Synthesis and X-ray characterization of Li(1−2x)NixTiO(PO4) (0≤x≤0.50)

2003 ◽  
Vol 18 (4) ◽  
pp. 301-305 ◽  
Author(s):  
B. Manoun ◽  
A. El Jazouli ◽  
P. Gravereau ◽  
J. P. Chaminade
Keyword(s):  
Dilute Solutions ◽  
Final Temperature ◽  
Monoclinic System ◽  
Orthorhombic System ◽  
Space Group ◽  
X Ray

Li(1−2x)NixTiO(PO4) oxyphosphate powders were prepared from dilute solutions of NiCl2⋅6H2O, Li2CO3, (NH4)2HPO4, and TiCl4 in ethanol. The final temperature was 850 °C. Li(1−2x)NixTiO(PO4) oxyphosphates with 0≤x≤0.10 crystallize in the orthorhombic system with space group Pnma, while those with 0.10<x≤0.25 crystallize in the monoclinic system with space group P21/c.

Synthesis and X-ray powder diffraction characterization of tetra- and hexa-imidazole complexes of magnesium(II)

2008 ◽  
Vol 23 (4) ◽  
pp. 286-291 ◽  
Author(s):  
Norberto Masciocchi ◽  
Luigi Garlaschelli ◽  
Giulia Peli
Keyword(s):  
Powder Diffraction ◽  
Molecular Structures ◽  
Water Molecules ◽  
Powder Diffraction Data ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Imidazole Complexes ◽  
Full Profile

X-ray powder diffraction data for two ionic salts containing imidazole (Him) complexes of the magnesium(II) ion, [Mg(Him)4(H2O)2]Cl2 and [Mg(Him)6](NO3)2, are reported. Their crystal and molecular structures were determined by simulated annealing and full-profile Rietveld refinement methods. [Mg(Him)4(H2O)2]Cl2 was found to crystallize in the monoclinic system with space group C2/c, a=12.3980(3) Å, b=11.0234(2) Å, c=14.4691(3) Å, and β=107.024(1)°. [Mg(Him)6](NO3)2 crystallizes in the trigonal R-3 space group with a=b=12.4631(4) Å and c=14.9449(6) Å. Both species contain centrosymmetric complexes, and Mg is octahedrally coordinated by six imidazoles, as in [Mg(Him)6](NO3)2, or by four imidazoles and two water molecules, as in [Mg(Him)4(H2O)2]Cl2. Additional analytic, thermogravimetric, calorimetric, and spectroscopic characterizations were also performed.

X-ray powder diffraction studies of aniline derivatives

2003 ◽  
Vol 18 (3) ◽  
pp. 266-268
Author(s):  
A. Rafalska-Łasocha ◽  
W. Łasocha
Keyword(s):  
Powder Diffraction ◽  
Room Temperature ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Orthorhombic System ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Aniline Derivatives ◽  
Diffraction Patterns

The X-ray powder diffraction patterns of two liquid aniline derivatives o-chloroaniline, and m-chloroaniline were measured at 250 °K in a low temperature chamber. Both compounds crystallize in the orthorhombic system with the unit cell parameters refined to a=1.8391(3) nm, b=1.0357(2) nm, c=0.6092(1) nm, space group Pmmm(47) and a=0.450 39(9) nm, b=1.9820(4) nm, c=1.2699(4) nm, space group Pcca(54) for o-chloroaniline and m-chloroaniline, respectively. Investigated at room temperature, 2,6-dichloroaniline crystallizes in the monoclinic system, space group P21/c(14), a=1.1329(2) nm, b=0.41093(8) nm, c=1.5445(3) nm, α=γ=90° β=99.96(2)°.

