Synthesis, Structure, and Magnetic Properties of Hydroxo‐Bridged Vanadium Oxalate V2O2(OH)2(C2O4)(H2O)2

Yang, Sihai; Li, Guobao; Tian, Shujian; Liao, Fuhui; Lin, Jianhua

doi:10.1002/ejic.200600103

Cited by 10 publications

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“…The relatively low melting point of oxalic acid (103.5 °C) and its self-flux property add further advantage of mild synthesis conditions to the exploration of novel oxalates . The magnetic properties of many oxalate-based materials have been reported, formed from isolated clusters, 1D chains, 2D layers, or 3D networks of metal ion centers. − …”

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confidence: 99%

Diverse Family of Layered Frustrated Magnets with Tailorable Interlayer Interactions

et al. 2017

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Single crystals of the compounds I, II and III were synthesised by hydrothermal methods using 23 mL teflonlined autoclaves. Starting materials from commercial companies were applied without further processing. For I, FeC2O42H2O, oxalic acid, KBF4 and K2CO3 were sealed within the autoclave with 2 mL distilled water in a molar ratio of 1:3:2:4. Reactions were performed at 160-190 °C for two days. For II, FeC2O42H2O, oxalic acid, sulfuric acid and Na2CO3 were reacted with 0.5 mL distilled water in a molar ratio of 10:15:10:2. Reactions were performed at 190 °C for four days. For III, FeCl22H2O, oxalic acid, and Li2CO3 were reacted with 5 mL 1M acetic acid in a molar ratio of 1:1:3. The autoclave was kept at 120°C for four days. After heating, the autoclaves were cooled down in air. The resulting products were repeatedly washed with distilled water and acetone and dried at 60°C. Similar procedures were carried out with variants of reactant ratios, water, temperature and time. Unsuccessful reactions typically produced yellow FeC2O42H2O crystallites. Single crystal X-ray diffraction. Transparent crystallites were selected and mounted on nylon loops in inert oil and SXRD data were collected on a Rigaku SCX Mini diffractometer using Mo Kα radiation (λ = 0.710 73 Å) at 173 K. Rigaku CrystalClear 2.0 was employed to index and process the data. Structures were then solved by direct methods and refined using SHELX-2014 1 incorporated in the WinGX program. Absorption corrections were performed semi-empirically from equivalent reflections on the basis of multi-scans. Non-H atoms were refined anisotropically. Characterisation: Fourier-transform infrared spectroscopy was carried out with the objective of determining the coordination of atoms in the sample and to detect any incorporation of H2O or OH-. The mid-infrared spectrum was obtained at room temperature using a Perkin Elmer Spectrum GX IR spectrometer. The spectra were collected in the range 400 to 4000 cm-1 with a resolution of 1 cm-1. Powder X-ray diffraction PXRD patterns were recorded on a Stoe STADI/P diffractometer operating in transmission mode with Fe Kα1 radiation (λ = 1.936 Å) in the 2θ range 10 °-100 °. Step scan mode, step size 0.4 °, steps time 250 s. Data sets were refined by conventional Rietveld methods using the GSAS package with the EXPGUI interface. 2 The refinement of the orthorhombic Cmc21 structural model of KFe(C2O4)F to room temperature PXRD data yields lattice constants a = 7.7802(1) Å, b = 11.8831(2) Å and c = 10.4216(2)Å. The background, scale factor, zero point, lattice parameters and coefficients for the peak shape function were refined to convergence. Thermogravimetric analysis (TGA) were carried out with hand-ground crystals using NETZSCH TG 209 thermal analyser. Samples (about 5 mg) of ground crystallites were placed in an alumina crucible and heated from room temperature until no obvious weight loss at a rate of 5 o C /min in flowing air atmosphere. The residues were examined and analysed by PXRD, all of which showed a typical pattern o...

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Diverse Family of Layered Frustrated Magnets with Tailorable Interlayer Interactions

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“…No clear hysteresis loops for ferromagnetic components were observed; therefore, options (c) and (e) are unlikely to play a role in the magnetic reversal in the present case. Therefore, it is expected that only the existence of exchange‐bias effects of antiferromagnetic sublattices can play a role in reversal of magnetization . As described above, the Tb is present in two oxidation states; therefore, Tb 3+ and Tb 4+ antiferromagnetic sublattices are responsible for the magnetization reversal in the present case .…”

Section: Resultsmentioning

confidence: 65%

Facile Synthesis, Structure Elucidation, and Magnetic Properties of Perovskite BaTb_1–xBi_xO₃

et al. 2017

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A series of perovskite BaTb1–xBixO3 (0.0 ≤ x ≤ 0.25) solid solutions were synthesized by a typical solid‐state method. Their structures were analyzed by a combination of X‐ray diffraction, neutron diffraction, and selected‐area electron diffraction. All of the materials crystalize in the P1 space group [a = 6.0582(1) Å, b = 6.0473(1) Å, c = 6.0693(1) Å, α = 60.00(1)°, β = 59.84(1)°, γ = 60.06(1)° for x = 0.0 at room temperature]. Magnetic measurements revealed that the magnetic‐ordering temperature decreases with increasing Bi content in BaTb1–xBixO3; therefore, the presence of Bi decreases the magnetic interactions of Tb. Furthermore, the magnetic structure for BaTb1–xBixO3 has been fully described in space group P1.

