Ionothermal Synthesis of Cadmium Coordination Polymers: Ionic Liquid Effects on the Synthesis, Structural, and Thermal Characterization

Ionothermal synthesis is a little used method for the preparation of coordination polymers. By this method, two cadmium compounds were synthesized, <b>1</b>, with formula Cd<sub>3</sub>(ox)F<sub>2</sub>(Ina)<sub>2</sub> (Ina = isonicotinate) and <b&...

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Main Authors: Iñigo PerezF, Edurne S. Larrea, Begoña Bazán, Gotzone Barandika, M. Karmele Urtiaga, Maria I. Arriortua
Format: Article
Language:English
Published: MDPI AG 2019-11-01
Series:Molecules
Subjects:
Online Access:https://www.mdpi.com/1420-3049/24/22/4059
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author Iñigo PerezF
Edurne S. Larrea
Begoña Bazán
Gotzone Barandika
M. Karmele Urtiaga
Maria I. Arriortua
author_facet Iñigo PerezF
Edurne S. Larrea
Begoña Bazán
Gotzone Barandika
M. Karmele Urtiaga
Maria I. Arriortua
author_sort Iñigo PerezF
collection DOAJ
description Ionothermal synthesis is a little used method for the preparation of coordination polymers. By this method, two cadmium compounds were synthesized, <b>1</b>, with formula Cd<sub>3</sub>(ox)F<sub>2</sub>(Ina)<sub>2</sub> (Ina = isonicotinate) and <b>2</b>, Cd(NO<sub>3</sub>)<sub>2</sub>(4,4&#8242;-Bpy) (4,4&#8242;-Bpy = 4,4&#8242;-Bipyridine). The modification of the reaction conditions has allowed to obtain <b>2</b> as a pure phase. The structure of both compounds was determined by a single-crystal X-ray diffraction. Compound <b>1</b> is isostructural to the previously reported Cd<sub>2</sub>Zn(ox)(OH)<sub>2</sub>(Ina)<sub>2</sub>. It crystallizes in the monoclinic space group P<i>2</i><sub>1</sub><i>/n</i> and present a three-dimensional (3D) network, built-up from [Cd<sub>3</sub>(ox)F<sub>2</sub>]<sub>n</sub><sup>2n+</sup> layers, linked by isonicotinate ligands. Crystals of <b>2</b> are formed by twins of two components which are rotated ca. 180&#176; to each other. This compound crystallizes in the triclinic P<i>-1</i> space group and its structure can be describe as a two-dimensional (2D) 4 connected <i>&#8216;sql&#8217;</i> net. The layers are composed by [Cd(NO<sub>3</sub>)<sub>2</sub>]<sub>n</sub> chains linked through 4,4&#8242;-Bpy ligands, and are pillared along the [011] direction. The thermal decomposition of <b>2</b> was studied by thermogravimetric and thermodiffractiometric techniques. The compound decomposes gradually starting from 160 &#176;C, and due to heating, the structure suffers slight reversible changes in the bond distances and angles.