Synthesis and X-ray characterization of Li0.5M0.25TiOAsO4 (M=Mg,Co,Ni,Zn) oxyarsenates

2006 ◽  
Vol 21 (3) ◽  
pp. 229-235 ◽  
Author(s):  
M. Chakir ◽  
A. El Jazouli ◽  
J. P. Chaminade
Keyword(s):  
Coprecipitation Method ◽  
Dilute Solution ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Ion Size ◽  
New Compounds

Li0.5M0.25TiOAsO4 (M=Mg,Co,Ni,Zn) oxyarsenates powders were prepared by coprecipitation method from dilute solution of Li2CO3,M(NO3)2×H2O (M=Mg,Co,Ni,Zn), (NH4)H2AsO4 and TiCl4 in ethanol. The resulting powders, obtained after drying at about 60 °C, were heated progressively with intermittent grindings at 200 °C–750 °C in air. These new compounds crystallize in the monoclinic system with space group P21∕c. Their parameters are functions of M2+ ion size.

Powder diffraction investigations of 2,2′-Thiobis(4-methyl-6-tert-butylphenol) and 2,2′-Methylenebis(4-methyl-6-tert-butylphenol)

2005 ◽  
Vol 20 (1) ◽  
pp. 67-70
Author(s):  
B. Lasocha ◽  
M. Grzywa ◽  
W. Lasocha
Keyword(s):  
Room Temperature ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Orthorhombic System ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Phenol Derivatives

X-ray diffraction investigations of two phenol derivatives - 2,2′-Thiobis(4-methyl-6-tert-butylphenol) and 2,2′-Methylenebis(4-methyl-6-tert-butylphenol) were carried out. Both compounds at room temperature have similar cell volume and the same number of molecules in an unit cell. However, 2,2′-Thiobis(4-methyl-6-tert-butylphenol) crystallizes in the monoclinic system with unit cell parameters refined to a=0.8278(2) nm, b=1.2968(4) nm, c=1.9493(7) nm, β=90.93(2)°, space group P21∕n(14), whereas 2,2′-Methylenebis(4-methyl-6-tert-butylphenol) crystallizes in the orthorhombic system with unit cell parameters refined to a=1.6203(5) nm, b=1.2827(5) nm, c=1.0197(3) nm, space group Pna21(33). The investigated C22H30O2S turned out to be a new polymorph of 2,2′-Thiobis(4-methyl-6-tert-butylphenol).

X-ray powder diffraction study of DMAN complexes with phthalic acids

2005 ◽  
Vol 20 (1) ◽  
pp. 62-66
Author(s):  
A. Rafalska-Lasocha ◽  
K. Surówka ◽  
W. Lasocha
Keyword(s):  
Diffraction Study ◽  
Powder Diffraction ◽  
Terephthalic Acid ◽  
Phthalic Acid ◽  
Lattice Parameters ◽  
Monoclinic System ◽  
Orthorhombic System ◽  
Space Group ◽  
X Ray ◽  
Phthalic Acids

Complexes of 1,8-bis(dimethylamino)naphthalene, known also as DMAN, with phthalic acid, terephthalic acid, and 5-aminoisophthalic acid were synthesized and investigated by means of powder diffraction methods. DMAN and phthalic acid complexes crystallize in the orthorhombic system, space group Pnmm (59) with the lattice parameters a=1.17423(3) nm, b=1.7124(4) nm, c=0.9933(4) nm, V=1.997 24 nm3, whereas DMAN complexes with terephthalic acid or 5-aminoisophthalic acid crystallize in the monoclinic system in the space group P2 or P2∕m with the lattice parameters a=2.4337(5) nm, b=0.9665(2) nm, c=1.1800(3) nm, β=91.53(2)°, V=2.774 51 nm3 and a=2.1609(7) nm, b=1.1017(6) nm, c=1.8921(7) nm, β=112.095(34)°, V=4.173 46 nm3, respectively.

scholarly journals Kinetic Analysis of the Thermal Decomposition of Iron(III) Phosphates: Fe(NH3)2PO4 and Fe(ND3)2PO4

2020 ◽  
Vol 21 (3) ◽  
pp. 781
Author(s):  
Isabel Iglesias ◽  
José A. Huidobro ◽  
Belén F. Alfonso ◽  
Camino Trobajo ◽  
Aránzazu Espina ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Kinetic Analysis ◽  
Room Temperature ◽  
Isoconversional Methods ◽  
Iron Phosphate ◽  
Dihydrogen Phosphate ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Group A

