The synthesis and characterisation of coordination and hydrogen-bonded networks based on 4-(3,5-dimethyl-1H-pyrazol-4-yl)benzoic acid.
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| Title: | The synthesis and characterisation of coordination and hydrogen-bonded networks based on 4-(3,5-dimethyl-1H-pyrazol-4-yl)benzoic acid. |
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| Authors: | Bryant, Macguire R.1, Burrows, Andrew D.2, Fitchett, Christopher M.3, Hawes, Chris S.3, Hunter, Sally O.1, Keenan, Luke L.2, Kelly, David J.2, Kruger, Paul E.3,4, Mahon, Mary F.2, Richardson, Christopher1 |
| Source: | Dalton Transactions: An International Journal of Inorganic Chemistry. 5/21/2015, Vol. 44 Issue 19, p9269-9280. 12p. |
| Subjects: | Coordination compounds, Chemical synthesis, Coordination polymers synthesis, Hydrogen bonding, Pyrazolyl compounds, Benzoic acid, Ligand binding (Biochemistry) |
| Abstract: | The synthesis, structural and thermal characterisation of a number of coordination complexes featuring the N,O-heteroditopic ligand 4-(3,5-dimethyl-1H-pyrazol-4-yl)benzoate, HL are reported. The reaction of H2L with cobalt(ii) and nickel(ii) nitrates at room temperature in basic DMF/H2O solution gave discrete mononuclear coordination complexes with the general formula {[M(HL)2(H2O)4]·2DMF} (M = Co (1), Ni (2)), whereas the reaction with zinc(ii) nitrate gave [Zn(HL)2]∞, 3, a coordination polymer with distorted diamondoid topology and fourfold interpenetration. Coordination about the tetrahedral Zn(ii) nodes in 3 are furnished by two pyrazolyl nitrogen atoms and two carboxylate oxygen atoms to give a mixed N2O2 donor set. Isotopological coordination polymers of zinc(ii), {[Zn(HL)2]·2CH3OH·H2O}∞, 4, and cobalt(ii), [Co(HL)2]∞, 5, are formed when the reactions are carried out under solvothermal conditions in methanol (80 °C) and water (180 °C), respectively. The reaction of H2L with cadmium(ii) nitrate at room temperature in methanol gives {[Cd(HL)2(MeOH)2]·1.8MeOH}∞6, a 2-D (4,4)-connected coordination polymer, whereas with copper(ii) the formation of green crystals that transform into purple crystals is observed. The metastable green phase [Cu3(HL)4(μ2-SO4)(H2O)3]∞, 7, crystallises with conserved binding domains of the heteroditopic ligand and contains two different metal nodes: a dicopper carboxylate paddle wheel motif, and, a dicopper unit bridged by sulfate ions and coordinated by ligand pyrazolyl nitrogen atoms. The resultant purple phase {[Cu(HL)2]·4CH3OH·H2O}∞, 8, however, has single copper ion nodes coordinated by mixed N2O2 donor sets with trans-square planar geometry and is threefold interpenetrated. The desolvation of 8 was followed by powder X-ray diffraction and single crystal X-ray diffraction which show desolvation induces the transition to a more closely packed structure while the coordination geometry about the copper ions and the network topology is retained. Powder X-ray diffraction and microanalysis were used to characterise the bulk purity of the coordination materials 1–6 and 8. The thermal characteristics of 1–2, 4–6 and 8 were studied by TG-DTA. This led to the curious observation of small exothermic events in networks 4, 6, and 8 that appear to be linked to their decomposition. In addition, the solid state structures of H2L and that of its protonated salt, H2L·HNO3, were also determined and revealed that H2L forms a 2-D hydrogen bonded polymer incorporating helical chains formed through N–H…O and O–H…N interactions, and that [H3L]NO3 forms a 1-D hydrogen-bonded polymer. [ABSTRACT FROM AUTHOR] |
| Copyright of Dalton Transactions: An International Journal of Inorganic Chemistry is the property of Royal Society of Chemistry and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.) | |
