Structure and spectroscopy of uranyl salicylaldiminate complexes

2013 ◽  
Vol 101 (10) ◽  
pp. 631-636 ◽  
Author(s):  
A. L. Tamasi ◽  
C. L. Barnes ◽  
J. R. Walensky
Keyword(s):  
Schiff Base ◽  
Nmr Spectroscopy ◽  
Coordination Sphere ◽  
Ancillary Ligand ◽  
Schiff Base Ligands ◽  
Uranyl Complexes ◽  
X Ray ◽  
X Ray Crystallography ◽  
Chloride Ligand ◽  
C Nmr

Summary The synthesis of uranyl complexes coordinated to tridentate, monoanionic salicylaldiminate (Schiff base) ligands was achieved by the reaction of UO2Cl2(THF)3, 1, with one equivalent of the corresponding sodium salicylaldiminate salts affording [(C9H6N)N=C(H)C6H2t Bu2O]UO2Cl(THF), 2, [(NC5H4)N=C(H)C6H2 t Bu2O]UO2Cl(THF), 3, and [(C6H4SCH3)N=C(H)C6H2tBu2O]UO2Cl(THF), 4. These are uncommon examples of uranyl complexes with a monoanionic ancillary ligand to stabilize the coordination sphere and one chloride ligand. Compounds 2-4 have been characterized by 1H and 13C NMR spectroscopy as well as IR and UVVis spectroscopy and their structures determined by X-ray crystallography.

[Zn(phen)2(CX3COO)]+, X = H orCl; Influence of X on the Coordination Mode of the Carboxylate Group (phen = 1,10-Phenanthroline)

2005 ◽  
Vol 60 (10) ◽  
pp. 1049-1053 ◽  
Author(s):  
Zeanab Talaei ◽  
Ali Morsali ◽  
Ali R. Mahjoub
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Coordination Mode ◽  
Bidentate Ligand ◽  
Carboxylate Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Coordinate Geometry ◽  
C Nmr

Two new ZnII(phen)2 complexes with trichloroacetate and acetate anions, [Zn(phen)2(CCl3COO)- (H2O)](ClO4) and [Zn(phen)2(CH3COO)](ClO4), have been synthesized and characterized by elemental analysis, IR, 1H NMR, 13C NMR spectroscopy. The single crystal X-ray data of these compounds show the Zn atoms to have six-coordinate geometry. From IR spectra and X-ray crystallography it is established that the coordination of the COO− group is different for trichloroacetate and acetate. The former acts as a monodentate whereas the latter acts as a bidentate ligand.

Synthesis, structure, and electrochemistry of cobalt(III) complexes with bis(benzoylacetone)ethylenediimine Schiff base

2002 ◽  
Vol 80 (9) ◽  
pp. 1196-1203 ◽  
Author(s):  
Mehdi Amirnasr ◽  
Rasoul Vafazadeh ◽  
Amir H Mahmoudkhani
Keyword(s):  
Schiff Base ◽  
Reduction Potential ◽  
Crystal And Molecular Structure ◽  
Acetonitrile Solution ◽  
Potential Range ◽  
Carbon Electrode ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
C Nmr

A series of complexes of the type trans-[Co((BA)2en)(amine)2]ClO4 — where (BA)2en is the bis(benzoylacetone)ethylenediimine dianion and the amines are morpholine (mrpln) 1, aniline (aniln) 2, benzylamine (bzlan) 3, piperidine (pprdn) 4, p-toluidine (p-toldn) 5, and pyrrolidine (prldn) 6 — has been synthesized and characterized by elemental analysis, UV–vis, 1H NMR, and 13C NMR spectroscopy. The crystal and molecular structure of trans-[Co((BA)2en)(mrpln)2]ClO4 (1) has been determined by X-ray crystallography. The electrochemical reduction of these complexes at a glassy-carbon electrode, in the potential range of 0.5 to –2.0 V (vs. Ag/AgCl), in acetonitrile solution, indicates that the first reduction potential of Co(III/II) is irreversible, which is accompanied by the dissociation of the axial amine–cobalt bonds. This potential is dependent on the pKa of the axial amines. The second reduction potential of Co(II/I) shows reversible behavior and is also independent of the axial amine pKa. These results indicate the loss of the axial amines in the first redox process and the involvement of a four-coordinate species in the second redox step.Key words: Schiff base, cobalt(III), axial amine, electrochemical properties, crystal structure.

