scholarly journals Two Beta-Phosphorylamide Compounds as Ligands for Sm3+, Eu3+, and Tb3+: X-ray Crystallography and Luminescence Properties

Molecules ◽  
2020 ◽  
Vol 25 (13) ◽  
pp. 2971
Author(s):  
Alan R. Lear ◽  
Jonah Lenters ◽  
Michael G. Patterson ◽  
Richard J. Staples ◽  
Eric J. Werner ◽  
...  

This paper describes the synthesis of two beta-phosphorylamide ligands and their coordination chemistry with the Ln ions Tb3+, Eu3+, and Sm3+. Both the ligands and Ln complexes were characterized by IR, NMR, MS, and X-ray crystallography. The luminescence properties of the Tb3+ and Eu3+ complexes were also characterized, including the acquisition of lifetime decay curves. In the solid state, the Tb3+ and Sm3+ ligand complexes were found to have a 2:2 stoichiometry when analyzed by X-ray diffraction. In these structures, the Ln ion was bound by both oxygen atoms of each beta-phosphorylamide moiety of the ligands. The Tb3+ and Eu3+ complexes were modestly emissive as solutions in acetonitrile, with lifetime values that fell within typical ranges.

2008 ◽  
Vol 63 (3) ◽  
pp. 339-341 ◽  
Author(s):  
Ajay Venugopal ◽  
Alexander Willner ◽  
Norbert W. Mitzel

The reaction of N,O-bis(trimethylsilyl)hydroxylamine with potassium hydride in pentane affords a product of the formula {K6[OSiMe3]4[ON(SiMe3)2]2}, resulting from deprotonation followed by N-O bond cleavage and 1,2-silylshift. The compound was characterised by elemental analysis and by single crystal X-ray diffraction. The aggregate consists of a K3O3 bis-cubane core, with N(SiMe3)2 groups at the oxygen atoms shared by the two cubes, andMe3Si groups attached to the four O vertices. Two weak K···N interactions are also detected in the solid state structure.


1990 ◽  
Vol 68 (7) ◽  
pp. 1128-1134 ◽  
Author(s):  
Robert Glaser ◽  
André Michel ◽  
Marc Drouin

The solid-state structure of nefopam methiodide, a quaternary ammonium salt of nefopam hydrochloride (a non-narcotic analgesic drug), has been determined by single crystal X-ray diffraction analysis. Nefopam methiodide gives crystals belonging to the monoclinic P21/c space group and, at 298 K, a = 10.001(1), b = 9.928(1), c = 17.598(1) Å, β = 94.41(1)°, V = 1742.2(2) Å3, Z = 4, R(F) = 0.086, and Rw(F) = 0.108. Due to disorder, the boat (flattened chair) and twist-chair (flattened chair) conformations of the 2,5-benzoxazocine eight-membered ring were both observed in the crystal with 55:45 occupancy, respectively. Positional disorder was also observed for the iodide counterion, which showed occupancies of 81:9.5:9.5. Keywords: nefopam, analgesic, X-ray crystallography, conformation.


1992 ◽  
Vol 47 (7) ◽  
pp. 952-956
Author(s):  
P. Mikulcik ◽  
P. Bissinger ◽  
J. Riede ◽  
H. Schmidbaur

Ester cleavage of aspartame (L-α-aspartyl-L-phenylalanine methylester) (1), by equimolar quantities of thallium ethoxide is accompanied by intramolecular cyclisation to give thallium 3-benzyl-6-(carboxylatomethyl)-2,5-dioxopiperazine (2). The solid state structure of the crystalline product was determined by single-crystal X-ray diffraction analysis. The cations were found to form four short and four elongated contacts to seven oxygen atoms and one nitrogen atom of a total of six neighbouring 3-benzyl-6-(carboxylatomethyl)-2,5-dioxopiperazine anions. There are inter-anionic hydrogen bonds only between the imino groups and the carbonyl oxygen atoms (O3, O4), featuring a pattern similar to that found for cytosine-guanosine contacts in DNA.


2011 ◽  
Vol 66 (5) ◽  
pp. 549-552
Author(s):  
Yan Bai ◽  
Guo Qiang Zhang ◽  
Dong Bin Dang ◽  
Ze Yan Qi ◽  
Li Zhang

The title compound [FTMA]2[CdI4] has been synthesized from [FTMA]I (ferrocenylmethyltrimethylammonium iodide) and 3CdSO4・8H2O and was characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The Cd(II) atom has a slightly distorted tetrahedral coordination sphere. In the solid state there are C-H・ ・ ・π interactions between adjacent ferrocenyl cations to generate a chain structure. The luminescence properties of the title compound were investigated in the solid state at room temperature


2015 ◽  
Vol 73 (1) ◽  
Author(s):  
Nur Zu Ira Bohari ◽  
R. Hussin ◽  
Zuhairi Ibrahim ◽  
Hendrik O. Lintang

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.  


Inorganics ◽  
2021 ◽  
Vol 9 (7) ◽  
pp. 52
Author(s):  
Maximilian Dehmel ◽  
Helmar Görls ◽  
Robert Kretschmer

Dianionic N,N-chelating ligands play a crucial role in coordination chemistry, but reports on related complexes remain limited to certain types of ligands. In here, the reactions of two diprotic ligands, i.e., a biguanide and a carbothiamide, with trimethylaluminium, are reported, which give rise to mono- and dinuclear aluminium(III) complexes. In addition, single deprotonation of the diprotic biguanide using potassium bis(trimethylsilyl)amide gives rise to a one-dimensional coordination polymer. All complexes have been fully characterized, and their solid-state structures were determined by single crystal X-ray diffraction analysis.


