DOI: 10.1002/zaac.200700460. Synthesis and Characterization of the New Copper Tetraphosphonate Cu2[(HO3PCH2)4C6H2]·2H2O

Synthesis and Characterization of the New Copper Tetraphosphonate Cu2[(HO3PCH2)4C6H2]·2H2O

10.1002/zaac.200700460

Crossref journal-article

Wiley

Zeitschrift für anorganische und allgemeine Chemie (311)

Abstract

AbstractFollowing the strategy of using polyfunctional phosphonic acids for the synthesis of three‐dimensional metal phosphonates, the ethyl ester of a tetraphosphonic acid, i. e. 1,2,4,5‐(Et2O3PCH2)4C6H2, was used in the hydrothermal synthesis of the new copper tetraphosphonate, Cu2[(HO3PCH2)4C6H2]·2H2O (1). The in situ hydrolysis of the ethyl ester leads to the acid (1,2,4,5‐(H2O3PCH2)4C6H2) which reacts with the Cu2+ ions to form the green coarse‐crystalline product. The title compound is the first fully characterized copper tetraphosphonate. Its structure was solved from single crystal data (1: triclinic, $\rm P{\bar 1}$, a = 4.9262(10), b = 8.1890(16), c = 11.800(2) Å, α = 71.17(3), β = 89.15(3), γ = 88.56(3)°, V = 450.39(16) Å3, Z = 2, R1 = 0.0284, wR2 = 0.0682). The structure is built up from edge‐sharing CuO5 polyhedra each containing a single H2O molecule. Thus, dimeric [Cu2O8] units are formed. In the second coordination sphere of each of the Cu2+ ions four HO3PCH2R units are observed. The [Cu2O8] polyhedra are connected to eight other [Cu2O8] polyhedra by these organic linkers and a three‐dimensional framework structure is formed. Thermogravimetric, magnetic, and temperature dependent powder XRD measurements and the Raman‐spectrum are also presented.

Bibliography

Kaempfe, P., & Stock, N. (2008). Synthesis and Characterization of the New Copper Tetraphosphonate Cu2[(HO3PCH2)4C6H2]Â·2H2O. Zeitschrift FÃ¼r Anorganische Und Allgemeine Chemie, 634(4), 714â717. Portico.

Authors 2

Paulina Kaempfe (first)
Norbert Stock (additional)

References 15 Referenced 16

10.1002/(SICI)1521-3757(19991115)111:22<3466::AID-ANGE3466>3.0.CO;2-M
10.1002/(SICI)1521-3773(19991115)38:22<3268::AID-ANIE3268>3.0.CO;2-U
{'key': 'e_1_2_1_3_2', 'first-page': '164', 'volume-title': 'Comprehensive Supramolecular Chemistry', 'author': 'Alberti G.', 'year': '1996'} / Comprehensive Supramolecular Chemistry by Alberti G. (1996)
{'key': 'e_1_2_1_4_2', 'first-page': '371', 'volume-title': 'Progress in Inorganic Chemistry', 'author': 'Clearfield A.', 'year': '1988'} / Progress in Inorganic Chemistry by Clearfield A. (1988)
10.1002/ange.200351718
10.1002/anie.200351718
10.1016/j.jssc.2003.08.005
10.1016/j.micromeso.2003.12.026
10.1002/zaac.200400455
10.1039/b106780j
10.1039/b309475h
10.1039/b304610a
10.1021/ic011124v
10.1016/j.solidstatesciences.2004.10.010
{'key': 'e_1_2_1_14_2', 'first-page': '23', 'volume': '58', 'author': 'Ouarsal R.', 'year': '2002', 'journal-title': 'Acta Crystallogr.'} / Acta Crystallogr. by Ouarsal R. (2002)

Dates

Type	When
Created	17 years, 5 months ago (March 4, 2008, 9:56 a.m.)
Deposited	1 year, 10 months ago (Oct. 17, 2023, 1:38 p.m.)
Indexed	1 year, 7 months ago (Jan. 18, 2024, 11:25 a.m.)
Issued	17 years, 5 months ago (March 4, 2008)
Published	17 years, 5 months ago (March 4, 2008)
Published Online	17 years, 5 months ago (March 4, 2008)
Published Print	17 years, 4 months ago (April 1, 2008)