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“…Adapting this method, and using oxalic acid as the reducing agent, we were able to successfully synthesize blue single crystals of Ba 3 [(VO) 2 (C 2 O 4 ) 5 (H 2 O) 6 ]·(H 2 O) 3 ( 1 ) in excellent yield. This new reduced vanadium oxalate joins a number of vanadium(IV) oxalates that have been reported over the past decades, including [( n -C 4 H 9 ) 4 N] 2 [V 8 O 8 (OCH 3 ) 16 (C 2 O 4 )], V 2 O 2 (OH) 2 (C 2 O 4 )(H 2 O) 2 , (Ph 4 P) 2 [(VO) 2 (H 2 O) 2 (C 2 O 4 ) 3 ]·4H 2 O, (Ph 4 P)[VOCl(C 2 O 4 )], [V 2 O 2 (C 2 O 4 )(H 2 O) 6 ]Cl 2 ·4Bu 4 NCl·H 2 O, [FeCp 2 *] 2 [Et 4 N] 2 [V 2 O 2 (C 2 O 4 )(NCS) 6 ], (C 5 H 5 NH)[VOF(C 2 O 4 )(H 2 O) 2 ], (NH 4 )[V 2 O 2 (OH)(C 4 O 4 ) 2 (H 2 O) 3 ]·H 2 O, [V 2 O 2 Cl 2 (C 2 O 4 )(CH 3 OH) 4 ]·2Ph 4 Cl …”

Section: Introductionmentioning

confidence: 67%

Observation of Multiple Crystal-to-Crystal Transitions in a New Reduced Vanadium Oxalate Hybrid Material, Ba₃[(VO)₂(C₂O₄)₅(H₂O)₆]·(H₂O)₃, Prepared via a Mild, Two-Step Hydrothermal Method

Abeysinghe

Smith

Yeon

et al. 2014

Crystal Growth & Design

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A new reduced vanadium oxalate, Ba 3 [(VO) 2 (C 2 O 4 ) 5 -(H 2 O) 6 ]•(H 2 O) 3 , 1, was synthesized via a two-step, mild hydrothermal method using oxalic acid as the reducing agent. This compound undergoes multiple single-crystal to single-crystal phase transitions as a function of water content to form Ba3, after heating 1 to 50 and 100 °C, respectively. In addition, exposing 1 to a vacuum for 12 h also transforms it into 2, but not 3. All three compositional variants were structurally characterized by single crystal X-ray diffraction and are found to crystallize in the monoclinic space groups of C2/c and P2 1 /c, for 1 and 2, and 3, respectively. Vanadium in these structures retains the +4 oxidation state, indicating exceptional crystal stability. The magnetic susceptibility of these compounds was measured, and all three materials were found to be paramagnetic down to 2 K. Compound 1 was further characterized by IR, UVvis spectroscopy, and thermal analysis.

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Synthesis, Structure, and Magnetic Properties of Hydroxo‐Bridged Vanadium Oxalate V₂O₂(OH)₂(C₂O₄)(H₂O)₂

Abstract: (1), which crystallizes in the triclinic system, space group P1 with a = 5.2405(10) Å, b = 5.7340(11) Å, c = 7.1778(14) Å, α = 76.44(3)°, β = 69.37(3)°, γ = 75.37(3)°. The vanadium atoms in 1 form dimers by sharing edges consisting of µ-OH groups, and these dimers are con-

Cited by 10 publications

References 29 publications

Diverse Family of Layered Frustrated Magnets with Tailorable Interlayer Interactions

Diverse Family of Layered Frustrated Magnets with Tailorable Interlayer Interactions

Facile Synthesis, Structure Elucidation, and Magnetic Properties of Perovskite BaTb_1–xBi_xO₃

Observation of Multiple Crystal-to-Crystal Transitions in a New Reduced Vanadium Oxalate Hybrid Material, Ba₃[(VO)₂(C₂O₄)₅(H₂O)₆]·(H₂O)₃, Prepared via a Mild, Two-Step Hydrothermal Method

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Synthesis, Structure, and Magnetic Properties of Hydroxo‐Bridged Vanadium Oxalate V2O2(OH)2(C2O4)(H2O)2

Abstract: (1), which crystallizes in the triclinic system, space group P1 with a = 5.2405(10) Å, b = 5.7340(11) Å, c = 7.1778(14) Å, α = 76.44(3)°, β = 69.37(3)°, γ = 75.37(3)°. The vanadium atoms in 1 form dimers by sharing edges consisting of µ-OH groups, and these dimers are con-

Cited by 10 publications

References 29 publications

Diverse Family of Layered Frustrated Magnets with Tailorable Interlayer Interactions

Diverse Family of Layered Frustrated Magnets with Tailorable Interlayer Interactions

Facile Synthesis, Structure Elucidation, and Magnetic Properties of Perovskite BaTb1–xBixO3

Observation of Multiple Crystal-to-Crystal Transitions in a New Reduced Vanadium Oxalate Hybrid Material, Ba3[(VO)2(C2O4)5(H2O)6]·(H2O)3, Prepared via a Mild, Two-Step Hydrothermal Method

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Synthesis, Structure, and Magnetic Properties of Hydroxo‐Bridged Vanadium Oxalate V₂O₂(OH)₂(C₂O₄)(H₂O)₂

Facile Synthesis, Structure Elucidation, and Magnetic Properties of Perovskite BaTb_1–xBi_xO₃

Observation of Multiple Crystal-to-Crystal Transitions in a New Reduced Vanadium Oxalate Hybrid Material, Ba₃[(VO)₂(C₂O₄)₅(H₂O)₆]·(H₂O)₃, Prepared via a Mild, Two-Step Hydrothermal Method