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spelling doaj.art-c06fcd2349184d1e93840de0f91053462022-12-22T02:18:57ZengMDPI AGMolecules1420-30492019-11-012422405910.3390/molecules24224059molecules24224059Ionothermal Synthesis of Cadmium Coordination Polymers: Ionic Liquid Effects on the Synthesis, Structural, and Thermal CharacterizationIñigo PerezF0Edurne S. Larrea1Begoña Bazán2Gotzone Barandika3M. Karmele Urtiaga4Maria I. Arriortua5Dpto. Mineralogía y Petrología, Universidad del País Vasco, UPV/EHU, Sarriena s/n, 48940 Leioa, SpainDpto. Mineralogía y Petrología, Universidad del País Vasco, UPV/EHU, Sarriena s/n, 48940 Leioa, SpainDpto. Mineralogía y Petrología, Universidad del País Vasco, UPV/EHU, Sarriena s/n, 48940 Leioa, SpainBCMaterials (Basque Center for Materials, Applications &amp; Nanostructures), UPV/EHU Scientific Park, Martina Casiano Building, 3th floor, Sarriena s/n, 48940 Leioa, SpainDpto. Mineralogía y Petrología, Universidad del País Vasco, UPV/EHU, Sarriena s/n, 48940 Leioa, SpainDpto. Mineralogía y Petrología, Universidad del País Vasco, UPV/EHU, Sarriena s/n, 48940 Leioa, SpainIonothermal synthesis is a little used method for the preparation of coordination polymers. By this method, two cadmium compounds were synthesized, <b>1</b>, with formula Cd<sub>3</sub>(ox)F<sub>2</sub>(Ina)<sub>2</sub> (Ina = isonicotinate) and <b>2</b>, Cd(NO<sub>3</sub>)<sub>2</sub>(4,4&#8242;-Bpy) (4,4&#8242;-Bpy = 4,4&#8242;-Bipyridine). The modification of the reaction conditions has allowed to obtain <b>2</b> as a pure phase. The structure of both compounds was determined by a single-crystal X-ray diffraction. Compound <b>1</b> is isostructural to the previously reported Cd<sub>2</sub>Zn(ox)(OH)<sub>2</sub>(Ina)<sub>2</sub>. It crystallizes in the monoclinic space group P<i>2</i><sub>1</sub><i>/n</i> and present a three-dimensional (3D) network, built-up from [Cd<sub>3</sub>(ox)F<sub>2</sub>]<sub>n</sub><sup>2n+</sup> layers, linked by isonicotinate ligands. Crystals of <b>2</b> are formed by twins of two components which are rotated ca. 180&#176; to each other. This compound crystallizes in the triclinic P<i>-1</i> space group and its structure can be describe as a two-dimensional (2D) 4 connected <i>&#8216;sql&#8217;</i> net. The layers are composed by [Cd(NO<sub>3</sub>)<sub>2</sub>]<sub>n</sub> chains linked through 4,4&#8242;-Bpy ligands, and are pillared along the [011] direction. The thermal decomposition of <b>2</b> was studied by thermogravimetric and thermodiffractiometric techniques. The compound decomposes gradually starting from 160 &#176;C, and due to heating, the structure suffers slight reversible changes in the bond distances and angles.https://www.mdpi.com/1420-3049/24/22/4059cadmium coordination polymersionothermal synthesiscrystal structure determination
spellingShingle Iñigo PerezF
Edurne S. Larrea
Begoña Bazán
Gotzone Barandika
M. Karmele Urtiaga
Maria I. Arriortua
Ionothermal Synthesis of Cadmium Coordination Polymers: Ionic Liquid Effects on the Synthesis, Structural, and Thermal Characterization
Molecules
cadmium coordination polymers
ionothermal synthesis
crystal structure determination
title Ionothermal Synthesis of Cadmium Coordination Polymers: Ionic Liquid Effects on the Synthesis, Structural, and Thermal Characterization
title_full Ionothermal Synthesis of Cadmium Coordination Polymers: Ionic Liquid Effects on the Synthesis, Structural, and Thermal Characterization
title_fullStr Ionothermal Synthesis of Cadmium Coordination Polymers: Ionic Liquid Effects on the Synthesis, Structural, and Thermal Characterization
title_full_unstemmed Ionothermal Synthesis of Cadmium Coordination Polymers: Ionic Liquid Effects on the Synthesis, Structural, and Thermal Characterization
title_short Ionothermal Synthesis of Cadmium Coordination Polymers: Ionic Liquid Effects on the Synthesis, Structural, and Thermal Characterization
title_sort ionothermal synthesis of cadmium coordination polymers ionic liquid effects on the synthesis structural and thermal characterization
topic cadmium coordination polymers
ionothermal synthesis
crystal structure determination
url https://www.mdpi.com/1420-3049/24/22/4059
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