Preparation and Structures of Rare Earth 3-Benzoylpropanoates and 3-Phenylpropanoates

2020 ◽  
Vol 73 (12) ◽  
pp. 1250
Author(s):  
Nicholas C. Thomas ◽  
Owen A. Beaumont ◽  
Glen B. Deacon ◽  
Cornelius Gaertner ◽  
Craig M. Forsyth ◽  
...  
Keyword(s):  
Hydrogen Bond ◽  
Rare Earth ◽  
Solid State ◽  
Coordination Polymers ◽  
Surface Interactions ◽  
X Ray Diffraction ◽  
Hydrogen Bond Acceptor ◽  
X Ray ◽  
Sodium Carboxylate ◽  
Rare Earth Chloride

Rare earth (RE) complexes of 3-benzoylpropanoate (bp), [RE(bp)3(H2O)n] (RE=La, n=2; RE=Y, Ce, Pr, Nd, Yb, n=1) and 3-phenylpropanoate (pp), [RE(pp)3] (RE=Y, La, Ce, Nd, Yb), have been prepared by metathesis reactions between the corresponding rare earth chloride and the appropriate sodium carboxylate. Analysis by single-crystal X-ray diffraction finds that both RE bp and pp complexes favour formation of carboxylate-bridged 1-D coordination polymers in the solid state. Here, the former favours heteroleptic 9 or 10-coordinate complexes (splitting between Ce and La) with the carbonyl remaining uncoordinated but participating as a hydrogen bond acceptor with water in the coordination sphere. Lack of bp carbonyl coordination leaves this group available for surface interactions during corrosion inhibition and complex solubilization. The latter pp derivatives form eight-coordinate complexes for Y and Yb and are the first examples of homoleptic RE pp complexes to be reported.

Single Crystal Formation by Solid-State Reaction Between p-Benzoquinone and 2,4,5-Trichlorophenol

2002 ◽  
Vol 55 (4) ◽  
pp. 271 ◽  
Author(s):  
N. B. Singh ◽  
A. Pathak ◽  
R. Fröhlich
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Single Crystal ◽  
Single Crystals ◽  
Solid State Reaction ◽  
Carbonyl Oxygen ◽  
Crystal Formation ◽  
X Ray Diffraction ◽  
X Ray

Vapours of p-benzoquinone (BQ) have been found to react with solid 2,4,5-trichlorophenol (TCP). The reaction product (BQ-TCP) separated in the form of monoclinic single crystals, the structure of which was determined by X-ray diffraction to reveal that the two molecules are linked by a single hydrogen bond between the carbonyl oxygen of BQ and the phenolic hydrogen of TCP.

A Solid-State NMR, X-ray Diffraction, and ab Initio Computational Study of Hydrogen-Bond Structure and Dynamics of Pyrazole-4-Carboxylic Acid Chains

2001 ◽  
Vol 123 (32) ◽  
pp. 7898-7906 ◽  
Author(s):  
Concepción Foces-Foces ◽  
Aurea Echevarría ◽  
Nadine Jagerovic ◽  
Ibon Alkorta ◽  
José Elguero ◽  
...  
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Carboxylic Acid ◽  
Ab Initio ◽  
Solid State Nmr ◽  
Computational Study ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure And Dynamics

Structural characterization of p-benzosemiquinone radical in a solid state: the radical stabilization by a low-barrier hydrogen bond

2006 ◽  
Vol 62 (6) ◽  
pp. 1051-1060 ◽  
Author(s):  
Krešimir Molčanov ◽  
Biserka Kojić-Prodić ◽  
Mario Roboz
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Variable Temperature ◽  
Organic Radical ◽  
X Ray Diffraction ◽  
X Ray ◽  
Crystal Packings ◽  
Dynamical Disorder ◽  
Benzenoid Ring

Semiquinone (p-benzosemiquinone), a transient organic radical, was detected in the solid state by EPR spectroscopy revealing four symmetrically equivalent protons. A variable-temperature X-ray diffraction analysis (293 and 90 K) and EPR data support a dynamical disorder of the proton. A low-barrier O—H···O hydrogen bond stabilizes the radical. The C—O bond length is 1.297 (4) Å, corresponding to a bond order of ca 1.5. The geometry of the radical implies an electron delocalization throughout the benzenoid ring. Two polymorphs of semiquinone, monoclinic and triclinic, were observed and their structures determined. Their crystal packings were compared with those of quinhydrone polymorphs.

scholarly journals Synthesis and Characterization of Sr2CeO4 Phosphor Doped with Erbium

2010 ◽  
Vol 13 (1-2) ◽  
pp. 17
Author(s):  
K.V.R. Murthy ◽  
K. Suresh ◽  
B. Nageswara Rao ◽  
B. Walter Ratna Kumar ◽  
Ch. Atchyutha Rao ◽  
...  
Keyword(s):  
Rare Earth ◽  
Solid State ◽  
Sem Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Rare Earth Ion ◽  
Solid State Reaction Technique ◽  
X Ray ◽  
Pl Emission

