scholarly journals N-Tris[(2-aminoethyl)-2-(diphenylphosphoryl) acetamide)] — novel CMPO tripodand: synthesis, extraction studies and luminescent properties of lanthanide complexes

2012 ◽  
Vol 10 (1) ◽  
pp. 146-156 ◽  
Author(s):  
Elena Sharova ◽  
Oleg Artyushin ◽  
Alexander Turanov ◽  
Vasilii Karandashev ◽  
Svetlana Meshkova ◽  
...  

AbstractA ligand system containing three carbamoylmethylphosphine oxide (CMPO) moieties attached to a tripodal platform with a central nitrogen atom has been synthesized for metal complexation and extraction from neutral and nitric acid solutions. Liquid-liquid extractions performed for Ln(III), both from neutral and acidic media, show excellent extraction properties which exceeded those for the known mono- and di-CMPO derivatives as well as the related tripodands. A considerable enhancement of the DLn values was observed in the presence of IL ([bmim][Tf2N]) in the organic phase towards lanthanide ions from 3M HNO3 solutions. The protonation of the central amine nitrogen atom of the ligand 1 in the acidic media provides also the effective extraction of the perrhenate anionic complexes. The europium complexes formed by mono- and tris-CMPO ligands in the solid state, as well as Eu(III) and Tb(III) complexes generated in solutions, possess intensive luminescence at 300K

1996 ◽  
Vol 74 (4) ◽  
pp. 574-582 ◽  
Author(s):  
H. Alarabi ◽  
R.A. Bell ◽  
H.E. Howard-Lock ◽  
J. Kowanetz ◽  
C.J.L. Lock

The ligand molecule N10-(2′-mercaptoethanoyl)-2,2,5,5-tetramethyl-3,4-dithia-7,10-diazabicyclo[5.3.0]decane has been prepared and characterized by 1H and 13C NMR spectroscopy and by mass spectrometry. The protected analogue, N10-[(2′-triphenylmethylthio)ethanoyl]2,2,5,5-tetramethyl-3,4-dithia-7,10-diazabicyclo[5.3.0]decane dimethanol hemihydrate, was examined by the same techniques and also by X-ray crystallography. Crystals were triclinic, P-1, a = 11.125(2), b = 11.986(2), c = 13.562(3) Å, α = 103.54(3)°, β = 90.29(3)°, γ = 107.11(3)°, and Z = 2. The crystal was unstable in air at room temperature, so measurements were made on a crystal sealed in a tube that contained methanol vapour Intensities were measured with a Rigaku AFC6R diffractometer and monochromated CuKα radiation (λ = 1.54178 Å). The structure was solved by direct methods and refined to R = 0.1497, wR = 0.0655 based on 5000 independent reflections. The high residuals were caused by solvent disorder. Bond lengths and angles were normal. The reaction of the ligand with oxotrichlorobis(triphenylphosphine)rhenium(V) yielded an unexpected asymmetric complex, oxo(1,1-dimethyl-1,8-dimercapto-3,6-diazaoctan-7-onato-N3,N6,S1,S8) rhenium(V). Crystals were monoclinic, P21/n, a = 10.633(2), b = 11.221(2), c = 11.678(1) Å, β = 116.10(1)°, Z = 4. Intensities were measured with a Siemens P4 diffractometer and monochromated MoKα radiation (λ = 0.71073 Å). The structure was solved by the heavy atom method and refined to R = 0.0471, wR = 0.0340 based on 2866 unique reflections. Most bond lengths and angles were normal. The Re≡O distance of 1.681(5) Å was longer than normal. It is postulated that this was caused by competitive π bonding between the deprotonated amidic nitrogen atom and the rhenium atom, as shown by the short Re—N distance (1.997(6) Å) compared to the equivalent distance for the amine nitrogen atom (Re—N, 2.151(4) Å). Key words: N2S2 ligands, rhenium, crystal structure.


2004 ◽  
Vol 74 (11) ◽  
pp. 1728-1733 ◽  
Author(s):  
Yu. A. Mednykh ◽  
Yu. A. Manaev ◽  
V. V. Volchkov ◽  
B. M. Uzhinov

ChemMedChem ◽  
2009 ◽  
Vol 4 (12) ◽  
pp. 2080-2097 ◽  
Author(s):  
Maria Grazia Perrone ◽  
Laura Bleve ◽  
Ernesto Santandrea ◽  
Paola Vitale ◽  
Mauro Niso ◽  
...  

