K2FeIII0.5TiIII0.5TiIV1.0(PO4)3: Preparation and Characterization of a Langbeinite-related Phosphate Containing Iron(III) and Mixed-valent Titanium

2008 ◽  
Vol 63 (3) ◽  
pp. 261-266 ◽  
Author(s):  
Ivan V. Ogorodnyk ◽  
Igor V. Zatovsky ◽  
Vyacheslav N. Baumer ◽  
Nikolay S. Slobodyanik ◽  
Oleg V. Shishkin ◽  
...  

A potassium mixed iron(III)-titanium(III)-titanium(IV) phosphate K2FeIII0.5TiIII0.5TiIV1.0(PO4)3 has been obtained using a two-step flux interaction in evacuated sealed silica tubes. It forms tetrahedrally-shaped dark violet crystals which belong to the cubic system (space group P213) with the cell parameter a = 9.8592(5) Å . The structure was refined from single-crystal X-ray diffraction data. [MO6] octahedra and [PO4] tetrahedra share their vertices forming a rigid 3D framework. The potassium cations are located in large closed cavities of the framework. A distribution of the 3d metals’ valence states in K2FeIII0.5TiIII0.5TiIV1.0(PO4)3 has been proposed on the basis of magnetic measurements, structure investigations and bond-valence calculations as well as UV/vis and EPR spectroscopy.

1984 ◽  
Vol 39 (2) ◽  
pp. 185-188 ◽  
Author(s):  
Hidenari Inoue ◽  
Ekkehard Fluck

Three compounds of the type Ti[MB(CN)6] (MB = Co, Rh, and Ir) have been synthesized and characterized by means of their X-ray diffraction powder patterns, magnetic measurements, infrared, electronic, and X-ray photoelectron spectra. All compounds crystallize in the facecentered cubic system and form a three-dimensional framework of two octahedral coordination units MBC6 and TiN6. Upon the formation of Ti[MB(CN)6] from the corresponding potassium salt, the π back-donation in the [MB(CN)6]3- moiety is enhanced by the bridge formation through the cyanide ligand


2003 ◽  
Vol 793 ◽  
Author(s):  
Arwyn L. E. Smalley ◽  
Brandon Howe ◽  
David C. Johnson

ABSTRACTA series of cerium-containing CoSb3 samples were synthesized, with cerium quantities varying from 0 to 2 stoichiometric equivalents. These samples were annealed at low temperatures to crystallize the kinetically stable phases CexCo4Sb12 (x = 0–0.5). X-ray diffraction showed that these samples were phase pure, and Rietveld analysis on x-ray diffraction data from powder samples indicated that these samples were 25–88% crystalline. Electrical measurements showed that these samples are n-type, which was previously unknown in CexCo4Sb12. Magnetic measurements showed that the samples were paramagnetic due to the cerium being incorporated into the diamagnetic CoSb3 compound. In addition, they contained a ferromagnetic component that was attributed to the amorphous, cerium-containing phase.


1996 ◽  
Vol 11 (4) ◽  
pp. 268-275 ◽  
Author(s):  
Winnie Wong-Ng ◽  
F. Jiang ◽  
Bryan R. Jarabek ◽  
Gregory J. McCarthy

Powder X-ray diffraction was used to investigate the solid solution range of the Bi14SrxCa12−xO33 series in the Bi–Sr–Ca–O system. Solid solution forms over the range 1≤x≤7 in Bi14SrxCa12−xO33. Experimental X-ray reference patterns of selected members with x=1, 3, 5, and 7 have been prepared for the powder diffraction file (PDF). These phases are monoclinic, C2/m, with cell parameter a ranging from 21.473(4) to 21.868(4) Å, b from 4.3564(9) to 4.3898(9) Å, c from 12.753(2) to 12.962(2) Å, β from 102.91(2)° to 102.79(1)°, and V from 1162.9(3) to 1213.5(3) Å3, respectively. These parameters increase monotonically as Ca is continuously replaced by the larger Sr.


1989 ◽  
Vol 46 (2) ◽  
pp. 281-296 ◽  
Author(s):  
C. Hoang-Van ◽  
Y. Kachaya ◽  
S.J. Teichner ◽  
Y. Arnaud ◽  
J.A. Dalmon

Author(s):  
Vera Pavlova ◽  
Elena Murashova

Abstract Ternary intermetallic compound Sm2Ru3Sn5 was synthesized in the system Sm-Ru-Sn by arc-melting and annealing at 600 °C in the field with high content of Sn. Its crystal structure was determined using single crystal X-ray diffraction data (at 240 K). The compound crystallizes in cubic system with space group I 4 ‾ 3m (No. 217), unit cell parameter is a = 9.4606 (8) Å, Z = 4, Pearson symbol c/40. The intermetallic compound Sm2Ru3Sn5 represents an ordered version of the centrosymmetric Ru3Sn7 structure (space group Im 3 ‾ m), in which 16f Sn-filled crystallographic site is split into two 8c sites, each of which is solely occupied of one sort of atoms – Sn or Sm. The occupation of these two 8c sites leads to a reduction of symmetry due to the removal of the inversion center.


