Synthesis, Spectral Properties of Methyl-2-Pyridyl Ketone Benzoyl Hydrazone and its Complexes with Rare Earth Nitrates

2011 ◽  
Vol 219-220 ◽  
pp. 565-568 ◽  
Author(s):  
Xi Shi Tai ◽  
Lin Tong Wang

A new schiffbase ligand, methyl-2-pyridyl ketone benzoyl hydrazone (L), and its complexes with rare earth nitrates have been synthesized. These new complexes with the general formula of Ln(L)2(NO3)3·nH2O(where Ln = La, n = 5.5; Ce, Pr, n = 5; Nd, Eu, n = 4 ) were characterized by mass spectra, elemental analysis, IR spectra, thermal analysis, UV spectra, molar conductivity and luminescent spectra. All the complexes are stable in air. The results show that the lanthanide ion in each complex are coordinated by oxygen and nitrogen atoms of the ligand, the oxygen atoms of the nitrate and coordinated water molecules. The amide-oxygen atoms of L coordinate to the Ln ions in its keto-form. Tentative structures for the complexes have been proposed.

2011 ◽  
Vol 366 ◽  
pp. 169-172
Author(s):  
Li Hua Wang

Two new Eu (III) complexes with multifunctional ligands, 2, 2'-dithiosalicylic acid (L1) and 1-acetyl-2-naphthol-4, 4'-diaminodiphenyl ether (L2) have been prepared in ethanol solution. The complexes are stable in air. The infrared spectrum and luminescent spectra of Eu (III) complexes were studied. The results indicate that the oxygen atoms of the ligands (L1 and L2), the nitrogen atoms of L2, the oxygen atoms of the nitrate and coordinated water molecules coordinate to Eu (III) ions. The luminescent property of Eu (III) complexes have been investigated in solid state.


1999 ◽  
Vol 52 (6) ◽  
pp. 497 ◽  
Author(s):  
David L. Kepert ◽  
Peter C. Junk ◽  
Brian W. Skelton ◽  
Allan H. White

Room-temperature single-crystal X-ray structure determinations are known for a number of ‘maximally hydrated" nitrates of, in particular, the lighter lanthanoid elements; in all cases, all nitrates coordinate as O,O′-bidentate ligands so that the series may be represented at the outset as Ln(O2NO)3.x H2O. Two distinct triclinic P 1 hexahydrate phases of similar cell dimensions are recognized, the most distinctive distinguishing feature being that in the La, Ce phase the 11-coordinate Ln is surrounded by three O,O′-bidentate nitrate and five O-unidentate water molecule ligands; the domain of the other, with four coordinated water molecules, extends from Ln = Pr to Ln = Dy (inclusive of Y). At local ambience, we have crystallized heavier members of the series as pentahydrates, isomorphous with the previously characterized Ln = Eu example, also containing a molecule of the form [Ln(O2NO)3(OH2)4] (with a molecule of water of crystallization), but a different stereoisomer to that found in the Ln = Pr(-)Dy array. Structure determinations are recorded for Ln = Dy, Er, Yb, conventional R on |F| 0·042, 0·034, 0·029 for No = 3858, 3980, 3935 independent ‘observed’ (I > 3σ(I)) diffractometer reflections. For Ln = Lu a new tetrahydrate phase is described, monoclinic P21/n, a 7·379(7), b 10·364(5), c 14·26(1) Å, β 96·09(7)°, Z = 4, R 0·048 for No 2324, together with a new triclinic P 1 trihydrate, a 12·591(4), b 12·144(3), c 7·355(2) Å, α 80·22(2), β 77·68(3), γ 62·30(2)°, Z = 4, R 0·051 for No 4552. In both of the latter, Lu is nine-coordinate, with three bidentate nitrate groups and three coordinated water molecules; remarkably, the two independent molecules of the asymmetric unit in the triclinic phase are distinct isomers, one having the water molecules fac, derivative of the 10-coordinate array of the Pr(-)Yb series with quasi-3 symmetry, while the other, like that in the monoclinic phase, is mer.


