scholarly journals Transition metal complexes with pyrazole based ligands, part 27: Structural and thermal characterization of cobalt(II) halide and pseudohalide complexes with 4-acetyl-3-amino-5-methylpyrazole

2007 ◽  
Vol 72 (12) ◽  
pp. 1281-1293 ◽  
Author(s):  
Vukadin Leovac ◽  
Zoran Tomic ◽  
Katalin Mészáros-Szécsényi ◽  
Ljiljana Jovanovic ◽  
Milan Joksovic
Keyword(s):  
Thermal Decomposition ◽  
Solid State ◽  
Transition Metal Complexes ◽  
Thermal Characterization ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Vis Spectroscopy

The crystal and molecular structures of four tetrahedral structurally similar [Co(aamp)2X2] complexes (aamp = 4-acetyl-3-amino-5-methylpyrazole, X = Cl, Br, I and NCS) were determined by X-ray diffraction analysis and are discussed in detail. It was found that the different capacity of the ligand X (NCS vs. Cl, Br, I) for the formation of non-bonding contacts influence the mode of molecular association in the solid state. The complexes were characterized by UV-Vis spectroscopy. The first step of the thermal decomposition of the compounds was checked and is discussed in the view of the IR spectrum of the intermediate isolated from [Co(aamp)2Br2] by the quasi-isothermal technique.

Structural and spectroscopic characterization of isotypic sodium, rubidium and cesium acesulfamates

2015 ◽  
Vol 70 (7) ◽  
pp. 491-496 ◽  
Author(s):  
Oscar E. Piro ◽  
Gustavo A. Echeverría ◽  
Eduardo E. Castellano ◽  
Beatriz S. Parajón-Costa ◽  
Enrique J. Baran
Keyword(s):  
Aqueous Solutions ◽  
Single Crystal ◽  
Potassium Salt ◽  
Spectroscopic Characterization ◽  
Molecular Structures ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal And Molecular Structures

AbstractThree new acesulfamate salts, NaC4H4NO4S, RbC4H4NO4S and CsC4H4NO4S, were prepared by reactions in aqueous solutions and thoroughly characterized. Their crystal and molecular structures were determined by single crystal X-ray diffraction methods. They crystallize in the monoclinic space group P21/a with a = 7.2518(2), b = 8.9414(4), c = 10.5929(4) Å, β = 99.951(3)°, V = 676.52(4) Å3 for the Na salt; a = 7.4663(3), b = 9.6962(4), c = 10.4391(4) Å, β = 95.150(3)°, V = 752.68(5) Å3 for the Rb salt and a = 7.5995(4), b = 9.9439(4), c = 10.8814(6) Å, β = 91.298(5)°, V = 822.08(7) Å3 for the Cs salt, and Z = 4 molecules per unit cell. The three compounds are isotypic to each other and to the previously reported potassium salt. The metal ions are in irregular polyhedral coordination with six neighboring acesulfamate anions through their nitrogen and carbonyl and sulfoxide oxygen atoms. The FTIR spectra of the compounds were also recorded and are briefly discussed.

Unprecedented transformation of [I−·I3−] to [I42−] polyiodides in the solid state: structures, phase transitions and characterization of dipyrazolium iodide triiodide

2015 ◽  
Vol 44 (42) ◽  
pp. 18447-18458 ◽  
Author(s):  
M. Węcławik ◽  
P. Szklarz ◽  
W. Medycki ◽  
R. Janicki ◽  
A. Piecha-Bisiorek ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Phase Transitions ◽  
Solid State ◽  
Dielectric Measurements ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Solid State Structures

Dipyrazolium iodide triiodide, [C3N2H5+]2[I−·I3−], has been synthesized and studied by means of X-ray diffraction, differential scanning calorimetry, dielectric measurements, and UV-Vis spectroscopy.