<p>The present paper reports the Photoluminescence (PL) of the Sr<sub>2</sub>CeO<sub>4</sub> phosphor, singly doped with Erbium rare-earth ion with different concentrations (0.01, 0.1, 0.2, 0.5 and 1%).The phosphor samples were synthesized using the standard solid state reaction technique. The effect of Er dopant on the structural, morphological, and Photoluminescent properties of the samples are studied with X-ray diffraction (XRD), PL and SEM analysis. The PL emission of undoped Sr<sub>2</sub>CeO<sub>4</sub> phosphor was observed at 470 nm with high intensity followed by the primary Er emissions with good intensity at 525, 530, 549, 557 and 565 nm.</p>

Convenient Synthesis of Copper(I) Halide Quasi-One-Dimensional Coordination Polymers: Their Structures and Solid-State Luminescent Properties

2021 ◽  
Author(s):  
Shingo Masahara ◽  
Hiromichi Yokoyama ◽  
Yuji Suzaki ◽  
Tomohito Ide
Keyword(s):  
Solid State ◽  
Coordination Polymers ◽  
Heterogeneous Reaction ◽  
Luminescent Properties ◽  
Pyridine Derivative ◽  
X Ray Diffraction ◽  
One Dimensional ◽  
X Ray ◽  
Convenient Synthesis

The heterogeneous reaction between copper(I) halide and pyridine derivative ligand in a suspension conveniently afforded luminescent copper(I) complexes. The progress of the reaction was confirmed by powder X-ray diffraction (PXRD)...

A Study of Diastereomeric Mandelate Salts of Cinchonidine and the Relation to Their Quasidiastereomeric Analogues

1997 ◽  
Vol 53 (4) ◽  
pp. 708-718 ◽  
Author(s):  
A. Gjerløv ◽  
S. Larsen
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Mandelic Acid ◽  
Crystal Packing ◽  
Steric Effects ◽  
Quinoline Ring ◽  
X Ray Diffraction ◽  
X Ray ◽  
Diastereomeric Salts ◽  
Vinyl Group

The crystal structures have been determined for the diastereomeric salts formed by cinchonidine and the two enantiomers of mandelic acid using low-temperature [122 (1) K] X-ray diffraction data. The less soluble salt is cinchonidinium (S)-mandelate, C19H23N20O+.C8H7O3 −, M r = 446.53, monoclinic, C2, a = 21.400 (2), b = 6.2777 (6), c = 17.853 (2) Å3, \beta = 109.304 (8)°, V = 2263.6 (4) Å3, Z = 4, D x = 1.310 g cm−3, \lambda(Cu K\alpha = 1.54184 Å, Z = 7.08 cm−1, F(000) = 952, R 1 = 0.0259 for 2684 observed reflections. The cinchonidine salt with (R)-mandelic acid, C19H23N2O+.C8H7O3, has M r = 446.53, monoclinic, P21, a = 6.410 (3), b = 32.808 (11), c = 11.222 (2) Å, \beta = 100.67 (2)°, V = 2319.2 (13) Å3, Z = 4, D x = 1.279 g cm−3, \lambda(Cu K\alpha) = 1.54184 Å, \mu = 6.91 cm−1, F(000) = 952, R 1 = 0.0380 for 8951 observed reflections. The two salts have virtually identical hydrogen-bond patterns and similar herringbone stacking of the quinoline ring systems. The crystal packing of the two salts differ only with respect to the packing of the phenyl groups. The packing of the cinchonidinium mandelates is significantly different from the crystal packing in the corresponding mandelates of cinchonine. The lack of a quasidiastereomeric relationship between the two sets of salts can be attributed to the steric effects of the vinyl group. The similarities between the two cinchonidinium mandelate structures is a possible explanation to the similar solubilities of the salts. DSC and NMR measurements showed that the cinchonidinium salts undergo a chemical opening reaction in the solid state. The arrangement of hydrogen-bonded chains of alternating cations and anions appear to be important for the solid-state reaction to take place.

Syntheses and crystal structures of trigonal rare-earth dioxymonocyanamides, Ln2O2CN2 (Ln=Dy, Ho, Er, Tm, Yb)

2007 ◽  
Vol 22 (1) ◽  
pp. 59-63 ◽  
Author(s):  
Min Li ◽  
Wenxia Yuan ◽  
Jingfang Wang ◽  
Cong Gu ◽  
Huaizhou Zhao
Keyword(s):  
Rare Earth ◽  
Infrared Spectroscopy ◽  
Solid State ◽  
Rietveld Method ◽  
Reaction Pathways ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Trigonal System ◽  
Xrd Patterns