2019 ◽  
Vol 75 (1) ◽  
pp. 8-14 ◽  
Author(s):  
Zhen Chen ◽  
Yanwen Sun ◽  
Zi-an Liu ◽  
Ning Wang ◽  
Xue Yang ◽  
...  

In recent years, coordination polymers constructed from multidentate carboxylate ligands and N-containing ligands have attracted much attention since these ligands can adopt a rich variety of coordination modes which can lead to crystalline products with intriguing structures and interesting properties. A new coordination polymer, namely poly[[diaqua[μ-2,7-bis(1H-imidazol-1-yl)fluorene-κ2 N 3:N 3′][μ-5,5′-methylenebis(3-carboxy-2,4,6-trimethylbenzoato)-κ2 O 1:O 1′]zinc(II)] hemihydrate], {[Zn(C23H22O8)(C19H14N4)(H2O)2]·0.5H2O} n , 1, was prepared by the self-assembly of Zn(NO3)2·6H2O with 5,5′-methylenebis(2,4,6-trimethylisophthalic acid) (H4BTMIPA) and 2,7-bis(1H-imidazol-1-yl)fluorene (BIF) under solvothermal conditions. The structure of 1 was determined by elemental analysis, single-crystal X-ray crystallography, powder X-ray diffraction, IR spectroscopy and thermogravimetric analysis. Each ZnII ion is six-coordinated by two O atoms from two H2BTMIPA2− ligands, by two N atoms from two BIF ligands and by two water molecules, forming a distorted octahedral ZnN2O4 coordination geometry. Adjacent ZnII ions are linked by H2BTMIPA2− ligands and BIF ligands, leading to the formation of a two-dimensional (2D) (4,4)-sql network, and intermolecular hydrogen-bonding interactions connect the 2D layer structure into the three-dimensional (3D) supramolecular structure. Each 2D layer contains two kinds of helices with the same direction, which are opposite in adjacent layers. The luminescence properties of complex 1 in the solid state have also been investigated.


2003 ◽  
Vol 81 (12) ◽  
pp. 1431-1437 ◽  
Author(s):  
Michael P Shaver ◽  
Robert K Thomson ◽  
Brian O Patrick ◽  
Michael D Fryzuk

The tridentate ligand precursors R′P(CH2SiMe2NR′′)2 (R′R′′[NPN]: R′ = Cy, Ph; R′′ = Ph, Mes, Me) were prepared from metathesis reactions of a lithiated amine, chloro(chloromethyl)dimethylsilane, the appropriate 1° phosphine, and n-butyl lithium and were isolated as solvent adducts. Metathesis between CyPh[NPN]Li2(OEt2), 2, and VCl3(THF)3 afforded (CyPh[NPN]VCl)2, 7, whose solid-state structure was established by X-ray crystallography. Reduction attempts of the (R′R′′[NPN]VCl)2 species with KC8 incorporated molecular nitrogen but were complicated by imide formation and ligand decomposition. Metathesis of 2 with NbCl2Me3 afforded the highly unstable complex CyPh[NPN]NbMe3, 15. Attempts to hydrogenate this species were unsuccessful.Key words: vanadium, niobium, metathesis, coordination chemistry, reduction, hydrogenation.


2005 ◽  
Vol 83 (6-7) ◽  
pp. 1037-1042 ◽  
Author(s):  
Robert K Thomson ◽  
Brian O Patrick ◽  
Laurel L Schafer

A photo and thermally stable bis(amidate)–dibenzyl complex of Hf ([DMP(NO)Ph]2Hf(CH2Ph)2(THF) (2a) was formed as a monosolvated THF adduct in near quantitative yield from Hf(CH2Ph)4 and N-2,6-dimethylphenyl(phenyl)amide (1). Isomerization between the THF-bound product and the THF-free product can be observed visually by the conversion from a red-orange product at low temperatures to a pale yellow product at high temperatures. Solid-state crystallographic characterization of the orange product confirmed its constitution as a monosolvated species. Kinetic parameters for the exchange of the THF moiety were determined from variable-temperature NMR experiments. The product of the hydrolysis of the Hf dibenzyl species by water was characterized by X-ray crystallography, and was found to be a rare tetrametallic Hf oxo cluster species (3).Key words: hafnium, protonolysis, amidate, coordination chemistry, organometallic chemistry, exchange processes.


CrystEngComm ◽  
2021 ◽  
Author(s):  
Sergey Chunikhin ◽  
Oleg V Ershov ◽  
Aleksandr V. Yatsenko ◽  
Viktor Tafeenko ◽  
Natalia Evgenievna Dmitrieva ◽  
...  

Five new salts of 3,4-dicyano-2-(dicyanomethylene)-5-methyl-6-phenyl-2H-pyridin-1-ide anion (TCPy−) with lithium, sodium, potassium, rubidium and cesium cations were synthesized and structurally characterized by the single-crystal X-ray diffraction method. Solid state photoluminescence characteristics...


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