The hydrothermal synthesis and both the chemical and structural characterization of a diamin iron phosphate are reported. A new synthetic route, by using n-butylammonium dihydrogen phosphate as a precursor, leads to the largest crystals described thus far for this compound. Its crystal structure is determined from single-crystal X-ray diffraction data. It crystallizes in the orthorhombic system (Pnma space group, a = 10.1116(2) Å, b = 6.3652(1) Å, c = 7.5691(1) Å, Z = 4) at room temperature and, below 220 K, changes towards the monoclinic system P21/n, space group. The in situ powder X-ray thermo-diffraction monitoring for the compound, between room temperature and 1100 K, is also included. Thermal analysis shows that the solid is stable up to ca. 440 K. The kinetic analysis of thermal decomposition (hydrogenated and deuterated forms) is performed by using the isoconversional methods of Vyazovkin and a modified version of Friedman. Similar values for the kinetic parameters are achieved by both methods and they are checked by comparing experimental and calculated conversion curves.

Distorted chiolite crystal structures of α-Na5M3F14 (M=Cr,Fe,Ga) studied by X-ray powder diffraction

2003 ◽  
Vol 18 (2) ◽  
pp. 128-134 ◽  
Author(s):  
A. Le Bail ◽  
A.-M. Mercier
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Rietveld Refinements ◽  
Space Group ◽  
X Ray ◽  
Precise Characterization

The crystal structures of the chiolite-related room temperature phases α-Na5M3F14 (MIII=Cr,Fe,Ga) are determined. For all of them, the space group is P21/n, Z=2; a=10.5096(3) Å, b=7.2253(2) Å, c=7.2713(2) Å, β=90.6753(7)° (M=Cr); a=10.4342(7) Å, b=7.3418(6) Å, c=7.4023(6) Å, β=90.799(5)° (M=Fe), and a=10.4052(1) Å, b=7.2251(1) Å, c=7.2689(1), β=90.6640(4)° (M=Ga). Rietveld refinements produce final RF factors 0.036, 0.033, and 0.035, and RWP factors, 0.125, 0.116, and 0.096, for MIII=Cr, Fe, and Ga, respectively. The MF6 polyhedra in the defective isolated perovskite-like layers deviate very few from perfect octahedra. Subtle octahedra tiltings lead to the symmetry decrease from the P4/mnc space group adopted by the Na5Al3F14 chiolite aristotype to the P21/n space group adopted by the title series. Facile twinning precluded till now the precise characterization of these compounds.

Crystallographic characterization of three cathinone hydrochlorides new on the NPS market: 1-(4-methylphenyl)-2-(pyrrolidin-1-yl)hexan-1-one (4-MPHP), 4-methyl-1-phenyl-2-(pyrrolidin-1-yl)pentan-1-one (α-PiHP) and 2-(methylamino)-1-(4-methylphenyl)pentan-1-one (4-MPD)

2022 ◽  
Vol 78 (1) ◽  
Author(s):  
Marcin Rojkiewicz ◽  
Piotr Kuś ◽  
Maria Książek ◽  
Joachim Kusz
Keyword(s):  
Chemical Structure ◽  
Crystallographic Data ◽  
New Psychoactive Substances ◽  
Monoclinic Space Group ◽  
Psychoactive Substances ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Analytical Laboratories

Cathinones belong to a group of compounds of great interest in the new psychoactive substances (NPS) market. Constant changes to the chemical structure made by the producers of these compounds require a quick reaction from analytical laboratories in ascertaining their characteristics. In this article, three cathinone derivatives were characterized by X-ray crystallography. The investigated compounds were confirmed as: 1-[1-(4-methylphenyl)-1-oxohexan-2-yl]pyrrolidin-1-ium chloride (1, C17H26NO+·Cl−, the hydrochloride of 4-MPHP), 1-(4-methyl-1-oxo-1-phenylpentan-2-yl)pyrrolidin-1-ium chloride (2; C16H24NO+·Cl−, the hydrochloride of α-PiHP) and methyl[1-(4-methylphenyl)-1-oxopentan-2-yl]azanium chloride (3; C13H20NO+·Cl−, the hydrochloride of 4-MPD). All the salts crystallize in a monoclinic space group: 1 and 2 in P21/c, and 3 in P21/n. To the best of our knowledge, this study provides the first detailed and comprehensive crystallographic data on salts 1–3.

