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Polymorphism and variable structural dimensionality in the iron(III) phosphate oxalate system : a new polymorph of 3D [Fe-2(HPO4)(2)(C2O4)(H2O)(2)]center dot 2H(2)O and the layered material [Fe-2(HPO4)(2)(C2O4)(H2O)(2)]
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Lethbridge, Zoe A. D., Clarkson, Guy J., Turner, S. S. (Scott S.) and Walton, Richard I. (2009) Polymorphism and variable structural dimensionality in the iron(III) phosphate oxalate system : a new polymorph of 3D [Fe-2(HPO4)(2)(C2O4)(H2O)(2)]center dot 2H(2)O and the layered material [Fe-2(HPO4)(2)(C2O4)(H2O)(2)]. Dalton Transactions (No.42). pp. 9176-9182. doi:10.1039/b911757a ISSN 1477-9226.
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Official URL: http://dx.doi.org/10.1039/b911757a
Abstract
Two new iron (III) phosphate oxalates have been isolated under hydrothermal conditions as phase-pure samples and their crystal structures determined from single crystal X-ray diffraction. [Fe-2(HPO4)(2)(C2O4)(H2O)(2)]center dot 2H(2)O, I, is a polymorph of a known phase and differs in the local arrangement of hydrophosphate, oxalate and coordinated water about iron, presenting a mer orientation of three coordinated phosphates, rather than fac as previously seen. The structure of I is three-dimensionally connected with similar network connectivity to the known phase but different overall topology. [Fe-2(HPO4)(2)(C2O4)(H2O)(2)], II, has a layered structure constructed from octahedral Fe(III) centres coordinated by hydrophosphate, oxalate and water in a fac arrangement. The amount of water used in synthesis is one of the key experimental parameters in stabilising one phase over the other. Thermogravimetric analysis shows that both I and II ultimately collapse into dense tridymite type FePO4 above 600 degrees C and variable temperature powder XRD shows that this occurs via crystalline intermediate phases. Variable temperature magnetisation measurements show that both materials order antiferromagnetically at low temperatures, with similar Neel temperatures (similar to 29 K) despite their long-range structural differences.
Item Type: | Journal Article | ||||
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Subjects: | Q Science > QD Chemistry | ||||
Divisions: | Faculty of Science, Engineering and Medicine > Science > Chemistry | ||||
Library of Congress Subject Headings (LCSH): | Polymorphism (Crystallography), Oxalates, Crystals -- Structure, Thermochemistry, Phosphates, Crystallization, Antiferromagnetism, Iron | ||||
Journal or Publication Title: | Dalton Transactions | ||||
Publisher: | Royal Society of Chemistry | ||||
ISSN: | 1477-9226 | ||||
Official Date: | 2009 | ||||
Dates: |
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Number: | No.42 | ||||
Number of Pages: | 7 | ||||
Page Range: | pp. 9176-9182 | ||||
DOI: | 10.1039/b911757a | ||||
Status: | Peer Reviewed | ||||
Publication Status: | Published | ||||
Access rights to Published version: | Restricted or Subscription Access | ||||
Funder: | Engineering and Physical Sciences Research Council (EPSRC) | ||||
Grant number: | EP/C516591 (EPSRC) |
Data sourced from Thomson Reuters' Web of Knowledge
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