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.

[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.

The reaction of chloro(triphenylphosphine)gold(I) with 1-methylthymine

1987 ◽  
Vol 65 (7) ◽  
pp. 1568-1575 ◽  
Author(s):  
R. Faggiani ◽  
H. E. Howard-Lock ◽  
C. J. L. Lock ◽  
M. A. Turner
Keyword(s):  
Aqueous Methanol ◽  
Orthorhombic Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Cell Dimensions ◽  
Cell Data ◽  
Unit Cell Data ◽  
Related Compounds ◽  
C Nmr

1-Methylthyminato-N3-triphenylphosphinegold(I) was prepared by reacting chloro(triphenylphosphine)gold(I) with 1-methylthymine in aqueous methanol at pH 11. The product was examined by X-ray crystallography and was found to have the orthorhombic space group C2221 (no. 20) with cell dimensions a = 12.760(7) Å, b = 11.530(2) Å, c = 31.893(5) Å, and eight formula units in the unit cell. Data were collected with use of MoKα radiation and a Syntex P21, diffractometer. The crystal structure was determined by standard methods and refined to R = 0.112 and Rw = 0.076 on the basis of 4760 unique reflections. Bond lengths and bond angles are normal. Packing in the crystal lattice is dominated by the triphenylphosphine rings which arrange roughly as blades of a propellor and are the source of the crystal's chirality. The title and related compounds were also examined by 1H nmr, 13C nmr, and vibrational spectroscopy.

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

2,9-Dimethyl-1,10-phenanthroline as Ligand in the Holo- and Hemidirected 1:1 and 1:2 Lead(II) Complexes

2005 ◽  
Vol 60 (2) ◽  
pp. 149-154 ◽  
Author(s):  
Ali Morsali
Keyword(s):  
Nmr Spectroscopy ◽  
Single Crystal ◽  
Elemental Analysis ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Coordinate Geometry ◽  
C Nmr

1:1 and 1:2 lead(II) complexes with 2,9-dimethyl-1,10-phenanthroline (Dmphen), {[Pb(Dmphen)(NO3)n] and [Pb(Dmphen)2(ClO4)2]} have been synthesized and characterized by CHN elemental analysis, IR, 1H NMR, 13C NMR and 207Pb NMR spectroscopy. The structure of these complexes was confirmed by X-ray crystallography. The single crystal X-ray data of [Pb(Dmphen)(NO3)n] show the complex to be polymeric and the Pb atom to have an unsymmetrical eight-coordinate geometry, the coordination being holodirected, whereas the [Pb(Dmphen)2(ClO4)2] complex is monomeric and the Pb atom has an unsymmetrical eight-coordinate geometry with the coordination hemidirected.

Synthesis, Characterization and Complexation Studies with K + and Ca2+ Cations of trans-1.2-Cyclohexanedioxydiacetamides

1988 ◽  
Vol 43 (2) ◽  
pp. 165-170 ◽  
Author(s):  
Whei Oh Lin ◽  
Maria C. B. V. de Souza ◽  
Helmut G. Alt
Keyword(s):  
Nmr Spectroscopy ◽  
Mass Spectroscopy ◽  
H Nmr ◽  
Coordination Sites ◽  
Complexation Studies ◽  
Ir And Nmr Spectroscopy ◽  
Elemental Analyses ◽  
C Nmr

The synthesis of trans-1.2-cyclohexanedioxydiacetamides starting with trans-1.2-cyclohexane-diol is described. Eleven of these compounds are characterized by IR, 1H NMR, 13C NMR and mass spectroscopy as well as elemental analyses. Most of these compounds are suitable ionophors for the cations K+ and Ca2+. The coordination sites of these ligands in the 1:2 complexes were determined by IR and NMR spectroscopy

scholarly journals Synthesis and characterization of a new bis-NHC palladium complex and its catalytic activity in the Mizoroki–Heck reaction

2020 ◽  
Vol 44 (11-12) ◽  
pp. 684-688
Author(s):  
Can Feng ◽  
Cheng-xin Liu ◽  
Yu-fang Wang ◽  
Jin Cui ◽  
Ming-jie Zhang
Keyword(s):  
Palladium Complex ◽  
Coupling Reaction ◽  
Aryl Halides ◽  
Heck Coupling ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Excellent Stability ◽  
C Nmr

A new bis- N-heterocyclic carbene palladium complex, (C13H9N2F2)2PdCl2, is synthesized by a three-step reaction and characterized by 1H NMR and 13C NMR spectroscopy as well as by X-ray crystallography. This new bis- N-heterocyclic carbene palladium complex has excellent stability and is capable of efficiently catalyzing the Mizoroki–Heck coupling reaction of aryl halides with acrylates.

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.

Synthesis and characterization of silver(I) complexes of thioureas and thiocyanate: crystal structure of polymeric (1,3-diazinane-2-thione)thiocyanato silver(I)

2015 ◽  
Vol 70 (8) ◽  
pp. 541-546 ◽  
Author(s):  
Muhammad Nawaz Tahir ◽  
Anvarhusein A. Isab ◽  
Fozia Afzal ◽  
Kashif Raza ◽  
Shah Muhammad ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Nmr Spectrum ◽  
Coordination Environment ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Ir And Nmr Spectroscopy ◽  
A Chain ◽  
Distorted Tetrahedral Coordination ◽  
C Nmr

AbstractSilver(I) complexes of thioureas and thiocyanate, [(Tu)AgSCN], [(Metu)AgSCN], [(Dmtu)AgSCN], [(Tmtu)(AgSCN)1.5], [(Imt)AgSCN], and [(Diaz)AgSCN] (where Tu = thiourea, Metu = N-methylthiourea, Dmtu = N,N′-dimethylthiourea, Tmtu = N,N,N′,N′-tetramethylthiourea, Imt = 1,3-imidazolidine-2-thione, and Diaz = 1,3-diazinane-2-thione), have been prepared and characterized by elemental analysis, IR and NMR spectroscopy, and thermal analysis. The crystal structure of one of them, [(Diaz)Ag(SCN)] (1), was determined by X-ray crystallography. The crystal structure of 1 shows that the complex exists in the form of a chain-like polymer comprising [Ag(μ2-Diaz)(μ2-SCN)] units. The silver atoms are bridged by μ2-thione sulfur atoms of Diaz and μ2-thiocyanate sulfur atoms. Thereby each silver atom adopts a distorted tetrahedral coordination environment comprising four sulfur atoms, two from thione and two from thiocyanate ligands. An upfield shift in the >C=S resonance of thiones in 13C NMR and a downfield shift in the N–H resonance in 1H NMR are consistent with the sulfur coordination to silver(I). The appearance of a band around 2100 cm–1 in the IR and a resonance around 125 ppm in the 13C NMR spectrum indicates the binding of thiocyanate to silver(I).

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.

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