Crystals ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 812
Author(s):  
Noura Othman Alzamil ◽  
Ghareeba Mussad Al-Enzi ◽  
Aishah Hassan Alamri ◽  
Insaf Abdi ◽  
Amor BenAli

Two new nonmetal cation tetrafluoroborate phases [H3tren](BF4)3 (I) and [H3tren](BF4)3 HF (II) were synthesized by microwave-assisted solvothermal and characterized by single crystal X-ray diffraction, IR spectroscopy and thermal analysis DTA-TGA. [H3tren](BF4)3 is cubic (P213) with unit cell parameter a = 11.688(1) Å. [H3tren](BF4)3•HF is trigonal (R3c) with unit cell parameters a = 15.297(6) Å and c = 12.007(2) Å. Both (I) and (II) structures can be described from isolated tetrafluoroborate BF4- anions, triprotonated tris-(2-aminoethyl)amine (tren) [H3tren]3+. Phase (II) contains disordered BF4- tetrahedron and hydrofluoric acid.


Nanomaterials ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 1959
Author(s):  
Matjaž Kristl ◽  
Sašo Gyergyek ◽  
Srečo D. Škapin ◽  
Janja Kristl

The paper reports the synthesis of nickel tellurides via a mechanochemical method from elemental precursors. NiTe, NiTe2, and Ni2Te3 were prepared by milling in stainless steel vials under nitrogen, using milling times from 1 h to 12 h. The products were characterized by powder X-ray diffraction (pXRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS), vibrating sample magnetometer (VSM), UV-VIS spectrometry, and thermal analysis (TGA and DSC). The products were obtained in the form of aggregates, several hundreds of nanometers in size, consisting of smaller nanosized crystallites. The magnetic measurements revealed a ferromagnetic behavior at room temperature. The band gap energies calculated using Tauc plots for NiTe, NiTe2, and Ni2Te3 were 3.59, 3.94, and 3.70 eV, respectively. The mechanochemical process has proved to be a simple and successful method for the preparation of binary nickel tellurides, avoiding the use of solvents, toxic precursors, and energy-consuming reaction conditions.


2004 ◽  
Vol 98 (4) ◽  
pp. 203-210 ◽  
Author(s):  
P. Dutta ◽  
N. O. Elbashir ◽  
A. Manivannan ◽  
M. S. Seehra ◽  
C. B. Roberts

2022 ◽  
Vol 3 (1) ◽  
pp. 41-52
Author(s):  
Michael Vogl ◽  
Martin Valldor ◽  
Roman Boy Piening ◽  
Dmitri V. Efremov ◽  
Bernd Büchner ◽  
...  

We present the synthesis and characterization of the iridium-based sulfide Ca1−xIr4S6(S2). Quality and phase analysis were conducted by means of energy-dispersive X-ray spectroscopy (EDXS) and powder X-ray diffraction (XRD) techniques. Structure analysis reveals a monoclinic symmetry with the space group C 1 2/m 1 (No. 12), with the lattice constants a = 15.030 (3) Å, b = 3.5747 (5) Å and c = 10.4572 (18) Å. Both X-ray diffraction and EDXS suggest an off-stoichiometry of calcium, leading to the empirical composition Ca1−xIr4.0S6(S2) [x = 0.23–0.33]. Transport measurements show metallic behavior of the compound in the whole range of measured temperatures. Magnetic measurements down to 1.8 K show no long range order, and Curie–Weiss analysis yields θCW = −31.4 K, suggesting that the compound undergoes a magnetic state with short range magnetic correlations. We supplement our study with calculations of the band structure in the framework of the density functional theory.


2003 ◽  
Vol 58 (10) ◽  
pp. 1009-1014 ◽  
Author(s):  
Subrata Kumar Dey ◽  
Bappaditya Bag ◽  
Dilip Kumar Dey ◽  
V. Gramlich ◽  
Yadong Li ◽  
...  

The synthesis, structure, and physical properties of a series of mononuclear complexes viz. [Cu(L)2] 1, [CuL2(CH3O)2] 2 and [Zn(L)2] 3 (where L = 1-Phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP)) are presented. The complexes were characterized by elemental analysis, IR and electronic spectroscopy (1 and 2), magnetic measurements at room temperature (1 and 2) and thermogravimetric analysis. The structures of all the three complexes were determined by single crystal X-ray diffraction studies. The coordination geometry around complexes CuL2 (1) and ZnL2 (3) is slightly distorted square planar while the geometry around Cu(II) of [Cu(L)2(CH3O)2] (2) is distorted octahedral with four oxygen atoms of two PMBP ligand occupying the equatorial positions and two methanol molecules occupying the two axial positions.


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