Hydrothermal synthesis, structural approach, magnetic and Mössbauer study of the layered Fe(III) carboxyethylphosphonate [Fe(OH)(H 2O)(O 3P-(CH 2) 2-CO 2H)] or MIL-37

• Published in: Solid state sciences 2000-11, Vol.2 (7), p.717-724
• Main Authors: Riou-Cavellec, Myriam, Sanselme, Morgane, Grenèche, Jean-Marc, Férey, Gérard
• Format: Article
• Language: English
• Subjects: Chemistry; Colloidal state and disperse state; Condensed matter: electronic structure, electrical, magnetic, and optical properties; Condensed matter: structure, mechanical and thermal properties; Exact sciences and technology; General and physical chemistry; Hydrothermal synthesis; Inorganic compounds; Iron (III) carboxyethylphosphonate; Layered; Magnetic; Magnetic properties and materials; Magnetic resonances and relaxations in condensed matter, mössbauer effect; Magnetically ordered materials: other intrinsic properties; Metal complexes; Mossbauer effect; other γ-ray spectroscopy; Mössbauer effect; other γ-ray spectroscopy; Physics; Porous materials; Saturation moments and magnetic susceptibilities; Structure of solids and liquids; crystallography; Structure of specific crystalline solids
• ISSN: 1293-2558; 1873-3085
• DOI: 10.1016/S1293-2558(00)01080-3

[Fe(OH)(H 2O)(O 3P-(CH 2) 2-CO 2H)] or MIL-37 was synthesized hydrothermally (443 K, 24 h) under autogenous pressure. Its layered structure was determined by single crystal X-ray diffraction (space group Pbc2 1 (n°29), a=7.4364(2) Å, b=9.5646(4) Å, c=20.4537(7) Å, V=1454.79(9) Å 3, Z=8). It is built up from [FeO 3(OH) 2(H 2O)] octahedral chains linked via hydroxyl vertices; these chains are then bonded by [PO 3C] tetrahedra in such a way that each octahedron shares three oxygen atoms with three different tetrahedra. This layout leads to inorganic sheets which are well-known in phosphates, for instance in the iron phosphate ULM-11. At the other end of the organic chains, carboxylic groups are dangling. A Mössbauer study and magnetic measurements reveal a canted antiferromagnetic behaviour below T N=20(1) K.