Crystal and Molecular Structures of the Functional Lithium Cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph, Me

2000 ◽  
Vol 55 (11) ◽  
pp. 1005-1010 ◽  
Author(s):  
Ulrich Jürgen Bildmann ◽  
Martin Winkler ◽  
Gerhard Müller Fachbereich
Keyword(s):  
Solid State ◽  
Functional Group ◽  
Molecular Structures ◽  
The Other ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal and molecular structures of the phosphinomethyl-substituted lithium cyclopentadienides [Li(tmeda)][R2PCMe2C5H4], R = Ph (1), Me (2) (tmeda = N,N,N',N'-tetramethylethylenediamine) were determined as their tmeda adducts on the basis of low temperature single crystal X-ray diffraction. (Crystal data: 1: monoclinic, space group P21/n, a = 8.511(5), b = 11.936(2), c = 24.20(1) Å, β = 90.02(3)°, Z = 4.2: monoclinic, space group P21/n, a = 10.887(2), b = 13.326(2), c = 13.131(2) Å, β= 92.872(6)°, Z = 4). In both compounds lithium has a slightly distorted 17 coordination to the cyclopentadienide (Cp) ring. There are no interactions between lithium and the phosphine donors in the solid state as the phosphinomethyl substituents are oriented to the other side of the Cp ring for steric reasons. The isopropene-substituted lithium cyclopentadienide, which is formed as a by-product in the synthesis of phosphinomethyl cyclopentadienides containing a CMe2 bridge, was also structurally characterized as its tmeda adduct [Li(tmeda)][H2C=CMeC5H4] (3). (Crystal data: monoclinic, P21/c, a = 8.00(2), b = 16.701(2), c = 11.942(6) Å, β= 112.68(7)°, Z = 4). As in 1 and 2, lithium is η5 -coordinated to the Cp ring, and there is no interaction of the functional group (isopropene) with lithium.

The synthesis and structural characterization of linear and macrocyclic bis(dinitrosyliron) complexes supported by bis(phosphine) bridging ligands

2003 ◽  
Vol 81 (6) ◽  
pp. 468-475 ◽  
Author(s):  
Lijuan Li ◽  
Nada Reginato ◽  
Michael Urschey ◽  
Mark Stradiotto ◽  
John D Liarakos
Keyword(s):  
Solid State ◽  
Structural Characterization ◽  
Mononuclear Complex ◽  
Phosphine Ligands ◽  
Molecular Structures ◽  
X Ray Diffraction ◽  
Bridging Ligands ◽  
X Ray ◽  
Phosphine Complexes

Reactions involving Fe(NO)2(CO)2 and the bis(phosphine) ligands bis(diphenylphosphino)methane (DPPM), bis(diphenylphosphino)acetylene (DPPA), 1,6-bis(diphenylphosphino)hexane (DPPH), and 1,4-bis(diphenyl phosphino)benzene (DPPB) have been examined. From these reactions, the mononuclear complex, Fe(κ1-DPPM)(NO)2(CO) 3, linear dinuclear species of the type Fe2(µ-L)(NO)4(CO)2 (L = Ph2PCH2PPh2 4, Ph2PC[Formula: see text]CPPh2 5, Ph2PCH2(CH3)4CH2PPh2 6, and Ph2P(p-C6H4)PPh2 7), and macrocyclic dinuclear species of the type Fe2(µ-L)2(NO)4 (L = Ph2PCH2PPh2 8 and Ph2PC[Formula: see text]CPPh2 9) were isolated and spectroscopically characterized. For 4, 5, 8, and 9, the solid-state molecular structures of the products were determined by use of single-crystal X-ray diffraction techniques. Key words: dinitrosyliron, iron nitrosyls, dinuclear macrocycles, bis(phosphine) complexes.