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| Items | – Name: Title Label: Title Group: Ti Data: The synthesis and characterisation of coordination and hydrogen-bonded networks based on 4-(3,5-dimethyl-1H-pyrazol-4-yl)benzoic acid. – Name: Author Label: Authors Group: Au Data: <searchLink fieldCode="AR" term="%22Bryant%2C+Macguire+R%2E%22">Bryant, Macguire R.</searchLink><relatesTo>1</relatesTo><br /><searchLink fieldCode="AR" term="%22Burrows%2C+Andrew+D%2E%22">Burrows, Andrew D.</searchLink><relatesTo>2</relatesTo><br /><searchLink fieldCode="AR" term="%22Fitchett%2C+Christopher+M%2E%22">Fitchett, Christopher M.</searchLink><relatesTo>3</relatesTo><br /><searchLink fieldCode="AR" term="%22Hawes%2C+Chris+S%2E%22">Hawes, Chris S.</searchLink><relatesTo>3</relatesTo><br /><searchLink fieldCode="AR" term="%22Hunter%2C+Sally+O%2E%22">Hunter, Sally O.</searchLink><relatesTo>1</relatesTo><br /><searchLink fieldCode="AR" term="%22Keenan%2C+Luke+L%2E%22">Keenan, Luke L.</searchLink><relatesTo>2</relatesTo><br /><searchLink fieldCode="AR" term="%22Kelly%2C+David+J%2E%22">Kelly, David J.</searchLink><relatesTo>2</relatesTo><br /><searchLink fieldCode="AR" term="%22Kruger%2C+Paul+E%2E%22">Kruger, Paul E.</searchLink><relatesTo>3,4</relatesTo><br /><searchLink fieldCode="AR" term="%22Mahon%2C+Mary+F%2E%22">Mahon, Mary F.</searchLink><relatesTo>2</relatesTo><br /><searchLink fieldCode="AR" term="%22Richardson%2C+Christopher%22">Richardson, Christopher</searchLink><relatesTo>1</relatesTo> – Name: TitleSource Label: Source Group: Src Data: <searchLink fieldCode="JN" term="%22Dalton+Transactions%3A+An+International+Journal+of+Inorganic+Chemistry%22">Dalton Transactions: An International Journal of Inorganic Chemistry</searchLink>. 5/21/2015, Vol. 44 Issue 19, p9269-9280. 12p. – Name: Subject Label: Subjects Group: Su Data: <searchLink fieldCode="DE" term="%22Coordination+compounds%22">Coordination compounds</searchLink><br /><searchLink fieldCode="DE" term="%22Chemical+synthesis%22">Chemical synthesis</searchLink><br /><searchLink fieldCode="DE" term="%22Coordination+polymers+synthesis%22">Coordination polymers synthesis</searchLink><br /><searchLink fieldCode="DE" term="%22Hydrogen+bonding%22">Hydrogen bonding</searchLink><br /><searchLink fieldCode="DE" term="%22Pyrazolyl+compounds%22">Pyrazolyl compounds</searchLink><br /><searchLink fieldCode="DE" term="%22Benzoic+acid%22">Benzoic acid</searchLink><br /><searchLink fieldCode="DE" term="%22Ligand+binding+%28Biochemistry%29%22">Ligand binding (Biochemistry)</searchLink> – Name: Abstract Label: Abstract Group: Ab Data: The synthesis, structural and thermal characterisation of a number of coordination complexes featuring the N,O-heteroditopic ligand 4-(3,5-dimethyl-1H-pyrazol-4-yl)benzoate, HL are reported. The reaction of H2L with cobalt(ii) and nickel(ii) nitrates at room temperature in basic DMF/H2O solution gave discrete mononuclear coordination complexes with the general formula {[M(HL)2(H2O)4]·2DMF} (M = Co (1), Ni (2)), whereas the reaction with zinc(ii) nitrate gave [Zn(HL)2]∞, 3, a coordination polymer with distorted diamondoid topology and fourfold interpenetration. Coordination about the tetrahedral Zn(ii) nodes in 3 are furnished by two pyrazolyl nitrogen atoms and two carboxylate oxygen atoms to give a mixed N2O2 donor set. Isotopological coordination polymers of zinc(ii), {[Zn(HL)2]·2CH3OH·H2O}∞, 4, and cobalt(ii), [Co(HL)2]∞, 5, are formed when the reactions are carried out under solvothermal conditions in methanol (80 °C) and water (180 °C), respectively. The reaction of H2L with cadmium(ii) nitrate at room temperature in methanol gives {[Cd(HL)2(MeOH)2]·1.8MeOH}∞6, a 2-D (4,4)-connected coordination