117 Budapest, HungaryDepartment of Organic Chemistry and Technology, Budapest University of Technology and Economics, Műegyetem rkp. 3., 1111 Budapest, HungaryResearch Centre for Natural Sciences, Hungarian Academy of Sciences, Magyar Tudósok krt. 2., 1117 Budapest, HungaryA hemipyridine solvate of bis(pyridine)silver(I) perchlorate, [Agpy<sub>2</sub>ClO<sub>4</sub>]·0.5py (compound <b>1</b>) was prepared and characterized by single crystal X-ray analysis and vibrational spectroscopy (R and low-temperature Raman). Compound <b>1</b> was prepared via the trituration of [Agpy<sub>2</sub>ClO<sub>4</sub>] and 4[Agpy<sub>2</sub>ClO<sub>4</sub>]·[Agpy<sub>4</sub>]ClO<sub>4</sub> (as the source of the solvate pyridine) in a mixed solvent of acetone:benzene =1:1 (v = v) at room temperature. The monoclinic crystals of compound <b>1</b> were found to be isomorphic with the analogous permanganate complex (a = 19.1093(16) Å, b = 7.7016(8) Å, c = 20.6915(19) Å, β = 105.515(7)°; space group: C2/c). Two [Agpy<sub>2</sub>]<sup>+</sup> cations formed a dimeric unit [Agpy<sub>2</sub>ClO<sub>4</sub>]<sub>2</sub>, and each silver ion was connected to two ClO<sub>4</sub><sup>−</sup> anions via oxygen atoms. The Ag∙∙∙Ag distance was 3.3873(5) Å, the perchlorate ions were coordinated to silver ions, and the Ag∙∙∙O distances were 2.840(2) Å and 2.8749(16) Å in the centrosymmetric rectangle of Ag-O-Ag-O. The stoichiometric ratio of the monomer [Agpy<sub>2</sub>ClO<sub>4</sub>] and the solvent pyridine was 1:0.5. The guest pyridine occupied 527.2 Å<sup>3</sup>, which was 18.0% of the volume of the unit cell. There was no additional residual solvent-accessible void in the crystal lattice. The solvate pyridine was connected via its a-CH to one of the O atoms of the perchlorate anion. Correlation analysis, as well as IR and low-temperature Raman studies, were performed to assign all perchlorate and pyridine vibrational modes. The solvate and coordinated pyridine bands in the IR and Raman spectra were not distinguishable. A perchlorate contribution via Ag-O coordination to low-frequency Raman bands was also assigned.https://www.mdpi.com/2304-6740/10/9/123pyridine complexessilver perchloratevibrational spectroscopysingle crystal structurehydrogen bond |
| spellingShingle | Nóra V. May Niloofar Bayat Kende Attila Béres Petra Bombicz Vladimir M. Petruševski György Lendvay Attila Farkas László Kótai Structure and Vibrational Spectra of Pyridine Solvated Solid Bis(Pyridine)silver(I) Perchlorate, [Agpy<sub>2</sub>ClO<sub>4</sub>]·0.5py Inorganics pyridine complexes silver perchlorate vibrational spectroscopy single crystal structure hydrogen bond |
| title | Structure and Vibrational Spectra of Pyridine Solvated Solid Bis(Pyridine)silver(I) Perchlorate, [Agpy<sub>2</sub>ClO<sub>4</sub>]·0.5py |
| title_full | Structure and Vibrational Spectra of Pyridine Solvated Solid Bis(Pyridine)silver(I) Perchlorate, [Agpy<sub>2</sub>ClO<sub>4</sub>]·0.5py |
| title_fullStr | Structure and Vibrational Spectra of Pyridine Solvated Solid Bis(Pyridine)silver(I) Perchlorate, [Agpy<sub>2</sub>ClO<sub>4</sub>]·0.5py |
| title_full_unstemmed | Structure and Vibrational Spectra of Pyridine Solvated Solid Bis(Pyridine)silver(I) Perchlorate, [Agpy<sub>2</sub>ClO<sub>4</sub>]·0.5py |
| title_short | Structure and Vibrational Spectra of Pyridine Solvated Solid Bis(Pyridine)silver(I) Perchlorate, [Agpy<sub>2</sub>ClO<sub>4</sub>]·0.5py |
| title_sort | structure and vibrational spectra of pyridine solvated solid bis pyridine silver i perchlorate agpy sub 2 sub clo sub 4 sub ·0 5py |
| topic | pyridine complexes silver perchlorate vibrational spectroscopy single crystal structure hydrogen bond |
| url | https://www.mdpi.com/2304-6740/10/9/123 |
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