Solvothermal Synthesis and Characterization of Two Iron Complexes

2011 ◽  
Vol 492 ◽  
pp. 324-327
Author(s):  
Ya Wei Hu ◽  
Yang Min Ma

Two iron complexes, Fe3(dtdb)2(HCO2)2(DMF)2(H2O)2(1) and Fe(bpy)(Hdtdb)(H2O) (2) were solvothermally synthesized and characterized by single crystal X-ray diffraction. Fe3(dtdb)2(HCO2)2(DMF)2(H2O)2 (1) shows 2D layer structure crystallized in a triclinic with space group P-1 and cell parameters, a = 8.5591(10) nm, b = 11.2502(13) nm, c = 11.4370(14) nm, α = 90.687(2)º, β = 110.275(2)º , γ = 90.712(2)º, and Z = 1. Fe(bpy)(Hdtdb)(H2O) (2) shows surper- molecular architecture crystallized in a triclinic with space group P-1 and cell parameters, a = 8.286(12) nm, b = 11.5937(16) nm, c = 11.8477(17) nm, α = 93.932(3)º, β = 102.442(3)º, γ = 97.117(3)º, and Z = 1.

2014 ◽  
Vol 602-603 ◽  
pp. 19-22 ◽  
Author(s):  
Lin Qiang Gao ◽  
Hai Yan Chen ◽  
Zhen Wang ◽  
Xin Zou

Nanoscale LiTaO3 powders with perovskite structure were synthesized using the solvothermal technique with glycol as solvent at 240°C for 12h. The powders were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). XRD was used to elucidate room temperature structures using Rietveld refinement. The powders were pure single pervoskite phase with high crystallinity. FESEM and TEM were used to determine particle size and morphology. The average LiTaO3 grain size was estimated to be < 200nm, and TEM images indicated that LiTaO3 particles had a brick-like morphology. In addition, the effect of the temperature on the LiTaO3 power characterisitics was also detailed studied.


2000 ◽  
Vol 53 (8) ◽  
pp. 687 ◽  
Author(s):  
Noah A. Epstein ◽  
Jennifer L. Horton ◽  
Christopher M. Vogels ◽  
Nicholas J. Taylor ◽  
Stephen A. Westcott

We have prepared four N-substituted hydroxypyridinones containing alcohol and morpholine groups. Complexes of the type cis-MoO2L2, where L represents the hydroxypyridinonato ligands have also been synthesized. The ethanolamine derivative, cis-MoO2(hep)2 (5), has been characterized by an X-ray diffraction study whereby the pyridinone ligands are bound to molybdenum in a cis bidentate fashion via the deprotonated hydroxy groups and the ketone moieties. Crystals of (5) are triclinic, with a 9.1930(7), b 14.2718(8), c 14.6219(9) Å, α 106.816(5), β 95.902(5), γ 96.350(5)°, Z 4, space group P–1.


2017 ◽  
Vol 72 (9) ◽  
pp. 677-685
Author(s):  
Teresa S. Ortner ◽  
Hubert Huppertz

AbstractThe praseodymium borate-nitrate Pr[B5O8(OH)(H2O)0.87]NO3·2H2O was obtained in a hydrothermal synthesis. It crystallizes monoclinically in the space groupP21/n(no. 14) with four formula units (Z=4) and unit cell parameters ofa=641.9(3),b=1551.8(7),c=1068.4(5) pm, withβ=90.54(2)° yieldingV=1.0643(8) nm3. The defect variant constitutes the missing member in the series of isostructural, early rare earth borate-nitrates of the compositionRE[B5O8(OH)(H2O)x]NO3·2H2O [RE=La (x=0; 1), Ce (x=1), Nd (x=0.85), Sm (x=0)]. In addition to powder and single-crystal X-ray diffraction data, the novel borate-nitrate was characterized through IR and Raman spectroscopy.


2014 ◽  
Vol 29 (4) ◽  
pp. 379-382 ◽  
Author(s):  
Sandra Amaya ◽  
Johana Arboleda ◽  
Adriana Echavarría

A new trimetallic compound with formula (NH4)Ni2.4Co0.6O(OH)(MoO4)2•1.5H2O was obtained by hydrothermal synthesis. The solid was characterized by X-ray diffraction, thermal analysis (thermogravimetric analysis and differential thermal analysis), Fourier-transformed infrared spectroscopy, Laser Raman spectroscopy, and chemical analysis by atomic absorption, confirming the formation of the layered phase ϕy. Crystallographic studies showed that the compound obtained is trigonal with hexagonal unit-cell parameters, a = 6.0468 ± 0.0016 Å and c = 21.8433 ± 0.0001 Å, and space group R-3m.