polymer, whereas with copper(ii) the formation of green crystals that transform into purple crystals is observed. The metastable green phase [Cu3(HL)4(μ2-SO4)(H2O)3]∞, 7, crystallises with conserved binding domains of the heteroditopic ligand and contains two different metal nodes: a dicopper carboxylate paddle wheel motif, and, a dicopper unit bridged by sulfate ions and coordinated by ligand pyrazolyl nitrogen atoms. The resultant purple phase {[Cu(HL)2]·4CH3OH·H2O}∞, 8, however, has single copper ion nodes coordinated by mixed N2O2 donor sets with trans-square planar geometry and is threefold interpenetrated. The desolvation of 8 was followed by powder X-ray diffraction and single crystal X-ray diffraction which show desolvation induces the transition to a more closely packed structure while the coordination geometry about the copper ions and the network topology is retained. Powder X-ray diffraction and microanalysis were used to characterise the bulk purity of the coordination materials 1–6 and 8. The thermal characteristics of 1–2, 4–6 and 8 were studied by TG-DTA. This led to the curious observation of small exothermic events in networks 4, 6, and 8 that appear to be linked to their decomposition. In addition, the solid state structures of H2L and that of its protonated salt, H2L·HNO3, were also determined and revealed that H2L forms a 2-D hydrogen bonded polymer incorporating helical chains formed through N–H…O and O–H…N interactions, and that [H3L]NO3 forms a 1-D hydrogen-bonded polymer. [ABSTRACT FROM AUTHOR] – Name: AbstractSuppliedCopyright Label: Group: Ab Data: <i>Copyright of Dalton Transactions: An International Journal of Inorganic Chemistry is the property of Royal Society of Chemistry and its content may not be copied or emailed to multiple sites without the copyright holder's express written permission. Additionally, content may not be used with any artificial intelligence tools or machine learning technologies. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract.</i> (Copyright applies to all Abstracts.) |
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| RecordInfo | BibRecord: BibEntity: Identifiers: – Type: doi Value: 10.1039/c5dt00011d Languages: – Code: eng Text: English PhysicalDescription: Pagination: PageCount: 12 StartPage: 9269 Subjects: – SubjectFull: Coordination compounds Type: general – SubjectFull: Chemical synthesis Type: general – SubjectFull: Coordination polymers synthesis Type: general – SubjectFull: Hydrogen bonding Type: general – SubjectFull: Pyrazolyl compounds Type: general – SubjectFull: Benzoic acid Type: general – SubjectFull: Ligand binding (Biochemistry) Type: general Titles: – TitleFull: The synthesis and characterisation of coordination and hydrogen-bonded networks based on 4-(3,5-dimethyl-1H-pyrazol-4-yl)benzoic acid. Type: main BibRelationships: HasContributorRelationships: – PersonEntity: Name: NameFull: Bryant, Macguire R. – PersonEntity: Name: NameFull: Burrows, Andrew D. – PersonEntity: Name: NameFull: Fitchett, Christopher M. – PersonEntity: Name: NameFull: Hawes, Chris S. – PersonEntity: Name: NameFull: Hunter, Sally O. – PersonEntity: Name: NameFull: Keenan, Luke L. – PersonEntity: Name: NameFull: Kelly, David J. – PersonEntity: Name: NameFull: Kruger, Paul E. – PersonEntity: Name: NameFull: Mahon, Mary F. – PersonEntity: Name: NameFull: Richardson, Christopher IsPartOfRelationships: – BibEntity: Dates: – D: 21 M: 05 Text: 5/21/2015 Type: published Y: 2015 Identifiers: – Type: issn-print Value: 14779226 Numbering: – Type: volume Value: 44 – Type: issue Value: 19 Titles: – TitleFull: Dalton Transactions: An International Journal of Inorganic Chemistry Type: main |
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