1,2-Bis(1-aryl-3-alkyltriazen-3-yl)ethanes and related compounds

1998 ◽  
Vol 76 (1) ◽  
pp. 125-135 ◽  
Author(s):  
Donald L Hooper ◽  
Ian R Pottie ◽  
Marc Vacheresse ◽  
Keith Vaughan
Keyword(s):  
Nmr Spectroscopy ◽  
Line Broadening ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Ir And Nmr Spectroscopy ◽  
Diazonium Coupling ◽  
Significant Line ◽  
Related Compounds ◽  
C Nmr

A series of novel bistriazenes, the 1,2-bis(1-aryl-3-methyltriazen-3-yl)ethanes, Ar-N T N-NMe-CH2CH2-NMe-N T N-Ar, have been synthesized by diazonium coupling with N,N'-dimethylethylenediamine. These bistriazenes are stable crystalline compounds and have been unequivocally characterized by IR and NMR spectroscopy (1H and 13C), and elemental analysis. The structures of two compounds in the series have been confirmed by X-ray crystallography. The 1H NMR spectra show significant line broadening of the N-methyl resonances arising from the restricted rotation around the N2-N3 bond of the triazene units. The presence of strongly electron-withdrawing groups on the aryl ring restricts the rotation to the point where the N-methyl signals of the rotamers are distinct even at room temperature; four resonances of the N-methyl signal are clearly evident and these can be assigned to the anti-anti, syn-syn, and syn-anti conformations of the bistriazene. Diazonium coupling with N,N'-diethylethylenediamine affords the N,N'-diethyl homologues of the bistriazenes, which have been similarly characterized. As model compounds to assist in spectroscopic analysis, a series of related triazenes, the 1-(1-aryl-3-methyltriazen-3-yl)-N,N-dimethyl-2-ethanamines, were prepared by diazonium coupling with N,N,N'-trimethylethylenediamine. These dialkyltriazenes exist mainly as oils, but characterization was achieved by IR, 1H NMR, and 13C NMR spectroscopy, also showing the presence of two rotamers in solution when strongly electron-withdrawing substituents are bonded to the aryl moiety.Key words: triazene, bistriazene, diazonium, ethylenediamine, molecular dynamics, NMR.

Synthesis of novel α-aminoecdysteroids via regio- and stereoselective oximation/hydrogenation of 20-hydroxyecdysone derivatives

2017 ◽  
Vol 95 (2) ◽  
pp. 130-133 ◽  
Author(s):  
Rimma G. Savchenko ◽  
Svetlana A. Kostyleva ◽  
Ekaterina S. Meshcheryakova ◽  
Leonard M. Khalilov ◽  
Lyudmila V. Parfenova ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Two Dimensional ◽  
One Dimensional ◽  
X Ray ◽  
X Ray Crystallography ◽  
C Nmr

Oximation of 20-hydroxyecdysone oxo derivatives proceeds regio- and stereoselectively and provides (E)-configured oximes in quantitative yields. The Ni–Ra-catalyzed hydrogenation of the oximes affords novel α-aminoecdysteroids with the unchanged 14α-hydroxy-7-en-6-on native chromophore of ecdysteroids. The structures of synthesized compounds were confirmed by the means of homo- and heteronuclear one-dimensional and two-dimensional 1H and 13C NMR spectroscopy and X-ray crystallography.

Synthesis and Crystal Structure of Lead(II) Thenoyltrifluoroacetonate Complexes with Substituted 2,2' -Bipyridines: Interplay of Intermolecular Interactions in Crystals

2010 ◽  
Vol 65 (2) ◽  
pp. 128-134 ◽  
Author(s):  
Farzin Marandi ◽  
Zahra Nikpey ◽  
Jia Hao Goh ◽  
Hoong-Kun Fun
Keyword(s):  
Crystal Structure ◽  
Thermal Analysis ◽  
Nmr Spectroscopy ◽  
Intermolecular Interactions ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
C Nmr

Three substituted 2,2'-bipyridine adducts of lead(II) thenoyltrifluoroacetonate, [Pb(4,4'-dm-2,2’- bpy)(ttfa)2]2, 1, [Pb(5,5' -dm-2,2’-bpy)(ttfa)2]2, 2, and [Pb(4,4'-dmo-2,2’-bpy)(ttfa)2], 3, (4,4’ -dm- 2,2’-bpy, 5,5’-dm-2,2’-bpy, 4,4’-dmo-2,2’-bpy and ttfa are the abbreviations for 4,4’-dimethyl-, 5,5’-dimethyl-, and 4,4’-dimethoxy-2,2’-bipyridine, and thenoyltrifluoroacetonate, respectively) have been synthesized, characterized by elemental and thermal analysis, IR and 1H- and 13C-NMR spectroscopy, and studied by X-ray crystallography. The supramolecular features in these complexes are guided/controlled by weak directional intermolecular interactions.