1998 ◽  
Vol 12 (11) ◽  
pp. 427-431
Author(s):  
K. Jeyabalan ◽  
L. K. Kaliyaperumal ◽  
A. Sekar ◽  
J. Srinivas

Synthesis and characterization of A 2 CaCuO 5( A=Nd, Sm ) system is reported. Powder X-ray diffraction analysis shows that the compounds crystallizes in an orthorhombic crystal systems and the unit cell parameters are found to be a=6.399(9)Å, b=7.218(8) Å and c=12.167(17) Å for Nd 2 CaCuO 5 and a=5.872(8) Å, b=7.457(3) Å and c=12.682(18) Å for Sm 2 CaCuO 5.


2014 ◽  
Vol 912-914 ◽  
pp. 318-320 ◽  
Author(s):  
Yin Xia Chen ◽  
Xian Bing Ji ◽  
Yu Lian Quan

Hierarchical calcium carbonate spheres composed of nanoparticles has been successfully synthesized via a solvothermal process. The structures are fabricated by the reaction of Ca (CH3COO)2with (CO(NH2)2) at 110 °C in diethylene glycolwater mixed solvents in the presence of polyvinylpyrrolidone. The as-prepared products were characterized by field emission scanning electron microscopy (FESEM) and X-ray diffraction (XRD). The characterization results revealed that the average diameter of the hierarchical calcium carbonate spheres is about 5 μm, and the size of the nanoparticals range from 50 to 100 nm. In addition, a small amount of bundle-like aragonite calcium carbonate is also obtained in the experimental parameters.


Nanoscale ◽  
2020 ◽  
Vol 12 (15) ◽  
pp. 8511-8518 ◽  
Author(s):  
Nils Lau Nyborg Broge ◽  
Frederik Søndergaard-Pedersen ◽  
Martin Roelsgaard ◽  
Xenia Hassing-Hansen ◽  
Bo Brummerstedt Iversen

The redox properties of five common solvents under solvothermal conditions are demonstrated through synthesis and characterization of 3d metal based materials.


2004 ◽  
Vol 817 ◽  
Author(s):  
Fushan Wen ◽  
Jiesheng Chen ◽  
Jin Hyeok Kim ◽  
Taeun Kim ◽  
Wenlian Li

AbstractA new 3-dimensional zinc carbonate Zn(NH3)CO3 has been synthesized from a glycol system with urea and zinc acetate as raw materials. The crystal structure and photoluminescent properties have been investigated using X-ray diffraction, smart CCD and FL. The compound had an orthorhombic system with space group of Pna21 with M = 142.41, a = 9.1449(18) Å, b = 7.5963(15) Å, c = 5.4982(11) Å, V = 381.95(13) Å3, Z = 4, R = 0.0285 and RW = 0.0745. The NH3 and CO32- were connected through the Zn-N bond and Zn-O bond in the symmetric unit. Photoluminescent property was observed in the compound at room temperature and the exited and emission peaks were located at about 350 nm and 426 nm, respectively.


2020 ◽  
Vol 75 (1-2) ◽  
pp. 83-90
Author(s):  
Christiane Stoll ◽  
Markus Seibald ◽  
Hubert Huppertz

AbstractThe potassium oxidofluoridostannate(IV) fluoride K5Sn2OF11 was synthesized via a solid-state route at T = 300°C in arc-weldeded copper ampoules. It crystallizes in the orthorhombic system in the acentric space group Ama2 (no. 40) with a unit cell volume of V = 2.5727(4) nm3. The cell parameters are a = 1758.3(2), b = 2452.3(2) and c = 596.7(1) pm. As a main structural motif, K5Sn2OF11 exhibits two different kinds of dinuclear [Sn2OF11]5‒ units, which are embedded into a matrix consisting of potassium cations and fluoride anions. The substance was characterized by single-crystal and powder X-ray diffraction, as well as by FT-IR spectroscopy.


2021 ◽  
Vol 12 (2) ◽  
pp. 2586-2602

The triphosphate dodecahydrate of cobalt and sodium CoNa3P3O10.12H2O was prepared by the ion exchange resin process. Its structure was studied by X-ray diffraction and determined in the monoclinic space group P121/c1with the unit-cell parameters a = 14.6650(5) Å, b=9.1916(3) Å, c = 15.0239(5) Å, =90.2210(10) °, Z = 4 and V = 2025.13(12) Å3. The thermal dehydration of this compound was performed, leading to an anhydrous new form, CoNa3P3O10, which was characterized by X-ray diffraction. The obtained CoNa3P3O10 crystallized in monoclinic space group P21/n with the unit-cell parameters a=15,3774 Å, b=7,6988 A°, c=14,2832A°, β=92,9115°.The characteristic IR wavenumbers of the P3O105− ions observed in the vibrational spectra were calculated using isotopic substitutions, which confirms the existence of these groups in the studied compound. A comparison between the IR and Raman wavenumbers of CoNa3P3O10.12H2O, CoNa3P3O10 and Na5P3O10.12H2O was performed. A kinetic study was also made for CoNa3P3O10·12H2O.


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