Trigonal rare-earth dioxymonocyanamides Ln2O2CN2 (Ln=Dy, Ho, Er, Tm, Yb) were synthesized by the modified solid-state metathesis (SSM) method, in which Ln2O3 and melamine C3N6H6 were mixed and heated at 850 °C in vacuumed silica ampoules. Possible chemical reaction pathways are proposed. X-ray diffraction (XRD) patterns of Ln2O2CN2 were refined using the Rietveld method. Compounds Ln2O2CN2 crystallize in the trigonal system with space group P3m1, Z=1, and cell parameters of a and c varying from 3.7267(1) to 3.6407(1) Å and from 8.1848(3) to 8.1152(3) Å, respectively, as Ln atoms change from Dy to Yb. These compounds have stacking structures of Ln2O22+ and CN22− layers, similar to those of previously reported compounds Ln2O2CN2 (Ln=Ce, Pr, Nd, Sm, Eu, Gd). The presence of CN22− ions has been confirmed by infrared spectroscopy, with two characteristic peaks in the vicinity of 651 and 2075 cm−1.

Self-association and stereochemistry study of 2-methylthio-, 2-dimethylaminocyclohexanone oximes and the parent cyclohexanone oxime

2001 ◽  
Vol 57 (5) ◽  
pp. 705-713 ◽  
Author(s):  
Paulo R. Olivato ◽  
Douglas S. Ribeiro ◽  
J. Zukerman-Schpector ◽  
Gabriella Bombieri
Keyword(s):  
Hydrogen Bond ◽  
Solid State ◽  
Parent Compound ◽  
Chair Conformation ◽  
Orbital Interaction ◽  
Cyclohexanone Oxime ◽  
X Ray Diffraction ◽  
X Ray ◽  
Shift Analysis ◽  
Self Association

X-ray diffraction analyses of 2-substituted cyclohexanone oximes C5H9(X)C=NOH [X = SMe (1), NMe2 (2)] and of the parent compound [X = H (3)] showed that their cyclohexyl rings are in a slightly distorted chair conformation. These compounds assume in the solid state the (E) configuration bearing the 2-substituents in the axial conformation. Compounds (1) and (2) exist as dimeric and polymeric hydrogen-bond associates, respectively. Low-temperature X-ray analysis of the cyclohexanone oxime (3) showed that the molecules are associated forming two independent trimers. The dimer in (1) and the trimer in (3) are built up via [O—H...N=C] hydrogen bonds, while the polymer of (2) is via the [OH...NMe2] hydrogen bond. The comparative IR νOH and νC=N analysis of the title compounds, in the solid state and in CCl4 solution, fully supports the nature of the associates for (1)–(3) obtained by X-ray diffraction. The IR azomethyne frequency shift analysis (ΔνC=N) also suggests the occurrence of the πC=N/σ*C—X orbital interaction which stabilizes the axial conformations of (1) and (2).

Synthesis and Luminescence Properties of Doped Magnesium Boro-Tellurite Ceramics

2015 ◽  
Vol 73 (1) ◽  
Author(s):  
Nur Zu Ira Bohari ◽  
R. Hussin ◽  
Zuhairi Ibrahim ◽  
Hendrik O. Lintang
Keyword(s):  
Rare Earth ◽  
Solid State ◽  
Solid State Reaction Method ◽  
Luminescence Properties ◽  
X Ray Diffraction ◽  
X Ray ◽  
Emission Transition ◽  
Bending Mode ◽  
Two Phases ◽  
Rare Earth Doped

Glass has been widely utilized in the field of lighting, telecommunication and spectroscopy. Boro-tellurite is one of the suitable glasses used for solid state lighting and laser application. The investigation on the luminescence properties of rare earth doped ceramic is rarely used due to the opacity. In this paper boro-tellurite prepared in ceramic can show the better luminescence with the less advantage. The aim of this paper is to present the effect and advantages in luminescence results of boro-tellurite ceramics doped with the constant amount of rare earth. Doped magnesium boro-tellurite with Eu3+ and Dy3+ ceramic have been prepared using solid state reaction method with the compositions of xTeO2-(70-x)B2O3-30MgO with 10≤x≤40, and have been doped with Eu2O3 (1mol%) and Dy2O3 (1mol%) . The characterizations of the samples have been investigated by means of X-Ray diffraction, Raman, Infrared and Photoluminescence spectroscopy. From the X-ray diffraction results, two phases are assigned to MgTe2O5 and Mg2B2O5. Raman spectroscopy showed strong bands observed in the vicinity of 140, 175, 220, 266, 332, 403, 436, 646, 694, 723, 757 and 806 cm-1. FTIR spectra showed bands located in the range between 400-800 cm-1 are assigned to the bending mode of Te-O-Te, TeO3 and TeO4. In the range of 800-1400 cm-1,the bands are associated with B-O, B-O-B, BO3 and BO4 bonds. The emission transition 5D0-7F2 corresponded to the red emission (612 nm) was found to be the most intense in all the Eu3+-doped magnesium boro-tellurite ceramics.  

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