2011 ◽  
Vol 366 ◽  
pp. 161-164
Author(s):  
Li Hua Wang

A new terbium complex with aromatic multicarboxylate ligand, 2, 2'-dithiosalicylic acid (L), has been synthesized. The terbium complex was characterized by elemental analysis, infrared spectrum and luminescent spectra, and the complex conforms to 1:1 metal-to-ligand stoichiometry. The complex is stable in air. The results show that the Tb (III) ion in the complex is coordinated by oxygen atoms of the ligand and the oxygen atoms of the nitrate and coordinated water molecules. The luminescent properties of terbium complex have also been investigated in solid state and in organic solvents.


2011 ◽  
Vol 219-220 ◽  
pp. 574-577
Author(s):  
Xi Shi Tai ◽  
Lin Tong Wang

The reaction of 2-acetyl-2'-chloroacetanilide (L) with rare earth nitrates in CH3CH2OH followed by recrystallization in CH3CH2OH gave rise to colorless block crystals materials. The complexes and ligand were analyzed by FAB, elemental analysis(C, H, N), FT-IR spectra, TG-DTA, molar conductivity and X-ray single crystal diffraction. The fluorescence properties of ligand and the Eu (Ⅲ) complex also have been investigated. The results of crystal structure and spectral data show that the rare earth ions coordinated with oxygen and nitrogen atoms of the ligand, the nitrate and coordinated water molecules. The Eu (Ⅲ) complex material shows characteristic red emissions.


1998 ◽  
Vol 51 (8) ◽  
pp. 775 ◽  
Author(s):  
Jack M. Harrowfield ◽  
Raj Pal Sharma ◽  
Brian W. Skelton ◽  
Paloth Venugopalam ◽  
Allan H. White

Room-temperature single-crystal X-ray structure determinations are recorded for 4-nitrophenolate (4-np-) salts of Group 2 metal ions, variously hydrated, M(4-np)2.xH2O, M = Mg, Ca, Sr, Ba. Mg(4-np)2.8H2 O is monoclinic, P21/c, a 12·402(3), b 6·673(7), c 11·833(6) Å, β 93·70(3)°, Z = 2; conventional R on |F| was 0·041 for No 1995 independent ‘observed’ (I > 3σ(I)) reflections. Ca(4-np)2.4H2O is monoclinic, P21/c, a 13·109(8), b 3·644(1), c 21·181(8) Å, β 125·55(3)°, Z= 2, R 0·050 for No 1371. Sr(4-np)2.8H2O is monoclinic, P21/n, a 7·934(1), b 10·658(1), c 23·602(2) Å, β 91·36(1)°, Z = 4, R 0·038 for No 2050. Ba(4-np)2.8H2O is monoclinic P21/c, a 15·990(8), b 6·337(3), c 25·634(8) Å, β 126·1(3)°, Z = 4, R 0·021 for No 3115. The magnesium salt is ionic with [Mg(OH2)6]2+ cations and interleaved anion stacks up b. The calcium salt is a one-dimensional polymer with ... Ca(µ-O)2Ca(µ-O)2Ca ... spine, the bridges being phenolic oxygen atoms.trans-Coordinated water molecules make up six-coordination about the calcium, the anion planes stacking at the b spacing. The strontium adduct is also a one-dimensional polymer with a similar spine, but with water molecule oxygen atoms bridging, the nine-coordinate strontium environment being made up by a chelating nitro group and three unidentate water molecules. Coordinated anions stacked up a are interleaved by free anions. The barium salt is simply [Ba(4-np)(OH2)8]+ (4-np-), the ligand anion (semi)chelated through the nitro pair of oxygen atoms, again with interleaving anion/ligand stacking.


