Hydrothermal synthesis, structure and magnetic properties of [Fe-3(PO4)(3)F-2,H3N-(CH2)(4)-NH3]: The analog of the three-dimensional gallophosphate structure-type ULM-3

被引:58
作者
Cavellec, M
Riou, D
Greneche, JM
Ferey, G
机构
[1] UNIV MAINE,FAC SCI,LAB PHYS ETAT CONDENSEE,URA CNRS 807,F-72017 LE MANS,FRANCE
[2] UNIV MAINE,FAC SCI,LAB FLUORURES,URA CNRS 449,F-72017 LE MANS,FRANCE
关键词
hydrothermal synthesis; oxyfluorinated compounds; microporous compounds; superexchange; X-ray diffraction; Mossbauer spectrometry;
D O I
10.1016/S0304-8853(96)00302-2
中图分类号
T [工业技术];
学科分类号
08 ;
摘要
[Fe-3(PC)(4))(3)F-2, H3N-(CH2)(4)-NH3] has been synthesized hydrothermally (453 K, 24 h, autogenous pressure). Its structure was determined by single-crystal X-ray diffraction. It is orthorhombic (space group Pbca No. 61) with cell parameters a = 10.203(1) Angstrom, b = 18.670(1) Angstrom, c = 16.268(1) Angstrom, V = 3099(1) Angstrom(3) and Z = 8. Its three-dimensional structure, refined to R(1)(F-0) = 0.036 and wR(2)(F-0(2)) = 0.093 from 6821 unique reflections (I > 2 sigma(I)) is isostructural with the oxyfluorinated gallophosphate ULM-3. From a structural point of view, this leads to 10-membered channels along [100]. It is also an antiferromagnetic compound which orders at T-N = 37(2) K. Mossbauer data are consistent with the presence of two distinct Fe3+ sites in the high spin state: one corresponding to Fe3+ in an octahedral site and the other to two Fe3+ in trigonal bipyramids, Magnetic couplings are discussed in terms of superexchange and supersuperexchange interactions.
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页码:173 / 183
页数:11
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