Funders 0

None

BibTeX

@article{Kaempfe_2008, title={Synthesis and Characterization of the New Copper Tetraphosphonate Cu2[(HO3PCH2)4C6H2]·2H2O}, volume={634}, ISSN={1521-3749}, url={http://dx.doi.org/10.1002/zaac.200700460}, DOI={10.1002/zaac.200700460}, number={4}, journal={Zeitschrift für anorganische und allgemeine Chemie}, publisher={Wiley}, author={Kaempfe, Paulina and Stock, Norbert}, year={2008}, month=mar, pages={714–717} }

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  "abstract": "<jats:title>Abstract</jats:title><jats:p>Following the strategy of using polyfunctional phosphonic acids for the synthesis of three\u2010dimensional metal phosphonates, the ethyl ester of a tetraphosphonic acid, i. e. 1,2,4,5\u2010(Et<jats:sub>2</jats:sub>O<jats:sub>3</jats:sub>PCH<jats:sub>2</jats:sub>)<jats:sub>4</jats:sub>C<jats:sub>6</jats:sub>H<jats:sub>2</jats:sub>, was used in the hydrothermal synthesis of the new copper tetraphosphonate, Cu<jats:sub>2</jats:sub>[(HO<jats:sub>3</jats:sub>PCH<jats:sub>2</jats:sub>)<jats:sub>4</jats:sub>C<jats:sub>6</jats:sub>H<jats:sub>2</jats:sub>]\u00b72H<jats:sub>2</jats:sub>O (<jats:bold>1</jats:bold>). The <jats:italic>in situ</jats:italic> hydrolysis of the ethyl ester leads to the acid (1,2,4,5\u2010(H<jats:sub>2</jats:sub>O<jats:sub>3</jats:sub>PCH<jats:sub>2</jats:sub>)<jats:sub>4</jats:sub>C<jats:sub>6</jats:sub>H<jats:sub>2</jats:sub>) which reacts with the Cu<jats:sup>2+</jats:sup> ions to form the green coarse\u2010crystalline product. The title compound is the first fully characterized copper tetraphosphonate. Its structure was solved from single crystal data (<jats:bold>1</jats:bold>: triclinic, <jats:styled-content>$\\rm P{\\bar 1}$<jats:inline-graphic xmlns:xlink=\"http://www.w3.org/1999/xlink\" xlink:href=\"graphic/tex2gif-ueqn-1.gif\" xlink:title=\"equation image\" /></jats:styled-content>, <jats:italic>a</jats:italic> = 4.9262(10), <jats:italic>b</jats:italic> = 8.1890(16), <jats:italic>c</jats:italic> = 11.800(2) \u00c5, \u03b1 = 71.17(3), <jats:italic>\u03b2</jats:italic> = 89.15(3), \u03b3 = 88.56(3)\u00b0, <jats:italic>V</jats:italic> = 450.39(16) \u00c5<jats:sup>3</jats:sup>, <jats:italic>Z</jats:italic> = 2, <jats:italic>R</jats:italic>1 = 0.0284, <jats:italic>wR</jats:italic><jats:sub>2</jats:sub> = 0.0682). The structure is built up from edge\u2010sharing CuO<jats:sub>5</jats:sub> polyhedra each containing a single H<jats:sub>2</jats:sub>O molecule. Thus, dimeric [Cu<jats:sub>2</jats:sub>O<jats:sub>8</jats:sub>] units are formed. In the second coordination sphere of each of the Cu<jats:sup>2+</jats:sup> ions four HO<jats:sub>3</jats:sub>PCH<jats:sub>2</jats:sub>R units are observed. The [Cu<jats:sub>2</jats:sub>O<jats:sub>8</jats:sub>] polyhedra are connected to eight other [Cu<jats:sub>2</jats:sub>O<jats:sub>8</jats:sub>] polyhedra by these organic linkers and a three\u2010dimensional framework structure is formed. Thermogravimetric, magnetic, and temperature dependent powder XRD measurements and the Raman\u2010spectrum are also presented.</jats:p>",
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