2011 ◽  
Vol 66 (8) ◽  
pp. 813-818 ◽  
Author(s):  
Masoumeh Tabatabaee ◽  
Boris-Marko Kukovec ◽  
Vajieh Razavimahmoudabadi

A dinuclear cobalt(II) complex, [Co2(H2O)4(dipic)2(μ-apyz)] (dipicH2 = pyridine-2,6-dicarboxylic (dipicolinic) acid, apyz = 2-aminopyrazine) (1), has been hydrothermally synthesized and characterized by elemental analyses, spectroscopic methods (IR, UV/Vis), thermal analysis as well as by X-ray diffraction studies. The dinuclear complex is composed of two cobalt(II) ions bridged by a 2-aminopyrazine molecule. Each cobalt(II) ion is coordinated by one nitrogen and two oxygen atoms of the tridentate dipicolinate anion, one heterocyclic nitrogen atom of the 2-aminopyrazine and two oxygen atoms of coordinated water molecules. The resulting geometry for the CoN2O4 coordination environment can be described as distorted octahedral. Various hydrogen bonds of the type O-H···O and N-H···O are also present in the crystal structure. This arrangement leads to the formation of a 3D structure.


Author(s):  
Anna V. Pavlishchuk ◽  
Inna V. Vasylenko ◽  
Matthias Zeller ◽  
Anthony W. Addison

The core of the title complex, bis[hexaaquahemiaquapentakis(μ3-glycinehydroxamato)sulfatopentacopper(II)terbium(III)] sulfate hexahydrate, [TbCu5(SO4)(GlyHA)5(H2O)6.5]2(SO4)·6H2O (1), which belongs to the 15-metallacrown-5 family, consists of five glycinehydroxamate dianions (GlyHA2−; C2H4N2O2) and five copper(II) ions linked together forming a metallamacrocyclic moiety. The terbium(III) ion is connected to the centre of the metallamacrocycle through five hydroxamate oxygen atoms. The coordination environment of the Tb3+ ion is completed to an octacoordination level by oxygen atoms of a bidentate sulfate and an apically coordinated water molecule, while the copper(II) atoms are square-planar, penta- or hexacoordinate due to the apical coordination of water molecules. Continuous shape calculations indicate that the coordination polyhedron of the Tb3+ ion in 1 is best described as square antiprismatic. The positive charge of each pair of [TbCu5(GlyHA)5(H2O)6.5(SO4)]2 2+ fragments is compensated by a non-coordinated sulfate anion, which is located on an inversion center with 1:1 disordered oxygen atoms. Complex 1 is isomorphous with the previously reported compounds [LnCu5(GlyHA)5(SO4)(H2O)6.5]2(SO4), where Ln III = Pr, Nd, Sm, Eu, Gd, Dy and Ho.


2018 ◽  
Vol 74 (12) ◽  
pp. 1691-1694
Author(s):  
Chatphorn Theppitak ◽  
Filip Kielar ◽  
Kittipong Chainok

The first benzohydrazide complex of a lanthanide is reported. In the title compound, [Sm(C8H4O4)(C7H8N2O)3(H2O)2]NO3, systematic name diaquatris(benzohydrazide-κ2 N,O)(isophthalato-κO)samarium(III) nitrate, the SmIII ion is nine-coordinated in a distorted tricapped trigonal–prismatic geometry by three oxygen atoms and three nitrogen atoms from three benzhydrazide (bzz) ligands, one oxygen atom from the isophthalate (itp2−) ligand, and two oxygen atoms from coordinated water molecules. The nitrate group is disordered over two sets of sites with occupancy factors of 0.310 (17) and 0.690 (17). In the crystal, adjacent molecules are linked into chains via pairs of O—H...O and N—H...O hydrogen bonds between the carboxylate acceptor and the coordinated water and amine NH2 donors. Molecules are further stacked by π–π interactions involving the benzene ring of the itp2− ligands, forming double chains that extend in the b-axis direction. These double chains are further linked into a three-dimensional supramolecular network via hydrogen bonds (O—H...O, N—H...O and C—H...O) between the complex molecule and the nitrate groups along with C—H...π and π–π interactions involving the benzene rings of the bzz and itp2− ligands.


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