Darstellung, Reaktionen und spektroskopische Charakterisierung von [Os2X8]2-, X = Cl, Br, I, und Kristallstruktur von (PPN)2[Os2I8] · 2 CH2Cl2 / Preparation, Reactions and Spectroscopic Characterization of [Os2X8]2-, X = Cl, Br, I, and Crystal Structure of (PPN)2[Os2I8] · 2 CH2Cl2

1990 ◽  
Vol 45 (10) ◽  
pp. 1416-1424 ◽  
Author(s):  
W. Preetz ◽  
P. Hollmann ◽  
G. Thiele ◽  
H. Hillebrecht
Keyword(s):  
Crystal Structure ◽  
Structure Determination ◽  
Triple Bond ◽  
Room Temperature ◽  
Spectroscopic Characterization ◽  
Spectroscopic Constants ◽  
Monoclinic System ◽  
X Ray ◽  
Fine Structures

The triply bonded octahalogenodiosmate(III) anions [Os2X8]2-, previously known with X = Cl, Br, have now been extended to include the iodide with two staggered OsI4 units. This compound was prepared by treating [Os2Cl8]2- with Nal at room temperature in acetone solution. The structure determination by X-ray diffractometry on single crystals of (PPN)2[Os2I8] · 2 CH2Cl2, reveals crystallization in the monoclinic system, space group P21/c with Z = 4. The Os-Os triple bond is with 2.212(1) Å the longest within the three octahalogenodiosmates(III). The Raman spectra show ν(OsOs) at 285, [Os2Cl8]2-; at 287, [Os2Br8]2- and for the iodo compound at 270.1 cm-1 with up to three overtones. The spectroscopic constants are calculated to be ω1 = 270.9 cm-1; X11 = -0.50 cm-1. The 10 Κ UV-VIS spectra of solid [(n-C4H9)4N]2[Os2X8] exhibit δ-π* transitions with maxima at 723, 690 and 643 nm, superimposed by vibrational fine structures with long progressions of 195, 211 and 183 cm-1 for X = Cl, Br, I, respectively. Oxidation of [Os2X8]2-, X = Cl, Br with the corresponding halogen leads to the cleavage of the Os-Os bond, and the dekahalogenodiosmates(IV), [Os2X10]2-, are formed

scholarly journals Serendipitous formation and characterization of K2[Pd(NO3)4]·2HNO3

2019 ◽  
Vol 74 (4) ◽  
pp. 381-387
Author(s):  
Michael Zoller ◽  
Jörn Bruns ◽  
Gunter Heymann ◽  
Klaus Wurst ◽  
Hubert Huppertz
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Monoclinic Space Group ◽  
Solvothermal Process ◽  
X Ray Diffraction ◽  
Glass Ampoule ◽  
Space Group ◽  
X Ray ◽  
Complex Anions

AbstractA potassium tetranitratopalladate(II) with the composition K2[Pd(NO3)4] · 2HNO3 was synthesized by a simple solvothermal process in a glass ampoule. The new compound crystallizes in the monoclinic space group P21/c (no. 14) with the lattice parameters a = 1017.15(4), b = 892.94(3), c = 880.55(3) Å, and β = 98.13(1)° (Z = 2). The crystal structure of K2[Pd(NO3)4] · 2HNO3 reveals isolated complex [Pd(NO3)4]2− anions, which are surrounded by eight potassium cations and four HNO3 molecules. The complex anions and the cations are associated in layers which are separated by HNO3 molecules. K2[Pd(NO3)4] · 2HNO3 can thus be regarded as a HNO3 intercalation variant of β-K2[Pd(NO3)4]. The characterization is based on single-crystal X-ray and powder X-ray diffraction.

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