Characterization of some mesogenic alkyl 1-thioglycosides

2002 ◽  
Vol 80 (8) ◽  
pp. 1162-1165 ◽  
Author(s):  
B Henrissat ◽  
G K Hamer ◽  
M G Taylor ◽  
R H Marchessault
Keyword(s):  
Phase Transition ◽  
Liquid Crystal ◽  
Solid State ◽  
Solid State Nmr ◽  
Liquid Crystalline ◽  
Liquid Crystal Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Liquid Crystalline Phases

A series of dodecyl 1-thio-β-D-glycosides has been synthesized and characterized (DSC, NMR, CP MAS, X-ray diffraction) as possible new marking materials with liquid-crystalline properties. These compounds undergo solid to liquid crystal phase transitions at various temperatures, which depend on the nature of the carbohydrate part of the structure. Their liquid-crystalline phases show extreme shear thinning behaviour.Key words: liquid crystal, powder X-ray diffraction, phase transition, thioglycoside, solid-state NMR, marking material

scholarly journals Characterization of a brazilian smectite by solid state NMR and X-ray diffraction techniques

1997 ◽  
Vol 8 (6) ◽  
pp. 581-586 ◽  
Author(s):  
Alcides Wagner Serpa Guarino ◽  
Rosane A. S. San Gil ◽  
Helena Polivanov ◽  
Sonia M.C. Menezes
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray

Lewis-Base Adducts of Group 1B Metal(I) Compounds. XXI The Crystal and Molecular Structures of the Unsolvated Forms of Dibromotris(triphenylphosphine)dicopper(I) and 'step' Tetrabromotetrakis(triphenyl-phosphine)tetracopper(I)

1985 ◽  
Vol 38 (8) ◽  
pp. 1243 ◽  
Author(s):  
JC Dyason ◽  
LM Engelhardt ◽  
C Pakawatchai ◽  
PC Healy ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Molecular Structures ◽  
Lewis Base ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
Triphenyl Phosphine ◽  
X Ray ◽  
Crystal And Molecular Structures

The crystal structures of the title compounds have been determined by single-crystal X-ray diffraction methods at 295 K. Crystal data for (PPh3)2CuBr2Cu(PPh3) (1) show that the crystals are iso-morphous with the previously studied chloro analogue, being monoclinic, P21/c, a 19.390(8), b 9.912(5), c 26.979(9) Ǻ, β 112,33(3)°; R 0.043 for No 3444. Cu( trigonal )- P;Br respectively are 2.191(3); 2.409(2), 2.364(2) Ǻ. Cu(tetrahedral)- P;Br respectively are 2.241(3), 2.249(3); 2.550(2), 2.571(2) Ǻ. Crystals of 'step' [PPh3CuBr]4 (2) are isomorphous with the solvated bromo and unsolvated iodo analogues, being monoclinic, C2/c, a 25.687(10), b 16.084(7), c 17.815(9) Ǻ, β 110.92(3)°; R 0.072 for No 3055. Cu( trigonal )- P;Br respectively are 2.206(5); 2.371(3), 2.427(2) Ǻ. Cu(tetrahedral)- P;Br are 2.207(4); 2.446(2), 2.676(3), 2.515(3) Ǻ.

scholarly journals Making and Characterization of Limnpo4 Using Solid State Reaction Method for Lithium Ion Battery Cathodes

2019 ◽  
pp. 583-588
Author(s):  
Adelyna Oktavia ◽  
Kurnia Sembiring ◽  
Slamet Priyono
Keyword(s):  
Solid State ◽  
Lithium Ion Battery ◽  
Lithium Ion ◽  
Solid State Reaction Method ◽  
Raw Material ◽  
X Ray Diffraction ◽  
Solid State Method ◽  
X Ray ◽  
General Investigation

Hospho-material of olivine, LiMnPO4 identified as promising for cathode material generation next Lithium-ion battery and has been successfully synthesized by solid-state method with Li2Co3, 2MnO2, 2NH4H2PO4 as raw material. The influence of initial concentration of precursors at kalsinasi temperatures (400-800 ° C) flows with nitrogen. The purity and composition phase verified by x-ray diffraction analysis (XRD), scanning electron microscopy (SEM), spectroscopy, energy Dispersive x-ray Analysis (EDS), Raman spectra. General investigation shows that there is a correlation between the concentration of precursors, the temperature and the temperature of sintering kalsinasi that can be exploited to design lithium-ion next generation.

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