Mild hydrothermal synthesis, crystal structure, thermal behavior, spectroscopic and magnetic properties of the (NH4)[Fe(AsO4)1−x(PO4)xF] (x=0.3, 0.6, 0.8) series. Thermal transformation of (NH4)[Fe(AsO4)0.7(PO4)0.3F] into the textural porous orthorhombic Fe(AsO4)0.7(PO4)0.3

Berrocal, Teresa; Mesa, José L.; Pizarro, José L.; Bazán, Begoña; Lezama, Luís; Arriortua, Marı́a I.; Rojo, Teófilo

doi:10.1016/j.jssc.2009.01.026

Cited by 3 publications

(1 citation statement)

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“…AsO 4 forms the same tetrahedral coordination polyhedra, but the As–O bond lengths are slightly longer, which may lead to changes in both crystal structure and physical properties. Example structures with mixed P/As positions are (NH 4 )[Fe(AsO 4 ) 1‑ x (PO 4 ) x F], LiTiOAs 1‑ x P x O 4 and the mineral olivenite Cu 2 AsO 4 OH, where some of the arsenate can be replaced by phosphate. In K 2 (HSeO 4 ) 1.5 (H 2 PO 4 ) 0.5 another kind of solid solution has been reported, where Se 6+ and P 5+ occupy a mixed position.…”

Section: Introductionmentioning

confidence: 99%

Synthesis and Crystal Structure of the Solid Solution Co₃(SeO₃)_3-x(PO₃OH)_x(H₂O) Involving Crystallographic Split Positions of Se⁴⁺ and P⁵⁺

Zimmermann

Johnsson

2013

Inorg. Chem.

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Three new cobalt selenite hydroxo-phosphates laying in the solid solution Co3(SeO3)3-x(PO3OH)x(H2O), with x = 0.8, x = 1.0, and x = 1.2 are reported. Single crystals were obtained by hydrothermal synthesis and the crystal structure was determined by single crystal X-ray diffraction. The structure can be described as a 3D framework having selenite and hydroxo-phosphate groups protruding into channels in the crystal structure. Se(4+) and P(5+) share a split position in the structure so that either SeO3 groups having a stereochemically active lone pair or tetrahedrally coordinated PO3OH groups are present. The OH-group is thus only present when the split position is occupied by P(5+). The crystal water is coordinated to a cobalt atom and TG and IR measurements show that the water and hydroxyl groups leave the structure at unusually high temperatures (>450 °C). Magnetic susceptibility measurements show antiferromagnetic coupling below 16 K and a magnetic moment of 4.02(3) μB per Co atom was observed.

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Section: Introductionmentioning

confidence: 99%

Synthesis and Crystal Structure of the Solid Solution Co₃(SeO₃)_3-x(PO₃OH)_x(H₂O) Involving Crystallographic Split Positions of Se⁴⁺ and P⁵⁺

Zimmermann

Johnsson

2013

Inorg. Chem.

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ChemInform Abstract: Mild Hydrothermal Synthesis, Crystal Structure, Thermal Behavior, Spectroscopic and Magnetic Properties of the (NH₄) [Fe(AsO₄)_1‐x(PO₄)_xF] (I) (x = 0.3, 0.6, 0.8) Series. Thermal Transformation of (NH₄) [Fe(AsO₄)_0.7(PO₄)_0.3F] into the Textural Porous Orthorhombic Fe(AsO₄)_0.7(PO₄)_0.3 (II).

Berrocal¹,

Mesa²,

Pizarro³

et al. 2009

ChemInform

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Iron I 7100 Mild Hydrothermal Synthesis, Crystal Structure, Thermal Behavior, Spectroscopic and Magnetic Properties of the (NH 4 )[Fe(AsO 4 ) 1-x (PO 4 ) x F] (I) (x = 0.3, 0.6, 0.8) Series. Thermal Transformation of (NH4)[Fe(AsO4)0.7(PO4)0.3F] into the Textural Porous Orthorhombic Fe(AsO4)0.7(PO4)0.3 (II). -Light-green single crystals of compounds (I) (orthorhombic space group Pna21 with Z = 8) are hydrothermally prepared from a mixture of Fe2(SO4)3, As2O5, H3PO4, HF, and NH4OH in H2O (autoclave, pH 3, 170°C, 5 d). Brown single crystals of (II) (orthorhombic, space group Imam, Z = 12) are obtained by heating single crystals of (NH4)[Fe(AsO4)0.7(PO4)0.3F] in air at 465°C for 40 h. Compounds (I) and (II) exhibit a related three-dimensional structure.The framework of (I) contains perpendicular chains formed by alternating Fe(2)O4F2 or Fe(1)O4F2 octahedra and As/P(2)O4 or As/P(1)O4 tetrahedra, respectively. (II) contains chains of alternating Fe (2)O 6 octahedra and As/P(2)O 4 tetrahedra. Magnetic measurements indicate the predominance of antiferromagnetic interactions in all the compounds. -(BERROCAL, T.; MESA*, J. L.; PIZARRO, J. L.; BAZAN, B.; LEZAMA, L.; ARRIORTUA, M. I.; ROJO, T.; J. Solid State Chem. 182 (2009) 4, 932-941;

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Reversible Solid-State Transformation in {Ni₂(H₂O)₂(Bpa)₂}(V₆O₁₇) Proved by Synchrotron Radiation: Color and Magnetic Properties Change