Synthesis and structural characterization of m-terphenyl Schiff base ligands and their aluminum complexes

2004 ◽  
Vol 82 (9) ◽  
pp. 1346-1352 ◽  
Author(s):  
Diane A Dickie ◽  
Hanifa Jalali ◽  
Rahul G Samant ◽  
Michael C Jennings ◽  
Jason AC Clyburne
Keyword(s):  
Schiff Base ◽  
Schiff Bases ◽  
Structural Characterization ◽  
Condensation Reaction ◽  
Schiff Base Ligands ◽  
X Ray ◽  
X Ray Crystallography ◽  
Aluminum Complexes

2,4,6-Triphenylbenzaldehyde 1 undergoes a condensation reaction with 2-aminophenol to give N-(2′,4′,6′-triphenylbenzylidene)-2-iminophenol (TPIP) 2. The imine 2 can be reduced with NaBH4 in ethanol to form N-(2′,4′,6′-triphenylbenzyl)-2-aminophenol (TPAP) 3. Addition of trimethylaluminum to 2 or 3 results in the formation of the complexes TPIP-AlMe2·AlMe3 (4) or TPAP-AlMe2 (5). Compounds 2, 3, and 4 have been crystallographically characterized.Key words: N,O ligands, aluminum, m-terphenyl, Schiff bases, X-ray crystallography.

scholarly journals Synthesis, characterization and crystal structures of the bidentate Schiff baseN,N′-bis(2-nitrocinnamaldehyde)ethylenediamine and its complex with CuNCS and triphenylphosphane

2015 ◽  
Vol 71 (7) ◽  
pp. 578-583 ◽  
Author(s):  
William Clegg ◽  
Ross W. Harrington ◽  
Kazem Barati ◽  
Mohammad Hossein Habibi ◽  
Morteza Montazerozohori ◽  
...  
Keyword(s):  
Schiff Base ◽  
Nmr Spectroscopy ◽  
Nitro Group ◽  
Bidentate Ligand ◽  
Molar Ratio ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Bite Angle ◽  
Elemental Analyses

Reaction of copper(I) thiocyanate and triphenylphosphane with the bidentate Schiff baseN,N′-bis(trans-2-nitrocinnamaldehyde)ethylenediamine {Nca2en, (1); systematic name (1E,1′E,2E,2′E)-N,N′-(ethane-1,2-diyl)bis[3-(2-nitrophenyl)prop-2-en-1-imine]}, C20H18N4O4, in a 1:1:1 molar ratio in acetonitrile resulted in the formation of the complex {(1E,1′E,2E,2′E)-N,N′-(ethane-1,2-diyl)bis[3-(2-nitrophenyl)prop-2-en-1-imine]-κ2N,N′}(thiocyanato-κN)(triphenylphosphane-κP)copper(I)], [Cu(NCS)(C20H18N4O4)(C18H15P)] or [Cu(NCS)(Nca2en)(PPh3)], (2). The Schiff base and copper(I) complex have been characterized by elemental analyses, IR, electronic and1H NMR spectroscopy, and X-ray crystallography [from synchrotron data for (1)]. The molecule of (1) lies on a crystallographic inversion centre, with atransconformation for the ethylenediamine unit, and displays significant twists from coplanarity of its nitro group, aromatic ring, conjugated chain and especially ethylenediamine segments. It acts as a bidentate ligand coordinatingviathe imine N atoms to the CuIatom in complex (2), in which the ethylenediamine unit necessarily adopts a somewhat flattenedgaucheconformation, resulting in a rather bowed shape overall for the ligand. The NCS−ligand is coordinated through its N atom. The geometry around the CuIatom is distorted tetrahedral, with a small N—Cu—N bite angle of 81.56 (12)° and an enlarged opposite angle of 117.29 (9)° for SCN—Cu—P. Comparisons are made with the analogous Schiff base having no nitro substituents and with metal complexes of both ligands.

2,2'-Bipyridine Mercury(II) Complexes [Hg(bpy)(NO2)X] (X = NO2 –, SCN– , CH3COO–); Π-Π Stacking In The Crystal Structure Of [Hg(bpy)(NO2)2]

2005 ◽  
Vol 60 (3) ◽  
pp. 289-293 ◽  
Author(s):  
Ali Ramazani ◽  
Ali Morsali ◽  
Leila Dolatyari ◽  
Bijan Ganjeie
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Aromatic Rings ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Π Stacking ◽  
Π Stacking Interaction ◽  
Coordinate Geometry ◽  
C Nmr

The mercury(II) complexes of 2,2′-bipyridine (bpy), [Hg(bpy)(NO2)2], [Hg(bpy)(NO2) (CH3COO)], and [Hg(bpy)(NO2)(NCS)] have been synthesized and characterized by elemental analysis, IR, 1H NMR and 13C NMR spectroscopy. The structure of [Hg(bpy)(NO2)2] has been confirmed by X-ray crystallography. The complex is a monomer and the Hg atom has an unsymmetrical six-coordinate geometry, formed by two nitrogen atoms of the bpy ligand and four oxygen atoms of the two nitrite anions. There is a short intermolecular π-π stacking interaction between parallel aromatic rings

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