IUCrData ◽  
2020 ◽  
Vol 5 (10) ◽  
Author(s):  
Clifford W. Padgett ◽  
Kirkland Sheriff ◽  
Will E. Lynch

Our work in the area of synthesis of metal–organic frameworks (MOFs) based on organic N-oxides led to the crystallization of pyridine-4-carboxamidoxime N-oxide. Herein we report the first crystal structure of the title compound, C6H7N3O2 [systematic name: (Z)-4-(N′-hydroxycarbamimidoyl)pyridine N-oxide]. The hydroxycarbamimidoyl group is essentially coplanar with the aromatic ring, r.m.s.d. = 0.112 Å. The compound crystallizes in hydrogen-bonding layers built from the formation of strong O—H...O hydrogen bonds between the oxime oxygen atom and the oxygen atom of the N-oxide, and the formation of N—H...O hydrogen bonds between one amine nitrogen atom and the N-oxide oxygen atom. These combined build R 3 4(24) ring motifs in the crystal. The crystal structure has no π–π interactions.


1985 ◽  
Vol 63 (10) ◽  
pp. 2752-2756 ◽  
Author(s):  
Alastair K. S. Muir ◽  
Penelope W. Codding

The crystal and molecular structures of methyl β-carboline-3-carboxylate, C13H10N2O, a high-affinity ligand for the benzodiazepine receptor, are reported. This candidate for the endogenous ligand for the receptor produces a biological response that is opposite to the anxiety-reducing effect of the usual agonists of the receptor and is, therefore, classified as an inverse-agonist. The space group is P21/c with a = 11.4866(9), b = 5.8091(3), c = 32.417(3) Å, β = 97.111(3)°, Z = 8. In both of the unique molecules, the ester side chain has an extended conformation and is coplanar with the β-carboline moiety. The carbonyl oxygen atom and the aromatic nitrogen atom are cis and form a three-centre hydrogen bond to the amine nitrogen atom of the other molecule in the asymmetric unit.


2002 ◽  
Vol 67 (2) ◽  
pp. 111-113 ◽  
Author(s):  
Alexei Pankratov ◽  
Inna Uchaeva

By means of the PM3 method it has been shown that the protonation of 2-, 3 4-methoxyanilines, 4-methylthioaniline, 2-, 3-, 4-aminobenzoic acids, 2 3-, 4-nitroanilines in the gaseous phase proceeds via the amine nitrogen atom. The same result, attributed to the aqueous medium, was obtained for 4-methoxyaniline, 4-aminobenzoic acid and 4-nitroaniline.


2011 ◽  
Vol 322 ◽  
pp. 337-340
Author(s):  
Lian Cai Du

A tripodal ligand, 2-acetylpyridine-tris(2-aminoethyl)amine (L), pyridine-N-oxide and their ternary complexes with rare earth nitrates have been synthesized. These new complexes with the general formula of Ln·L·PyNO·(NO3)3·nH2O (where Ln = La, Nd, Tb, Pr, Eu, n = 1~3 ) were characterized by elemental analysis, IR spectra, thermal analysis and molar conductivity. All the complexes are stable in air. The results show that the lanthanide ions in each complex are coordinated by nitrogen atoms of the ligand, oxygen atoms of PyNO and the nitrates. The fluorescent properties of the Eu(III) and Tb(III) complexes in solid were investigated.


Nanomaterials ◽  
2019 ◽  
Vol 9 (8) ◽  
pp. 1153 ◽  
Author(s):  
Daniel González-Mancebo ◽  
Ana Isabel Becerro ◽  
Ariadna Corral ◽  
Marcin Balcerzyk ◽  
Manuel Ocaña

Due to the high atomic number of lutetium and the low phonon energy of the fluoride matrix, Lu-based fluoride nanoparticles doped with active lanthanide ions are potential candidates as bioprobes in both X-ray computed tomography and luminescent imaging. This paper shows a method for the fabrication of uniform, water-dispersible Eu3+:(H3O)Lu3F10 nanoparticles doped with different Eu contents. Their luminescent properties were studied by means of excitation and emission spectra as well as decay curves. The X-ray attenuation capacity of the phosphor showing the highest emission intensity was subsequently analyzed and compared with a commercial contrast agent. The results indicated that the 10% Eu3+-doped (H3O)Lu3F10 nanoparticles fabricated with the proposed polyol-based method are good candidates to be used as dual probes for luminescent imaging and X-ray computed tomography.


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