Luis

Orive

Larrea

et al. 2014

Crystal Growth & Design

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A B S T R A C T : T h e 3 D c r y s t a l s t r u c t u r e o f {Ni 2 (H 2 O) 2 (Bpa) 2 }(V 6 O 17 ) (NiBpaRT), were Bpa is 1,2-bis(4-pyridil)ethane, was determined by single crystal X-ray diffraction. The crystal structure is constructed from {Ni-(H 2 O)(Bpa)} metal−organic and (V 3 O 8.5 ) vanadate chains. The connectivity of these one-dimensional units generates a three-dimensional inorganic substructure, and also a threedimensional inorganic−organic framework. The asymmetric unit contains two crystallographically pseudoequivalent vanadate and metal−organic chains. The stacking of these crystallographically pseudoequivalent units seems to be nearly related to the twinning law of the crystals, and with the diffuse scattering observed in the diffraction pictures. Several models of local disorders for the packing of these one-dimensional units have been proposed to explain the origin of the diffuse scattering observed in the diffraction images. The obtained single crystals are systematically twinned. The origin of this twining is clearly related to the packing of the crystallographically independent chains along the [100] direction. The topology of the crystal structure is a new self-catenated three nodal net. The simplified structure can be described also as the natural tiling of two different tiles. NiBpaRT shows a reversible solid state transformation due to the loss of coordinated water molecules at 180°C. The high temperature compound, {Ni 2 (Bpa) 2 }(V 6 O 17 ) (NiBpaHT), maintains the crystallinity, but the solid state transformation involves a single crystal to polycrystalline reaction. So, the determination of the high temperature structure have been carried out by rigid body Rietveld refinement of the room temperature crystal structure, from synchrotron X-ray diffraction radiation. The loss of coordinated water molecules of the nickel cations is compensated by the incorporation of the terminal oxygen atoms, belonging to the adjacent VO 4 tetrahedra, into the coordination environment of the nickel cations. We have referred to this mechanism of reorganization of the structural units as padlock solid state transformation. The UV−vis spectra corroborate the presence of octahedrally coordinated nickel cations in the high temperature crystal structure. The IR and Raman spectra show strong changes in the absorption maxima related to the stretching vibration of VO terminal bonds, in good agreement with the proposed padlock mechanism. The dimeric ferromagnetic coupling of the nickel cations through the VO 4 tetrahedra is similar for NiBpaRT and NiBpaHT, showing also an antiferromagnetic coupling at low temperatures. However, the distortion of the nickel coordination environment during the transformation implies an important difference in the g values for NiBpaRT and NiBpaHT.

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Mild hydrothermal synthesis, crystal structure, thermal behavior, spectroscopic and magnetic properties of the (NH4)[Fe(AsO4)1−x(PO4)xF] (x=0.3, 0.6, 0.8) series. Thermal transformation of (NH4)[Fe(AsO4)0.7(PO4)0.3F] into the textural porous orthorhombic Fe(AsO4)0.7(PO4)0.3

Cited by 3 publications

References 45 publications

Synthesis and Crystal Structure of the Solid Solution Co₃(SeO₃)_3-x(PO₃OH)_x(H₂O) Involving Crystallographic Split Positions of Se⁴⁺ and P⁵⁺

Synthesis and Crystal Structure of the Solid Solution Co₃(SeO₃)_3-x(PO₃OH)_x(H₂O) Involving Crystallographic Split Positions of Se⁴⁺ and P⁵⁺

Reversible Solid-State Transformation in {Ni₂(H₂O)₂(Bpa)₂}(V₆O₁₇) Proved by Synchrotron Radiation: Color and Magnetic Properties Change

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Mild hydrothermal synthesis, crystal structure, thermal behavior, spectroscopic and magnetic properties of the (NH4)[Fe(AsO4)1−x(PO4)xF] (x=0.3, 0.6, 0.8) series. Thermal transformation of (NH4)[Fe(AsO4)0.7(PO4)0.3F] into the textural porous orthorhombic Fe(AsO4)0.7(PO4)0.3

Cited by 3 publications

References 45 publications

Synthesis and Crystal Structure of the Solid Solution Co3(SeO3)3-x(PO3OH)x(H2O) Involving Crystallographic Split Positions of Se4+ and P5+

Synthesis and Crystal Structure of the Solid Solution Co3(SeO3)3-x(PO3OH)x(H2O) Involving Crystallographic Split Positions of Se4+ and P5+

Reversible Solid-State Transformation in {Ni2(H2O)2(Bpa)2}(V6O17) Proved by Synchrotron Radiation: Color and Magnetic Properties Change

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Synthesis and Crystal Structure of the Solid Solution Co₃(SeO₃)_3-x(PO₃OH)_x(H₂O) Involving Crystallographic Split Positions of Se⁴⁺ and P⁵⁺

Synthesis and Crystal Structure of the Solid Solution Co₃(SeO₃)_3-x(PO₃OH)_x(H₂O) Involving Crystallographic Split Positions of Se⁴⁺ and P⁵⁺

Reversible Solid-State Transformation in {Ni₂(H₂O)₂(Bpa)₂}(V₆O₁₇) Proved by Synchrotron Radiation: Color and Magnetic Properties Change